CN112481007A - Air valve oil seal repairing agent and preparation method thereof - Google Patents
Air valve oil seal repairing agent and preparation method thereof Download PDFInfo
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- CN112481007A CN112481007A CN202011484942.3A CN202011484942A CN112481007A CN 112481007 A CN112481007 A CN 112481007A CN 202011484942 A CN202011484942 A CN 202011484942A CN 112481007 A CN112481007 A CN 112481007A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/402—Castor oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/086—Imides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/061—Esters derived from boron
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/02—Unspecified siloxanes; Silicones
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/02—Unspecified siloxanes; Silicones
- C10M2229/025—Unspecified siloxanes; Silicones used as base material
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Abstract
The invention discloses a valve oil seal repairing agent which comprises, by weight, 8-12 parts of an oil seal activating agent, 12-20 parts of an antiwear agent, 2-6 parts of an organic friction modifier, 5-10 parts of a dispersing agent and 50-80 parts of synthetic oil. The valve oil seal repairing agent provided by the invention contains a lasting oil seal activating agent and a fluorine-containing antiwear agent, can be used for continuously activating a valve oil seal, can effectively reduce the abrasion of an engine, and has good comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of lubricating oil additives, and particularly relates to a valve oil seal repairing agent and a preparation method thereof.
Background
The oil seal is a common name of a sealing element, namely simply the seal of lubricating oil, and separates a part needing to be lubricated in a transmission part from a force-applying part so as not to allow the lubricating oil to leak. The valve oil seal is one kind of oil seal, and is generally formed by vulcanizing an outer framework and fluororubber together, and a radial opening part of the oil seal is provided with a self-tightening spring or a steel wire for sealing an engine valve guide rod. The valve oil seal can prevent engine oil from entering the air inlet and outlet pipe, avoid engine oil loss, prevent mixed gas of gasoline and air and exhaust waste gas from leaking, and prevent engine oil from entering the combustion chamber. Since a valve oil seal is one of important parts of an engine valve assembly and comes into contact with gasoline and engine oil at high temperatures, it is necessary to use a material having excellent heat resistance and oil resistance, and it is generally made of fluororubber.
When the sealing element of the valve oil seal is used, the sealing element is easy to age and burn oil (the oil enters a combustion chamber of an engine and participates in combustion with mixed gas) due to long-time high-temperature contact and abrasion. The oxygen sensor of the vehicle can be damaged too quickly by burning the engine oil, so that the adverse effects of carbon deposition increase of a combustion chamber, unstable idling, weak acceleration, increased oil consumption, overproof exhaust emission and the like are caused, the lubrication of the engine is insufficient for serious people, the engine is damaged or even scrapped, and the maintenance cost is greatly increased or even hidden accident danger is caused. Therefore, an oil seal repairing agent is generally required to be added into the engine oil, and the oil seal repairing agent generally contains an activating component and an antiwear component.
The activator can soften and expand the aged oil seal, effectively protect the rubber seal and enhance the sealing performance, but the oil seal needs to be continuously activated and repaired for a long time in the using process, and the conventional method is to add the activator into the engine oil at one time, so that the rubber seal can be softened and expanded for a short time, but the continuous effect cannot be achieved.
Antiwear agents reduce friction on the surface of metal parts through lubrication, which can reduce engine wear. The borate additive has good anti-wear extreme pressure effect, particularly has good anti-wear extreme pressure effect in low-viscosity oil, is superior to phosphorus-containing sulfur-chlorine additives in many aspects, and is non-toxic, tasteless and harmless. However, it is used only as a gear oil for vehicles because it has a slightly poor water resistance and is unstable in the presence of water.
To sum up, how to design a valve oil seal repairing agent not only can continuously activate the valve oil seal, but also can effectively reduce the abrasion of an engine, has good comprehensive performance, and is a problem which is urgently needed to be solved at present.
Disclosure of Invention
The present invention is directed to solving the above problems, and an object of the present invention is to provide a valve oil seal repairing agent which can continuously activate a valve oil seal, can effectively reduce engine wear, and has good overall performance.
The invention achieves the aim through the following technical scheme, and the valve oil seal repairing agent comprises 8-12 parts of an oil seal activating agent, 12-20 parts of an antiwear agent, 2-6 parts of an organic friction modifier, 5-10 parts of a dispersing agent and 50-80 parts of synthetic oil in parts by weight.
Further, the preparation method of the oil seal activator comprises the following steps:
(1) placing the microporous ceramic in a 5000-plus-6000-W ultrasonic cleaning machine for cleaning for 20-40min, removing pore impurities, taking out the microporous ceramic, drying, and then placing in a 700-plus-800 r/min ultrafine pulverizer for pulverizing into 0.1-1 mu m microporous ceramic powder;
(2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1-2h, filtering, putting the microporous ceramic powder after water absorption into a vacuum drying box at 40-50 ℃, vacuumizing and drying for 10-20min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing box at the temperature of- (5-20) DEG C, and freezing for 30-60 min;
(3) uniformly mixing the liquid fluorine rubber and the coumarone resin in a high-speed mixer at 80-100 ℃ and 500r/min with 400-;
(4) and (3) quickly putting the microporous ceramic powder obtained in the step (2) into a mixed solution of liquid fluororubber and coumarone resin, soaking for 1-2h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
Further, by weight, 5-10 parts of microporous ceramic in the step (1), 4-8 parts of liquid fluororubber in the step (3), 10-30 parts of coumarone resin and 40-60 parts of silicone oil in the step (4).
Further, the preparation method of the antiwear agent comprises the following steps:
A. ester exchange reaction: mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at 70-80 ℃, heating to 80-90 ℃ after dropwise adding, stirring, refluxing, reacting for 4-6 hours, removing alcohol by distillation at normal pressure after the reaction is finished, and neutralizing with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product;
B. and (3) uniformly mixing the nano-scale polytetrafluoroethylene micro powder and the castor oil in a high-speed mixer at the temperature of 60-80 ℃ and the speed of 400-500r/min, then adding the product obtained in the step A, and uniformly stirring to obtain the finished product.
Furthermore, the mass ratio of the trifluoroethanol to the trioctyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is (1.1-1.3)/1/(0.02-0.08)/(1.5-3).
Further, the mass ratio of the catalyst to the tri-n-octyl borate is (0.02-0.04)/1, and the catalyst is a sodium hydroxide solution or a potassium hydroxide solution.
Further, the dispersant is prepared from succinimide and succinate in a ratio of 1: (0.5-2) in mass ratio.
Further, the organic friction modifier is unsaturated composite ester or methacrylate, and the synthetic oil is poly-alpha-olefin synthetic oil or silicone oil.
A preparation method of a valve oil seal repairing agent comprises the following steps:
s1, placing the synthetic oil in an oven at the temperature of 100-120 ℃ for 30-60min, taking out the synthetic oil, mixing the synthetic oil with the organic friction modifier, and uniformly stirring;
s2, evaporating the solvent of the antiwear agent at 50-60 ℃, and then uniformly mixing the solvent and the product obtained in the step S1 in a high-speed mixer at 60-80 ℃ and 800r/min of 700-80 ℃;
and S3, cooling the product obtained in the step S2 to room temperature, adding an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
The invention has the beneficial effects that:
(1) the valve oil seal repairing agent disclosed by the invention contains a lasting oil seal activating agent and a fluorine-containing antiwear agent, so that the valve oil seal can be continuously activated, the abrasion of an engine can be effectively reduced, and the comprehensive performance is good;
(2) when the oil seal activator is prepared, the liquid fluororubber and the coumarone resin are compounded into the softener, so that the softener has a good softening effect on an oil seal, the expansion capacity of the oil seal can be obviously adjusted, and then the softener is introduced into the microporous ceramic, so that the softener can be slowly and continuously released from pores, and a lasting activation effect is achieved;
(3) when the antiwear agent is prepared, fluorine atoms are grafted into tri-n-octyl borate through ester exchange reaction, and the synthesized compound integrates the advantages of fluorine and boric acid ester, so that the product not only has excellent antiwear extreme pressure effect of the boric acid ester, but also has the hydrophobicity, corrosion resistance, high temperature resistance and weather resistance of the fluorine compound;
(4) when the antiwear agent is prepared, the nano polytetrafluoroethylene micro powder and the castor oil are added, so that a good lubricating effect is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a valve oil seal repairing agent which comprises 8 parts of an oil seal activating agent, 12 parts of an antiwear agent, 2 parts of an organic friction modifier, 5 parts of a dispersing agent and 50 parts of synthetic oil in parts by weight.
The preparation method of the oil seal activator comprises the following steps:
(1) cleaning the microporous ceramic in a 5000W ultrasonic cleaning machine for 20min, removing pore impurities, taking out the microporous ceramic, drying, and pulverizing into 0.1 μm microporous ceramic powder in a 700r/min ultrafine pulverizer;
(2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1h, filtering, putting the microporous ceramic powder after water absorption into a vacuum drying oven at 40 ℃, vacuumizing and drying for 10min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing oven at-5 ℃, and freezing for 30 min;
(3) uniformly mixing the liquid fluorine rubber and the coumarone resin in a high-speed mixer at 80 ℃ and 400r/min, and then preserving heat at 60 ℃ for later use;
(4) and (3) quickly putting the microporous ceramic powder obtained in the step (2) into a mixed solution of liquid fluororubber and coumarone resin, soaking for 1h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
According to parts by weight, the microporous ceramic in the step (1) is 5 parts, the liquid fluororubber in the step (3) is 4 parts, the coumarone resin is 10 parts, and the silicone oil in the step (4) is 40 parts.
The preparation method of the antiwear agent comprises the following steps:
A. ester exchange reaction: mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at 70 ℃, heating to 80 ℃ after dropwise adding, stirring, refluxing and reacting for 4 hours, distilling to remove alcohol under normal pressure after the reaction is finished, and neutralizing with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product;
B. and (3) uniformly mixing the nano polytetrafluoroethylene micro powder and the castor oil in a high-speed mixer at 60 ℃ and 400r/min, then adding the product obtained in the step A, and uniformly stirring to obtain a finished product.
The mass ratio of the trifluoroethanol to the trioctyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.1/1/0.02/1.5.
The mass ratio of the catalyst to the tri-n-octyl borate is 0.02/1, and the catalyst is sodium hydroxide solution.
The dispersant is prepared from succinimide and succinate in a weight ratio of 1: 0.5 mass ratio.
The organic friction modifier is unsaturated composite ester, and the synthetic oil is poly-alpha-olefin synthetic oil.
The embodiment also provides a preparation method of the valve oil seal repairing agent, which comprises the following steps:
s1, placing the synthetic oil in a baking oven at 100 ℃ for 30min, taking out the synthetic oil, mixing the synthetic oil with the organic friction modifier, and uniformly stirring;
s2, evaporating the solvent of the antiwear agent at 50 ℃, and then uniformly mixing the solvent and the product obtained in the step S1 in a high-speed mixer at 60 ℃ and 700 r/min;
and S3, cooling the product obtained in the step S2 to room temperature, adding an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
Example 2
The embodiment provides a valve oil seal repairing agent which comprises, by weight, 10 parts of an oil seal activating agent, 16 parts of an antiwear agent, 4 parts of an organic friction modifier, 8 parts of a dispersant and 65 parts of synthetic oil.
The preparation method of the oil seal activator comprises the following steps:
(1) cleaning microporous ceramic in 5500W ultrasonic cleaning machine for 30min, removing pore impurities, taking out microporous ceramic, drying, and pulverizing into 0.5 μm microporous ceramic powder in 750r/min ultrafine pulverizer;
(2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1.5h, filtering, putting the microporous ceramic powder after water absorption into a vacuum drying box at 45 ℃, vacuumizing and drying for 15min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing box at-12 ℃, and freezing for 45 min;
(3) uniformly mixing the liquid fluorine rubber and the coumarone resin in a high-speed mixer at 90 ℃ and 450r/min, and then preserving heat at 70 ℃ for later use;
(4) and (3) quickly putting the microporous ceramic powder obtained in the step (2) into a mixed solution of liquid fluororubber and coumarone resin, soaking for 1.5h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
According to parts by weight, the microporous ceramic in the step (1) is 8 parts, the liquid fluororubber in the step (3) is 6 parts, the coumarone resin is 20 parts, and the silicone oil in the step (4) is 50 parts.
The preparation method of the antiwear agent comprises the following steps:
A. ester exchange reaction: mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at 75 ℃, heating to 85 ℃ after dropwise adding, stirring, refluxing and reacting for 5 hours, distilling to remove alcohol under normal pressure after the reaction is finished, and neutralizing with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product;
B. and (3) uniformly mixing the nano polytetrafluoroethylene micro powder and the castor oil in a high-speed mixer at 70 ℃ and 450r/min, then adding the product obtained in the step A, and uniformly stirring to obtain a finished product.
The mass ratio of the trifluoroethanol to the trioctyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.2/1/0.05/2.2.
The mass ratio of the catalyst to the tri-n-octyl borate is 0.03/1, and the catalyst is potassium hydroxide solution.
The dispersant is prepared from succinimide and succinate in a weight ratio of 1: 1, and the components are compounded according to the mass ratio of 1.
The organic friction modifier is methacrylate, and the synthetic oil is silicone oil.
The embodiment also provides a preparation method of the valve oil seal repairing agent, which comprises the following steps:
s1, placing the synthetic oil in a drying oven at 110 ℃ for 45min, taking out the synthetic oil, mixing the synthetic oil with the organic friction modifier, and uniformly stirring;
s2, evaporating the solvent of the antiwear agent at 55 ℃, and then uniformly mixing the solvent and the product obtained in the step S1 in a high-speed mixer at 70 ℃ and 750 r/min;
and S3, cooling the product obtained in the step S2 to room temperature, adding an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
Example 3
The embodiment provides a valve oil seal repairing agent which comprises, by weight, 12 parts of an oil seal activating agent, 20 parts of an antiwear agent, 6 parts of an organic friction modifier, 10 parts of a dispersant and 80 parts of synthetic oil.
The preparation method of the oil seal activator comprises the following steps:
(1) cleaning the microporous ceramic in a 6000W ultrasonic cleaning machine for 40min, removing pore impurities, taking out the microporous ceramic, drying, and pulverizing into 1 μm microporous ceramic powder in an 800r/min ultrafine pulverizer;
(2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 2h, filtering, putting the microporous ceramic powder after water absorption into a vacuum drying oven at 50 ℃, vacuumizing and drying for 20min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing oven at-20 ℃, and freezing for 60 min;
(3) uniformly mixing the liquid fluororubber and the coumarone resin in a high-speed mixer at 100 ℃ and 500r/min, and then preserving heat at 80 ℃ for later use;
(4) and (3) quickly putting the microporous ceramic powder obtained in the step (2) into a mixed solution of liquid fluororubber and coumarone resin, soaking for 2 hours, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
According to parts by weight, 10 parts of microporous ceramic in the step (1), 8 parts of liquid fluororubber in the step (3), 30 parts of coumarone resin and 60 parts of silicone oil in the step (4).
The preparation method of the antiwear agent comprises the following steps:
A. ester exchange reaction: mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at the temperature of 80 ℃, heating to 90 ℃ after dropwise adding, stirring, refluxing, reacting for 6 hours, distilling to remove alcohol at normal pressure after the reaction is finished, and neutralizing with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product;
B. and (3) uniformly mixing the nano polytetrafluoroethylene micro powder and the castor oil in a high-speed mixer at 80 ℃ and 500r/min, then adding the product obtained in the step A, and uniformly stirring to obtain a finished product.
The mass ratio of the trifluoroethanol to the trioctyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.3/1/0.08/3.
The mass ratio of the catalyst to the trioctyl borate is 0.04/1, and the catalyst is potassium hydroxide solution.
The dispersant is prepared from succinimide and succinate in a weight ratio of 1: 2, and the components are compounded according to the mass ratio.
The organic friction modifier is methacrylate, and the synthetic oil is silicone oil.
The embodiment also provides a preparation method of the valve oil seal repairing agent, which comprises the following steps:
s1, placing the synthetic oil in a baking oven at 120 ℃ for 60min, taking out the synthetic oil, mixing the synthetic oil with the organic friction modifier, and uniformly stirring;
s2, evaporating the solvent of the antiwear agent at 60 ℃, and then uniformly mixing the solvent and the product obtained in the step S1 in a high-speed mixer at 80 ℃ and 800 r/min;
and S3, cooling the product obtained in the step S2 to room temperature, adding an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
Comparative example 1
The comparative example provides a valve oil seal repairing agent, which is different from that of example 1 in that the valve oil seal repairing agent is a commercially available oil seal repairing agent.
Comparative example 2
The comparative example provides a valve oil seal repairing agent, which is different from that of example 1 in that the weight of an oil seal activating agent in the valve oil seal repairing agent is 6 parts.
Comparative example 3
The comparative example provides a valve oil seal repairing agent, which is different from that of example 1 in that the weight of an oil seal activating agent in the valve oil seal repairing agent is 14 parts.
Comparative example 4
The comparative example provides a valve oil seal repairing agent, which is different from that of example 1 in that the weight of an abrasive resistant agent in the valve oil seal repairing agent is 10 parts.
Comparative example 5
The present comparative example provides a valve oil seal repairing agent, which is different from example 1 in that the weight of the abrasive resistance agent in the valve oil seal repairing agent is 22 parts.
Comparative example 6
The present comparative example provides a method for preparing a valve oil seal repairing agent, which is different from example 1 in that step S2 is: and (4) uniformly mixing the antiwear agent and the product obtained in the step S1 in a high-speed mixer at 60 ℃ and 700 r/min.
Comparative example 7
The present comparative example provides a method for preparing a valve oil seal repairing agent, which is different from example 1 in that step S3 is: and (5) mixing the product obtained in the step (S2) with an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
Comparative example 8
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 2 in that the oil seal activating agent does not contain microporous ceramics, and the preparation method of the oil seal activating agent comprises the following steps: (1) uniformly mixing the liquid fluorine rubber and the coumarone resin in a high-speed mixer at 90 ℃ and 450r/min, and then preserving heat at 70 ℃ for later use; (2) and (2) mixing the mixed liquid of the liquid fluororubber and the coumarone resin obtained in the step (1) with silicone oil, and uniformly stirring to obtain a finished product.
Comparative example 9
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 2 in that the oil seal activating agent does not contain liquid fluororubber, and the step (3) of the preparation method of the oil seal activating agent is as follows: heating coumarone resin to 90 deg.C to melt, and keeping at 70 deg.C for use. The step (4) is as follows: and (3) quickly putting the microporous ceramic powder obtained in the step (2) into coumarone resin, soaking for 1.5h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
Comparative example 10
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 2 in that the oil seal activating agent does not contain coumarone resin, and the step (3) of the preparation method of the oil seal activating agent is as follows: the liquid fluororubber is heated to 90 ℃ and then kept warm at 70 ℃ for later use. The step (4) is as follows: and (3) quickly putting the microporous ceramic powder obtained in the step (2) into liquid fluororubber, soaking for 1.5h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
Comparative example 11
The comparative example provides a valve oil seal repairing agent, which is different from that of example 2 in that the weight of microporous ceramics in an oil seal activator is 3 parts.
Comparative example 12
The comparative example provides a valve oil seal repairing agent, which is different from that of example 2 in that the weight of microporous ceramics in an oil seal activator is 12 parts.
Comparative example 13
This comparative example provides a valve oil seal repairing agent, which is different from example 2 in that the weight of liquid fluororubber in the oil seal activator is 2 parts.
Comparative example 14
This comparative example provides a valve oil seal repairing agent, which is different from example 2 in that the weight of liquid fluororubber in the oil seal activator is 10 parts.
Comparative example 15
The comparative example provides a valve oil seal repairing agent, which is different from the embodiment 2 in that the preparation method of the oil seal activating agent comprises the following steps (1): putting the microporous ceramic into a superfine pulverizer of 750r/min to pulverize into microporous ceramic powder of 0.5 μm.
Comparative example 16
The comparative example provides a valve oil seal repairing agent, which is different from the embodiment 2 in that the step (2) of the preparation method of the oil seal activating agent is as follows: and (2) putting the microporous ceramic powder obtained in the step (1) into a vacuum drying oven at the temperature of 45 ℃, vacuumizing and drying for 15min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing oven at the temperature of-12 ℃, and freezing for 45 min.
Comparative example 17
The comparative example provides a valve oil seal repairing agent, which is different from the embodiment 2 in that the step (2) of the preparation method of the oil seal activating agent is as follows: soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1.5h, filtering, putting the microporous ceramic powder after water absorption into a drying box at 45 ℃, drying for 15min, taking out the microporous ceramic powder, quickly putting into a freezing box at-12 ℃, and freezing for 45 min.
Comparative example 18
The comparative example provides a valve oil seal repairing agent, which is different from the embodiment 2 in that the step (2) of the preparation method of the oil seal activating agent is as follows: and (2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1.5h, then filtering, putting the microporous ceramic powder after water absorption into a vacuum drying box at 45 ℃, vacuumizing and drying for 15 min.
Comparative example 19
The comparative example provides a valve oil seal repairing agent, which is different from the embodiment 2 in that the preparation method of the oil seal activating agent comprises the following steps (3): uniformly mixing the liquid fluororubber, the coumarone resin and the silicone oil in a high-speed mixer at 90 ℃ and 450r/min, and then preserving heat at 70 ℃ for later use. The step (4) is as follows: and (3) quickly putting the microporous ceramic powder obtained in the step (2) into the mixed liquid obtained in the step (3), and soaking for 1.5h to obtain a finished product.
Comparative example 20
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 3 in that a commercially available borate additive is adopted as an antiwear agent.
Comparative example 21
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in the example 3 in that the antiwear agent does not contain nano polytetrafluoroethylene micro powder, and the step B of the preparation method of the antiwear agent is as follows: and D, uniformly mixing the castor oil and the product obtained in the step A in a high-speed mixer at 80 ℃ and 500r/min to obtain a finished product.
Comparative example 22
The difference between the valve oil seal repairing agent and the repairing agent in the embodiment 3 is that in the step A of the preparation method of the antiwear agent, the temperature for dripping the tri-n-octyl borate is 65 ℃.
Comparative example 23
The difference between the valve oil seal repairing agent and the repairing agent in the embodiment 3 is that in the step A of the preparation method of the antiwear agent, the temperature for dripping the tri-n-octyl borate is 85 ℃.
Comparative example 24
The comparative example provides a valve oil seal repairing agent, and the difference from the example 3 is that the preparation method of the antiwear agent comprises the following steps: after mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at the temperature of 80 ℃, stirring and refluxing the mixture for reaction for 6 hours after the dropwise adding is finished, distilling the mixture under normal pressure to remove alcohol after the reaction is finished, and then neutralizing the mixture with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product.
Comparative example 25
The comparative example provides a valve oil seal repairing agent, and is different from the repairing agent in example 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol, the tri-n-octyl borate, the nano polytetrafluoroethylene micro powder and the castor oil is 1/1/0.08/3.
Comparative example 26
The comparative example provides a valve oil seal repairing agent, and is different from the embodiment 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol to the tri-n-octyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.4/1/0.08/3.
Comparative example 27
The comparative example provides a valve oil seal repairing agent, and is different from the embodiment 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol to the tri-n-octyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.3/1/0.01/3.
Comparative example 28
The comparative example provides a valve oil seal repairing agent, and is different from the embodiment 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol to the tri-n-octyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.3/1/0.09/3.
Comparative example 29
The comparative example provides a valve oil seal repairing agent, and is different from the embodiment 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol to the tri-n-octyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.3/1/0.08/1.3.
Comparative example 30
The comparative example provides a valve oil seal repairing agent, and is different from the embodiment 3 in that in the preparation method of the antiwear agent, the mass ratio of the trifluoroethanol to the tri-n-octyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is 1.3/1/0.08/3.2.
Comparative example 31
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 3 in that in the preparation method of the antiwear agent, the mass ratio of the catalyst to the tri-n-octyl borate is 0.01/1.
Comparative example 32
The comparative example provides a valve oil seal repairing agent, which is different from the repairing agent in example 3 in that in the preparation method of the antiwear agent, the mass ratio of the catalyst to the tri-n-octyl borate is 0.05/1.
Comparative example 33
The comparative example provides a valve oil seal repairing agent, and the difference from example 3 is that in the preparation method of the antiwear agent, a catalyst is hydrochloric acid solution.
Firstly, the influence of a valve oil seal repairing agent on the mechanical property of a valve oil seal
Respectively putting the fluororubber valve oil seal into 150 ℃ SL 5W-40W engine oil, 150 ℃ SL 5W-40W engine oil and a valve oil seal repairing agent, soaking for 72 hours, totaling 23 groups of tests, and then detecting various mechanical properties of the fluororubber valve oil seal. The valve oil seal repairing agent is prepared according to examples 1-3 and comparative examples 1-19, the addition amount is 2% (mass percent), and the mechanical property parameters of each test group are shown in Table 1:
from the results in table 1, it is understood that the valve oil seal repairing agents prepared in examples 1 to 3 of the present invention can reduce the hardness and weight loss of the oil seal, increase the tensile strength and volume expansion, and show good mechanical properties without being affected by the breaking force, as compared with the engine oil and comparative examples 1 to 19.
Second, the continuous activation effect test of the oil seal activator
Respectively soaking the fluororubber valve oil seal in 150 ℃ SL 5W-40W engine oil, 150 ℃ SL 5W-40W engine oil and an oil seal activating agent, and recording the volume change condition every 24 hours for 15 groups of tests in total. Wherein the oil seal activator was a product prepared in accordance with examples 1 to 3 and comparative examples 8 to 19, and the amount thereof added was 2% (mass percent), the results of which are shown in Table 2:
as can be seen from the results in Table 2, the oil seal activators prepared in examples 1 to 3 according to the present invention have a continuous activation effect after 120 hours of soaking, and the volume expansion of the oil seal rubber is as high as 19%, compared with the engine oil and comparative examples 8 to 19. While other comparative examples not only had less volume expansion but also had poor sustained activation capability.
Third, the result of the detection of the anti-wear performance of the anti-wear agent
The antiwear agents of examples 1 to 3 and comparative examples 20 to 33 were subjected to an anti-wear performance test using GB/T3142, the results of which are shown in Table 3:
as is clear from the results in Table 3, the antiwear agents prepared in examples 1 to 3 of the present invention have excellent antiwear extreme pressure effects as compared with those of comparative examples 20 to 33.
Fourthly, the water resistance detection result of the antiwear agent
The anti-wear agents of examples 1-3 and comparative examples 20-33 were tested for water resistance and the results are shown in Table 4:
as is clear from the results in Table 4, the antiwear agents prepared in examples 1 to 3 of the present invention have excellent water resistance as compared with comparative examples 20 to 33. Compared with the comparative example 20, the invention can be known that fluorine atoms are grafted into the tri-n-octyl borate through ester exchange reaction, and the synthesized compound integrates the advantages of fluorine and boric acid ester, so that the product has the water resistance of the fluorine compound.
The invention has the beneficial effects that: the valve oil seal repairing agent provided by the invention contains a lasting oil seal activating agent and a fluorine-containing antiwear agent, can be used for continuously activating a valve oil seal, can effectively reduce the abrasion of an engine, and has good comprehensive performance. The repairing agent can be used for repairing valve oil seals, and also can be used for repairing oil seal parts made of rubber such as crankcase oil seals, camshaft oil seals and the like, and has good activation effect.
Finally, it should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or some technical features thereof can be replaced. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The valve oil seal repairing agent is characterized in that: the lubricating grease comprises, by weight, 8-12 parts of an oil seal activator, 12-20 parts of an antiwear agent, 2-6 parts of an organic friction modifier, 5-10 parts of a dispersant and 50-80 parts of synthetic oil.
2. The valve oil seal repairing agent according to claim 1, wherein: the preparation method of the oil seal activator comprises the following steps:
(1) placing the microporous ceramic in a 5000-plus-6000-W ultrasonic cleaning machine for cleaning for 20-40min, removing pore impurities, taking out the microporous ceramic, drying, and then placing in a 700-plus-800 r/min ultrafine pulverizer for pulverizing into 0.1-1 mu m microporous ceramic powder;
(2) soaking the microporous ceramic powder obtained in the step (1) in water at room temperature for 1-2h, filtering, putting the microporous ceramic powder after water absorption into a vacuum drying box at 40-50 ℃, vacuumizing and drying for 10-20min, taking out the microporous ceramic powder, quickly putting into a vacuum freezing box at the temperature of- (5-20) DEG C, and freezing for 30-60 min;
(3) uniformly mixing the liquid fluorine rubber and the coumarone resin in a high-speed mixer at 80-100 ℃ and 500r/min with 400-;
(4) and (3) quickly putting the microporous ceramic powder obtained in the step (2) into a mixed solution of liquid fluororubber and coumarone resin, soaking for 1-2h, filtering to remove redundant liquid, mixing filter residues with silicone oil, and uniformly stirring to obtain a finished product.
3. The valve oil seal repairing agent according to claim 2, wherein: according to parts by weight, 5-10 parts of microporous ceramic in the step (1), 4-8 parts of liquid fluororubber in the step (3), 10-30 parts of coumarone resin and 40-60 parts of silicone oil in the step (4).
4. The valve oil seal repairing agent according to claim 1, wherein: the preparation method of the antiwear agent comprises the following steps:
A. ester exchange reaction: mixing trifluoromethanol and an alkali catalyst, dropwise adding the mixture into tri-n-octyl borate at 70-80 ℃, heating to 80-90 ℃ after dropwise adding, stirring, refluxing, reacting for 4-6 hours, removing alcohol by distillation at normal pressure after the reaction is finished, and neutralizing with a hydrochloric acid solution to obtain a tri-n-octyl trifluoroethylborate product;
B. and (3) uniformly mixing the nano-scale polytetrafluoroethylene micro powder and the castor oil in a high-speed mixer at the temperature of 60-80 ℃ and the speed of 400-500r/min, then adding the product obtained in the step A, and uniformly stirring to obtain the finished product.
5. The valve oil seal repairing agent according to claim 4, wherein: the mass ratio of the trifluoroethanol to the trioctyl borate to the nano polytetrafluoroethylene micro powder to the castor oil is (1.1-1.3)/1/(0.02-0.08)/(1.5-3).
6. The valve oil seal repairing agent according to claim 4, wherein: the mass ratio of the catalyst to the tri-n-octyl borate is (0.02-0.04)/1, and the catalyst is sodium hydroxide solution or potassium hydroxide solution.
7. The valve oil seal repairing agent according to claim 1, wherein: the dispersant is prepared from succinimide and succinate in a ratio of 1: (0.5-2) in mass ratio.
8. The valve oil seal repairing agent according to claim 1, wherein: the organic friction modifier is unsaturated composite ester or methacrylate, and the synthetic oil is poly-alpha-olefin synthetic oil or silicone oil.
9. The preparation method of the valve oil seal repairing agent according to claim 1, characterized by comprising the following steps: the method comprises the following steps:
s1, placing the synthetic oil in an oven at the temperature of 100-120 ℃ for 30-60min, taking out the synthetic oil, mixing the synthetic oil with the organic friction modifier, and uniformly stirring;
s2, evaporating the solvent of the antiwear agent at 50-60 ℃, and then uniformly mixing the solvent and the product obtained in the step S1 in a high-speed mixer at 60-80 ℃ and 800r/min of 700-80 ℃;
and S3, cooling the product obtained in the step S2 to room temperature, adding an oil seal activating agent and a dispersing agent, and uniformly stirring to obtain a finished product.
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