CN111117727A - Efficient lubricating oil composite antioxidant and preparation method thereof - Google Patents
Efficient lubricating oil composite antioxidant and preparation method thereof Download PDFInfo
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- CN111117727A CN111117727A CN201911355304.9A CN201911355304A CN111117727A CN 111117727 A CN111117727 A CN 111117727A CN 201911355304 A CN201911355304 A CN 201911355304A CN 111117727 A CN111117727 A CN 111117727A
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- composite antioxidant
- lubricating oil
- oil composite
- alkylphenol
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- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 86
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- -1 alkyl diphenylamine Chemical compound 0.000 claims abstract description 61
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000006078 metal deactivator Substances 0.000 claims abstract description 27
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- BIGYLAKFCGVRAN-UHFFFAOYSA-N 1,3,4-thiadiazolidine-2,5-dithione Chemical compound S=C1NNC(=S)S1 BIGYLAKFCGVRAN-UHFFFAOYSA-N 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N acrylic acid methyl ester Natural products COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- LVZUNTGFCXNQAF-UHFFFAOYSA-N n-nonyl-n-phenylaniline Chemical compound C=1C=CC=CC=1N(CCCCCCCCC)C1=CC=CC=C1 LVZUNTGFCXNQAF-UHFFFAOYSA-N 0.000 claims description 6
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 5
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 5
- RQVGZVZFVNMBGS-UHFFFAOYSA-N n-octyl-n-phenylaniline Chemical compound C=1C=CC=CC=1N(CCCCCCCC)C1=CC=CC=C1 RQVGZVZFVNMBGS-UHFFFAOYSA-N 0.000 claims description 5
- MDWVSAYEQPLWMX-UHFFFAOYSA-N 4,4'-Methylenebis(2,6-di-tert-butylphenol) Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 MDWVSAYEQPLWMX-UHFFFAOYSA-N 0.000 claims description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012964 benzotriazole Substances 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- DKCPKDPYUFEZCP-UHFFFAOYSA-N 2,6-di-tert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O DKCPKDPYUFEZCP-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 239000010725 compressor oil Substances 0.000 abstract description 7
- 239000010720 hydraulic oil Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 description 17
- 239000002199 base oil Substances 0.000 description 16
- 239000003921 oil Substances 0.000 description 14
- 238000007254 oxidation reaction Methods 0.000 description 10
- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 9
- 239000002480 mineral oil Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000007689 inspection Methods 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920013639 polyalphaolefin Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
-
- 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
-
- 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
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
- C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
- C10M2219/106—Thiadiazoles
Abstract
The invention provides a high-efficiency lubricating oil composite antioxidant and a preparation method thereof, wherein the high-efficiency lubricating oil composite antioxidant comprises the following components in parts by weight: 20-35 parts of alkyl diphenylamine, 10-25 parts of alkylphenol, 1-10 parts of phenolic acrylate, 45-55 parts of aminothioester and 0.1-0.5 part of metal deactivator. Through the technical scheme of the invention, the prepared high-efficiency lubricating oil composite antioxidant has the advantages of easily available raw materials, common raw materials, low price and obvious antioxidant effect improvement, and when the high-efficiency lubricating oil composite antioxidant is added into air compressor oil or hydraulic oil, the rotating oxygen bomb time can reach more than one thousand minutes by 0.5 percent of addition.
Description
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to a high-efficiency lubricating oil composite antioxidant and a preparation method of the high-efficiency lubricating oil composite antioxidant.
Background
With the development of equipment manufacturing and automobile industry, the lubrication of mechanical parts is more and more emphasized by mechanical manufacturing and users, and the problem of oil oxidation is more and more prominent in the use process of lubricating oil. In particular, the lubrication parts of machines such as air compressors and hydraulic equipment are very easy to generate high temperature, and oil products are oxidized and deteriorated too fast, which leads to increase of maintenance cost and shortening of the service life of the mechanical equipment.
Therefore, the development of efficient antioxidant complexing agents for lubricating oil is urgently needed, and oil products prepared by the complexing agents are applied to modern mechanical equipment to greatly improve the oxidation stability of the lubricating oil products and integrally improve the antioxidant performance of domestic lubricating oil.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art or the related art.
The invention aims to provide a high-efficiency lubricating oil composite antioxidant and a preparation method of the high-efficiency lubricating oil composite antioxidant.
In order to achieve the purpose, the technical scheme of the first aspect of the invention provides a high-efficiency lubricating oil composite antioxidant, which comprises the following components in parts by weight: 20-35 parts of alkyl diphenylamine, 10-25 parts of alkylphenol, 1-10 parts of phenolic acrylate, 45-55 parts of aminothioester and 0.1-0.5 part of metal deactivator.
Preferably, the alkyl diphenylamine is one or more of octyl diphenylamine and nonyl diphenylamine.
Preferably, the alkylphenol is one or more of 2, 6-di-tert-butyl-p-cresol, 2, 6-di-tert-butylphenol and 4, 4-methylenebis (2, 6-di-tert-butylphenol).
Preferably, the metal deactivator is one or more of N, N' -di-N-butylaminomethylene benzotriazole and 2, 5-dimercaptothiadiazole.
Preferably, the phenolic acrylate is one or more of 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate and 3, 5-di-tert-butyl-4-hydroxyphenyl ethyl acrylate.
Preferably, the effective content of the alkylphenol is 99.50-99.99%; the effective content of the phenolic acrylate is 98.0-99.99%.
Preferably, the content of the alkyl diphenylamine nitrogen is 4.0-5.0%, and the total base number is 155
mgKOH/g～175mgKOH/g。
Preferably, the sulfur content of the aminothioester is 28 to 31 percent.
In the technical scheme, the raw materials for preparing the high-efficiency lubricating oil composite antioxidant are easily available, the raw materials are relatively common, the price is low, and the antioxidant effect is obviously improved, the high-efficiency lubricating oil composite antioxidant provided by the invention can be dissolved in various mineral oils, the sensitivity to various mineral oils is good, and simultaneously, the antioxidant capacity of various mineral oils is greatly improved, the high-efficiency lubricating oil composite antioxidant provided by the invention is beneficial to breaking the situation that foreign companies monopolize the Chinese market for high-grade lubricating oil composite agents, the national branding, the autonomy and the market for composite agents are fully promoted, and the condition that the high-performance lubricating oil composite agents are imported is changed, and if the high-efficiency lubricating oil composite antioxidant provided by the invention is added into air compressor oil or hydraulic oil, the dosage of 0.5 percent can ensure that the rotating oxygen bomb time reaches more than one thousand minutes.
In the above technical scheme, preferably, the high-efficiency lubricating oil composite antioxidant comprises the following components in parts by weight: 23 parts of alkyl diphenylamine, 15.5 parts of alkylphenol, 6 parts of phenolic acrylate, 55 parts of aminothio ester and 0.5 part of metal deactivator.
In the technical scheme, the component proportion of the high-efficiency lubricating oil composite antioxidant is further optimized, the antioxidant capacity of various mineral oils is further improved, and the high-efficiency lubricating oil composite antioxidant is added into 150N base oil, so that the rotating oxygen bomb time can reach more than one thousand to four percent by 0.5 percent of the additive amount.
The antioxidant mechanism of the high-efficiency lubricating oil composite antioxidant provided by the invention is as follows:
the oxidation of lubricating oil is caused by the action of light, heat, transition metal and the like, free radicals are firstly generated and then react with oxygen to generate peroxide, the peroxide is decomposed to generate peroxide free radicals, and a series of chain reactions lead the oil to be finally oxidized and deteriorated. It can be seen that the most fundamental method to prevent oxidation is to capture free radicals. The components of the high-efficiency lubricating oil composite antioxidant provided by the invention are mostly phenol low-temperature antioxidants and high-temperature-resistant amine antioxidants, and the phenol low-temperature antioxidants and the high-efficiency amine antioxidants are high-efficiency free radical trapping agents and can terminate chain reactions when an oil product is subjected to an oxidation reaction initially to generate free radicals, so that the oil product is prevented from being oxidized.
The technical scheme of the second aspect of the invention also provides a preparation method of the high-efficiency lubricating oil composite antioxidant, which comprises the following steps: weighing the alkyl diphenylamine according to the formula, adding the alkyl diphenylamine into a reaction kettle, stirring, heating to 50-60 ℃, and then sequentially adding the phenol, the phenolic acrylate, the aminothioester and the metal deactivator according to the formula; after the addition is finished, the temperature is raised to 60-70 ℃, the mixture is stirred for 1.5-2 h under normal pressure, and the mixture is filtered and barreled after being qualified.
In the technical scheme, the preparation method of the efficient lubricating oil composite antioxidant is simple, the process is simple, the operability is strong, the preparation cost is low, and the large-scale popularization and use are facilitated.
The rotating speed of stirring can be 80 r/min; the product is uniformly stirred with 150N base oil at normal temperature according to the adding amount of 1 percent, and the mixture is transparent and is judged to be qualified after no turbidity exists.
Through the technical scheme, (1) the raw materials for preparing the high-efficiency lubricating oil composite antioxidant are easily available, the raw materials are common, the price is low, and the antioxidant effect is obviously improved. (2) The high-efficiency lubricating oil composite antioxidant provided by the invention can be dissolved in various mineral oils, has good sensitivity to various mineral oils, and simultaneously greatly improves the oxidation resistance of various mineral oils. (3) The high-efficiency lubricating oil composite antioxidant provided by the invention is beneficial to breaking the situation that foreign companies monopolize the Chinese market for high-grade lubricating oil composite agents, fully pushes national branding, autonomy and marketization of composite agents, and changes the condition that the high-performance lubricating oil composite agents are imported. (4) The high-efficiency lubricating oil composite antioxidant provided by the invention is added into air compressor oil or hydraulic oil, and the rotating oxygen bomb time can reach more than one thousand minutes by 0.5% of the additive amount.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The invention discloses a high-efficiency lubricating oil composite antioxidant and a preparation method thereof, and a person skilled in the art can use the contents for reference and appropriately improve process parameters to realize the preparation. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The raw materials adopted by the invention can be purchased from the market, are common and have low price.
The invention is further illustrated by the following examples:
example 1
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 30 parts of alkyl diphenylamine, 16 parts of alkylphenol, 8 parts of phenolic acrylate, 46 parts of aminothio ester and 0.1 part of metal deactivator.
The alkyl diphenylamine is octyl diphenylamine; the alkylphenol is 2, 6-di-tert-butyl-p-cresol; the metal deactivator is 2, 5-dimercaptothiadiazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 30 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 16 parts of alkylphenol, 8 parts of phenol acrylate, 46 parts of aminothio ester and 0.1 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
Example 2
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 30 parts of alkyl diphenylamine, 20 parts of alkylphenol, 6 parts of phenolic acrylate, 43.7 parts of aminothio ester and 0.3 part of metal deactivator.
The alkyl diphenylamine is octyl diphenylamine; the alkylphenol is 2, 6-di-tert-butyl-p-cresol; the metal deactivator is N, N' -di-N-butylaminomethylene benzotriazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 34 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 20 parts of alkylphenol, 6 parts of phenol acrylate, 43.7 parts of aminothio ester and 0.3 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
Example 3
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 23 parts of alkyl diphenylamine, 15.5 parts of alkylphenol, 6 parts of phenolic acrylate, 55 parts of aminothio ester and 0.5 part of metal deactivator.
The alkyl diphenylamine is nonyl diphenylamine; the alkylphenol is 2, 6-di-tert-butylphenol; the metal deactivator is 2, 5-dimercaptothiadiazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 23 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 15.5 parts of alkylphenol, 6 parts of phenol acrylate, 55 parts of aminothio ester and 0.5 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
Example 4
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 20 parts of alkyl diphenylamine, 25 parts of alkylphenol, 8.9 parts of phenolic acrylate, 46 parts of aminothio ester and 0.1 part of metal deactivator.
The alkyl diphenylamine is a mixture of octyl diphenylamine and nonyl diphenylamine in a ratio of 1: 1; the alkylphenol is 2, 6-di-tert-butyl-p-cresol; the metal deactivator is 2, 5-dimercaptothiadiazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl ethyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 20 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 25 parts of alkylphenol, 8.9 parts of phenolic acrylate, 46 parts of aminothio ester and 0.1 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
Example 5
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 20 parts of alkyl diphenylamine, 24.9 parts of alkylphenol, 10 parts of phenolic acrylate, 45 parts of aminothio ester and 0.1 part of metal deactivator.
The alkyl diphenylamine is nonyl diphenylamine; the alkylphenol is 4, 4-methylene bis (2, 6-di-tert-butylphenol); the metal deactivator is 2, 5-dimercaptothiadiazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl ethyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 20 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 24.9 parts of alkylphenol, 10 parts of phenol acrylate, 45 parts of aminothio ester and 0.1 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
Example 6
The efficient lubricating oil composite antioxidant comprises the following components in parts by weight: 35 parts of alkyl diphenylamine, 10 parts of alkylphenol, 1 part of phenolic acrylate, 53.9 parts of aminothio ester and 0.1 part of metal deactivator.
The alkyl diphenylamine is nonyl diphenylamine; the alkylphenol is 4, 4-methylene bis (2, 6-di-tert-butylphenol); the metal deactivator is N, N' -di-N-butylaminomethylene benzotriazole; the phenol acrylate is 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate.
The preparation method of the high-efficiency lubricating oil composite antioxidant comprises the following steps:
weighing 35 parts of alkyl diphenylamine, adding the alkyl diphenylamine into a reaction kettle, starting stirring, heating to 50-60 ℃, stirring at a rotating speed of 80r/min for 20min, and sequentially adding 10 parts of alkylphenol, 1 part of phenolic acrylate, 53.9 parts of aminothioester and 0.1 part of metal deactivator;
after the addition is finished, the temperature is raised to 60-70 ℃, the stirring is carried out for 1.5-2 h under normal pressure, the stirring rotating speed is 80r/min, and the high-efficiency lubricating oil composite antioxidant provided by the invention is prepared after the inspection is qualified.
The prepared high-efficiency lubricating oil composite antioxidant is added into 150N base oil according to the dosage of 0.5 percent for testing, and the test results are shown in table 1.
A complex antioxidant sold by a foreign additive company was added to 150N base oil at a dosage of 0.5% for comparison.
After the oil products prepared by using the high-efficiency compound antioxidant for lubricating oil provided in the embodiments 1 to 6 of the present invention and the oil products prepared by using the compound antioxidant sold by a certain foreign additive company are tested, the test results are shown in the following table 1,
the test method SH/T0193 specifically comprises the steps of putting a sample, water and a copper catalyst coil into a glass sample holder with a cover, and placing the glass sample holder in an oxygen bomb provided with a pressure gauge. The oxygen bomb was charged with oxygen at a pressure of 620kpa, and placed in a specified constant temperature oil bath to be axially rotated at an angle of 30 ° to the horizontal plane at a speed of 100 r/min. The time (min) required for the test to reach the specified pressure drop is the oxidation stability of the sample.
Application example 1
The high-efficiency lubricating oil composite antioxidant provided by the invention is added into 350N base oil according to the proportion of 0.5%, and is uniformly mixed.
Application example 2
The high-efficiency lubricating oil composite antioxidant provided by the invention is added into 150SN base oil according to the proportion of 0.5%, and is uniformly mixed.
Application example 3
The high-efficiency lubricating oil composite antioxidant provided by the invention is added into 500N base oil according to the proportion of 0.5%, and is uniformly mixed.
Application example 4
The high-efficiency lubricating oil composite antioxidant provided by the invention is added into 10# white oil according to the proportion of 0.5% and is uniformly mixed.
Application example 5
The high-efficiency lubricating oil composite antioxidant provided by the invention is added into poly α -olefin synthetic base oil PAO 6# in a proportion of 0.5% and uniformly mixed.
The samples obtained in application examples 1 to 5 were subjected to the test, and the test results are shown in table 2 below:
the test results obtained in application examples 1, 2, 3, 4 and 5 show that the high-efficiency lubricating oil composite antioxidant provided by the invention has obvious good compatibility with various base oils when being added into various mineral oils or synthetic base oils, and can obviously improve the oxidation stability of various base oils.
Application example 6
The high-efficiency lubricating oil composite antioxidant prepared in the embodiment 3 of the invention is added into L-L-DAB air compressor oil according to the proportion of 1% at the temperature of 50-60 ℃ and is uniformly mixed.
And (3) detecting the sample obtained in the application example 6 and the L-DAB air compressor oil without the high-efficiency lubricating oil composite antioxidant, wherein the obtained detection results are shown in the following table 3:
the detection result obtained by the application example 6 shows that the antioxidant capacity of the air compressor oil can be effectively improved by adding the product into the air compressor oil, so that the oxidation time of the oil product in the using process is prolonged, and the stability of the oil product can be effectively protected by the invention.
Application example 7
The high-efficiency lubricating oil composite antioxidant prepared in the embodiment 3 of the invention is added into HM 46# antiwear hydraulic oil in a proportion of 1% at a temperature of 50-60 ℃, and is mixed uniformly.
The sample obtained in application example 7 and HM 46# anti-wear hydraulic oil without adding the high-efficiency lubricating oil composite antioxidant are detected, and the detection results are shown in the following table 4:
the detection result obtained by the application example 7 shows that the antioxidant capacity of the hydraulic oil can be effectively improved by adding the product into the antiwear hydraulic oil, so that the oxidation time of an oil product in the using process is prolonged, and the stability of the oil product can be effectively protected by the invention.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The efficient lubricating oil composite antioxidant is characterized by comprising the following components in parts by weight:
20-35 parts of alkyl diphenylamine, 10-25 parts of alkylphenol, 1-10 parts of phenolic acrylate, 45-55 parts of aminothioester and 0.1-0.5 part of metal deactivator.
2. The high efficiency lubricant composite antioxidant of claim 1,
the alkyl diphenylamine is one or more of octyl diphenylamine and nonyl diphenylamine.
3. The high efficiency lubricant composite antioxidant of claim 1,
the alkylphenol is one or more of 2, 6-di-tert-butyl-p-cresol, 2, 6-di-tert-butylphenol and 4, 4-methylene-bis (2, 6-di-tert-butylphenol).
4. The high efficiency lubricant composite antioxidant of claim 1,
the metal deactivator is one or more of N, N' -di-N-butylaminomethylene benzotriazole and 2, 5-dimercaptothiadiazole.
5. The high efficiency lubricant composite antioxidant of claim 1,
the phenolic acrylate is one or more of 3, 5-di-tert-butyl-4-hydroxyphenyl methyl acrylate and 3, 5-di-tert-butyl-4-hydroxyphenyl ethyl acrylate.
6. The high efficiency lubricant composite antioxidant of claim 1,
the effective content of the alkylphenol is 99.50-99.99%;
the effective content of the phenolic acrylate is 98.0-99.99%.
7. The high efficiency lubricant composite antioxidant of claim 1,
the content of the alkyl diphenylamine nitrogen is 4.0-5.0%, and the total base number is 155 mgKOH/g-175 mgKOH/g.
8. The high efficiency lubricant composite antioxidant of claim 1,
the sulfur content of the amino thioester is 28 to 31 percent.
9. The high-efficiency lubricating oil composite antioxidant as claimed in any one of claims 1 to 8, which is characterized by comprising the following components in parts by weight:
23 parts of alkyl diphenylamine, 15.5 parts of alkylphenol, 6 parts of phenolic acrylate, 55 parts of aminothio ester and 0.5 part of metal deactivator.
10. The preparation method of the high-efficiency lubricating oil composite antioxidant is suitable for the high-efficiency lubricating oil composite antioxidant as described in any one of claims 1 to 9, and is characterized by comprising the following steps:
weighing alkyl diphenylamine according to the formula, adding the alkyl diphenylamine into a reaction kettle, stirring, heating to 50-60 ℃, and then sequentially adding alkylphenol, phenolic acrylate, aminothioester and a metal deactivator according to the formula;
after the addition is finished, the temperature is raised to 60-70 ℃, the mixture is stirred for 1.5-2 h under normal pressure, and the mixture is filtered and barreled after being qualified.
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