CN116640614A - Composite barium-based lubricating grease and preparation method thereof - Google Patents
Composite barium-based lubricating grease and preparation method thereof Download PDFInfo
- Publication number
- CN116640614A CN116640614A CN202310526371.2A CN202310526371A CN116640614A CN 116640614 A CN116640614 A CN 116640614A CN 202310526371 A CN202310526371 A CN 202310526371A CN 116640614 A CN116640614 A CN 116640614A
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- China
- Prior art keywords
- barium
- composite
- parts
- thickening agent
- acid
- 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.)
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- 229910052788 barium Inorganic materials 0.000 title claims abstract description 80
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000004519 grease Substances 0.000 title claims abstract description 72
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002562 thickening agent Substances 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 230000008569 process Effects 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 27
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 26
- 239000002199 base oil Substances 0.000 claims abstract description 26
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 25
- 239000000654 additive Substances 0.000 claims abstract description 25
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 25
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008117 stearic acid Substances 0.000 claims abstract description 25
- -1 polyol ester Chemical class 0.000 claims abstract description 23
- 229920005862 polyol Polymers 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims description 61
- 238000003756 stirring Methods 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 239000003963 antioxidant agent Substances 0.000 claims description 26
- 230000003078 antioxidant effect Effects 0.000 claims description 26
- 238000010008 shearing Methods 0.000 claims description 16
- 239000013556 antirust agent Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 238000005086 pumping Methods 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 9
- 239000000344 soap Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 7
- 229920001577 copolymer Polymers 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 6
- QDCPNGVVOWVKJG-VAWYXSNFSA-N 2-[(e)-dodec-1-enyl]butanedioic acid Chemical compound CCCCCCCCCC\C=C\C(C(O)=O)CC(O)=O QDCPNGVVOWVKJG-VAWYXSNFSA-N 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003508 Dilauryl thiodipropionate Substances 0.000 claims description 3
- 235000019304 dilauryl thiodipropionate Nutrition 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 2
- 239000012964 benzotriazole Substances 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 239000011669 selenium Substances 0.000 claims description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 3
- 239000013538 functional additive Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 229920013639 polyalphaolefin Polymers 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- 239000003112 inhibitor Substances 0.000 description 5
- GGPZWVLYZOHZNX-UHFFFAOYSA-N 1-$l^{1}-selanyldodecane Chemical group CCCCCCCCCCCC[Se] GGPZWVLYZOHZNX-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920002396 Polyurea Polymers 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Chemical class 0.000 description 1
- 239000002184 metal Chemical class 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
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- 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
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- 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
- C10M173/00—Lubricating compositions containing more than 10% water
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- 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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- 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
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- 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
- C10M2207/126—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 monocarboxylic
- C10M2207/1265—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 monocarboxylic used as thickening agent
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- 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
- C10M2207/127—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 polycarboxylic
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- 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
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- 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
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/142—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic
- C10M2207/1426—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic used as thickening agent
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- 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
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
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- 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
- C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2211/08—Halogenated waxes
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- 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
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/0613—Perfluoro polymers used as thickening agents
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- 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
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
- C10M2213/0626—Polytetrafluoroethylene [PTFE] used as thickening agents
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- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- 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
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- 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
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/024—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of esters, e.g. fats
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- 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
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- 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
- C10M2223/041—Triaryl phosphates
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- 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
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- 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
- C10N2030/08—Resistance to extreme temperature
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- 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
- C10N2030/26—Waterproofing or water resistance
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- 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
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- 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
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/02—Bearings
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- 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 application belongs to the technical field of grease manufacture, and particularly relates to composite barium-based grease and a preparation method thereof. The composite barium-based lubricating grease comprises 40-63 parts of lubricating base oil, 20-30 parts of composite barium-based thickening agent, 2-4 parts of organic thickening agent, 1.6-2.4 parts of additive and 10-15 parts of process water; the lubricating base oil is a mixture of PAO and polyol ester in a mass ratio of 3-4:1-2; the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide. The application uses the mixture of PAO and polyol ester as base oil, uses the reactant of dodecahydroxy stearic acid, terephthalic acid and barium hydroxide as the composite barium-based thickening agent, and simultaneously adds a small amount of fluorocarbon thickening agent and functional additive, so that the obtained composite barium-based lubricating grease has good comprehensive properties such as high temperature resistance, water resistance, adhesiveness, colloid stability and the like, has wider high-low temperature performance and low noise performance, and can effectively prolong the service life.
Description
Technical Field
The application belongs to the technical field of grease manufacture, and particularly relates to composite barium-based grease and a preparation method thereof.
Background
The grease is a solid lubricant prepared by thickening base oil by a thickening agent, and the application performance of the grease is improved by adding a proper additive. At present, the types of thickeners in grease can be classified into soap-based type, non-soap-based type and hydrocarbon-based type. Wherein the soap-based grease is a soap-oil two-phase structure formed by fatty acids and metal salt ions, and comprises lithium-based grease, composite lithium-based grease, barium-based grease, composite barium-based grease and the like.
The composite barium-based lubricating grease is prepared from composite barium soap thickening base oil generated by the reaction of two or more acids and barium hydroxide, is novel lubricating grease with excellent comprehensive performance, and has good high temperature resistance, waterproof performance and oxidation resistance, and better extreme pressure wear resistance and mechanical stability than polyurea lubricating grease; the state is stable in the running process of the bearing, the bearing cannot leak or overflow, and the bearing has higher temperature resistance, water resistance and acid and alkali resistance than lithium-based lubricating grease.
At present, the composite barium-based lubricating grease in the domestic market is basically KluyB brand in Germany, and has the advantages of excellent performance, more outstanding defects, such as incapacity of meeting the low noise requirement, incapacity of better prolonging the service life of the bearing, relatively narrower high-low temperature range and the like, and the use of the composite barium-based lubricating grease is restricted to a certain extent.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor at the early stage finds that the organic thickening agent can effectively reduce the low noise performance of the lubricating grease and can widen the high-low temperature performance to a certain extent through a large amount of researches, so that in order to solve the technical problems of the application, a small amount of organic thickening agent is added into the barium-based lubricating grease, the low noise performance can be effectively improved, the high-low temperature range is widened, and the service life of the bearing is effectively prolonged.
The application aims to provide composite barium-based lubricating grease which comprises, by weight, 40-63 parts of lubricating base oil, 20-30 parts of composite barium-based thickening agent, 2-4 parts of organic thickening agent, 1.6-2.4 parts of additive and 10-15 parts of process water;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 3-4:1-2;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide.
In the technical scheme, the poly alpha-olefin base oil and the polyol ester are matched to be used as the lubricating base oil, so that the lubricating base oil has the characteristics of good viscosity-temperature performance, high viscosity index, small evaporation loss, excellent lubricating performance and the like, and has good compatibility with other additives; after the polyacid is added for compounding, the performances of high temperature resistance, water resistance, adhesiveness, colloid stability and the like of the lubricating grease can be greatly improved, and the service life of the bearing can be prolonged; by adding a small amount of fluorocarbon organic thickener, the high temperature resistance and low temperature resistance are further improved, the noise resistance is good, and the service life is prolonged; by adding the functional additive, the functions of antioxidation, extreme pressure wear resistance, rust prevention and the like are improved.
Further, in a preferred scheme, the mass ratio of the dodecahydroxystearic acid, the stearic acid, the terephthalic acid and the barium hydroxide is 8-10:1-2:1-2:12-18. In the technical scheme, the composite reaction of the dodecahydroxystearic acid, the stearic acid, the paraxylylene and the barium hydroxide can effectively improve the performances of high temperature resistance, oxidation stability, water resistance and the like of the lubricating grease.
Further, in a preferred embodiment, the organic thickener is any one of polytetrafluoroethylene or tetrafluoroethylene-hexafluoropropylene copolymer. According to the technical scheme, polytetrafluoroethylene or tetrafluoroethylene-hexafluoropropylene copolymer is a fluorocarbon thickener, has good high temperature resistance, lubricating property and low temperature performance, is not easy to act with other solvents, has good stability, and can effectively improve the high-low temperature range of the grease, reduce noise and prolong the service life of a salt bearing when being added into the composite barium-based grease.
Further, in a preferred scheme, the additive comprises an antioxidant, an anti-rust agent and an extreme pressure antiwear agent, and the mass ratio of the antioxidant to the anti-rust agent is 2:1:1.
Further, in a preferred embodiment, the antioxidant is any one of dilauryl thiodipropionate and selenium dodecyl; the antirust agent is any one of barium petroleum sulfonate, dodecenyl succinic acid, oxidized petroleum barium soap and benzotriazole.
Further, in a preferred scheme, the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate in a mass ratio of 1:1. In the technical scheme, the chloride and the phosphide are matched to be used as the extreme pressure antiwear agent, so that the extreme pressure antiwear agent is good in extreme pressure property and excellent in antiwear property.
The application also aims to provide a preparation method of the composite barium-based lubricating grease, which comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 60-90 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving the heat for 1-2 hours;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 0.5-1h, heating to 100-120 ℃, adding terephthalic acid and 1/2-7/10 of process water, and continuously stirring and reacting for 0.5-1h;
s5, heating the S4 reaction kettle to 90-100 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding the antioxidant and the extreme pressure antiwear agent, and carrying out heat preservation reaction for 2-3h;
s6, after the S5 reaction is finished, rapidly heating to 190-200 ℃ for one time, rapidly stopping the fire, cooling, and keeping for 1-1.5h;
s7, carrying out secondary rapid heating to 190-200 ℃, stopping heating, and pumping materials in the reaction kettle to the blending kettle;
s8, starting a blending kettle circulating cooling system, shearing materials for 0.5-1h under a pressurized state, adding the rest additives when the temperature is reduced to 100 ℃ after shearing is finished, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenization when the temperature in the blending kettle is reduced to below 85 ℃;
s9, putting the homogenized material of the S8 into a grinder for grinding for 2-5 hours, filtering, removing mechanical impurities, vacuumizing and degassing to obtain the product.
Further, in a preferred embodiment, in S5, the temperature of the incubation is 90-110 ℃.
Further, in a preferred scheme, in S6, the temperature rising time is controlled within 5-10min, and the temperature reducing method is as follows: the materials in the reaction kettle are cooled to 150-155 ℃ by introducing normal-temperature heat conduction oil.
Further, in a preferred embodiment, in S8, the shearing pressure is 0.15-0.25MPa and the homogenizing pressure is 15-20MPa.
The application has the beneficial effects that:
1. the application takes the mixture of PAO and polyol ester as base oil, and the reactants of dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide as the composite barium-based thickening agent, and meanwhile, a small amount of fluorocarbon thickening agent and functional additives are added, so that the obtained composite barium-based lubricating grease has good comprehensive properties such as high temperature resistance, water resistance, adhesiveness, colloid stability and the like, has wider high-low temperature performance and low noise performance, and can effectively prolong the service life;
2. the composite barium-based lubricating grease produced by the application is clean and fine, can effectively reduce the vibration of the bearing, has small decibel value, runs stably without garbage noise, has good low-noise performance, and can greatly prolong the service life of the bearing;
3. the process of the reaction process is unique, the reaction is complete through the high-low temperature switching of the reaction temperature, and simultaneously, the oil soap structure and the fiber structure of the lubricating grease are optimized to the greatest extent in a refining mode at high temperature;
4. the application carries out post-treatment such as homogenization, grinding and the like after the reaction is finished, so that the lubricating grease is fully refined, meanwhile, the contained coarse liposome and mechanical impurities are removed, and the generation of mechanical noise can be further reduced.
Detailed Description
The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials according to the following examples are all commercially available and commercially available unless otherwise specified; the detection methods are conventional unless otherwise specified.
The application is described in further detail below with reference to examples:
example 1
The composite barium-based lubricating grease comprises 40 parts of lubricating base oil, 20 parts of composite barium-based thickening agent, 2 parts of organic thickening agent, 1.6 parts of additive and 10 parts of process water in parts by weight;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 3:1;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide, wherein the mass ratio of the dodecahydroxystearic acid to the stearic acid to the terephthalic acid to the barium hydroxide is 8:1:1:12;
the organic thickening agent is polytetrafluoroethylene;
the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent, wherein the mass ratio of the antioxidant to the antirust agent to the extreme pressure antiwear agent is 2:1:1, and the antioxidant is dilauryl thiodipropionate; the rust inhibitor is barium petroleum sulfonate; the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate with the mass ratio of 1:1;
the process water is pure water.
The preparation method of the composite barium-based lubricating grease comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 60 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving the temperature at 90 ℃ for 2 hours;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 1h, heating to 100 ℃, adding terephthalic acid and 1/2 of process water, and continuing stirring and reacting for 1h;
s5, heating the reaction kettle S4 to 90 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding an antioxidant and an extreme pressure antiwear agent, and carrying out heat preservation reaction for 3 hours;
s6, after the S5 reaction is finished, rapidly heating to 190 ℃ once (finishing within 5 min), rapidly stopping the fire, cooling the materials in the reaction kettle to 150 ℃ by introducing normal-temperature heat conduction oil, and keeping for 1.5h;
s7, carrying out secondary rapid heating to 190 ℃, stopping heating, and pumping materials in the reaction kettle to the blending kettle;
s8, starting a blending kettle circulating cooling system, shearing the materials for 1h under the pressurized state of 0.15MPa, adding the rest additives when the temperature is reduced to 100 ℃ after shearing, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenizing when the temperature in the blending kettle is reduced to below 85 ℃, wherein the homogenizing pressure is 20MPa;
s9, putting the homogenized material of the S8 into a grinder for grinding for 2 hours, filtering, removing mechanical impurities, vacuumizing, and degassing to obtain the composite barium-based lubricating grease.
Example 2
The composite barium-based lubricating grease comprises, by weight, 50 parts of lubricating base oil, 250 parts of composite barium-based thickening agent, 3 parts of organic thickening agent, 2 parts of additive and 12 parts of process water;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 2:1;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide, wherein the mass ratio of the dodecahydroxystearic acid to the stearic acid to the terephthalic acid to the barium hydroxide is 9:1.5:1:15;
the organic thickening agent is tetrafluoroethylene-hexafluoropropylene copolymer;
the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent, wherein the mass ratio of the antioxidant to the antirust agent to the extreme pressure antiwear agent is 2:1:1, and the antioxidant is dodecyl selenium; the rust inhibitor is dodecenyl succinic acid; the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate with the mass ratio of 1:1;
the process water is pure water.
The preparation method of the composite barium-based lubricating grease comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 80 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving the temperature at 100 ℃ for 1.5 hours;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 0.5h, heating to 110 ℃, adding terephthalic acid and 6/10 of process water, and continuing stirring and reacting for 1h;
s5, heating the S4 reaction kettle to 100 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding an antioxidant and an extreme pressure antiwear agent, and carrying out heat preservation reaction for 2.5 hours;
s6, after the reaction of S5 is finished, rapidly heating to 195 ℃ for 8min, rapidly stopping the fire, and cooling the materials in the reaction kettle to 153 ℃ and keeping for 1.2h by introducing normal-temperature heat conduction oil;
s7, carrying out secondary rapid heating to 195 ℃, stopping heating, and pumping materials in the reaction kettle to the blending kettle;
s8, starting a blending kettle circulating cooling system, shearing the materials for 0.8h under the pressurized state of 0.2MPa, adding the rest additives when the temperature is reduced to 100 ℃ after shearing, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenizing when the temperature in the blending kettle is reduced to below 85 ℃, wherein the homogenizing pressure is 17MPa;
s9, putting the homogenized material of the S8 into a grinder for grinding for 3 hours, filtering, removing mechanical impurities, vacuumizing, and degassing to obtain the composite barium-based lubricating grease.
Example 3
The composite barium-based lubricating grease comprises, by weight, 63 parts of lubricating base oil, 30 parts of a composite barium-based thickening agent, 4 parts of an organic thickening agent, 2.4 parts of an additive and 15 parts of process water;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 3:2;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide, wherein the mass ratio of the dodecahydroxystearic acid to the stearic acid to the terephthalic acid to the barium hydroxide is 10:2:2:18;
the organic thickening agent is tetrafluoroethylene-hexafluoropropylene copolymer;
the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent, wherein the mass ratio of the antioxidant to the antirust agent to the extreme pressure antiwear agent is 2:1:1, and the antioxidant is dodecyl selenium; the rust inhibitor is oxidized petroleum barium soap; the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate with the mass ratio of 1:1;
the process water is pure water.
The preparation method of the composite barium-based lubricating grease comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 90 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving heat for 2 hours at 110 ℃;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 0.5h, heating to 120 ℃, adding terephthalic acid and 1/2-7/10 of process water, and continuously stirring and reacting for 0.5h;
s5, heating the reaction kettle S4 to 100 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding an antioxidant and an extreme pressure antiwear agent, and carrying out heat preservation reaction for 2 hours;
s6, after the reaction of S5 is finished, rapidly heating to 200 ℃ once (finishing within 10 min), rapidly stopping fire, cooling the materials in the reaction kettle to 155 ℃ by introducing normal-temperature heat conduction oil, and keeping for 1h;
s7, carrying out secondary rapid heating to 200 ℃, stopping heating, and pumping materials in the reaction kettle to the blending kettle;
s8, starting a blending kettle circulating cooling system, shearing the materials for 0.5h under the pressurized state of 0.25MPa, adding the rest additives when the temperature is reduced to 100 ℃ after shearing, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenizing when the temperature in the blending kettle is reduced to below 85 ℃, wherein the homogenizing pressure is 15MPa;
s9, putting the homogenized material of the S8 into a grinder for grinding for 2 hours, filtering, removing mechanical impurities, vacuumizing, and degassing to obtain the composite barium-based lubricating grease.
Comparative example 1
A complex barium-based grease is distinguished from example 2 in that the lubricating base oil used is PAO, otherwise the same as example 2.
Comparative example 2
A complex barium-based grease is distinguished from example 2 in that the complex barium-based thickener used does not contain terephthalic acid, otherwise the same as example 2.
Comparative example 3
A complex barium-based grease was different from example 2 in that an organic thickener was not added, and the same as in example 2 was used.
Comparative example 4
The composite barium-based lubricating grease comprises, by weight, 50 parts of lubricating base oil, 250 parts of composite barium-based thickening agent, 3 parts of organic thickening agent, 2 parts of additive and 12 parts of process water;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 2:1;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide, wherein the mass ratio of the dodecahydroxystearic acid to the stearic acid to the terephthalic acid to the barium hydroxide is 9:1.5:1:15;
the organic thickening agent is tetrafluoroethylene-hexafluoropropylene copolymer;
the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent, wherein the mass ratio of the antioxidant to the antirust agent to the extreme pressure antiwear agent is 2:1:1, and the antioxidant is dodecyl selenium; the rust inhibitor is dodecenyl succinic acid; the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate with the mass ratio of 1:1;
the process water is pure water.
The preparation method of the composite barium-based lubricating grease comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, then putting the dodecahydroxystearic acid, the stearic acid and the terephthalic acid into the reaction kettle again, uniformly stirring, dissolving, and preserving heat for 1.5h at 100 ℃;
s3, adding barium hydroxide into the reaction kettle of the S2, stirring and reacting for 0.5h, adding process water and an organic thickening agent, uniformly stirring, adding an additive, and continuously stirring and reacting for 1h;
s4, after the reaction of S3 is finished, heating to 195 ℃, stopping heating, cooling the materials in the reaction kettle to 153 ℃ by introducing normal-temperature heat conduction oil, keeping for 1.2h, and then pumping the materials in the reaction kettle to a blending kettle;
s5, starting a blending kettle circulating cooling system, shearing the materials for 0.8h under the pressurized state of 0.2MPa, adding the rest additives when the temperature is reduced to 100 ℃ after shearing, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenizing when the temperature in the blending kettle is reduced to below 85 ℃, wherein the homogenizing pressure is 17MPa;
s6, putting the homogenized material of the S5 into a grinder for grinding for 3 hours, filtering, removing mechanical impurities, vacuumizing, and degassing to obtain the composite barium-based lubricating grease.
Comparative example 5
The composite barium-based lubricating grease comprises, by weight, 50 parts of lubricating base oil, 250 parts of composite barium-based thickening agent, 3 parts of organic thickening agent, 2 parts of additive and 12 parts of process water;
the lubricating base oil is a mixture of PAO (poly alpha-olefin) and polyol ester in a mass ratio of 2:1;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide, wherein the mass ratio of the dodecahydroxystearic acid to the stearic acid to the terephthalic acid to the barium hydroxide is 9:1.5:1:15;
the organic thickening agent is tetrafluoroethylene-hexafluoropropylene copolymer;
the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent, wherein the mass ratio of the antioxidant to the antirust agent to the extreme pressure antiwear agent is 2:1:1, and the antioxidant is dodecyl selenium; the rust inhibitor is dodecenyl succinic acid; the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate with the mass ratio of 1:1;
the process water is pure water.
The preparation method of the composite barium-based lubricating grease comprises the following steps:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 80 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving the temperature at 100 ℃ for 1.5 hours;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 0.5h, heating to 110 ℃, adding terephthalic acid and 6/10 of process water, and continuing stirring and reacting for 1h;
s5, heating the S4 reaction kettle to 100 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding an antioxidant and an extreme pressure antiwear agent, and carrying out heat preservation reaction for 2.5 hours;
s6, after the reaction of S5 is finished, rapidly heating to 195 ℃ for 8min, rapidly stopping the fire, cooling the materials in the reaction kettle to 153 ℃ by introducing normal-temperature heat conduction oil, maintaining for 1.2h, and pumping the materials in the reaction kettle to the blending kettle;
s7, starting a blending kettle circulating cooling system, shearing the materials for 0.8h under the pressurized state of 0.2MPa, adding the rest additives when the temperature is reduced to 100 ℃ after shearing, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenizing when the temperature in the blending kettle is reduced to below 85 ℃, wherein the homogenizing pressure is 17MPa;
s8, putting the homogenized material of the S7 into a grinder for grinding for 3 hours, filtering, removing mechanical impurities, vacuumizing, and degassing to obtain the composite barium-based lubricating grease.
Comparative example 6
The composite barium-based lubricating grease is different from the example 2 in that the temperature rising reaction is slower than 30min for two times in the preparation method, and the other steps are similar to the example 2.
Performance test:
the performance of the complex barium-based greases prepared in examples 1 to 3 and comparative examples 1 to 6 prepared as described above and commercially available kluyb (NBU 15) was examined. Wherein, the drop point is measured by using a GB/T4929 method, the working cone penetration is measured by using a GB/T269 method, the oxidation stability is measured by using an SH/T0325 method, the impurity is measured by using an SH/T0379 correlation method, the extreme pressure property is measured by using an SH/T0202 correlation method, the water leaching loss is measured by using an SH/T0109 correlation method, the kinematic viscosity is measured by using a GB/T265 method, and the result is shown in Table 1.
TABLE 1
The performance test results show that the composite barium-based lubricating grease prepared by the proportioning and preparation method has excellent viscosity, dropping point, stability, waterproofness and extreme pressure performance, and excellent overall performance, particularly wider high-low temperature performance and low noise performance, small rotation vibration and long service life, and is superior to the prior KluyB performance.
In comparative examples 1 and 2, no complex base oil or one acid (terephthalic acid) was used, and the performance was slightly inferior to that of the complex barium-based grease prepared by the present application, indicating that the selection of base oil and thickened oil was also important; in comparative example 3, no organic thickener is added, and the overall performance of the composite barium-based lubricating grease is narrower than that of the composite barium-based lubricating grease, particularly the temperature range is narrow, and the vibration is large, so that the temperature range and the noise influence of the composite barium-based lubricating grease can be effectively improved; in comparative examples 4 to 6, the whole grease in comparative example 4 is mixed, no rapid heating is carried out, only one heating is carried out in comparative example 5, the two heating speeds are low, and the obtained composite barium-based grease has poor performance, which shows that the composite barium-based grease is prepared by the high-low temperature switching preparation method provided by the application, has sufficient reaction, and simultaneously, the oil soap structure and the fiber structure of the grease can be optimized to the greatest extent by rapidly heating to high temperature in a proper time, so that the comprehensive performance is improved.
Finally, it should be emphasized that the foregoing description is merely illustrative of the preferred embodiments of the application, and that various changes and modifications can be made by those skilled in the art without departing from the spirit and principles of the application, and any such modifications, equivalents, improvements, etc. are intended to be included within the scope of the application.
Furthermore, the preferred embodiments according to the application can be combined with the basic embodiments of the application individually or in any combination. All such combined solutions are included within the scope of the present application.
Claims (10)
1. The composite barium-based lubricating grease is characterized by comprising, by weight, 40-63 parts of lubricating base oil, 20-30 parts of composite barium-based thickening agent, 2-4 parts of organic thickening agent, 1.6-2.4 parts of additive and 10-15 parts of process water;
the lubricating base oil is a mixture of PAO and polyol ester in a mass ratio of 3-4:1-2;
the composite barium-based thickening agent is obtained by reacting dodecahydroxystearic acid, stearic acid, terephthalic acid and barium hydroxide.
2. The composite barium-based lubricating grease according to claim 1, wherein the mass ratio of the dodecahydroxystearic acid, the stearic acid, the terephthalic acid and the barium hydroxide is 8-10:1-2:1-2:12-18.
3. The composite barium-based grease according to claim 1, wherein the organic thickener is any one of polytetrafluoroethylene or tetrafluoroethylene-hexafluoropropylene copolymer.
4. The composite barium-based lubricating grease according to claim 1, wherein the additive comprises an antioxidant, an antirust agent and an extreme pressure antiwear agent in a mass ratio of 2:1:1.
5. The composite barium-based grease according to claim 4, wherein the antioxidant is any one of dilauryl thiodipropionate and selenium dodecyl; the antirust agent is any one of barium petroleum sulfonate, dodecenyl succinic acid, oxidized petroleum barium soap and benzotriazole.
6. The composite barium-based lubricating grease according to claim 4, wherein the extreme pressure antiwear agent is a mixture of chlorinated paraffin and tricresyl phosphate in a mass ratio of 1:1.
7. The method for preparing the composite barium-based grease according to any one of claims 1 to 6, comprising the steps of:
s1, preparing raw materials according to a proportion for later use;
s2, putting PAO and polyol ester into a reaction kettle, uniformly stirring, and heating to 60-90 ℃;
s3, sequentially adding the dodecahydroxystearic acid and the stearic acid into the reaction kettle of the S2, uniformly stirring, dissolving, and preserving the heat for 1-2 hours;
s4, adding barium hydroxide into the reaction kettle of the S3, stirring and reacting for 0.5-1h, heating to 100-120 ℃, adding terephthalic acid and 1/2-7/10 of process water, and continuously stirring and reacting for 0.5-1h;
s5, cooling the S4 reaction kettle to 90-100 ℃, adding the rest of process water and the organic thickening agent, uniformly stirring, adding an antioxidant and an extreme pressure antiwear agent, and carrying out heat preservation reaction for 2-3h;
s6, after the S5 reaction is finished, rapidly heating to 190-200 ℃ for one time, rapidly stopping the fire, cooling, and keeping for 1-1.5h;
s7, carrying out secondary rapid heating to 190-200 ℃, stopping heating, and pumping materials in the reaction kettle to the blending kettle;
s8, starting a blending kettle circulating cooling system, shearing materials for 0.5-1h under a pressurized state, adding the rest additives when the temperature is reduced to 100 ℃ after shearing is finished, fully stirring and uniformly mixing, and pumping the materials into a high-pressure homogenizer for homogenization when the temperature in the blending kettle is reduced to below 85 ℃;
s9, putting the homogenized material of the S8 into a grinder for grinding for 2-5 hours, filtering, removing mechanical impurities, vacuumizing and degassing to obtain the product.
8. The method for preparing a complex barium-based grease according to claim 6, wherein in S5, the temperature of the heat preservation is 90-110 ℃.
9. The preparation method of the composite barium-based lubricating grease according to claim 6, wherein in S6, the temperature rising time is controlled within 5-10min, and the temperature reducing method is as follows: the materials in the reaction kettle are cooled to 150-155 ℃ by introducing normal-temperature heat conduction oil.
10. The method for preparing a complex barium-based grease according to claim 6, wherein in S8, the shearing pressure is 0.15-0.25MPa and the homogenizing pressure is 15-20MPa.
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2023
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