CN113527551B - Thiazole modified polymer, grease and preparation method thereof - Google Patents
Thiazole modified polymer, grease and preparation method thereof Download PDFInfo
- Publication number
- CN113527551B CN113527551B CN202110712094.5A CN202110712094A CN113527551B CN 113527551 B CN113527551 B CN 113527551B CN 202110712094 A CN202110712094 A CN 202110712094A CN 113527551 B CN113527551 B CN 113527551B
- Authority
- CN
- China
- Prior art keywords
- thiazole
- modified polymer
- grease
- product
- temperature
- 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.)
- Active
Links
- 239000004519 grease Substances 0.000 title claims abstract description 77
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229920000642 polymer Polymers 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 230000001050 lubricating effect Effects 0.000 claims description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000002199 base oil Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000000376 reactant Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000010992 reflux Methods 0.000 claims description 17
- 239000003381 stabilizer Substances 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 14
- 230000001007 puffing effect Effects 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000012674 dispersion polymerization Methods 0.000 claims description 13
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 239000002562 thickening agent Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 239000003963 antioxidant agent Substances 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 239000013556 antirust agent Substances 0.000 claims description 5
- 239000007810 chemical reaction solvent Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000009467 reduction Effects 0.000 abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 11
- 239000004005 microsphere Substances 0.000 description 31
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 20
- 239000004926 polymethyl methacrylate Substances 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000007127 saponification reaction Methods 0.000 description 15
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 13
- 235000019441 ethanol Nutrition 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000011056 performance test Methods 0.000 description 8
- -1 alkyl/aryl phosphite Chemical compound 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- 239000010687 lubricating oil Substances 0.000 description 5
- 238000005461 lubrication Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000344 soap Substances 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- GDGIVSREGUOIJZ-UHFFFAOYSA-N 5-amino-3h-1,3,4-thiadiazole-2-thione Chemical compound NC1=NN=C(S)S1 GDGIVSREGUOIJZ-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229920002367 Polyisobutene Polymers 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 2
- 150000003557 thiazoles Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 1
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 102100039496 Choline transporter-like protein 4 Human genes 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 101000889282 Homo sapiens Choline transporter-like protein 4 Proteins 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 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 description 1
- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010696 ester oil Substances 0.000 description 1
- 239000010685 fatty oil Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000030279 gene silencing Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000006078 metal deactivator Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- C10M151/00—Lubricating compositions characterised by the additive being a macromolecular compound containing sulfur, selenium or tellurium
- C10M151/02—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/041—Mixtures of base-materials and additives the additives being macromolecular compounds only
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
-
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
-
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/026—Butene
-
- 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
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof 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
- C10M2221/00—Organic macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2221/02—Macromolecular compounds obtained by reactions of monomers involving only carbon-to-carbon unsaturated bonds
-
- 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
- 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
- C10M2223/045—Metal containing thio derivatives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/14—Metal deactivation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/72—Extended drain
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/76—Reduction of noise, shudder, or vibrations
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Abstract
The application provides a thiazole modified polymer, grease and a preparation method thereof, wherein the thiazole modified polymer contains a large amount of S, N active elements, is dispersed in the grease and is easy to adsorb on the surface of metal machinery to form physical and chemical adsorption, and the generated friction chemical reaction film can effectively improve the noise reduction, noise reduction and wear resistance of the grease.
Description
Technical Field
The application belongs to the technical field of silencing and antiwear materials, and particularly relates to thiazole modified polymers, lubricating grease and a preparation method thereof.
Background
Mechanical equipment is an important tool for industrial production, and good equipment operation depends on lubrication conditions. Lubrication refers to separating friction surfaces with liquids, gases, solids, etc., avoiding direct contact of the friction surfaces, reducing friction and wear. Grease is an important component of industrial lubricants, is a semi-solid lubricating material with plasticity consisting of a thickener and a base oil, and is widely applied to industries such as electronics, power, steel, automobiles and the like. Because of the inherent excellent performance, the lubricating grease not only can meet the conventional lubricating requirement, but also has the following advantages compared with a liquid lubricant: the adhesive property is good, and the loss is not easy; good lubricating ability can be maintained under high load; the lubrication period is long; the applicable temperature range and working condition are wide; has sealing effect. Therefore, the lubricating grease used for the machinery can simplify a mechanical lubricating system, avoid oil leakage, reduce energy consumption and reduce environmental pollution, and accords with the concept of green chemical advocacy.
On the other hand, when the machinery moves relatively, collision friction can be generated, so that noise is generated, proper lubrication can be realized, the noise can be reduced, along with the progress of modern society, people demand longer service life and lower noise for comfort life, such as household appliances, refrigerators, air conditioners, automobiles and the like, higher requirements are put on the noise, traditional lubricating grease isolates friction between friction pair components through an oil film, lubrication is realized, certain noise reduction performance is realized, and the requirements of people on higher noise at present cannot be met.
Disclosure of Invention
The application aims to provide a microsphere, grease and a preparation method thereof, and aims to solve the problem that the existing grease is insufficient in noise reduction capability to a certain extent.
In order to achieve the purposes of the application, the technical scheme adopted by the application is as follows:
in a first aspect, the application provides a thiazole modified polymer, wherein the structural formula of the thiazole modified polymer is shown in the following formula I:
wherein m, n, y are natural numbers greater than 0; and/or
R 1 Any one selected from alkyl groups having 1 to 5 carbon atoms; and/or
X is a thiazole group.
Further, X is a group represented by the following formula II or formula III:
R 2 selected from the group consisting of-NH-, -R 1 -NH-、-CO-、-O-R 1 -, -S-or-S-R 1 -any one of the following; and/or
R 3 Selected from any one of alkyl, mercapto or ester with 1-30 carbon atoms.
Further, the thiazole modified polymer is microspherical; and/or
The grain diameter of the thiazole modified polymer is 50-200um.
In a second aspect, the present application provides a method for preparing a thiazole-based modified polymer, for preparing the thiazole-based modified polymer, comprising the steps of:
step 1: dissolving a reactant A, acrylic acid, a stabilizer and an initiator in ethanol and/or water under a nitrogen atmosphere, and condensing and refluxing;
step 2: and (3) adding a cross-linking agent into the mixture in the step (1) for dispersion polymerization to obtain a product A emulsion.
Step 3: slowly adding the reactant B into the emulsion of the product A, and performing heat treatment to obtain the product B.
The structural formula of the reactant A is shown as the following formula IV:
wherein R1 is selected from any one of alkyl groups with 1-5 carbon atoms;
the reactant B is X-H, wherein X is a group shown in the formula II or the formula III;
and the product B is the thiazole modified polymer.
Further, the reaction solvent comprises a mixture of ethanol and water, and the ratio of ethanol to water is 2 (1-4); and/or
The temperature of the condensation reflux is 65-70 ℃, and the time of the condensation reflux is 1-3h; and/or
The temperature of the dispersion polymerization is 65-70 ℃, and the time of the dispersion polymerization is 10-20h; and/or
The temperature of the heat treatment is 70-80 ℃, and the time of the heat treatment is 2-5h.
In a third aspect, the present application provides a grease comprising a base oil and the thiazole-based modified polymer described above.
Further, the thiazole modified polymer accounts for 1-3% of the lubricating grease by mass.
Further, the grease further comprises one or more of a thickener, a tackifier and an additive, and/or
The additive comprises one or more of an antiwear extreme pressure agent, an antirust agent, a metal passivating agent and an antioxidant.
In a fourth aspect, the present application provides a method for preparing a grease for use in preparing the above grease, comprising the steps of: and (3) after puffing the base oil, cooling, adding the thiazole modified polymer, and grinding to obtain the lubricating grease.
Further, the temperature of the puffing treatment is 160-190 ℃, the puffing time is 10-30min, and the temperature is reduced to 120-140 ℃.
The thiazole modified polymer provided by the first aspect of the application contains a large amount of S, N active elements, is easy to adsorb on the surface of metal machinery, forms physical and chemical adsorption, and generates a tribochemical reaction film, thereby weakening friction between the metal machinery.
The preparation method of the thiazole modified polymer provided by the second aspect of the application is used for preparing the thiazole modified polymer, and the reactant A is polymerized with acrylic acid and then reacts with thiazole compounds, so that the generated thiazole modified polymer has stable structure, is rich in a large number of thiazole groups and has high activity.
The lubricating grease provided by the third aspect of the application comprises the thiazole modified polymer, and the thiazole modified polymer is dispersed in the lubricating grease, so that the noise reduction, noise reduction and wear resistance of the lubricating grease can be effectively improved, and meanwhile, the thiazole modified polymer can also play a role in passivating metal, so that the catalysis of the metal on the lubricating grease is reduced, and the service life of the lubricating grease is prolonged.
According to the preparation method of the lubricating grease provided by the fourth aspect of the application, the base oil is fully puffed, so that the cohesion and adhesion of the lubricating grease are enhanced, and the lubricating effect of the lubricating grease is further improved.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
In the present application, the term "and/or" describes an association relationship of an association object, which means that three relationships may exist, for example, a and/or B may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. The character "/" generally indicates that the context-dependent object is an "or" relationship.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c" may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
It should be understood that, in various embodiments of the present application, the sequence number of each process described above does not mean that the execution sequence of some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weights of the relevant components mentioned in the description of the embodiments of the present application may refer not only to the specific contents of the components, but also to the proportional relationship between the weights of the components, so long as the contents of the relevant components in the description of the embodiments of the present application are scaled up or down within the scope of the disclosure of the embodiments of the present application. Specifically, the mass described in the specification of the embodiment of the application can be mass units known in the chemical industry field such as mu g, mg, g, kg.
The terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated for distinguishing between objects such as substances from each other. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the application. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature.
The first aspect of the embodiment of the application provides a thiazole modified polymer, which has a structural formula shown in the following formula I:
wherein m, n, y are natural numbers greater than 0; and/or
R1 is selected from any one of alkyl groups with 1-5 carbon atoms; and/or
X is a thiazole group.
The thiazole modified polymer contains a large amount of S, N active elements, is easy to adsorb on the surface of metal machinery, forms physical and chemical adsorption, and generates a tribochemical reaction film, thereby weakening friction between the metal machinery.
In some embodiments, X is a group of formula ii or formula iii:
R 2 selected from the group consisting of-NH-, -R 1 -NH-、-CO-、-O-R 1 -, -S-or-S-R 1 -any of, -NH 2 、-R 1 -NH 2 、-COH、HO-R 1 -, -SH or HS-R 1 Both react with-COOH and are stable with-CO-linkages; and/or
R 3 Is selected from any one of alkyl, mercapto or ester with 1-30 carbon atoms, and has stable structure.
In one embodiment of the application, the thiazole-based modified polymer is microspherical, and the microspherical thiazole-based modified polymer can roll on the surface of the metal machine to further reduce direct collision of the friction pair components, thereby further reducing noise between the friction pair components.
In some embodiments, the thiazole modified polymer has a particle size of 50-200um, more preferably 80-150um, and the micron-sized microspheres have higher specific surface area and high chemical stability, can better affinity and synergistic effect with other components in the lubricating grease, improve the noise reduction, noise reduction and wear resistance of the lubricating grease, and easily cause abrasion and increase noise if the microsphere particle size is too large to form large particles.
The second aspect of the embodiment of the application provides a preparation method of a thiazole modified polymer, which is used for preparing the thiazole modified polymer and comprises the following steps:
step 1: dissolving a reactant A, acrylic acid, a stabilizer and an initiator in a reaction solvent under the nitrogen atmosphere, and condensing and refluxing;
step 2: and (3) adding a cross-linking agent into the mixture in the step (1) for dispersion polymerization to obtain a product A emulsion.
Step 3: slowly adding the reactant B into the emulsion of the product A, and performing heat treatment to obtain the product B.
The structural formula of the reactant A is shown as the following formula IV:
wherein R1 is selected from any one of alkyl groups with 1-5 carbon atoms;
the reactant B is X-H, and X is a group shown in the formula II or the formula III;
the product B is thiazole modified polymer.
The specific reaction formula is as follows:
reaction formula 1:
the application provides a preparation method of thiazole modified polymer, which is characterized in that a reactant A is polymerized with acrylic acid and then reacts with thiazole compounds, and the generated thiazole modified polymer has stable structure, is rich in a large number of thiazole groups and has high activity
In some embodiments, the reaction solvent comprises a mixture of ethanol and water in a ratio of 2 (1-4), the temperature of the reflux condensation is 65-70 ℃, and the reflux condensation time is 1-3 hours; and/or
The temperature of the dispersion polymerization is 65-70 ℃, and the time of the dispersion polymerization is 10-20h; and/or
The heat treatment temperature is 70-80 ℃, and the heat treatment time is 2-5h.
In some embodiments, the preparation method of the thiazole modified polymer specifically comprises the following steps:
step 1: introducing nitrogen into a four-neck flask with a stirrer, a thermometer, a reflux condenser and a nitrogen guide pipe for 20min, sequentially adding a reactant A, acrylic acid, a stabilizer and an initiator into the four-neck flask with ethanol and water, stirring and heating to 65-70 ℃ until the raw materials are completely dissolved, and condensing and refluxing for 1-3h.
Step 2: and (3) adding a cross-linking agent into the mixture in the step (1) to carry out dispersion polymerization for 10-20h, so as to obtain a product A emulsion.
Step 3: slowly adding the raw material C into the emulsion of the product A, heating to 70-80 ℃ and reacting for 2-5h to obtain the product B.
Step 4: filtering the product B, washing the filtered product with absolute ethyl alcohol, performing ultrasonic dispersion, filtering again, repeatedly treating until the redundant monomer and the stabilizer are cleaned, and performing vacuum drying on the separated product B solid at the temperature of below 70 ℃ to obtain the monodisperse micron-sized crosslinked thiazole modified polymer microsphere.
The stabilizer is one or more of polyethylene glycol, polyacrylic acid, polyvinyl alcohol, dextrin, polymethacrylic acid, hydroxypropyl cellulose, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate; the initiator adopts any one or more of benzoyl peroxide, azodiisoheptonitrile and azodiisobutyronitrile; the cross-linking agent adopts any one or more of ethoxylated trimethylolpropane triacrylate, ethylene glycol dimethacrylate and divinylbenzene.
A third aspect of this embodiment provides a grease comprising a base oil and the above thiazole-based modified polymer, wherein the base oil is one or more selected from the group consisting of ester oil, silicone oil, fluorine oil, polyether oil, mineral oil and synthetic oil, the base oil content is 55 to 97%, specifically 55%, 60%, 70%, 80%, 90%, etc., and the viscosity of the base oil is 20 to 100mm 2 The thiazole modified polymer is dispersed in the lubricating grease, so that the noise reduction, noise reduction and wear resistance of the lubricating grease can be effectively improved, meanwhile, the thiazole modified polymer can also play a role in passivating metal, the catalysis of the metal on the lubricating grease is reduced, and the service life of the lubricating grease is prolonged.
In some embodiments, the weight ratio of the thiazole modified polymer in the lubricating grease is 1-3%, specifically may be 1%, 1.5%, 2%, 2.5%, 3%, etc., and the quantity of the thiazole modified polymer microspheres in the lubricating grease is too small to fill the gaps between the friction pair components, so that the noise reduction performance of the lubricating grease is easily weakened; the quantity of thiazole modified polymer microspheres in the lubricating grease is excessive, excessive friction is generated among the microspheres, and the noise reduction performance of the lubricating grease can be weakened.
In some embodiments, the grease further comprises one or more of a thickener, a tackifier, and an additive, and/or the additive comprises one or more of an antiwear extreme pressure agent, a rust inhibitor, a metal deactivator, an antioxidant.
The thickener is saponification product of higher fatty acid, in the saponification process of higher fatty acid, the saponifier is selected from one or more of lithium soap, calcium soap, barium soap, sodium soap, PTFE, silicon dioxide powder and bentonite, the content of the thickener is 10-45%, and can be 10%, 15%, 25%, 35%, 45% and the like, the thickener is used for thickening lubricating oil into paste, and the performance of the lubricating grease is changed and adjusted, the thickener is dispersed in base oil and forms a framework, and the lubricating oil is adsorbed in the framework to form pasty lubricating grease;
the tackifier is one or more of polyisobutylene, ethylene-propylene rubber and polymethyl methacrylate, the content of the tackifier is 5-20%, and particularly can be 5%, 10%, 15%, 20% and the like, in the metal mechanical friction process, the high polymer in the lubricating grease is sheared under the action of mechanical shearing, the viscosity of an oil product is reduced, the lubricating effect of the lubricating grease is weakened, and the addition of the tackifier can enhance the shearing stability of the high polymer in the lubricating grease and maintain the lubricating effect of the lubricating grease;
the additive comprises an antiwear extreme pressure agent, an antirust agent, a metal passivating agent and an antioxidant, and the extreme pressure antiwear agent comprises at least one of dialkyl dithiophosphate, dialkyl dithioformate, vulcanized fatty oil, vulcanized olefin, alkyl/aryl phosphite, alkyl/aryl phosphate, TPPT, molybdenum disulfide, graphite, zinc oxide, calcium carbonate and zirconium phosphate, and is used for enhancing the antiwear performance of the lubricating grease, prolonging the service life of the lubricating grease and improving the utilization rate of the lubricating grease;
the antirust agent comprises at least one of sulfonate, naphthalene sulfonate, imidazoline, phosphate and phosphite ester, has oil solubility, can be uniformly dispersed in base oil, and can be adsorbed on the surface of metal to prevent the surface of the metal from contacting water or acidic medium and protect the metal parts from rust;
the metal passivating agent comprises a benzotriazole derivative, is used for passivating the surface of metal, reduces the catalysis of the metal on the lubricating grease, and prolongs the service life of the lubricating grease;
the antioxidant comprises at least one of amine, phenols, triazinetrione and pentaerythritol dodecyl thiopropyl ester, and is used for breaking the reaction chain of the oxidation chain locking reaction, thereby stopping the further progress of the oxidation reaction, preventing the lubricating oil from being oxidized and prolonging the service life of the lubricating oil.
According to a fourth aspect of the present application, there is provided a method for preparing a grease for use in preparing the grease described above, comprising the steps of: after the base oil is puffed, the temperature is reduced, the thiazole modified polymer is added for grinding to obtain the lubricating grease, the base oil is fully puffed, the cohesion and the adhesion of the lubricating grease are enhanced, and the lubricating effect of the lubricating grease is improved. .
In some embodiments, the temperature of the puffing process is 160-190 ℃, the puffing time is 10-30 minutes, the temperature is reduced to 120-140 ℃, the puffing temperature is too low or too short to be puffing, and the puffing temperature is too high or too long to easily cause the deterioration of the base oil paste.
In some embodiments, the method of preparing the grease described above further comprises the steps of:
step 1: dividing the base oil into two parts, namely a first base oil and a second base oil, mixing the first base oil with higher fatty acid, adding a saponification agent, and performing saponification treatment;
step 2: dehydrating the mixture obtained in the step one, and adding second base oil;
step 3: puffing the mixture obtained in the second step;
step 4: cooling, adding tackifier, and grinding;
step 5: and (3) adding the additive and the thiazole modified polymer microsphere into the mixture obtained in the step (IV), and grinding to obtain the lubricating grease.
The saponification reaction is the reaction of the higher fatty acid and the saponification agent to generate the thickening agent, the saponification agent is preferably lithium soap, the base oil does not participate or minimally participates in the saponification reaction, the saponification reaction is a mass transfer and heat transfer process, the concentration of the reactant is higher, the reaction is quicker, but the concentration of the reactant is too high, the material is thick in the later period of the reaction, the stirring is not easy, the reaction of the reactant is incomplete, so the first base oil is added in advance before the saponification, the reactant is diluted, the reaction is smoothly carried out, and the thickening agent is also beneficial to being uniformly dispersed in the base oil in the subsequent process; and after the second base oil is added, puffing treatment is carried out, so that the base oil and the thickening agent in the lubricating grease are fully puffed, the cohesion and the adhesion of the lubricating grease are enhanced, and the lubricating effect of the lubricating grease is further improved.
In some embodiments, the temperature of the saponification treatment is 90-110 ℃ and the saponification treatment time is 0.5-3.0 hours; and/or the temperature of the dehydration treatment is 140-160 ℃, the dehydration treatment is carried out until no steam escapes, the mixture in the step 4 is ground by adopting a colloid mill, and the ratio of the first base oil to the second base oil is (0.5-1.5): 1.
In order that the details and operations of the present application may be clearly understood by those skilled in the art, and that the improved performance of the microsphere, the grease and the preparation method thereof according to the embodiments of the present application may be significantly embodied, the following examples are given to illustrate the above technical solutions.
Preparation of thiazole modified polymer:
example 1
Step 1: introducing nitrogen into a four-neck flask with a stirrer, a thermometer, a reflux condenser and a nitrogen guide pipe for 20min, sequentially adding 25g of acrylic acid (A A), 100g of Methyl Methacrylate (MMA), 4g of stabilizer polyvinylpyrrolidone (PVP) and 3g of initiator Azobisisobutyronitrile (AIBN) into the four-neck flask with 600g of ethanol and 900g of water, stirring and heating to 65-70 ℃ to dissolve all raw materials, and performing condensation reflux reaction for 1-3h;
step 2: adding 12g of trimethylolpropane triacrylate (ethoxylated trimethylolpropane) serving as a cross-linking agent for dispersion polymerization, and reacting for 10-20 hours to obtain a product A emulsion;
step 3: slowly adding 36g of 2-amino-5-mercapto-1, 3, 4-thiadiazole into the emulsion of the product A, heating to 70-80 ℃ and reacting for 2-5 hours to obtain a product B;
step 4: filtering the product B, washing the filtered product with absolute ethyl alcohol, performing ultrasonic dispersion, then filtering, repeatedly treating until the redundant monomer and the stabilizer are cleaned, and performing vacuum drying on the separated solid at the temperature of below 70 ℃ to obtain monodisperse micron-sized thiazole modified PMMA crosslinked microspheres, which are marked as PMMA microspheres 1.
The PMMA microsphere 1 obtained had an average particle size of 200. Mu.m, and a degree of crosslinking of 46%.
Example 2
Step 1: introducing nitrogen into a four-neck flask with a stirrer, a thermometer, a reflux condenser and a nitrogen guide pipe for 20min, sequentially adding 25g of acrylic acid (A A), 100g of Methyl Methacrylate (MMA), 4g of stabilizer polyvinylpyrrolidone (PVP) and 3g of initiator Azobisisobutyronitrile (AIBN) into the four-neck flask with 600g of ethanol and 900g of water, stirring and heating to 65-70 ℃ to dissolve all raw materials, and performing condensation reflux reaction for 1-3h;
step 2: adding 12g of cross-linking agent ethylene glycol dimethacrylate for dispersion polymerization, and reacting for 10-20 hours to obtain a product A emulsion;
step 3: slowly adding 36g of 2-amino-5-mercapto-1, 3, 4-thiadiazole into the emulsion A, heating to 70-80 ℃ and reacting for 2-5 hours to obtain a product B;
step 4: filtering the product B, washing the filtered product with absolute ethyl alcohol, performing ultrasonic dispersion, then filtering, repeatedly treating until the redundant monomers and the stabilizing agent are cleaned, and performing vacuum drying on the separated solid at the temperature of below 70 ℃ to obtain monodisperse micron-sized thiazole modified PMMA crosslinked microspheres, namely PMMA microspheres 2;
the PMMA microspheres 2 obtained had an average particle size of 90 μm and a degree of crosslinking of 48%.
Example 3
Step 1: introducing nitrogen into a four-neck flask with a stirrer, a thermometer, a reflux condenser and a nitrogen guide pipe for 20min, sequentially adding 25g of acrylic acid (A A), 100g of Methyl Methacrylate (MMA), 4g of stabilizer polyvinylpyrrolidone (PVP) and 3g of initiator Azobisisobutyronitrile (AIBN) into the four-neck flask with 600g of ethanol and 900g of water, stirring and heating to 65-70 ℃ to dissolve all raw materials, and performing condensation reflux reaction for 1-3h;
step 2: adding 12g of cross-linking agent divinylbenzene for dispersion polymerization, and reacting for 10-20 hours to obtain a product A emulsion;
step 3: slowly adding 36g of 2-amino-5-mercapto-1, 3, 4-thiadiazole into the emulsion A, heating to 70-80 ℃ and reacting for 2-5 hours to obtain a product B;
step 4: filtering the product B, washing the filtered product with absolute ethyl alcohol, performing ultrasonic dispersion, filtering again, repeatedly treating until the excessive monomer and stabilizer are cleaned, and vacuum drying the separated solid below 70 ℃. The monodisperse micron-sized thiazole modified PMMA crosslinked microsphere is obtained and is marked as PMMA microsphere 3.
The PMMA microspheres 3 obtained had an average particle size of 150. Mu.m, and a degree of crosslinking of 44%.
Example 4
The amounts of stabilizer in step 1 and crosslinking agent in step 2 were doubled, i.e., 8g of stabilizer and 24g of crosslinking agent, and the rest of the procedure was the same as in example 2.
The PMMA microspheres 4 obtained had an average particle diameter of 40. Mu.m, and a degree of crosslinking of 30%.
Example 5
The amounts of stabilizer in step 1 and crosslinking agent in step 2 were reduced by half, i.e., 2g of stabilizer and 6g of crosslinking agent, and the rest of the procedure was the same as in example 3.
The PMMA microspheres 5 obtained had an average particle size of 350. Mu.m, and a degree of crosslinking of 48%.
Preparation of lubricating grease and performance test results:
example 1
Step 1: 50g of PAO base oil with the viscosity of 30mm2/s and 10g of 12 hydroxystearic acid are added into a reaction vessel, heated to 85-100 ℃ for dissolution, 12g of 15% lithium hydroxide aqueous solution is slowly added for saponification reaction, the saponification temperature is 90-110 ℃, and the saponification time is 0.5-3.0h;
step 2: heating to 140-160deg.C, dehydrating for 30-60 min until no water vapor escapes, and adding 40g base oil;
step 3: heating to 160-190 deg.C, puffing for 10-30min;
step 4: stopping heating, cooling to 120-140 ℃, adding 15g of tackifier polyisobutene, stirring and dissolving, and passing through a colloid mill for two times;
step 5: 3g of PMMA microspheres 1, 2g of extreme pressure antiwear agent dialkyl dithiophosphate, 1g of metal antirust agent and 0.5g of phenolic antioxidant are added, and the mixture is uniformly stirred and then ground for 2 times by a three-roller grinder.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to an automobile combination switch, and the noise was tested to be 65db.
Example 2
The PMMA microspheres 1 added in step 5 were replaced with PMMA microspheres 2, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was tested to be 66db.
Example 3
The PMMA microspheres 1 added in step 5 were replaced with PMMA microspheres 3, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was tested to be 63db.
Example 4
The PMMA microspheres 1 added in step 5 were replaced with PMMA microspheres 4, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was measured to be 70db.
Example 5
The PMMA microspheres 1 added in step 5 were replaced with PMMA microspheres 5, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was measured to be 73db.
Example 6
The PMMA microspheres 1 added in step 5 were 10g, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was measured to be 74db.
Comparative example 1
In step 5, PMMA microspheres 1 were not added, and the rest was the same as in example 1.
Noise reduction performance test:
the grease composition obtained in the above experiment was applied to a car combination switch, and the noise was measured to be 78db.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (9)
1. The thiazole modified polymer is characterized by having a structural formula shown in the following formula I:
i
Wherein m, n, y are natural numbers greater than 0;
R 1 any one selected from alkyl groups having 1 to 5 carbon atoms;
x is a thiazole group;
x is a group of formula III:
，
III
R 2 Any one selected from-NH-, -CO-, or-S-;
the thiazole modified polymer is adsorbed on the surface of a metal machine to form physical and chemical adsorption, so as to generate a tribochemical reaction film.
2. The thiazole-based modified polymer according to claim 1, wherein the thiazole-based modified polymer is microspherical; and/or
The grain diameter of the thiazole modified polymer is 50-200um.
3. A process for producing a thiazole-based modified polymer, characterized by comprising the steps of:
step 1: dissolving a reactant A, acrylic acid, a stabilizer and an initiator in a reaction solvent under the nitrogen atmosphere, and condensing and refluxing;
step 2: adding a cross-linking agent into the mixed material in the step 1 for dispersion polymerization to obtain a product A emulsion;
step 3: slowly adding a reactant B into the emulsion of the product A, and performing heat treatment to obtain a product B;
the structural formula of the reactant A is shown as the following formula IV:
IV
Wherein R1 is selected from any one of alkyl groups with 1-5 carbon atoms;
reactant B is X-H, wherein X is a group shown in the following formula III:
，
III
R 2 Any one selected from-NH-, -CO-, or-S-; and the product B is the thiazole modified polymer.
4. The method for producing a thiazole-based modified polymer as defined in claim 3, wherein the reaction solvent comprises a mixture of ethanol and water in a ratio of 2 (1-4); and/or
The temperature of the condensation reflux is 65-70 ℃, and the time of the condensation reflux is 1-3h; and/or
The temperature of the dispersion polymerization is 65-70 ℃, and the time of the dispersion polymerization is 10-20h; and/or
The temperature of the heat treatment is 70-80 ℃, and the time of the heat treatment is 2-5h.
5. A grease comprising a base oil and the thiazole-based modified polymer according to claim 1 or 2.
6. The grease of claim 5, wherein the thiazole-based modified polymer is present in the grease in an amount of 1 to 3% by mass.
7. The grease of claim 5, further comprising one or more of a thickener, a tackifier, and an additive,
the additive comprises one or more of an antiwear extreme pressure agent, an antirust agent, a metal passivating agent and an antioxidant.
8. A method for preparing a grease, characterized in that it is used for preparing a grease according to claims 6-7, comprising the steps of: and (3) after puffing the base oil, cooling, adding the thiazole modified polymer according to the claims 1-2, and grinding to obtain the lubricating grease.
9. The method for preparing the lubricating grease according to claim 8, wherein the temperature of the puffing treatment is 160-190 ℃, the puffing time is 10-30min, and the temperature is reduced to 120-140 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110712094.5A CN113527551B (en) | 2021-06-25 | 2021-06-25 | Thiazole modified polymer, grease and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110712094.5A CN113527551B (en) | 2021-06-25 | 2021-06-25 | Thiazole modified polymer, grease and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113527551A CN113527551A (en) | 2021-10-22 |
| CN113527551B true CN113527551B (en) | 2023-10-24 |
Family
ID=78125878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110712094.5A Active CN113527551B (en) | 2021-06-25 | 2021-06-25 | Thiazole modified polymer, grease and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113527551B (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4301019A (en) * | 1980-10-29 | 1981-11-17 | Mobil Oil Corporation | Mercaptothiadiazole adducts of unsaturated esters and lubricants containing same |
| EP0104667A1 (en) * | 1982-09-29 | 1984-04-04 | Pennwalt Corporation | Metal salts of 1,2,4-thiadiazole and lubricants containing these metal salts |
| US5188746A (en) * | 1990-11-01 | 1993-02-23 | Mobil Oil Corporation | Antiwear/antioxidant additives based on dimercapto derivatives of acrylates and methacrylates polymers and amine reaction products thereof |
| US5318712A (en) * | 1992-10-13 | 1994-06-07 | The Lubrizol Corporation | Lubricants, greases, aqueous fluids and concentrates containing additives derived from dimercaptothiadiazoles |
| CN101960001A (en) * | 2008-02-29 | 2011-01-26 | 卢布里佐尔公司 | The liquid extreme pressure additive |
| CA2784331A1 (en) * | 2009-12-14 | 2011-07-07 | The Lubrizol Corporation | Lubricating composition containing an antiwear agent |
| JP2015086314A (en) * | 2013-10-31 | 2015-05-07 | 株式会社日本触媒 | Novel polymer and viscosity index improver, and lubricant composition |
| CN108026468A (en) * | 2015-07-28 | 2018-05-11 | 路博润公司 | Sealing sweller for lubricating composition |
| CN109942510A (en) * | 2019-03-25 | 2019-06-28 | 深圳市优宝新材料科技有限公司 | Thiazole derivative grafted olefin and its preparation method and application |
| WO2020127389A1 (en) * | 2018-12-18 | 2020-06-25 | Castrol Limited | Lubricating compositions comprising carboxylic acid salt additive, uses and methods of preparing |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7378379B2 (en) * | 2003-06-10 | 2008-05-27 | The Lubrizol Corporation | Functionalized polymer composition for grease |
| WO2006115666A1 (en) * | 2005-04-22 | 2006-11-02 | Exxonmobil Chemical Patents Inc. | Improved corrosion protection for lubricants |
| WO2007068102A2 (en) * | 2005-12-12 | 2007-06-21 | Queen's University At Kingston | Oil dispersible polymer nanoparticles |
| JP5822706B2 (en) * | 2011-12-13 | 2015-11-24 | 株式会社Adeka | Friction and wear reducing agent for lubricating oil and lubricating oil composition containing the same |
-
2021
- 2021-06-25 CN CN202110712094.5A patent/CN113527551B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4301019A (en) * | 1980-10-29 | 1981-11-17 | Mobil Oil Corporation | Mercaptothiadiazole adducts of unsaturated esters and lubricants containing same |
| EP0104667A1 (en) * | 1982-09-29 | 1984-04-04 | Pennwalt Corporation | Metal salts of 1,2,4-thiadiazole and lubricants containing these metal salts |
| US5188746A (en) * | 1990-11-01 | 1993-02-23 | Mobil Oil Corporation | Antiwear/antioxidant additives based on dimercapto derivatives of acrylates and methacrylates polymers and amine reaction products thereof |
| US5318712A (en) * | 1992-10-13 | 1994-06-07 | The Lubrizol Corporation | Lubricants, greases, aqueous fluids and concentrates containing additives derived from dimercaptothiadiazoles |
| CN101960001A (en) * | 2008-02-29 | 2011-01-26 | 卢布里佐尔公司 | The liquid extreme pressure additive |
| CA2784331A1 (en) * | 2009-12-14 | 2011-07-07 | The Lubrizol Corporation | Lubricating composition containing an antiwear agent |
| JP2015086314A (en) * | 2013-10-31 | 2015-05-07 | 株式会社日本触媒 | Novel polymer and viscosity index improver, and lubricant composition |
| CN108026468A (en) * | 2015-07-28 | 2018-05-11 | 路博润公司 | Sealing sweller for lubricating composition |
| WO2020127389A1 (en) * | 2018-12-18 | 2020-06-25 | Castrol Limited | Lubricating compositions comprising carboxylic acid salt additive, uses and methods of preparing |
| CN109942510A (en) * | 2019-03-25 | 2019-06-28 | 深圳市优宝新材料科技有限公司 | Thiazole derivative grafted olefin and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| 2-巯基苯并噻唑衍生物的合成进展;朱继琴;李景宁;;化学通报(第08期);11-16 * |
| Anti-Wear Properties of Highly Reactive Polyisobutylene Derivatives Containing Thiadiazole;Park, MS;POLYMER-KOREA;第44卷(第2期);132-138 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113527551A (en) | 2021-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104830432B (en) | A kind of oil additives composition and preparation method thereof | |
| JP5420237B2 (en) | Lubricating oil additive and lubricating oil composition | |
| CN108034484A (en) | A kind of lubricating oil | |
| CN102337175B (en) | Hydraulic oil composition with high extreme pressure performance | |
| CN105087107A (en) | Preparation method of bearing lubricating grease | |
| CN113817530B (en) | Drawing oil containing nano-particle additive | |
| JPS6226673B2 (en) | ||
| CN105273805A (en) | Lubricant additive | |
| CN107892986A (en) | A kind of carboxyl-functional graphene lubricating oil and preparation method thereof | |
| CN113527551B (en) | Thiazole modified polymer, grease and preparation method thereof | |
| CN103497814A (en) | Lubricating grease specially used in high-temperature kiln car, and preparation method thereof | |
| CN110373250B (en) | Lubricant composition, preparation method thereof and trace lubricant prepared from lubricant composition | |
| CN101519621A (en) | High-performance high-water base lubricant | |
| CN109913308A (en) | Washing machine deceleration machine clutch lubrication oil/fat composition and preparation method | |
| CN104974822B (en) | A kind of preparation method of anti-pressure and abrasion-proof lubricant | |
| Ngaile et al. | Formulation of polymer-based lubricant for metal forming | |
| CN109627805B (en) | Preparation method and application of modified nano calcium carbonate | |
| JPH10259392A (en) | Lubricant for high-temperature plastic working | |
| CN111040828A (en) | Trace lubricant of lubricating composition containing phosphorus, boron and nitrogen and preparation method thereof | |
| JPH0672233B2 (en) | Oily lubricant for cold plastic working of metallic materials | |
| CN111040854A (en) | Trace lubricating oil containing P-B-N composition and its preparing process | |
| CN112175692B (en) | Lubricating grease composition and preparation method and application thereof | |
| CN110331027B (en) | Lubricating oil composition, preparation method thereof and trace lubricating oil prepared by combination | |
| CN101244458A (en) | Metallic nano-particle surface amendment | |
| CN111484887B (en) | Organic molybdenum lubricant composition trace lubricant 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |