CN112779077B - Preparation method of lubricating grease for aviation high-temperature motor bearing - Google Patents
Preparation method of lubricating grease for aviation high-temperature motor bearing Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/06—Well-defined aromatic compounds
- C10M2203/065—Well-defined aromatic compounds used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2207/02—Hydroxy compounds
- C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
- C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
- C10M2219/106—Thiadiazoles
Abstract
The invention discloses a preparation method of lubricating grease for aviation high-temperature motor bearings. The lubricating grease prepared by the method has excellent wear resistance and long service life, can be used for lubricating grease of aviation high-temperature motor bearings and motor lubrication in other industries, has better high-temperature bearing life, extreme pressure wear resistance and other properties meeting the requirements of relevant standards compared with the existing lubricating grease for the motor, and can be widely used in the field of motor lubrication.
Description
Technical Field
The invention relates to a preparation method of a lubricating grease product, in particular to a preparation method of a lubricating grease which has excellent wear resistance and long service life and can be used for aviation high-temperature motor bearings, and the lubricating grease product can also be used for motor lubrication in other industries.
Background
Aviation grease plays an important role in ensuring the operational reliability and maintainability of an aircraft. The aviation grease is mainly used for lubricating and protecting bearings, gears, chains and control mechanism nodes of parts such as aviation motors, instruments, engine accessory wheels and the like.
With the development of the aviation industry, the flying speed of an aviation aircraft is higher and higher, the consumption of electronic equipment is higher and higher, the power consumption demand of aviation onboard equipment is higher and higher, the requirements on an aviation motor are higher and higher, and particularly, the requirements on a medium-power motor and a high-power motor are increasingly strict, and motor lubricating grease with excellent wear resistance and long service life is required to meet the use requirements of the high-power motor. The Chan boaka lubricating grease for Russia is motor lubricating grease with excellent wear resistance designed for medium and high-power motors, is suitable for aviation motors with the temperature of-60-180 ℃, and has longer service life compared with lubricating grease for other Russia motors.
A Russian U-MUM 201 and U-AT 201 use refined mineral oil base oil, and to obtain better low-temperature performance, the greases of O-122-7, T-O-K-122-8, and T-O-K-12 are changed into silicone oil as main mineral oil, U-MA-221, U-MA-22C, and BY-NIN-220 use silicone oil base oil, U-NIN-207 uses ethyl silicone oil and MAC-35 lubricating oil mixed oil to improve wear resistance, and ester oil base oil is used.
These greases mainly use refined mineral oil, ester oil, silicone oil or mixed oil of these oils as base oil. The low-viscosity refined mineral oil has a low application range and a low application temperature; ester oil has strict requirements on material compatibility and has the problem of hydrolytic stability; the silicone oil system is expensive, and has poor self anti-wear performance and extreme pressure performance, and the sensitivity of the silicone oil system to additives is poor, so that the prepared lubricating grease product has low anti-wear performance. At present, motor lubricating grease which is excellent in abrasion resistance, extreme pressure property, hydrolysis resistance, high-temperature performance, long in service life and low in price is not integrated. At present, the lubricating and anti-wear performance of high-power aviation motors in China is insufficient, and part of the high-power aviation motors need to use imported calcium sulfate grease. However, with the development of the motor industry, higher requirements are provided for the maintenance guarantee of motor equipment, and the maintenance period of the aviation motor is required to be longer, so that higher requirements are provided for the high-low temperature performance and the wear resistance of motor bearing lubricating grease, and particularly, in order to enable the aviation industry of China not to be restricted by people, the self lubricating grease product must be developed and produced.
In a previous application (patent number ZL 201310706860.2) filed by the inventor, a multipurpose universal aviation grease is disclosed, which can meet the requirement of MIL-PRF-81322 specification, and is composed of a base oil, a thickening agent, an antioxidant and an extreme pressure antiwear agent, wherein the base oil is a compound oil of PAO4 and PAO6 base oils, the weight ratio of the two oil stocks is 18. The aviation grease can normally work at 177 ℃ for 560 hours. However, the lubricating grease is mainly used for mounting splines and servo mechanism parts of a motor, is not ideal for a bearing of a high-power motor, and is not successfully used. On a 60kVA motor bearing, a certain product meeting the MIL-PRF-81322 specification is tried to replace Russian imported lubricating grease, the problem of lubricating channel blockage occurs, and the use requirement cannot be met. The Russian imported motor lubricating grease has certain defects in abrasion resistance and bearing service life, and when the motor is in actual use and the maintenance period is not up, problems such as bearing abrasion and the like occur, so that the maintenance period has to be shortened, and the actual use requirements cannot be met.
Therefore, motor grease with excellent wear resistance and longer service life under high-temperature working conditions needs to be developed to meet the use requirements of medium and high power motors.
Disclosure of Invention
In view of the above current domestic and foreign conditions, according to one aspect of the present invention, the present invention provides a method for preparing a grease for an aviation high-temperature motor bearing, the method comprising the steps of:
1) Adding PAO6 base oil and alkyl naphthalene base oil with preset weight into a reaction kettle, adding a modifier under stirring, heating to 100-110 ℃, adding azelaic acid, adding 12-hydroxystearic acid after the azelaic acid is dissolved, cooling while dissolving 12-hydroxystearic acid, slowly adding a lithium hydroxide suspension when the temperature is reduced to 98 ℃, wherein the molar total amount of lithium hydroxide is equal to the molar amount of 12-hydroxystearic acid and twice the molar amount of azelaic acid, heating to 105 ℃, saponifying for 2 hours, heating to 120-130 ℃, and dehydrating for 1 hour.
2) Then adding a saturated boric acid aqueous solution and a salicylic acid solution at the temperature of 90 ℃, heating to 140-150 ℃, slowly adding a lithium hydroxide suspension, wherein the molar total amount of lithium hydroxide is equal to the equimolar amount of boric acid and twice the molar amount of salicylic acid, saponifying for 2 hours, dehydrating for 1 hour, heating to 180-190 ℃, keeping for 10 minutes, adding pentaerythritol n-heptyl ester base oil and modifier n-heptanol, naturally cooling, adding an antioxidant, an antiwear agent, an extreme pressure agent and an antirust agent at the temperature of 100-110 ℃, keeping stirring at a constant temperature for 30 minutes, cooling to room temperature, and homogenizing to obtain a final product.
Wherein, the LiOH. H in the step 1) 2 LiOH & H in O suspension 2 The weight ratio of O to water is 1;
the addition amount of the azelaic acid is 4-6 parts by weight and the addition amount of the 12-hydroxystearic acid is 11-15 parts by weight based on 100 parts by weight of the compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil;
the modifier in the step 1) is selected from n-hexanol, n-heptanol or n-octanol, preferably n-heptanol, and is added in an amount of 7% based on 100 parts by weight of compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil;
in the step 2), based on 100 parts by weight of the compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil, the addition amount of the boric acid is 1-3 parts by weight, and the addition amount of the salicylic acid is 1.5-3.5 parts by weight.
In the step 2), the salicylic acid solution is obtained by dissolving salicylic acid in isobutanol to form a salicylic acid isobutanol solution, and the isobutanol is added in an amount of dissolving the salicylic acid.
Wherein the contents of the various components are as follows, based on the weight of the final grease product:
a base oil content of 75% to 90%;
the thickening agent content is 8-29%;
the content of the antioxidant is 1 to 8 percent;
the content of the antiwear agent is 1 to 5 percent;
the content of the extreme pressure agent is 0.5 to 5 percent;
the content of the antirust agent is 0.5 to 1.5 percent;
the sum of the total amount of all the components is 100 percent.
Preferably, the contents of the various ingredients are as follows, based on the weight of the final grease product:
the base oil content is 70% to 85%;
the thickening agent content is 10-25%;
the content of the antioxidant is 3 to 8 percent;
the content of the antiwear agent is 1 to 3 percent;
the content of the extreme pressure agent is 1 to 3 percent;
the content of the antirust agent is 0.5 to 1.0 percent;
the sum of the total amount of all the components is 100 percent.
Preferably, the contents of the various ingredients are as follows, based on the weight of the final grease product:
the base oil content was 74.5%;
the thickener content is 17.9%;
the content of the antioxidant is 3 percent;
the content of the antiwear agent is 2.5 percent;
the content of the extreme pressure agent is 1.5 percent;
the content of the antirust agent is 0.6 percent
The sum of the total amount of all the components is 100 percent.
Wherein the base oil is a PAO6 base oil, a compound oil of alkyl naphthalene base oil and ester oil, and the weight ratio of the three is 60-90.
Preferably, the base oil is a PAO6 base oil, a compound oil of alkyl naphthalene base oil and ester oil, and the weight ratio of the three is 75-90.
Preferably, the base oil is a PAO6 base oil, a compound oil of alkyl naphthalene base oil and ester oil, and the weight ratio of the three is 86.
The ester oil is pentaerythritol ester base oil selected from pentaerythritol n-hexyl ester base oil, pentaerythritol n-heptyl ester base oil and pentaerythritol n-octyl ester base oil.
More preferably, the ester oil is pentaerythritol n-heptyl ester base oil.
The modifier is selected from n-hexanol, n-heptanol or n-octanol, preferably n-heptanol, and is added in an amount of 7% based on 100 parts by weight of a compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil.
The thickener is not particularly limited, and thickeners commonly used in aviation greases, including but not limited to complex soap-based thickeners, bentonite thickeners, organic fuel thickeners, and the like, may be used. For example, a composite lithium thickener used in chinese patent ZL2013107068602 may be used.
The antioxidant is selected from phenol type antioxidant and amine type antioxidant as main materials, alkyl thiocarbamate or alkyl thiocarbamate and alkyl thiocarbamate or alkyl, and the like as auxiliary materials, and is preferably one or a combination of two or three of p-diisooctyl diphenylamine, compound amine antioxidant 9317, 4' -methylene-bis (2, 6-di-tert-butylphenol), antioxidant 1076, antioxidant 1010 and antioxidant 7723 according to any weight ratio.
The antiwear agent is selected from one or a combination of more of tricresyl phosphate and derivatives thereof, zinc dialkyl dithiocarbamate, zinc dialkyl dithiophosphate, antimony dialkyl dithiocarbamate and thiadiazole according to any weight ratio.
The extreme pressure agent is selected from molybdenum disulfide, graphite and CaCO 3 One or two of mercaptobenzothiadiazole, thiadiazole derivative and phosphate ester are combined according to any weight proportion.
The antirust agent is one or a combination of two of benzotriazole and derivatives thereof, thiadiazole and derivatives thereof and overbased barium sulfonate according to any weight proportion.
Advantageous effects
Compared with the current domestic motor lubricating grease and foreign motor lubricating grease, the lubricating grease for the aviation high-temperature motor bearing provided by the invention has better high-temperature bearing service life, wear resistance, oxidation resistance, shearing resistance, extreme pressure wear resistance and other properties meeting the requirements of related standards, and therefore, can be widely applied to the field of motor lubrication.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The prior product mostly uses silicone oil or silicone oil ester oil mixed oil as base oil, has poor wear resistance and has limited service life for medium and high power motors. The motor lubricating grease prepared by using the base oil with PAO (polyamide oil) or the base oil (mixed oil of PAO and ester oil or mixed oil of PAO and alkyl naphthalene) mainly containing PAO has excellent wear resistance, extreme pressure performance and oxidation resistance, and has the characteristic of long service life.
The aviation grease in China is basically a standard product. The existing motor bearing lubricating greases such as 933, 7014, 7016, 7017 and the like in China mainly adopt silicone oil as base oil, and part of the lubricating greases are added with part of ester oil for improving the lubricating performance. Due to the inherent defects of the base oil, the existing aviation motor bearing lubricating grease has certain defects in wear resistance. The existing aviation motor bearing lubricating grease basically has no requirement on the wear resistance, and the actually measured comprehensive wear index data (LWI) is not more than 30N.
At present, lubricating grease needs to be added to a bearing when some high-power motors, such as a certain type 60kVA alternating-current generator, work for 600 hours and a certain type 40kVA alternating-current generator work for 300 hours, and imported lubricating grease for releasing ethylene glycol sulfate (EDA) is used. In addition, with the development of the motor industry, higher requirements are provided for the maintenance guarantee of motor equipment, and the maintenance period of the aviation motor is longer, so that higher requirements are provided for the high-low temperature performance and the abrasion resistance of the motor bearing lubricating grease.
A new motor bearing lubricating grease developed at the end of Russian twentieth century, which has high and low temperature performance and good wear resistance, instead of Russian VIN-220, VIN-242, LIDIC-1, JUSA M-221, EPIAL-176, and other lubricating greases, is a high-performance motor bearing lubricating grease used in Russia. Lithium ferrous sulfate lubricating grease has excellent long service life and friction and wear resistance, which is not possessed by the motor bearing lubricating grease currently used in China. With higher load and longer flight time of the airplane, higher requirements are put forward on the reliability and the long service life of components, so that the development of long-service-life anti-wear bearing lubricating grease is needed to meet the use requirements of the existing airplane and the future airplane.
The high-temperature lubricating grease for the aero-motor, which is disclosed by the invention, is completely different from the existing aero-motor bearing lubricating grease in China due to the fact that the base oil is the compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil.
The Russian C-E & En grease conforms to the standard requirement of TYB381011242-89, the composite calcium thickening pentaerythritol ester is used, the use temperature range is-60-180 ℃, the use temperature range is wide, and due to the use of the ester base oil, the Russian C & En grease has good wear resistance and long service life and is used for aviation motors, starting motor bearings and the like. A variety of lubricating grease products such as Usin-207, usin-281, usin-221, uchin-122-7, and Usin-242 can be substituted. In China, various lubricating grease products in the temperature range, such as 933, kk-3, 7112, 7104 and other electric motor lubricating greases, mainly use silicone oil as base oil, or the silicone oil is mainly used as auxiliary oil and mixed with a small amount of ester oil base oil, has a certain difference with Russian products in the aspect of wear resistance, and has the problem of short service life for medium and high power electric motor equipment due to the defect of self wear resistance of the lubricating grease. Meanwhile, the Russian standard product uses ester oil base oil, so that the water resistance is problematic, and the use of the Russian standard product is limited.
The performance of the lubricating grease for aviation high-temperature motor bearings is superior to that of the Russia boaka lubricating grease, and the lubricating grease has excellent extreme pressure performance, abrasion resistance, water resistance, oxidation resistance and long service life.
In the PAO based motor grease according to the present invention, the choice of base oil has a decisive influence on the final properties of the grease. The target lubricating grease needs to have excellent high-temperature performance and low-temperature performance at the same time, so that the selection of base oil is directly limited, and the conventional lubricating grease uses ester oil, silicone oil or mixed oil of the ester oil and the silicone oil as the base oil and has the inherent defects of insufficient abrasion resistance or insufficient water resistance respectively. For this purpose, the invention selects the compound oil using PAO6 base oil, alkyl naphthalene base oil and ester oil as base oil. A small amount of ester oil base oil can improve the low-temperature performance of the lubricating grease and improve the sensitivity of the additive, but the water resistance can be affected at the same time, so the dosage needs to be controlled; the small amount of alkylnaphthalene improves the sensitivity of the grease to additives and improves the antioxidant properties, but reduces the low temperature properties of the grease, so the amount of alkylnaphthalene used needs to be controlled. The PAO base oil has the characteristics of high viscosity index, low-temperature flow property number, high-temperature viscosity retention, low pour point, low volatility, thermal oxidation stability and the like, is the core base oil used in the invention, has lower sensitivity to additives than ester oil and alkyl naphthalene, and can overcome the defect by selecting a proper additive system. The PAO base oil mainly comprises oil products such as PAO2, PAO4, PAO6, PAO8, PAO10 and the like, and is produced by FOX, mobil, dalian macrogen and the like in Shanghai. In the technical scheme of the invention, the PAO base oil adopted by the inventor is between PAO4 and PAO10, preferably between PAO6 and PAO8, and most preferably PAO6. Depending on the low temperature requirements, a higher viscosity PAO base oil may be selected.
Alkyl naphthalene base oil (SynNaph)
AN5, shanghai Nake lubrication technology Co., ltd (NACO)
Alkylated aromatic ring compounds have been used as base oils for lubricating oils in germany as early as the world war ii, but have not been used in large quantities until recently. The alkylated aromatic ring base oil comprises a very wide range of liquids, and the different properties of different alkylated aromatic ring base oils are very different, so that the alkylated aromatic ring base oils with different properties can be synthesized by selecting different aromatic ring compounds. In particular, the alkylated aromatic ring base oils may be an alkyl naphthalene base oil, an alkyl benzene base oil, and a heteroatom-containing alkyl aromatic ring base oil, respectively.
The electron-rich naphthalene ring in the alkyl naphthalene base oil can absorb oxygen to interrupt the transmission of an oxidation chain, prevent the continuous oxidation of alkane radicals and prevent the oxidation.
The grease according to the invention further comprises a modifier selected from n-hexanol, n-heptanol or n-octanol, preferably n-heptanol. By adding long-chain alkyl alcohol, the structure of the thickener soap is improved, the shear stability of the lubricating grease is improved, and the completion of the second step saponification reaction is facilitated. The inventor researches and discovers that if the alkyl chain of the alkyl alcohol as a modifier is too short, such as n-butyl alcohol or n-amyl alcohol, the volatility is too strong, the improvement effect on the soap structure is not ideal, the shear stability of the lubricating grease is insufficient, and the completion of the second step saponification reaction is also not favorable, so that the performance of the lubricating grease is reduced; if the alkyl alcohol has a long alkyl chain, for example, more than 10 carbon atoms, the alkyl alcohol itself has a high boiling point and is not favorable for removing excess alkyl alcohol during the subsequent heating process, and thus the modifier is preferably n-heptanol.
The ester oil comprised in the base oil of the grease according to the present invention is a pentaerythritol ester base oil selected from the group consisting of pentaerythritol n-hexyl ester base oil, pentaerythritol n-heptyl ester base oil and pentaerythritol n-octyl ester base oil, most preferably pentaerythritol n-octyl ester.
In comparison, 1) PAO base oils have difficulty dissolving additives, but ester base oils can more easily dissolve additives; 2) Meanwhile, the PAO base oil corrodes the rubber oil seal to cause shrinkage, the ester corrodes the rubber oil seal to cause expansion, and balance can be achieved through proper allocation; 3) Esters are more hydrophilic than PAO, and particularly, in the present invention, aqueous boric acid and aqueous salicylic acid are used as saponifiers, which puts certain demands on the water solubility of the base oil.
According to the actually measured low-temperature performance of the Russian aka grease, the grease prepared from the PAO8 base oil has similar viscosity exceeding 1800Pa s, and cannot meet the requirements. With PAO4 base oils, evaporation losses are unacceptable.
For the thickener, since the grease product needs to have a high-temperature use environment which can withstand 177 ℃ or even higher for a long time, the high-temperature thickener needs to be used. The Ruoseca boaka lubricating grease uses a composite calcium soap thickener, the thickener can be a composite lithium thickener, a composite calcium thickener, a bentonite thickener, an organic dye thickener and the like, the composite lithium thickener and the composite calcium thickener are preferably selected, the lithium soap thickener is most preferably selected, and the composite lithium thickener has the characteristics of excellent high and low temperature performance, water resistance, good sensitivity to additives and the like.
According to the application field of the PAO-based motor lubricating grease, the lubricating grease needs to have excellent high and low temperature performance, and meanwhile, the lubricating grease also needs to have better wear resistance, extreme pressure performance, water resistance and long service life, so that a proper additive needs to be added to modify the lubricating grease, and the wear resistance, extreme pressure performance, water resistance, service life and the like of the lubricating grease are improved.
For the antioxidant, since the grease product needs to have excellent high-temperature performance and long service life, the antioxidant having excellent use performance is required. The antioxidant of the invention is selected from phenol type antioxidant and amine type antioxidant, and alkyl thiocarbamate or ester and the like as auxiliary materials, preferably p-diisooctyl diphenylamine, compound amine antioxidant 9317, 4 'methylene-bis (2, 6-di-tert-butylphenol), antioxidant 1076, antioxidant 1010, 7723 or a combination of two or three of the two or three in any weight proportion, and most preferably compound amine antioxidant 9317, 4' methylene-bis (2, 6-di-tert-butylphenol) and antioxidant 7723. The antioxidant combination has good synergistic effect and excellent oxidation resistance.
As to the anti-wear agentIn other words, since the anti-wear performance of the grease product is a characteristic requirement and is one of the important means for improving the service life of the grease product, it is necessary to use a suitable anti-wear agent to make the grease have good anti-wear performance. The antiwear agent of the invention is selected from molybdenum disulfide, graphite and CaCO 3 One or two of mercaptobenzothiadiazole, thiadiazole derivative and phosphate ester are combined according to any weight proportion.
For rust inhibitors, grease products are required to have good barrier properties, which is also one of the important measures to ensure their long life characteristics. The antirust agent used in the invention is selected from one or a combination of two of benzotriazole and derivatives thereof, thiadiazole and derivatives thereof and overbased barium sulfonate according to any weight proportion.
The pretreated base oil is then saponified in a first step by adding azelaic acid, 12-hydroxystearic acid and a portion of the lithium hydroxide. Boric acid, salicylic acid and the remaining lithium hydroxide are then added to perform a second saponification. By selecting a specific saponifying agent and a two-step saponification method, the dropping point, the mechanical stability, the oxidation resistance, the high-temperature bearing service life, the wear resistance and other properties of the final product of the lubricating grease are further improved.
In addition, the ester oil base oil needs to be added after completion of saponification. The inventors have found that if the lipid oil base oil is added prematurely, for example, after the first saponification step, before the second saponification step, or before the entire saponification process, it is possible that the ester bonds in the ester oil base oil are broken, resulting in a reduction in the final product properties. The product performance is also greatly influenced by reasonably controlling the adding time of the lipid oil base oil.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Examples
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention.
Example 1
1) According to the following weight ratio of 86
AN5, NACO lubricating technology, inc. (NACO) 26.08g, and ester oil (Shandongting coal Intelligent Equipment, inc.) 26.08g, total 372.5g.
2) Adding PAO6 base oil and alkyl naphthalene base oil into a reaction kettle, heating to 100-110 ℃ under stirring, adding 16.2g of azelaic acid, adding 51.7g of 12-hydroxystearic acid after the azelaic acid is dissolved, cooling while dissolving the 12-hydroxystearic acid, slowly adding a lithium hydroxide suspension when the temperature is reduced to 98 ℃, wherein the molar total amount of lithium hydroxide is equal to the molar amount of the 12-hydroxystearic acid and twice the molar amount of the azelaic acid (the LiOH suspension is formed by dissolving LiOH & H2O by using distilled water at 100 ℃, the weight ratio of LiOH to water is about 1).
3) Adding a 90 ℃ saturated boric acid aqueous solution (containing 7.5g of boric acid) and a salicylic acid isobutanol solution (containing 10g of salicylic acid), then slowly adding a lithium hydroxide suspension, wherein the molar total amount of lithium hydroxide is equal to the molar amount of boric acid and twice the molar amount of salicylic acid, heating to 105 ℃, saponifying for 2 hours, heating to 140-150 ℃, dehydrating for 1 hour, heating to 180-190 ℃, keeping for 10 minutes, adding pentaerythritol n-heptyl base oil and 35g of n-heptyl alcohol, naturally cooling, adding an antioxidant, an antiwear agent, an extreme pressure agent and an antirust agent at 100-110 ℃, keeping for stirring for 30 minutes at a constant temperature, cooling to room temperature, and homogenizing to obtain 500g of a final lubricating grease product.
Wherein, based on 100 parts by weight of the final grease product, the base oil content is about 74.5%, the modifier content is 7%, and the thickener content is 12.9%; the antioxidant content is 2%, the antiwear agent content is 1.5%, the extreme pressure agent content is 1.5%, and the antirust agent content is 0.6%.
Based on 100 parts by weight of the final grease product,
the antioxidant is 1% of a compound amine antioxidant 9317 and 1% of 4,4' methylene-2, 4,6 di-tert-butylphenol.
The antiwear agent is as follows: 1.5% thiadiazole.
The extreme pressure agent is: 1.5% mercaptobenzothiadiazole.
The antirust agent is as follows: 0.1% benzotriazole, 0.25% rust inhibitor 323 (manufacturer: van der waals, is a derivative of benzotriazole) and 0.25% rust inhibitor 424 (manufacturer: van der waals, is a derivative of thiadiazole).
Comparative example 1
A grease product was prepared in the same manner as in example 1, except that n-heptanol, a modifier, was not added, wherein the modifier was changed to a thickener of equal weight.
Comparative example 2
A grease product was prepared in the same manner as in example 1, except that the lipid oil pentaerythritol n-heptyl ester base oil was not added in step 3).
Test example 1: abrasion resistance test
The conventional 7031A grease, 936 grease, 7014 grease, calcium sulfate grease and the grease of example 1 of the present invention were tested for anti-wear properties according to the method described in astm5707, and the results are shown in table 1 below, SRV test conditions: 20kg, stroke 1mm,50 ℃,120 minutes, 50HZ.
TABLE 1
From the data in table 1, it can be seen that the grease of the present invention has the smallest wear scar diameter after the detection in the same manner, which indicates that the grease of the present invention has excellent anti-wear lubricating effect.
Test example 2: extreme pressure Performance test
The grease product prepared in example 1 and the grease of ammonium sulfate were tested according to the test methods described in SH/T0202-1992, GB/T269, and ASTM5483 standards, and the results are set forth in Table 2 below.
TABLE 2
Test example 3: test for Oxidation resistance
The oxidation resistance of the conventional grease for carbon dioxide and the grease of example 1 of the present invention were tested according to the method described in ASTM5483 standard, and the results are shown in table 3 below.
TABLE 3
In table 3 the term "new grease" refers to a grease product that has not been used before the test, and "518h post-use grease" refers to a grease product that has been used 518 hours before the test. As can be seen from the data in table 3, the oxidation induction period of the unused product of the grease of the present invention is more than 3 times that of the Russian grease, and is still higher than that of the Russian grease even after 518 hours of use.
Test example 4: high temperature bearing performance testing
The grease product prepared in example 1 was tested according to the test method described in SH/T0248-1992, and the results are listed in Table 4 below.
TABLE 4
Test example 5: actual performance test
The grease of example 1 and russia sulfate were used in a 60kVA generator. After the actual use test, samples of the two motors were taken, the sample points were respectively a generator transmission end holder, a generator transmission end cover and a generator ventilation end cover, PDSC (high differential pressure thermal scanning), SRV (high frequency linear oscillation test) and elemental analysis were performed on the two samples of ethylene oxide, and the results are listed in table 5 below, wherein the PDSC test was performed according to the method described in ASTM D5483, the SRV test was performed according to the method described in ASTM D5707, and the elemental analysis was performed according to the method described in NB/SH/T0865 in the atomic emission spectrometry for measuring wear metals and pollution elements in lubricating oil.
Table 5: analysis of grease samples after testing
It can be seen that the grease of example 1 in accordance with the present invention has excellent antioxidant and antiwear properties even after 1400+ hours of actual use, and the actual use performance is far superior to that of the russian grease.
Claims (7)
1. A preparation method of lubricating grease for aviation high-temperature motor bearings comprises the following steps:
1) Adding PAO6 base oil and alkyl naphthalene base oil with preset weight into a reaction kettle, adding a modifier while stirring, heating to 100-110 ℃, adding azelaic acid, adding 12-hydroxystearic acid after the azelaic acid is dissolved, cooling while dissolving the 12-hydroxystearic acid, slowly adding a lithium hydroxide suspension when the temperature is reduced to 98 ℃, wherein the molar total amount of lithium hydroxide is equal to the molar amount of 12-hydroxystearic acid and twice the molar amount of azelaic acid, heating to 105 ℃, saponifying for 2 hours, heating to 120-130 ℃, and dehydrating for 1 hour;
2) Then adding a saturated boric acid aqueous solution and a salicylic acid solution at the temperature of 90 ℃, heating to 140-150 ℃, slowly adding a lithium hydroxide suspension, wherein the molar total amount of lithium hydroxide is equal to the molar weight of boric acid and twice the molar weight of salicylic acid, saponifying for 2 hours, dehydrating for 1 hour, heating to 180-190 ℃, keeping for 10 minutes, adding pentaerythritol n-heptyl base oil, naturally cooling, adding an antioxidant, an antiwear agent, an extreme pressure agent and an antirust agent at the temperature of 100-110 ℃, keeping stirring at a constant temperature for 30 minutes, cooling to room temperature, and homogenizing to obtain a final product;
the base oil is a compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil, the weight ratio of the base oil to the alkyl naphthalene base oil is 86:7:7, and the ester oil is pentaerythritol n-heptyl ester base oil;
the addition amount of the azelaic acid is 4-6 parts by weight and the addition amount of the 12-hydroxystearic acid is 11-15 parts by weight based on 100 parts by weight of the compound oil of PAO6 base oil, alkyl naphthalene base oil and ester oil;
the modifier is n-heptanol.
2. The method according to claim 1, wherein the lithium hydroxide suspension in the step 1) is LiOH. H 2 Suspension of O in which LiOH. H 2 The weight ratio of O to water is 1.
3. The method according to claim 1, wherein the boric acid is added in an amount of 1 to 3 parts by weight and the salicylic acid is added in an amount of 1.5 to 3.5 parts by weight, based on 100 parts by weight of the formulated oil of the PAO6 base oil, the alkylnaphthalene base oil and the ester oil.
4. The method according to claim 1, wherein the salicylic acid solution is an isobutanol solution of salicylic acid obtained by dissolving salicylic acid in isobutanol.
5. The preparation method according to claim 1, wherein the modifier is added in an amount of 7% based on 100 parts by weight of a formulated oil of the PAO6 base oil, the alkylnaphthalene base oil and the ester oil;
the antioxidant is one or the combination of two or three of p-diisooctyl diphenylamine, a compound amine antioxidant 9317 and 4,4' -methylene-bis (2, 6-di-tert-butylphenol), an antioxidant 1076, an antioxidant 1010 and an antioxidant 7723 according to any weight proportion;
the antiwear agent is selected from one or a combination of more of tricresyl phosphate and derivatives thereof, zinc dialkyl dithiocarbamate, zinc dialkyl dithiophosphate, antimony dialkyl dithiocarbamate and thiadiazole according to any weight ratio;
the extreme pressure agent is selected from molybdenum disulfide, graphite and CaCO 3 One or two of mercaptobenzothiadiazole and phosphate ester are combined according to any weight proportion;
the antirust agent is one or a combination of two of benzotriazole and derivatives thereof, thiadiazole and derivatives thereof, and high-alkaline barium sulfonate according to any weight proportion.
6. The lubricating grease for aviation high-temperature motor bearings, which is prepared according to the preparation method of claim 1, is characterized in that based on the weight of the lubricating grease, the lubricating grease comprises the following components in percentage by weight:
the base oil content is 70% to 85%;
the thickening agent content is 10-25%;
the content of the antioxidant is 3 to 8 percent;
the content of the antiwear agent is 1 to 3 percent;
the content of the extreme pressure agent is 1 to 3 percent;
the content of the antirust agent is 0.5 to 1.0 percent;
the sum of the total amount of all the components is 100 percent.
7. The lubricating grease for aviation high-temperature motor bearings, which is prepared according to the preparation method of claim 1, is characterized in that based on the weight of the lubricating grease, the lubricating grease comprises the following components in percentage by weight:
the base oil content was 74.5%;
the thickening agent content is 17.9%;
the content of the antioxidant is 3 percent;
the content of the antiwear agent is 2.5 percent;
the content of the extreme pressure agent is 1.5 percent;
the content of the antirust agent is 0.6 percent
The sum of the total amount of all the components is 100 percent.
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| CN101955835A (en) * | 2010-10-13 | 2011-01-26 | 中国石油化工股份有限公司 | Composition of four-component lithium complex grease and preparation method thereof |
| CN102807908A (en) * | 2012-09-04 | 2012-12-05 | 陕西省石油化工研究设计院 | Wide temperature range polyol ester lubricating oil composition suitable for aircraft engine |
| CN103333726A (en) * | 2013-07-25 | 2013-10-02 | 中国石油化工股份有限公司 | Lithium base grease and preparation method thereof |
| CN103666658A (en) * | 2013-12-19 | 2014-03-26 | 中国人民解放军空军油料研究所 | Multi-use universal aviation grease |
| CN112063434A (en) * | 2020-09-18 | 2020-12-11 | 刘佩仓 | High-temperature lubricating grease for aviation and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015172846A1 (en) * | 2014-05-16 | 2015-11-19 | Ab Nanol Technologies Oy | Additive composition for lubricants |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955835A (en) * | 2010-10-13 | 2011-01-26 | 中国石油化工股份有限公司 | Composition of four-component lithium complex grease and preparation method thereof |
| CN102807908A (en) * | 2012-09-04 | 2012-12-05 | 陕西省石油化工研究设计院 | Wide temperature range polyol ester lubricating oil composition suitable for aircraft engine |
| CN103333726A (en) * | 2013-07-25 | 2013-10-02 | 中国石油化工股份有限公司 | Lithium base grease and preparation method thereof |
| CN103666658A (en) * | 2013-12-19 | 2014-03-26 | 中国人民解放军空军油料研究所 | Multi-use universal aviation grease |
| CN112063434A (en) * | 2020-09-18 | 2020-12-11 | 刘佩仓 | High-temperature lubricating grease for aviation and production method thereof |
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