CN114480000A - Wear-resistant lubricating oil and preparation method thereof - Google Patents
Wear-resistant lubricating oil and preparation method thereof Download PDFInfo
- Publication number
- CN114480000A CN114480000A CN202210035342.1A CN202210035342A CN114480000A CN 114480000 A CN114480000 A CN 114480000A CN 202210035342 A CN202210035342 A CN 202210035342A CN 114480000 A CN114480000 A CN 114480000A
- Authority
- CN
- China
- Prior art keywords
- lubricating oil
- ceramic powder
- modified
- oil
- nano ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002199 base oil Substances 0.000 claims abstract description 41
- 239000011347 resin Substances 0.000 claims abstract description 38
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011230 binding agent Substances 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 230000001050 lubricating effect Effects 0.000 claims abstract description 29
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 26
- 239000003755 preservative agent Substances 0.000 claims abstract description 25
- 230000002335 preservative effect Effects 0.000 claims abstract description 25
- 229920001800 Shellac Polymers 0.000 claims abstract description 22
- 239000004208 shellac Substances 0.000 claims abstract description 22
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 claims abstract description 22
- 229940113147 shellac Drugs 0.000 claims abstract description 22
- 235000013874 shellac Nutrition 0.000 claims abstract description 22
- 241001474374 Blennius Species 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 8
- 239000011707 mineral Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000003784 tall oil Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 claims description 4
- 244000259229 Grindelia squarrosa Species 0.000 claims description 4
- 239000001191 butyl (2R)-2-hydroxypropanoate Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 3
- 238000005260 corrosion Methods 0.000 claims 1
- 230000007797 corrosion Effects 0.000 claims 1
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 claims 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 claims 1
- 239000003112 inhibitor Substances 0.000 claims 1
- 239000013638 trimer Substances 0.000 claims 1
- VTWRDJZXRSJZKM-UHFFFAOYSA-L zinc;butoxy-octoxy-oxido-sulfanylidene-$l^{5}-phosphane Chemical compound [Zn+2].CCCCCCCCOP([O-])(=S)OCCCC.CCCCCCCCOP([O-])(=S)OCCCC VTWRDJZXRSJZKM-UHFFFAOYSA-L 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 11
- 238000001556 precipitation Methods 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 6
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000003292 glue Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 238000005299 abrasion Methods 0.000 description 11
- 235000019198 oils Nutrition 0.000 description 10
- 125000005456 glyceride group Chemical group 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- XEOXZSREIVIEIP-UHFFFAOYSA-N trizinc [butyl(octyl)-lambda4-sulfanylidene]-dioxido-sulfido-lambda5-phosphane Chemical group C(CCC)S(=P([S-])([O-])[O-])CCCCCCCC.[Zn+2].C(CCC)S(=P([S-])([O-])[O-])CCCCCCCC.[Zn+2].[Zn+2] XEOXZSREIVIEIP-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- AGNTUZCMJBTHOG-UHFFFAOYSA-N 3-[3-(2,3-dihydroxypropoxy)-2-hydroxypropoxy]propane-1,2-diol Chemical compound OCC(O)COCC(O)COCC(O)CO AGNTUZCMJBTHOG-UHFFFAOYSA-N 0.000 description 1
- VRJULIWWOHUBFB-UHFFFAOYSA-N P(=S)(O)(O)O.C(CCC)[Zn]CCCCCCCC Chemical compound P(=S)(O)(O)O.C(CCC)[Zn]CCCCCCCC VRJULIWWOHUBFB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- -1 hydroxycarboxylic acid fatty acid Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- COTPAMORPWZHKE-UHFFFAOYSA-H trizinc;thiophosphate;thiophosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([S-])=O.[O-]P([O-])([O-])=S COTPAMORPWZHKE-UHFFFAOYSA-H 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of 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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/003—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen 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
- 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
-
- 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
-
- 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
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
-
- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
-
- 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
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
-
- 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
-
- 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
- C10N2030/04—Detergent property or dispersant property
-
- 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
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/015—Dispersions of solid lubricants
- C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses wear-resistant lubricating oil which comprises the following components: lubricating base oil, a modified binder, modified nano ceramic powder, a dispersant and a preservative; the invention also discloses a preparation method of the wear-resistant lubricating oil, which comprises the following steps: preparing nano ceramic powder; modifying the nano ceramic powder; uniformly stirring the shellac, the liquid resin and the seaweed glue to obtain a modified binder; adding the modified binder, the modified nano ceramic powder, the dispersant and the preservative into lubricating base oil, adding the silane coupling agent, and stirring to obtain wear-resistant lubricating oil; according to the invention, the modified binder, the modified nano ceramic powder, the dispersant and the preservative are added into the lubricating base oil for mixing, and are modified by the silane coupling agent, and the silane coupling agent couples and connects the lubricating base oil, so that the overall stability of the lubricating oil is improved, and the problem that the lubricating oil forms insufficient oil film strength and toughness on the surface of a workpiece due to the precipitation of the modified additive in the lubricating oil caused by insufficient dispersibility and stability is solved.
Description
Technical Field
The invention relates to the technical field of lubricating oil, in particular to wear-resistant lubricating oil and a preparation method thereof.
Background
Dry friction occurs when the engine is running if some of the friction sites are not properly lubricated. The heat generated by dry friction in a short time is enough to melt the metal, causing damage or even seizure of the machine parts. Therefore, it is necessary to give good lubrication to the friction parts in the engine. When the lubricating oil flows to the friction part, the lubricating oil is adhered to the friction surface to form a layer of oil film, so that the resistance between the friction parts is reduced, and the strength and the toughness of the oil film are the key for playing the lubricating role. The additive in the lubricating oil has poor dispersibility and stability, is easy to agglomerate and precipitate, and causes the lubricating oil to form an oil film on the surface of a workpiece with insufficient strength and toughness and poor antiwear effect.
Therefore, how to improve the dispersibility and stability of the additive, how to form a high-strength and high-toughness oil film on the surface of a workpiece, and how to improve the wear resistance are technical problems that researchers must face.
Disclosure of Invention
The invention aims to provide an anti-wear lubricating oil and a preparation method thereof, aiming at the defects of the prior art.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
an abrasion-resistant lubricating oil comprises the following components in parts by weight: 80-100 parts of lubricating base oil, 10-20 parts of modified binder, 3-5 parts of modified nano ceramic powder, 1-5 parts of dispersant and 1-5 parts of preservative.
Further, the lubricating base oil comprises one or more of mineral base oil, synthetic base oil and vegetable oil base oil.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 2-5: 1-3: 1-2.
Further, the liquid resin is a liquid rosin resin.
Further, the dispersing agent is one or more of stearic acid, sodium dodecyl benzene sulfonate, fatty glyceride, triglycerol monolaurate, stearic acid monoglyceride and quaternary ammonium compound.
Further, the preservative is any one or more of zinc alkyl thiophosphate, butyl octyl zinc thiophosphate and dialkyl zinc thiophosphate.
A preparation method of wear-resistant lubricating oil comprises the following steps:
crushing wear-resistant ceramic to obtain nano ceramic powder with the particle size of 20-100 nm;
adding a silane coupling agent and an ethanol solution into the nano ceramic powder, heating to 50-60 ℃, stirring for 20-30min, filtering, washing with deionized water, and removing the unreacted silane coupling agent completely to obtain modified nano ceramic powder;
adding the shellac into butyl lactate, stirring for dissolving, then adding liquid resin and seaweed gel, heating to 70-80 ℃, stirring for 1-2h, and uniformly stirring to obtain a modified binder;
and step four, adding the modified binder, the modified nano ceramic powder, the dispersant and the preservative into lubricating base oil, adding the silane coupling agent, heating to 60-70 ℃, stirring by adopting a stirrer at the stirring speed of 800-1000r/min for 2-3h to obtain the wear-resistant lubricating oil.
Further, in the second step, the nano ceramic powder: silane coupling agent: the mass ratio of the ethanol solution is 1:0.1-0.2: 1-2.
Further, in the fourth step, the total amount of the lubricating oil mixture is as follows: the mass ratio of the silane coupling agent is 1: 0.1-0.15.
Further, the ethanol solution is 50-75% ethanol solution.
Further, the silane coupling agent is one of vinyltriethoxysilane, vinyltrimethoxysilane and vinyltris (beta-methoxyethoxy) silane.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
according to the invention, the modified nano ceramic powder is added, nano particles in the nano ceramic powder are mostly spherical, the nano ceramic powder plays a role of a ball bearing in a friction process, and has stronger mechanical property, after being mixed with lubricating oil, the wear resistance of the lubricating oil is effectively improved, and the nano ceramic particles can be filled in damaged parts on the surface of a workpiece, so that in-situ repair of the friction surface can be realized.
The modified binder is added, so that the modified binder can improve the cohesiveness of each component in the lubricating oil, prevent layering and precipitation, improve the cohesive force of the lubricating oil and a workpiece, form an oil film with high strength and toughness on the surface of the workpiece, protect the workpiece, prevent dry friction and wear the workpiece; the modified binder comprises liquid resin, shellac and seaweed glue; the liquid resin can improve the bonding strength of the oil film and the workpiece and reduce the damage of the oil film; the shellac film contains a large amount of shellac resin, which is an elastic network structure composed of hydroxycarboxylic acid fatty acid and sesquiterpene acid, can enhance the ductility of the oil film, and can effectively improve the toughness, wear resistance and mechanical properties of the lubricating oil; the addition of the seaweed gel is beneficial to improving the stability and film formability of the lubricating oil, and is beneficial to forming a stable oil film on the surface of a workpiece by the lubricating oil and protecting the surface of the workpiece.
In the preparation process, the nano ceramic powder is firstly modified, and the nano ceramic powder has hydrophobic and oleophylic properties after being modified by the silane coupling agent and the ethanol solution, so that the bonding property of nano ceramic particles and lubricating oil is greatly improved, the problems of layering and agglomeration are reduced, and the water resistance and weather resistance of the lubricating oil are improved;
in the preparation process, the modified binder, the modified nano ceramic powder, the dispersant and the preservative are added into the lubricating base oil for mixing, and are modified by the silane coupling agent, and the silane coupling agent couples the lubricating base oil and the modified nano ceramic powder, so that the adhesiveness, the dispersibility and the stability of the modified binder and the modified nano ceramic powder in the lubricating oil can be improved, the integral stability of the lubricating oil is improved, the modified binder and other additives in the lubricating oil can be adsorbed on a workpiece together, the functions of various additives are fully exerted, and the problem that the oil film strength and the toughness of the lubricating oil formed on the surface of the workpiece are insufficient due to the precipitation of the modified additives in the lubricating oil caused by insufficient dispersibility and stability is solved.
Detailed Description
The following examples further describe embodiments of the present invention in detail. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 80 parts of lubricating base oil, 10 parts of modified binder, 3 parts of modified nano ceramic powder, 1 part of dispersant and 1 part of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 3:1: 1; the liquid resin is liquid rosin resin.
A preparation method of wear-resistant lubricating oil comprises the following steps:
crushing wear-resistant ceramic to obtain nano ceramic powder with the particle size of 20-100 nm;
adding a silane coupling agent and an ethanol solution into the nano ceramic powder, wherein the ethanol solution is a 75% ethanol solution, and the nano ceramic powder comprises the following components in parts by weight: silane coupling agent: heating the ethanol solution to 50 ℃ at a mass ratio of 1:0.2:2, stirring for 30min, filtering, washing with deionized water, and removing unreacted silane coupling agent to obtain modified nano ceramic powder;
adding the shellac into butyl lactate, stirring for dissolving, then adding liquid resin and seaweed gel, heating to 75 ℃, stirring for 1h, and uniformly stirring to obtain a modified binder;
adding the modified binder, the modified nano ceramic powder, the dispersant and the preservative into lubricating base oil, and then adding the silane coupling agent, wherein the total amount of the lubricating oil mixture is as follows: heating the silane coupling agent to 65 ℃ at a mass ratio of 1:0.1, stirring by a stirrer at a stirring speed of 1000r/min for 2h to obtain the wear-resistant lubricating oil.
Further, the silane coupling agent is vinyl triethoxysilane.
Example 2
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 90 parts of lubricating base oil, 15 parts of modified binder, 4 parts of modified nano ceramic powder, 3 parts of dispersant and 3 parts of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 3:1: 1; the liquid resin is liquid rosin resin.
The preparation method of the wear-resistant lubricating oil is the same as that of the embodiment 1.
Example 3
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 100 parts of lubricating base oil, 20 parts of modified binder, 5 parts of modified nano ceramic powder, 5 parts of dispersant and 5 parts of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 3:1: 1; the liquid resin is liquid rosin resin.
The preparation method of the wear-resistant lubricating oil is the same as that of the embodiment 1.
Comparative example 1
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 100 parts of lubricating base oil, 5 parts of modified nano ceramic powder, 5 parts of dispersing agent and 5 parts of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
A preparation method of wear-resistant lubricating oil comprises the following steps:
crushing wear-resistant ceramic to obtain nano ceramic powder with the particle size of 20-100 nm;
adding a silane coupling agent and an ethanol solution into the nano ceramic powder, wherein the ethanol solution is a 75% ethanol solution, and the nano ceramic powder comprises the following components in parts by weight: silane coupling agent: heating the ethanol solution to 50 ℃ at a mass ratio of 1:0.2:2, stirring for 30min, filtering, washing with deionized water, and removing unreacted silane coupling agent to obtain modified nano ceramic powder;
and step three, adding the modified nano ceramic powder, the dispersing agent and the preservative into lubricating base oil, heating to 65 ℃, stirring by using a stirrer at the stirring speed of 1000r/min for 2 hours to obtain the wear-resistant lubricating oil.
Further, the silane coupling agent is vinyl triethoxysilane.
Comparative example 2
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 100 parts of lubricating base oil, 20 parts of modified binder, 5 parts of dispersant and 5 parts of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 3:1: 1; the liquid resin is liquid rosin resin.
A preparation method of wear-resistant lubricating oil comprises the following steps:
step one, adding shellac into butyl lactate, stirring for dissolving, then adding liquid resin and seaweed gel, heating to 75 ℃, stirring for 1h, and stirring uniformly to obtain a modified binder;
and step two, adding the modified binder, the dispersant and the preservative into the lubricating base oil, heating to 65 ℃, stirring by using a stirrer at the stirring speed of 1000r/min for 2 hours to obtain the wear-resistant lubricating oil.
Comparative example 3
An abrasion-resistant lubricating oil comprises the following components in parts by weight: 100 parts of lubricating base oil, 20 parts of liquid resin, 5 parts of nano ceramic powder, 5 parts of dispersing agent and 5 parts of preservative.
Further, the lubricating base oil is a mineral base oil; the dispersing agent is fatty glyceride; the preservative is zinc butyl octyl dithiophosphate.
Further, the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 3:1: 1; the liquid resin is liquid rosin resin.
A preparation method of wear-resistant lubricating oil comprises the following steps:
crushing wear-resistant ceramic to obtain nano ceramic powder with the particle size of 20-100 nm;
and step two, adding the liquid resin, the nano ceramic powder, the dispersing agent and the preservative into the lubricating base oil, heating to 65 ℃, stirring by using a stirrer at the stirring speed of 1000r/min for 2 hours to obtain the wear-resistant lubricating oil.
Further, the silane coupling agent is vinyl triethoxysilane.
In order to comprehensively evaluate the application properties of the lubricating oil prepared by the invention, the storage stability and the wear resistance of the lubricating oils of the examples and the comparative examples are respectively tested.
And (4) testing the storage stability:
the method comprises the following steps: 100ml of each of the lubricating oils obtained in examples 1 to 3 and comparative examples 1 to 3 was allowed to stand at 25 ℃ for 0 day, 15 days, 30 days, 60 days and 180 days, respectively, and then the agglomeration, delamination and precipitation phenomena of the lubricating oil were observed, and the results are shown in Table 1;
appearance evaluation criteria:
1. the dispersion is stable, and the phenomena of agglomeration, layering and precipitation are avoided;
2. the dispersion is stable, and slight agglomeration, layering and precipitation phenomena occur;
3. the dispersion is unstable, and the phenomena of agglomeration, delamination and precipitation are obvious;
4. the dispersion is extremely unstable, and serious agglomeration, delamination and precipitation phenomena occur;
TABLE 1 lubricating oils prepared in the examples and comparative examples agglomerate, delaminate, and precipitate after storage
| Test sample | Day 0 | 15 days | 30 days | 60 days | 180 days |
| Example 1 | 1 | 1 | 1 | 1 | 1 |
| Example 2 | 1 | 1 | 1 | 1 | 1 |
| Example 3 | 1 | 1 | 1 | 1 | 1 |
| Comparative example 1 | 1 | 1 | 1 | 2 | 3 |
| Comparative example 2 | 1 | 1 | 1 | 1 | 2 |
| Comparative example 3 | 1 | 2 | 2 | 3 | 4 |
As can be seen from the data in Table 1, the storage stability of the lubricating oils prepared in examples 1-3 in which the modifier was added to the base oil was significantly better than that of the lubricating oils prepared in comparative examples 1-3, and the dispersibility and stability were good.
And (3) testing the wear resistance: the test is carried out according to the standard SH/T0189-1992, an MRS-10A four-ball friction abrasion tester is adopted, the test condition load is 392N, the temperature is 25 ℃, the time is 60min, the rotating speed is 1200r/min, and the abrasion resistance of a test sample is judged according to the size of the abrasion mark diameter, and the abrasion mark diameter is shown in a table 2.
TABLE 2 antiwear Properties of lubricating oils obtained in examples and comparative examples
As can be seen from Table 2, the lubricating oils prepared in examples 1-3 had significantly smaller wear scar diameters than the lubricating oils prepared in comparative examples 1-3, and the lubricating oils prepared using the formulations and methods of the present invention had significantly improved antiwear properties.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The wear-resistant lubricating oil is characterized by comprising the following components in parts by weight: 80-100 parts of lubricating base oil, 10-20 parts of modified binder, 3-5 parts of modified nano ceramic powder, 1-5 parts of dispersant and 1-5 parts of preservative.
2. The antiwear lubricating oil of claim 1, wherein the lubricating base oil comprises one or more of a mineral base oil, a synthetic base oil, and a vegetable oil base oil.
3. The wear-resistant lubricating oil of claim 1, wherein the modified binder comprises liquid resin, shellac and seaweed gel, and the mass ratio of the liquid resin to the shellac to the seaweed gel is 2-5: 1-3: 1-2.
4. The antiwear lubricating oil of claim 3, wherein the liquid resin is a liquid rosin resin.
5. The antiwear lubricating oil of claim 1, wherein the dispersant is one or more of stearic acid, sodium dodecylbenzene sulfonate, fatty acid glyceride, glycerol trimer monolaurate, glycerol monostearate, and quaternary ammonium compound.
6. The antiwear lubricating oil of claim 1, wherein the corrosion inhibitor is any one or more of zinc alkyl thiophosphate, zinc butyl octyl thiophosphate, and zinc dialkyl thiophosphate.
7. The preparation method of the wear-resistant lubricating oil is characterized by comprising the following steps of:
crushing wear-resistant ceramic to obtain nano ceramic powder with the particle size of 20-100 nm;
adding a silane coupling agent and an ethanol solution into the nano ceramic powder, heating to 50-60 ℃, stirring for 20-30min, filtering, washing with deionized water, and removing the unreacted silane coupling agent completely to obtain modified nano ceramic powder;
adding the shellac into butyl lactate, stirring for dissolving, then adding liquid resin and seaweed gel, heating to 70-80 ℃, stirring for 1-2h, and uniformly stirring to obtain a modified binder;
and step four, adding the modified binder, the modified nano ceramic powder, the dispersant and the preservative into lubricating base oil, adding the silane coupling agent, heating to 60-70 ℃, stirring by adopting a stirrer at the stirring speed of 800-1000r/min for 2-3h to obtain the wear-resistant lubricating oil.
8. The method for preparing an antiwear lubricating oil according to claim 7, wherein in step two, the nano ceramic powder: silane coupling agent: the mass ratio of the ethanol solution is 1:0.1-0.2: 1-2.
9. The method for preparing an antiwear lubricating oil according to claim 7, wherein in the fourth step, the total amount of the lubricating oil mixture is as follows: the mass ratio of the silane coupling agent is 1: 0.1-0.15.
10. The method of claim 7, wherein the ethanol solution is a 50-75% ethanol solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210035342.1A CN114480000A (en) | 2022-01-13 | 2022-01-13 | Wear-resistant lubricating oil and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210035342.1A CN114480000A (en) | 2022-01-13 | 2022-01-13 | Wear-resistant lubricating oil and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114480000A true CN114480000A (en) | 2022-05-13 |
Family
ID=81511732
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210035342.1A Pending CN114480000A (en) | 2022-01-13 | 2022-01-13 | Wear-resistant lubricating oil and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114480000A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754687A (en) * | 2016-03-10 | 2016-07-13 | 吴其增 | Active nano high-abrasion-resistance lubricating oil and preparation method thereof |
| CN105985828A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Nano-ceramic energy-saving anti-friction lubricating oil and preparation method therefor |
| CN108368446A (en) * | 2015-12-10 | 2018-08-03 | 艺康美国股份有限公司 | Abrasion masked composition and its application method for reusable container |
| CN110484328A (en) * | 2019-08-16 | 2019-11-22 | 鸿源新能源科技(广州)有限公司 | A kind of antiwear lubricating oil additive and preparation method thereof for mechanical equipment |
-
2022
- 2022-01-13 CN CN202210035342.1A patent/CN114480000A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105985828A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Nano-ceramic energy-saving anti-friction lubricating oil and preparation method therefor |
| CN108368446A (en) * | 2015-12-10 | 2018-08-03 | 艺康美国股份有限公司 | Abrasion masked composition and its application method for reusable container |
| CN105754687A (en) * | 2016-03-10 | 2016-07-13 | 吴其增 | Active nano high-abrasion-resistance lubricating oil and preparation method thereof |
| CN110484328A (en) * | 2019-08-16 | 2019-11-22 | 鸿源新能源科技(广州)有限公司 | A kind of antiwear lubricating oil additive and preparation method thereof for mechanical equipment |
Non-Patent Citations (1)
| Title |
|---|
| 汪海燕，章于川: "纳米陶瓷粉体的表面改性与应用", 《佛山陶瓷》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103282707A (en) | Tubular threaded joint having improved high torque performance | |
| CN1804016A (en) | Self-repairing multi-soap based composite bearing lubricating grease and preparation method thereof | |
| CN1301319C (en) | Lubricating oil additive and preparation method | |
| CN111378520A (en) | MoS-containing2Water soluble trace amount lubricating liquid | |
| CN111057607A (en) | Lubricating oil with self-repairing function and preparation method thereof | |
| CN114480000A (en) | Wear-resistant lubricating oil and preparation method thereof | |
| CN101684427A (en) | Antiwear additive of lubricating oil | |
| Wang et al. | Experimental study on the suspension stability and tribological properties of nano-copper in LCKD-320# lubricating oil | |
| CN105802700A (en) | Lubricating type anti-rust oil special for bearing bush | |
| CN113201390A (en) | Antifriction heat-resistant lithium-based grease and preparation method thereof | |
| CN102703181A (en) | Energy-saving self-repairing automobile gear oil | |
| CN112877119B (en) | Extreme pressure-resistant wear-resistant long-acting lubricating oil composition and preparation method thereof | |
| CN115477972B (en) | Preparation method and application of lubricating oil additive for engine | |
| CN114989876B (en) | Preparation method of black phosphorus/silicon dioxide water-based lubricating additive | |
| CN100569417C (en) | A kind of metallic nano-particle surface amendment | |
| CN101684428A (en) | Nano copper antiwear lubricating oil additive | |
| CN114276864B (en) | Water-based stainless steel fastener anti-seizure agent and preparation method thereof | |
| CN108251185B (en) | Preparation and application of nano material composition used as lubricating oil additive | |
| CN113801717B (en) | BN/Cu/PDA nano composite particles and preparation method and application thereof | |
| CN112410107A (en) | Nano synthetic lubricating oil and preparation method thereof | |
| CN109337732A (en) | A kind of high-speed overload rolling bearing extreme pressure anti-wear additives and preparation method thereof | |
| CN106893623A (en) | Metal nano Graphene composite additive of self-rehabilitation | |
| CN109705952B (en) | Graphene extreme pressure antiwear agent | |
| CN103666649B (en) | A kind of engine repair agent and preparation method thereof | |
| CN117625295B (en) | Dry film 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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220513 |