September / October 2016 NLGI Spokesman

NLGI

SPOKESMAN

Serving the Grease Industry Since 1933 – VOL. 80, NO. 4, SEPT/OCT 2016

In this issue . . .

4 President’s Podium 8 83rd Annual Meeting Photos 10 83rd Annual Sports Awards 12 Blast from the Past 13 The Auburn NLGI Ralph Beard Memorial Scholarship Recipients

AND MUCH MORE!

2016 Annual Meeting Photo Issue

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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

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

Tom Schroeder Axel Americas, LLC P.O. Box 12337 Kansas City, MO 64116 Raj Shah Koehler Instrument Co. 85 Corporate Dr. Holtsville, NY 11716-1796 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

SPOKESMAN

Serving the Grease Industry Since 1933 – VOL. 80, NO. 4, SEPT/OCT 2016

4 President’s Podium 8 83rd Annual Meeting Photos 10 8 3rd Annual Sports Awards 12 Blast from the Past 13 The Auburn NLGI Ralph Beard Memorial Scholarship Recipients

14 NLGI Member Spotlight 16 Lubricating Behavior of a Superior PTFE Powder in

Lithium Grease

Mary Moon, PhD, MBA

Mike Washington The Lubrizol ­Corpo­ration 29400 ­Lakeland Blvd.

Mail Drop 051E Wickliffe, OH 44092

31 Advertiser’s Index 32 Optimizing Heat distribution in Grease Manufacturing

Ruiming “Ray” Zhang R.T. Vanderbilt Company, Inc. 30 Winfield St. Norwalk, CT 06855

Lisa Tocci Lubes ’n’ Greases 6105 Arlington Blvd., Suite G Falls Church, VA 22044

Dennis Parks Texas Refinery Corp.

One Refinery Place Ft. Worth, TX 76101

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

David Turner CITGO 1293 Eldridge Parkway Houston, TX 77077

SERVICE INDUSTRY ASSISTANCE COMMITTEE

Dr. Navendu Bhatnagar, Dr. Anoop Kumar and Bill Mallory

42 Evaluation of Boron Esters in Lithium Complex

TECHNICAL COMMITTEE

Process - A critical parameter for Quality Assurance

Greases Prepared with Hydrogenated Castor Oil Vijay Deshmukh, Bhupendra K. Rajput

50 Ask the Expert 52 Industry Calendar of Events 54 New 2016 NLGI Members 58 NLGI Industry News

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 Annual Meeting at the Homestead Resort in Hot Springs, VA

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 September 2016 David Como Dow Corning Corporation NLGI President

Hello again from high atop the podium of the NLGI. The good news is that I can see you all better from up here. The bad news is that I lost ½ inch in stature since I was last checked a couple years ago … very disconcerting, indeed. It has been a very busy and productive year for the NLGI headquarters as well as your board of directors; but how would you know if you are not updated on our progress? So I’m here to tell ya!

Those who were paying attention already know that

we were working with an outside consultant last year to breathe new life into our organizational efficacy and long-range planning. Under the guidance of Mr. Mark Levin, we revamped both our vision and our mission statements and laid the groundwork for revising our constitution and by-laws (C&BL) both for accuracy as well as for structural efficacy. Our proposal will be in the form of a revised NLGI Constitution (including the aforementioned statements) and a new NLGI Policy Manual. We hope to be able to present the results of these efforts later this year.

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-4VOLUME 80, NUMBER 4

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On the long-range planning front, we boiled down the various outputs from the board into these priority areas:

•M embership growth and outreach

•P rovide expanded educational opportunities

•E fficacy of governance and leadership for NLGI

• Basic research

•C ommunication of the value of knowledge-based resources and certification

• Global NLGI outreach Committees and sub-committees are now being organized (or re-organized) to address these areas that will include the membership. We have heard from several members who have energy

around these topics which is great to hear … so don’t be left out if you are interested in contributing! We are also actively restructuring and re-emphasizing our existing committees’ purpose and commitment. Much of our C&BL work brought some gaps to light for us here.

Most importantly, we are striving to both listen to AND ask support from the NLGI Membership. THIS MEANS YOU!!! We are always open to constructive change and are now making a point of involving non-board members in committees in order to gain your input DIRECTLY … so please don’t be shy!

Simply,

Dave Como

15 N IO IS S V R E E O X R F O S D B N E R E V A M RO GE E I S PP ER W A ND O E N L F

INTRODUCING

GEAR

RUST, DUST, DEBRIS - WHEN LUBRICANT FILM FAILS, METAL TOUCHES METAL, BEARINGS SCRATCH, GEAR TEETH SCORE AND GEARBOXES DIE. IN A WORLD WHERE INDUSTRIAL GEAR BOXES ARE INCREASING IN POWER DENSITY, PROTECTION TECHNOLOGY IS CRUCIAL FOR EXTENDING GEARBOX LIFE AND OIL DRAIN INTERVALS WHILE REDUCING OPERATING COSTS. INDUSTRIAL GEAR MICROBOTZ™ DEFEND GEARBOXES WITH A PROTECTIVE SHIELD. AND, AS OEMS INTRODUCE NEW, MORE DEMANDING SPECIFICATIONS, AFTON’S GEAR TECHNOLOGIES RISE TO THE CHALLENGE. HITEC® 307 AND HITEC® 352 PERFORMANCE ADDITIVES DELIVER EXCELLENT CLEAN GEAR PERFORMANCE; SUPERIOR COMPATIBILITY WITH PAINTS & SEALS AND OUTSTANDING BEARING WEAR PROTECTION - BUT NOW THEY HAVE ANOTHER ACCOLADE: THEY ARE BOTH SIEMENS REVISION 15 APPROVED FOR FLENDER GEARBOXES! AS THE WORKING ENVIRONMENT GETS TOUGHER, THE INDUSTRIAL MICROBOTZ™ GEAR UP FOR PROTECTION

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© 2016. Afton Chemical Corporation is a wholly owned subsidiary of NewMarket Corporation (NYSE:NEU).

AFTON®, HiTEC®, MicrobotzTM and Passion for Solutions® are trademarks owned by Afton Chemical Corporation.

Passion for Solutions® is a registered trademark in the United States.

Autumn Events November 2016 Amsterdam

Grease Training Course 8th-9th November 2016 Base Oils Thickeners Production Additives Compliance Testing Application Food Trends

Working Group Meetings 7th November 2016 Food Grade Lubricants Grease Particle Evaluation Test Methods Bio-base Grease Railway Lubricants ICIS Industrial Lubricants Conference 9th-10th November 2016

ELGI, Hemonylaan 26, 1074 BJ Amsterdam, Netherlands Telephone: +31 20 67 16 162 Email: carol@elgi.demon.nl

Online: www.elgi.org

83rd Annual Meeting Photos

Homestead Resort Hot Springs, Va

ception

Sat

g Re n i n e v E y urda

First Time Attendee Reception

-8VOLUME 80, NUMBER 4

Table Top Display

Graham Gow Keynote Speaker

vaganza ght Extra

Ni Tuesday

Tuesday Night Extravaganza mo Abe Lincoln & Mercedes Co

- Choir

Tuesday Night Extravaganza Horse Races

Tuesday Photo b Night Extravaga ooth nza

2016 NLGI ANNUAL MEETING SPORTS AWARDS

Golf Tournament Award Winners

1st Place Team

2nd Place Team

3rd Place Team

4th Place Team

Closest to Pin:

Longest Drive:

Bill Dominick Alex Kocin John Lorimor Matt Hardy

Don Eggimann Kim Smallwood Courtney Scruggs Al Parrish

Ed Blank 18th Hole

Bob Reh Ed Blank Matt McGinnis Luke Bame

Rob Heverly Dennis Parks John Sander Bill Campbell

Chris Connor 3rd Hole

- 10 VOLUME 80, NUMBER 4

Fun Run Award Winners Sponsored by FMC

Male Fun Run Winners 1st Place 2nd Place 3rd Place

Mark Nyholm, Amsoil Asif Aleem, ExxonMobil Chemical Vincent Vasely, Vanderbilt Chemicals

Female Fun Run Winners 1st Place 2nd Place 3rd Place

Andrea Sander, Lubrication Engineers Christine Karako, NCH Corporation Annie Jarquin, Kline

- 11 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

A BLAST FROM THE PAST CHARLES OSGOOD

HAROLD “HANK” H. SCHREIMANN Charles Osgood was the Keynote Speaker at the 1983 NLGI 50th Annual Meeting and wrote this wonderful poem about Grease!

I am pleased to be invited here at the NLGI although frankly for the life of me I cannot figure why.

I can speak of things political, discourse on war and peace but know nothing whatsoever about lubricating grease.

Though I cover news events both in the world and in the nation, I’m abysmally untutored about grease and lubrication.

Harold “Hank” H. Schreimann, who was NLGI’s 50th President in 1983, recently sent this poem to us. Hank served during the NLGI’s 50th Anniversary and facilitated the appearance of Mr. Osgood. While he was on the board, Hank was employed

by Container Corporation of America and later had his own company with another gentleman that was named MSI Ltd. Hank is still going strong at age 93 and wanted to share this great poem with us. Our thanks and gratitude to Hank!

I know something about music you could play on your Victrola, but GREASE I have to tell you I do not know from shinola.

You’re all elegantly dressed and all your pants have fresh pressed creases; you’ve revised my total image of the world of oils and greases!

An American radio and television commentator and writer, his daily program, The Osgood File, has been broadcast on the CBS Radio Network since 1971.

Osgood has hosted the CBS News Sunday Morning television show since 1994.

On Sunday, August 28, 2016, Osgood formally announced his retirement from CBS News Sunday Morning. His final appearance as host will be Sunday, September 25, 2016.

- 12 VOLUME 80, NUMBER 4

The Auburn NLGI Ralph Beard Memorial Scholarship Recipients for the 2016-17 Academic Year Every year since 2014, NLGI has sponsored a scholarship for Auburn University’s Tribology Program. Following are the 2 students who have received our scholarship funding for the academic year 2016-2017. Until Ralph’s passing last year, the award was simply the NLGI Scholarship, however, Ralph was so active in the Auburn program and in establishing this scholarship, that the name was changed to honor him. A big thanks to our loyal members who make this scholarship possible!

On September 19, 2016, Auburn held it’s 4th Tribology and Lubrication Science Minor Symposium at Auburn University, Auburn, Al. Our thanks to John Sander of Lubrication Engineers, Inc. who attended on behalf of NLGI.

Matthew Wise Senior Major: Mechanical Engineering with a minor in Tribology Auburn, AL

Katie Bowman Sophomore Major: Pre-Mechanical Engineering with a minor in Tribology Moore, OK

NLGI MEMBER

SPOTLIGHT

Company: Texas Refinery Corp Member Category: Manufacturer Address: P O Box 711

Fort Worth, Texas 76101 Website: http://www.texasrefinery.com/

Contact Name: Dennis Parks Title: Executive Vice President Telephone: 1-800-827-0711 Email: dparks@texasrefinery.com

We hope you’ll enjoy learning more about our long-time member Texas Refinery Corp, located in Fort Worth, Texas. TRC has shown a real commitment to innovation over its many years of operation. We’re proud to feature their company in this month’s edition of the NLGI Member Spotlight.

It was the summer of 2012 when the construction of a new TRC plant was first envisioned. Now 4 years later that vision has become a reality in Mansfield, Texas. TRC has built the Nation’s newest Grease/Oil Manufacturing Plant. From the very beginning, TRC had four key goals in mind during the design phase.

The first goal was to ensure the new facility could build the Superior Quality Products to which TRC customers had come to expect since 1922.

The second goal was for TRC to design a facility with the inherent flexibility to build tomorrow’s products.

The third TRC goal was to build a facility that respected and protected

our environment by being ECO Friendly.

And, finally, the fourth goal was to build the safest facility possible so as to protect TRC employees and the surrounding community.

TRC ownership and management well understood that the decision to build a new plant would represent a massive undertaking. Much of the safety, technological and process requirements necessary to meet today’s strict Federal, State and Local code and environmental standards did not exist prior to the beginning of construction…which makes where TRC is now even more amazing.

TRC knew it would take special expertise to meet these challenges, but where does a company turn for

such expertise? Who could aid TRC and its General Contractor, Systems Integration, Inc., in designing and building such a World-Class facility?

Early in the process, it wasn’t a surprise that TRC reached out to numerous NLGI members for needed guidance.

For the design and fabrication of grease kettles, TRC called upon Patterson Industries, the premiere manufacturer of grease kettles worldwide, and a long time NLGI member.

To help TRC overcome key technical design, environmental and safety challenges, TRC sought out the services of another long-time NLGI member, Mr. Dick Burkhalter and his Company…Covenant Engineering Services, LLC.

“Few plants have had the opportunity to leap from simply a good operation to an outstanding operation. This plant has certainly met those expectations through the diligent involvement of TRC personnel, top to bottom, and all those who contributed to the design effort; truly a team effort.

Covenant Engineering Services, LLC was proud to be a part of this historic accomplishment.”

— Dick Burkhalter

COMMITTED TO THE FUTURE TRC’s commitment to the future included building an on-site laboratory to ensure that strict Quality Control standards could be maintained. Additionally, the on-site lab allows TRC’s Research & Development team the ability to work more efficiently, effectively and safely. This enables R&D personnel to spend more time developing new formulations and new products to be introduced in the future.

HI-TECH SOLUTIONS FOR TRC CUSTOMER NEEDS

There is no doubt that with a state-of-the-art facility such as this, there are tremendous efficiency and technical improvements that were intentionally considered and included into the design, engineering and construction phases of the project.

For example, an automated pigging system was installed to clear process supply lines to prevent any crosscontamination of raw materials, additives and finished product.

TRC prides itself in providing some of the cleanest products in the

industry and this same cleanliness is reflected in the working environment within the plant. To carry this one step further, TRC recognizes the value of clean products supplied to its customers and that is why a hightech filtering system was designed and installed, which filters TRC finished lube oils thru a 10-micron filter and TRC greases thru a 100-micron filter.

SAFETY

The TRC Plant was designed and constructed to meet the latest Federal, State, and Local Fire Codes. All electric motors, automation, computer, electronics and communication devices are not only energy efficient, but intrinsically safe and of explosionproof design.

Offices, laboratory, warehouse, electrical control room and hazardous

material storage areas incorporate elaborate water, foam and gas fire suppression systems for the protection and safety of assets and personnel.

UP AND RUNNING

Since mid-2015, TRC has been in full production in this model plant. On September 9, 2016 TRC proudly celebrated its 94th year of operations…and what better way to celebrate than with a Grand Opening to introduce its World-Class Lube/Oil Manufacturing Plant to the world.

The journey from dream to reality was years in the making. In the end it was well worth the blood, sweat and tears. TRC boasts a World-Class Facility that proudly represents our industry and the boldness of the American Spirit.

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

Lubricating Behavior of a Superior PTFE Powder in Lithium Grease Mary Moon, PhD, MBA

Consultant to Shamrock Technologies, Inc., Newark, NJ 07114 USA Abstract

Anti-friction and anti-wear effects of polytetrafluoroethylene (PTFE) additives in lubricating greases depend on characteristics of specific grades of PTFE powders. In a recent study, seven experimental PTFE powders were formulated and milled to prepare models of simple lithium greases. One of seven grades of PTFE gave superior performance in four-ball tests where loads up to 1 765 N (180 kgf) were applied gradually to decrease run-in effects. This grease is a good starting point for formulations with benefits from PTFE. [1-3] The present paper analyzes friction data from these experiments with simple statistics. At low applied loads (< 500-700 N or 50-70 kgf), statistics are similar for polyalphaolefin (PAO) base oil and lithium and PTFE-lithium greases. At higher loads, there are abrupt changes or spikes in friction. For PAO and some PTFElithium greases, these friction spikes are associated with lubrication failure and adhesive wear, which trigger significant increases in friction, temperature and wear scar diameter. A superior grade of PTFE provides antifriction and anti-wear protection against failure and adhesive wear in these tests, however. Analysis of friction data and wear scars indicates that this superior PTFE may be entrained in contacts (and/or at their inlets), compressed and have a resilient protective effect. Results from the literature in support of this mechanism are discussed.

modification significantly reduced run-in effects. Fourball tests with load ramps were used to measure friction, temperature and wear scars for PTFE-lithium greases, control grease (no PTFE) and base oil. [1-3] In lithium grease, one grade of PTFE was superior to the other six grades. As the applied load was increased, abrasive wear was observed at low loads until adhesive wear occurred for base oil, control grease, and six of seven PTFE-lithium greases. Adhesive wear released heat, softened or melted contact surfaces, and significantly increased wear scar diameters. For the seventh grade of PTFE, adhesive wear did not occur as the load was increased to 1 765 N (180 kgf), the limit of the test machine. As a result, friction and temperature were lower and wear scars were smaller, than for other cases where adhesive wear occurred. This superior model PTFE-lithium grease is a good starting point for formulation studies. It could be enhanced with other additives such as anti-oxidants. [1-3] The present paper addresses several intriguing questions associated with lubricating behavior of this superior grade of PTFE. Are results for this PTFE powder anomalous, or are they reasonable in the context of results for other greases and PAO base oil? What are some similarities and differences for lubrication with PAO base oil, control lithium grease and PTFE greases?

Is there a possible explanation for effects of superior PTFE on lubrication? Do results from the literature support these findings?

Introduction

Background about PTFE

Previous papers discussed the use of polytetrafluoroethylene (PTFE) as an anti-friction and anti-wear additive, grease formulation guidelines, and a modified four-ball test for friction and wear. Greases were prepared from PTFE, lithium thickener and PAO base oil. Standard four-ball friction and wear tests were performed to evaluate the performance of seven grades of PTFE in greases. However, run-in effects interfered with this comparison. A standard test procedure was modified by gradually applying the load in a ramp. This

Polytetrafluoroethylene or PTFE is a synthetic fluoropolymer of tetrafluoroethylene (-CF2- CF2-)n that resembles ethylene (-CH2-CH2-)n but with fluorine instead of hydrogen atoms. High molecular weight PTFE is a thermoplastic solid that can be ground into powders and dispersed in oil or water. The surface of PTFE is extremely slippery with coefficients of friction, COF, between 0.04 (sliding friction) and 0.1 (ASTM D1894).

Other useful properties include resistance to chemicals, solvents and temperature extremes (highs and lows). [4]

- 16 VOLUME 80, NUMBER 4

However, effects of PTFE powders depend upon their dispersion in lubes and greases, particle size and shape and surface polarity as well as test conditions (geometry of the contact, roll-to-slide ratio, speed, load, viscosity, etc.) [5-7]

Grease Formulation Strategy

Thus, it makes sense to first compare grades of PTFE in simple model formulations to identify the PTFE powder with the best inherent properties as a lube additive. Formulating grease from only PTFE, thickener and base oil avoids possible interference from interactions between other lubricant additives and PTFE, grease fibers and contact surfaces. The best grade of PTFE can be developed, and greases can be formulated with it.

For PTFE, this approach can be more efficient than trial-and-error using more complex formulations.

Seven experimental grades of PTFE were compared in simple model greases made ‘from scratch’.

Greases were prepared by mixing and heating 4 wt.% PTFE and 8 wt.% preformed lithium 12-hydroxy stearate (Li12OHSt) thickener powder in PAO base oil (25-35 cSt at 40°C) until the soap melted, the mixture thickened, and the soap recrystallized. PTFE- Li12OHSt greases and Li12OHSt control grease (12 wt.% Li12OHSt in PAO) were off- white, smooth, buttery and NLGI grade 2. PTFE-Li12OHSt greases were slightly softer than Li12OHSt greases, and storage stability was similar for all greases.

[2] Each batch was milled with a pilotscale high-pressure homogenizer, which provided a consistent

method for forming grease fibers similar to grease manufacturing.

In this study, three PTFE powders were ‘sub-micron’ with average primary particle diameter < 1 μ, and four PTFE powders had average diameters > 1 μ. Milling ensured that grease fibers formed around well-dispersed PTFE particles. In the literature, electron micrographs show grease fibers (and gaps between fibers) from approximately 0.1 to 10 μ. [8] When nanoparticles (at least one dimension <0.1 μ) were mixed (not milled) in lithium grease, particles were not dispersed among grease fibers, Fig. 2 in [9].

Four-Ball Test Strategy

Greases were evaluated with a commercial four-ball wear machine and ASTM D2266 Standard Test Method for Wear Preventive Characteristics of Lubricating Grease in a laboratory maintained at 21-23°C. [10] Wear scars were measured and photographed with commercial light microscopes and cameras. [2] A test was stopped if welding occurred or friction approached the upper limit of the load cell (1 765 N or 180 kgf). [2] When Li12OHSt and PTFELi12OHSt greases were tested with D2266, friction spiked at the start of each test and then fluctuated. [2] Wear during run-in could produce wear particles; these particles could entrain in contacts, cause three-body wear, create more particles, and affect test results. [11] Thus, a fourball procedure with smaller run-in effects was developed.

In practice, D2266 is applied to evaluate fully-formulated lubricants relative to specifications for qualification and quality control

purposes. Grease is heated to 75°C and tested under an applied load of 392 N (40 kgf) at 20 Hz (1 200 rpm) for 60 min. However, the D2266 procedure was too severe for these simple model greases.

This procedure was modified by gradually applying the load in a ramp of increments of 29.4 N/ min (3 kgf/min) from 29 to 1 765 N (3 to 180 kgf). Grease was not pre-heated. Ramping up the load corresponded to progressing to the left on Stribeck’s curve in mixed and, possibly, boundary lubrication regimes. This is similar to progressive loading during breakin, which prolongs service life of machinery [12] and may enhance oil bleed from grease [13].

Modifying D2266 with a load ramp made it possible to evaluate these simple model greases.

This modified four-ball test provides an additional benefit: friction and temperature can be observed as the load is increased. In this study, friction and wear were measured at 2 s intervals (0.5 Hz) or 0.05 s intervals (20 Hz). Significant differences were observed in friction and temperature data for PAO, control grease and various PTFELi12OHSt greases.

Four-Ball Results

Experiments with this modified four-ball procedure differentiated between PTFE-Li12OH greases, Li12OHSt control grease and PAO base oil. Figure 1 shows data for PAO from a test where the applied load was ramped up from 29 to 1 765 N in increments of 29 N/min (from 3 to 180 kgf in increments of 3 kgf /min), maintained for

- 17 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

15 min, and ramped down. Friction and temperature initially increased steadily with applied load. [2] When the load was 753 N (75 kgf), friction spiked sharply for approximately 1 min. [2] Afterward, friction more than doubled (from 2 to 4 – 5 N) and temperature shifted higher by approximately 10°C, Fig. 2.

Failure was mechanical, not chemical (oxidation), and associated with adhesive wear. [2] Adhesive wear released heat, softened or melted contact surfaces and increased wear scar diameters. [2] After the test, oil was black due to suspended wear particles (< 0.1 mm), and larger particles (0.1 - 1 mm) were visible in the bottom of the cup. [2] The best PTFE-Li12OHSt grease was a significantly better lubricant than PAO. In Fig. 3, friction spiked at loads of 677 N (69 kgf, 23 min), 794 N (81 kgf, 27 min), several times above 1 030 N (105 kgf, 35 min) on the ‘up’ ramp and once on the ‘down’ ramp. Spikes were 1 min or less in duration. Lubrication failure and adhesive wear were not observed.

After friction spiked for the best PTFE-Li12OHSt grease, friction recovered almost entirely and temperature shifted slightly or not at all, Fig. 4.

Maximum temperature (65°C) was less than half that observed for PAO (150°C) during similar tests, Fig. 1. Only slight discoloration of grease and few wear particles were observed after these tests.

Although friction spiked, this grease prevented most of the damage and heat accumulation observed for PAO. Friction data suggests that grease solids contributed to lubrication. At low loads, friction fluctuations resembled those for PAO, Fig. 2. After the first spike (23 min, 677 N, 69 kgf), friction fluctuations appeared more regular with larger amplitude and higher frequency.

These changes indicated a somewhat more resilient response to the load. An opposite pattern was observed on the ‘down’ load ramp. These observations suggested that grease solids entrained in contacts and respond to applied loads in a more resilient manner than metal surfaces. While asperity contacts or stress concentrations may initiate friction spikes, these entrained solids prevented development of adhesive wear.

Data from another experiment (below) are shown in

Figs. 5 and 6. Friction data were comparable at low loads for PAO, Li12OHSt grease and this PTFE-Li12OHSt grease. Load and number, shape and effects (temperature, friction) of spikes were similar for PAO, Li12OHSt grease and this PTFE-Li12OHSt grease – but not the best PTFELi12OHSt grease.

The best PTFE-Li12OHSt grease was unique: friction spikes were more numerous and briefer in duration (narrower), and effects on friction and temperature were smaller than for Li12OHSt grease and other PTFE-Li12OHSt greases. However, data for the best PTFE- Li12OHSt grease were not anomalous; friction at low loads and onset of spikes at higher loads were comparable to those for PAO, control grease and other PTFE-Li12OHSt greases.

Thus, results for the best PTFE-Li12OHSt grease are associated with the specific PTFE powder used to formulate this grease. This superior grade of PTFE is submicron with average particle diameter < 1 μ. A statistical data analysis was performed to gain additional insight about effects of this superior grade of PTFE on grease lubrication.

Fig. 1 Friction (black) and temperature (red) data for PAO. The blue line represents the applied load (N)/100, which was ramped up from 30 to 1 765 N in increments of 29.4 N/min (from 3 to 180 kgf in increments of 3 kgf / min), maintained for 15 min, and ramped down.

Data were collected at intervals of 2 s (0.5 Hz).

- 18 VOLUME 80, NUMBER 4

Fig. 2 Friction (black) and temperature (red) data for PAO, Fig. 1.

After the friction spike, friction more than doubled and temperature shifted higher by approximately 10°C (arrow).

Fig. 3 Friction (green) and temperature (red) data for the best PTFE-Li12OHSt grease as the load was ramped up 0.3 to 1 471 N in increments of 0.3 N/min (from 3 to 150 kgf in increments of 3 kgf /min) and ramped down. The scale of the vertical axis is smaller than Fig. 1.

Data were collected at intervals of 2 s (0.5 Hz).

Fig. 4 Friction (green) and temperature (red) data for the best PTFE-Li12OHSt grease from Fig. 3.

The scale of this vertical axis of this figure is the same as Fig. 2 for PAO. Data were collected at intervals of 2 s (0.5 Hz).

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Fig. 5 Friction data (N) for PAO, Li12OHSt control grease and PTFE-Li12OHSt greases.

Fig. 6 Temperature data (°C) for PAO, Li12OHSt control grease and PTFE-Li12OHSt greases.

Statistical Analysis of Four-Ball Data

Friction and wear are statistical in nature; asperity size, wear, fatigue, grease and bearing lifetimes and so forth are described by distributions (statistical) and not fixed values. [13] Thus, it is reasonable to apply a statistical approach to examine friction data and characterize effects of PTFE powders on grease lubrication, Table 1. Statistics were calculated from 30 (or 1 200) data points collected during 1 minute at each load.

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Table 1 Statistics calculated from friction data points (x1, x2, x3, …, xn) where n=30 or n=1 200. For random data points with a normal (bell-curve) distribution, |Skew| < 0.18 and |Kurt| < 0.69 when n=30, and |Skew| < 0.005 and |Kurt| < 0.020 when n= 1 200. [14] Distributions may be non-normal when sources of data are biased and/or auto-correlated (memory effects).

Statistics for PAO friction data (Fig. 1) are shown in Fig. 7. The mean (X) clearly shifts upward after the friction spike. The ratio of standard deviation to mean (s/X) decreases during run-in and formation of grooves in contacts. The ratio s/X decreases again when X increases after the friction spike. Skew and Kurt are larger than typical for random data (|Skew| < 0.18 and |Kurt| < 0.69 for n=30 data with a normal distribution or ‘bell curve’).

There is no obvious feature in data at low loads that precedes the friction spike at 753 N (75 kgf).

However, number of data points at each load (30), frequency of data collection (0.5 Hz), number of contacts (3) and load cell sensitivity may limit these particular results.

Friction statistics for the best PTFE-Li12OHSt grease (Fig. 3) are compared with PAO in Fig. 8. This PAO test was stopped before adhesive wear occurred; wear scars showed abrasive wear. [2] For the best grease, X was very similar to PAO below 650 N (66 kgf), i.e., abrasive wear. At higher loads, X shifted due to friction spikes unrelated to adhesive wear (Fig. 1) and possibly because grease solids were entrained and compressed.

The ratio s/X reflected larger fluctuations in friction for the best grease than PAO as in Fig. 4. As the load was increased above 300 N, s/X tended to increase for grease but not PAO. These results suggest that additional solids are entrained and compressed as the load was increased.

Skew and Kurt for this grease varied less than for than PAO. Entrained solids (and fewer wear particles) possibly resulted in more stable lubrication and friction for grease than PAO.

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Fig. 7 Statistics calculated from friction data for PAO (Figs. 1 and 2). Friction spiked when the load was 753 N (75 kgf), yellow fill.

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Fig. 8 Statistics calculated from friction data for the best PTFE-Li12OHSt grease (Figs. 3 and 4), green. Statistics from another PAO test (data not shown), which was stopped before adhesive wear occurred, are shown in black.

[2] Figure 9 compares X calculated from friction data for several greases and PAO (Fig. 5 and below). At loads below 500 N (51 kgf), X was similar for greases and PAO. At higher loads, friction spikes were brief in duration and had small effects on X for the best PTFE-Li12OHSt grease (Fig. 5). Instead of failure, lubrication recovered after friction spikes, which was consistent with entrainment and compression of grease solids instead of adhesive wear.

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In-depth Statistical Analysis of Four-Ball Data

For a more in-depth analysis of lubrication behavior, the load was increased in increments of 0.3 N/min until lubrication failed and then maintained. Data were measured before, during and after lubrication failure. At each load, 1 200 data points were collected at intervals of 0.05 s, equal to the frequency of rotation of one bearing on three fixed bearings (20 Hz). Each data point corresponded to one complete rotation of the top ball instead of an average over multiple rotations.

In Fig. 10, friction data for PAO were collected by increasing the load until lubrication failed at 677 N and then maintaining the load at 677 N. Statistics in Fig. 11 showed that X and s increased steadily with load until failure.

The ratio s/X was relatively steady, consistent with increasing asperity interactions proportional to load. Skew and Kurt were more stable than in Figs. 7 and 8 and showed that friction fluctuations were not random. Instead, these friction fluctuations were probably biased and/or auto-correlated for reasons such as mechanisms of wear and lubrication, effects of grooves in contact surfaces and so forth.

Figure 12 is a bar chart that compares statistics at 677 N before, during and after lubrication failure at the same load. There were significant differences in friction during abrasive (blue) and adhesive wear (orange). After adhesive wear (green), friction recovered partially due to damage to contact surfaces and, possibly, presence of wear particles in lubricant and contacts.

Fig. 10 These friction data for PAO were collected by increasing the load from 29.4 N in increments of 29.4 N/ min until lubrication failed at 677 N. The load was maintained at 677 N and data were collected during and after failure. Data were measured at intervals of 0.05 s, which is the same frequency as the rotation of one bearing on three fixed bearings (20 Hz).

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Fig. 11 Statistics calculated from friction data in Fig. 10 prior to lubrication failure.

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Fig. 12 Statistics calculated from friction data before, during and after lubrication failure of PAO at an applied load of 677 N.

In Fig. 13, friction data for the best PTFE-Li12OHSt grease were collected by increasing the load from 29.4 to 1 353 N in increments of 29.4 N/min.

This load was maintained while friction spiked briefly at 632 and 971 N.

Figure 14 showed that X increased steadily with load before and after friction spikes. The ratio s/X decreased more strongly than for PAO as the load was increased to 400 N, possibly because grease solids were compressed.

Skew and Kurt increased only during friction spikes.

Fig. 14 Statistics calculated from friction data for the best PTFE-Li12OHSt grease in Fig. 13.

For the best PTFE-Li12OHSt grease, friction spikes briefly interrupted lubrication. In contrast, for PAO, friction spikes corresponded to distinct changes in lubrication. In the case of the best PTFE-Li12OHSt grease, friction spiked due to entrained solids not adhesive wear.

Lubrication failure was observed for a different PTFELi12OHSt grease (applied load 927 N) and control Li12OHSt grease (500 N), Fig. 9. Statistics were calculated from friction data before, during and after lubrication failure of these two greases, Figs. 15 and 16. This PTFE powder provided a modest advantage in that failure occurred at a higher load (927 N) than for control grease (500 N). However, statistics suggested that lubricant failure was similar for both greases and PAO and related to adhesive wear. After failure, friction recovered only somewhat due to damage to contacts and wear particles.

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Fig. 15 Statistics calculated from friction data before, during and after lubrication failure of a PTFE-Li12OHSt control grease at an applied load of 927 N.

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Fig. 16 Statistics calculated from friction data before, during and after lubrication failure of Li12OHSt control grease at an applied load of 500 N.

Wear Scars

A typical wear scar from the best PTFE-Li12OHSt grease is shown in Fig. 17. Scars were oval, elongated perpendicular to direction of sliding, while scars from tests with PAO and other greases were round. In Fig. 17, the average wear scar diameter was 1.41 mm, and 0.93 and 1.89 mm parallel and perpendicular to the direction of sliding, respectively.

Parallel to sliding, this diameter was similar to scars from abrasive wear for PAO. [2] Perpendicular to sliding, stresses in contacts affected scar shape. Along inlets and outlets of contacts, scar edges were irregular. Similar irregular edges were observed for round scars from PAO tests that were stopped immediately after adhesive wear started. (Scar edges were relatively smooth and regular for PAO tests with no adhesive wear.) [2] However, no softening or melting of metal was present on the wear scar. (Likewise, there was no evidence for adhesive wear in friction and temperature data for the best PTFE-Li12OHSt grease.)

Thus, this superior grade of PTFE provided anti-wear as well as anti-friction benefits in simple lithium grease.

The appearance of wear scars was consistent with the proposed mechanism that grease solids were entrained and compressed in contacts, giving rise to brief friction spikes but preventing adhesive wear.

Fig. 9 Enlarged photograph of a magnified (5x) wear scar for the best PTFELi12OHSt grease (Figs. 3 and 4). [2]

Anti-friction and anti-wear mechanism of a superior sub-micron PTFE powder

In general, adhesive wear is initiated by localized direct metal-to-metal contact between asperities on two surfaces in relative motion. Adsorbed molecular layers of sacrificial anti- wear additives and lubricating oil films can prevent asperity contacts and adhesive wear.

However, friction can remove adsorbed anti-wear additives, and asperities can penetrate oil films, triggering adhesive wear. The present study did not include a chemical analysis of scar scars, and there was no information about the possible presence of PTFE on contact surfaces.

In this study, four-ball data and wear scars suggested that the best lubrication behavior was obtained with a superior PTFE powder that was entrained and compressed in contacts during these tests. There is some evidence in the literature that supports this interpretation.

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Several authors reported observations of PTFE in liquid lubricants undergoing elastohydrodynamic lubrication (EHL). Palios et al., Wan et al. and Jia et al. observed individual PTFE particles in contacts during EHL that helped support applied loads. Lubricating effects and mechanisms of PTFE depended on particle properties (size, shape, surface polarity, etc.), dispersion and test conditions (contact geometry, roll-to-slide ratio, speed, load, etc.) [5-7] A fluid dynamics model for mixed EHL was developed

by Ishimaru et al. Their calculations showed that details of asperity size, shape and location relative to a Hertzian contact can detract from or enhance oil flow through surface grooves and film thickness in rolling- sliding and pure rolling contacts. [15] Their findings imply that PTFE particles at surfaces of inlets and contacts could affect lubrication as observed in the present study.

Electron photomicrographs from the literature show inorganic nanoparticles inside grooves in wear scars generated by tribotests. [8] In this study, it is possible that some PTFE particles likewise accumulated in grooves and inlets of wear scars, preventing adhesive wear.

The best PTFE-Li12OHSt grease in this study is a useful starting point formulation for the development of greases with good anti-friction and anti-wear performance.

Conclusions

1. A superior sub-micron PTFE powder provided antifriction and anti-wear effects when formulated and milled in simple lithium greases and tested at applied loads up to 1 765 N (180 kgf) in four-ball tests with load ramps. This model grease is a useful starting point for developing formulations with anti-friction and anti-wear benefits from PTFE. 2. Friction data, statistics and the appearance of wear scars indicated that this superior PTFE was entrained in contacts or their inlets and compressed. This lubrication mechanism is feasible in the context of results in the literature for PTFE and other types of particles.

3. In these tests, friction data were similar at low loads (< 500 N) for PTFE-lithium greases, lithium control grease and PAO base oil. At higher loads, there were abrupt changes or spikes in friction. For PAO and some greases, these spikes were associated with adhesive wear and increases in friction, temperature and wear scar diameters. For a superior PTFE powder, friction spikes were harmless because this PTFE prevented lubrication failure in these tests.

4. Preparing and milling individual batches of PTFElithium greases ensured consistent dispersion of particles among grease fibers as in commercial manufacturing. Four-ball friction and wear tests with load ramps provided useful information about PTFE additives and avoided interference from runin effects and other chemical additives. Statistical analysis provided useful insights about grease lubrication performance.

Acknowledgements

The author gratefully acknowledges Shamrock Technologies, Inc. for support of this experimental project and permission to present this paper at the NLGI 82nd Annual Meeting, Coeur dâ&#x20AC;&#x2122; Alene, ID USA, June 6-9, 2015.

References

1. M. Moon, A Superior PTFE Powder for Grease, Extended Abstract, Society of Tribologists and Lubrication Engineers, National Meeting, Dallas, TX, May 21, 2015.

2. M. Moon, PTFE for Lubricating Greases, Paper #1408, National Lubricating Grease Institute Annual Meeting, Palm Beach Gardens, FL, June 17, 2014, accepted for publication in The Spokesman, 2015.

3. M. Moon, PTFE for Lubricating Greases, Extended Abstract, Society of Tribologists and Lubrication Engineers National Meeting, Orlando, FL, May 20, 2014.

4. L.R. Rudnick, Ed., Lubricant Additives: Chemistry and Applications, Second edition, CRC Press, Taylor and Francis Group, Boca Raton, FL, USA, p 181-2.

5. S. Palios, P.M. Cann and H.A. Spikes, Behavior of PTFE in Rolling/Sliding Contacts, The Third Body Concept, D. Dowson et al., Editors, Elsevier Science , B.V.1996.

6. G.T.Y. Wan and H.A. Spikes, The Behavior of Suspended Solid Particles in Rolling/Sliding Elastohydrodynamic Contacts, STLE Transactions, 31, pp. 12-24, 1987.

7. Z. Jia and Y. Tang, Composites Part B: Engineering, Vol 43, Issue 4, June 2012, pp. 2072-2078.

8. NLGI, Lubricating Grease Guide, Fourth, Fifth and Sixth Editions, National Lubricating Grease Institute, Leeâ&#x20AC;&#x2122;s Summit, MO, USA, 1996, 2009 and 2015.

9. L. Rapoport, N. Fleischer and R. Tenne, FullereneLike WS2 Nanoparticles: Superior Lubricants for Harsh Conditions, Advanced Materials 15:7-8, 61-65, 2003.

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10. A STM D2266 Standard Test Method for Wear Preventive Characteristics of Lubricating Grease (Four-Ball Method), ASTM International, West Conshohocken, PA, USA. 11. M .Moon, Taking Lubricant Cleanliness to the Next Level, Gear Solutions Magazine, June, 2009.

12. K .C. Ludema, Friction, Wear, Lubrication, A Textbook in Tribology, CRC Press, 1996.

13. P .M. Lugt, Grease Lubrication in Rolling Bearings, John Wiley & Sons Ltd, West Sussex, UK, 2013..

14. W ikipedia, May 28, 2015.

15. K .Ichimaru and T. Morita, A Deterministic Model of Mixed EHL in Line Contact Considering the Three-Dimensional Surface Roughness, Transient Processes in Tribology, G.Dolmas, et al. Editors, Elseview B.V., 2004, pp. 225-233.

Advertiser’s Index Afton Chemical, page 6 Biederman Enterprises Ltd., page 4 Covenant Engineering, page 13 ELGI, page 7 F&L Asia, page 49 Lubes ‘n’ Greases, page 61 Lubrizol Corporation, back cover Patterson Industries Canada, A Division of All-Weld, Co. Ltd, page 5 Vanderbilt Chemicals, LLC, inside front cover

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Optimizing Heat distribution in Grease Manufacturing Process A critical parameter for Quality Assurance Dr. Navendu Bhatnagar, Dr. Anoop Kumar and Bill Mallory Royal Mfg. Co. LP

Abstract

Lubricating greases are NonNewtonian fluids and nonconducting in nature which makes manufacturing of lubricating greases a complex process. As lubricating greases predominantly consists of base oil (75-85 %), thickener (1015 %) and balance additives, high temperatures adversely affect the quality of grease resulting in rapid thermal oxidation or carbonization though dependent upon mixing profile. Due to semi-solid nature of lubricating greases results in slow dissipation of heat compared to that in case of lubricating oils. This fact holds importance in the grease manufacturing process where large quantities of grease ( 5000-20000 lbs ) is heated by circulating thermic fluids at temperatures ranging from 400 °F – 480 °F [204°C – 249°C].

Imparting desired quality and performance characteristics to the grease product depends on ensuring proper control of the heat transfer from thermal exchange systems in a manner that temperatures stay well within the defined range as per the formulation process. A thermal

shock can occur if temperature at the heat source is not regulated properly or reacting mass is not mixing in proper fashion resulting in adverse effects on grease quality.

Proper control of heat during exothermic/endothermic reactions is needed to maintain the reaction kinetics.

This paper will focus on understanding the factors (such as mixing profiles) that affect the heat transfer in grease manufacturing process. Role of Heat transfer coefficients will be discussed from a commercial industry standpoint.

Comparison in heat transfer profiles for different greases (for example lithium based vs. calcium sulfonate) will also be studied and analyzed. Another aspect that will be studied is the difference in heating profiles between a contactor and an open kettle cook. The conclusion of this paper will focus on identifying proper methods for ensuring uniform and controlled heat distribution during the grease manufacturing process.

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INTRODUCTION

Lubricating grease has been defined in ASTM terms as dispersion of thickening agent in a liquid lubricant where the dispersion is a solid to semi-fluid product.

Three basic components that form are oil, thickener and various additives as required [1, 2].

Over the years, a prominent debate has been the choice of oil or grease for lubrication purposes. Strong points for grease include better start-stop performance, ability to stick to the surface offering better retain characteristics, application as a sealant thereby serving as a protective coating and ability to disperse solid additives that may impart certain unique properties in operation. With such strong attributes on offer, it is imperative that manufactured grease must be high on quality standards and should be able to deliver the promises that are expected theoretically in a particular application.

Grease manufacturing however, is not a simple process, when compared to the case of lubricating

oils which involves mixing the different base oils and liquid additives for small period of time at room or slightly elevated temperatures. One of the main challenges for grease is the presence of different phases [3, 4] during the manufacture process which starts in a liquid phase but transforms into a semi-liquid to a semisolid phase during the course of chemical reaction and addition of additives, in many cases. This multi-phase operation requires a significantly more robust control of parameters to achieve a better quality product.

Scale-up of grease manufacturing process from lab to commercial level is challenging and requires a careful consideration of factors that can significantly affect the replication of product quality achieved at small scale [5].

Some of the notable factors are, a) Temperature control – Saponification reaction, like other reactions is known to accelerate with the rise in temperature [6]. However, there is no linear relationship between the kinetics and heat supplied. b) Mixing profiles – Even though a single uniform mixing profile can be employed for both reaction and finishing stages, mostly it is beneficial to provide a two stage mixing for process optimization. c) Exposure to open environment – Whether or not the saponification reaction is carried out under pressure changes the reactions times as well as grease formulations which plays an important role in commercial grease manufacture process.

Manufacturing can be performed in a batch or a continuous manner, however a batch process is the more popular one as it provides more flexibility in grease cooking and finishing compared to the continuous operation. Batch process may employ an open kettle cook where grease is manufactured at atmospheric pressure and complete process is finished in one kettle in contrast to closed kettle cook where saponification reaction is carried out under pressure in a contactor followed by finishing in a second kettle [6].

Main focus of this study is to understand the parameters and factors that play an important part in temperature control during the grease manufacturing process. Base oils are known to get oxidized at elevated temperatures and since they volumetrically contribute 75 – 85 % in grease formation, pose a danger of causing thermal oxidation of grease at temperatures above the recommended range. This oxidation results in darkening of grease and generation of unwanted oxidation products

which may have an adverse effect on the thickener causing softening, oil bleeding followed by leakage when exposed to certain applications. Also, chain oxidation causes carbonization which results in crust formations.

All these unwanted occurrences can be reduced or even eliminated by marking a better control on heat transfer to and from the reaction mixture and final grease product.

Overall Heat Transfer Coefficient (U)

One of the parameters that is used to study and measure the efficacy of heat transfer is the overall heat transfer coefficient which is defined as the ability of a certain medium or series of mediums to conduct heat.

The rate with which heat is removed or transferred from the surface can be defined by the following equation [8],

where Q is the heat removal rate, U is the overall heat transfer coefficient, A is the surface area of heat transfer and ΔT is the difference in temperature of solid surface and fluid in contact.

For systems involving coils or jackets, overall heat transfer coefficient can be calculated using the standard equation [8],

where α and αs are the process and service side heat transfer coefficients and 1/αF is the service side fouling resistance.

A higher overall heat transfer coefficient is an indication of better heat conduction through the material which is desirable. For grease manufacture, the cooking kettles and jackets are generally constructed from carbon steel or stainless steel material. This brings the typical value of ‘U’ equal to 400 W/m2-K (70.45 BTU/hr.ft2.°F) when heating the product [8]. In some cases cast iron may also be used. U can be calculated for a specific case by getting process and service side heat transfer coefficients using the equations between Nusselt and Reynolds number. This parameter cannot be varied on a daily basis and holds importance only when designing or modifying a grease manufacturing unit.

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FACTORS CONTRIBUTING TO HEAT TRANSFER CONTROL

a) b) c) d) e) f) g)

Oxidation occurs when HT oil comes in contact with air at high temperatures (>200°F [93°C]) resulting in formation of sludge that eventually deposits in the hot oil circuit thereby reducing the heat transfer efficiency.

Thermal degradation of petroleum based fluids refers to the breakage of carbon-carbon bonds when exposed to temperatures in excess of recommended bulk operation temperature of oil. This increases the acid number of the oil resulting in slow corrosion of hot oil circuit. This results in chipping of solid wall material in contact with hot oil which may deposit on the heat transfer surface adversely affecting the heat transfer efficiency.

Type of heat transfer fluid.

Method of heat transfer Flow rate.

Distance from heat source.

Mixing profiles and efficiency.

Properties of reaction fluid Heat losses

Type of Heat Transfer medium

Old techniques employed exposing the grease kettle to a direct fire where a flame would be in touch with the outside kettle wall. This approach had obvious disadvantages as temperature control was a big concern and due to lack of surface area, heating times were increased. If mixing was not fast and effective, this type of heating could lead to burning or scorching of final product [7]. Also, direct fire increases the fire hazard, especially when dealing with oils of low volatility and flash points. Added precautions and considerations are required in plant designing when installing direct fire equipment [6]. Modern grease kettles are built with jackets where a heat transfer (HT) fluid is circulated to heat the reaction mixture. For low temperature cooking where reaction mixtures are to be heated up to 150 deg C, steam is a viable option. High pressure steam (operating @ 100-150 psi) can attain such temperature range. However, recent advances in grease formulations have enabled the manufacturers to make better quality greases if cooked at higher temperatures in the range of 380-410 deg F which cannot be provided by steam. One of the most common heat transfer fluids used in the current grease manufacturing industry is heat transfer oil. The formulation can be Group I or Group II oil based with either a naphthenic or paraffinic content in it depending on the application. These oils can provide working temperatures in the range of 100-600°F. However, since source is set at high temperature, better control of heat transfer is required. If not controlled properly, this can cause the temperatures to go out of the recommended range and affect grease in an adverse manner. Also, heat losses to the environment can lower the efficiency of the heat transfer if proper measure are not followed. These include insulation of transfer lines, kettle jackets and minimum distance between the source and kettle. Another factor to consider is the thermal degradation and oxidation of heat transfer (HT) oil.

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Method of heat transfer

Heat transfer in agitated vessels is carried out using the external jackets or internal coils or a combination of both [8]. External jackets can be conventional in design using spiral baffles welded to the wall of kettle or it can be dimpled jacket. In some cases, a half pipe (limpet coils) jacket can also be used but with a disadvantage that it covers less surface area and requires a higher extent of welding which may cause mechanical stability concerns when thermal shocks are encountered [9].

Figure 1[8]: External jackets; (a) spiral baffle, (b) dimpled, (c) half-pipe In addition to external jackets, certain agitated kettles also employ internal coils which may be fully helical in shape or a series of smaller ringlet coils.

VOLUME 80, NUMBER 4

Figure 2[8]: Internal coil jackets; (a) Full helical, (b) ringlet coils As it is evident, full helical coil offers an advantage of providing more surface area than the ringlet coils but requires the kettle body to be two-piece increasing the overall initial cost of fabrication. Ringlet coils can be inserted in a single piece vessel but may generate temperature gradient in the reaction mixture if mixing is not sufficient. In context to grease manufacturing, a conventional style spiral baffle jacket is more advantageous than other external jackets as it offers a higher surface area for heat transfer. This however is true when considering the open kettle cooks. One of the foremost innovations in grease manufacturing has been the advent of contactor [10] reactor which allows reactions to take place in closed, highly pressurized environments thereby increasing the kinetics of reactions by a multifold. This unit employs an internal double walled circulation tube which is an extension of a full helical coil in conjunction with an external heating jacket. This increases the heat transfer surface area almost by a factor of three when compared to an external jacket open kettle as shown in Figure 3.

Figure 3: Kettle TOP view; (a) External jacket only, (b) External jacket + internal coils To summarize, a combination of external jacket system and internal coil network should be utilized to achieve a higher degree of heat transfer in grease manufacturing processes. Rate of heat transfer from the heating medium to reaction fluid depends on various factors such as type of heat transfer fluid, impeller speed, vessel geometry, area of heat transfer and also the temperature difference between the source and reaction fluid. This relationship is mathematically expressed as [8], Where q is the rate of heat transfer, U is the overall heat transfer coefficient, A is the area of transfer and TH / TF are temperatures of heating fluid and reaction mixture respectively.

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Energy balance involved in this step can be expressed as follows, where qin is the heat input to the system, qout is the heat released from the system and qloss is the heat loss from the system.For simplification purposes considering the case of transient heat transfer in a batch manufacturing process with good insulation and minimal losses the above equation can be expressed as [11],

where mw is weight of mixture and C is the specific heat.

This equation is integrated to yield,

This equation provides a simplified method to estimate the overall heat transfer coefficients for a batch process.

However, other factors such as mixing profiles (Reynolds number, Prandtl number) need to be considered for a more realistic depiction which is out of scope for this current study. Authors studied the temperature profile of grease mixture cooked in an open kettle and also in the contactor. Grease in contactor was lithium based and sodium based in the open kettle. Greases were of similar NLGI grade to avoid the effect of thickness on recorded data. Heating was started from same temperature and was continued till the desired temperature was achieved.

Heat transfer fluid flow rate was also maintained at an equal level between the open kettle and contactor to achieve comparable conditions. Source temperature was maintained at 410°F [210°C].

Figure 4: Comparing heating profile for grease cooked in (a) contactor vs. (b) open kettle As can be observed in the above figure, contactor unit utilizing an open jacket in conjunction with a closed internal coil network takes approximately two to three hours less than an open kettle (with just one external jacket) to heat up a grease reaction mixture. Contactors (or any pressurized kettle) are used where water is required to be present in the reaction mixture at a temperature higher than the boiling point [6]. It is important to mention here that pressure is also generated in the closed kettle when heating the reaction mixture.

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Flow rate of Heat Transfer Fluid

Flow rate of heating fluid (heat transfer oil in the current study) directly affects the rate of temperature rise which can be critical when the reaction mixture is being heated to the required range. If the reaction mixture is heated too fast then it may cause problems of a varied nature. In some cases, saponification reaction may not complete thereby lowering the overall yield and in some cases it may affect the quality of manufactured soap.

In one of the studies performed, authors looked at two different cases for Lithium 12-hydroxystearicacid (12HSA) thickener based grease where the HT oil flow rate was increased by a factor of two and the effect on grease was evaluated. In the first case, temperature increased with a rate of 1.5째F/minute and comparatively in the second case, flow rate was increased by a factor of two which allowed the temperature to rise with a rate of 3.0째F/minute. After the reaction completed and soap was transferred into the finishing kettle, base penetrations and drop points were measured and overall grease appearance was compared. One of the striking results was the difference in appearance of soap. While the soap cooked with slower flow rate had a uniform texture, black particles were found to be uniformly distributed in the soap with an increased flow rate and a steep rise in temperature. This occurrence is attributed to the burnt solid powdered ingredient particles which did not get enough time to dissolve and an extremely fast heating rate scorched the powder resting on the inner heating coils. A slow heating rate allows enough time to mix and dissolve the solid raw materials thus avoiding such occurrence. In addition to this, penetration for case 1was lower than for case 2 which means that soap cooked with a slow uniform heating was thicker than the one cooked with a fast heating rate. This allows the yield to be higher for case 1. Drop points were also higher for case 1 than for case 2 which is a direct indication of better grease quality.

Role of mixing in achieving effective heat transfer

One of the major factors that plays a role in ensuring proper heat transfer in grease manufacture specifically is the type of mixing involved. Grease cooks pass through several stages during the manufacture. As mentioned earlier, it is a multiphase reaction where initial stage have more of a liquid phase with base oil acting as the dissolving medium for solid raw materials and liquid additives. During the course of reaction and subsequent soap formation, mixture thickens up to a semi-solid phase which is then thinned out in the finishing stages to a semi-liquid phase depending on the grease grade required. It is imperative that mixing needs to be vigorous in the initial stages of grease manufacture to improve the reaction kinetics and reduce the time taken for reaction completion. However, in the later stages when soap network is formed, mixing needs to be slow but effective. In terms of heat transfer, if mixing is not vigorous enough, it will generate a temperature gradient in the reaction mixture allowing pockets of low and high temperature regions. Another concern arises from the fact that, if mixing is poor, heat removal rate from the jacket wall (maintained at a temperature of around 400째F [204째C]) will be low which may end up scorching the product.

A typical temperature gradient plot in agitated reaction vessels is shown below,

Figure 6: Schematic of a typical temperature gradient in an agitated vessel.

Figure 5: Lithium grease cooked with (a) low HT oil flow rate; (b) high HT oil flow rate

Authors carried out experiments where two grease manufacturing kettles with different mixing profiles were considered. Kettle 1 was equipped with a counter rotation

- 37 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

agitator (480V, 40 H.P.) with an RPM of 30. Kettle 2 was equipped with a single rotation agitator (480V, 30 H.P.) with an RPM of 22. Authors cooked similar greases in both kettles and monitored the temperatures along the central kettle axis. Temperatures were taken in similar working conditions when the source temperature / jacket temperature was stable at 240째F. A plot was generated with the data as shown below,

Figure 7: Temperature gradient for kettles with fast counter rotation (a) and slow single rotation mixing (b) It can be clearly observed from the resulting plot that kettles having a vigorous mixing profile has a less temperature gradient (shown by red arrow) compared to the cased where mixing profile is relatively slow. The difference in the current study was about 30째F at the center of kettle when the source temperature was at 240째F [116째C]. This result is qualitative in nature and the temperature difference may change based on the source temperature, mixing profile or type of grease.

Another parameter that assists in evaluating the mixing needs for a particular mixture is tip speed which is defined as distance travelled by the outermost point of the mixer blade in a given amount of time. This is mathematically expressed as [12],

Where D is the diameter of mixer blade in ft. and N is the mixer rotation speed in rpm.

During scale-up calculations, the aim should be to attain a constant tip speed with varying diameter and

rotational speeds. This mixing factor holds importance in the grease industry as grease matrix is known to deform under high shear conditions. One example is that of aluminum soap based greases which possibly are extremely sensitive to shear and are known to break down mechanically losing both their consistency and lubricating effectiveness [13]. A simple rule of thumb is that lower tip speeds are preferred for mixtures with higher viscosities and higher tip speeds for thin fluidic mixtures.

This holds true for grease manufacturing as well where tip speeds in contactor are higher than in the finishing kettle almost by a factor of 10 thereby producing high shear rates. However, high tip speeds in the finishing kettles with viscous grease mixtures is not advisable as it may lead to grease break down.

Heat transfer dependence on grease composition / reaction fluid

Grease composition may also be a factor affecting the rate of heat transfer through the reaction fluid and also once the grease is put under application. One reason for this is the difference in thermal conductivities of base oils. Base oil is the name given to lubrication grade oils initially produced from refining crude oil (mineral base oil) or through chemical synthesis (synthetic base oil). Base oil is typically defined as oil with a boiling point range between 550 and 1050 F, consisting of hydrocarbons with 18 to 40 carbon atoms. One of the studies shows that group V base oils have a higher thermal conductivity than group II base oils [14]. Base oils can be paraffinic or naphthenic based and another study shows that paraffin based oil have a better thermal conductivity than naphthenic base oil [15]. Since grease is ~ 80% base oil, thermal conductivity of grease reaction mixture is dominated by base oil properties.

A study was carried out where Lithium 12-hydroxystearicacid (HSA) thickener based grease samples with different base oils were heated with a constant heat supply rate. A temperature vs. time reading data was accumulated (Table 1)

- 38 VOLUME 80, NUMBER 4

Table 1: Rate of heat transfer for grease composed of Paraffinic base oil (CASE-1) and Naphthenic base oil (CASE-2) The data above shows that rate of heat transfer is higher for case-1 with an average heat transfer rate of 5.85째F/min compared to 5.06째F/min for case-2. This result indicates a higher thermal conductivity for greases cooked in paraffinic base oils compared to those cooked in naphthenic base oils.

Table 2: Rate of heat transfer for lithium complex structure grease (CASE-1) and standard lithium grease (CASE-2) Another experiment with a similar set up was performed to test the effect of complex formation on the grease ability to conduct heat. A lithium soap based and a lithium complex soap based grease were heated at a constant rate to ~ 300째F [149째C] and the temperature vs time data was collected (Table 2).

Results show that lithium complex grease provides more resistance to heat transfer than the regular - 39 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

lithium greases. This probably is due to the microstructure of complex greases where more energy is required to break the complex structure than that for a simple lithium grease. Test samples were additive inclusive finished greases. These data are mostly qualitative and indicative of the effect of grease composition and structure on the ability of grease to transfer or conduct heat.

Effect of heat absorption capacity

Another study was performed to check the effect of grease composition on heat absorption capacity and subsequent rate of temperature rise. Heat capacity of a material is defined as the ratio of heat energy transferred to an object and the resulting increase in temperature of that material.

This is represented by the following equation [16],

or it can also be expressed as,

where Q is the heat transferred to a material, m is the mass of material and c is the specific heat of the material.

Grease 1 was lithium based and grease 2 was poly urea based and both were in the same penetration range of 300 – 305. 1000 gm of grease sample was put in an open mixer exposed to a heating coil bath. Heat source was set at a constant heating rate with the maximum attainable temperature of 180°F [82°C]. Heating was started from room temperature and data was recorded till a constant temperature was attained for both samples. Results for grease 1 and grease 2 were plotted together and are shown in Figure 8.

Figure 8: Effect of composition on heat absorption rate of lithium based (a) and poly urea based (b) grease.

Since the temperature difference between bath and grease mixture is higher in the beginning, the rate of heat absorption and temperature rise is higher initially for both grease samples and as it reaches close to the maximum temperature of bath (~180°F [83°C]), the rate decreases significantly towards the end. One clear difference between the two grease samples is that lithium

based grease attains a temperature of 174°F [79°C] after almost 3 hours of mixing whereas poly urea grease is at 158°F [70°C] after the same amount of time. This is an indication that lithium based grease has a higher heat capacity compared to poly urea based grease. Rate of temperature is comparable for both greases till 130°F [54°C] mark after which it slows down significantly for poly urea base grease compared to lithium base grease.

Result of this nature suggests that during the manufacture of poly urea grease, more heat should be provided to reach a certain temperature compared to the case of lithium base grease.

SUMMARY / CONCLUSION

This study focused on significance of heat transfer and also the role of efficient mixing in controlling grease manufacturing operations at a commercial level. There is a constant objective to improve and optimize the manufacturing process by reducing the batch cycle time while improving the product quality in conjunction.

Proper temperature control is a necessity to achieve this goal as shown in the above study. Various factors that affect heat transfer in batch operations were discussed with specific focus on grease manufacturing. Difference in temperature control between a contactor and open kettle were studied and it was established that heat transfer is more effective in a contactor owing to more heat transfer surface area and vigorous mixing profiles.

Flow rate of heat transfer media is directly proportional to achieving heat transfer efficiency; however, proper control of the same is of paramount importance. Role of overall heat transfer coefficient (U) was discussed (with the defining mathematical relations) in deciding the materials for grease kettle construction. A higher value of ‘U’ indicates better capability of the material for heat transfer. Mixing has a direct effect on circulation of heat by reducing temperature gradients in the grease mixture.

Studies indicated that counter rotating mixers were more effective than single rotation mixers in achieving a uniform temperature control. Grease is a broad term and based on the type of soap used for formation of multiphase grease network determines various grease properties. On similar lines, heat transfer may also be different for different greases and experimental results indicate that lithium based grease has a lesser resistance to heat transfer than a lithium complex grease. Also, results show that choice of base oil also affects the heat transfer properties. Overall, grease manufacture, just

like any other chemical reaction is sensitive to methods of heat transfer and based on various factors (such as mixing, type of grease and so on) encountered in real life manufacturing processes, it is important to control and optimize the heat transfer mechanism to ensure reduction of batch cycle time while maintaining high quality standards.

ACKNOWLEGEMENT

Authors acknowledge the help of grease cooks in generating and documenting the data used in this study.

Authors are also thankful to lab personnel especially Daniel Cruz for preparing grease samples and running some designed experiments relevant to the current study.

BIBLIOGRAPHY 1. ASTM D-288; www.astm.org 2. Wright, J., “Grease Basics” Machinery Lubrication Issue 5, 2008 3. Couronne, I. et al. Tribology transactions, Vol. 46 (2003), 1, 31-36 4. Christiernsson, A. White Paper, Lubrisense, 04, 01 5. Euzen, J. P., Tramboze, P., Wauquier, J. P. “Scale up Methodology for Chemical Processes”, Editions TECHNIP, 1993.

6. Boner, C. J., “Manufacturing and Applications of Lubricating Greases” Reinhold Publishing Corp., 430 Park Ave. NY, 1954 7. NLGI. “Lubricating Grease Guide” Published in Kansas City, Missouri, 2006, pp. 11.

8. Carpenter, K. J. “Agitated Vessel Heat Transfer”, Thermopedia (2011) 9. Markovitz, R. E. “Picking the Best Vessel Jacket”, Chemical Engineering (1973) 10. STRATCO Inc.; www.stratcoinc.com 11. Nassar, N. N. et al. Education for Chemical Engineers, 6 e83-e89 (2011) 12. Stuart, M.C. “Air propeller performance and design by the specific-speed method” Practical Engineer and Engineers Gazette. Volume 58, p 148-149 (1918) 13. “Thickeners in Grease Matrix” Lubrisense (2005) 02.

14. Scott, W. et al. Proceedings of World Tribology Congress 64316 (2005) 15. Kraweic, S. et al. International Doble Conference LUB-2403E (08.11) 16. http://en.wikipedia.org/wiki/Heat_capacity

- 41 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

EVALUATION OF BORON ESTERS IN LITHIUM COMPLEX GREASES PREPARED WITH HYDROGENATED CASTOR OIL Vijay Deshmukh, Bhupendra K. Rajput Standard Greases & Specialities Pvt. Ltd.

Abstract:

Traditionally, lithium complex greases are prepared using complexing agents such as boric acid, sebacic acid, azelaic acid etc. to boost the dropping point of lithium base greases. These complexing agents are added in the initial stage of soap making. The process of lithium complex grease preparation using these complexing agents is tedious, time consuming and not very flexible.

The advent of Boron Esters as dropping point boosters has made the Lithium Complex grease making process very simple, less time consuming, flexible and economical. The commercial boron esters are recommended in lithium greases prepared using 12 hydroxy stearic acid (12 HSA) and these boron esters are added at the final stage of the process before homogenization and at temperatures below 90°C, like other performance additives. The boron ester additive suppliers recommend their additives to be used in Lithium Grease prepared with 12 HSA as the same are not very effective in boosting the dropping point in lithium grease prepared with Hydrogenated Castor Oil (HCO).

Lithium complex greases using boron esters with Hydrogenated Castor Oil (HCO) have been prepared with a modified process to get higher dropping point. This paper describes the evaluation of some commercially available boron esters as dropping point boosters in lithium greases prepared using Hydrogenated Castor Oil (HCO) in place of 12 hydroxy stearic acid (12 HSA). The resulting boost in dropping point is almost same as in lithium complex grease with 12 HSA. Lithium complex greases have been prepared with HCO in different base oils using the modified process and different boron esters. The results are discussed. Lithium complex grease prepared with HCO & one of the boron esters has been tested fully & its properties are compared with lithium complex grease prepared with 12 HSA with the same boron ester. The comparative test data indicates that the developed process gives superior lithium

complex grease. The various advantages of the process have been discussed.

Introduction: NLGI Annual Production Survey of 2013 indicates that over 77 % of the total grease produced in the world is based on lithium soap. Out of this, around 19% is lithium complex grease. As per the survey, Lithium Greases having dropping point above 210°C are considered as complex greases in the NLGI Production Survey.

In India, around 90% of the total grease produced is lithium base and out of this, around 5-­‐7% is Lithium complex grease.₁ Lithium Complex Greases are popular for high temperature applications especially in Steel Plants where the operating conditions are most severe.

These greases are also used as long life wheel bearing greases in automotive industry. For wide temperature applications, lithium complex greases are also prepared using synthetic oils such as PAO, OSP etc.

Traditionally, lithium complex greases are prepared using complexing agents such as boric acid, salicylic acid, dibasic acids etc. Among the dibasic acids, sebacic acids and azelaic acids are the most popular. Lithium complex greases prepared using sebacic acid and azelaic acid in synthetic hydrocarbon have similar physical properties.₂ Cost of these acids keep on varying and plays a role in the final selection of these acids for use as a complexing agent.

In lithium complex grease, the boric acid & dibasic acids as complexing agents are introduced in the initial stage of saponification. The use of these complexing agents increases the percentage of lithium hydroxide and there by increases the cost of the product. The manufacturing process for these greases is generally an open kettle process and is tedious, long and not very flexible.

It is known that lithium complex greases having high dropping points, good extreme pressure properties and very satisfactory water resistance properties can be

- 42 VOLUME 80, NUMBER 4

prepared by employing boron esters/ boron esters-­‐amine complexes in lithium hydroxy fatty acid soap thickened greases. It appears on the basis of IR analysis and other evidence that a stable co-­‐ordinated compound is formed by electron sharing between the boron atom of the boron ester and hydroxyl group of the hydroxy fatty acid soap, which accounts for the difference in the effect of the boron ester compounds in hydroxy fatty acid soap thickened greases and conventional fatty acid soap thickened greases.₃ The advent of Boron Esters as complexing agents has made the lithium complex grease making process simple. The presence of boron esters is not required in the initial cooking stage. It is added at the end of the manufacturing stage before homogenization/milling like other performance additives. The addition of boron ester does not increase the percentage of lithium hydroxide. Lithium complex greases produced by adding boron esters as complexing agents have shorter batch cycle times as compared to lithium complex greases conventionally manufactured using dibasic acids. This results in energy savings & improved production efficiency.₄ The boron esters employed to raise the dropping point of lithium greases are compounds of alkyl or aryl borates or aliphatic amines/ amides to form boron ester adducts or complexes. The boron esters added to lithium base greases form lithium borates which change the dropping point of lithium base greases. The change in dropping point varies depending upon the type of lithium borate formed i.e. monolithium borate, dilithium borate or trilithium borate or

mixture of these borates. It has been established that presence of dilithium borate increases the dropping point to a large extent.₅ Presence of lithium phosphate also plays a role in boosting the dropping point.

It is also known that boron esters possess friction reducing, antiwear and antioxidant characteristics when blended in lubricating oils.

X-­‐ray photo electron spectroscopy and X-­‐ray diffraction reveal that boron esters can be adsorbed on the rubbing surface and some of the adsorbed borate film degrades and forms boron nitride which is responsible for reducing the friction.₆ It has been observed that lithium complex greases prepared from 12 HSA are slightly transparent and darker in color and have poor mechanical stability. The lithium complex grease preparation with boron ester is definitely easier and less time consuming as compared to preparing lithium complex grease using dibasic acids or boric acid as complexing agent. In addition, use of boron esters gives flexibility and reliability regarding getting the required high dropping point.

The commercially available boron esters from various additive manufacturers are recommended in lithium base greases made from 12 HSA. Although, the lithium base greases prepared with 12 HSA are converted to lithium complex greases with high dropping point by addition of boron esters, the lithium complex greases so formed have poor mechanical stability as compared to complex greases prepared using dibasic acids as complexing agents.

The mechanical stability in terms of difference between 60 strokes and 100 k strokes penetration and

roll stability is inferior in lithium complex grease prepared with 12 HSA as compared to lithium complex grease with HCO. The cost of the final grease also goes up as 12 HSA is costlier than HCO. Further, the batch cycle time of lithium complex grease with HCO is reduced as the saponification is carried out in pressure vessel.

Dropping point booster additives based on boron ester chemistry are available in the market from reputed additive manufacturers. All these additive suppliers advise to use their additive in lithium base grease prepared with 12 HSA. The dosage recommended by most of the additive manufacturers range from 1 to 3 % of the total charge and the additives are recommended to be added at temperatures below 90° C. The regular use of these additives in lithium greases prepared with 12 HSA in recommended dosages have confirmed that the use of these additives raises the dropping point to more than 260°C there by converting normal lithium base grease into lithium complex grease.

However, the same boost in the dropping point is not observed if these additives are added in lithium base grease prepared from HCO. A special process has been developed to convert conventional lithium base greases prepared with HCO into lithium complex greases with the addition of boron ester.

The same additives which are used as dropping point boosters based on Boron ester chemistry in lithium base greases with 12 HSA are used in lithium complex greases prepared with HCO to boost the dropping point.

- 43 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

Experimental Work

FIG.1

Experiment 1 For the study, five samples of commercially available boron esters were collected. These additive samples were identified as A, B, C, D & E. As per the Technical Data Sheets of these boron additives, the chemical structures of these additives are different. They are alkyl boron esters, boron amide complex or boron amine complexes etc.

Lithium complex greases were prepared in the laboratory using Group 1 paraffinic oil of VG-­‐ 100, Hydrogenated Castor Oil (HCO) and the boron ester additives. Each batch was prepared separately for each additive. The developed process was used to manufacture these batches. In all the batches same dosage (3 %) of boron ester additives were used. The batches were milled through colloid mill. All the batches were tested for dropping point as per ASTM D-­‐2265 test method. The results are given in Table 1.

TABLE 1

The additives C&D give highest boost in dropping point.

It was observed that the developed process of preparing lithium complex grease from the lithium base grease with HCO has been successful and gives dropping point above 260°C with all the boron esters tested. The boost in dropping point varies depending upon the type of boron ester used. The dosages of boron esters can be further optimized there by further reducing the cost of the lithium complex grease.

Experiment 2 Dropping Point of Lithium Complex Greases with HCO & Paraffinic oil Table 1 shows the results of dropping point of lithium base greases made with HCO, paraffinic oil and with different boron ester additives. The developed process was successful in raising the dropping point of all lithium base greases prepared from HCO with all the different boron esters. The additive dosages in all the samples were same. The efficiency in boosting the dropping point was however different. But all the samples gave dropping points more than 260°C which is generally the requirement in the specification of Lithium complex grease.

The dropping point of Lithium Complex greases using boron esters A, B, C, D &E are depicted on bar chart below.

As the developed process was found to be successful in paraffinic oil, the same was tried out in different types of base oils to check the efficacy of the process. The boron esters C &D which have given maximum boost in dropping point were selected for this study.

Following oils were selected.

Paraffinic Naphthenic Poly Alfa Olefin (PAO) Oil Soluble Polyalkylene glycol (OSP) Since the majority of Automotive and Industrial greases are made with base oil viscosity of VG-­‐ 220, the same viscosity grade was used for making these greases. VG-­ ‐220 viscosity was achieved by blending light oil and heavy oil. No polymer was used to boost the viscosity.

The properties of the oils used are given in Table 2

- 44 VOLUME 80, NUMBER 4

TABLE 2 Only two of the above boron esters C & D which had given very good results were selected for further study. Lithium complex greases were prepared using the same developed method with HCO. Greases were prepared separately with these base oils of ISO VG-­‐220 Grade using the boron esters C&D. In all these greases same dosages of the boron ester C & D were added. Also in all the greases 0.5 % of ZDDP was added.

It has been observed that addition of ZDDP further boosts the dropping point of lithium complex greases. It has been reported that ZDDP interacts with lithium hydroxide forming lithium dithiophosphate, zinc oxide and water.

Zinc oxide further reacts with ZDDP forming basic ZDDP. Sivik and coworkers proposed that ZDDP has polar-­‐ polar association with lithium soap fibers.⁷ This could be the reason for further increase in dropping point of lithium complex greases by addition of ZDDP. The dropping point of all these greases were determined by ASTM D-­‐2265 test method and given in Table 3.

TABLE 3 The dropping point results are shown in bar chart .Fig.-­‐2 FIG.2 It is observed that both the additives C &D boost the dropping point of lithium base greases prepared with HCO in different base oils such as PAO, OSP, Naphthenic & Paraffinic oils.

However, the increase in dropping point is different with different base oils.

Although the boost in dropping point of lithium complex grease by addition of boron ester is not fully understood, there are different theories proposed.

G.S. Bright had carried out systematic studies on the relationship of solubility parameters of various oils and the properties of lithium soap greases. He concluded that there appears to be straight line (inverse) relationship between the solubility parameters of - 45 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

the oils and the dropping points of lithium 12 hydroxy stearate greases made from them. The higher the solubility parameter, the lower the dropping point.⁸ So the different solubility parameters of different oils might be responsible for different boost in dropping points of lithium complex greases prepared from these oils with addition of boron esters.

Experiment 3

Further, one of the additives (C) was used to prepare fully formulated lithium complex grease (Grease CX) with developed process from lithium base grease with HCO. This grease was evaluated for all the major tests.

The properties of this grease were compared with the properties of fully formulated lithium complex grease (Grease CY) prepared with the same base oil and

TABLE 4

additives and with same boron ester but with lithium grease prepared with 12 HSA. One more batch of lithium complex grease (Grease DY) prepared from lithium grease with 12 HSA using boron ester D was also taken for comparison. The base oil used in all the three greases is same (VG-­‐100 Paraffinic oil of Group 1). All the three greases were fortified with same EP and AW additives in the same dosages.

Grease CX-­‐ Lithium Complex Grease prepared from lithium grease with HCO & borate ester C in paraffinic oil of VG-­‐100 with EP & AW additives.

Grease CY-­‐Lithium complex grease prepared from lithium base Grease with 12 HSA & borate ester C in paraffinic oil of VG-­‐100 with EP& AW additives.

Grease DY-­‐ Lithium complex grease prepared from lithium base Grease with 12 HSA & borate ester D in paraffinic Oil of VG-­‐100 with EP& AW additives.

The properties of these three greases were compared and the test data is given in Table 4.

Discussions Mechanical Stability

Table 4 gives the properties of the three greases CX, CY and DY prepared using boron esters C & D. A good comparison can be made between grease CX and grease CY prepared using boron ester C. The grease CX prepared using HCO has better mechanical stability than the grease CY prepared using 12 HSA. The difference in 100 K strokes penetration for grease CX is +18 units against +28 units for grease CY. The same trend is observed in Roll Stability test carried out for 16 Hrs. at room temperature. The percentage change in penetration for grease CX is 11.4 against percentage change of 17.8 and 19.3 for greases CY and DY respectively. This indicates that the lithium complex grease with HCO has better mechanical stability than the one prepared with 12 HSA.

High Temperature properties

The Lithium complex greases are recommended for many Automotive and Industrial applications as high temperature greases. Generally, the maximum recommended operating temperature for these greases is around 160 °C. The wheel bearing leakage test as per ASTM D-­‐4290 was carried out on all the three samples.

The test temperature is 160°C. All the three greases have given the leakage within 10 gms. which is the limit specified by GC specification under ASTM D-­‐4950. The dropping points of all the three greases are above 260°C.

Fretting Wear Test

Fretting wear is a surface damage that occurs between two contacting surfaces which are in cyclic motions of small amplitude. Fretting Wear Test determines the ability of the grease to withstand such cyclic motions or vibrations or oscillatory motions. The test is carried out as per ASTM D-­‐4170 test method. The results of all the three greases show that the weight loss due to oscillatory motion for all the three greases in Fretting wear test is almost similar and well within the limit of Chassis Grease requirement of LB as per ASTM D-­‐ 4950.

Fretting Wear Test Apparatus All the other properties such as EP, AW, corrosion inhibition and oxidation resistance properties of the three greases CX, CY and DY are comparable.

Water absorption Property

The ability of the grease to absorb water without undergoing much change in the consistency is an important property and for certain application becomes very critical. In many steel plant applications, where the grease comes in contact with copious amount of water, this property plays an important role. Lithium complex greases are very popular and widely used in steel plant applications. If the grease is able to maintain its consistency even in presence of water it is an added advantage. Lithium complex greases prepared with HCO and the boron ester have the ability to absorb water and still maintain its consistency.

Two greases A &B were taken. These are fully formulated greases with VG 100 paraffinic oil. One was prepared with Hydrogenated castor oil and the other with 12 hydroxy stearic acid. Both were fortified with boron ester C and other extreme pressure, antiwear, corrosion inhibitor and antioxidant additives at the same dosages. Both the greases were tested for 60 strokes penetration, 10,000 strokes penetration and 10,000 strokes penetration after addition of 10% water. The results are shown in Table 5

- 47 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

TABLE 5 The results show that the lithium complex grease prepared with HCO and the boron ester C has better stability in presence of water than the lithium complex grease prepared with 12 hydroxy stearic and the boron ester C. So this property of better stability in presence of water is expected to give better performance in applications where there is a possibility of copious amount of water coming in contact with grease such as steel plant applications.

Acknowledgement

The authors wish to thank the management of Standard Greases & Specilities Pvt. Ltd. for their support and permission to present this paper in NLGI Annual Meeting at Idaho, USA.

References

Conclusions

Various boron esters have been evaluated and a process has been developed to manufacture Lithium complex greases with HCO & using these commercial additives based on boron esters chemistry.

Lithium complex greases prepared with HCO and boron ester have better mechanical stability as compared to lithium complex greases prepared with 12 HSA and same boron ester as demonstrated by the prolonged work penetration test and roll stability test results.

The developed process also works in other types of base oils such as naphthenic, poly alpha olefin oils and oil soluble polyalkylene glycol in raising the dropping point of lithium complex greases prepared with HCO. Lithium complex grease prepared with hydrogenated castor oil and boron ester show superior water absorption property as compared to lithium complex grease prepared with 12 hydroxy stearic acid and the same boron ester.

- 48 VOLUME 80, NUMBER 4

1. NLGI Lubricating Grease Survey 2013 2. “An Evaluation of sebacic acid and azelaic acid as thickeners in Lithium Complex Greases” by W. Tuszynski, Ivanhoe Industries Inc. & Paul Besette, Triboscience & Engineering Inc. NLGI Spokesman, Vol.72, July 2008.

3. US Patent 3,125,525 May 17, 1964 W.R. Siegart et al.

4. “An Investigation into use of Boron Esters to improve High-­‐Temperature capability of Lithium 12 Hydroxy stearate Soap thickened Grease” By John Lorimor.

Presented at NLGI 76th Annual Meeting, Arizona.

5. US Patent 4, 802, 999. Feb. 7, 1989. Koizumi et al.

6. “Boron Esters used as lubricant additives” J. B. Yao et al., Lubrication Science Vol.14, issue 4,415-­‐423, Aug. 2013.

7. “Interactions of Zinc Dithiophosphates with Lithium 12 hydroxystearate Grease” Sivik M.R. Zeitz J.B. Bayus D. Presented at NLGI Annual Meeting 2001 at Florida.

8. “Base oils-­‐An evolving landscape” by Alan Outhwaite & John Rosenbaum, White paper Lubrisense 2011.

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the Expert Q:

We have used uroflax type gear coupling in Boiler feed pump - booster pump rotate at 1480rpm and couple between motor & booster pump. We used molycoat 1000 type grease for lubrication purpose, but after some running grease dry and it effect erosion & corrosion of gear tooth and damaged the tooth. So please suggest the proper grease type for lubrication purpose.

A:

Euroflex (UK) and Euroflex India reportedly manufacture non-lubricated flexible disc couplings.

Dow Corning Molykote (R) 1000 is an anti-seize paste containing solid lubricants and metal powders, not a coupling grease. Grease-lubricated gear couplings require specialized products that do not readily separate base oil in service. Such products typically contain high concentrations of polymers. Coupling greases are typically not suitable for use in bearings or other applications where greases are normally used.

Coupling gear tooth corrosion and damage may indicate inadequate performance of the lubricant, or an excessively long relubrication interval. The interval between grease changes on a grease-lubricated coupling should be adjusted so that the performance of the product does not significantly degrade over the service

period. Factors such as elevated temperature can significantly shorted relubrication intervals.

Seizing of Threaded Couplings A frequent complaint expressed about stainless steel fasteners an other threaded couplings is the problem of seizing. The problem is frequently not that of the material itself but more than likely caused by mismatched threads, Nonuniform threads, an dirt on threaded surfaces. Reasonable care should be exercised in the handling of fasteners to prevent damage and to keep threads clean.

Fasteners made in accordance with nationally recognized standards, such as published by the American National Standards Institute, Inc. (ANSI), will assure that nuts and bolts are uniformly threaded.

Torque should also be considered for a properly fastened joint. Suggested maximum torque values for stainless steels are published in the booklet “Stainless Steel Fasteners A Systematic Approach to Their Selection.”, copies of which are available from the Committee of Stainless Steel Producers. Nevertheless, galling may occur in clean, carefully machined threads, and it may be desirable to use a lubricant if another alloy material either cannot be used or is not available.

If a lubricant is going to be used with threaded fasteners, tests should be conducted to determine torque

- 50 VOLUME 80, NUMBER 4

requirements and to evaluate the compatibility of the lubricants to the environment. Among the popular lubricants are those containing substantial amounts of molybdenum disulfide, graphite, mica, talic, copper or zinc fines, or zinc oxide. Zinc-bearing lubricants are not recommended for use with stainless steels at elevated temperature.

Q:

Can a blend of fumed silica and bright stock be called a silicon grease?

A:

In general, greases that are claimed to be “silicone” (not silicon) are those based on a silicone fluid (some form of siloxane fluid). Some of those products are thickened with fumed silica, but other thickeners are also possible in greases based on silicone fluids. In the case of the composition described, it would be proper to call the product “silica-thickened grease,” but not simply “silicon grease,” since the majority of the composition would be mineral oil (bright stock), which contains no silicon.

that causes the oil to become opaque. Less thickener (better yield) in the grease is controlled by the base oil characteristics (chemical make-up, solvency) as well as the manufacturing procedure and conditions. A product that contains a significant portion of naphthenic base oil (relatively low aniline point) will have a better yield (contain less thickener) than a product based only on paraffinic base oils. In particular, if the soap is formed in naphthenic base oil during saponification, the yield will be significantly improved. A word of warning, though - if the thickener content is too low, the oil separation, mechanical stability, and water resistance properties of the grease can be affected. Grease formulation is a balance, and striving for transparency should not be allowed to compromise other performance properties.

Q:

We are trying to manufacture Lithium based grease with high transparency. Can you give us any advice?

A:

Transparent, or at least translucent, lithium soap greases tend to be made with light-colored base oils and additives that do not cause them to become opaque. The degree of translucency is related to the amount of thickener in the product. A product with less thickener will be more translucent, since it is the thickener

- 51 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

Industry Calendar of Events Please contact Marilyn if there are meetings/conventions you’d like to add to our Industry Calendar. marilyn@nlgi.org (Your company does not have to be an NLGI member to post calendar items.)

September 20 – 22, 2016 2016 China International Lubricants, Base Oils & Additives Conference Langham Place Guang Zhou, PR China

October 10-12, 2016 13th ICIS Middle Eastern Base Oils & Lubricants Conference Intercontinental Dubai Festival City - UAE http://www.icisbaseoils.com/ mebaseoils2016

October 15-18, 2016 ILMA Annual Meeting Fairmont Scottsdale Princess Scottsdale, AZ http://www.fairmont.com/ scottsdale/

October 17, 2016, 4 – 7 PM Stratco Open House – Office & Laboratory 7440 E. Karen Dr. Suite 400 Scottsdale, AZ 85260 http://www.stratco.com

October 26 – 28, 2016 UEIL Annual Congress Berlin, Germany More Information

November 1-3, 2016 5th ICIS African Base Oils and Lubricants Conference Dar es Salaam, Tanzania, Aftrica http://www.icisconference.com/ africanbaseoils

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November 7, 2016 Working Group Meeting November 8-9, 2016 Grease Training Course November 9-10, 2016 The 3rd ICIS & ELGI Industrial Lubricants Conference Amsterdam, The Netherlands http://www.icisconference.com/ Industriallubricants

November 30 – December 2, 2016 12th ICIS Pan American Base Oils & Lubricants Conference Hyatt Regency Jersey City, USA http://www.icisbaseoils.com/ panambaseoils2016

February 15-17, 2017 21st ICIS World Base Oils & Lubricants Conference Park Plaza Westminster Bridge, London, UK http://www.icisconference.com/ worldbaseoils2017

March 7 – 10, 2017 F+L Week 2017 Four Seasons Hotel, Singapore Call for Papers until Sept. 9, 2016 submit to: conference@ fuelsandlubes.com More Information: http:// fuelsandlubes.com/

April 5 & 6, 2017 5th ICIS Indian Base Oils & Lubricants Conference Mumbai, India http://www.icisconference.com/ indianbaseoils2017

April 20-22, 2017 ILMA Management Forum Park Hyatt Aviara Carlsbad, CA

May 6-9, 2017 29th ELGI AGM Hilton Kalastajatorppa Helsinki, Finland Visit Website

May 21-25, 2017 72nd STLE Annual Meeting & Exhibition Hyatt Regency Atlanta, Georgia (USA) More Information

June 10th – 13th, 2017 NLGI 84th Annual Meeting Olympic Valley, CA Resort at Squaw Creek October 10 – 14, 2017 CLGI Biannual National Conference China Location and more information to come

October 14-17, 2017 ILMA Annual Meeting Hyatt Regency Grand Cypress Orlando, FL October 31 – November 2, 2017 2017 Chem Show The Event for Processing Technology Javits Center New York City, New York www.chemshow.com

April 19-21, 2018 ILMA Management Forum Fort Lauderdale Marriott Harbor Beach Resort & Spa Fort Lauderdale, FL

June 9 – 12, 2018 NLGI 85th Annual Meeting The Coeur d’Alene Resort Coeur d’Alene, ID

October 6-9, 2018 ILMA Annual Meeting JW Marriott Desert Springs Resort & Spa Palm Desert, CA

June 8 – 11, 2019 NLGI 86th Annual Meeting JW Marriott Las Vegas Resort Las Vegas, NV

Welcome our 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.

New 2016 NLGI Members

AMSOIL Inc. - Marketing

Axxess Chemicals – Supplier

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

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.

- 54 VOLUME 80, NUMBER 4

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

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 - Technical

Derek Benedyk 500 West Bradley Road, A#219 Fox Point, WI 53217 USA 312-206-4819 www.dtbtwo.com 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, United Arab Emirates 41506 009-716-526-4944 www.gulfpetrochem.com Base Oil Trading, Lubricant Manufacturing - 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.

- 55 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 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 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.

MRG Labs

Richard Wurzbach 410 Kings Mill Rd., York, PA 17401, USA 717-843-8884 www.mrgcorp.com MRG is a full-service lubricant analysis laboratory dedicated to improving the maintenance programs of our customers through the development of individualized maintenance strategies. In order to meet these objectives, we offer a variety of valuable MRG offers analysis of both in-service oil and grease from industrial equipment. Our innovative test slates have been developed to require minimal

sample sizes while providing extensive lubricant condition data. Specifically, development of the Grease Thief© and Grease Thief Analyzer allow us to provide complete used grease analysis with less than two grams of grease. Our experienced analysts deliver custom recommendations for individual components based on our innovative test slate. Consulting Services Our senior staff, with over forty combined years of maintenance and analysis experience, can provide expert advice on the specifics of managing your condition-based monitoring program. Whether on-site, over the phone, or through video conferencing, we put our expertise to work to diagnose maintenance problems, improve CBM strategies and lower plant operations costs.

Pan American Equipment – Marketing

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

Runningland Metrology & Testing (Shanghai) Co., Ltd - Technical

David Zhou 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

- 56 VOLUME 80, NUMBER 4

industries. Runningland undertakes products testing for petrochemical products and equipment condition monitoring. The company operates two professional labs in Shanghai for:

•Instruments 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.

Thames River Chemical – Supplier Andy McGivern 5230 Harvester Road Burlington, ON L7L 4X4 Canada 905-220-2321 www.trc-corp.com

to Mount Milligan Mine, we own and operate a metallurgical facility in Pennsylvania, USA, at which it roasts molybdenum concentrate and other metals.

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.

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.

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 - 57 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

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.)

Acme-Hardesty To Distribute Solvay Fentamine Polyurethane Catalyst Line In North America Blue Bell, Pa – September 1, 2016 - Acme-Hardesty, a division of Jacob Stern & Sons, has been appointed by Solvay, a leading global supplier of amines, as the exclusive distributor of Solvay’s Fentamine polyurethane catalyst line in North America. The agreement makes Solvay polyurethane amine catalysts, produced in Zhangjiagang, China, available to the U.S. market. Amine catalysts are widely used in the production of polyurethane foam to control and balance the polyurethane reaction. They are primarily used for the blowing reaction in polyurethane foam formation, but also contribute to the gelling reaction in many cases. To read the complete press release visit: https://www.nlgi.org/newsand-events/industry-news/

Branson, Missouri – August 25, 2016 – Covenant Engineering Services, LLC is celebrating 20 years of being in business. CES was incorporated as a business in the state of Indiana in 1995 and reincorporated in the state of Missouri in 2013. The main purpose of CES has been to provide innovative engineering solutions to our client’s process and operations problems to improve their operating efficiency in a safe and environmentally sound manner.

The mission of CES has been to be a primary resource for process engineering support to the chemical and related industries by providing quality engineering services backed with integrity. We want to thank all our clients we have served over the past 20 years for putting their confidence in the staff of CES.

Richard and Margaret Burkhalter

Halocarbon Hires H. Carl Walther as Technical Services Manager 31-year veteran spent 18 years with Krytox™ Performance Lubricants ATLANTA – August 2, 2016 –Halocarbon Products Corporation, a leading worldwide producer of specialty fluorochemicals, inert lubricants and inhalation anesthetics, today announced that H. Carl Walther has joined the company as Manager, Technical Services/ Support. To read the complete press release visit: https://www.nlgi.org/news-and-events/ industry-news/

- 58 VOLUME 80, NUMBER 4

Patent Issued for Lubrication of Valve Stems YORK, Pa., July 27, 2016 — The United States Patent Office has issued Patent #9,360,130 for “METHOD FOR GREASING THE MATED THREADS OF A THREADED CONNECTOR AND RELATED DEVICE”. This device, known as the “StemThief ”, can be attached to an inservice motor operated valve (MOV) utilizing an adapter and lubricator unit. Once attached, the lubricator unit creates a seal around the stem nut, allowing the introduction of grease with the use of a standard grease gun. The grease gun is attached to a typical hydraulic zerk fitting, allowing pressurized grease to displace the existing lubrication on the stem threads and in the stem nut, and providing a new layer of lubrication. The displaced grease can be gathered at the base of the nut for sampling and analysis purposes, using ASTM Method D7718 sampling tools.

To read the complete press release visit: https://www.nlgi.org/news-and-events/industry-news/

ACME-HARDESTY WELCOMES THREE NEW REGIONAL SALES MANAGERS Blue Bell, Pa – Acme-Hardesty, a division of Jacob Stern & Sons, has hired three new U.S. Regional Sales Managers:

Read the entire press release to learn more about Brad, Tom & Ron visit: https://www.nlgi. org/news-and-events/industry-news/

Brad Merz is the new Regional Sales Manager for the Midwest region, covering Ohio, Indiana, Michigan, Kentucky and West Virginia

Tom Koutsos is now the Regional Sales Manager for the Midwest region based out of Chicago.

Ron Barker is the new Regional Sales Manager for the western region, based in Redondo Beach, Ca.

- 59 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

NLGI Industry News

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-andevents/industry-news/

Jet-Lube Inc. Relocates its Houston, Texas Manufacturing Plant to a State-ofthe-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/

- 60 VOLUME 80, NUMBER 4

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- 61 NLGI SPOKESMAN, SEPTEMBER/OCTOBER 2016

Helping the World Run a Little More Efficiently In todayâ&#x20AC;&#x2122;s complex marketplace, you need a technology partner that understands the demands of ever-changing applications, environmental concerns, LEAN manufacturing and worldwide standards and protocols.

Lubrizol is at the forefront of industry advancements offering our customers superior functionality, product consistency, R&D and testing. We are improving grease performance and processes worldwide.

To learn more visit www.lubrizol.com.

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