US2968619A

US2968619A - Lubricant composition

Info

Publication number: US2968619A
Application number: US606585A
Authority: US
Inventors: Allan A Manteuffel; William D Gilson
Original assignee: Pure Oil Co
Current assignee: Pure Oil Co
Priority date: 1956-08-28
Filing date: 1956-08-28
Publication date: 1961-01-17
Anticipated expiration: 1978-01-17

Description

disadvantages.

United States Patent F LUBRICANT COMPOSITION Allan A. Manteulfel and William D. Gilson, Crystal Lake, 111., assignors to The Pure Oil Company, Chicago, Ill., a corporation of Ohio No Drawing. Filed Aug. 28, 1956, Ser. No. 606,585

6 Claims. (Cl. 252-333) This invention relates to lubricants and to lubricant additives, and more particularly to extreme pressure lubricants and to additives capable of imparting to mineral and other lubricating oils high load-carrying ability, and to their method of manufacture.

The use of chlorine-, sulfur-, and phosphorus-containing compositions as 13.1. lubricant additives is well nown. Each type of additive has its advantages and The halogen-containing additives, while capable of imparting high load-carrying characteristics to oils, have the disadvantage of being corrosive and hydrolyzing in service to form objectionable acids. The ability of sulfur to impart high load-carrying characteristics to a lubricating oil is dependent on the activity of the sulfur, which in turn is dependent on the tightness with which it is chemically bound in a compound. Elemental or loosely bound sulfur, while imparting high load-carrying characteristics, is too corrosive to be allowed to remain in an automotive differential or other gear assembly over a long. period of time. The same is true of the phosphorus sulfides. On the otherhand, sulfur and phosphorus sulfides when tightly bound chemically to organic compounds such as fatty acids, fatty esters, fatty alco hols and terpenes, impart excellent load-carrying characteristics to a lubricating oil and are substantially noncorrosive. However, additives of this type will not give the desired protection against wear to new gears during the initial break-in period. 7

An object of this invention is to provide an extreme pressure lubricant. Another object of this invention is to provide a composition which can be added to mineral and other lubricating oils to impart thereto extreme pressure characteristics. A further object of the invention is to provide a lubricant which will protect gears against Wear during the initial break-in period and during the subsequent running life of the gears. Still another object of the invention is to provide a composition which can be added to mineral oil and other types of lubricants to enable such lubricants to satisfactorily lubricate automotive gears during the initial break-in period and during the subsequent running life thereof. A still further object of the invention is to provide an extreme pressure lubricant which will satisfactorily lubricate gear assemblies during the initial break-in period and during the subsel quent running life thereof Without causing undue corrosion of the gear elements. Still another object is to provide a method for making the aforesaid compositions and lubricants.

Other objects of the invention will become manifest from the following detailed description of the invention.

We have discovered that by incorporating in alubrieating oi! sulfurized and phosphorized fatty material and free sulfur, sulfides of phosphorus and/or unstable organic polysulfides which liberate sulfur under service conditions, the lubricant will afford satisfactory protection and lubrication for the gear assembly during the initial break-in period and during the subsequent running life of the gears without producing harmful corrosion 2,968,619 Patented Jan. 17, 1961 thereof. During the initial break-in period the sulfur, in conjunction with thesulfurized-phosphorized fatty material, affords anti-weld protection to the gears. As the gear-tooth contact areas for load-carrying become established and as a lesser degree of anti-weld protection is required, the active sulfur or sulfur compound gradually reacts with the sulfurized-phosphorized fatty material to form a non-corrosive composition, and the resulting oil continues to impart to the oil extreme-pressure properties without causing undue corrosion.

As sulfurized and phosphorized compositions which are effective for the purpose of our invention we prefer sulfurized and phosphori zed fatty bodies such as those made in accordance with Whittier et al. Patent 2,211,306. As therein disclosed, such sulfurized and phosphorized fatty bodies are prepared by sulfurizing a fatty material such as vegetable, animal, or marine oils and waxes, including but not limited to wool grease, cotton seed, castor, rape seed, sperm and lard oils, and synthetic esters of high molecular weight, mono-unsaturated fatty acids (C C24), such as glyceryl trioleate, propylene glycol dioleate and butylene glycol dioleate, at a temperature of approximately 330-340" F. with elemental sulfur until a satisfactory copper strip test is obtained, and then phosphorizing the sulfurized material with a phosphorus sulfide, preferably phosphorus sesquisulfide, at a temperature of about 220230 F. until a satisfactory copper strip is obtained.

Instead of following the process setforth in the aforesaid Whi-ttier et al. patent, the initial sulfurization step may be terminated prior to the time a satisfactory copper strip test is obtained, that is, when the copper strip shows a tan color, and then phosphorized with a phosphorus sulfide for a sufficiently long period of time to more firmly bind the sulfur and phosphorus. This method is particularly effective where higher amounts of phosphorus sesquisulfide within the limits of those disclosed in the aforesaid patent are used in the phosphorization step. As a specific example, lard oil was mixed with 7.5% of sulfur and then was stirred with constantagit-ation in a kettle at a temperature of 325-340 F. Heating was continued for approximately four hours, at which time the copper strip gave a tan color upon immersion in a sample of the product at 300 F. for one minute. The mixture was then rapidly cooled to approximately 220 F., 0.8% by weight of phosphorus sesquisulfide was slowly added in finely divided form, and the reaction was allowed to continue at 220-230 F. for a period of eight hours, after which the mixture was rapidly cooled to F. and thereafter allowed to cool to room temperature. The final product contained 7.85% sulfur and 0.45% phosphorus by weight, and gave a tan color in the copper strip test at 220 F. for one minute.

In preparing sulfurized-phosphorized fatty materials in accordance with the method just described, the fatty material may be reacted with about 5 to 10% of sulfur in the first stage and with from about 0.4 to 5% of phosphorus sesquisulfide or equivalent amount of other phosphorus sulfide in the second stage. This method of preparing sulfurized-phosphorized fatty materials, in which sulfur is not tightly bound in the first stage and relatively largeamounts of phosphorus sulfide are reacted in the second stage, is disclosed and claimed in' the co -pending application of P. R. Chapman and A. Manteuffel, Serial NO. 553,419.

The sulfurized-phosphorized lard oil bases used'in the blends reported in the ensuing Table I were made as follows: I 4

Base (1) was made by heating 91.7 parts by weight of lard oil to 285, plus or minus 10 F., and then dusting in slowly with agitation 7.5 parts by weight of splfur. After the addition of the sulfur the temperature was vor more sulfur atoms in the molecule.

an ammonium or amine salt of sulfonic acids. "acids suitable for preparing the salts are the mahogany raised to 335, plus or minus F., and held at that level for four hours. At the completion of the heating period a copper strip was immersed in the bath for three minutes and was only slightly tarnished.

The temperature of the reaction mixture was then lowered to 220 F.,.plus or minus 5 F., and 0.8 part by weight of phosphorus sesquisulfide was slowly added. This temperature level was maintained for eight hours with continuous mechanical agitation of the reaction mixture. At the end of this period a copper strip immersed in the bath at 220 F. for three minutes gave a pink coating, indicating that the reaction was completed.

The sulfurized-phosphorized lard oil (2) of Table I was made by heating 92.5 parts of lard oil to 285, plus or minus F., and slowly dusting in 5 parts by weight of sulfur with continuous mechanical agitation. The

temperature of the batch was then raised to 335, plus or minus 5 F., and held for three hours. After this period of heating, a copper strip immersed in the bath for three minutes was lightly tarnished.

The temperature of the bath was then lowered to 220, plus or minus 5 F., and 2.5 parts by weight of phosphorus sesquisulfide was slowly dusted in. The batch was held at this temperature level for twelve hours with continuous stirring, that is, until a copper strip immersed in the bath for three minutes had a pink coating.

Sulfurized and phosphorized lard oil base (3) was made in the same manner as base (2) except 5% of phosphorus sesquisulfide was added instead of 2.5% and heating at 220, plus or minus 5 F., was continued for 18 hours, at which time a copper strip immersed in the bath for three minutes had a pinkish coating.

Instead of using elemental sulfur in conjunction with the sulfurized-phosphorized fatty material, we may add to the oil an unstable sulfur compound which will release elemental sulfur as, for example, dibenzyl trisulfide or other alkyl, aryl or arylalkyl polysulfides containing three A phosphorus sulfide such as phosphorus sesquisulfide suspended or dissolved in the mineral oil will also function to provide the anti-weld properties for which the elemental sulfur is added. If desired, both sulful and a phosphorus sulfide such as phosphorus sesquisulfide may be used in combination within the limits of the amounts specified above for sulfur. If a sulfur-liberating compound is used, it should be added in amounts sufficient to liberate the desired amount of sulfur.

In preparing lubricants in accordance with our invention, we have found that it is advantageous to add to the lubricant a substance which will promote the reaction of the sulfur with the sulfurized and phosphorized fatty oil or ester so as to shorten the break-in period or the period during which corrosive sulfur is present in the suitable for this purpose, we prefer lead naphthenate because of the additional load-carrying characteristics which it imparts to the oil during the break-in period.

We have further found that reduction of sulfur activity and corrosiveness of the gear oil can be still further accelerated by adding, as a fourth constituent of the oil, Sulfonic sulfouation of mineral lubricating oil stocks with sulfur trioxide, as well as sulfonic acids resulting from the sulfonation of pure hydrocarbons, such as substituted and unsubstituted naphthalene. A compound which has been found to be effective for this purpose is the ethylene diamine salt of dinonyl naphthalene sulfonic acid. Other sulfonates which are suitable are the ammonium salts of oil-soluble sulfonic acids obtained from the sulfonation of solvent-refined neutral oils with sulfur trioxide.

In preparing gear oils in accordance with our invention, the sulfur or active sulfur-containing compound is dissolved in a portion or all of the mineral oil at a temperature of about 270-290 F. After the addition of the sulfur or active sulfur compound is complete, the temperature of the oil is reduced to about 200 F. before adding the sulfurized-phosphorized fatty material. It is important to reduce the temperature to this level to avoid immediate or rapid reaction of the sulfur with the sulfurized-phosphorized fatty body. A suitable temperature of admixture of the sulfur-containing oil and the sulfurized-phosphorized fatty body is about -200 F.

The manner of mixing the several constituents together or the order in which they are admixed is not important, provided temperatures are properly adjusted to a level which will permit solution of the additives in the oil within a reasonable period of time without causing substantial reaction between the active sulfur and the sulfurized-phosphorized fatty material. The sulfurizedphosphorized fatty material, dibenzyl disulfide, naphthenate salt, and sulfonate salt, as well as other additives such as pour point depressors, V.I. improvers, and antifoam agents, may be added separately to the oil or may be admixed together and added as an admixture. They may be dissolved directly in the oil in which the sulfur or active-sulfur compound has been previously dissolved, or they may be admixed with a portion of the oil to which the sulfur or active-sulfur compound has not been added and this portion added to the portion containing the sulfur or active-sulfur compound. We prefer to add dibenzyl disulfide, or equivalent disulfide as disclosed in claims in Reissue Patent 22,911, in order to improve the load-carrying properties of the oil. We also, preferably, incorporate in the finished lubricant a sufficient amount of aromatic extract obtained in the solvent extraction of mineral lubricating oil fractions by means of phenol, furfural, nitrobenzene and equivalent solvents to prevent precipitation.

In order to realize the benefits of our invention, it is necessary to adjust the proportions of sulfurizedphosphorized fatty material and sulfur, or active-sulfur compound, so that the active sulfur is absorbed or inactivated by the sulfurized-phosphorized material and does not remain in the oil in a corrosive form over a long period of time. If the ratio of sulfur or activesulfur compound to sulfurized-phosphorized fatty material is too high, the sulfur will not be completely absorbed and the, corrosive condition of the gear oil will continue for an indefinite period of time with resultant harmful wear of the gear parts. Not only will the amount of sulfur which can be chemically absorbed be determined by the amount of the sulfurized-phosphorized fatty oil and other materials present, but also by the amount of sulfur bound in the sulfurized-phosphorized material. A sulfurized-phosphorized material containing a relatively low amount of bound sulfur as, for example, 5% by weight, enables the use of a larger amount of free sulfur or active sulfur-containing material than does a sulfurized-phosphorized material containing a higher amount as, for example, 10% of bound sulfur. In general, we have found that an amount of sulfur or equivalent active sulfur-containing compound between 1 and 50% of the quantity of sulfurized-phosphorized fatty material is effective in providing initial anti-weld characteristics to the oil during the break-in period and of being subsequently absorbed or reacted with the sulfurized-phosphorized fatty material to a substantially nn-c0rrosive state. We prefer an amount of sulfur equivalent to about 3 to 10% by weight of the sulfurizedphosphorized fatty material.

The amount of free sulfur or active sulfur-containing compatibility of the additives, particularly sulfurizedphosphorized lard oil, in the finished oil and to inhibit precipitation.

After the sulfur had been dissolved in a portion of material to be added will be determined to some extent the mineral oil the remainder of the oil was added, by the nature of the gears to be lubricated. For exresulting in cooling of the solution to below 200 F. ample, in the case of phosphate-coated gears the number Sulfurized-phosphorized. lard oil, dibenzyl disulfide, lead of miles required for breaking them in is probably not naphthenate and the ethylene diarm'ne salt of dinonyl sulmore than 100 and may be as low as 25 to 50. In such fonic acid were then added as indicated in the specific cases, therefore, it may be desirable to incorporate blends. During the addition of these additives, the oil smaller amounts of sulfur so that the sulfur will be was at atemperature between 160 and 200 F. The tembound in an inactive or non-corrosive form within a perature was maintained below 200 F. to avoid preshort period of time, probably not more than 24 hours. mature inactivation of the sulfur. On the other hand green gears, that is, gears which After all the constituents had been added to the oil, are not precoated, are usually considered to be broken the completed blends were placed in an oil bath at in after 500 miles of recommended driving speed. In 200 F. and subjected to a three minute copper strip such cases, sufficient sulfur should be present so that it test upon reaching bath temperature, i.e., in about a will not be completely bound before the end of the half-hour, Thereafter, the oil was maintained continuperiod required to drive 500 miles, which on an average ously at a temperature of 200 F. and subjected to the may be approximately one week. copper strip test after one hour, two hours, twenty-four The amount of sulfur required in the oil to furnish hours, and one week. The temperature of 200 F. was anti-weld protection during the necessary period of breakselected as representing the average temperature to which in can be approximated by subjecting an oil blend to the gear oils are subjected in service. The sulfurized and copper strip test, performed by immersing aclea n copper phosphorized lard oil used in the blends given in the strip for three minutes in the oil maintained at a temensuing table was made in the manner previously deperature of 210 F. The appearance of the strip after scribed in this application and covered in application this test provides an indication of the amount of cor- Serial No. 553,419, now U.S. Patent No. 2,910,438. In rosion which occurred and hence the extent to which the each case the period for sulfurization was four hours active sulfur has been bound in a non-active form. If v and the period for reacting the phosphorus sesquisulfide the color is light peacock or tan, the sulfur is substanwas eight hours. tially non-corrosive. As the color of the strip progresses From an examination of the table, the following conthrough medium peacock, light brown, medium brown, clusions can be reached: (1) by comparison of blends 1 mottled brown, brown-black and black, it indicates that and 2 it is seen that the gear oil was less corrosive after the oil is more and more corrosive.- one hours heating at 200 F. when it contained S,P In order to demonstrate the effectiveness of compolard oil in addition to sulfur than when it containedo-nly sitions made in accordance with our invention, a number sulfur alone; (2) by comparison of blends 2, 3 and 4 of blends were prepared and subjected to the copper it can be deduced that sulfurized and phosphorized lard strip corrosion test. The blends tested and thecorrosion oil containing a lesser amount of sulfur and a greater tests on each blend are given in the following table. 4 amount of phosphorus sesquisulfide chemically absorbs Blends were made by dissolving free sufur in approxithe active sulfur more rapidly than S--P lard oil containmately half of the total mineral oil, previously blended, ing a greater amount of sulfur and a lesser amount of at a temperature of 270-290 F. with stirring. The total phosphorus sesquisulfide; (3) by comparison of blends 1 mineral oil consisted of a blend of neutral oil, bright and 6 it can be deduced that dibenzyl disulfide has no stock and solvent extract. These three constituents were significant effect in reducing the corrosivity of the gear blended together to give the desired finished viscosity oil; (4) by comparison of blends 5 and 7 it is apparent and V1. The extract oil was used to insure complete that the lead naphthenate accelerated the absorption of Table I Blend No. Composition in parts by weight of gear oil Nesigtrfall oil, 200 SUS, viscosity at 100 F. 46.7-.-" 46.7".-- 46.7---" 40.7.-. 46.7-.-" 46.7"--. 46.7. Brggg siz oizk, 160-170 SUS, viscosity at 212 22.0.--" 22.0 22.0 22.0 22.0..-" 22.0..... 22.0. Phenol extract Suliur 0.3 S-P lard oil 9.0 Dibenzyl di fi 0.8 .l Lead naphthenate (30% Pb) Ethylenediamine dinonyl naphthalene vsulloriiate.

ittite F R19 934 1 945 s97 771 983 9 1 887. at 130 330.23-..- 386.1,.-. 387.65-..- 390.2 3725-..- 31121..-. 4062.- 346.6 3901.... 370. at210 74.4"-.- 83.5-.-" s5.5 s4.3 82.4..." 72.9-- s5.1 .19..." 83.8..... 82.0. Viscosity Index 81 92 96. 9' 93. 82 l 93.0 3 Min. Cu strip test, upon reaching bath loose mottled flaky gray mottled brown brown black. medium brown temp. (200 F.). black black black black brown. black black brown black 3 Min. Cu strip test, after 1 hr. at 200 F--- do.. .do do. dodo -do do loose medium Do.

black. pea}; C00 3 Min. Cu strip test, after 2hr. at 200 F.-. do -.do .do.. do do do... mggirlmn do.-. do Do. 3 Min. Cu strip test after 24 hr at 200 F do do mottled mottled do do do do do Do.

brown. brown. 3Min. Cu strip test,aiter lweek at 200 F.. do.. -do do medium do do light do. tan Do.

brown. brown.

1 Suliurized and phosphortzcd lard oil made by reacting 91.7% lard oil, 7.5% S and 0.8% P48 2 Sulturized and phosphorized lard oil made by react ng 92.5% lard 911, 5.0% S and 2.5% P 8 5 Suliurized and phosphorized lard oil made by reacting 90% lard 011, 5.0% S and 5.0% ns the active sulfur into a non-corrosive state; (5) by comparison of blends 7 and 8 it is evident that in the absence of the SP lard oil the lead naphthenate was ineffective to accelerate the absorption of the active sulfur; (6) comparison of blends 7 and 9 indicates that the ethylene diamine salt of dinonyl sulfonic acid further accelerated the absorption of the active sulfur so that at the end of one week the product obtained was substantially noncorrosive.

Although the blends were all prepared using sulfurizedphosphorized lard oil with or without lead naphthenate and .the ethylene diamine salt of dinonyl sulfonic acid,

other fatty oils or esters of high molecular weight fatty acids may be used in place of lard oil in making the sulfurized-phosphorized additive, as previously set forth. Likewise, other naphthenates and amine salts of sulfonic acids can be used in place of the specific salt used in the specific blends.

The amount of sulfurized and phosphorized fatty material in the blend may range from about 5 to 20% by weight and the amount of dibenzyl disulfide which may be used in the blends may vary within the limits disclosed in Reissue Patent 22,911, but preferably between 0.5 and 2% The amount of naphthenate salt effective to accelerate the reaction of sulfur with the sulfurizedphosphorized lard oil may vary between approximately 0.1 and 5% by weight of the gear oil blend. The amount of ammonium or amine salt of sulfonic acid required to accelerate the reaction will be dependent on the particular compound chosen, the amount of active sulfur present, and the desired rate of sulfur inactivation. In general, amounts between 0.1 and 5% of the total gear oil blend are effective.

The amount of solvent extract in the blend may vary from to 100% of the mineral oil portion,,depending upon the desired V.I. and the compatibility characteristics of the finished 'blend. In general, amounts from to 30% will prevent precipitation and at the same time give an oil with a commercially desirable V.I. The solvent extract used in the blends reported in the foregoing table had the following characteristics:

Any solvent extract of high aromaticity (above 50%), obtained by extraction of mineral lubricating oil fractions with solvents selective for separating parafiinic from aromatic hydrocarbons, may be used in place of the specific extract used in preparing the blends given in the foregoing table.

We claim as our invention:

1. A lubricant composition characterized by initiall high antiweld properties and decreasing corrosivity with extended use at elevated temperatures, consisting essentially of a petroleum lubricating oil, sufficient amount of a sulfurized-phosphorized fatty material, in the range from about 5-20 percent wt. of the composition to enhance the load-carrying properties of the oil, said sulfurized-phosph-orized fatty material being prepared by heating at least one ester of a non-drying high-molecularweight fatty acid with 5-10 percent wt. of sulfur at 325-340 F. until a tan copper strip end-point is obtained after one minute immersion of a copper strip at 300 F., then heating the sulfurized ester with 0.4-5 percent wt. of phosphorus sesquisulfide at 220-230 F. until a tan copper strip end-point is obtained after one minute immersion of a copper strip at 220 R, an amount of elemental sulfur in the range from about l-50 percent wt. of the sulfurized-phosphorized fatty material sufficient to enhance the antiweld properties of the composition but not in excess of that amount which can react with the sulfurized-phosphorized fatty material to the extent necessary to convert the sulfur to a substantially non-corrosive form upon extended use, and an amount of a naphthenate salt, in the range from about 0.1-5

' percent wt. of the composition, sufficient to accelerate the API gravity 13.2 COC flash, F. 550 C00 fire, F. 640 SUS viscosity:

at 100 F. 34,000

at 150 F. 2,824

at 210 F. 404 Viscosity Index 17 Pour pt., F. +65 Carbon res.(Conradson) 4.23 Sulfur, total, percent w 2.39 Neut. No. (ASTM D974) 2.8

reaction of the sulfur with the sulfurized-phosphorized fatty material.

2. A lubricant composition in accordance with claim 1 in which the naphthenate salt is lead naphthenate.

3. A lubricant composition in accordance with claim 1 which contains a substance from the group consisting of ammonium and amine salts of sulfonic acids in an amount, in the range from about 0.1-5 percent wt. of the composition, sufficient to accelerate the reaction of sulfur and sulfurized-phosphorized fatty material.

4. A lubricant composition in accordance with claim 1 in which the petroleum lubricating oil contains 9 percent wt. of sulfurized-phosphorized lard oil, 0.8 'percent wt. of dibenzyl disulfide, 0.3 percent wt. of sulfur, about 4 percent wt. of lead naphthenate, and sufiicient aromatic extract obtained in the solvent extraction of mineral lubricating oil fractions to prevent precipitate of the aforesaid constituents from the lubricant composition.

5. A lubricant composition in accordance with claim 3 in which the sulfonic acid salt is the ethylene diamine salt of dinonyl naphthalene sulfonic acid.

6. A lubricant composition in accordance with claim 4 containing about 1 percent wt. of the ethylene diamine salt of dinonyl naphthalene sulfonic acid.

References Cited in the file of this patent UNITED STATES PATENTS 2,212,899 Flaxman Aug. 27, 1940 2,322,209 Prutton June 22, 1943 2,382,115 Stucker Aug. '14, 1945 2,480,873 Musselman Sept. 6, 1949 2,580,005 Cyphers Dec. 25, 1951 OTHER REFERENCES ASTM Standards on Petroleum Products and Lubricants, pub. by ASTM, Phila., Pa. November 1956 pages -94.

Georgi, Motor Oils and Engine Lubrication, Reinhold Pub. Corp., 1950, pages 20, 180 and 181.

Claims

1. A LUBRICANT COMPOSITION CHARACTERIZED BY INITIALLY HIGH ANTIWELD PROPERTIES AND DECREASING CORROSIVITY WITH EXTENDED USE OF ELEVATED TEMPERATURES, CONSISTING ESSENTIALLY OF A PETROLEUM LUBRICATING OIL, SUFFICIENT AMOUNT OF A SULFURIZED-PHOSPHORIZED FATTY MATERIAL, IN THE RANGE FROM ABOUT 5-20 PERCENT WT. OF THE COMPOSITION TO ENHANCE THE LOAD-CARRYING PROPERTIES OF THE OIL, AND SULFURIZED-PHOSPHORIZED FATTY MATERIAL BEING PREPARED BY HEATING AT LEAST ONE ESTER OF A NON-DRYING HIGH-MOLECULARWEIGHT FATTY ACID WITH 5-10 PERCENT WT. OF SULFUR AT 325*-340*F. UNTIL A TAN COPPER STRIP END-POINT IS OBTAINED AFTER ONE MINUTE IMMERSION OF A COPPER STRIP AT 300*F., THEN HEATING THE SULFURIZED ESTER WITH 0.4-5 PERCENT WT. OF PHOSPHORUS SESQUISULFIDE AT 200*-230*F. UNTIL A TAN COPPER STRIP END-POINT IS OBTAINED AFTER ONE MINUTE IMMERSION OF A COPPER STRIP AT 220*F., AN AMOUNT OF ELEMENTAL SULFUR IN THE RANGE FROM ABOUT 1-50 PERCENT WT. OF THE SULFURIZED-PHOSPHORIZED FATTY MATERIAL SUFFICIENT TO ENHANCE THE ANTIWELD PROPERTIES OF THE COMPOSITION BUT NOT IN EXCESS OF THAT AMOUNT WHICH CAN REACT WITH THE SULFURIZED-PHOSPHORIZED FATTY MATERIAL TO THE EXTENT NECESSARY TO CONVERT THE SULFUR TO A SUBSTANTIALLY NON-CORROSIVE FORM UPON EXTENDED USE, AND AN AMOUNT OF NAPHTHENATE SALT, IN THE RANGE FROM ABOUT 0.1-5 PERCENT WT. OF THE COMPOSITION, SUFFICIENT TO ACCELERATE THE REACTION OF THE SULFUR WITH THE SULFURIZED-PHOSPHORIZED FATTY MATERIAL.