US3095376A - Grease composition and process for its preparation - Google Patents
Grease composition and process for its preparation Download PDFInfo
- Publication number
- US3095376A US3095376A US852979A US85297959A US3095376A US 3095376 A US3095376 A US 3095376A US 852979 A US852979 A US 852979A US 85297959 A US85297959 A US 85297959A US 3095376 A US3095376 A US 3095376A
- Authority
- US
- United States
- Prior art keywords
- grease
- weight
- oil
- clay
- borate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000004519 grease Substances 0.000 title claims description 42
- 239000000203 mixture Substances 0.000 title claims description 42
- 238000000034 method Methods 0.000 title description 11
- 230000008569 process Effects 0.000 title description 11
- 238000002360 preparation method Methods 0.000 title description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 21
- 239000004927 clay Substances 0.000 claims description 20
- 235000007586 terpenes Nutrition 0.000 claims description 19
- VKCLPVFDVVKEKU-UHFFFAOYSA-N S=[P] Chemical compound S=[P] VKCLPVFDVVKEKU-UHFFFAOYSA-N 0.000 claims description 15
- 229910052783 alkali metal Inorganic materials 0.000 claims description 12
- GIWKOZXJDKMGQC-UHFFFAOYSA-L lead(2+);naphthalene-2-carboxylate Chemical compound [Pb+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 GIWKOZXJDKMGQC-UHFFFAOYSA-L 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000010687 lubricating oil Substances 0.000 claims description 10
- 150000003505 terpenes Chemical class 0.000 claims description 7
- 230000005661 hydrophobic surface Effects 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- -1 alkali metal borate Chemical class 0.000 description 31
- 235000010339 sodium tetraborate Nutrition 0.000 description 20
- 229910021538 borax Inorganic materials 0.000 description 19
- 239000004328 sodium tetraborate Substances 0.000 description 19
- 239000003921 oil Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
- 239000011593 sulfur Substances 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 10
- 239000000725 suspension Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 125000002091 cationic group Chemical group 0.000 description 5
- 238000010348 incorporation Methods 0.000 description 5
- 239000000314 lubricant Substances 0.000 description 5
- 230000001050 lubricating effect Effects 0.000 description 5
- 239000012053 oil suspension Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000001993 wax Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 2
- 150000001642 boronic acid derivatives Chemical class 0.000 description 2
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000003349 gelling agent Substances 0.000 description 2
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 2
- 229910000271 hectorite Inorganic materials 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000010688 mineral lubricating oil Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 241000894007 species Species 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000005069 Extreme pressure additive Substances 0.000 description 1
- 239000001293 FEMA 3089 Substances 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical class NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- GTVWRXDRKAHEAD-UHFFFAOYSA-N Tris(2-ethylhexyl) phosphate Chemical compound CCCCC(CC)COP(=O)(OCC(CC)CCCC)OCC(CC)CCCC GTVWRXDRKAHEAD-UHFFFAOYSA-N 0.000 description 1
- FZQSLXQPHPOTHG-UHFFFAOYSA-N [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 Chemical compound [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 FZQSLXQPHPOTHG-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- 229930006739 camphene Natural products 0.000 description 1
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 159000000006 cesium salts Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- FYSNRPHRLRVCSW-UHFFFAOYSA-N dodecasodium;tetraborate Chemical class [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-] FYSNRPHRLRVCSW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 125000005608 naphthenic acid group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000003854 p-chlorophenyl group Chemical group [H]C1=C([H])C(*)=C([H])C([H])=C1Cl 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- JVUYWILPYBCNNG-UHFFFAOYSA-N potassium;oxido(oxo)borane Chemical compound [K+].[O-]B=O JVUYWILPYBCNNG-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical class [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/04—Reaction products of phosphorus sulfur compounds with hydrocarbons
-
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- C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
-
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/082—Inorganic acids or salts thereof containing nitrogen
- C10M2201/083—Inorganic acids or salts thereof containing nitrogen nitrites
-
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/085—Phosphorus oxides, acids or salts
-
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/087—Boron oxides, acids or salts
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
-
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/16—Naphthenic acids
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/34—Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
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- C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2211/06—Perfluorinated compounds
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- C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2211/08—Halogenated waxes
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- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/02—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen and halogen only
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- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
- C10M2215/065—Phenyl-Naphthyl amines
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/08—Amides
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/08—Amides
- C10M2215/082—Amides containing hydroxyl groups; Alkoxylated derivatives
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/12—Partial amides of polycarboxylic acids
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- C10M2215/26—Amines
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- C10M2215/28—Amides; Imides
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- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/046—Polyamines, i.e. macromoleculars obtained by condensation of more than eleven amine monomers
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- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/042—Metal salts thereof
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/12—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions obtained by phosphorisation of organic compounds, e.g. with PxSy, PxSyHal or PxOy
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- C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2225/04—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions obtained by phosphorisation of macromolecualr compounds not containing phosphorus in the monomers
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- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/02—Esters of silicic acids
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- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/061—Esters derived from boron
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- C10N2010/00—Metal present as such or in compounds
- C10N2010/08—Groups 4 or 14
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/02—Bearings
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
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- C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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- C10N2040/241—Manufacturing joint-less pipes
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- C10N2040/243—Cold working
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- C10N2040/245—Soft metals, e.g. aluminum
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- C10N2040/244—Metal working of specific metals
- C10N2040/246—Iron or steel
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
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- C10N2040/247—Stainless steel
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- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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- C10N2070/00—Specific manufacturing methods for lubricant compositions
Definitions
- This invention relates to improved lubricating grease compositions. More particularly, the invention relates to greases gelled with oleophilic clays and containing a combination of extreme pressure additives as well as a process for the preparation of said grease.
- Plastic lubricating compositions suit-able for general use throughout the mechanical arts should possess good lubricating properties and, for heavy duty use, should also inherently possess extreme pressure characteristics when operated in either a dry or wet environment. The latter condition is particularly prevalent in such industrial uses as steel rolling mill applications and the like.
- greases gelled with oleophilic clays can be improved with respect to their extreme pressure properties even under wet conditions as Well as dry by the combination therein of an alkali metal borate and a phosphorus and sulfur reaction prod uct ofan olefinic hydrocarbon, especially a terpene, and a phosphorus sulfide.
- a process for the preparation of such compositions which comprises separately forming a substantially anhydrous oleophilic clay grease oomposition and a substantially anhydrous oil suspension of the alkali metal bora-te in particulate form and commingling the bor-ate-oil suspension and the grease compositiomthe phosphorus sulfide-olefin reaction product preferably being added after incorporation of the alkali metal borate.
- the subject grease compositions contain additive amounts of one or more lead soaps (particularly a lead napthenate), with or without a chlorinated aryl disulfide and/or a chlorinated hydrocarbon, all as more particularly described hereinafter.
- alkali metal bor-ate which may be used in the compositions of this invention include particularly the sodium borates (both hydrated and anhydrous) and including sodium meta-borate and sodium tetraborates, of which the preferred species is borax.
- Potassium bo-r-ate may be utilized, such as potassium meta-borate and potassium tetraborate.
- the corresponding lithium or cesium salts may be employed in addition to or in place of the potassium or sodium salts. These are to be utilized in the form of finely divided particles, the more finely divided the better but no critically limited particle size has been established.
- the borates should be employed in amounts between about 2 and about 10% by weight, based on the total grease composition, preferably between about 2.5 and 4.5 by weight thereof.
- finely divided borax is suspended in the water-insoluble lubricating oil prior to incorporation in the substantially anhydrous grease composition.
- This is a relatively simple operation, but care must be exercised to Wet as effectively as possible the surfaces of the finely divided borate with the lubricating oil.
- This can be accomplished by slowly adding the oil to the borax with vigorous stirring.
- the suspension contain 0.252.5 parts of the ho-rate for each part by weight of the lubricating oil in which it is suspended. While the suspending operation may be conducted at about room temperature it may be desirable to warm the oil to a temperature between room temperature and about F. for the purpose of lowering the viscosity of the oil, thereby facilitating mixing of the powdered borate and the oil if this is necessary.
- the substantially anhydrous. grease composition with which the oil suspension of the alkali metal borate is cornmingled may be well known in the art wherein the principal gelling agent present is an olephilic clay, preferably an oleophilic montmorillinitic clay, such as b-entonite or hectorite.
- the oleophilic character of the clay grease gelling agent is imparted thereto by reacting with or adsorbing on the clay surface a cationic oleophilic surface aotive agent, particularly relatively highmolecular weight amines, amino amides, or quaternary ammonium compounds, all of which are known in the art.
- the clays which are useful as startingmaterials for making the modified oleophilic clay in accordance with these known principles are those exhibiting substantially base exchange properties, and particularly those exhibiting com arativel high base exchan e ro erties and conas those referred to in US. Patent 2,531,427, issued to E. A. Hauser. Suitable cationic materials for adsorption on clays are described in numerous patents including U.S. 2,831,809 and 2,875,152. The clays are normally converted to a satisfactory oleophilic form by the use of 0.25-
- the oil ingredient in the greases provided by this invention may be any of the oils of lubricating grade customarily used in compounding greases.
- the oil may be a refined, unrefined or semi-refined, parafiinic, naphthenic or asphaltic base mineral oil having a viscosity of from about 50 to about 4000 SUS at 100 F.
- Synthetic lubricants may be employed in place of, or in addition to the mineral oils. The various classes of synthetic lubricants are Well known in the art and do not require detailed description here.
- Typical classes of such lubricants include phosphates, such as tris(2-ethylhexyl)phosphate, dicarboxylates, such as bis(2-ethylhexyl)sebacate and corresponding silicates and borates.
- phosphates such as tris(2-ethylhexyl)phosphate
- dicarboxylates such as bis(2-ethylhexyl)sebacate and corresponding silicates and borates.
- the agent cooperating with the borax for the preservation of extreme pressure properties under wet operating conditions is preferably prepared by reaction at temperatures between about 100 and about 160 of a phosphorus sulfide and a bicyclic terpene or a material predominantly comprised of a bicyclic terpene. All of the phosphorus sulfides, such as P 8 P 8 P P 8 P 8 etc. are contemplated as reactants in the preparation of these reaction products but P 8 is particularly preferred.
- the designation bicyclic terpene refers to those terpenes which are characterized by the presence of one double bond in the molecule and built up of a two-rings system. Illustrative of such compounds are pinene, camphene and fenchene. Typical oils containing such materials are turpentine oil, the major constituent of which is pinene. i
- reaction product contains phosphorus and sulfur in substantially the same amounts and ratios as in the particular phosphorus sulfide reacted with the terpene. It would, therefore, appear that the reaction is one of addition, that is, addition of phosphorus sulfide at a site of unsaturation present in the terpene.
- the proportions of reagents used in the preparation of these reaction products may be varied in order to obtain reaction products having different degrees of oil-solubility, tailored to meet the solubility characteristics of the oil or grease employed.
- Suitable ratios for most purposes contemplated are 1 mole of phosphorus sulfide for 3-5 moles of bicyclic I terpene.
- the olefin-phosphorus sulfide reaction product is preferably employed in amounts between about 0.5% and about 5% by weight based on the total grease composition.
- the additive is preferably incorporated in the greases subsequent to addition of borax. Conveniently, however, it is added to the composition subsequent to dehydration and prior to milling of the composition for the purpose of creating a suitable grease structure.
- alkali metal borate with the phosphorusand sulfur-containing reaction products with a bicyclic terpene cures the water sensitivity of borax when contained in grease but does not provide the grease composition with maximum extreme pressure properties.
- These are substantially improved by the further incorporation of a lead naphthenate to the extent of 0.25-2% based on the total weight of the grease.
- the improvement in extreme pressure properties without damage to the grease structure is a surprising feature of the invention in view of the mild extreme pressure properties which lead naphthenate exhibits in the absence of other materials.
- lead naphthenate hardened the unworked penetration of a grease so that an unduly wide spread occurred between unworked and worked penetrations.
- Lead naphthenates are materials well known in the art and may be prepared by reaction of lead compounds with naphthenic acids such as those obtained from certain American crudes, especially those obtained from California. These acids are obtained as mixtures and have average molecular weights of about 250 or higher.
- a lead oxide such as litharge
- the proportion of lead is in the order of 25-35% and it is preferred to make the lead naphthenate from the oxide instead of utilizing other lead salts although these, such as carbonates, may be employed, if desired.
- Still further improvements in the extreme pressure properties of the described class of greases is effected by the addition of a chlorinated diaryl disulfide.
- a chlorinated diaryl disulfide This may contain about 10% chlorine, although both larger and smaller percentages may be used.
- Bis(parach1orobenzyl) disulfide is the preferred species but other corresponding compounds may be utilized such as bis(paraphenyl)disulfide, bis(metachloroparatolyl)disulfide and the corresponding chlorinated xylene disulfides, as well as mixed disulfides such as paria-chloro benzyl and para-chloro phenyl disulfide. These materials are preferably employed in amounts between about 0.25 and 2.5% by weight of the total grease composition.
- Chlorinated waxes higher molecular weight hydrocarbons, such as paratfins, may be employed in place of or in addition to the chlorinated diaryl disulfide.
- the chlorinated waxes are preferably chlorinated parafiin Wax containing from 20 to 50% chlorine, preferably from 30 to 45% by Weight.
- Corresponding chlorinated rubber may be used.
- Example 1 Formula. percent w. Sample A Sample B Hectorite clay 4. 90 5.03 Amide of 'lctraethylenepentamine and tall oil acids 3. 69 3.79 Phosphoric Acid 0. 40 0. 41 Sodium Nitrite 0. 46 0. 47 Ihenyl-alpha-na-phthylamine 0. 46 0. 47 Borax (Impalpable Powder) r. 3. 3.00 Pass-turpentine Reaction Product. 2.00 Lead Naphthenate 0.50 Lubricating Oil 84. 59 86.83
- Example II vBy adding the borax as an oil-borax mixture a subrnicron size dispersion Was obtained, no plating out Was experienced during homogenizing or in bearing tests, and the grease was excellent in all respects, as long as the borax comprised at least 65% by weight of particles having less than 50 micron diameters. If the proportion of larger particles is greater than about 35%, it is p neferred that the oil suspension of the borate be added to the grease at an elevated temperature and the resulting mixture stirred for 1560 minutes at 200-300 F. in order to obtain maximum dispersion.
- a grease composition comprising a major proportion of a lubricating oil, a grease-forming proportion of a colloidally dispersed clay, said clay being Waterproofed with a cationic hydrophobic surface active agent, 210% by weight of an alkali metal borate, at least 65% by weight of said borate being particles having diameters of less than 50 microns, O.252% by weight of a lead naphthenate and 0.55% by Weight of a phosphorusand sulfur-containing reaction product obtained b reaction of a bicyclic terpene and a phosphorus sulfide.
- a grease composition comprising a major proportion of a mineral lubricating oil, a grease-forming proportion of a colloidally dispersed clay, said clay being Waterproofed with a cationic hydrophobic surface active agent, 210% by weight of borax, 0.252% by weight of a lead naphth-enate and 0.5-5% by Weight of a phosphorusand sulfur-containing reaction product obtained by reaction of a bicyclic terpene and a phosphorus sultide, at least 65 by weight of borax having particle size diameters of less than 50 microns.
- a 'borax-oil suspension is formed and dispersing the suspension in a substantially anhydrous oleophilic clay grease composition by mixing followed by milling, said composition containing 0.252% by Weight of a lead naphthenate and 0.55% by Weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide, at least by weight of borax having particle size diameters of less than 50 microns.
- a substantially anhydrous composition of grease-forming components comprising a major proportion of a mineral lubricating oil, a grease-forming proportion of an organophilic montmorillonite clay 0.252% by weight of a lead napthenate and 0.55% by weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide; separately forming a substantially anhydrous lubricating oil suspension of 025-25 parts particulate alkali metal borate per part by Weight of oil, :at least 65 by Weight of said borate being particles having diameters of less than 50 microns; and commingling the composition and suspension.
- a substantially anhydrous composition of grease-forming components comprising a major proportion of a lubricating oil, 0.'25-2% by Weight of a lead naphthenate, a grease-forming proportion of an organophilic montmorillonite clay and 0.5-5% by Weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide; separately forming a substantially anhydrous lubricating oil suspension of 0.25-2.5 parts particulate alkali metal borate per part by weight of oil, at least 65 by weight of said borate being particles having diameters of less than 50 microns; and :commingling the composition and suspension.
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Description
. proved grease compositions.
United States Patent 3,tl95,376 GREASE COMPOSETEON AND PROCESS FOR ITS PREPARA'HON Harvey E. Hook, Danville, and Harold A. Woods,
Martinez, Calii., assignors to Shell Gil Company, a corporation of Deiaware No Drawing. Filed Nov. 16, 1959, Ser. No. 852,979 a 6 Ciaims. (ill. 252-28) This invention relates to improved lubricating grease compositions. More particularly, the invention relates to greases gelled with oleophilic clays and containing a combination of extreme pressure additives as well as a process for the preparation of said grease.
Plastic lubricating compositions suit-able for general use throughout the mechanical arts should possess good lubricating properties and, for heavy duty use, should also inherently possess extreme pressure characteristics when operated in either a dry or wet environment. The latter condition is particularly prevalent in such industrial uses as steel rolling mill applications and the like.
It has been possible in the past to formulate clay grease compositions having good resistance to leaching by water as well as having desirable mechanical characteristics. The ability to operate under extreme loading, however, has not been satisfactorily obtained by the use of most Well known extreme pressure agents such as are employed in oil and grease compositions. The addition of certain inorganic oil-insoluble materials to grease-s for this purpose has been suggested, but it has been found in practice that if they impart any load bearing capacity to the grease this is at a maximum only when the latter is employed in substantially anhydrous environments. Once water is incorporated in the grease, either purposely or accidently, the
. those originally added. This causes the formation of a film (plating out) of the oil-insoluble additive on machinery being lubricated with the composition. Agglomeration of the particles on the other hand causes clogging of screens, plugging of lines and valves of centralized dispensing systems, and the impartingof a grittiness to the composition which is a disadvantageous feature.
It is an object of the present invention to provide im- It is a particular object of the invention to provide a process for the preparation of such compositions. It is a further particular object to provide improved clay grease compositions having extreme pressure properties not only under anhydrous conditions but under wet operating conditions as well. Other objects will become apparent from the following detailed description of the invention. t
Now, in accordance with the present invention, greases gelled with oleophilic clays can be improved with respect to their extreme pressure properties even under wet conditions as Well as dry by the combination therein of an alkali metal borate and a phosphorus and sulfur reaction prod uct ofan olefinic hydrocarbon, especially a terpene, and a phosphorus sulfide. Still in accordance with this inventiona process is provided for the preparation of such compositions which comprises separately forming a substantially anhydrous oleophilic clay grease oomposition and a substantially anhydrous oil suspension of the alkali metal bora-te in particulate form and commingling the bor-ate-oil suspension and the grease compositiomthe phosphorus sulfide-olefin reaction product preferably being added after incorporation of the alkali metal borate. Still in accordance with a preferred aspect of the invention,
more substantial improvements in extreme pressure properties are encountered when the subject grease compositions contain additive amounts of one or more lead soaps (particularly a lead napthenate), with or without a chlorinated aryl disulfide and/or a chlorinated hydrocarbon, all as more particularly described hereinafter.
Examples of the alkali metal bor-ate which may be used in the compositions of this invention include particularly the sodium borates (both hydrated and anhydrous) and including sodium meta-borate and sodium tetraborates, of which the preferred species is borax. Potassium bo-r-ate may be utilized, such as potassium meta-borate and potassium tetraborate. The corresponding lithium or cesium salts may be employed in addition to or in place of the potassium or sodium salts. These are to be utilized in the form of finely divided particles, the more finely divided the better but no critically limited particle size has been established. The borates should be employed in amounts between about 2 and about 10% by weight, based on the total grease composition, preferably between about 2.5 and 4.5 by weight thereof.
In accordance with the preferred process for the preparation of such greases, finely divided borax is suspended in the water-insoluble lubricating oil prior to incorporation in the substantially anhydrous grease composition. This is a relatively simple operation, but care must be exercised to Wet as effectively as possible the surfaces of the finely divided borate with the lubricating oil. This can be accomplished by slowly adding the oil to the borax with vigorous stirring. It is preferred that the suspension contain 0.252.5 parts of the ho-rate for each part by weight of the lubricating oil in which it is suspended. While the suspending operation may be conducted at about room temperature it may be desirable to warm the oil to a temperature between room temperature and about F. for the purpose of lowering the viscosity of the oil, thereby facilitating mixing of the powdered borate and the oil if this is necessary.
The substantially anhydrous. grease composition with which the oil suspension of the alkali metal borate is cornmingled may be well known in the art wherein the principal gelling agent present is an olephilic clay, preferably an oleophilic montmorillinitic clay, such as b-entonite or hectorite. The oleophilic character of the clay grease gelling agent is imparted thereto by reacting with or adsorbing on the clay surface a cationic oleophilic surface aotive agent, particularly relatively highmolecular weight amines, amino amides, or quaternary ammonium compounds, all of which are known in the art.
The clays which are useful as startingmaterials for making the modified oleophilic clay in accordance with these known principles are those exhibiting substantially base exchange properties, and particularly those exhibiting com arativel high base exchan e ro erties and conas those referred to in US. Patent 2,531,427, issued to E. A. Hauser. Suitable cationic materials for adsorption on clays are described in numerous patents including U.S. 2,831,809 and 2,875,152. The clays are normally converted to a satisfactory oleophilic form by the use of 0.25-
1.5 parts by weight of the cationic material for each part by weight of the degangued clay.
The oil ingredient in the greases provided by this invention may be any of the oils of lubricating grade customarily used in compounding greases. The oil may be a refined, unrefined or semi-refined, parafiinic, naphthenic or asphaltic base mineral oil having a viscosity of from about 50 to about 4000 SUS at 100 F. Synthetic lubricants may be employed in place of, or in addition to the mineral oils. The various classes of synthetic lubricants are Well known in the art and do not require detailed description here. Typical classes of such lubricants include phosphates, such as tris(2-ethylhexyl)phosphate, dicarboxylates, such as bis(2-ethylhexyl)sebacate and corresponding silicates and borates.
The incorporation of an alkali metal borate in the described class of oleophilic clay greases imparts a surprising amount of load carrying ability and, even more unexpected, oxidation resistance, to the compositions when they are operated in the virtual absence of water. However, it has been found that when water is present, such as may occur, for example, in wheel bearings under wet driving conditions or in steel mill rolling lubricants, the lubricating characteristics of the grease are maintained but the extreme pressure properties are seriously degraded. Hence, the prime objective of this invention is to overcome this disadvantageous reduction in extreme pressure properties by borate-containing greases in the presence of water. It has been discovered that this feature is overcome by the presence in the grease, together with the borate, of a phosphorusand sulfur-containing reaction product formed between an olefin hydrocarbon of at least 8 carbon atoms, and particularly a cyclic olefin such as a terpene, and a phosphorus sulfide.
The agent cooperating with the borax for the preservation of extreme pressure properties under wet operating conditions is preferably prepared by reaction at temperatures between about 100 and about 160 of a phosphorus sulfide and a bicyclic terpene or a material predominantly comprised of a bicyclic terpene. All of the phosphorus sulfides, such as P 8 P 8 P P 8 P 8 etc. are contemplated as reactants in the preparation of these reaction products but P 8 is particularly preferred. As used herein, the designation bicyclic terpene refers to those terpenes which are characterized by the presence of one double bond in the molecule and built up of a two-rings system. Illustrative of such compounds are pinene, camphene and fenchene. Typical oils containing such materials are turpentine oil, the major constituent of which is pinene. i
Although a complete understanding of the chemical composition of the reaction products of phosphorus sulfides and bicyclic terpenes has not been achieved at this time, a partial understanding of their composition may be obtained by noting the characteristics involved in the reaction. For example, the reaction is exothermic and the viscosity increases appreciably during reaction. Little, if any hydrogen sulfide is evolved. Therefore, the reaction product contains phosphorus and sulfur in substantially the same amounts and ratios as in the particular phosphorus sulfide reacted with the terpene. It would, therefore, appear that the reaction is one of addition, that is, addition of phosphorus sulfide at a site of unsaturation present in the terpene.
(The proportions of reagents used in the preparation of these reaction products may be varied in order to obtain reaction products having different degrees of oil-solubility, tailored to meet the solubility characteristics of the oil or grease employed. In this regard, it is preferred that about one mole of phosphorus sulfide be reacted with four moles of a bicyclic terpene in order to obtain a reaction product relatively soluble in ordinary petroleum oils. Suitable ratios for most purposes contemplated are 1 mole of phosphorus sulfide for 3-5 moles of bicyclic I terpene.
The olefin-phosphorus sulfide reaction product is preferably employed in amounts between about 0.5% and about 5% by weight based on the total grease composition. The additive is preferably incorporated in the greases subsequent to addition of borax. Conveniently, however, it is added to the composition subsequent to dehydration and prior to milling of the composition for the purpose of creating a suitable grease structure.
The addition of these reaction products has been found to have the surprising effect of maintaining the extreme pressure properties of the borax even when water is present. The low cost of borax makes it a desirable additive to employ in large scale use, such as in steel mill rolling greases. Now, with the ability to maintain the extreme pressure properties of the borax grease even in the presence of water by incorporation of the phosphorus sulfideterpene reaction product, a highly satisfactory low cost industrial lubricant is provided. The means by which this maintenance of extreme pressure properties in the presence of water is attained has not been elucidated at this time. However, it has been determined that many other proprietary products useful in themselves as extreme pressure agents have failed to provide borax-containing oleophilic clay greases with the desired maintenance of extreme pressure properties in the presence of water.
The combination of alkali metal borate with the phosphorusand sulfur-containing reaction products with a bicyclic terpene cures the water sensitivity of borax when contained in grease but does not provide the grease composition with maximum extreme pressure properties. These are substantially improved by the further incorporation of a lead naphthenate to the extent of 0.25-2% based on the total weight of the grease. The improvement in extreme pressure properties without damage to the grease structure is a surprising feature of the invention in view of the mild extreme pressure properties which lead naphthenate exhibits in the absence of other materials. Moreover, when utilized alone in amounts in excess of 1%, lead naphthenate hardened the unworked penetration of a grease so that an unduly wide spread occurred between unworked and worked penetrations. Lead naphthenates are materials well known in the art and may be prepared by reaction of lead compounds with naphthenic acids such as those obtained from certain American crudes, especially those obtained from California. These acids are obtained as mixtures and have average molecular weights of about 250 or higher. In producing lead naphthenate the requisite amount of a lead oxide, such as litharge, is added to the acid and the temperature is raised to eifect reaction. The proportion of lead is in the order of 25-35% and it is preferred to make the lead naphthenate from the oxide instead of utilizing other lead salts although these, such as carbonates, may be employed, if desired.
Still further improvements in the extreme pressure properties of the described class of greases is effected by the addition of a chlorinated diaryl disulfide. This may contain about 10% chlorine, although both larger and smaller percentages may be used. Bis(parach1orobenzyl) disulfide is the preferred species but other corresponding compounds may be utilized such as bis(paraphenyl)disulfide, bis(metachloroparatolyl)disulfide and the corresponding chlorinated xylene disulfides, as well as mixed disulfides such as paria-chloro benzyl and para-chloro phenyl disulfide. These materials are preferably employed in amounts between about 0.25 and 2.5% by weight of the total grease composition.
Chlorinated waxes, higher molecular weight hydrocarbons, such as paratfins, may be employed in place of or in addition to the chlorinated diaryl disulfide. The chlorinated waxes are preferably chlorinated parafiin Wax containing from 20 to 50% chlorine, preferably from 30 to 45% by Weight. Corresponding chlorinated rubber may be used.
The following examples illustrate the advantages gained by the use of the process and product of this invention.
Example 1 Formula. percent w. Sample A Sample B Hectorite clay 4. 90 5.03 Amide of 'lctraethylenepentamine and tall oil acids 3. 69 3.79 Phosphoric Acid 0. 40 0. 41 Sodium Nitrite 0. 46 0. 47 Ihenyl-alpha-na-phthylamine 0. 46 0. 47 Borax (Impalpable Powder) r. 3. 3.00 Pass-turpentine Reaction Product. 2.00 Lead Naphthenate 0.50 Lubricating Oil 84. 59 86.83
13.1. Timken Test, lbs:
0 K load, dry 50 20 OK load, wet 35 10 or less a Added to the grease as a 50/50 concentrate of borax and oil after dehydration.
b Saturated with water.
Example II vBy adding the borax as an oil-borax mixture a subrnicron size dispersion Was obtained, no plating out Was experienced during homogenizing or in bearing tests, and the grease was excellent in all respects, as long as the borax comprised at least 65% by weight of particles having less than 50 micron diameters. If the proportion of larger particles is greater than about 35%, it is p neferred that the oil suspension of the borate be added to the grease at an elevated temperature and the resulting mixture stirred for 1560 minutes at 200-300 F. in order to obtain maximum dispersion.
We claim as our invention:
1. A grease composition comprising a major proportion of a lubricating oil, a grease-forming proportion of a colloidally dispersed clay, said clay being Waterproofed with a cationic hydrophobic surface active agent, 210% by weight of an alkali metal borate, at least 65% by weight of said borate being particles having diameters of less than 50 microns, O.252% by weight of a lead naphthenate and 0.55% by Weight of a phosphorusand sulfur-containing reaction product obtained b reaction of a bicyclic terpene and a phosphorus sulfide.
2. A grease composition comprising a major proportion of a mineral lubricating oil, a grease-forming proportion of a colloidally dispersed clay, said clay being Waterproofed with a cationic hydrophobic surface active agent, 210% by weight of borax, 0.252% by weight of a lead naphth-enate and 0.5-5% by Weight of a phosphorusand sulfur-containing reaction product obtained by reaction of a bicyclic terpene and a phosphorus sultide, at least 65 by weight of borax having particle size diameters of less than 50 microns.
3. The process for the preparation of a grease containing borax which comprises mim'ng horax and oil together,
whereby a 'borax-oil suspension is formed and dispersing the suspension in a substantially anhydrous oleophilic clay grease composition by mixing followed by milling, said composition containing 0.252% by Weight of a lead naphthenate and 0.55% by Weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide, at least by weight of borax having particle size diameters of less than 50 microns.
4. The process for the preparation of a grease containing an alkali metal borate which comprises forming a suspension of 0.252.5 parts by Weight of particulate borate in 1 part of a lubricating oil, at least 65% by weight of said borate being particles having diameters of less than 50 microns and thereafter adding the suspension to a substantially anhydrous oleophilic clay grease composition, said grease composition containing 0.25-2% by weight of a lead napthenate and (LS-5% by weight of a phosphorus and sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide.
5. In a process for the formation of a grease composition having improved extreme pressure properties in the presence of water, the steps comprising forming a substantially anhydrous composition of grease-forming components, said composition comprising a major proportion of a mineral lubricating oil, a grease-forming proportion of an organophilic montmorillonite clay 0.252% by weight of a lead napthenate and 0.55% by weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide; separately forming a substantially anhydrous lubricating oil suspension of 025-25 parts particulate alkali metal borate per part by Weight of oil, :at least 65 by Weight of said borate being particles having diameters of less than 50 microns; and commingling the composition and suspension.
6. In a process for the formation of a grease composition having improved extreme pressure properties in the presence of Water, the steps comprising forming a substantially anhydrous composition of grease-forming components, said composition comprising a major proportion of a lubricating oil, 0.'25-2% by Weight of a lead naphthenate, a grease-forming proportion of an organophilic montmorillonite clay and 0.5-5% by Weight of a phosphorusand sulfur-containing reaction product of a bicyclic terpene and a phosphorus sulfide; separately forming a substantially anhydrous lubricating oil suspension of 0.25-2.5 parts particulate alkali metal borate per part by weight of oil, at least 65 by weight of said borate being particles having diameters of less than 50 microns; and :commingling the composition and suspension.
References Cited in the file of this patent UNITED STATES PATENTS 2,654,712 Cyphers et a1. Oct. 6, 1953 2,932,615 Jordan et a1. Apr. 12, 1960 FOREIGN PATENTS 789,421 Great Britain Jan. 22, 1958
Claims (1)
1. A GREASE COMPOSITION COMPRISING A MAJOR PROPORTION OF LUBRICATING OIL, A GREASE-FORMING PROPORTION OF A COLLODIALLY DISPERSED CLAY, SAID CLAY BEING WATERPROOFED WITH A CATIONIC HYDROPHOBIC SURFACE ACTIVE AGENT, 2-10% BY WEIGHT OF AN ALKALI METAL BORATE, AT LEAST 65% BY WEIGHT OF SAID BORATE BEING PARTICLES HAVING DIAMETERS OF LESS THAN 50 MICRONS, 0.25-2% BY WEIGHT OF A LEAD NAPHTHENATE AND 0.5-5% BY WEIGHT OF A PHOSPHORUS- AND SULFUR-CONTAINING REACTION PRODUCT OBTAINED BY REACTION OF A BICYCLIC TERPENE AND A PHOSPHORUS SULFIDE.
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL257915D NL257915A (en) | 1959-11-16 | ||
US852979A US3095376A (en) | 1959-11-16 | 1959-11-16 | Grease composition and process for its preparation |
GB39005/60A GB915403A (en) | 1959-11-16 | 1960-11-14 | Improvements in or relating to lubricating grease compositions |
FR843828A FR1278762A (en) | 1959-11-16 | 1960-11-14 | Lubricating grease composition and its preparation process |
DES71258A DE1137160B (en) | 1959-11-16 | 1960-11-14 | High pressure grease and process for its manufacture |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US852979A US3095376A (en) | 1959-11-16 | 1959-11-16 | Grease composition and process for its preparation |
Publications (1)
Publication Number | Publication Date |
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US3095376A true US3095376A (en) | 1963-06-25 |
Family
ID=25314705
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US852979A Expired - Lifetime US3095376A (en) | 1959-11-16 | 1959-11-16 | Grease composition and process for its preparation |
Country Status (4)
Country | Link |
---|---|
US (1) | US3095376A (en) |
DE (1) | DE1137160B (en) |
GB (1) | GB915403A (en) |
NL (1) | NL257915A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3370007A (en) * | 1964-09-08 | 1968-02-20 | Shell Oil Co | Extreme-pressure grease compositions |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3033107A1 (en) * | 1980-09-03 | 1982-04-08 | The British Petroleum Co., Ltd., London | Light-coloured open gear lubricating grease - contg. clay thickener, polymer, particulate mineral and extreme pressure additives |
US4435296A (en) | 1981-05-22 | 1984-03-06 | The British Petroleum Company Limited | Lubricating grease |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2654712A (en) * | 1949-09-12 | 1953-10-06 | Standard Oil Dev Co | Sulfurized monocyclic terpenes and oil compositions containing them |
GB789421A (en) * | 1955-03-03 | 1958-01-22 | Bataafsche Petroleum | Lubricating grease compositions |
US2932615A (en) * | 1957-07-22 | 1960-04-12 | Texnco Inc | Extreme pressure lubricant |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL68461C (en) * | 1943-04-09 | |||
NL71486C (en) * | 1944-06-09 | |||
US2758087A (en) * | 1953-05-14 | 1956-08-07 | Socony Mobil Oil Co Inc | Noncorrosive lubricating oil composition |
-
0
- NL NL257915D patent/NL257915A/xx unknown
-
1959
- 1959-11-16 US US852979A patent/US3095376A/en not_active Expired - Lifetime
-
1960
- 1960-11-14 GB GB39005/60A patent/GB915403A/en not_active Expired
- 1960-11-14 DE DES71258A patent/DE1137160B/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2654712A (en) * | 1949-09-12 | 1953-10-06 | Standard Oil Dev Co | Sulfurized monocyclic terpenes and oil compositions containing them |
GB789421A (en) * | 1955-03-03 | 1958-01-22 | Bataafsche Petroleum | Lubricating grease compositions |
US2932615A (en) * | 1957-07-22 | 1960-04-12 | Texnco Inc | Extreme pressure lubricant |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3370007A (en) * | 1964-09-08 | 1968-02-20 | Shell Oil Co | Extreme-pressure grease compositions |
Also Published As
Publication number | Publication date |
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DE1137160B (en) | 1962-09-27 |
GB915403A (en) | 1963-01-09 |
NL257915A (en) |
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