July / August 2016 NLGI Spokesman

NLGI

SPOKESMAN

Serving the Grease Industry Since 1933 – VOL. 80, NO. 3, JULY/AUGUST 2016

In this issue . . .

8 2016 NLGI Awards 14 Open Gear Lubricants Exploring the Depths of a Technology in a Constant Evolution 34 Reducing Fire Hazards in Mining with Fire Resistant Grease 44 The Development of More Environmentally Considerate Greases

2016-2017 Board of Directors Picture taken at the 83rd Annual Meeting, Hot Springs, VA

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NLGI

OFFICERS PRESIDENT:

VICE PRESIDENT:

David Como Dow Corning Corp.

P.O. Box 0994 Midland, MI 48686

Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

SECRETARY:

TREASURER:

Jim Hunt Tiarco Chemical 1300 Tiarco Drive Dalton, GA 30720

Dr. Anoop Kumar Royal Manufacturing Co., LP 516 S, 25th West Ave. Tulsa, Oklahoma 74127

PAST-PRES./ADVISORY:

EXECUTIVE DIRECTOR:

Chuck Coe Grease Technology Solutions LLC 7010 Bruin Ct. Manassas, VA 20111

Kimberly Hartley NLGI Inter­national Headquarters 249 SW Noel, Suite 249 Lee’s Summit, MO 64063

Richard Burkhalter Covenant Engineering Services 140 Corporate Place Branson, MO 65616 Faith Corbo King Industries, Inc. Science Road Norwalk, CT 06852 Gary Dudley Exxon Mobil Corporation 3225 Gallows Road Room 7C1906 Fairfax, VA 22037 Gian L. Fagan Chevron Lubricants 100 Chevron Way Room 71-7338 Richmond, CA 94802-0627 Tyler Jark Lubricating Specialties Co. 8015 Paramount Blvd.

Pico Rivera, CA 90660 Wayne Mackwood Chemtura 199 Benson Rd. Middlebury, CT 06749 Dwaine (Greg) Morris Shell Lubricants 526 S. Johnson Drive Odessa, MO 64076

Serving the Grease Industry Since 1933 – VOL. 80, NO. 3, JULY/AUGUST 2016

Tom Schroeder Axel Americas, LLC P.O. Box 12337 Kansas City, MO 64116

4 President’s Podium 8 2016 NLGI Awards 14 O pen Gear Lubricants Exploring the Depths of a

Raj Shah Koehler Instrument Co. 85 Corporate Dr. Holtsville, NY 11716-1796

DIRECTORS Barbara Bellanti Battenfeld Grease & Oil Corp. of NY P.O. Box 728 • 1174 Erie Ave. N. Tonawanda, NY 14120-0728

SPOKESMAN

Dr. Huafeng “Bill” Shen Bel-Ray Co. P.O. Box 526 Farmingdale, NJ 07727 Terry Smith Lubrication Engineers, Inc. P.O. Box 16447 Wichita, KS 67216 Thomas W. Steib The Elco Corporation 1000 Belt Line Street Cleveland, OH 44109 Lisa Tocci Lubes ’n’ Greases 6105 Arlington Blvd., Suite G Falls Church, VA 22044 Mike Washington The Lubrizol ­Corpo­ration 29400 ­Lakeland Blvd.

Mail Drop 051E Wickliffe, OH 44092 Ruiming “Ray” Zhang R.T. Vanderbilt Company, Inc. 30 Winfield St. Norwalk, CT 06855

Dennis Parks Texas Refinery Corp.

One Refinery Place Ft. Worth, TX 76101

Technology in a Constant Evolution

28 Blast from the Past 30 NLGI Member Spotlight 32 Ask the Expert 34 Reducing Fire Hazards in Mining with Fire Resistant Grease

Joel Garrett, Brian Cichoski, Brian Kusak, Matt Bailey, Kevin Dickey

40 New 2016 NLGI Members 44 T he Development of More Environmentally

TECHNICAL COMMITTEE CO-CHAIRS:

CHAIR, SESSION PLANNING:

Chad Chichester Dow Corning Corporation 2200 W. Salzburg Rd., C40C00 Midland, MI 48686

Wayne Mackwood Chemtura 199 Benson Rd. Middlebury, CT 06749

Hocine Faci, Martin Maass, John Haspert, Soman Dhar

Considerate Greases

Gareth Fish, PhD CLS CLGS

56 NLGI Industry News 59 Advertiser’s Index

David Turner CITGO 1293 Eldridge Parkway Houston, TX 77077

SERVICE INDUSTRY ASSISTANCE COMMITTEE CHAIR: J im Hunt Tiarco Chemical 1300 Tiarco Drive Dalton, GA 30720

EDITORIAL REVIEW COMMITTEE CHAIR: Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

NOTE: Due to various personal issues, Kim Smallwood of CITGO, has resigned from the NLGI Board of Directors. NLGI wishes him well.

ON THE COVER 2016-2017 Board of Directors

Published bi-monthly by NLGI. (ISSN 0027-6782) KIMBERLY HARTLEY, Editor NLGI International Headquarters 249 SW Noel, Suite 249, Lee’s Summit, MO 64063 USA Phone (816) 524-2500, FAX: (816) 524-2504 Web site: http://www.nlgi.org — E-mail: nlgi@nlgi.org One-year subscriptions: U.S.A. $65.00; Canada $80.00; International $109.00; Airmail $147.00. Claims for missing issues must be made within six months for foreign subscribers and three months for domestic. Periodicals postage paid at Kansas City, MO. The NLGI Spokesman is indexed by INIST for the PASCAL database, plus by Engineering Index and Chemical Abstracts Service. Microfilm copies are available through University Microfilms, Ann Arbor, MI. The NLGI assumes no responsibility for the statements and opinions advanced by contributors to its publications. Views expressed in the editorials are those of the editors and do not n­ ecessarily represent the official position of NLGI. Copyright 2015, NLGI. Postmaster: Send address corrections to the above address.

PRESIDENT’S PODIUM Joe Kaperick Afton Chemical Corp.

NLGI Vice-President

Recap of the 2016 83rd Annual Meeting NLGI 2016 – Revolutions in Grease

The 83rd NLGI Annual Meeting was held at the Homestead Resort in the beautiful Shenandoah mountain town of Hot Springs, Virginia on June 11-14, 2016. The resort celebrated its 250th anniversary just days before our event and inspired this year’s theme, “Revolutions in Grease – Changing Technology for Changing Times”. Authors were solicited for research and presentations that challenged the existing way of thinking with regard to new thickeners, additives or improved test methods as well as novel applications or improved manufacturing techniques and an everchanging regulatory environment. Our keynote speaker, Graham Gow, touched on many of these subjects with his recap of a truly historic career in his presentation “Amazing Grease: Tales from a 36 year (R)evolution in our Industry”. The technical portion of the program was kicked off by our industry speaker, Carl Stevens, the equipment manager for the Lynchburg district

of the Virginia Department of Transportation. Mr. Stevens is responsible for maintenance of a fleet worth $35 million and gave a very interesting presentation on the implementation of their Reliability Centered Maintenance program with many examples focused on grease lubrication. Although the theme was “revolutionary”, the basics of the meeting were “tried and true”: great participation in the Working Groups, excellent technical sessions and networking opportunities galore.

Medals of Honor

Awards presented for best technical papers from the 2015 meeting continued to highlight new ideas and technology in the grease industry. The winners of the two NLGI Author awards were John Lorimor (Axel Americas - “Development of next generation electrical motor greases offering improved frictional characteristics”) for Development and Jason Galary (Nye Lubricants - “Investigation into the Dynamic Particle Generation of Lubricating Greases”) for Applications.

Andy Waynick (NCH Corporation) was recognized for his work on “Calcium Biederman Plastic Sulfonate Complex Greases Using Grease Cartridges Calcium Hydroxyapatite as a HydroxideContaining Basic Reactant” with the Clarence E. Earle Award for Contribution to Technical Literature. Additionally, several members were recognized for their service to NLGI and the industry, while a new NLGI Founders Award was introduced which honors a company that Less Damage + Less Leakage has had a positive impact on the NLGI + Less Scrap in the tradition established by its three founding fathers. Battenfeld Oil and = Superior quality and Grease was honored with this award in its cost savings! inaugural year.

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With a total attendance of 384 plus 78 guests at this year’s meeting, NLGI

maintained its international flavor by attracting attendees from such areas as Australia, China, Sweden, India and the United Kingdom. Additionally, Terry Dicken, chairman of ELGI (the European counterpart of NLGI) and Dr. E. Sayanna, Vice President of NLGI’s Indian Chapter, both addressed the conference with updates from their respective organizations, while NLGI Board Member Ray Zhang brought news from the Chinese Lubricating Grease Institute (CLGI).

Working toward Change

Members of the Working Groups that are sponsored by both NLGI and ELGI continued to make advances in several different areas.

Meetings of each of the Joint Working Groups (Food Grade, Grease Particle Evaluation, and Bio-Based) were held with continued progress in each. All of these groups draw their membership from both ELGI and NLGI with sessions being held in Europe and North America. The newest Working Group was started by NLGI last year to update its Automotive Service Grease specification. All of these groups are chaired by volunteers from within the industry and are aimed at addressing current topics of real interest and concern to the global grease community. Those with an interest in participating more fully in any of these discussions should contact the respective chairs which are posted on the NLGI website along with the latest minutes from each of the meetings.

Revolutions per Year

For those interested in learning more about grease issues in various regions, meeting new potential customers outside of the United States or looking for information on the latest revolution in grease technology, the opportunities continue to abound. NLGI-India Chapter will hold their 19th Annual conference in Varanasi, India on February 2-4, 2017, while ELGI will host their 29th Annual General Meeting on May 6-9, 2017 in Helsinki, Finland. Finally, NLGI’s next Annual Meeting will be held on June 10-13, 2017 in the Lake Tahoe region at the Resort

at Squaw Creek. All of these meetings welcome technical contributions and attendees from all over the globe.

So while the roots of the Homestead Resort go back to Revolutionary times, new and ever-changing technologies on the grease frontier present us with our own opportunities for revolution on a smaller scale. The Annual Meeting continues to offer fantastic networking opportunities in historic venues for friends and foe alike.

And learning the news of the battles on the research frontier is much easier now with the technical expertise and content that is available at the Annual meeting or readily accessible on the NLGI website - much easier than having to wait for the town crier to pass on the news!

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2016

NLGI AWARDS John A. Bellanti, Sr. Memorial Meritorious Service Award This award acknowledges meritorious service on the NLGI Board, or on Technical Committee projects or to the industry.

Jim Hunt, Tiarco Chemical

Jim Hunt obtained his Associates in Computer Engineered Science in 1985. He has been the Global Sales and Marketing Director for Tiarco Chemical for almost 15 years. It was Jim’s initial vision and passion that drove the decision for Tiarco Chemical to be directly involved in the global grease and lubricant market with their specially additives many years ago. Jim began his career in the paint and coatings market in the early 80's. After only a few years in QC and operations, Jim was promoted to General Manager of Chemex Paints in 1986 and ran all operations for 2 years until he transitioned into to chemical distribution sales. Jim began his sales career at Lomas International more than 25 years ago. Jim was awarded Salesman of the Year Honors as well as outstanding business development awards from suppliers including Wacker Silicones. Jim also worked for Cytec's Polymer Additives business for over 4 years once again achieving excellent sales and outstanding performance in development of new business in the plastics market. Jim was elected in June 2016 as Treasurer of the NLGI Board of Directors. He is also a long-standing member of STLE and ILMA.

-8VOLUME 80, NUMBER 3

NLGI Fellow Award

The award acknowledges valuable work within the Institute, in the technical development of greases, grease tests, or the promotion of grease usage.

Jaime Spagnoli, ExxonMobil Research & Engineering

Jaime received his B.S. in Engineering Technology from Trenton State College, New Jersey. He has spent Thirty-nine years working at ExxonMobil in technical services and lubricant research and development with over 25 years of experience in grease R&D. He is currently working as a Senior Researcher in the Industrial Lubricants & Grease Section at ExxonMobil Research and Engineering. He is a member and active participant in STLE, NLGI and ELGI activities and past Chairman of ASTM Sub Committee G. He is the recipient of the NLGI Chevron Lubricants Author Award and the NLGI Shell Lubricants Award for Instructor Excellence. He is also the recipient of the ELGI Best Paper award in 2012. He is an NLGI Certified Lubricating Grease Specialist (CLGS).

NLGI Author Award – Development Sponsored by Royal Mfg. Co. LP

This award is for the best paper presented at our 2015 Annual Meeting that focuses on formulation, development and manufacture of finished greases.

John Lorimor, Axel Americas (with co-authors Mihir Patel, Rob Heverly and Brian Stunkel)

“Development of next generation electrical motor greases offering improved frictional characteristics”

John is currently Technical Director for AXEL Americas LLC. John’s primary responsibility is the strategic management of AXEL technical resources, specifically focused on driving new product innovation in commercially targeted areas, optimization of product formulation and manufacturing processes, and ensuring successful transfer of technology within the AXEL group of grease manufacturing plants. Over a 22-year career, John has held a variety of technical and commercial leadership roles at some of the most well-known companies in the grease and additives industry. John received his bachelor degree in Chemical Science from Kansas State University in 1994, and MBA from the University of Phoenix in 2001. He has authored and presented numerous papers at NLGI on grease product development, and was also previously recognized with the NLGI Author Award at its 2010 annual meeting. John is an STLE Certified Lubrication Specialist (C.L.S.®), and was among the first recognized by NLGI as Certified Lubricating Grease Specialist (CLGS®).

NLGI Author Award – Application Sponsored by Chevron Global Lubricants

This award is for the best paper presented at our Annual Meeting that focuses on testing, selection, application or use of greases.

Jason Galary, Nye Lubricants

“Investigation into the Dynamic Particle Generation of Lubricating Greases”

Jason is currently the Engineering Development and Application Manager at Nye Lubricants located in Fairhaven, Ma where he has over 18 years working in the lubrication industry. He graduated from the University of Massachusetts at Dartmouth with a Bachelor’s degree in Electrical Engineering and a Master’s degree in Mechanical Engineering.

Currently he is working on his Doctoral Degree in Engineering and Applied Science. Jason is the founder of the ADVT (Application Development and Validation Testing) Laboratory where the focus is on developing new testing equipment and methods to simulate real world lubricant applications and environments. He has authored or co-authored over 10 Technical Research publications and presentations. His research interests currently include mechanical fretting, dynamic particle generation of lubricants, vacuum tribology, and life modeling of lubricating greases.

- 10 VOLUME 80, NUMBER 3

Clarence E. Earle Memorial Award Sponsored by Rockwood Lithium This award is for an outstanding contribution to the technical literature relating to lubricating greases during the year.

J. Andrew Waynick, NCH

“Calcium Sulfonate Complex Greases Using Calcium Hydroxyapatite as a Hydroxide-Containing Basic Reactant”

Andy Waynick received his B.A. in Chemistry in 1974 from Central Methodist College, and his M.S. in Physical Chemistry in 1977 from Purdue University. For the 39 years since that time, Andy has been a professional research chemist. For more than 36 of those years he has been involved in fluid lubricants, greases, fuels, and fuel additives. Andy’s work includes 17 years at Amoco Oil Company and more than 7 years as a senior research scientist at Southwest Research Institute. His primary areas of responsibility have been and continue to be technology and product development and technical problem solving. Andy has developed commercially successful lubricating greases for automotive CV joints, sealed-for-life automotive wheel bearings, and rail track/wheel flange grease. One of the more interesting projects that Andy completed was the development of an extremely high performance polyurea U-joint grease that allowed a major automotive manufacturer to use the U-joint from a compact car in their heavy-duty 4x4 pickup truck. Andy developed the first documented commercially successful polyurea thickened grease for steel mill continuous caster bearings. Under contract with the U.S. military, Andy developed a lithium-based grease for the engine thrust bearings used in strategic cruise missiles that resulted in a new MIL spec written specifically for it. Sponsored by and in cooperation with South Dakota School of Mines and Technology, Andy developed the first lubricating greases thickened in part or entirely by carbon nanotubes. At the invitation of the editor of ACS peer-reviewed journal “Energy and Fuels”, Andy submitted and had published the only review article ever written on the development and use of metal deactivating additives in the petroleum industry. Andy has 31 U.S. patents and at least as many published research papers.

- 11 NLGI SPOKESMAN, JULY/AUGUST 2016

Award for Education Excellence Sponsored by SOPUS Products

This award is for outstanding instruction as exemplified by subject knowledge and presentation skills in NLGI Educational Courses.

Carl Wainwright, ExxonMobil Fuels, Lubricants & Specialties Marketing Company

Carl graduated from the Rutgers University College of Pharmacy in New Brunswick, New Jersey in 1990, interning at the United States Veteran’s Administration and Rhone Poulenc Rorer Pharmaceuticals.

He joined Mobil Oil’s Environmental and Health Sciences Laboratory in Princeton, New Jersey in June 1990, responsible for the formulation and analytical testing of materials for toxicology and environmental assessments.

In 1997, Carl transferred to the Product Safety Department at Mobil, supporting lubes product development at the Mobil Technology Center in Paulsboro, New Jersey, working with lubes formulators to mitigate health, safety and regulatory concerns prior to commercialization.

After the merger with Exxon, Carl assumed the role as Global Formulation Disclosure Advisor for the ExxonMobil Lubes business. He coordinated the health, safety and regulatory support relating to customer and government agency enquiries.

In 2011, he was promoted to the Americas Lubes Product Stewardship Advisor, ensuring regulatory compliance, including all GHS implementations in the Americas zone.

He has been an instructor at NLGI for the past 10 years, providing the Environmental and Safety module in the Basic Grease Course and recently, the H1 Incidental Food Contact module for the Advanced Grease Course.

NLGI Founders Award (New in 2016)

In recognition of the three NLGI founding Companies, the Founders Award is presented to a company that has had a positive impact on the NLGI in the tradition established by its founding fathers.

Battenfeld Grease & Oil Corporation of New York

Barbara Bellanti accepted this award on behalf of Battenfeld Grease & Oil Corporation of New York, for the leading role Battenfeld has taken in the development and promotion of NLGI for many decades. NLGI recognizes Battenfeld Grease & Oil Corporation of New York for their continuous support and dedication to the institute.

- 12 VOLUME 80, NUMBER 3

NLGI Honorary Membership

This award entitles lifetime honorary membership to those who, over a period of years, have served the Institute in some outstanding capacity and are not now with a member company.

Terry Smith, Lubrication Engineers (Retired)

Tom Pane, King Industries (Retired)

Bill Ward, Lubrizol (Retired)

- 13 NLGI SPOKESMAN, JULY/AUGUST 2016

OPEN GEAR LUBRICANTS Exploring the Depths of a Technology in a Constant Evolution By: Hocine Faci, Martin Maass, John Haspert, Soman Dhar Castrol Industrial

Abstract

Unlike underground mining operations, open pit mining is a surface mining technique that allows extraction of mineral ores or rocks from the ground of an open pit. This technique requires usage of heavy pieces of equipment, namely shovels and draglines. Shovels, usually electrically powered, are used for removing dirt from the earth with the help of a hydraulic bucket.

Draglines are much larger in size and are commonly used in strip-mining operations. These machines are equipped with numerous rotating components, including open gears, and require lubrication under extremely harsh conditions. Load carrying capacity, wear protection, water resistance, adhesiveness, dust tolerance as well as mobility are the most critical characteristics for an open gear compound. The lubricant technology associated with this application has significantly evolved over the last decades.

This paper will cover the journey of this technology as the OEM specifications evolved over time; from the first heavy open gear compounds and the solid highly fortified lubricants, to the solvent based and lately solvent free compounds ‌and onto the bio-based and environmentally friendly lubricants Introduction Open pit mining is a surface mining technique that allows extraction of mineral ores from the ground of an open pit. To mine the ore, it is generally necessary to excavate, remove and relocate immense quantities of “overburdenâ€? as waste rocks (or dirt).

Mining economics are directly dependent of the handling and storing of these rock quantities, constrained

frequently by certain geologic and mining engineering challenges. Minerals and waste are removed in successive layers forming mine benches at different elevations. This technique requires the use of heavy pieces of equipment, namely shovels and draglines. Shovels, usually electrically powered, are used for removing the dirt from earth with the help of a hydraulic bucket. The large type of draglines which are typically built on site are commonly used in strip mining operations to remove dirt above minerals or coal and more recently for oil sands mining . Their weight can vary between 8,000 and 13,000 tons. These massive machines are equipped with numerous rotating components, including open gears and guide rails, and require lubrication under extremely harsh conditions.

Load carrying capacity, wear protection, water resistance, adhesiveness, dust tolerance as well as mobility are the most critical characteristics for an open gear compound.

The lubricant technology associated with this application has significantly evolved over the last decades.

Background

Dirt removal operations for the pyramid building during the ancient Egyptian era go back to the 17th Century BC. Based on archaeological discoveries, construction crews used to remove the stones from open caverns and move them to the construction site using wet sand, fine clay, gypsum. Olive oil was in use as lubricant in the same era (Figure 1). Since 50 A.D., various other oils obtained from palm oil, castor beans, rapeseed, etc. were used until the early period of the 19th century [1, 2, 3].

Three to four centuries later, beef and mutton fat (tallow), animal lard, wool grease, and sperm whale oil to name a few were used. Sometimes, vegetable oils and

- 14 VOLUME 80, NUMBER 3

plant based materials were also employed as materials.

Persian chariots and windmills used vegetable oils or animal fats to lubricate the rotating component axles [4] (Figure 2).

Petroleum Lubrication Era

Even after the discovery of the petroleum in abundant quantities (drilling of first oil wells in Pennsylvania in 1850’s [5, 6]), lubricants continued to be made mainly from vegetable oils and animal fat. The raw crude oil did not make a good lubricant as it could not perform as well as the “conventional” vegetable oils and animal

fat. Towards the end of the 19th century, Asphaltic compounds originated from heavy petroleum were used to lubricate the carts, wagons and other rotating equipment. In 1856, the first industrial refinery was built on the outskirts of Ploiesti, Romania (Figure 3). Early Refinery installations were quite primitive. Cylindrical vessels were made with cast iron and directly heated with wood fire to make lighter fractions that would be used for domestic illumination. The residual material remaining after removal of light fractions was used as is for lubrication of heavy rotating

machinery [5, 6].

In 1920’s, Solvent Refining emerged as one of the most viable processes to make the first petroleum distillates from paraffinic crudes. This Process (Figure 5) is still in use to make the API Group 1 base oils. The Solvent Refining process.

With the increase of automotive demand for both improved fuels and Higher Performance lubricants, refiners investigated petroleum refining as a potential source of lubricants, should the refining processes be capable of providing heavier and narrower cuts of distillates. The notion of viscosity ranges became key criteria for the classification of base oils beginning in the 1920s. For automotive engines, base oils were categorized as Light, Medium or Heavy oils by the Society of Automotive Engineers (SAE) classification. These early oils did not contain any additives.

Effectively until the 1930’s, lubrication was achieved using neat oils [7]. Selection of the lubricating oil grade was based mainly on whether the lubricated system was closed or open, operated in a low or high ambient temperature, a reciprocated oscillating mechanism or uni-directional rotational system, rotating at high, medium or low speed and; finally, whether the system is operating under high loads and shock loading. These criteria determined the selection of the base oil grades

more robust lubricant formulations with superior performance properties and improved mobility. These lubricants also needed to be dispensed through newly adopted centralized lubrication systems.

Lubrication on drilling machinery, percussion type or rotary drills where gears are involved, was achieved by the application of a soft grease or petrolatum for the gears and oil for the cylinders [7]

Additive era ranging from Light to Medium to Heavy or even to asphaltic compounds [8].

As the country embraced for the war in the early 1940s, Iron Ore became an important source required for making the large supply of steel required for the military. Iron ore along with coal mining in open pits which spread across a good part of the North American land, called for more sophisticated excavating machines.

The invention of the dragline and Power Shovel goes back to the late years of the 19th century and the early years of the 20th century. Page Engineering, Monigan, P&H, Bucyrus-Erie, Marion Power and R&R as well as Caterpillar were considered founding pillars of the draglines and shovels industry. Generalization of the

The additive chemistry started to flourish between the 2 World Wars. Corrosion inhibitors, oxidation inhibitors, pour point depressants and more emerged in the early 1930s. In the 1940, other additive technologies especially those that prolong oil performance and service life were in extensive use in vehicle engine oils. Antiwear and extreme pressure additives were then incorporated into nearly every lubricant destined for heavy duty operation equipment such as in the military heavy vehicles, mining, metal and cement factories.

Lubrication of Open Gear Systems

Excavating machines used in open pit mining operation have typically type 1 open gear drives which consist of a pinion and a rack system for the transmission of the power (Figure 8). This configuration is mainly used on electrical shovels cable hoist drums, swing motion drives, and in the hoist and drag drives of mining shovels and draglines. These open gears are challenged by the bi-direction motion. The gear teeth operate with thin lubrication film (under boundary lubrication regime)

usage of these pieces equipment coincided with the industrial revolution supported significantly by the developing petroleum industry. Draglines and Shovels (Figures 6 and 7) became larger and heavier demanding - 16 VOLUME 80, NUMBER 3

and constantly with intermittent loading. The lubricant assures reduction of friction and protection against wear at the meshing gear tooth surfaces and act as cushion against repeated shock loading.

Key Characteristics for Open Gear Compounds: • Tackiness / adhesion to adhere to gear teeth in vertical position • Resistance to high loads and shock loading • Strong film under starved conditions • Resistance to water spray off • Ability to cushion vibration • Protection against wear (even in presence of large amount of mining dust) • Protection against corrosion • Good sprayability / spreadability / mobility at low ambient temperatures • Good thermal retention at high ambient temperatures Industry specifications and standards for open gear lubricants have been around for a number of years.

Active in the development of specifications are the American Gear Manufacturers Association (AGMA) and other Original Equipment Manufacturers (OEM’s); such as (Bucyrus, P&H, Komatsu). The early standards were targeting mainly a minimum kinematic viscosity, a minimum load carrying capacity determined by Timken (Figure 9), FZG test (Figure 10) , or Four ball EP (Figure 11) or combinations of these tests. Pumpability per

Lincoln Ventmeter (Figure 12) was a key test parameter required for all lubricants formulated for the cold areas applications.

The formulations of open gear Compounds during these periods were typically based on heavy oils (resin and asphaltic materials) in combination with light naphthenic oils and solvent, fortified with large amounts of solids additives either for thickening capacity or for boosting the load carrying capacity. Liquid additives for wear, oxidation and corrosion protection were being expanded from use in motor oils to the gear oils and subsequently greases and open gear compounds technologies.

of solvent was necessitated for easing the pumping properties especially for those that are dispensed through automatic lubrication systems on equipment operated in cold zones. The solvent sprayed on the gear teeth, evaporates leaving behind a thick, dry film on the surface. The evaporation rate is influenced by ambient temperature, wind conditions, amount of the dispensed product and the frequency of its application. Additives associated with metals such as antimony, zinc, zirconium, lead, copper, tin and boron were quite popular in more than one application.

Asphaltic compounds, which were obtained from the distillation of residua, or from the de-asphalting process, (Figure 5) became more popular in the formulation of open gear compounds. This material displays an excellent water resistance, tackiness and adhesion. Being highly concentrated in sulfur components, it provides the open gear compound improved load carrying capacity and to some extent oxidation resistance properties.

The Resin materials are typically much lighter than the asphaltic compound, therefore the resins find their use in lubricants destined to moderately loaded applications and warm to mild ambient temperatures.

The soft nature and fluidity of the open gear compounds (NLGI 0-00) can be achieved with minimum content of thickening material, and this content is even smaller when using thickeners with high thickening capacity. Carbon black, bentonite and fumed silica were among the preferred materials for this function. They have relatively large surface area to adsorb sufficient oil for adequate lubrication. Graphite was in more instances added to boost the load carrying capacity but also for thickening the grease at the same time. Other solids such as copper flakes, aluminum flakes, calcium carbonates, calcium hydroxides, talc, mica, zinc dust, and metal oxides or sulfides were also commonly used to enhance the load carrying capacity. Some of these materials have demonstrated some synergy with a number of sulfurized type additives.

The grease compositions reflect also a good number of solvents varying between chlorinated materials and later replaced by organic hydrocarbons such as 140 Solvent, Isopropyl alcohols or white spirits. The incorporation

Calcium and later barium thickened greases were probably the first types of lubricating greases that have been produced and marketed in large volumes [9]. These were based on soaps that were made with a panoply of fatty acids (stearic, palmitic, oleic, etc.) and/ or any animal fats (cattle, horses and swine), abundant in US. The popularity of these soaps was due mainly to their outstanding mechanical stability, excellent water resistance and their moderate costs. As multi-purpose greases and compounds for open gear applications the calcium and barium based thickeners make good greases for chassis, wheel bearings, universal joints and many industrial applications such as bearings in steel mill casters and open gears in mining heavy equipment.

Lithium greases were in full expansion in the early 1940s and 1950s. C.E. Earle recognized the attributes of the lithium soap base grease through a series of patents filed in early 1940s [10, 11, 12, 13, and 14]. The prestigious applications that made the lithium grease based formulations “fly� higher are those associated with the aviation. All were made with lithium stearate.

In a 10 year period lithium based soap has risen to over 50 million pounds/year [9]. The reasons behind the vertiginous increase in volumes of lithium greases include: its properties associated with its easiness in manufacturing in batch or continuous process, its fibrous texture flexibility, compatibility with all types of mineral and synthetic oils, high shear stability even under high loads. Its high responsiveness to the additives and its high thickening capacity make the lithium based greases extremely cost effective, chemically, mechanically and thermally stable under the most aggressive environments.

Its usage in open gear instead of the powdered thickening systems, and even the barium and calcium types, was justified by the fact that lithium has an extremely high thickening capacity, lower torque resistance in bearings, and better pumpability & mobility at low temperatures.

- 18 VOLUME 80, NUMBER 3

Since the adoption of lithium base grease as the thickener of choice for the years that followed the 1960 and 1970s, open gear formulations, have seen the content of solvent decreasing or completely disappearing.

This was the result of lower content of lithium soap in comparison with the calcium or barium soap based greases, the outstanding low temperature properties making it the first choice by excellence in cold zone mining areas such as the Canadian and northern regions of the United States.

capabilities. The R&D lab manager, W.D Janssens, in an interview tells the “solids” story: “Throughout my years with Imperial, it has been my responsibility to develop new oil products and make sure that the solids are compatible. Every discovery that we have come up with has increased the overall lubrication ability of our solid additives. We have never compromised and we have never sacrificed. The only changes we have made have been for the better. We are gaining all the time, continuing to make products that no one else has [15].”

Molub-Alloy technology ”From Imperial Valley to the World”

Imperial Oil & Grease Company became a part of Castrol Industrial organization in the early 1990’s.

On February 17, 1952, in Section Two of the Long Beach Press-Telegram Publication [15] credit was given to George Gerber, President of Imperial Oil & Grease Company for pioneering the usage of molybdenum disulfide in greases: “According to Mc Vicar, metallurgists knew the lubricating value of certain metals for years, but no one did much about it until along came along his father-in-law, George Gerber, of North Hollywood, president of the Company. When Gerber introduced metallic grease (composed of microscopic bits of molybdenum disulfide and a copper-lead alloy), he found that only 10 pounds a day was required to lubricate a specific cam, whereas 25 pounds of ordinary grease was formerly used. Likewise the cam had to be greased twice a day before the introduction of Gerber’s metallic product and now it requires a greasing only once every 13 days” [15].

Reference [15] commenting the advertisement of Figures 13a and 13b: “Ford had narrowed a hundred competing lubrication products down to eight, and the survivor of the eight was Molub-Alloy. Ford’s announcement was the first national advertisement Molub-Alloy had ever received.”

From the solvent containing to the solvent free Open Gear Compounds: This transition occurred in 2 different stages: Chlorinated solvents such as 1, 1, 1 trichlorethane, trichloroethylene, etc.., that were used mainly for their non-flammability and rapid evaporation properties were banned for health concerns by the end of the 1990s.

This initial combination of molybdenum disulfide and metal alloys gave birth to the Molub-Alloy technology, becoming later the brand for most of the gear oils and greases containing solid lubricants.

Later in the reference [15] again one can read: “Certainly in mining there were many needs for a superior lubrication product, many applications such as walking cams, cat tracks, wire ropes, bearings, open gears and the like. Some of the equipment was enormous, weighing 2,000 to 3,000 tons, and requiring six or seven lubricants on a single machine. Molub-Alloy with its pressure resistance qualities, impervious to dust, to extremes of temperatures and so on, was a much needed item.”

Molub-Alloy technology in following years continued to grow fiercely. More investment was made in both Research and Development and the manufacturing - 19 NLGI SPOKESMAN, JULY/AUGUST 2016

These chlorinated solvents were replaced by hydrocarbon-type solvents (140 solvents, white spirits, iso-propyl alcohol, etc.).

These types of solvents raised other concerns associated with volatile organic compounds (VOCs) emissions and risks of fires on the machinery due to the low flash points.

In early 1990s, with legislational developments mentioned above, the general tendency was to go solvent free. The new solvent free open gear compound technology would be affected mainly by the lubricant delivery challenges as the new machinery was becoming bigger and heavier, the lubricant dispensing system in centralized configurations requiring longer and more tortuous dispensing lines to reach all of the lubricated points. It became obvious that the solvent free open gear compound had to be tailored to the geographical area where the product would be used. This gave birth to the Heavy, Medium and Light grades, and even Arctic grades reflecting the kinematic viscosity of the base oils. These grades might be containing similar or close additive packages, displaying similar or close physical and performance properties, but showing different behaviors in terms of pumpability and dispensability at low temperatures. Table 1, regroups the typical data for these 4 grades. Low temperature properties could not be met without solvent with the lightest grade. Arctic grades with much lower viscosity continued to be the product of choice for these colder climatic areas where ambient temperature can drop below -35 to -40°C. It doesn’t meet all the OEM specifications in terms of viscosity but provides the same protection as the heavier grades do.

We still see different OEM specifications for open gear applications referring to solvent containing compounds. Other specifications such as AGMA 251.01 specified a Timken OK Load and an FZG pass stage requirements, while other specifications such as US Steel, has a requirement for a Timken Retention test value instead of an OK Load.

From “rigid” to “relaxed” Open Gear Compounds

In late 1990s, a new version of the Open Gear heavy grade compound was developed to accommodate the overseas remote areas that used to necessitate lengthy storage durations and various handlings and transfers prior to product utilization. Requirements such as good resistance to oil separation, and resistance to set back (hardening under normal storage conditions) were highly desired. Good performance in these critical areas makes the pumping operation and transfer through the central lubrication system easier. As one can expect, the base oil nature has been revisited (keeping the viscosity within the acceptable range). A couple of additives that were thought to have an effect on rheological properties and structure of the grease matrix were reviewed in this program. The newly developed compound could meet the objectives with minimum change to the formulation.

The field testing confirmed the laboratory findings, not only under normal temperatures but also under the lowest temperatures that commonly seen in these areas.

High Efficiency Open Gear Compound

In early 2000, it was proposed to consider the possibility of improving the grease efficiency by reducing friction without impacting load carrying capacity, or wear protection [17]. A set of 8 commercial products

- 20 VOLUME 80, NUMBER 3

were considered in the benchmarking program. These products were based on diverse technologies. The base oils of these products included asphaltic compounds, naphthenic oils, paraffinic oils, synthetic fluids or combinations. The viscosity of the base fluids varied from as low as 250 cSt at 40°C to as high as 800 cSt at 100°C. The thickeners included lithium 12 hydroxy-stearate, aluminum complex, calcium sulfonate, bentonite, carbon black and fumed silica. Solids lubricants included graphite, molybdenum disulfide, calcium carbonate, calcium hydroxides, etc. or combinations, Packages of EP / AW additives including Sulfur-Phosphorus- Nitrogen

compounds by themselves or in association with metallic elements such as Zinc, Molybdenum, Calcium, Boron, Antimony. Other additives including anti corrosion, anti-oxidant, VI improvers, tackifiers, etc. were present as well.

The EP and anti-wear properties were measured using Four Ball EP test (ASTM D- 2596) and Four Ball Wear (ASTM D- 2266) (Figure 14).

The SRV test rig (Figure 15) was chosen for evaluation of friction for mainly 2 reasons: (1) the end user as

- 21 NLGI SPOKESMAN, JULY/AUGUST 2016

well as the OEM (mining) have data in the possession that correlates the performance of a series of open gear compounds to the laboratory results obtained on SRV machine, and (2) the SRV machine offers the possibility of simulating open gear contact conditions (starved film).

the solid film lubricants which were also a combination of several different types and finally optimization and search for synergisms between different AW, EP and FR compounds but also with the solid additive packages. The results of this study are shown in Figure 16, 17, 18 and 19.

The SRV machine used in this study utilizes a top specimen (flat surface disk) oscillating in contact with a bottom specimen (disk) at a preprogrammed settings of frequency, stroke, load and temperature. The specimen contact is lubricated with the lubricant sample. The approach that has been taken is to make sure that there

Welding Loads of the 8 benchmark products, listed in Table 2, were varying between 315 and 800 kgf, the 4-Ball wear scars between 0.58 and 1.2 mm, and the SRV COF (after 2 hours run) were varying between 0.09 and 0.22. The new prototype passed the 800 kgf level in EP test, measured 0.63 mm in the wear test and remarkably outperformed all the other benchmark

is no compromise on the welding load, as measured by Four Ball EP (800 kg minimum, which was deemed a critical requirement for any product used on the draglines and shovels in mining exploitation. In the same line, the wear was considered acceptable if the ball scar diameter remains below 0.7 mm as measured as per Four Ball Wear test. A target of 0.08 coefficient of friction (COF) as measured by SRV was set as the maximum acceptable value in this program.

Development work was started by (1) optimizing of the base oil fluid viscosity built with a combination of paraffinic, naphthenic and synthetic oils. (2)optimizing - 22 VOLUME 80, NUMBER 3

products with a COF as low as 0.02 in duplicate test runs.

In coordination with the OEM, extensive SRV testing was carried out to compare performances of this prototype when used in bushings (steel bronze configuration).

Coefficients of friction of 0.02 have been replicated. The product has been since then applied in drag gearing, center pintle, slew rack, roller/rail, propels, shaft/

bushings in draglines. The results of the field testing can be summarized within this statement from an end user: “Product was used without interruption in open gears and bushings for 50,400 operating hours. Recent inspections revealed that all bushes had the original machining marks intact”. This year the product entered its 20th year of utilization. It continues to maintain its exceptional performance in all the lubrication points in which it is applied.

Getting to “Super Heavy”

As we all know, in recent years, OEM specifications continued to change to adapt to the new lubrication requirements of the massive machinery. A new specification was issued to reflect the new requirements for the electrical hoist drum gearing present in a mining shovel calling for higher base oil viscosity. The “Heavy” version open gear compound with an initial base oil viscosity of 1890 cSt at 40°C has been upgraded to a “Super Heavy” version with a base oil viscosity of 6,000 cSt at 40°C for 5,000 cSt minimum required by the new specification [17].

The challenge for the formulator was to pick suitable base fluids to meet the new spec requirement in terms of viscosity but also keep the rest of physical and performance properties the same or within acceptable ranges including dispensability.

Table 3 below shows data sets for both low friction heavy

grade as well as Super Heavy grade.

Field testing was carried out in 2012/2013. The Super Heavy lubricant seems to handle both the heavy and the super heavy applications, not only in terms of gear performance “ I have not seen a better looking gear set with the 2500 hours that they have on them” as stated by the OEM gear inspector, but also in terms of pumpability, sprayability, dispersability and coverage as well in spite of the high base oil viscosity involved.

Biodegradable Lubricants

In recent years, awareness of the utilization of mineral based oils and their possibly undesirable effects on the surrounding areas has created the opportunity to produce environmentally friendly lubricants from agricultural products. These products have the advantages of being less volatile, having minimal health and safety risks and being more easily disposed due to their inherent biodegradability. Several biodegradable precursors such as esters and vegetable oils have been proposed for use in lubricants. Thus, such lubricants discussed in [19, 20, 21, 22, 23, and 24] references suggest that bio-based products could represent a potential feedstock that may provide an acceptable cost performance balance without carrying any risk to the safety, health and environment.

This is particularly true for systems where lubricant may be lost after use or accidentally comes in contact with the environment. A vegetable based platform for biodegradable products was developed to address these new challenges in the open pit mining industry.

Laboratory test results along with the field testing data side by side with those obtained on conventional mineral oil based products was undertaken.

Biodegradable Open Gear Lubricant for Mining Machinery

Combinations of vegetable oils, thickening systems, solid compounds and a package of functional additives constituted the formula of the finished grease that was subjected to laboratory and field testing. The product was homogenized through a stone mill improving grease consistency and eventually its stability over time. The lab test set consisted of those shown in Table 4 below.

Based on Table 4 results, one can say that the biodegradable open gear lubricant versus a mining industry standard lubricant, a petroleum based lubricant, displays equivalent if not better, physical and performance characteristics. These conclusions are valid for EP and antiwear properties, mechanical stability, water resistance,

corrosion inhibition, reversibility, thermal retention, and pumpability.

A field testing was conducted on a mining dragline. The trialed components were Drag gearing, Centre pintle, slew rack, rollers / rail, and RHS propel shafts/bushings.

Performance indicators were visual inspection, sound level, temperatures, and lubricant sample analysis.

Procedure consists of isolating the lubrication systems, purging lines and injectors, loading the flushing product, then the bio-based product. The detailed results of the field testing are presented in the reference [19]. These can be summarized in the following extract from the field testing report [25]:” At 6 minutes purge cycles, the BOGL (biodegradable Open Gear Lubricant) film was washing off. As cycles were gradually extended, film was being worked and gave good adherence. Film of BOGL is very black-tenacious. Film of BOGL drag gearing is darker that PBOGL on hoist gearing, appearance excellent. At 3 minute cycles for drag gearing, the coverage is still very good and you can still leave finger lines on the load face after 24 hours at 30 minute cycles. If the adhesion of the lube to the drag gear is anything to go by, I don’t think we will have any problems once the film of BOGL has been established. Coverage is very good. Pitch line has plated out nicely. BOGL is still working its way up the non-load side of the drag gear. New BOGL is showing at top flange, center pintle bushing and temperatures are good”. Later towards the end of the report, one can read: “The trial, although clearly in early days, is going very well. MISL, the acknowledged Mining Industry Standard Lubricant and our benchmark reference for BOGL, shows early evidence of being outperformed by BOGL”.

Other Bio-based Lubricants

The above bio-based technology platform has been extended to include other total loss application products, namely seal compounds for tunneling boring machines [26] or even mill liner lubricants to protect mill housings and roll bearing chocks [27].

Conclusions

This is the story of evolution of open gear compound technology that didn’t cease reshaping itself since its conception following the time when the first shovels and draglines were put in operation. To adapt to the excavating technology transformation, the open gear technology had

- 25 NLGI SPOKESMAN, JULY/AUGUST 2016

to adopt the use of early base oils produced from the first oil refining processes and to adjust to the new lubrication requirements. Initial asphaltic material (with solvents) and later with various metal based additives for wear and extreme pressure protection, contributed to the extension of service life of open gear components. Development of open gear compounds based on lithium greases and newly introduced lubricating solids, have drastically improved the impact of lubrication on the operation and service life of the mining heavy equipment. Solvent removal from the open gear formulations, the solvent free technology has been challenged by the low temperature applications.

Heated lubricant dispensing lines, utilization of synthetic base oils in the formulations and diversification of the grades to reflect the variety of the geographies, have significantly contributed to the adaptability of the new technology to new performance and environment requirements as the OEM new specifications developed.

Finally, bio-based (or biodegradable products) specifically those designed for total loss applications, while timidly moving into mining applications, are bringing high performance attributes to Industrial applications, as they continue to gain broader acceptance in the Mining Sector.

References

1. K. Carnes, The 10 greatest events in tribology history, TLT Magasine, June 2005 2. Ilija Gawrilow, Vegetable Oils in Usage in Lubricants, Oleochemicals, Vol. 15, Nov 2004 3. Lou Honary, Biodegradable / Biobased Lubricants and Greases, Machinery Lubrication, Sep 2001 4. L Honary, E Richter, Biobased Lubricants and Greases – Technology and Products, John Wiley & Sons, 2011 5. G. Ivănu, Istoria petrolului în România, Editura AGIR, 2004 6. Constantin M. Boncu, Contribuii la istoria petrolului românesc, Ed. Academiei R. S. România, 1971 7. Lubrication of Coal Mining Machinery, Lubrication, December 1926 8. The evolution of the base oil technology industry focus, Machinery Lubrication, March 2003 9. C. J Boner, manufacture and Application of Lubricating Greases, Reinhold Publishing Corporation, NY 1954 10. C.E. Earle, US Patent Nr. 2,274,673, March 1942 11. C.E. Earle, US Patent Nr. 2,274,674, March 1942 12. C.E. Earle, US Patent Nr. 2,274,675, March 1942 13. C.E. Earle, US Patent Nr. 2,274,676, March 1942 14. C.E. Earle, US Patent Nr. 2,293,052, August 1942 15. C. Mason Imperial Valley to the World, An Adventure in American Free Enterprise, 1981 16. Specification for Open Gear Lubricant - SD4713 (August 18, 2005) - 27 -

17. H. Faci, I. Bjel, A. Medrano, B. Cisler, “Frictionless” Open Gear Lubricant, NLGI Spokesman, Vol 66, Nr 6 , September 2002 18. Caterpillar 1ESD4732 Specification for Open Gear Lubricant, March 2013 19. H. Faci, A. Medrano, B. Cisler, “Biodegradable Open Gear Lubricant”, NLGI Spokesman, Vol 67, Nr.12, March 2004 20. H. Faci, Open Gear Lubricant, Castrol Limited, US Patent 6, 251, 839, June 26, 2001 21. T. Mang, Environmentally Harmless Lubricants, NLGI Spokesman, Vol 57, Nr 6, Sept 1993 22. T. W. Dicken, Biodegradable greases, Industrial Lubrication and Technology, Vol 46, Nr. 3, 1994 23. L. Honary, a.t. Potential Utilization of Soybean Oil as Industrial Hydraulic Oil, SAE Technical Paper Nr 941760, Warrandle, PA SAE Publications (1994).

24. J.W. Lambert, Vegetable Oil Lubricants for Internal Combustion Engines and Total Loss Lubrication, Agro management Group, US Patent 5,888,947, March 30, 1999 25. Preliminary Trials, Biodegradable Open Gear Lubricant, Field Testing Report, Applied Chemicals Pty Ltd, DDD/242-98 (Internal Distribution) 26. H. Faci, B. Cisler, Biobased Lubricants for Tunnel Boring Machines, NLGI Spokesman, Vol 72, Nr. 5, August 2008 27. H. Faci, B, Cisler, A. Medrano, M. Inns “When Performance and Biodegradability Converge – A Superior Product in a Demanding Environment, NLGI Spokesman, Vol 70, Nr.1, April 2006

NLGI SPOKESMAN, JULY/AUGUST 2016

A BLAST FROM THE PAST

- 28 VOLUME 80, NUMBER 3

NLGI MEMBER

SPOTLIGHT

Company: Nynas Member Category: Supplier Address: P O Box 10700, SE-121 29 Stockholm, Sweden Website: http://www.nynas.com/

Contact Name: Dr. Valentina Serra-Holm Title: Marketing & Technology Director Telephone: +0046 602 12 00 Email: vase@nynas.com

We hope you’ll enjoy learning more about our long-time member Nynas. Located in Stockholm, Sweden, Nynas has shown a real commitment to innovation over it’s many years of operation. We’re proud to feature their company in this month’s edition of the NLGI Member Spotlight.

A Different Kind of Oil Company

In almost ninety years in the market, Nynas has been transformed from being a regular national oil company to a leading global corporation with a focus on specialty products.

Nynas business operations started back in 1928 with the construction of Sweden’s very first refinery. During the first few decades a large number of products were manufactured for the Swedish market, including petrol and heating oil, but the focus gradually shifted and Nynas special products are now sold in niche markets in all parts of the world. In contrast to most other oil companies, which use oil as a source of energy, the focus is on products with a long service life, which in many cases can also be recycled.

Nynas oils are all around us and in many cases they bring major benefits to society. These include products used in transformers and

as binders in asphalt or sealing material. But the oils are also used in a number of other contexts – as components in adhesives, rubber soles, thermoplastic and graphical paint, as well as in lubricating greases metalworking fluids, hydraulic oils and other industrial lubricants, to name but a few examples.

The international focus is made possible by a global delivery network with regional hubs and a large number of local storage depots, including a recently opened depot in New Jersey, to further improve the service level and delivery performance for Nynas customers in North America.

This makes it possible to deliver to virtually anywhere in the world. In addition to the global network of depots, ships and road tankers, Nynas has at its disposal sales offices in more than thirty countries as well as its own or associated refineries in Europe and America.

- 30 VOLUME 80, NUMBER 3

Its own biggest facilities are the refinery in Nynäshamn and the Harburg refinery just outside Hamburg, which was recently acquired from Shell. At the moment Harburg is being converted from being mainly a fuel refinery into a special refinery. Once all the renovations have been completed in early 2016, Nynas annual production capacity will have increased by 350,000 tons.

After decades of research and development work, primarily in the field of hydrogenation technology,

Nynas is now the leading international brand when it comes to naphthenic specialty oils (NSP). The other main product area is bitumen. Bitumen is used to bind the aggregate in asphalt layers, and also in certain industrial applications, for example roofing felt and corrosion protection.

Limitations in viscosity range and solvency (compared to Group I) will be a great challenge to overcome, and will not be realistic for many kinds of formulations.

Naphthenic specialty oils are used primarily in four segments – electrical industry, chemical industry, lubricants and tyre oils – where strict demands are made on the oil having high solubility and withstanding significant temperature differences. Demand is expected to increase primarily in Asia, South America and Africa with the process of industrialization and improvements in prosperity.

Nynas has developed a range of base oils, covering a wide viscosity interval, from 60 SUS to 4000 SUS, with properties and performance similar to Group I, which can therefore be used in existing lubricant production with a minimal need for reformulation. These new oils will be available on the global market in the long term.

Nynas will capture extra growth due to the rapid ongoing restructuring of the global base oil markets. The traditional Group I base oil producers, many of which are located in Europe, face multiple challenges in the market. The main threat is the changing appetite within the dominant automotive engine oil segment, favouring base oils with no Sulphur, low viscosity and high viscosity index (VI). Scale of production, crude flexibility and product mix profitability are other factors.

But there is another alternative.

Over the course of almost 90 years in the market, Nynas has managed to combine tradition with innovation while at the same time nurturing its heritage from having originally been an entrepreneur-driven family company. The longterm objective is, by means of continued, stable growth, to secure the company’s position as a leading global supplier of naphthenic speciality oils and a significant operator primarily in the field of upgraded products in the European bitumen market.

Since Group I base oil properties such as high viscosity and high solvency remain crucially important for industrial lubricant manufacturers, this is a cause of great concern. It they cannot secure ample supply of Group I base oils , the will be forced to attempt to rapidly develop new formulation in more readily available base oils, such as Group II and Group II paraffinic base oils.

NLGI is proud to announce the introduction of the ‘NLGI Member Spotlight’, a new feature of the 2016 all-digital Spokesman magazine.

All NLGI members may take advantage of this opportunity to highlight your company’s history, global reach, vision, employees or whatever you’d like our readership to know about your company. You may talk about products & services, however, no competitor trade names may be used, nor mention of product pricing.

There is no limit on words and we welcome many photos

of your headquarters, offices, plant & employee photos. We will accept articles for publication on a first received, first published basis. Contact Marilyn Brohm Marilyn@nlgi.org at NLGI if you would like to submit an article for possible publication in an upcoming issue.

There is absolutely no charge to have your article appear in the NLGI Member Spotlight

the Expert Q: Do you have technical information of saponification temperatures for manufacturing Lithium Greases available?

A:

Q: Could you please tell me the difference between KP2K and KP2N. Both are in grade NLGI 2.

A:

The temperature at which to carry out the saponification reaction for the manufacture of lithium greases is dependent upon the equipment being used for the manufacturing process. In an open kettle, the temperature should be in the range 85 – 95°C, hot enough to drive the reaction while maintaining the water present in liquid form. The time required to carry out the reaction can vary, depending on the amount and concentration of thickener present at that point. In a closed vessel – pressure kettle or Contactor® reactor – the temperature can be higher, since the elevated pressure will elevate the boiling point of water.

The KP2K and KP2N designations are from DIN 51825, Type K Lubricating Greases, Classification, requirements and testing. Greases of type KP are designated as containing anti-friction and anti-wear additives and being designed for applications requiring a higher load-carrying capacity (generally referred to as Extreme Pressure or EP greases). The 2 in the designation indicates the NLGI consistency grade.

The final character in the designations relates to the recommended maximum operating temperature for the grease and its performance in the presence of water.

K indicates a maximum temperature of 120°Cand a performance of 0-90 or 1-90 in DIN 51807-1 (water resistance). N indicates a maximum operating temperature of 140°C, but no requirement regarding water resistance.

- 32 VOLUME 80, NUMBER 3

NLGI member H. L. Blachford makes metallic stearates and related materials. Their contact information (from the NLGI member directory) is as follows: H.L. Blachford Blachford is a manufacturer of specialty metallic stearates and soaps. These include aluminum and calcium stearates as well as our most popular grease pre thickeners, lithium 12-Hydroxystearate and our Calford G-200 (lithium stearate) specifically designed for use in lithium greases. http://www.blachford.ca/ Aldo Pighin 2323 Royal Windsor Drive Mississauga, Ontario, L5J 1K5 Canada Phone: 905-823-3200 Fax: 905-823-9290 Email: apighin@blachford.ca They may be able to supply a lithium complex thickener.

Q: Is lube base oil 600N recommended as base fluid to form greases for wheel bearings of light and heavy vehicles?

A:

600 Neutral Oil (600N) refers to a paraffinic base oil with a viscosity of approximately 600 SUS at 100°F. This translates to about 100 - 125 cSt @ 40°C. It is typically either conventionally refined (API Group I) or catalytically refined (API Group II). That type of base oil is generally suitable for use in formulating a grease for automotive and heavy duty wheel bearing applications, but may be too low in viscosity to be used as the only base oil is such a product. Wheel

bearing grease typically has a base oil viscosity of about 220 cSt @ 40°C. To obtain that viscosity, the 600 Neutral Oil would need to be blended with a higher viscosity stock to produce the desired viscosity. Of course, the quality of the base oil should be evaluated before selecting it for use in a wheel bearing grease.

Reducing Fire Hazards in Mining with Fire Resistant Grease By: Joel Garrett, Brian Cichoski, Brian Kusak, Matt Bailey, Kevin Dickey Summit Lubricants – A Quaker Chemical Company

INTRODUCTION According to Scott (2006), mining is an expansive industry that may be categorized according to surface (open cut), underground, process plant, and exploration.

The operational challenges include but are not limited to dust, difficult to operate machinery and health and safety hazards that range from visibility to oxygen deficiency to fire.

Despite all of the knowledge and awareness of fire hazards in mining, fires continue to exist. Fires result from uncontrolled processes where there is an ignition source combined with another element that makes up a fire. This paper reviews the fire risks associated with lubricating grease discusses the opportunity for reducing risks with the use of fire resistant greases.

In its most basic form, fire occurs when four elements of the fire tetrahedron are present (National Fire Protection Agency, 2008). These elements are heat, fuel, oxygen and a chain reaction. Without these, fire is not present. However, controlling these risk factors is not easy in mines.

This paper looks at the four elements of the fire tetrahedron and discusses how the use of fire resistant grease breaks the chain to reduce the risk of fires.

BACKGROUND AND SIGNIFICANCE Fires have always been an issue within the Mining Industry. Understanding the sources of how fires begin

and how they propagate provides the background to understand how the use of fire resistant greases can reduce some of these risks at mines.

For a fire to start and evolve, it must have four elements present: heat, fuel, oxygen and an uninhibited chain reaction. This is known as the fire tetrahedron. Once a fire is started, it can spread in three different ways (National Fire Protection Agency, 2008). The first is conduction, which is the passage of heat energy through or within a material because of direct contact. The second is convection, which is the flow of fluid or gas from hot areas to cooler areas. The third is radiation, which is heat traveling via magnetic waves, without objects or gases carrying it along.

According to the National Fire Protection Agency (2008), there are four ways to put out a fire.

1.

Cool the burning material

2.

Exclude oxygen

3.

Remove the fuel

4.

Break the chemical reaction In mines, the approach to putting out the fire is generally done with variations of cooling the burning material. With a fire resistant grease, the approach is removal of the fuel. This is because a typical mineral oil based lubricating grease is a good fuel source. A fire resistant grease is not as good a fuel source due to it having lower volatility and higher molecular weight relative to mineral oil products. This directly results in

- 34 VOLUME 80, NUMBER 3

higher flash and fire points.

system.

A solid or liquid fuel source relies on vaporization of the medium to act as a fuel. Low vapor pressure at elevated temperature compared with mineral oil reduces the ability of the lubricant to act as a fuel under equal temperature conditions.

Furthermore, fire resistant greases are made from materials that have low thermal conductivity requiring more energy input to reach combustion temperatures.

As mining has become more efficient, the hazards have grown as well. The operators are required to look at the hazards associated with the following machines and equipment described by Scott (2006): 1. F ans, pumps and compressors 2. W inders and haualages 3. L ongwall face equipment for underground coal mining 4. C ontinuous miners and shuttle cars 5. D raglines for overburden removal in surface mining 6. Drilling rigs 7. C rushers, comminution mills, and conveyors 8. M obile equipment such as dozers, excavators and load-hauldump trucks 9. B ucket wheel excavators 10. Vibratory screen and centrifuges 11. Stacker-reclaimers

PURPOSE AND SCOPE The purpose for writing this paper was to provide more awareness of the fire risks associated with the use of mineral oil based lubricants and to help understand how alternative lubrication formulas reduce these risks. This is important for a few reasons. First, fire hazards are inherently part of many of the mining processes. Second, there is a high tendency to accept the risk relative to the cost of using fire resistant greases. Third and like most industries, making changes within mining, lubrication being no exception, can be time consuming.

Since fire hazards are relatively accepted, the solutions for addressing the fires are somewhat rudimentary.

This can range from letting grease burn itself out when the fuel source is completely consumed to an employee using a small extinguisher to put out the fire, to a more advanced, hardpiped, water-based extinguishing

While mining has become more efficient to drive out cost and maximize profitability, it has further created the need to reduce hazards, particularly fire hazards. While there have been many safety improvements over time, the industry has also learned to work with dangerous conditions since the beginning.

Because heat is created in mining processes and because lubricating grease is needed to keep machinery operational, there is potential every day for heat to come into contact with lubricating grease resulting in a fire.

- 35 NLGI SPOKESMAN, JULY/AUGUST 2016

DISCUSSION Types of Lubricants Used in Mines According to Scott (2006), the mining industry consumes several types of lubrication. The lubricants are primarily hydraulic fluids, gear oils/greases, wire rope lubricants and bearing greases.

A majority of the mining lubrication volume is consumed in power hydraulic systems. The primary function of hydraulic fluid is to create force and motion so the fluid creates pressure at the point of use. The lubricating function, while important, is a secondary function of hydraulic fluid.

Hydraulic fluids are classified under ISO 6743/4. While there are many classifications, some of the most common include water-based and mineral oil-based fluids. If there is potential for heat or hot metal contact, water glycols and ester based fire resistant fluids are used.

All types of gears are used in the mining industry. This creates the need for all types of gear lubrication, including those for open gears as well as those for gear boxes. Generally, gear boxes require oil lubrication, while open gears require more viscous products such as greases.

Product selection is further varied by temperatures, speeds, loads and environmental conditions.

Another type of mining lubricant is

that used for wire ropes. Although there doesn’t seem to be a good scientific approach to product selection and applying the product, there are some basic recognized points that are important to note.

First, the lubrication points are the sliding surfaces within the rope strands. If the lubricant does not penetrate the rope, the sliding surfaces are not being lubricated.

Second, the lubrication must be low enough in viscosity to ensure that excess lubrication is not on the outside of the wire rope, as this will increase the likelihood of contaminants adhering to the lubricant. The contamination can lead to the introduction of foreign materials that will cause wear on the rope strands. Third, compatibility of the materials coming in contact with the lubricant should be addressed to ensure that strand breakdown does not occur.

All types are bearings are used in mining. Those used in tools tend to be higher speeds and lower loads than those used for mining processes that tend to carry heavier loads at slower speeds.

In general, bearings consume greases. Some of the greases are those that are “lubricated for life,” especially those greases used in tools and other small equipment.

The machinery that is larger and conducting heavier loaded tasks (e.g., machines cutting longwall surfaces) usually requires greases with higher base oil viscosity.

Fire Hazards in Mining According to Collins (2013), fire is one of the top ten hazards in the mining industry. Because the challenges within mining environments make it extremely difficult to manage fires, a “safety first” approach from everyone is critical.

Fire hazards exist in many places within mines. As a result, fires can occur in mines for a range of reasons.

The most common being gas leaks, electrical faults, or the spillage of flammable chemicals. Because bearing grease is often overfilled, this can be a significant source of a flammable chemical within a mine.

Because mining processes can also be extremely hot, and the risk of fire is high the need for safety is increased. Using higher flash point lubricants can help reduce fire risk.

To extinguish the fire, the National Fire Protection Agency (2008) describes the four main approaches.

These are cooling the burning material, eliminating the oxygen, removing the fuel and breaking the chemical reaction. Typically, mines cool the burning material. This is usually done with water either from a system or from a mining worker manually extinguishing the fire.

BENEFITS OF FIRE RESISTANT GREASES IN MINES In mines, the common approach to putting out fires is done with variations of cooling the burning

- 36 VOLUME 80, NUMBER 3

material. With a fire resistant grease, the approach is removal of the fuel. This is because a typical mineral oil based lubricating grease is a fuel source. A fire resistant grease is not a fuel source because the base oil and additive chemistry are selected based on their ability to resist combustion. Ultimately, the combustible hydrocarbons are removed from the formulation.

This results in materials with lower volatility, which minimizes the generation of combustible vapors that are able to ignite and propagate the flame after ignition. Furthermore, some base oils, such as esters require substantially more energy to ignite and sustain fires.

SUMMARY OF FIRE RESISTANCE GREASE TEST METHODS There are no international or national standards for determining the fire resistance of a grease. There are however methods that are used for hydraulic fluids. These methods were used as the initial baseline methods for test procedures in the development of fire resistant greases.

As the laboratory testing provided good insight to fire resistance, further test methods were developed based on field trials and experience to provide better evaluations of fire resistance relative to mine processes.

The chronology of the iterations are listed below.

Method 1 – Wick Test A modified Wick Test was developed. This was based on the Federal Test method 791C-352.1

and the MSHA method ASTP 5004 version 2010-02-12 – The Effect of Evaporation on Flammability. The standard test method consists of checking the flammability of the liquid (by passing a sample-soaked pipe cleaner repeatedly through a flame and noting the number of passes required for ignition), and storing the sample in an oven for the time and temperature required by the speciation, and rechecking flammability.

The modified Wick Test was conducted under the same conditions with the same steps.

However, the pipe cleaner (i.e., Wick) was coated with a lubricating grease instead of a liquid oil. This was then passed into, and removed from, a methane fired Bunsen burner, at regular intervals (approximately 30 cycles/sec) until the wick caught fire.

Based on several samples and types of products, a minimum cut off of 20 cycles prior to ignition was set to determine fire resistance.

Method 2 – Direct Flame Torch Test To better represent field conditions in a mine, a direct flame test was set up. A metal dish was used to represent a piece of slag steel. A 10g sample of grease was placed in the center of the dish, which was placed on a room temperature hot plate under a fume hood with the exhaust fan turned off.

The method was initially developed using a handheld torch placing a direct flame on high and aimed at the

bottom, center of the grease sample.

Mineral oil based greases ignited immediately and burned for more than 60 seconds. Samples based on mid range viscosity fire resistant base oils did not ignite.

The method was then standardized with the placement of the flame on the sample for 25 seconds. This was sufficient to ignite all grease samples.

The time it took for the flame to self extinguish was then recorded and became another measure of fire resistance.

Method 3 – Hot Washer Test Using samples that were previously tested under Methods 1 and 2 above, a third testing sequence was developed from customer feedback.

This Hot Washer test method consisted of placing a 25g sample of grease on a piece of angle iron and adding a heated washer on the sample of grease. The steel washer was heated to very high temperatures with a propylene oxygen torch until it was red hot. This was meant to better represent conditions in a mine where hot materials come into contact with excess lubricating grease.

Method 4 – Ceramic Pellet Test To standardize the testing, the hot washer was replaced with a Ceramic Pellet/Disk that was heated in a muffle furnace. The ceramic material has a thermal conductivity that is very similar to steel and obtaining these commercially is easier for various laboratories. The furnace was set at 1,500°F (815°C) for a four hour period. The Ceramic Disk was then

- 37 NLGI SPOKESMAN, JULY/AUGUST 2016

placed in a standard volume of grease held in a metal tray. This became the measure of Fire Resistance.

The unit of measure is time it takes for grease to self-extinguish with a pass/fail value. Fire resistant greases are those that self-extinguish in less than two minutes. Those greases taking longer than two minutes and those requiring equipment to extinguish, are determined not to be fire resistant.

CONCLUSIONS Safety hazards are inherent within the mining industry. In particular, fire hazards present a sizeable risk for mine workers as the nature of the processes require significant heat to produce the desired finished products. Minimizing and controlling the hazards is very challenging and this paper explains how fire resistant greases can reduce some of those risks.

Because mining greases are typically mineral oil based, this becomes the fuel for a fire event.

The authors propose that using a synthetic ester oil based grease would reduce the likelihood of the grease catching on fire. Typical flash points for mineral oil based greases is 250 C while ester oils have a flash point of > 280C. This technology is based on the same ester technology used in fire resistant hydraulic fluids.

This is further supported in that the ester technology requires a higher energy level to cause and sustain combustion. Additionally, the physical characteristics of this type of

grease has a tendency to char and reduce the oxygen needed for fire.

While there are no internationally or nationally recognized fire resistance test methods for lubricating greases, the authors have taken several steps to implement test methods similar to those used for fire resistant hydraulic fluids to demonstrate the fire resistance of lubricating greases.

These test methods mimic real world conditions in mines.

Therefore, the authors believe that using lubricating greases based on fire resistant base oils, provides mines with greater protection from fire hazards.

Furthermore, acceptable fire resistant greases can be determined through the Ceramic Pellet Test. The authors are in the initial stages to present a testing standard to ASTM for a new standard for all companies to follow. This will help work environments with similar risks determine the best solutions for reducing risks.

REFERENCES 1. N ational Fire Protection Agency, 20th Edition (2008).

Fire Protection Handbook. Quincy, Massachusetts.

2. S cott, W. (2006). Chapter 20. Mining Industry.

Handbook of Lubrication and Tribology: Volume 1 Application and Maintenance, Edited by Totten, G. pp.

18-3 – 18-59.

3. M allet, L. and Brnich, M. (1999). Focus on Prevention: Conducting a Fire Risk Assessment. Center for Disease Control & Prevention. Pittsburgh, PA. 4. C ollins, D. http://www.safetyrisk.net/top-10-safetyhazards-in-mining/ Mining Safety. (June, 2013).

5. http://www.miningiq.com/mine-health-safety-andwellbeing/articles/5-most-dangerous-hazards-thatminers-face-daily/ (February, 2013).

- 38 VOLUME 80, NUMBER 3

The North American

Industrial Lubricants Congress

SAVE* $300

September 13-14, 2016 Marriott O’Hare // Chicago, IL, USA

Optimizing value in lubricant formulation, selection and development in line with evolving OEM requirements ICIS and ELGI are delighted to announce that the inaugural North American Industrial Lubricants Congress will be taking place in Chicago this September. Covering both technical and commercial topics, the event will tackle some of the biggest challenges impacting the demand, formulation and performance of the industrial lubricants sector today.

Key topics on the program:

Confirmed speakers include:

Base stock market drivers – impact on

Dave Como, President, NLGI

lubricant supply and demand Globalization of supply – defining the characteristics of the additives marketplace Managing regulatory complexities – how are REACH and GHS being implemented within the industrial lubricants sector?

Chic Degler, North American Business Manager Industrial Additives, Lubrizol Andreas Dodos, Chemical Engineer, Eldon’s Herb Estreicher, Partner, Keller and Heckman Jeffrey Guevremont, Principal Scientist, American Refining Group

Evaluating the use of biocides and chlorine in metalworking fluids

Lou Honary, President, Environmental Lubricants Manufacturing

Performance optimization through innovative

Tim Langlais, Marketing Manager, Specialty Base Oils, Ergon

formulation – analyzing the demand for high

Brian Lipowski, Polymer Engineer, Functional Products

performance lubricants The OEM perspective – how is design evolution

Constantin Madius, Commercial Product Manager, Axel Americas

influencing lubrication requirements?

George Morvey, Industry Manager, Kline & Co

Applications and challenges in diverse environments –

Valentina Serra-Holm, Marketing Director, Nynas AB

challenges for water-based and high temperature operations

Michael Sheehan, Sr. Chemical MTS, Global Synthetics Technology, ExxonMobil Chemical Company

Media Partners:

Judith Taylor, Senior Editor, ICIS Nicole Webb, Technologist, Angus Chemical Company

*You must enter the promo code JGZ74706 to receive your discount!

- 39 +44 (0)20 8652 4659 NLGI SPOKESMAN, JULY/AUGUST 2016

www.icisconference.com/lubricantsusa

events.registration@icis.com

Welcome our new 2016 NLGI members!

New 2016 NLGI Members

Note: If your company is an NLGI member, you may login to our website’s ‘Member’s Area’ and obtain direct contact information for all NLGI members. You can also sort our directory by membership category.

AMSOIL Inc. - Marketing Doug Sturm 925 Tower Ave Superior, WI 54880 USA 715-399-6334 www.amsoil.com

Axxess Chemicals – Supplier Jay Lynn 522 Highway 9 North, Unit 110 Manalapan, NJ 07726 USA 732-851-1010 www.axxesschemicals.com

AMSOIL INC. specializes in developing synthetic lubricant technology designed for those who demand the best. Our full line of synthetic lubricants deliver superior wear protection, allowing customers to harness the full potential of their cars, trucks, motorcycles, industrial machinery and anything else they ride, drive or operate. By maximizing vehicle and equipment performance, reducing wear and increasing fuel efficiency, AMSOIL synthetic lubricants help millions of people worldwide get the most out of their vehicles and equipment while saving time and money.

Apex Grease (Shanghai) Co., Ltd - Marketing Estelle Zhu 5F, 58 Xiangcheng Rd, Pudong New District Shanghai 200122 CHINA 86-139-1786-4477 http://www.apexgrease.com/ Apex Grease is a marketing and branding division based in Shanghai, China with a global network providing food grade lubricants and industrial specialties. 100% manufacturing in Europe and the US, we are rooted in Chinese market with a strong distributing network and local know-how by seeking business opportunities worldwide.

Axxess Chemicals, founded in 2009, is a valueadded global distributor of Molybdenum Disulfide, Polybutene, Base Oils, Transformer Oils and many other specialty chemicals. Although the grease and lubricant market remains the largest markets we service, Axxess Chemicals also services the needs of the Industrial, Pharmaceutical, Steel, Automotive, PTFE, Cosmetics and Adhesives industries.

Biederman Enterprises- Supplier Pete Avery 2975 Long Lake Rd St. Paul, MN 55113 USA 314-440-7472 http://www.biederman.ca/ Grease cartridge supplier - HDPE with aluminum end. Biederman Enterprises Inc. has a long history of achieving excellence in quality products, services and business relationships. As a manufacturer of plastic cartridge tubes for greases, Biederman continues to gain momentum in the global marketplace. As a market leader for plastic grease cartridge tubes with metal ends, our tubes offer uncompromised stability on grease fill production lines, transport, and display shelves. Complete with an easy to open metal pull-tab removal, there is virtually no tearing and no tools are required, eliminating end-user frustration and product waste.

- 40 VOLUME 80, NUMBER 3

Caltex Australia – Manufacturer Melissa Quinn GPO Box 3916 Sydney, NSW 2001 Australia 61-477-934-083 https://www.caltex.com.au/

dtb2 LLC - Technical Derek Benedyk 500 West Bradley Road, A#219 Fox Point, WI 53217 USA 312-206-4819 www.dtbtwo.com

Caltex is Australia’s leading transport fuel supplier and convenience retailer and the only integrated oil refining and marketing company listed on the Australian Securities Exchange. Our business value chain incorporates operational excellence throughout supply, refining, logistics and marketing. Caltex Australia operates the country’s largest lubricants-blending facility, located at Lytton in Queensland, and is one of only 3 grease manufacturers in Australia.

Crystal, Inc – PMC - Supplier Ted Fickert 601 West 8th Street Lansdale, PA 19446, USA 215-368-1661 http://pmccrystal.com PMC Crystal combines over fifty years of experience in formulated specialty additives and products based upon wax and oleochemical feedstocks, a commitment to continuous product innovation and service and a broad range of manufacturing technologies to provide innovative solutions to its global customer base. Our product range includes specialty antifoam and defoaming agents, metallic stearates, rubber and plastic processing aids, cable filling compounds, wax emulsions, specialty petrolatum and waxes.

Dorf Ketal Chemicals LLC - Supplier Sally Pavlica 310 Willow Pointe Dr League City, TX 77573 USA 713-907-6525 www.dorfketal.com Dorf Ketal Chemicals is a global leader in the development, commercialization, marketing and application of specialty-engineered chemistries for the refining and petrochemical industries. Founded in 1992, Dorf Ketal has demonstrated product and service excellence in the largest refineries and petrochemical plants in the world.

dtb2 LLC is a research and development company, dedicated to providing solutions for; unique lubricant formulations and applications, as well as, technical field service support and analysis of lubrication applications and processes.

Fischbach USA – Supplier Terry Clagett 900 Peterson Drive Elizabethtown, KY 42701 USA 270-769-9333 www.plasticgreasecartridge.com Fischbach manufactures 100% plastic grease cartridges with manufacturing sites in the USA and the UK. We also manufacturer grease cartridge filling equipment, case packets and palletizes.

Gulf Petrochem FZZC - Supplier Sudip Shyam Hamriyah Free Zone Sharjah 41506 United Arab Emirates 009-716-526-4944 http://gulfpetrochem.com/business/lubricantsmanufacturing/ Gulf Petrochem recently acquired Sah Petroleums - an ISO 9001:2008 & EMS 14001:2004 certified company, specializes in designing, manufacturing and marketing, industrial & automotive lubricants, process oils, transformer oils, greases and other specialties under the brand name IPOL in India and internationally for more than three decades.

- 41 NLGI SPOKESMAN, JULY/AUGUST 2016

New 2016 NLGI Members

IHS Global SAS - Technical Souna Kang 16-18 Rue du Quatre Septembre Paris, France 75002 33-1-47-70-7849 www.ihs.com

Pan American Equipment – Marketing Jim Newcomm 2419 S 153rd St Omaha, NE 68144 USA 402-502-1229 http://www.panamequipment.com

In today’s global business economy, access to reliable, accurate data is crucial to making the best possible decision. As the premier provider of global market, industry and technical expertise, IHS Markit understands the rigor that goes into decisions of great importance with solutions that meet the needs of our customers.

Morgan Distributing Inc. - Marketing Beth Medlen 3425 N 22nd St Decatur, IL 62526 USA 217-877-3579 www.mdilubes.com Morgan Distributing Inc. is an oil distributor in Illinois, Missouri, Indiana, Iowa, Kentucky, and Arkansas. We deliver the highest quality motor oils, industrial lubricants, metalworking and specialty fluids to our customers. We pride ourselves on excellent customer service and take a total cost of ownership approach to lubrication. We provide industry-leading technology through synthetic lubrication, energy savings analysis and assist in the development of long term sustainable maintenance programs.

Pan American Lubricants are premium products formulated for a wide variety of applications and environments, with special emphasis on the requirements of commercial bakeries and other food producers. Pan American Lubricants include Food Grade and Non-Food Grade products that comply with USDA, NSF or USP specifications. Our products include petroleum/mineral based fluids, semi-synthetic and fully synthetic lubricants, coolants, greases & bearing gel, cleaners and de-scalers. unningland Metrology & Testing R (Shanghai) Co., Ltd - Technical David Ahou 128 Xiangyin Rd, Ste 101, Bldg C Shanghai, 200433 CHINA 0086-21-6530-1818 www.runningland.cn Runningland Metrology & Testing (Shanghai) Co., Ltd is a certified and accredited independent third party laboratory for instruments metering, calibration and testing in the petrochemical industries. Runningland undertakes products testing for petrochemical products and equipment condition monitoring.

The company operates two professional labs in Shanghai for:

• I nstruments Metering, Calibration & Testing

• Petroleum Oil Testing

• Condition Monitoring 3rd Party, ISO 17025 certificated, Oil, Grease fluid testing lab in China and Asia Pacific Region. We offer analysis, condition monitoring and instruments metrology. Our samples testing turn around time is very quick.

- 42 VOLUME 80, NUMBER 3

Thames River Chemical – Supplier Andy McGivern 5230 Harvester Road Burlington, ON L7L 4X4 Canada 905-220-2321 www.trc-corp.com Thames River Chemical Corp. distributes chemical products in specialized markets across North America. As a member of the Canadian Association of Chemical Distributors we value the protection of health, safety and environment and ethical business practices.

The Unami Group, LLC - Technical Bill Tuszynski 27 S Vassar Drive Quakertown, PA 18951 USA 267-374-1631 www.unamigroup.com The Unami Group, LLC is a consulting organization providing strategic, commercial and technical support to help clients identify and develop profitable business opportunities in the chemical, lubricant, materials and adjacent segments.

Thompson Creek Metals Co., USA – Supplier Mark Wilson 26 West Dry Creek Circle, Suite 810 Littleton, CO 80120 USA 303-761-8801 www.thompsoncreekmetals.com Molybdenum Producer - Thompson Creek Metals Company Inc. is a North American mining company engaged in the full mining cycle, which includes acquisition, exploration, development, and operation of mineral properties.

In the past several years, we have evolved from being a major primary molybdenum producer to becoming a copper and gold mining company with the construction and development of the Mount Milligan open-pit copper-gold mine and concentrator in British Columbia, Canada. In addition to Mount Milligan Mine, we own and operate a metallurgical facility in Pennsylvania, USA, at which it roasts molybdenum concentrate and other metals.

- 43 NLGI SPOKESMAN, JULY/AUGUST 2016

The Development of More Environmentally Considerate Greases By: Gareth Fish, PhD CLS CLGS The Lubrizol Corporation

Abstract

Reduced environmental impact through the choice of suitable greases has become an important consideration of many end users.

Emerging government legislation and policies place emphasis on product life cycle impact upon the future protection of global natural resources. Programs in Europe and North America have prompted research and development of new grease additive packages and component technologies. There is greater demand for environmentally considerate base fluids and thickeners. Recent technology developments have enabled biobased and eco-considerate grease products to achieve a high level of performance directed toward total loss applications including farming, forestry, marine and mining.

Environmentally considerate greases require carefully selected base fluid(s) meeting specific biodegradability or bio-based criteria while providing an acceptable level of performance to the end user. The base fluids can be either refined vegetable oils, estolides or synthetic

esters. Biodegradable polymeric esters to boost the viscosity of the base fluid can be included.

Thickener selection is also important in creating environmentally considerate greases. Simple thickeners can be prepared from pre-formed soaps such as calcium or lithium 12-hydroxystearate, or using inorganic thickeners such as clays or silica. Both simple lithium and high temperature lithium complex greases can now be prepared directly using anhydrous lithium hydroxide dispersions.

After a base fluid and thickener have been chosen, the next step is to select an additive that offers the performance desired without negatively impacting the environment. We reviewed current ecological and toxicological data and were able to create a variety of environmentally considerate grease formulations.

Introduction

In 1980, the Comprehensive Environmental Response, - 44 VOLUME 80, NUMBER 3

Compensation and Liability Act (CERCLA) was passed which established the setting up of process for identifying, containing and cleaning up contaminated toxic waste sites in the USA(1). It empowers the US Environmental Protection Agency (EPA) and its supporting organizations to control such sites and to compel responsible parties to perform cleanups or reimburse the government for EPA-lead cleanups. CERCLA is commonly known as “superfund�. The cost of this process is extremely high and it has been recognized that it is better to avoid pollution rather than pay for it to be cleaned up. According to EPA published figures (1) this has led to much improvement in the general environment and the successful re-use of once significantly contaminated land.

At the 1991 ELGI Annual Meeting (2), it was reported that in 1990 the European Commission had carried out a study into automotive greases and had concluded that more than 4000 tonnes of grease was lost into the environment from trucks. The basis for the calculation

is unclear but based on estimates of European grease production, this would amount to about 3% of the volume of automotive greases produced. The response of the Directorate-General for the Environment of the European Commission was to draw up voluntary codes for the development and use of more environmentally friendly lubricants. Prior to this there was no accepted or agreed definition of what environmentally acceptable lubricants (EALs) were.

In 1992, the EU launched their Eco-label voluntary scheme which in 2005 was extended to include lubricants. It was further modified in 2011 to include a wide range of thickeners and to clarify elements within the originally published document (3). In their 1999 Lubricants and Hydraulic Fluids Manual (4), the US Army Corps of Engineers (USACE) recommended use of the term “environmentally acceptable” lubricants (EALs) to describe lubricants that were both biodegradable and non-toxic and could be used in non-military USACE facilities such as hydropower plants, flood-control pumping plants, and lock-and-dam sites. Neither the requirement of a renewable content nor bioaccumulation potential were addressed within this original definition of EALs. It was reported that the “environmentally acceptable” terminology had been developed by various American Society for Testing and Materials (ASTM) committees to address environmental lubricant standards. It was noted (3) that “food grade” lubricants by their very nature are non-toxic and mostly based on white mineral oil, but because they are not normally readily biodegradable, cannot be EALs. Federal Water Pollution Control Act (4), commonly referred to as the Clean Water Act (CWA), was approved by congress in 1972. Its aim was to restore and maintain the chemical, physical, and biological integrity of the waters in the USA by preventing pollution. It also aimed to improve wastewater treatment along with maintaining the integrity of wetlands. This was further modified by the Clean Water Act of 1977 and the Water Quality Act of 1987 (4). Drinking water and ground water contamination are covered by other acts including CERCLA. It was identified that there is a need to prevent oil pollution from ships in both coastal and inland waters. In response to this the first vessel general permit (VGP) covering lubricants used on US inland

and coastal waters was enacted in 2008. Part of it was a voluntary code developed by the US Environmental Protection Agency (EPA) to encourage commercial ship owners to use EALs for all water interfaces. In December 2013 this became a mandatory requirement to use VGP compliant lubricants if they are available (5). In the introduction to the VGP regulation, it was reported that there are 4708 commercial ports and that globally ships make an estimated 1.7 million visits per annum to those ports. It was also noted that the average commercial vessel discharges 2.6 liters of lubricants per day, mostly from stern tubes. Total global lubricant loss to the marine environment was estimated at 50 million liters per annum, of which 16 million liters were stern tube discharges. One of the aims of the VGP was to reduce stern tube lubricant discharges, as they were estimated as costing the USA about $31 million in clean-up costs, which were about 10% of the global costs of marine lubricant spill mitigation. Both the EU and the EPA, along with other government regulators have imposed increasingly stringent regulations on the use, containment, and disposal of marine lubricants.

One aspect of newer legislation is that that as well as discharges from ships, no visible oil sheen be evident downstream from industrial facilities located in or close to waterways. Other regulation requires that discharges into waterways should not exceed 10 parts per million of mineral-based oils. All these regulations are driving the use of more environmentally compatible lubricants in marine applications.

Environmentally Acceptable Lubricants

Although EALs have been in commercial production for many years, they still comprise a small portion of the total lubricant market. According to the 2013 NLGI Grease Production Survey (6), it was identified that globally, 5340 tonnes of lubricating grease were reported as being produced using bio-base fluids, which represents 0.45% of the total annual volume. Bio-based greases are still regarded as niche products. Also from the survey, 40,000 tonnes of synthetic greases were produced. It was estimated that approximately 10% of synthetic base oils use synthetic esters, giving an additional 4000 tonnes of potentially biodegradable grease. Combining both biobased and synthetic esters, the total production volume is still represents <1.0% of the total grease market.

Looking at the market for mineral oil based greases,

- 45 NLGI SPOKESMAN, JULY/AUGUST 2016

they still account for approximately 93% of the volume manufactured with the rest being semi-synthetic, fully synthetic and bio-based. The higher cost of bio-base fluids is an issue. In 2013, comparative costs were presented (7) and showed that in relative terms, plant derived fluids such as soybean oils were about a 30% premium on the cost of 600N API group I mineral oil.

High erucic acid content canola oil was about an 80% cost premium and high oleic acid sunflower oil was about a 100% cost premium.

Looking at biodegradable synthetic esters and estolides, they command a four to five times multiple of the cost of mineral oil. As the base oil is 80 to 90wt% of the finished grease, this adds a considerable cost mark up to supplying bio-based and biodegradable over mineral oil based greases.

However, the market for EALs continues to expand, particularly in Europe. In some countries, legislation mandates the use of environmentally compatible lubricants. Examples of this are rail curve greases in Sweden and forestry machinery lubricants and greases in Austria. In some areas the use of such lubricants is being encouraged through a combination of governmental tax breaks or purchasing subsidies. There are also voluntary schemes for using environmentally better lubricants, based on well-defined criteria. Many lubricants are advertised as being environmentally preferable; however, currently there are limited standards for EALs, and no internationally accepted term by which they are defined. To distinguish lubricants which have been shown to be both biodegradable and non-toxic according to acceptable test methods

from those lubricants that are simply marketed as being “environmental” or with similar terminology. A review of publically available datasheets on the internet showed that at a minimum a lubricating greases without chlorine or heavy metals were considered to be environmentally friendly.

The technology of greases has moved forward in many areas. It was reported at the 2010 NLGI Annual Meeting (8) that many of the traditional extreme pressure (EP) additives used in greases were not usable. In Europe, lead additives and chlorinated paraffins have been banned. The global automotive industry has played a significant role in reducing or eliminating the use of hazardous chemicals in automobiles. It uses a black (banned) and grey (reportable or restricted) list of substances that is published on the Global Automotive Declarable Substance List (GADSL). This clearly states which chemistry is not allowed in automobile lubricants (9). Many other traditional chemistries used in lubricating greases are being reviewed as part of REACH activities.

Today, in North America, the use of lead and chlorinated paraffins is not so restricted. Greases containing lead additives, can be offered for sale but the containers would attract significant warning labels and this, combined with issues related to the used grease being labelled as hazardous waste have resulted in no domestic supply of leaded greases. More chemical hazard data is being generated as part of global REACH activities, and this will inevitably lead to restrictions in the use certain chemicals in lubricants.

The development of sustainable chemistry for lubricants is now on - 46 VOLUME 80, NUMBER 3

the center stage.

Vessel General Permit Greases As laid out in the provisions of the VGP, lubricants for marine applications must meet a series of criteria when they are used in shipwater interfaces. Similarly to the Ecolabel requirements, there are different criteria for liquid lubricants and greases. For VGP greases, it states that at least 75wt% of the grease must be a biodegradable base oil. The narrative in the document suggests that it can be from a biobased ester, a synthetic oil or a polyglycol provided it meets the biodegradability requirements. The requirements are >60%wt readily biodegradable within 28 days using Organization of Economic Co-operation and Development (OECD) 301-type tests or >70%wt inherently biodegradable using an OECD 302-type test. The second requirement is that the grease must be minimally toxic and thirdly it must be not bioaccumulative.

The remaining 25% of the grease formulation does not need to meet the readily / ultimately biodegradable requirement, but it does need to be either inherently or non-biodegradable and it cannot be (potentially) bioaccumulative.

It terms of VGP, inherently biodegradable means that it is between 20%wt and 60%wt using an OECD 301-type test or ≥70%wt OECD 302-type test. Similarly nonbiodegradable is defined as ≤ 20%wt when using an OECD 301-type test or ≤ 70% when using an OECD 302type test.

Within the VGP document, there are some things that are not clear and are currently open to interpretation.

With respect to having minimal

aquatic toxicity, it states that the complete formulation and main components must pass OECD 201(algae), OECD 202 (crustaceans) and OECD 203 (fish) for acute toxicity or OECD 210 and OECD 211 for chronic toxicity with an LC50 ≥ 1000 mg/L. Within the Ecolabel it defines what main components are (>5%wt of the finished formulation) but does not in the VGP. The VGP level of toxicity is similar to Ecolabel requirements of >1000 mg/L for main components. However the Ecolabel and VGP diverge with trace components. Under Ecolabel no substance which is present above 0.1%wt can have a toxicity of LC50 ≥ 100 mg/L. The VGP is seemingly less severe in that it allows no observable effect concentration (NOEC) to be used. Substances < 20% of the formulation must have either an 10 ≥ LC50 ≥ 100 mg/L or 1 ≥ NOEC ≥ 10 mg/L. Substances < 5% of the formulation must have either an 1 ≥ LC50 ≥ 10 mg/L or 0.1 ≥ NOEC ≥ 1 mg/L and substances < 1% of the formulation must have either an LC50 ≤ 1 mg/L or 0 ≥ NOEC ≥ 0.1 mg/L. The VGP also allows alternative tests may be used: ISO/ DIS 10253 for algae; ISO TC147/ SC5/W62 for crustaceans; and OSPAR 2005 for fish.

With respect to bio-accumulation potential data, VGP does not appear to state the concentration level in the final formulation that requires bioaccumulation potential to be determined. This is unlike Ecolabel where all substances present in the final formulation ≥ 0.10 %wt have to be reported. Other than the amount present, the criteria for bioaccumulation potential are almost identical. Large molecules which

cannot cross cell wall membranes based on molecular size with a molar mass of >800 g/mole or molecular diameter of >1.5 nm are exempt.

Polymers are also exempt when they have a molecular fraction of monomer or lower molecular weight (below 1000 Daltons) concentration of <1.0 %wt. The measured bioconcentration factor (BCF) in fish using OECD 305-type of test must be less than 100 L/kg. The final method defined is the octanol / water partition coefficient, Log Kow. It can be measured using OECD 107 or 117 test methods or calculated from model data using a variety of standardized commercially available models. VGP requires Log Kow to be less than 3 or greater than 7 (3< Log Kow >7) for it to be classified as non bioaccumulative. This is the same as Ecolabel.

VGP does not appear to outright ban many of the hazardous substances that the Ecolabel places restrictions on, but waste from ships cannot include substances on the hazardous waste list as defined in 40 CFR 401.15 (10). Many of the items on this list are similar to those banned substances on GADSL. In addition, this list includes antimony, whose dithiocarbamate is a powerful EP additive, and zinc compounds, which as zinc dithiophosphates are the most common anti-wear additives used in greases.

One advantage for global lubricant developers is that products approved as meeting the following standards are automatically approved as VGP approved lubricants: Blue Angel; EU Ecolabel; Nordic Swan; Swedish standards SS 1554434 and 155470; Convention for the protection of - 47 NLGI SPOKESMAN, JULY/AUGUST 2016

the marine environment of the NE Atlantic (OSPAR); and the EPA’s Design for the Environment (DfE) Ecolabel Grease and the Lubricant Substance Classification (LuSC) list As outlined (7) there are five sub-categories of lubricants under Ecolabel of which sub-category 2 covers lubricating and stern tube greases. There are seven basic requirements for each sub-category, some of which are slightly different based on the type of lubricant. For approval, a complete dossier must be provided to the EU competent body which contains all required supporting documentation, analysis, test reports and declarations. All constituent substances present above 0.010%wt which are intentionally added or formed during a chemical reaction must be stated, giving their chemical names and CAS and EC registration numbers where applicable. The criteria also aim to promote products that have a reduced impact on water and soil, as well as containing a large fraction of bio-based material.

One aspect of EU toxicology and chemical / substance testing is they wish to reduce the amount of testing that is necessary to safeguard health, safety and the environment and encourage data sharing. To this aim they have developed and regularly update the EU Lubricant Substance Classification (LuSC) list (11). Part 1 of this list defines what chemicals have been tested for biodegradability and aquatic toxicity / bioaccumulation potential and up to what level they can be used in lubricant formulations. Part 2 of the list, covers commercial, branded lubricant components and is broken down into base fluids,

thickeners and additives. In addition to biodegradability and aquatic toxicity / bioaccumulation potential, renewable carbon content is included. No thickeners are currently registered as trade names but several grease thickener components are included in part1, the listing of chemicals. When formulating Ecolabel lubricants is a substance, base fluid or additive is already present on the LuSC list and is used below the threshold limit, the need for full testing and registration of that component is unnecessary. It is however still necessary to provide a complete bill of substance, comply with the labelling requirements and pay the registration fees to a Competent National Body to have the lubricant Ecolabel approved and allow it to carry the flower symbol on the container and in promotional material.

Formulating VGP Greases

The starting point for all VGP greases is the base oil.

The narrative in the VGP document suggests that either bio-based fluids, synthetic esters, or polyglycols can be used as base fluids. The focus on this work has been to use bio-based fluids and synthetic esters rather than polyglycols.

The first issue is that the majority of vegetable oils sold on the market today are of much lower viscosity than is desired for greases for higher performance marine or industrial lubricants, with most fluids having kinematic viscosities of <100 mm2/s at 40 °C. A notable exception being rapeseed or canola oil. Typical industrial grease have base oil viscosities at ISO VG 220 and above whilst those used in automotive applications are typically ISO VG 100, 150 or 220. Wire rope greases typically have base oil viscosities of 500 mm2/s at 40 °C which makes it even more of a challenge to achieve. For industrial lubricants, brightstock is typically added to boost viscosity to the higher viscosity grades, but they cannot

be used in VGP oils. Another common solution for industrial lubricants is to use polyisobutylene (PIB) viscosity boosters, but they too cannot be used in Ecolabel greases and the amount that could be applied to VGP greases is limited to less than about 10%. One advantage that both vegetable and synthetic esters have over typical group I mineral oils is that they have base oil viscosity indices above 150.

The properties of five commercially available base fluids were chosen for the first part of the study. These included soybean oil, high erucic acid canola oil, high oleic sunflower oil, an estolide based on polyricinoleic acid and a synthetic diester. The basic properties of these fluids are compared in table 1 along with those of a 600N API group I mineral oil, which whilst it was not biodegradable was used as the performance control for the basic properties of the subsequent greases.

The best solution for boosting the low viscosity of biodegradable base oils to the required grades is to add polymer esters to them. There are a number of higher viscosity polymer esters on the market which have good biodegradable data and can be based on renewable, plant derived, raw materials such as coconut oil. The general properties of some of the polymer esters are compared with a typical PIB used as a brightstock replacement in industrial and open gear lubricants and greases.

Compatibility of the polymer esters with other oils was checked by making and storing blends to check for separation.

The next selection point is the thickener. When the first Ecolabel standard came out, only calcium or sodium soap thickeners were allowed. The relaxation of the Ecolabel standard allowed lithium and aluminum soaps to be used in greases. However the presence of water in a normal saponification reaction caused the water

- 48 VOLUME 80, NUMBER 3

sensitive bio-based esters to degrade and be strongly acidic. This meant that it was only possible to use preformed simple sodium, calcium or lithium soaps to thicken these water sensitive base oils. Pre-formed sodium soaps are available but not widely marketed.

Anhydrous calcium soaps (12-hydroxystearate) will give grease dropping points of 140 – 150 °C and those of preformed lithium stearate or 12-hydroxystearate will give grease dropping points of 180 to 200 °C, but these ranges are somewhat dependent on the base oils, especially if exotic fluids with significantly different polarities and solvencies compared to mineral oils are used. At the NLGI Annual Meeting in 2001, Bessette (12) outlined how to use pre-formed soaps “Dry Technology” to make greases with pre-formed simple thickeners in a variety of different base oils, including water sensitive ones.

One challenge using pre-formed soaps is that there is an absence of free alkali. The majority of directly saponified greases use a slight to moderate excess of the base metal.

In saponification this helps to drive the reaction forward.

This is not necessary when using pre-formed soaps.

With acidic base oils, any free alkalinity also neutralizes the acidity and helps to stabilize the grease, but this cannot be achieved with pre-formed soaps.

Honary (13) outlined several manufacturing techniques methods that could be used in the production of greases with temperature and water sensitive vegetable oils. He explored the various issues with the different ways of making grease in bio-based oils and noted the following issues. Pre-formed soaps still have to be heated to melt the soap and are not readily available as complexes. There were similar issues with soap concentrates which worked well but introduced mineral oils into the grease. Lithium hydroxide dispersions (14) were also investigated and

were reported as working well but again introduced small amounts of carrier fluids. At the time of reporting Honary (13) suggested that microwave heating technology was able to drive the saponification reaction quickly and heat the grease up to melting temperatures without significant degradation.

The small particle size (<10 μm) of the lithium hydroxide in the dispersion allows it to react very quickly with the thickener acid and if present the complexing acid. The only water present is from the saponification reaction and it is easily removed with minimal hydrolysis of the base oil. This also minimizes the foaming associated with the water removal, which is where hydrolysis of the ester normally occurs. Further development of the manufacturing process that utilized anhydrous lithium hydroxide dispersion technology showed that it could make high quality lithium and lithium complex greases directly in water sensitive base oils (15). For VGP greases, introducing a small amount of mineral oil and surfactant from the lithium hydroxide dispersion is acceptable but for Ecolabel greases all components above 0.1%wt need to be evaluated.

Available data led to the use of an anhydrous lithium hydroxide dispersion for use in an Ecolabel grease.

Reviewing the European LuSC (11), lithium 12-hydroxystearate is useable as a greases thickener for bio-greases as is dilithium sebacate, up to a prescribed limit. Dilithium azelate can be used to thicken sensitive and bio-based oils, but it is listed as having aquatic toxicity and is not useable in Ecolabel greases. This does not mean that azelate lithium complexes cannot be used in VGP greases, but their use gives little to room for performance additives to be included and significantly tightens the formulation space. From this

- 49 NLGI SPOKESMAN, JULY/AUGUST 2016

it is clear that making a grease with 12-hydroxystearic acid and sebacic acid can be used to make high dropping point Ecolabel and VGP greases. The use of these acids In VGP allows for other non-biodegradable but nonbioaccumulative components to be included in the overall formulation provided the amounts of nonbiodegradable components are within the allowable limits outlined above.

In order to verify the lithium hydroxide dispersion route, base greases were manufactured using the base oils listed in table 1. The thickener was either simple lithium or lithium complex utilizing a 3:1 12-hydroxystearic acid to sebacic acid ratio. The greases were made slightly stiff so that they could be cut back to an NLGI grade 2 using

the corresponding base fluid. The properties of the base greases are included in table 3.

From the results in table 3 of the greases manufactured, it is clear that no two VGP usable oils behave in a similar manner with respect to thickening or grease properties and nor do they behave similarly to mineral oils. This makes the task of formulating greases to meet technical targets much more difficult. Currently, the only way to progress the development of VGP greases is to manufacture the intended soap in the selected base oil and check the properties of the base grease. From there decide if more thickener is needed. A further issue noted was that when the three vegetable oils were heated to top temperature darkening occurred.

Simple lithium greases are normally

heated to over 200 °C to fully melt the soap and then recrystallize it.

The lithium complex greases are cooked to a top temperature around 190 °C and held. Fluids with a high degree of unsaturation are more prone to oxidation and degradation than saturated ones. Heating the grease too hot or holding it at top temperature too long oil causes the oil / grease to darken and may lead to a rancid odor. If the grease darkens during manufacturing or the oil appears to have degraded, it may be necessary to modify the cooking conditions in order to protect the oil from degradation.

One possible route is to add some or all of the anti-oxidant into the oil before cooking the thickener.

A grease additive package, which is listed on the EU LuSC was selected for incorporating into some greases

of the base greases listed above to see how it performed in terms of simple wear tests. The data is shown below in table 3 and compared to the grease industry NLGI GC-LB standard for those tests. The results show that all four of the greases gave good 4-Ball EP performance. The amount of wear measured in the 4-Ball wear tests was satisfactory for the canola and estolide fluids. Comparing this 4-Ball wear data with the D4170 fretting wear tests showed little correlation with each other. The fretting test is run at room temperature for 22 hours at room temperature and the 4-ball is run for 1 hour at 75 °C. It is known that greases with low viscosity oils that have higher oil bleed rates do well in the fretting test, which may explain the very good result of the soybean oil grease, and the worse result of the others.

In looking at the properties of the base greases, one other issue was identified. Many bearings use seals or shields manufactured from elastomers and synthetic rubbers. Some of these sealing materials contain plasticizers, typically either naphthenic oils or low molecular weight diesters such as dioctyl sebacate.

Synthetic ester base fluids have a tendency to diffuse into the seal material and there is an exchange with the base oil and oil soluble additives of the grease. In some instances this interchange can be beneficial such as bring in oil soluble anti-oxidants into the seal. In other cases the plasticizer can be extracted from the seal before the base oil can diffuse into the seal to replace it. This latter case is true of higher viscosity polymer esters which in the short term can result in shrinkage or loss of low temperature flexibility. When running standard elastomer tests such as D4289 with low viscosity synthetic esters, the reference ASM3217/3C polychloroprene elastomer was seen to swell up 50%wt compared to a typical specification limit of 40%wt. The nitrile reference elastomer ASM3217/2C was seen to

swell up to 45%wt compared to a typical specification limit of 30%wt. Out of specification hardness changes were also seen with many of the esters tested. The higher viscosity estolide and polymer esters, due to their much larger size and slower diffusion rates into the elastomers, did not causing excessive swelling or softening and were typically within specification limits. One thing that was also seen with the nitrile compatibility test is that running at 150 °C caused significant degradation of all the fluids and some surface oxidation of the test coupons.

For some applications such as wire ropes and also for enhanced water resistance, it is necessary to add a tackifier. For typical greases, styrene-isoprene (SIP) or ethylene-propylene (OCP) co-polymers and PIBs are used as tackifiers. The use of PIBs was discussed above, but the main issue with typical tackifiers is that they do not readily dissolve in the more polar esters. Several SIP and OCP tackifiers were tested in the base oils in table 1 and most did not dissolve. One of the polymers investigated was described as being soluble in esters, but it did not dissolve in the soybean oil. A trial grease was manufactured with the only OCP polymer that readily dissolved in most esters, and tested. The tackiness test results showed that the tackifier was not as effective in the bio-based oil (25% loss) as it was in a mineral oil (0% loss); nonetheless, a 75% improvement in cohesion/ adhesion was observed. The reasons for this are as yet unclear but it is likely that the greater polarity or solvency of the esters played a role. A second polymer, an SIP block co-polymer, was found to incorporate more readily than the OCP. Initial work showed this SIP to be a better choice of tackifier for the proposed VGP greases. From the work carried out, it is clear that testing for solubility of multiple polymers may be necessary to find one which works in the fluid of choice.

Based on the above work, a series of base oil blends to meet the required kinematic viscosities were developed, Table 5. These were then blended and de-aerated.

Their viscosities were measured and compared to the theoretical values and the blends were checked for compatibility.

Two out of three blends for the ester gave hazy mixtures which made measuring the viscosity difficult and so calculated results are reported, rather than actual measurements. The fluid blends 1 and 3 between Ester A and D showed clarity and compatibility, but blend 6 was slightly hazy. This illustrated that polymer esters can have limited solubility in lower viscosity esters. However when making greases from the fluids, some haziness was not found to impact the grease making.

Lithium complex greases using the 3:1 12-hydroxystearate and the anhydrous lithium dispersion were manufactured initially with 2% of the SIP added. The LuSC listed grease additive package described above was incorporated. The greases were milled and de-aerated and standard grease tests were carried out on them. Test results for the

greases are in table 6 below. A polymer ester similar in viscosity to Ester E was also tested for use in the 500 mm2/s grease but was found to be incompatible with the Diester, Ester A and Ester B. They mixed well in the laboratory and once de-aerated formed clear viscous mixtures, which separated into two phases on standing overnight at room temperature.

Open Gear Lubricants for Mining

Most open gear lubricants (OGL) and mining greases have very high base oil viscosity requirements.

They are higher than are seen with industrial oils and much higher than can be achieved with natural oils. Traditionally to boost the viscosity of mining lubricants bitumen was added. For lower viscosity requirements, brightstock is used for the same purpose.

Neither of these choices can be used in VGP or Ecolabel greases.

Polyisobutylenes (PIBs) have largely replaced bitumen in many mining lubricants and these are also applied along with high viscosity to industrial lubricants. PIBs are not biodegradable (OECD 301B <20%) due to their degree of branching and cannot be used in Ecolabel grease

- 52 VOLUME 80, NUMBER 3

in any significant volume. To make more environmentally considerate mining open lubricants, it was investigated to see if biodegradable polymer esters could be combined to meet the viscosity requirements of the AGMA Specification. Using the three higher viscosity polymers esters C, D, and a series of blends were calculated to meet the viscosity requirements. These were then blended and de-aerated. The blends were checked for compatibility. The data is shown in table 7.

As proof of concept, OGLs of each of the oil blends had 4%wt of a premium open gear additive package added and tested against some basic greases tests. The results are in table 8.

A second set OGLs of each of the oil blends had 6%wt of a premium open gear additive package added and tested against some basic greases tests. The results are in table 9.

The results in tables 8 and 9 showed that it is possible to formulate high viscosity OGL with good laboratory performance that are more environmentally considerate than existing technology.

- 53 NLGI SPOKESMAN, JULY/AUGUST 2016

From previous work (16), the other two key tests needed are Timken OK load and FZG testing. AGMA 9005-E02 requires an FZG D5182 (A/8.3/90) with a passing stage of 12. AGMA 251.02 requires FZG D5182 (A/8.3/90) with a passing stage of 12 and a minimum Timken OK load by ASTM D2782 of 45 pounds.

Testing on some of the better performing greases is reported in table 10, along with comparative data from a commercially available OGL and two PIB blends (16) which used the same additive package.

The data in table 10 suggests that OGL mining fluids could potentially be manufactured using more environmentally friendly base fluids. They meet the minimum performance levels to be considered for field trials.

Summary and Conclusions

This paper has shown that there is now technology available to help the grease developer produce high quality lithium complex greases to meet the requirements of the VGP. The key enabling technologies outlined are the use of anhydrous lithium hydroxide dispersions, polymers esters and a LuSC approved additive package.

The technology developed for VGP greases has also been shown to be applicable to the development of mining greases and OGLs for the development of environmentally considerate higher performance lubricants.

Acknowledgements

The author wishes to acknowledge many co-workers and departments within The Lubrizol Corporation for their contributions to this work.

References

(1) “Comprehensive Environmental Response, Compensation and Liability Act” 1980 published by the Office of the Law Revision Counsel of the U.S. House of Representatives available through www. epa.gov/superfund (2) Presentation at the 1991 ELGI Annual Meeting (3) Council of the European Union, “Establishing the Ecological Criteria for the Award of the EU Ecolabel to Lubricants”, Official Journal of European Union, 29.6.2011, L 169 pages 28 to 39 (www.ec.europa.eu/

environment/ecolabel) (4) “Engineering and Design Manual - Lubricants and Hydraulic Fluids” EM 1110-2-1424, U.S. Army Corps of Engineers, Department of the Army Washington, DC 20314-1000 published 28th February 1999 (5) http://water.epa.gov/polwaste/npdes/vessels/VesselGeneral-Permit.cfm (6) NLGI Grease Production Survey 2013 (2014), NLGI Lee’s Summit, MO 64063 (www.NLGI.org) (7) Fish, G., Robinson. P, and McSkimming, N. “Understanding Component Requirements for Formulating High Performance Environmentally Acceptable Greases” ASTM symposium on Environmentally Considerate Lubricants, December 9, 2013, Tampa, FL (8) Fish, G. and Ward Jr, W.C., “Extreme Pressure Performance of Greases: Testing and Additive Solutions” NLGI Spokesman (2011) volume 75(3) pp12-27.

(9) Global Automotive Declarable Substance List (GADSL). www.gadsl.org (10) US Government Publishing Office (2011) CFR 2011 40 volume 29 section 401 part 15 www.gpo. gov/fdsys/granule/CFR-2011-title40-vol29/CFR2011-title40-vol29-sec401-15 (11) EU Lubricant Substance Classification (LuSC) list www.ec.europa.eu/environment/ecolabel/ documents/LuSC-%20list.pdf (12) Bessette, P.A., “Manufacturing Grease Using Dry Technology”, NLGI Spokesman (2002) Volume 65 (11) pages 14-17 (13) Honary, L; “Market Opportunities in Biobased Lubricating Greases”, 76th NLGI Annual Meeting Address 2009, Loews Ventana Canyon, Tucson, AZ, June 15th 2009 (14) Nolan, S.J. and Zeitz, J.B. “Anhydrous Lithium Hydroxide Dispersion: A New and Efficient Way to Make Simple and Complex Lithium Greases”, NLGI Spokesman (2007) Volume 71 pp17-24 (15) Denis, R. A. and Nolan, S.J. “Grease Composition” US Patent 8,796,191 USPTO August 5, 2014 (16) Lorimor, J.J. and Hsu, C., “Understanding Open Gear Lubricants: Product Design Considerations”, NLGI Spokesman (2013) Volume 77 pp17-24

- 54 VOLUME 80, NUMBER 3

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NLGI Industry News Please send all industry news, events, employment news and press releases to Marilyn Brohm.

(Your company does not have to be an NLGI member to post items.)

7/18/16 – STRATCO’s NEW HEADQUARTERS – The new address at 7440 E. Karen Dr., Suite 400, Scottsdale, AZ, 85260 is not only our new offices; it is also our new Research Center with a lab, featuring the STRATCO® Pilot ContactorTM reactor.

We are excited about having our research lab fully operational again. We already have several intriguing research projects planned and we are looking forward to once again offering our laboratory services to existing and future Customers. The new Lab will combine elements of our previous laboratory with newer models of our Contactor reactor that allow us to develop new uses for our equipment and also support our Customers in developing new products. To read the complete press release visit: https://www.nlgi.org/news-and-events/industry-news/

Jet-Lube Inc. Relocates its Houston, Texas Manufacturing Plant to a State-of-the-Art Facility in Rockwall, Texas New Headquarters, Manufacturing & Distribution Location Rockwall, Texas. June 17, 2016 – Jet-Lube Inc., a CSW Industrials Company, and leading manufacturer of specialty chemical products announces its headquarters relocation to Rockwall, Texas. Jet-Lube plans to consolidate and combine forces with Whitmore, a specialty chemicals CSW Industrials Company.

“This was a strategic move on behalf of our company” says Jet-Lube Vice President of Sales, Tom Blake. “We wanted a central location with a state-of-the-art facility that would allow us to increase production and expedite delivery across our customer base.” To read the complete press release visit: https://www.nlgi.org/news-and-events/industry-news/ Croda Announces the Latest in Base Stock NEW CASTLE, DE (June 14, 2016) With years of formulation expertise and insightful trend knowledge, Croda, a global specialty chemical company, introduced a new base stock for automotive and industrial applications at STLE’s annual meeting on May 15, 2016 in Las Vegas, Nevada.

Base Stocks for the Future First in the line of a new category of synthetic base stocks, PriolubeTM HS 1000, provides improved performance in key industry market needs without compromising other performance requirements. This new technology is targeted across many synthetic lubricant applications initially including: industrial gear oils, turbine oil, engine oils, and metalworking. To read the complete press release visit: https://www.nlgi.org/news-and-events/industry-news/

- 56 VOLUME 80, NUMBER 3

ACME-HARDESTY TO DISTRIBUTE TEMIX OLEO SPECIALTY ESTERS AND OLEOCHEMICALS IN THE UNITED STATES Agreement Further Supports Sustainable Production and Sourcing Blue Bell, Pa – Temix Oleo SRL and Acme-Hardesty, a division of Jacob Stern & Sons, have signed a letter of intent (LOI) for Acme-Hardesty to distribute Temix Oleo products in the United States.

Acme-Hardesty will promote and sell Temix Oleo specialty esters and specialty oleochemicals and derivatives in the U.S. marketplace, primarily in lubricant and personal care markets. The products will be sold under the Temest and Acitem brands. Acme-Hardesty will manage the sales, marketing and distribution of these products along with Temix pelargonic and azelaic acids. Temix is the exclusive representative for the Matrilox® brand of products manufactured by Matrica in Sardinia. To read the complete press release visit: https://www.nlgi.org/news-and-events/ industry-news/

IT’S NEW, NEW, NEW FOR STRATCO, INC.; BACKED BY 88 YRS’ EXPERIENCE & A REPUTATION FOR ENGINEERING EXPERTISE & CUSTOMER SERVICE SCOTTSDALE, AZ – STRATCO, Inc. has a lot of NEW, NEW, NEW to share as Q2 of 2016 comes to a close. We’re talking new logo, new headquarters with a new lab, and a new Grease plant using STRATCO’s process design opening in Jakarta, Indonesia…. All exciting news, backed by the same STRATCO reputation for engineering expertise and customer service people have come to expect the past 88 years. To read the complete press release visit: https://www. nlgi.org/news-and-events/industry-news/

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NLGI Industry News Lubricant Formulators Gain Versatility with new SynPrime ™ Lubricant Esters CLEVELAND – June 9, 2016 – PolyOne Corporation today announced the launch of SynPrime™ Lubricant Esters, a family of synthetic base oils and additives featuring customizable diverse chemistries for automotive, aviation and industrial lubricant applications. To read the complete press release visit: https://www.nlgi.org/news-and-events/ industry-news/

Dow Sponsors 2016 National Lubricating Grease Institute Annual Meeting Dow Performance Lubricants Showcases Revolutionary Friction Modifiers MIDLAND, MI—(June 7, 2016)—The Dow Chemical Company (NYSE: DOW) will return as a Gold Sponsor for the 2016 NLGI Annual Meeting June 11-14 in Hot Springs, VA, where industry leaders from around the country will gather to explore emerging lubrication technology. Dow will enable collaboration by sponsoring “Meeting Central” at the conference, a central space for dialogue and innovation. To read the complete press release visit: https://www.nlgi. org/news-and-events/industry-news/

Mike Ryterski (1920 – 2016) We are saddened to announce that Mike Ryterski passed away on May 29, 2016, in St. Louis at the age of 96.

Admired and respected by his co-workers, Ryterski was known for his wry sense of humor and dedication to Schaeffer Manufacturing Co. Ryterski was one of the few master blenders of lubricants in the world; his expertise was integral to the superior performance of Schaeffer’s products. His ability to formulate new products and maintain quality control enabled Schaeffer to remain at the forefront of specialized lubricant companies throughout the country.

Tom Twining June 6, 2016 - We are saddened to announce that Tom Twining, International Sales Manager for Royal Mfg Co, LP was involved in a fatal auto accident outside of Beijing during a recent trip to China to see customers and friends. Tom will be missed by his many acquaintances in the lubricants business. To read the complete announcement visit: https:// www.nlgi.org/news-and-events/industry-news/ - 58 VOLUME 80, NUMBER 3

NLGI would like to congratulate its long-standing board member, Dr. Raj Shah, for recently being elected Fellow of The Society of Tribologists and Lubrication Engineers (STLE). Dr. Shah is currently the director at Koehler Instrument company, in Holtsville, NY where he has been for over 20 years.

STLE, located in Chicago, is the premier technical society serving the needs of more than 13,000 individuals and 200 companies and organizations that comprise the tribology and lubrication engineering business sector. Since 1970, STLE has elevated less than 150 members to its Fellow grade, (< 1 % of its membership ), and an election to the Fellow grade recognizes Members who have made a significant impact on the field of tribology and lubrication engineering with accomplishments that are beyond those normally expected of the average scientist or engineer in lubrication engineering. To read the complete press release visit: https://www.nlgi.org/news-and-events/industry-news/

Advertiser’s Index Afton Chemical, page 6 Biederman Enterprises Ltd., page 4 Covenant Engineering, page 27 F&L Asia, page 7 & 55 ICIS, page 39 Lubes ‘n’ Greases, page 60 Lubrizol Corporation, back cover Patterson Industries Canada, A Division of All-Weld, Co. Ltd, page 33 Petro Lubricant Testing Lab, page 7 Royal Mfg. Co., LP, page 57 Sea-Land Chemical Company, page 5 Vanderbilt Chemicals, LLC, inside front cover

- 59 NLGI SPOKESMAN, JULY/AUGUST 2016

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- 61 NLGI SPOKESMAN, JULY/AUGUST 2016

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