CN111763551A - Lubricating grease thickening agent and preparation method thereof - Google Patents
Lubricating grease thickening agent and preparation method thereof Download PDFInfo
- Publication number
- CN111763551A CN111763551A CN202010627083.2A CN202010627083A CN111763551A CN 111763551 A CN111763551 A CN 111763551A CN 202010627083 A CN202010627083 A CN 202010627083A CN 111763551 A CN111763551 A CN 111763551A
- Authority
- CN
- China
- Prior art keywords
- lubricating grease
- acid
- coome
- thickener
- grease thickener
- 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.)
- Pending
Links
- 239000004519 grease Substances 0.000 title claims abstract description 55
- 239000002562 thickening agent Substances 0.000 title claims abstract description 54
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 13
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetraline Natural products C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000000344 soap Substances 0.000 claims description 10
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 claims description 8
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 150000004665 fatty acids Chemical class 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 238000001953 recrystallisation Methods 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229920002396 Polyurea Polymers 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 125000004334 oxygen containing inorganic group Chemical group 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000005639 Lauric acid Substances 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229940067597 azelate Drugs 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- QFFPUGXEOWMNCP-UHFFFAOYSA-L dilithium;decanedioate Chemical compound [Li+].[Li+].[O-]C(=O)CCCCCCCCC([O-])=O QFFPUGXEOWMNCP-UHFFFAOYSA-L 0.000 claims description 2
- WZSAITQULFOWSY-UHFFFAOYSA-L dilithium;dodecanedioate Chemical compound [Li+].[Li+].[O-]C(=O)CCCCCCCCCCC([O-])=O WZSAITQULFOWSY-UHFFFAOYSA-L 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 125000005329 tetralinyl group Chemical group C1(CCCC2=CC=CC=C12)* 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 230000008719 thickening Effects 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 230000003750 conditioning effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002199 base oil Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 2
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 235000012216 bentonite Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- FPLIHVCWSXLMPX-UHFFFAOYSA-M lithium 12-hydroxystearate Chemical compound [Li+].CCCCCCC(O)CCCCCCCCCCC([O-])=O FPLIHVCWSXLMPX-UHFFFAOYSA-M 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000010689 synthetic lubricating oil Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
- C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
- C10M117/04—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen containing hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
- C10M123/02—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a non-macromolecular compound
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
- C10M123/06—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a compound of the type covered by group C10M121/00
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/087—Boron oxides, acids or salts
- C10M2201/0876—Boron oxides, acids or salts used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
- C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2217/045—Polyureas; Polyurethanes
- C10M2217/0456—Polyureas; Polyurethanes used as thickening agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
- C10M2219/0445—Sulfonic acids, Derivatives thereof, e.g. neutral salts used as thickening agents
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a lubricating grease thickening agent which is prepared from the following raw materials in percentage by weight: r1COOMe10‑100％、R2COOMe20‑50％、R3(COOMe1)20‑50％、(R4‑NH‑CO‑NH‑R5‑NH‑CO‑NH)n 0‑100％、R6SO3Me30-80% and XOMe10 to 30 percent; the preparation method comprises the following steps: (1) weighing and mixing the raw materials to obtain a material A; (2) adding an organic solvent into the material A, heating to 100-220 ℃ for melting or dissolving while stirring, and cooling to 50 DEG CRecrystallizing at-150 ℃ to obtain a material B; (3) distilling the material B under reduced pressure to obtain the final product. The lubricating grease thickener has a fibrous micro-crystalline structure, and the structure is expressed in a form that qualified thickening can be realized without heat treatment processing when oil is thickened by the thickener, and the microstructure can be observed by an electron microscope.
Description
Technical Field
The invention relates to the technical field of thickening agents, in particular to a lubricating grease thickening agent and a preparation method thereof.
Background
The lubricating grease is a thick grease-like semisolid which is used for a mechanical friction part to play a role in lubrication and sealing, is also used for a metal surface to play a role in filling gaps and preventing rust, and is mainly prepared from mineral oil (or synthetic lubricating oil) and a thickening agent.
At present, there are two types of obtaining methods for thickening agents of lubricating grease: one is that in the process of manufacturing lubricating grease, the oil liquid to be thickened is synthesized, mechanically treated and/or thermally treated to obtain the crystal structure of the target thickener, which is called a one-step method for short; the second method is to prepare pure chemical components of the thickener without oil, then mix the pure chemical components with thickened oil, and mechanically and/or thermally treat the mixture to obtain the crystal structure of the target thickener, which is called two-step method for short. Wherein, the two-step method supports the preposition and external commercialization of the one-step method, and effectively simplifies the production and preparation process of the target lubricating grease.
The marketed lubricating grease thickener comprises the following components in percentage by weight: fatty acid soaps, fatty acid composite soaps, polyureas, calcium petroleum sulfonates, bentonites, organic micro powders and fumed silica, wherein the ratio of the first four types is more than 90%. Meanwhile, the first four types are almost obtained by a one-step method; the latter are obtained in a two-step process.
Although the first four types of prior art have been two-step processes and their commercial products, the emphasis is only on obtaining the chemical components without paying attention to the crystalline structure, and the step of conditioning the crystalline structure is essentially put into the process of thickening into the grease.
Therefore, how to provide a grease thickener that accomplishes both chemical composition and microstructure conditioning is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention aims to provide a grease thickener and a preparation method thereof, so as to solve the problem in the prior art that only chemical components are emphasized and the microstructure is not conditioned.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lubricating grease thickening agent is prepared from the following raw materials in percentage by weight: r1COOMe10-100％、R2COOMe20-50％、R3(COOMe1)20-50％、(R4-NH-CO-NH-R5-NH-CO-NH)n0-100％、R6SO3Me30-80% and XOMe10 to 30 percent; the crystal structure of the lubricating grease thickener is in a fiber grid shape, and the using characteristic is that qualified lubricating grease can be thickened without heating.
The crystal form forming principle of the invention is as follows: heating a thickening agent in a solvent to ensure that an original crystal form is damaged by melting, dissolving, softening and local dissolving and melting, and recrystallizing to grow a target crystal form in a new environment, wherein the key elements of the new environment comprise: concentration, temperature, degree of stirring, time, physicochemical properties of the solvent.
The invention has the beneficial effects that: the obtained thickening agent has good use effect and comprehensive performance quality of the lubricating grease, including mechanical stability, structural stability and microscopic uniformity; the thickened lubricating grease has high-temperature dropping point, good oxidation resistance and excellent water resistance; the thickened lubricating grease has excellent high-temperature dropping point and high extreme pressure abrasion resistance.
Further, R1-R6Is a carbon chain, COO is a carboxyl group, Me1-Me3Is a metal radical, -NH-CO-NH-is a ureido radical, SO3Is sulfonate and XO is oxygen-containing inorganic acid radical; theoretical formula R1COOMe1100% by weight, further, 12-hydroxy lithium stearate or lithium stearate.
Further, the metal is any one or a mixture of several of lithium, calcium, sodium, barium, aluminum, zirconium, strontium and magnesium.
Further, the oxygen-containing inorganic acid is any one or a mixture of borate, phosphate, sulfate and acetate.
Further, the above R1COOMe1Is fatty acid soap, said R1COO is one or more of 12-hydroxystearic acid, stearic acid, lauric acid, palmitic acid, oleic acid, synthetic fatty acid, and petroleum acid.
Further, the above R3(COOMe1)2The soap is a dibasic fatty acid soap which is any one or a mixture of lithium sebacate, lithium azelate and lithium dodecanedioate.
Further, the above (R)4-NH-CO-NH-R5-NH-CO-NH) n is polyurea, wherein n is 1 or 2.
Further, the above R6SO3Me3Preferably, the sulfonic acid soap is calcium petroleum sulfonate.
The preparation method of the lubricating grease thickening agent specifically comprises the following steps:
(1) weighing the raw materials according to the weight parts of the lubricating grease thickening agent, and mixing the raw materials to obtain a material A;
(2) adding an organic solvent into the material A, heating to 100-220 ℃ for melting or dissolving while stirring, and cooling to 50-150 ℃ for recrystallization to obtain a material B;
(3) distilling the organic solvent from the material B under reduced pressure to obtain the solid pure product of the lubricating grease thickener.
The preparation method has the beneficial effects that: the microcosmic crystal form of the thickening agent can be purposefully conditioned through heating melting or dissolving, the grown target crystal form is in a slender fiber shape and is fixed in the cooling operation, and the crystal form has larger specific surface area and netting capacity and finer granularity; the random state of the crystal form before the step is changed, and the crystal form before the step is formed under reaction conditions and usually belongs to a nearly spherical or a thick short rod type.
Further, in the step (2), the organic solvent is tetralin or decalin.
The further beneficial effects are that the boiling point of the solvent is slightly higher than the temperature required for conditioning the crystal form of the crystal, the solvent is easy to volatilize and separate, and the solubility characteristic of the solution is close to that of the thickening agent, so that the solution is suitable for growing fiber type fine crystals.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the lubricating grease thickener has a fibrous micro-crystalline structure, the expression form of the structure is that when the thickener is used for thickening oil, thickening effect which is close to or even more excellent than that of heat treatment can be obtained without heat treatment processing, and the microstructure can be observed by using an electron microscope;
2. the invention adopts an organic solvent recrystallization method, which destroys the previous undesirable crystal form by high-temperature melting or dissolving or softening, creates comprehensive crystallization conditions such as concentration, temperature, stirring degree, time and the like, leads a thickening agent to grow a target crystal form according to the preset target result again, and fixes the crystal form by cooling measures; meanwhile, the organic solvent can be separated from the target product densifier by a reduced pressure distillation mode, and the organic solvent is removed by evaporation at a temperature which does not damage the micro-crystalline structure by controlling the vacuum degree;
3. the lubricating grease thickener is mainly used for manufacturing lubricating grease, but is not limited to the lubricating grease thickener and can also be used for similar applications;
4. compared with the thickening agent in the prior art, the lubricating grease thickening agent has the following differences:
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The lubricating grease thickening agent is prepared from the following raw materials in percentage by weight: 100% of lithium 12-hydroxystearate.
The preparation method comprises the following steps:
(1) weighing the raw materials according to the weight of the lubricating grease thickener, and mixing the raw materials to obtain a material A;
(2) adding decalin into the material A, heating to 100 ℃ for melting or dissolving while stirring at the speed of 5r/min, and then cooling to 50 ℃ for recrystallization to obtain a material B;
(3) distilling the material B under the reduced pressure condition that the vacuum degree is 0MPa and the temperature is 180 ℃ to obtain decahydronaphthalene, thus obtaining the solid pure product of the lubricating grease thickener.
Example 2
The lubricating grease thickening agent is prepared from the following raw materials in percentage by weight: 70% of 12-hydroxy lithium stearate and 30% of calcium sulfate.
The preparation method comprises the following steps:
(1) weighing the raw materials according to the weight of the lubricating grease thickener, and mixing the raw materials to obtain a material A;
(2) adding tetralin into the material A, heating to 220 ℃ for melting or dissolving at the speed of 100r/min while stirring, and then cooling to 150 ℃ for recrystallization to obtain a material B;
(3) distilling the tetrahydronaphthalene from the material B under the vacuum condition of 0.9MPa and 160 ℃ to obtain the solid pure product of the lubricating grease thickener.
Example 3
The lubricating grease thickening agent is prepared from the following raw materials in percentage by weight: 50% of lithium stearate, 20% of polyurea, 20% of calcium petroleum sulfonate and 10% of lithium borate.
The preparation method comprises the following steps:
(1) weighing the raw materials according to the weight of the lubricating grease thickener, and mixing the raw materials to obtain a material A;
(2) adding tetralin into the material A, heating to 150 ℃ for melting or dissolving at the speed of 50r/min while stirring, and then cooling to 100 ℃ for recrystallization to obtain a material B;
(3) distilling the tetrahydronaphthalene from the material B under the vacuum condition of 0.5MPa and 150 ℃ to obtain the solid pure product of the lubricating grease thickener.
Performance testing
60g of the pure solid product of the lubricating grease thickener prepared in the embodiment 1 of the invention is taken, 940g of national standard N500 base oil is added, the mixture is uniformly stirred and wetted, and the mixture is ground on a three-roller machine to obtain the lubricating grease. Similarly, a further portion of grease was prepared as a control by replacing the base oil with 350cSt (25 degrees) dimethicone. The technical indexes are tested according to the national standard method of the lubricating grease, the consistency is GB/T269, the oil distribution is SH/T0324, and the dropping point is GB/T4929. The results are shown in Table 1.
Table 1 grease performance test results
As can be seen from table 1, the grease thickener prepared in example 1 of the present invention can significantly improve the consistency of the thickened oil, reduce the thickening and the amount of the thickened oil, and has a fine and transparent appearance, an oil separation amount of less than 1%, a crystal structure of a fiber mesh shape, and a dropping point of more than 190.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A lubricating grease thickening agent is prepared from the following raw materials in percentage by weight:
R1COOMe10-100％、R2COOMe20-50％、R3(COOMe1)20-50％、(R4-NH-CO-NH-R5-NH-CO-NH)n0-100％、R6SO3Me30-80% and XOMe10-30%, and is characterized in that the crystal structure of the lubricating grease thickener is in a fiber mesh shape, and the use characteristic is that qualified lubricating grease can be thickened without heating.
2. The grease thickener of claim 1, wherein R is1-R6Is a carbon chain, the COO is a carboxyl group, the Me1-Me3Is a metal radical, the-NH-CO-NH-is a ureido radical, the SO3Is made of sulfurAnd the XO is an oxygen-containing inorganic acid radical.
3. The grease thickener according to claim 2, wherein the metal is any one or a mixture of lithium, calcium, sodium, barium, aluminum, zirconium, strontium and magnesium.
4. The grease thickener according to claim 2, wherein the oxygen-containing inorganic acid is any one or a mixture of borate, phosphate, sulfate and acetate.
5. The grease thickener of claim 1, wherein R is1COOMe1Is fatty acid soap, said R1COO is one or more of 12-hydroxystearic acid, stearic acid, lauric acid, palmitic acid, oleic acid, synthetic fatty acid, and petroleum acid.
6. The grease thickener of claim 1, wherein R is3(COOMe1)2The soap is a dibasic fatty acid soap which is any one or a mixture of lithium sebacate, lithium azelate and lithium dodecanedioate.
7. The grease thickener of claim 1, wherein (R) is4-NH-CO-NH-R5-NH-CO-NH) n is a polyurea, said n being 1 or 2.
8. The grease thickener of claim 1, wherein R is6SO3Me3Is sulfonic acid soap which is calcium petroleum sulfonate.
9. The preparation method of the lubricating grease thickening agent is characterized by comprising the following steps:
(1) weighing the raw materials according to the weight percentage of the lubricating grease thickener according to any one of claims 1 to 8, and mixing the raw materials to obtain a material A;
(2) adding an organic solvent into the material A, stirring and heating at the speed of 5-100r/min to 100-220 ℃ for melting or dissolving, and then cooling to 50-150 ℃ for recrystallization to obtain a material B;
(3) distilling the organic solvent from the material B under the vacuum degree of 0-0.9MPa and the temperature of less than 180 ℃ under the reduced pressure state to obtain the solid pure product of the lubricating grease thickener.
10. The method of claim 9, wherein in step (2), the organic solvent is tetralin or decahydronaphthalene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010627083.2A CN111763551A (en) | 2020-07-01 | 2020-07-01 | Lubricating grease thickening agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010627083.2A CN111763551A (en) | 2020-07-01 | 2020-07-01 | Lubricating grease thickening agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111763551A true CN111763551A (en) | 2020-10-13 |
Family
ID=72723515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010627083.2A Pending CN111763551A (en) | 2020-07-01 | 2020-07-01 | Lubricating grease thickening agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111763551A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB767448A (en) * | 1953-07-09 | 1957-02-06 | Exxon Research Engineering Co | Greases containing soaps of dihydroxy stearic acid |
| US4859352A (en) * | 1988-02-29 | 1989-08-22 | Amoco Corporation | Low temperature high performance grease |
| CN102453599A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Composite calcium-sulfonate-based tetrapolyurea lubricating grease and preparation method thereof |
| CN107653048A (en) * | 2016-07-26 | 2018-02-02 | 周丽 | A kind of high temperature resistant lubricating grease and preparation method thereof |
| CN108998147A (en) * | 2017-06-07 | 2018-12-14 | 汪健 | A kind of 12- hydroxy stearic acid, boric acid complex lithium prefabricated soap lubricant composition and preparation method thereof |
| CN111100743A (en) * | 2019-12-26 | 2020-05-05 | 辽宁海华科技股份有限公司 | Low-temperature long-life extreme pressure lubricating grease and preparation method thereof |
-
2020
- 2020-07-01 CN CN202010627083.2A patent/CN111763551A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB767448A (en) * | 1953-07-09 | 1957-02-06 | Exxon Research Engineering Co | Greases containing soaps of dihydroxy stearic acid |
| US4859352A (en) * | 1988-02-29 | 1989-08-22 | Amoco Corporation | Low temperature high performance grease |
| CN102453599A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Composite calcium-sulfonate-based tetrapolyurea lubricating grease and preparation method thereof |
| CN107653048A (en) * | 2016-07-26 | 2018-02-02 | 周丽 | A kind of high temperature resistant lubricating grease and preparation method thereof |
| CN108998147A (en) * | 2017-06-07 | 2018-12-14 | 汪健 | A kind of 12- hydroxy stearic acid, boric acid complex lithium prefabricated soap lubricant composition and preparation method thereof |
| CN111100743A (en) * | 2019-12-26 | 2020-05-05 | 辽宁海华科技股份有限公司 | Low-temperature long-life extreme pressure lubricating grease and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 商业部燃料局: "《农业机械用油手册》", 28 February 1978, 机械工业出版社 * |
| 颜志光 主编: "《润滑材料与润滑技术》", 31 January 2000, 中国石化出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107245362B (en) | Composite calcium sulfonate base grease and preparation method thereof | |
| CN108822938B (en) | Mixed lithium-based grease for improving dropping point and thermal stability and preparation method thereof | |
| CN107188231B (en) | A kind of preparation method of the micro-nano hierarchical structure of the spherical molybdenum disulfide of high dispersive | |
| CN107502419A (en) | A kind of gear type automobile steering gear lubricant composition | |
| CN111763551A (en) | Lubricating grease thickening agent and preparation method thereof | |
| CN106590814B (en) | A kind of preparation method of calcium sulfonate complex grease | |
| Shao et al. | The effect of agitation states on hydrothermal synthesis of Bi2S3 nanorods | |
| CN112824503B (en) | Nano soap-based thickener precursor for lubricating grease and preparation method and application thereof | |
| CN109153936B (en) | Composition and method for preparing calcium magnesium sulfonate lubricating grease without using conventional non-aqueous conversion agent | |
| JP2019501266A (en) | Manufacture of calcium sulfonate grease by using alkali metal hydroxide and delayed addition of non-aqueous conversion agent | |
| CN101898750A (en) | Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof | |
| CN114958461B (en) | Anhydrous calcium-based lubricating grease and preparation method thereof | |
| CN115058272B (en) | Lithium-based lubricating grease and preparation method thereof | |
| CN111100730B (en) | Metal soap-based lubricating grease and preparation method thereof | |
| CN107502422B (en) | Layered potassium calcium phosphate composite lithium-based lubricating grease composition and preparation method thereof | |
| CN107502423B (en) | Lithium-based lubricating grease with layered potassium magnesium phosphate as additive and preparation method thereof | |
| CN107446664B (en) | Layered potassium magnesium phosphate composite lithium-based lubricating grease composition and preparation method thereof | |
| CN107523383B (en) | Environment-friendly layered calcium potassium phosphate grease and preparation method thereof | |
| US2355359A (en) | Fluorescein and halogenated fluoresceins dye acids | |
| CN111088093A (en) | Core-shell-structured lubricating oil additive, preparation method thereof and lubricating oil | |
| CN115746939A (en) | Preparation method of biodegradable environment-friendly lubricant | |
| CN115678633B (en) | Composite lithium prefabricated thickener and preparation method thereof, lubricating grease composition and preparation method thereof | |
| CN111100722A (en) | Composite calcium-based lubricating grease and preparation method thereof | |
| CN117903859A (en) | Polydisperse flying wadding/MoS2Process for preparing nano composite particles | |
| CN114907905B (en) | Alkyl tetralin type lithium-based lubricating grease and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201013 |