DOCSLIB.ORG

Studies on the Preparation and the Structure of Lithium Soaps

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
Studies on the Preparation and the Structure of Lithium Soaps 426 Grasas y Aceites Vol. 50. Fase. 6 (1999), 426-434 Oleochemicals I: Studies on the preparation and the structure of lithium soaps By Zein E. Shoeb, Bayed M. Hammad and A.A. Yousef National Research Centre, Dokki, Cairo. Egypt. RESUMEN 1. INTRODUCTION Oleoquímica I: Estudios sobre la preparación y la es­ The term metallic soap is used to describe alkaline tructura de los jabones de litio. earth and heavy metal salts of fatty acids that are Se han preparado estearato, palnnitato, miristato, laurato, caprato insoluble in water and either soluble in or solvated by y caprilato de litio por fusión. Se ha realizado el análisis elemental, los organic solvents, such as aromatic hydrocarbons, espectros de absorción en el infrarrojo y las difracciones de rayos X de chlorinated or hydrogenated hydrocarbons. They are los Jabones de litio preparados, además del análisis termogravimétrico also soluble in oils, greases and fatty acids preferably de los mismos. Las sales de litio anhidra de los ácidos con 12 átomos de naphthenate, linoleate, myristate, palmitate, stéarate, carbono o menos mostraron una estabilidad térmica hasta los and cerotinate successively. Lithium stéarate is used in 300 ± 78 °C dependiendo de la longitud de la cadena. Por otro lubricating grease as gelling agent because it gives a lado las sales con 14 átomos de carbono o más se descompusie­ better thermal resistance property ron a 126 ± 4 °C formándose carbonato de litio. Los jabones homólogos de litio mostraron una estructura cristalina Ralston (1) prepared the lithium soaps of lauric, similar, siendo los enlaces metal-oxígeno del mismo tipo para los myristic, palmitic and stearic acids by adding the ácidos grasos de número de átomos de carbono entre 8 y 18. calculated amount of lithium acetate to ethanol Sin embargo el ángulo de inclinación que forma la molécula con el plano basal aumentó con la disminución del número de solution of the respective fatty acids and determined átomos de carbono, lo que se observó por difracción de rayos X. the solubility of those soaps in a number of solvents. Se comprobó por espectroscopia infrarroja la intensificación They found that the lithium salts of the long chain del carácter iónico del enlace metal-oxígeno al disminuir el fatty acids are sparingly soluble in water and número de átomos de carbono. somewhat were soluble in ethanol. PALABRAS-CLAVE: Análisis elemental - Análisis termogravi­ The same authors reported the following melting métrico - Difracción de rayos X - Espectrofotometría infrarroja - points for the lithium soaps: laurate 229.2-229.8, Hidróxido de litio - Jabón metálico. myristate 223.6-224.2, palmitate 224-225, stéarate 220.5-221.5 °C. Lottmoser and Giese (2) reported the preparation of lithium salts of higher fatty acids and also measured the SUMMARY surface tension of their solutions. Void (3) prepared Oleochemicals I: Studies on the preparation and the lithium palmitate using precipitation method. structure of lithium soaps. Many investigators (4-7) studied the lubricant character of plastics and greases using lithium Lithium stéarate, palmitate, myristate, laurate, caprate and soaps. Barbooty et al., (8) and Mysak et al., (9) caprylate were prepared by means of fusion method. Elementary analysis and the infrared absorptions spectra of the prepared lithium studied the thermogravimetric analysis of some soaps as well as their X-ray diffractions and the thermogravimetric lithium soaps as lithium stéarate, lithium 12-hydroxy analyses were carried out. stéarate and related greases. The anhydrous lithium salts of fatty acids with 12 carbon In this paper we describe the preparation of six atoms or less showed thermal stability up to ca. 300 ± 78 °C depending on the chain length. On other hand the salts with 14 lithium soaps with fatty acids having carbon chain of carbon atoms or more were decomposed at 126 ± 4 °C leading to 18 (stearic acid) till carbon chain of 8 (caprylic acid). formation of lithium carbonate. These soaps will be prepared by fusion method and The homologous lithium soaps had very similar crystal subjected to Elementary analysis, IR-analysis, structure among them and their metal -to- oxygen bonds were similar for the acyl chains between 8 and 18 carbons. However thermogravimetric analysis, and finally X-ray the angle of inclination of the molecular axes to the basal plane diffraction measurements. increased with the decreasing of the number of carbon atoms of the fatty acid chain, as determined by X-ray diffraction. In addition, the ionic character of the metal -to- oxygen bond was enhanced with the decrease of the number of carbon atoms as shown by 2. MATERIALS AND METHODS infrared spectroscopy. KEY-WORDS: Elementary analysis - Infrared spectrophotometry - • Lithium hydroxid-1-hydrate. Assay 98 %; Riedel- Lithium hydroxide - Metallic soap - Thermal gravimetric analysis - de Haën. X-ray diffraction. • Fatty acids CI 8-C8 (Merck) Assay «GC» (95-99 %). (c) Consejo Superior de Investigaciones Científicas http://grasasyaceites.revistas.csic.es Licencia Creative Commons 3.0 España (by-nc) Vol. 50. Fase. 6(1999) 427 2.1 Preparation of Lithium Soaps 3.2 Infrared Absorption Spectra of Lithium Soaps The fatty acids used for the preparation of lithium soaps under investigation are stearic acid, palmitic acid, myristic acid, lauric acid, capric acid and Infrared absorption spectra of the lithium soaps caprylic acid. The lithium soaps of the above fatty under investigation, and their corresponding fatty acids are prepared by fusion method using lithium acids, namely, stearic, palmitic, myristic, lauric, capric hydroxide-1 -hydrate. and caprylic acid were determined with a pu 9712 infrared spectrophotometric recording by the Procedure: potassium bromide pellet technique in the sodium chloride region (4000-200 cm"^) at room temperature • Equimolecular amounts of the lithium hydroxide- (ca. 25 °C). 1 -hydrate and the corresponding fatty acid are Figure 1 showes the infrared absorption spectra melted together at elevated temperature. The of the stearic and the lithium stéarate. The required reaction temperature of each of the frequencies (cm'^) of the absorption maxima in the six lithium soaps is specific. both spectra are also given with assignments for the • The calculated weight of the fatty acid is most of them in Table II. weighed in 250 ml glass beaker which heated There are marked differences between the in an oil bath at the required temperature. spectrum of the stearic acid and that of the lithium • The corresponding calculated weight of the stéarate in some spectral region (Figure 1). The lithium hydroxide-1 -hydrate is added gradually absorption maxima which are characteristic of the and slowly to the melted fatty acid during a aliphatic portion of the acid molecule are essentially period of 20 minutes with constant stirring. unchanged on going from the acid to the soap. They • The reaction mixture is agitated (1000 r.p.m.) are assigned with ease by referring to a table of for another 20 minutes to complete the characteristic group frequencies. It is well known that dehydration reaction period during which the fatty acids in the solid state exist with the dimeric considerable foaming occures. structure through hydrogen bonding. The absorption • The resulting hot lithium soap is transfered maxima in the spectrum of the stearic acid at into a petri dish and cooled. On cooling the 3200-2600 (very broad, probably consisting of two soap solidifies to the required particle size. separate broad absorption), 1702, 1431, 1296 and 943 cm"'' are thus associated with the localized -COOH group of the acid molecule in the dimeric 3. RESULTS AND DISCUSSION structure. In the spectrum of lithium stéarate the strong absorption maximum at 1702 cm'^ which has 3.1 Elementary Analysis its orgin in the C = O of the acid molecule has disappeared completely. This disappearance of the The check of purity of the lithium soaps were carbonyl frequancy in the soap spectrum indicates made by the elementary analysis as show in Table I. the fact that there is a complete resonance in the two C - O bonds of the carboxyl group of the soap Table I molecule. Duval et al., (10) have shown from the extensive Elementary Analysis of Lithium Soaps investigations of the infrared absorption spectra of many metal salts of mono- or dibasic organic acid, Soap %U %c %H whether acyclic or aromatic that the coi frequencies lie in the region 1400-1300 cm'\ the coa frequencies Lithium stéarate Found: 74 12.5 Calculated: 2.4 74.3 12.1 in the region 1610-1550 cm'^ and the m frequencies in the region 950-800 cm"\ Lithium palmitate Found: 73.3 13.7 Similar assignments were made for all the lithium Calculated: 2.6 73 13.3 soaps: Again, the absorptions due to the aliphatic Lithium myristate Found: 70.6 11.2 portion of the soap molecule are in general similar in Calculated: 3 71 11.5 intensities and in their frequencies of absorption maxima, although slight but significant spectral Lithium laurate Found: 69.8 11.3 Calculated: 3.4 69.8 11.2 differences can be observed in some restricted regions. Lithium caprate Found: 66.7 10.2 Calculated: 3.9 67.3 10.7 Of course, there exist considerable differences in the absorptions due to the aliphatic portion of soap Lithium capiryiate Found: 63.4 10.2 molecules if the spectra of soaps of different fatty Calculated: 4.6 63.9 10 acids are compared. (c) Consejo Superior de Investigaciones Científicas http://grasasyaceites.revistas.csic.es Licencia Creative Commons 3.0 España (by-nc) 428 Grasas y Aceites 60 Stearic acid Lithium stéarate OL AOOO 3000 200 Wavenumber (cm" ) Figure 1 IR Absorption Spectra of Stearic acid and Lithium Stéarate Table II The Frequencies (cm"^) of Absorption IVlaxima in the Spectra of Lithium Soaps (Fatty Acids from Cs to Cis) in the region 4000-700 cm"^ Frequency (cm"^) ^^ Aecsînnûinûnt ASbiyílcmcili Li caprylate Li caprate Li laurate Li myristate Li palmitate Li stéarate 3446 (b) 3446 (b) 3446 (b) 3446 (b) 3446 (b) 3446 (b) Broad absorption of 0-H stretching vibration 2960 (sh) 2960 (sh) 2960 (sh) 2960 (sh) 2960 (sh) 2960 (sh) CH3, C-H antisym .
Load more

Recommended publications
  • DTA Study on Oxidation of Lithium Soap Grease
    100 油 化 学 DTA Study on Oxidation of Lithium Soap Grease Seiichiro HIRONAKA, Masayuki TAKAHASHI*, and Toshio SAKURAI** Tokyo Institute of Technology (2-12-1, Ookayama, Meguro-ku, Tokyo) The phase behavior of lithium soap/hydrocarbon oil and lithium soap/synthetic oil greases has been investigated using DTA. The change in the shape and size of soap micelle in the grease was examined with an electron microscope. It has been found that the phase behavior and the shape and size of the soap micelles in the grease are greatly affected by the oxidation stability of the base oil used. For the lithium stearate/squalane grease, the phase transition temperature and the L/D value of the fibers formed by the soap micelles decreased with the oxidation time. However those of the grease prepared with pentaerythritol tetraoctanoate which was stable for oxidation were hardly affected. These facts may be rcduced to a small amount of the polar compounds produced by the oxidation of a base oil. microscopy. 1 Introduction 2 Experimental The phase transitions in lubricating grease have been investigated in detail by Vold ,l' ,2' Commercially available high-purity grade Suggitt,3} and Cox4' and other authors utilizing stearic acid was purified by repeated recrystal DTA. The phase transition of lithium soap lization. Lithium stearate was prepared from grease depends mainly upon the properties of high purity lithium hydroxide and stearic acid. the soap micelles in the grease. Cox5~ and To remove unreacted stearic acid, lithium Uzu6> have suggested that the phase diagrams stearate was extracted by benzene and are affected by the molecular weight of the finally dried.
    [Show full text]
  • Eco-Friendly Multipurpose Lubricating Greases from Vegetable Residual Oils
    Lubricants 2015, 3, 628-636; doi:10.3390/lubricants3040628 OPEN ACCESS lubricants ISSN 2075-4442 www.mdpi.com/journal/lubricants Article Eco-Friendly Multipurpose Lubricating Greases from Vegetable Residual Oils Ponnekanti Nagendramma * and Prashant Kumar Bio Fuels Division, CSIR-Indian Institute of Petroleum, Dehradun PIN-248005, India; E-Mail: [email protected] * Author to whom correspondence should be addressed; E-Mail: [email protected]; Tel.: +91-135-252-5924; Fax: +91-135-266-0203. Academic Editors: José M. Franco and Jesús F. Arteaga Received: 16 July 2015 / Accepted: 29 September2015 / Published: 21 October 2015 Abstract: Environmentally friendly multipurpose grease formulation has been synthesized by using Jatropha vegetable residual oil with lithium soap and multifunctional additive. The thus obtained formulation was evaluated for its tribological performance on a four-ball tribo-tester. The anti-friction and anti-wear performance characteristics were evaluated using standard test methods. The biodegradability and toxicity of the base oil was assessed. The results indicate that the synthesized residual oil grease formulation shows superior tribological performance when compared to the commercial grease. On the basis of physico-chemical characterization and tribological performance the vegetable residual oil was found to have good potential for use as biodegradable multipurpose lubricating grease. In addition, the base oils are biodegradable and non toxic. Keywords: vegetable oil; residual oil; lithium soap; performance evaluation; biodegradable; multipurpose grease 1. Introduction The worldwide trend to use more eco-friendly lubricating greases is motivated by environmental concerns [1]. Recent trends are heavily focused on price, performance as well as biodegradability and toxicity [2]. Lubricants 2015, 3 629 The biodegradability of greases essentially reflects the biodegradability of their base oils.
    [Show full text]
  • Grease Chemistry: THICKENER STRUCTURE the Thickener Largely Determines the Grease Properties
    WEBINARS Jeanna Van Rensselar / Senior Feature Writer Grease chemistry: THICKENER STRUCTURE The thickener largely determines the grease properties. © Can Stock Photo / Morphart and © Can Stock Photo / urfingus Photo Stock / Morphart and © Can Photo Stock © Can GREASE WAS FIRST USED ON CHARIOT AXLES MORE THAN 3,000 YEARS AGO. Today more than 80% of bearings are lubricated with grease. Lithium soap greases, the most prevalent, were introduced in the early 1940s. Lithium complex greases, introduced in the 1960s, are becoming the most prevalent in North America. 26 Satellites are why TV and other signals are no longer blocked. With so many satellites in orbit, even MEET THE PRESENTER This article is based on a Webinar originally presented by STLE Education on Sept. 16, 2015. Grease Chemistry: Thickener Structure is available at www.stle.org: $39 to STLE members, $59 for all others. Paul Shiller received his doctorate in physical chemistry from Case Western Reserve University in Cleve- land, studying the surface reactions at fuel cell electrodes. He holds a master’s of science degree in chemical engineering also from Case Western Reserve University, where he studied the characteristics of diamond-like films. Shiller holds a master’s of science degree in chemistry studying the spectro-electrochemistry of sur- face reactions, and he received a bachelor’s of engineering degree in chemical engineering from Youngstown State University. Shiller joined The Timken Co. as a product development specialist for lubricants and lubrication in 2004. He then became a tribological specialist with the Tribology Fundamentals Group at the Timken Technology Center in North Canton, Ohio.
    [Show full text]
  • 32O 7– - Aprepared by Co-Saponfication 3Oo
    March 22, 1960 L. W. SPROULE ET AL PHYSICAL COMBINATION OF CALCIUM AND LITHIUM 2,929,782 HYDROXY STEARATES FOR FORMING GREASES Filed July 17, 1957 38O 360 340 MIXTURE 32O 7– - APREPARED BY CO-SAPONFICATION 3OO 4O 6O 8O IOO % LITHIUM SOAP 6O 40 2O % CACUM SOAP Lorne W. Sproule inventors Worren C. Pottenden By 3 oz. Sizzlace-é Attorney 2,929,782 United States Patent Office Patented Mar. 22, 1960 2 These greases are valued for their high dropping points. 2,929,782 Their water resistance leaves something to be desired, the PHYSICAL COMBINATION OF CALCUM AND conventional calcium greases usually giving better service LITHIUM HYDROXY SEARATES FOR FORM in the presence of water. In order to use a minimum NG GREASES 5 amount of thickener in a grease, the lithium soaps must be prepared at a temperature above 400 F. Lorne W. Sproule, Sarnia, Lambton, Ontario, and War ren C. Pattenden, Courtright, Lambton, Ontario, Can Ca 12-hydroxy stearate greases have also been dis ada, assignors to Essa Research and Engineering Comic closed in the art, and are valued because they do not have pany, a corporation of Delaware to be plasticized with water. Their dropping points, O however, do not exceed 290 F., and they must be pre Application July 17, 1957, Seria No. 672,432 pared at relatively low temperatures in the order of 275 F. It has also been found, and this is believed to be un 3 Claims. (C. 252-40) appreciative by the art, that calcium 12-hydroxy stearate greases are very water sensitive.
    [Show full text]
  • Fundamental Study of the Initial Agglomeration of Lithium Soap Thickener in Lubricating Oil
    Fundamental study of the initial agglomeration of lithium soap thickener in lubricating oil Paul Shiller1, Nikhil Prasad1, and Gary Doll1 1The University of Akron Contents 1 Introduction 4 1.1 How does the grease thickener structure form? . 5 1.2 Model of grease bleed? . 6 1.3 What is the relation of grease bleed to lubrication? . 7 2 Motivation 7 3 Testing 8 3.1 Grease Formulation . 8 3.2 Rheology . 8 3.3 Dynamic Light Scattering . 9 3.4 Atomic Force Microscopy . 10 3.5 Size Exclusion Chromatography . 10 4 Modeling 11 4.1 Geometry . 11 4.2 Theory . 14 4.2.1 ASED Theory . 14 4.3 Density Functional Theory . 16 4.3.1 Molecular Dynamics Theory . 17 4.3.2 Micelle Formation Theory . 18 5 Results 18 5.1 ASED modeling of interatomic forces . 18 5.1.1 Separation Distance . 18 5.1.2 Growth of Micelles . 19 5.2 Rheology . 19 5.2.1 Rheology: Oscillating Stress Sweep . 19 5.2.2 Rheology: Frequency Sweep . 21 5.3 Dynamic Light Scattering Results . 23 5.4 Atomic Force Microscopy . 24 5.5 Size Exclusion Chromatography . 24 6 Discussion 25 References 27 A Grease making procedure 29 B Rheology testing procedure 31 List of Figures 1 Continuum of micelle structures over water, oil, and surfactant (soap) concentrations. 4 2 Storage and loss moduli plotted against angular frequency of oscillation showing the relative intensity. Scaling is identical for both y-axes. The storage modulus is greater than the loss modulus at 20% grease and above which is an indication that it is still grease-like.
    [Show full text]
  • Fatty Acids and Antioxidant Effects on Grease Microstructuresଝ
    Industrial Crops and Products 21 (2005) 285–291 Fatty acids and antioxidant effects on grease microstructuresଝ A. Adhvaryu a,c, C. Sung b, S.Z. Erhan c,∗ a Department of Chemical Engineering, Pennsylvania State University, University Park, PA 16802, USA b Center for Advanced Materials, Department of Chemical and Nuclear Engineering, University of Massachusetts, Lowell, MA 01854, USA c USDA/NCAUR/ARS, Food and Industrial Oil Research, 1815 N. University Street, Peoria, IL 61604, USA Received 24 January 2003; accepted 30 March 2004 Abstract The search for biobased material as industrial and automotive lubricants has accelerated in recent years. This trend is primarily due to the nontoxic and biodegradable characteristics of seed oils that can substitute mineral oil as base fluid in grease making. The paper discusses the preparation of lithium soap-based soy greases using different fatty acids and the determination of crystallite structure of soap using transmission electron microscopy (TEM). Lithium soaps with palmitic, stearic, oleic, and linoleic acids were synthesized and mixed with soybean oil (SBO) and additives to obtain different grease compositions. TEM measurements have revealed that the soap crystallite structure impact grease consistency. Soap fiber length and their cross-linking mechanism in the matrix control grease consistency (National Lubricating Grease Institute (NLGI) hardness, ASTM D-217 method). Lithium stearate-based soy grease has a relatively more compact fiber structure than Li palmitate. Linoleic acid (C18, ==) with two sites of C–C unsaturation in the chain has a much thinner and more compact fiber network than oleic acid (C18, =). The presence of additive in grease produces a soap with looser network and larger fiber structure than similar grease containing no additive.
    [Show full text]
  • Bagi Uta 2502M 11920.Pdf (4.726Mb)
    EFFECT OF ADDITIVE MORPHOLOGY & CHEMISTRY ON WEAR & FRICTION OF GREASES UNDER SPECTRUM LOADING by SUJAY DILIP BAGI Presented to the Faculty of the Graduate School of The University of Texas at Arlington in Partial Fulfillment of the Requirements for the Degree of MASTER OF SCIENCE IN MATERIALS SCIENCE AND ENGINEERING THE UNIVERSITY OF TEXAS AT ARLINGTON December 2012 Copyright © by Sujay Bagi 2012 All Rights Reserved ACKNOWLEDGEMENTS I would sincerely like to express the deepest appreciation and gratitude to my advisor and committee chair, Dr. Pranesh Aswath, who has continually encouraged me the with the spirit of independent thinking and instilled a research acumen in me throughout my time as a graduate student in the Department of Materials Science & Engineering at the University of Texas at Arlington. His fabulous knowledge of subject matter and meticulous way of guidance makes him the most remarkable mentor in the department. My sincere gratitude to the committee members, Dr. Yaowu Hao and Dr. Fuqiang Liu for being so encouraging and cordial; I am indebted to many of my colleagues and friends at UTA for making this time one of the most memorable moments in my life. I would like to whole-heartedly thank Dr Xin Chen for all the help regarding the chemistry formulations and Soxhlet apparatus. I would like to express my deepest gratitude to Dr. Mihir Patel for being a great friend and a mentor; I would like to acknowledge all my colleagues in the Tribology & Bio-materials group Megen Velten, Olumide Oruwajoye, Pradip Sairam, Vibhu Sharma, Ami Shah, Olusanmi Adeniran for all the help and the support I received.
    [Show full text]
  • Grease Manufacturing: Chemistries and Processes
    WEBINARS Dr. Nancy McGuire / Contributing Editor Grease manufacturing: Chemistries and processes © Can Stock Photo / apopium KEY CONCEPTS • ThThee grease manufacturinmanufacturingg The right materials and processes process is as importantimportant as ththee formulationformulation inin providinproviding the can make the difference between desireddesired propertiesproperties and success and failure. performance.performance. • OpOpenn kettles, pressurepressure kettles,kettles, ConContactortactor® vvesselsessels aandnd continuouscontinuous procesprocess unitsunits each offeroffer advantaadvantagesges forfor various GREASE MANUFACTURING GOES BEYOND BLENDING OILS. The formulations and processes. manufacturing process is as important as the formulation in providing the desired properties and performance. A wide va- • Maintainint g control ofof the startingstarting riety of applications requires an equally diverse range of grease mamaterialsterials and the reacreactiontion aandnd compositions and physical properties. Grease is typically about 80%-95% base oil, 2%-20% thickener and 0%-15% additives. processing conditions increases However, some greases contain as much as 98% base oil and productproduct consistencyconsistency aandnd processprocess others contain more than 20% thickener. predictability.predictability. 32 • MARCH 2017 TRIBOLOGY & LUBRICATION TECHNOLOGY WWW.STLE.ORG MEET THE PRESENTER This article is based on a Webinar presented by STLE Education on Sept. 27, 2016. “Grease Manufacturing” is available at www.stle.org: $39 to STLE members, $59 for all others. David Turner is a product specialist with the Lubricants Fluid Technology Group of CITGO Petroleum Corp. in Houston. He is a graduate of Lamar University in Beaumont, Texas, with a bachelor’s of science in chemical engineering. Turner has more than 35 years of experience in the lubricants industry in the areas of formulation, manufacturing, selection, application and technical service of lubricants and greases.
    [Show full text]
  • A Fresh Look at Lithium Complex Greases Part 1: How Did We Get Here?
    A Fresh Look at Lithium Complex Greases Part 1: How Did We Get Here? J. Andrew Waynick August 26, 2020 Overview of Presentation • Review of the lithium complex grease literature • Not exhaustive • But representative • Mountaintop flyover approach • Primarily taken from patent literature, published research papers, NLGI Lubricating Grease Guide, 6th Edition • Provides foundation for Part 2 presentation Beginnings • In 1942, five U.S. patents issued with Clarence E. Earle as inventor • Defined simple lithium soap thickened greases for subsequent decades • High temperature applicability limited, in part due to dropping point • Dropping point (D.P.) typically about 200 C • Shortly after the Earle patents issued, modifications to simple lithium soap greases began to be developed • The first ones did not increase D.P. , but did suggest directions in subsequent development that led to today’s lithium complex greases • A good discussion of these “pre-lithium complex” greases can be found in “A Brief History of Lubricating Greases” by Arthur T. Polishuk, Chapter 12C U.S. Patent No. 2,898,296 • Issued August 4, 1959; Pattendon, et. al., only months after the Earle patents expired • The first use of shorter chain dicarboxylic acids to produce higher dropping points • Used di-esters of sebacic acid (C10) or adipic acid (C6) • Longer chain monocarboxylic acid was stearic acid • Stearic acid and diester of dicarboxylic acid in base oil reacted with LiOH(aq), heated to about 204 C, then cooled and finished • Stearic/sebacic ratio = 2.1 (wt/wt) • D. P. ranged from 248 C to >260 C • When dicarboxylic acids used instead of esters: grainy product; D.P ~182 C • Likely reason was that the esters and/or transient alcohols acting as coupling agent • Enhanced “co-crystallization” of lithium stearate and di-lithium sebacate.
    [Show full text]
  • Grease-Oil Compatibility in Tribological Applications – Supergrease
    Grease-oil compatibility in tribological applications – Supergrease ANNA VON KRUSENSTIERNA Master Thesis in Materials Chemistry Chemical Engineering Faculty of Engineering, LTH Performed at ABB AB Corporate Research in Västerås, Sweden Lund University Supervisor ABB: Åke Öberg Supervisor LTH: Staffan Hansen Examiner LTH: Sven Lidin Grease – oil compatibility in tribological applications – Supergrease Master’s Thesis in Materials Science 30 ECTS credits Author: Anna von Krusenstierna Contact: [email protected] Centre for Analysis and Synthesis Department of Chemistry Lund University SE-221 00 LUND Sweden Tel: +46 (0) 46 – 222 00 00 ABB Corporate Research SE-72178 VÄSTERÅS Sweden Tel: +46 (0) 21 – 32 30 02 © Anna von Krusenstierna, June 2016 2 Abstract A common reason to malfunctioning of tap-changers is wear of tribological contacts. In order to reduce wear, it would be desirable to lubricate the contacts. Since the tap-changer is working in transformer oil, it is necessary that whatever lubricant is added is compatible with transformer oil. In this work, the compatibility of lubricating grease in transformer oil has been investigated. A wide variety of greases have been studied in order to understand what chemical properties that is desirable for this type of application. Compatibility tests of grease in transformer oil at 80°C have been performed. A ball-on-plate tribological test was performed on the successful grease candidates from the compatibility test. The successful candidates were also exposed to a vapour-phase dehydration process, in order to guarantee that the lubricant could be added to the transformer before delivering the tap-changer to clients. Finally, the transformer oil samples were analysed with FTIR, tan delta and surface tension measurements to evaluate if the greases had, by any means affected the oil.
    [Show full text]
  • United States Patent Office 2,600,058 Lubricant Containing Soap of Phos Phated: Hydroxy Fatty Acid Or
    Patented June 10, 1952 2,600,058 UNITED STATES PATENT OFFICE 2,600,058 LUBRICANT CONTAINING SOAP OF PHOS PHATED: HYDROXY FATTY ACID OR. GLYCEROE Edwin C. Knowles, Glenham,. Oney P. Puryear, Fishkil, and George W. Eckert, Glenham, N.Y., assignors to The. Texas Company, New York, N.Y., a corporation:of Delaware NoDrawing. Application March 9, 1949, Serial No. 80,574. 11. Claims. (C1.252-32.5) . 2 This invention relates to a lubricating: composi forming fatty material, phosphated: castor. oil tion and particularly a-lubricating grease: pre and phosphated hydrogenated castor oils are spe pared from a soap of a phosphated hydroxy fatty cifically mentioned. In the following descrip acid or glyceride. tion, phosphated castor oil will be specifically One of the principal objects of the present.in 5 discussed by way of preferred example, but it is vention is to provide a lubricating composition to be understood that the inventions applies in containing as an additive to improve the lubricat the same manner to the phosphated hydrogenat ing characteristics thereof a metal soap . of a ed castor oil and to the phosphated hydroxy fatty phosphated soap-forming hydroxy fatty acid. Or acids enumerated above. glyceride thereof, such as: phosphated castor oil 10 Castor oil contains the:glyceride of ricinoleic or phosphated hydrogenated castor oil. acid, an unsaturated hydroxy C18- acid, having Another object of the invention is to provide the-formula . a lubricating grease comprising an oleaginous-liq- OH luid lubricating, base containing a sufficient pro- - or in n-a- - - - --- portion of a soap of a phosphated hydroxy fatty lö CH(CH):CHCH-CH=CHCCH);coof acid or glyceride of this character to thicken the Phosphated castor oil has the phosphate:group lubricating base to a gel-like consistency.
    [Show full text]
  • GREASES Matrix Specialty Lubricants Bio Lubricants
    GREASES Matrix Specialty Lubricants Bio Lubricants Matrix Specialty Lubricants is a company based This group of products includes biodegradable hydraulic, gear, and other lubricants as well as a range of greases and concrete mould in The Netherlands, producing and marketing release agents. High performance, long life, low toxicity and biodegradabilty are key factors within this product group. specialty lubricants and greases. Compressor, Vacuum and Refrigeration Fluids Matrix Specialty Lubricants was created by a nucleus of industry specialists with a collective experience A comprehensive range of gas and refrigeration compressor fluids providing long life and low maintenance costs in combination with of many years working for major oil companies. high efficiency. The range consists of mineral, and synthetic (hydro treated, PAO, POE, Alkyl Benzenes, Di-Ester, Ester, PAG, PFPE) Our vision is to harness new technology and, with based lubricants with performance up to 12.000 hour drain intervals. the expertise of our chemists, provide the correct lubricant for each application. It is just a matter of knowledge. Food Grade Lubricants Specific product information is available in our A complete range of fluids, lubricants and greases for applications whenever a food grade lubricant is required. The high performance ® brochures and most of the technical data sheets Foodmax line is NSF and InS approved and includes a range of spray cans. can be found on our website; www.matrix-lubricants.com. Our main products are Industrial Specialty Products divided into groups with the most common being presented in our brochures. The most up to date This product group includes a range of specialty chain lubricants, gear oils, transformer oils and many more products.
    [Show full text]