CN110747041A - Preparation method of high-temperature oxidation-resistant anti-corrosion antiwear agent - Google Patents

Preparation method of high-temperature oxidation-resistant anti-corrosion antiwear agent Download PDF

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CN110747041A
CN110747041A CN201910980797.9A CN201910980797A CN110747041A CN 110747041 A CN110747041 A CN 110747041A CN 201910980797 A CN201910980797 A CN 201910980797A CN 110747041 A CN110747041 A CN 110747041A
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parts
corrosion
stirring
preparation
temperature oxidation
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余十轮
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/02—Polyamines
    • C08G73/026—Wholly aromatic polyamines
    • C08G73/0266—Polyanilines or 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
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • 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
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • C10M2207/0225—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C10M2207/1233—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic 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
    • C10M2207/127—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
    • C10M2207/1273—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 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
    • C10M2207/40—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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/402—Castor oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/046—Polyamines, i.e. macromoleculars obtained by condensation of more than eleven amine monomers
    • 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
    • C10M2219/042—Sulfate esters
    • 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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  • General Chemical & Material Sciences (AREA)
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  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses a preparation method of a high-temperature oxidation-resistant anti-corrosion anti-wear agent, and belongs to the technical field of anti-wear agent preparation. In the process of the aluminum oxide/polyaniline core-shell lubricating particles, after the aluminum oxide particles are modified by the silane coupling agent, the bonding force between the aluminum oxide particles and the polyaniline is enhanced, the dispersibility of the aluminum oxide particles in the anti-wear agent is improved, the agglomeration phenomenon of the aluminum oxide particles can be effectively inhibited, the distribution uniformity of the aluminum oxide particles in the anti-wear agent is ensured, the rolling anti-wear effect of the aluminum oxide particles in the anti-wear agent is improved, the lubricating particles take the polyaniline as a shell structure, and because the polyaniline has special redox capability, a very thin oxide film is formed on the metal surface due to the inductive coupling effect of the polyaniline, so that the anti-wear agent has better anti-corrosion protection capability on mechanical equipment; the modified antioxidant is prepared by modifying phenol antioxidant 1010 with diphenylamine, can obviously improve the high-temperature antioxidant performance, and has wide application prospect.

Description

Preparation method of high-temperature oxidation-resistant anti-corrosion antiwear agent
Technical Field
The invention discloses a preparation method of a high-temperature oxidation-resistant anti-corrosion anti-wear agent, and belongs to the technical field of anti-wear agent preparation.
Background
The antiwear agent is a high-tech additive for engine oil (lubricating oil), and the antiwear agents usually used in the lubricating oil include sulfur type antiwear agents, phosphorus type antiwear agents, sulfur and phosphorus type antiwear agents, halogen type antiwear agents, organic metal type antiwear agents and boron type antiwear agents, which can reduce the abrasion of an engine and increase the power of the engine.
Because the traditional antiwear agent mainly contains substances which are corrosive or harmful to the environment, such as sulfur, phosphorus and the like, the antiwear agent is harmful to parts per se after being used for a long time, and also causes pollution to the environment, and has the problems of poor multifunctionality, poor oxidation resistance, detergency resistance, poor repair function and the like, and can not meet the requirements of higher and higher metal processing level and green manufacture. With the intensive research of nanotechnology and nanomaterials, the application prospect of the nanoparticles in the lubrication field is gradually known. In recent years, researchers at home and abroad have conducted a great deal of research work 0 on nano lubricating oil additives. The use of the inorganic nano additive can effectively improve the wear resistance and the bearing capacity of the antiwear agent, has good development and application prospects, and becomes an important development direction of lubricating materials. However, common inorganic nanoparticles are inherently unstable, are easily affected by the environment after polymerization, can generate a layering phenomenon after long-term storage, and are easily precipitated after being added into base oil, so that the stable dispersibility of the nanoparticles in the base oil is affected, and the anti-friction effect of the lubricating oil is affected.
The commonly used antiwear agents on the market at present have the defects of poor extreme pressure antiwear performance and easy oxidation at high temperature, so the invention of the antiwear agent with strong antiwear performance and good high-temperature stability has positive significance in the technical field of the preparation of the antiwear agent.
Disclosure of Invention
The invention mainly solves the technical problems that the existing antiwear agent has poor antiwear effect, is easy to oxidize under an extreme pressure high temperature state, and oxidized lubricating oil possibly generates chemical corrosion on engine parts, and provides a preparation method of a high temperature oxidation resistant anti-corrosion antiwear agent.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high-temperature oxidation resistant anti-corrosion antiwear agent is characterized by comprising the following specific preparation steps:
adding dibasic acid, dihydric alcohol and vegetable oil acid into a stirring reaction kettle with a reflux device, starting a stirrer under the protection of nitrogen, stirring and mixing at the rotating speed of 200-230 r/min, heating the stirring reaction kettle to 50-65 ℃, preserving heat, stirring and reacting until the reflux device does not discharge water, adding alumina/polyaniline core-shell lubricating particles, a modified antioxidant and zinc stearate into the stirring reaction kettle, stirring and dispersing at normal temperature for 40-50 min, discharging, canning and sealing to obtain a high-temperature oxidation resistant anticorrosion antiwear agent;
the preparation method of the aluminum oxide/polyaniline core-shell lubricating particles comprises the following specific steps:
(1) adding 100-120 parts by weight of deionized water and 10-12 parts by weight of cationic emulsifier into a three-neck flask, stirring and pre-emulsifying for 30-40 min, adding 20-25 parts by weight of aniline, simultaneously dropwise adding 10-15 parts by weight of 5% ammonium persulfate solution into the three-neck flask at a dropping rate of 6-10 mL/min by using a dropping funnel, reacting at normal temperature for 4-5 h after dropwise adding, and discharging to obtain polyaniline emulsion;
(2) adding 1/4 volume of acetone into the polyaniline emulsion, carrying out chemical stirring demulsification for 3-4 h to obtain a demulsifying solution, placing the demulsifying solution in a high-speed centrifuge, carrying out centrifugal treatment at a rotating speed of 3000-4500 r/min for 10-12 min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake with deionized water for 3-5 times, placing a product obtained after suction filtration and washing in a vacuum drying oven with a set temperature of 40-45 ℃, drying for 12-14 h, grinding, and sieving with a 400-mesh sieve to obtain outer-layer rubber powder;
(3) dropwise adding ammonia water with the mass fraction of 5% into an aluminum nitrate solution with the mass fraction of 20% until the pH of the solution is 9.2-9.5, standing for 5-10 min to obtain a suspension, adding 20-25 parts of the suspension into 200-300 parts of absolute ethyl alcohol in parts by weight, stirring, adding 5-8 parts of a silane coupling agent, 10-15 parts of outer layer rubber powder and 4-5 parts of hydrogen peroxide with the mass fraction of 10%, heating in a water bath to 40-45 ℃, performing centrifugal treatment, removing filtrate, and washing to obtain aluminum oxide/polyaniline core-shell lubricating particles;
the modified antioxidant is prepared by the following specific steps:
(1) adding 40-60 parts by weight of antioxidant and 30-35 parts by weight of diphenylamine into a single-neck flask, adding 300-350 parts by weight of n-octane serving as a solvent, magnetically stirring at a rotating speed of 300-350 r/min for 3-4 hours under the protection of nitrogen, heating to 140-160 ℃, adding 80-100 parts by weight of di-tert-butyl peroxide into the single-neck flask, and stirring for reacting for 3-4 hours to obtain a reaction product;
(2) installing a condensation reflux device on the single-mouth flask, heating to 140-150 ℃, distilling for 1-2 hours, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol, freezing for 2-3 hours to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake with acetone for 3-5 times, placing in an oven, heating to 90-100 ℃, and drying for 4-5 hours to obtain a modified antioxidant;
the vegetable oil acid is prepared by the following specific steps:
mixing and stirring vegetable oil, sodium hydroxide and 75% by mass of ethanol solution according to a mass ratio of 5: 1: 10 for 15-20 min to obtain saponified solution, placing the saponified solution into a separating funnel, adding 20% by mass of hydrochloric acid into the separating funnel to make the pH of the saponified solution be 3-3.5, standing for 10-15 min, separating to remove a water layer to obtain an oil layer, and washing the oil layer with deionized water for 3-5 times to obtain the vegetable oleic acid.
The high-temperature oxidation resistant, corrosion resistant and antiwear agent is characterized in that raw materials of the high-temperature oxidation resistant, corrosion resistant and antiwear agent in the specific preparation steps comprise, by weight, 30-35 parts of dibasic acid, 40-50 parts of dihydric alcohol, 35-40 parts of vegetable oleic acid and 5-10 parts of alumina/polyphenyl
The lubricant comprises amine core-shell lubricating particles, 6-8 parts of modified antioxidant and 4-5 parts of zinc stearate.
In the specific preparation steps of the high-temperature oxidation resistant anti-corrosion antiwear agent, the diol is preferably neopentyl glycol with low polymerization degree
Polyethylene glycol.
The dibasic acid in the specific preparation steps of the high-temperature oxidation resistant anti-corrosion antiwear agent is preferably adipic acid, azelaic acid and sunflower
Diacid or phthalic acid.
The cationic emulsifier used in the specific preparation step (1) of the alumina/polyaniline core-shell lubricating particles is preferably sodium dodecyl sulfate or sodium dodecyl sulfate.
The silane coupling agent in the specific preparation step (3) of the alumina/polyaniline core-shell lubricating particles is preferably one of kh550 and kh 570.
The antioxidant used in the specific preparation step (1) of the modified antioxidant is preferably antioxidant 1010.
The modified antioxidant is prepared in the step (2) at the freezing temperature of-20 to-15 ℃.
The vegetable oil used in the specific preparation step of the vegetable oil acid is preferably one of peanut oil, castor oil, rapeseed oil and soybean oil.
The invention has the beneficial effects that:
(1) the invention uses cation emulsifier to pre-emulsify aniline monomer, dropwise adds ammonium persulfate as initiator to prepare polyaniline emulsion, then carries out demulsification centrifugation to prepare outer rubber powder of alumina/polyaniline core-shell lubricating particles, then adds rubber powder, silane coupling agent and hydrogen peroxide into alkalescent suspension containing aluminum ions, carries out centrifugation after micro-thermal reaction to prepare alumina/polyaniline core-shell lubricating particles, then esterifies raw materials such as vegetable oleic acid, binary acid and dihydric alcohol to prepare alumina/core-shell lubricating particles and modified antioxidant to prepare high-temperature oxidation resistant anti-corrosion anti-wear agent, in the process of alumina/polyaniline core-shell lubricating particles, the alumina particles are modified by silane coupling agent to enhance the bonding force with polyaniline, and improve the dispersibility of alumina particles in anti-wear agent, the polyaniline is used as the shell structure of the lubricating particles, and because the polyaniline has special oxidation-reduction capability, a very thin oxide film is formed on the metal surface due to the inductive coupling effect of the polyaniline, so that the corrosion resistance is increased, the corrosion rate is reduced, and the effect is distributed on the metal surface under the whole film, so that the anti-wear agent has better anti-corrosion protection capability on mechanical equipment;
(2) the antiwear agent of the invention takes a long chain of vegetable oil oleic acid as a framework to synthesize the ester antiwear agent through the reaction of dibasic acid and dihydric alcohol, because ester oil molecules are oxidized under the action of factors such as high temperature and oxygen generated by friction and the like to generate alkyl free radicals and alkyl peroxy radicals, and the stability of a product formed by combining a common phenol antioxidant and the free radicals is poor, the modified antioxidant is prepared by modifying the phenol antioxidant 1010 with diphenylamine, can obviously improve the high-temperature antioxidant performance, and reacts with the alkyl free radicals and the alkyl peroxy radicals to generate nitrogen free radicals and alcohol and acid compounds with lower activity, the nitrogen free radicals are very stable under the influence of the conjugated effect of benzene rings, do not have enough activity to react with the ester oil molecules and can only react with other free radicals, and the nitrogen free radicals and the peroxy radicals can continue to react with the peroxy radicals to generate the nitroxide radicals, the continuous regeneration of the nitroxide radical can regenerate the anti-oxidation effect of the modified antioxidant, so that the anti-oxidation process can be continued, and the generated antioxidant intermediate has high stability under the conjugation of a benzene ring and can only generate chain termination reaction of free radicals with other active free radicals and peroxy radicals, so that the anti-wear agent has stable high-temperature anti-oxidation performance and wide application prospect.
Detailed Description
Adding 100-120 parts of deionized water and 10-12 parts of cationic emulsifier into a three-neck flask, stirring and pre-emulsifying for 30-40 min, adding 20-25 parts of aniline, simultaneously dropwise adding 10-15 parts of ammonium persulfate solution with the mass fraction of 5% into the three-neck flask at the dropping speed of 6-10 mL/min by using a dropping funnel, reacting for 4-5 h at normal temperature after dropwise adding, and discharging to obtain polyaniline emulsion, wherein the cationic emulsifier is preferably sodium dodecyl sulfate or sodium dodecyl sulfate; adding 1/4 volume of acetone into the polyaniline emulsion, carrying out chemical stirring demulsification for 3-4 h to obtain a demulsifying solution, placing the demulsifying solution in a high-speed centrifuge, carrying out centrifugal treatment at a rotating speed of 3000-4500 r/min for 10-12 min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake with deionized water for 3-5 times, placing a product obtained after suction filtration and washing in a vacuum drying oven with a set temperature of 40-45 ℃, drying for 12-14 h, grinding, and sieving with a 400-mesh sieve to obtain outer-layer rubber powder; dropwise adding 5% ammonia water into 20% aluminum nitrate solution by mass until the pH of the solution is 9.2-9.5, standing for 5-10 min to obtain a suspension, adding 20-25 parts of the suspension into 200-300 parts of absolute ethyl alcohol by weight, stirring, adding 5-8 parts of a silane coupling agent, 10-15 parts of outer layer rubber powder and 4-5 parts of 10% hydrogen peroxide by mass, heating in a water bath to 40-45 ℃, performing centrifugal treatment, removing filtrate, and washing to obtain the aluminum oxide/polyaniline core-shell lubricating particles, wherein the silane coupling agent is preferably one of kh550 and kh 570. Adding 40-60 parts by weight of antioxidant 1010 and 30-35 parts by weight of diphenylamine into a single-neck flask, adding 300-350 parts by weight of n-octane serving as a solvent, magnetically stirring at a rotating speed of 300-350 r/min for 3-4 hours under the protection of nitrogen, heating to 140-160 ℃, adding 80-100 parts by weight of di-tert-butyl peroxide into the single-neck flask, and stirring for reacting for 3-4 hours to obtain a reaction product; installing a condensation reflux device on the single-neck flask, heating to 140-150 ℃, distilling for 1-2 hours, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol at the temperature of-20 to-15 ℃ for freezing for 2-3 hours to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake with acetone for 3-5 times, placing the filter cake in an oven, heating to 90-100 ℃, and drying for 4-5 hours to obtain a modified antioxidant; mixing and stirring vegetable oil, sodium hydroxide and 75% by mass of ethanol solution according to a mass ratio of 5: 1: 10 for 15-20 min to obtain saponified liquid, placing the saponified liquid in a separating funnel, adding 20% by mass of hydrochloric acid into the separating funnel to enable the pH of the saponified liquid to be 3-3.5, standing for 10-15 min, separating to remove a water layer to obtain an oil layer, washing the oil layer with deionized water for 3-5 times to obtain vegetable oleic acid, wherein the vegetable oil is preferably one of peanut oil, castor oil, rapeseed oil and soybean oil; according to the weight parts, 30-35 parts of dibasic acid, 40-50 parts of dihydric alcohol and 35-40 parts of vegetable oil acid are added into a stirring reaction kettle with a reflux device, a stirrer is started under the protection of nitrogen, the stirring reaction kettle is stirred and mixed at the rotating speed of 200-230 r/min, the stirring reaction kettle is heated to 50-65 ℃, the temperature is kept and the stirring reaction is carried out until the reflux device does not produce water, 5-10 parts of alumina/polyaniline core-shell lubricating particles, 6-8 parts of modified antioxidant and 4-5 parts of zinc stearate are added into the stirring reaction kettle, the mixture is stirred and dispersed at the normal temperature for 40-50 min, and the mixture is discharged and canned and sealed to obtain the high-temperature oxidation-resistant anti-corrosion antiwear agent, wherein the dibasic acid is preferably neopentyl glycol or low-polymerization-degree polyethylene glycol, and the dibasic acid is preferably one of adipic acid, azelaic acid, sebacic acid and.
Example 1
Adding 100 parts of deionized water and 10 parts of cationic emulsifier in parts by weight into a three-neck flask, stirring and pre-emulsifying for 30min, adding 20 parts of aniline, simultaneously dropwise adding 10 parts of ammonium persulfate solution with the mass fraction of 5% into the three-neck flask at the dropwise adding speed of 6mL/min by using a dropping funnel, reacting for 4h at normal temperature after dropwise adding is finished, and discharging to obtain polyaniline emulsion, wherein the cationic emulsifier is preferably sodium dodecyl sulfate or sodium dodecyl sulfate; adding 1/4 volume of acetone into the polyaniline emulsion, carrying out chemical stirring and demulsification for 3h to obtain a demulsifying solution, placing the demulsifying solution in a high-speed centrifuge, carrying out centrifugal treatment for 10min at the rotating speed of 3000r/min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake for 3 times by using deionized water, placing a product obtained after the suction filtration and the washing in a vacuum drying oven with the set temperature of 40 ℃, drying for 12h, grinding, and sieving by using a 400-mesh sieve to obtain outer-layer rubber powder; dropwise adding 5% ammonia water into 20% aluminum nitrate solution until the pH value of the solution is 9.2, standing for 5min to obtain a suspension, adding 20 parts of the suspension into 200 parts of absolute ethyl alcohol by weight, stirring, adding 5 parts of a silane coupling agent, 10 parts of outer layer rubber powder and 4 parts of 10% hydrogen peroxide by weight, heating in a water bath to 40 ℃, carrying out centrifugal treatment, removing filtrate, and washing to obtain the alumina/core-shell polyaniline lubricating particles, wherein the silane coupling agent is preferably one of kh550 and kh 570. Adding 40 parts by weight of antioxidant 1010 and 30 parts by weight of diphenylamine into a single-neck flask, adding 300 parts by weight of n-octane serving as a solvent, magnetically stirring for 3 hours at a rotating speed of 300r/min under the protection of nitrogen, heating to 140 ℃, adding 80 parts by weight of di-tert-butyl peroxide into the single-neck flask, and stirring for 3 hours to obtain a reaction product; installing a condensation reflux device on the single-mouth flask, heating to 140 ℃, distilling for 1h, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol at the temperature of-20 ℃ for freezing for 2h to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake for 3 times by using acetone, placing the filter cake in an oven, heating to 90 ℃, and drying for 4h to obtain a modified antioxidant; mixing vegetable oil, sodium hydroxide and 75% ethanol solution according to a mass ratio of 5: 1: 10, stirring for 15min to obtain saponified solution, placing the saponified solution into a separating funnel, adding 20% hydrochloric acid into the separating funnel to make the pH of the saponified solution be 3, standing for 10min, separating to remove a water layer to obtain an oil layer, washing the oil layer with deionized water for 3 times to obtain vegetable oleic acid, wherein the vegetable oil is preferably peanut oil; adding 30 parts by weight of adipic acid, 40 parts by weight of neopentyl glycol and 35 parts by weight of vegetable oleic acid into a stirring reaction kettle with a reflux device, starting a stirrer under the protection of nitrogen, stirring and mixing at a rotating speed of 200r/min, heating the stirring reaction kettle to 50 ℃, carrying out heat preservation stirring reaction until the reflux device does not discharge water, adding 5 parts by weight of alumina/polyaniline core-shell lubricating particles, 6 parts by weight of modified antioxidant and 4 parts by weight of zinc stearate into the stirring reaction kettle, stirring and dispersing at normal temperature for 40min, discharging, canning and sealing to obtain the high-temperature oxidation-resistant anticorrosive antiwear agent.
Example 2
According to the weight parts, adding 110 parts of deionized water and 11 parts of cationic emulsifier into a three-neck flask, stirring and pre-emulsifying for 35min, adding 23 parts of aniline, simultaneously dropwise adding 13 parts of ammonium persulfate solution with the mass fraction of 5% into the three-neck flask at the dropwise adding speed of 8mL/min by using a dropping funnel, reacting at normal temperature for 4.5h after dropwise adding is finished, and discharging to obtain polyaniline emulsion, wherein the cationic emulsifier is preferably sodium dodecyl sulfate or sodium dodecyl sulfate; adding 1/4 volume of acetone into the polyaniline emulsion, carrying out chemical stirring and demulsification for 3.5h to obtain a demulsifying solution, placing the demulsifying solution in a high-speed centrifuge, carrying out centrifugal treatment for 11min at the rotating speed of 4000r/min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake for 4 times by using deionized water, placing a product obtained after the suction filtration and the washing in a vacuum drying oven with the set temperature of 42 ℃, drying for 13h, grinding, and sieving by using a 400-mesh sieve to obtain outer-layer rubber powder; dropwise adding 5% ammonia water into 20% aluminum nitrate solution until the pH value of the solution is 9.3, standing for 8min to obtain a suspension, adding 23 parts of the suspension into 250 parts of absolute ethyl alcohol by weight, stirring, adding 7 parts of a silane coupling agent, 13 parts of outer layer rubber powder and 4.5 parts of 10% hydrogen peroxide by weight, heating in a water bath to 43 ℃, carrying out centrifugal treatment, removing filtrate, and washing to obtain the aluminum oxide/polyaniline core-shell lubricating particles, wherein the silane coupling agent is preferably one of kh550 and kh 570. Adding 50 parts by weight of antioxidant 1010 and 33 parts by weight of diphenylamine into a single-neck flask, adding 330 parts by weight of n-octane serving as a solvent, magnetically stirring for 3-4 hours at a rotating speed of 320r/min under the protection of nitrogen, heating to 150 ℃, adding 90 parts by weight of di-tert-butyl peroxide into the single-neck flask, and stirring for reaction for 3.5 hours to obtain a reaction product; installing a condensation reflux device on the single-neck flask, heating to 145 ℃, distilling for 1.5h, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol at-18 ℃ for freezing for 2.5h to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake with acetone for 4 times, placing in an oven, heating to 95 ℃, and drying for 5h to obtain a modified antioxidant; mixing and stirring castor oil, sodium hydroxide and 75% by mass of ethanol solution according to a mass ratio of 5: 1: 10 for 20min to obtain saponified solution, placing the saponified solution in a separating funnel, adding 20% by mass of hydrochloric acid into the separating funnel to make the pH of the saponified solution be 3.5, standing for 15min, separating to remove a water layer to obtain an oil layer, and washing the oil layer with deionized water for 5 times to obtain vegetable oleic acid; adding 33 parts by weight of azelaic acid, 45 parts by weight of polyethylene glycol with low polymerization degree and 38 parts by weight of vegetable oil acid into a stirring reaction kettle with a reflux device, starting a stirrer under the protection of nitrogen, stirring and mixing at the rotating speed of 210r/min, heating the stirring reaction kettle to 55 ℃, keeping the temperature and stirring for reaction until the reflux device does not discharge water, adding 8 parts by weight of alumina/polyaniline core-shell lubricating particles, 7 parts by weight of modified antioxidant and 4 parts by weight of zinc stearate into the stirring reaction kettle, stirring and dispersing for 45min at normal temperature, discharging, canning and sealing to obtain the high-temperature oxidation resistant anti-corrosion and anti-wear agent.
Example 3
Adding 120 parts of deionized water and 12 parts of cationic emulsifier in parts by weight into a three-neck flask, stirring and pre-emulsifying for 40min, adding 25 parts of aniline, dropwise adding 15 parts of ammonium persulfate solution with the mass fraction of 5% into the three-neck flask at the dropwise adding rate of 10mL/min by using a dropping funnel, reacting for 5h at normal temperature after dropwise adding is finished, and discharging to obtain polyaniline emulsion, wherein the cationic emulsifier is preferably sodium dodecyl sulfate or sodium dodecyl sulfate; adding acetone with the volume of 1/4 into the polyaniline emulsion, carrying out chemical stirring and demulsification for 4h to obtain a demulsifying solution, placing the demulsifying solution into a high-speed centrifuge, carrying out centrifugal treatment for 12min at the rotating speed of 4500r/min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake for 5 times by using deionized water, placing a product obtained after the suction filtration and the washing into a vacuum drying oven with the set temperature of 45 ℃, drying for 14h, grinding, and sieving by using a 400-mesh sieve to obtain outer-layer rubber powder; dropwise adding 5% ammonia water into 20% aluminum nitrate solution until the pH value of the solution is 9.5, standing for 10min to obtain a suspension, adding 25 parts of the suspension into 300 parts of absolute ethyl alcohol by weight, stirring, adding 8 parts of a silane coupling agent, 15 parts of outer layer rubber powder and 5 parts of 10% hydrogen peroxide by weight, heating in a water bath to 45 ℃, carrying out centrifugal treatment, removing filtrate, and washing to obtain the alumina/polyaniline core-shell lubricating particles, wherein the silane coupling agent is preferably one of kh550 and kh 570. Adding 60 parts of antioxidant 1010 and 35 parts of diphenylamine into a single-neck flask, adding 350 parts of n-octane serving as a solvent, magnetically stirring for 4 hours at the rotating speed of 350r/min under the protection of nitrogen, heating to 160 ℃, adding 100 parts of di-tert-butyl peroxide into the single-neck flask, and stirring for reacting for 4 hours to obtain a reaction product; installing a condensation reflux device on the single-mouth flask, heating to 150 ℃, distilling for 2 hours, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol at the temperature of-15 ℃ for freezing for 3 hours to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake for 5 times by using acetone, placing the filter cake in an oven, heating to 100 ℃, and drying for 5 hours to obtain a modified antioxidant; mixing vegetable oil, sodium hydroxide and 75% ethanol solution according to a mass ratio of 5: 1: 10, stirring for 20min to obtain saponified solution, placing the saponified solution into a separating funnel, adding 20% hydrochloric acid into the separating funnel to make the pH of the saponified solution be 3.5, standing for 15min, separating to remove a water layer to obtain an oil layer, washing the oil layer with deionized water for 5 times to obtain vegetable oleic acid, wherein the vegetable oil is preferably one of peanut oil, castor oil, rapeseed oil and soybean oil; adding 35 parts by weight of phthalic acid, 50 parts by weight of polyethylene glycol with low polymerization degree and 40 parts by weight of vegetable oleic acid into a stirring reaction kettle with a reflux device, starting a stirrer under the protection of nitrogen, stirring and mixing at a rotating speed of 230r/min, heating the stirring reaction kettle to 65 ℃, keeping the temperature and stirring for reaction until the reflux device does not discharge water, adding 10 parts by weight of alumina/polyaniline core-shell lubricating particles, 8 parts by weight of modified antioxidant and 5 parts by weight of zinc stearate into the stirring reaction kettle, stirring and dispersing for 50min at normal temperature, discharging, canning and sealing to obtain the high-temperature oxidation-resistant anti-corrosion and anti-wear agent.
Comparative example
The anti-wear agent produced by Jiangsu company is used as a comparative example, the high-temperature oxidation resistant anti-corrosion anti-wear agent prepared by the invention and the anti-wear agent in the comparative example are used as samples for performance detection, and the detection results are shown in Table 1:
1. the test method comprises the following steps:
and (3) testing the friction performance:
the friction coefficient test adopts a four-ball machine to test the friction coefficient of the antiwear agent, the maximum non-seizing load PB, the sintering load PD and the size of the grinding spot under the condition of step-by-step loading;
and (3) testing the corrosion resistance:
the bearing is taken as a test target, and detection is carried out according to GB/T501-85:
and (3) after the new bearing coated with the sample is operated for 60s under the condition of light thrust load, fully distributing the antiwear agent on the surface of the bearing, then storing the bearing for 48h under the conditions of 50-55 ℃ and 60% relative humidity, and then cleaning and checking the corrosion signs of the raceway of the outer ring of the bearing.
TABLE 1
Test items Example 1 Example 2 Example 3 Comparative example
PB(kgf) 98 101 108 75
PD(kgf) 145 158 165 126
Coefficient of friction (40 kgf, 80 min) 0.045 0.035 0.030 0.065
Coefficient of friction (60 kgf, 80 min) 0.058 0.055 0.052 0.097
Friction systemNumber (80 kgf, 80 min) 0.065 0.068 0.074 0.095
Grinding spot size (mm/40 kgf, 80 min) 0.353 0.365 0.374 0.594
Grinding spot size (mm/60 kgf, 80 min) 0.401 0.420 0.435 0.659
Grinding spot size (mm/80 kgf, 80 min) 0.645 0.667 0.675 0.869
Oxidation induction period (min) 33.7 34.5 35.6 18.3
Signs of corrosion No pocking mark No pocking mark No pocking mark With pock marks
According to the data, the high-temperature oxidation resistant, corrosion resistant and anti-wear agent prepared by the invention is proved to have obvious improvement on the maximum seizure-free load PB and the maximum sintering load PD through the four-ball machine test data of examples 1-3 and a comparative example, can obviously reduce the friction coefficient and the wear scar size, can embody the excellent performance at higher load, has long oxidation induction period, has no pocking mark phenomenon in a corrosion test, has good corrosion resistance and oxidation resistance, and has wide application prospect.

Claims (9)

1. A preparation method of a high-temperature oxidation resistant anti-corrosion antiwear agent is characterized by comprising the following specific preparation steps:
adding dibasic acid, dihydric alcohol and vegetable oil acid into a stirring reaction kettle with a reflux device, starting a stirrer under the protection of nitrogen, stirring and mixing at the rotating speed of 200-230 r/min, heating the stirring reaction kettle to 50-65 ℃, preserving heat, stirring and reacting until the reflux device does not discharge water, adding alumina/polyaniline core-shell lubricating particles, a modified antioxidant and zinc stearate into the stirring reaction kettle, stirring and dispersing at normal temperature for 40-50 min, discharging, canning and sealing to obtain a high-temperature oxidation resistant anticorrosion antiwear agent;
the preparation method of the aluminum oxide/polyaniline core-shell lubricating particles comprises the following specific steps:
(1) adding 100-120 parts by weight of deionized water and 10-12 parts by weight of cationic emulsifier into a three-neck flask, stirring and pre-emulsifying for 30-40 min, adding 20-25 parts by weight of aniline, simultaneously dropwise adding 10-15 parts by weight of 5% ammonium persulfate solution into the three-neck flask at a dropping rate of 6-10 mL/min by using a dropping funnel, reacting at normal temperature for 4-5 h after dropwise adding, and discharging to obtain polyaniline emulsion;
(2) adding 1/4 volume of acetone into the polyaniline emulsion, carrying out chemical stirring demulsification for 3-4 h to obtain a demulsifying solution, placing the demulsifying solution in a high-speed centrifuge, carrying out centrifugal treatment at a rotating speed of 3000-4500 r/min for 10-12 min, carrying out suction filtration, removing filtrate to obtain a filter cake, washing the filter cake with deionized water for 3-5 times, placing a product obtained after suction filtration and washing in a vacuum drying oven with a set temperature of 40-45 ℃, drying for 12-14 h, grinding, and sieving with a 400-mesh sieve to obtain outer-layer rubber powder;
(3) dropwise adding ammonia water with the mass fraction of 5% into an aluminum nitrate solution with the mass fraction of 20% until the pH of the solution is 9.2-9.5, standing for 5-10 min to obtain a suspension, adding 20-25 parts of the suspension into 200-300 parts of absolute ethyl alcohol in parts by weight, stirring, adding 5-8 parts of a silane coupling agent, 10-15 parts of outer layer rubber powder and 4-5 parts of hydrogen peroxide with the mass fraction of 10%, heating in a water bath to 40-45 ℃, performing centrifugal treatment, removing filtrate, and washing to obtain aluminum oxide/polyaniline core-shell lubricating particles;
the modified antioxidant is prepared by the following specific steps:
(1) adding 40-60 parts by weight of antioxidant and 30-35 parts by weight of diphenylamine into a single-neck flask, adding 300-350 parts by weight of n-octane serving as a solvent, magnetically stirring at a rotating speed of 300-350 r/min for 3-4 hours under the protection of nitrogen, heating to 140-160 ℃, adding 80-100 parts by weight of di-tert-butyl peroxide into the single-neck flask, and stirring for reacting for 3-4 hours to obtain a reaction product;
(2) installing a condensation reflux device on the single-mouth flask, heating to 140-150 ℃, distilling for 1-2 hours, naturally cooling to room temperature, placing the distillation flask in absolute ethyl alcohol, freezing for 2-3 hours to obtain a reaction product containing crystals, performing suction filtration on the obtained reaction product, removing filtrate to obtain a filter cake, washing the filter cake with acetone for 3-5 times, placing in an oven, heating to 90-100 ℃, and drying for 4-5 hours to obtain a modified antioxidant;
the vegetable oil acid is prepared by the following specific steps:
mixing and stirring vegetable oil, sodium hydroxide and 75% by mass of ethanol solution according to a mass ratio of 5: 1: 10 for 15-20 min to obtain saponified solution, placing the saponified solution into a separating funnel, adding 20% by mass of hydrochloric acid into the separating funnel to make the pH of the saponified solution be 3-3.5, standing for 10-15 min, separating to remove a water layer to obtain an oil layer, and washing the oil layer with deionized water for 3-5 times to obtain the vegetable oleic acid.
2. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the high-temperature oxidation resistant, corrosion resistant and antiwear agent is characterized in that raw materials of the high-temperature oxidation resistant, corrosion resistant and antiwear agent in the specific preparation steps comprise, by weight, 30-35 parts of dibasic acid, 40-50 parts of dihydric alcohol, 35-40 parts of vegetable oleic acid and 5-10 parts of alumina/polyphenyl
The lubricant comprises amine core-shell lubricating particles, 6-8 parts of modified antioxidant and 4-5 parts of zinc stearate.
3. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: in the specific preparation steps of the high-temperature oxidation resistant anti-corrosion antiwear agent, the diol is preferably neopentyl glycol with low polymerization degree
Polyethylene glycol.
4. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the dibasic acid in the specific preparation steps of the high-temperature oxidation resistant anti-corrosion antiwear agent is preferably adipic acid, azelaic acid and sunflower
Diacid or phthalic acid.
5. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the cationic emulsifier used in the specific preparation step (1) of the alumina/polyaniline core-shell lubricating particles is preferably sodium dodecyl sulfate or sodium dodecyl sulfate.
6. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the silane coupling agent in the specific preparation step (3) of the alumina/polyaniline core-shell lubricating particles is preferably one of kh550 and kh 570.
7. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the antioxidant used in the specific preparation step (1) of the modified antioxidant is preferably antioxidant 1010.
8. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the modified antioxidant is prepared in the step (2) at the freezing temperature of-20 to-15 ℃.
9. The preparation method of the high-temperature oxidation resistant anti-corrosion antiwear agent according to claim 1, characterized by comprising the following steps: the vegetable oil used in the specific preparation step of the vegetable oil acid is preferably one of peanut oil, castor oil, rapeseed oil and soybean oil.
CN201910980797.9A 2019-10-16 2019-10-16 Preparation method of high-temperature oxidation-resistant anti-corrosion antiwear agent Withdrawn CN110747041A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113337243A (en) * 2021-05-19 2021-09-03 张碧军 Sealing silica gel and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113337243A (en) * 2021-05-19 2021-09-03 张碧军 Sealing silica gel and preparation method thereof

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