Preparation method of modified silicone oil for high-temperature-resistant lubricating oil

Perfluoroalkyl modified amino silicone oil was prepared through esterification, amino silicone oil modification and polymerization, which solved the problem of poor use of silicone oil in high-temperature environments and achieved modified silicone oil with high chemical stability and corrosion resistance.

CN119505113AInactive Publication Date: 2025-02-25GUANGZHOU CAMAROL LUBRICANTS CO LTD
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Patent Information

Application Number
CN202411316669.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-20
Publication Date
2025-02-25
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Existing silicone oil is not effective in high-temperature environments, and it is difficult to meet the needs of modern industry for high-temperature lubrication.

Method used

Perfluoroalkyl modified amino silicone oil is prepared by esterification reaction and amino silicone oil modification, combined with anion ring-opening polymerization reaction and grafting reaction, and mixed with polyalkylphenyl silicone oil to form modified silicone oil for high-temperature resistant lubricating oil.

Benefits of technology

Excellent low surface tension, hydrophobicity, high chemical stability and corrosion resistance are obtained, which significantly improves the performance of silicone oil in high temperature environments.

✦ Generated by Eureka AI based on patent content.
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Abstract

The invention relates to the technical field of lubricating oil, and provides a preparation method of modified silicone oil for high-temperature-resistant lubricating oil, which comprises the following steps: preparing perfluoroalkyl modified amino silicone oil; preparing single-ended hydrogen-containing silicone oil; preparing a polyalkyl phenyl silicone oil mixture; and mixing the polyalkyl phenyl silicone oil mixture, perfluoroalkyl modified amino silicone oil and alkylene trimethoxy silane, adding cyclohexene and alpha-methyl styrene, adding a second catalyst in two times under the protection of inert gas, respectively carrying out heating reaction for a period of time, and carrying out vacuum treatment to remove low-boiling-point substances, thereby obtaining the modified silicone oil for the high-temperature-resistant lubricating oil. The obtained modified silicone oil has excellent molecular structure strength, high temperature resistance, chemical stability, hydrophobicity, oxidation resistance, corrosion resistance and the like, is endowed with excellent use performance, and has wide application prospects in the field of high-temperature lubricating oil.
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Description

Technical Field

[0001] The invention relates to the technical field of lubricating oils, and in particular to a method for preparing modified silicone oil for high-temperature resistant lubricating oils. Background Art

[0002] Lubricating oil is widely used in chemical, textile, machinery and other industries. Lubricating oil is mainly composed of two parts: base oil and additives. Base oil is the main component of lubricating oil, accounting for more than 85%. With the rapid development of science and technology, especially the rapid development of the automobile industry, and the strengthening of environmental protection and energy-saving requirements, although the total supply of lubricating oil has not increased significantly, the demand for high-end lubricating oil is growing. High speed and high temperature, these factors will lead to an increase in the temperature of the friction pair surface, and the high temperature state will have a huge impact on the friction coefficient and wear rate of the friction pair system. Therefore, the development of high temperature resistant lubricating oil has become a research hotspot in the field of lubricating oil in recent years.

[0003] Silicone oil has excellent heat resistance, electrical insulation, weather resistance, hydrophobicity, physiological inertness and low surface tension, as well as low viscosity-temperature coefficient and high compression resistance. In addition, silicone oil has many special properties, such as anti-oxidation, high flash point, low volatility, no corrosion to metals, and non-toxicity. As a high-grade lubricant, how to improve the use of silicone oil in high-temperature environments and high-temperature environments caused by high speeds is a technical problem that needs to be solved urgently in modern industry. Summary of the invention

[0004] The purpose of the present invention is to solve at least one of the technical problems existing in the prior art and provide.

[0005] The technical solution of the present invention is as follows:

[0006] Another aspect of the present invention provides a method for preparing a modified silicone oil for high temperature resistant lubricating oil, comprising the following steps:

[0007] S1, adding perfluoroalkylethanol and an alkenyl-containing organic acid into a solvent for esterification to obtain perfluoroalkylethanol organic acid ester, and then reacting the perfluoroalkylethanol organic acid ester with aminosilicone oil to obtain perfluoroalkyl-modified aminosilicone oil;

[0008] S2, mixing hexamethylcyclotrisiloxane with a solvent, adding a first catalyst to carry out anionic ring-opening polymerization, and then adding a capping agent to react to obtain a single-terminal hydrogen-containing silicone oil;

[0009] S3, after the single-end hydrogen-containing silicone oil and methylphenylcyclotetrasiloxane are evenly mixed, an inert gas is introduced, and then isopropanol, vanadium trichloride-tetrahydrofuran complex, and metallocene complex are added, and the mixture is heated to 70-80° C. and stirred for 2-4 hours, and then the temperature is lowered and the isopropanol is removed by distillation under reduced pressure;

[0010] S4, mixing the product obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane, adding cyclohexene and α-methylstyrene, heating to 70-100° C. and stirring under the protection of inert gas, then adding a portion of catalyst, heating to 90-130° C. and reacting for 1.5-3 hours;

[0011] S5. Add the remaining catalyst under the protection of inert gas, keep the temperature at 100-120°C and stir to react for 2-4 hours. After the reaction is completed, continue to heat to 150-160°C and keep warm for a period of time. Vacuum treatment to remove low-boiling substances to obtain modified silicone oil for high-temperature resistant lubricating oil.

[0012] Aminosilane is modified by long-chain fluorinated alkyl groups to solve the oxidation problem of amino groups, and at the same time, excellent properties such as low surface tension, hydrophobicity, high chemical stability and corrosion resistance are obtained; single-end hydrogen-containing silicone oil is first reacted with methylphenylcyclotetrasiloxane to obtain a polyalkylphenyl silicone oil mixture with good heat resistance; finally, perfluoroalkyl-modified aminosilicone oil, polyalkylphenyl silicone oil mixture, olefin trimethoxysilane are reacted with cyclohexene and α-methylstyrene to obtain polyolefin-grafted functional silicone oil, and the reaction adds carbon-carbon double bonds to Si-O-Si side chain groups, which can undergo grafting reaction with the polyalkylphenyl silicone oil mixture to obtain perfluoroalkyl-modified phenylaminomethoxy silicone oil, which has excellent molecular structure strength, high and low temperature resistance, chemical stability, hydrophobicity, oxidation resistance and corrosion resistance, etc., giving the modified silicone oil excellent performance.

[0013] As a preferred technical solution of the present invention, in step S1:

[0014] The perfluoroalkylethanol includes at least one of perfluorohexylethanol, perfluoroheptylethanol and perfluorooctylethanol;

[0015] The alkenyl-containing organic acid includes at least one of 3-decenoic acid and itaconic acid.

[0016] As a preferred technical solution of the present invention, the temperature of the anionic ring-opening polymerization reaction in step S2 is 20-30°C.

[0017] As a preferred technical solution of the present invention, the solvent in step S2 includes at least one of n-hexane, cyclohexane, ethylcyclohexane, toluene, xylene, and trimethylbenzene, the first catalyst includes alkyl lithium and alkyl alcohol lithium, and the capping agent includes at least one of dimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, and trimethylchlorosilane.

[0018] As a preferred technical solution of the present invention, the cooling temperature in step S3 is 40-55°C, and the mass ratio of the perfluoroalkyl modified amino silicone oil, the polyalkylphenyl silicone oil mixture, and the olefin trimethoxy silane in step S4 is 1-3:3-6:2-5.

[0019] As a preferred technical solution of the present invention, the total amount of cyclohexene and α-methylstyrene used in step S4 is 1 to 1.5 times the total mass of perfluoroalkyl modified amino silicone oil, polyalkylphenyl silicone oil mixture, and olefin trimethoxy silane.

[0020] As a preferred technical solution of the present invention, the catalyst in step S4 is a Karstedt catalyst.

[0021] As a preferred technical solution of the present invention, the stirring time in step S4 is 2 to 4 hours, and the amount of the catalyst added is 70 to 90 wt % of the total amount of the catalyst.

[0022] As a preferred technical solution of the present invention, the amount of the remaining catalyst added in step S5 is 10-30wt% of the total amount of the catalyst, and the insulation time is 45-90 minutes.

[0023] As a preferred technical solution of the present invention, the relative vacuum degree of the vacuum treatment in step S5 is -0.10 to -0.06 MPa, the temperature is 170 to 200° C., and the time is 20 to 40 minutes.

[0024] Another aspect of the present invention provides a modified silicone oil for high temperature resistant lubricating oil, which is prepared according to any of the preparation methods described above.

[0025] The beneficial effects that can be achieved by the present invention are:

[0026] The aminosilane is modified by a long-chain fluorinated alkyl group, which solves the oxidation problem of the amino group and obtains excellent properties such as low surface tension, hydrophobicity, high chemical stability and corrosion resistance; the single-end hydrogen-containing silicone oil and methylphenylcyclotetrasiloxane are first reacted to obtain a polyalkylphenyl silicone oil mixture with good heat resistance; finally, the perfluoroalkyl-modified aminosilicone oil, the polyalkylphenyl silicone oil mixture, and the olefin trimethoxysilane are reacted with cyclohexene and α-methylstyrene to obtain a functional silicone oil grafted and modified by polyolefins, and the reaction adds a carbon-carbon double bond to the Si-O-Si branched group, which can undergo a grafting reaction with the polyalkylphenyl silicone oil mixture to obtain a multifunctional perfluoroalkyl-modified phenyl aminomethoxy silicone oil. The present invention controls the reaction process by adding the catalyst twice, reduces side reactions, and ensures the molecular structure of the modified silicone oil. The addition of olefins can increase the reaction coupling between the polyalkylphenyl silicone oil mixture, the perfluoroalkyl-modified aminosilicone oil and the olefin trimethoxysilane, improve the strength of the product molecular structure, and finally form a modified silicone oil for high temperature resistant lubricating oil. The reaction process of the invention is controllable and has higher reaction rate and selectivity.

[0027] The modified silicone oil obtained by the present invention has excellent molecular structure strength, high temperature resistance, chemical stability, hydrophobicity, oxidation resistance and corrosion resistance, etc., which gives the modified silicone oil excellent performance and has broad application prospects in the field of high-temperature lubricating oils. DETAILED DESCRIPTION

[0028] The technical scheme in the embodiments of the present invention is clearly and completely described below. Obviously, the described embodiments are exemplary and are only used to explain the present invention, and cannot be interpreted as limiting the present invention. If specific techniques or conditions are not specified in the embodiments, they are carried out according to the techniques or conditions described in the literature in this area or according to the product instructions. The reagents or instruments used are conventional products that can be obtained by commercial purchase if the manufacturer is not specified.

[0029] Example 1

[0030] A method for preparing modified silicone oil for high temperature resistant lubricating oil comprises the following steps:

[0031] S1. Add 120 g of perfluorohexylethanol and 25 g of 3-decenoic acid to toluene for esterification to obtain perfluoroalkylethanol organic acid ester, and then react the perfluoroalkylethanol organic acid ester with aminosilicone oil at a mass ratio of 2.5:1 to obtain perfluoroalkyl modified aminosilicone oil;

[0032] S2, 150g of hexamethylcyclotrisiloxane was mixed with an equal amount of n-hexane, 17g of methyl lithium and 18g of methyl lithium alkoxide were added to carry out anionic ring-opening polymerization at 20-25°C, and then 2g of end-capping agent dimethylchlorosilane was added to react to obtain single-terminated hydrogen-containing silicone oil;

[0033] S3, after 100g of single-ended hydrogen-containing silicone oil and 100g of methylphenylcyclotetrasiloxane are uniformly mixed, an inert gas is introduced, and then isopropanol, 2g of vanadium trichloride-tetrahydrofuran complex, and 1g of metallocene complex are added, heated to 70°C and mixed and stirred for 4h, then cooled to 40°C, and isopropanol is removed by reduced pressure distillation to obtain a polyalkylphenyl silicone oil mixture;

[0034] S4, mixing the polyalkylphenyl silicone oil mixture obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane in a mass ratio of 3:1:5, adding cyclohexene and α-methylstyrene (mass ratio 1:1), the total mass of cyclohexene and α-methylstyrene being equal to the total mass of the aforementioned three reactants, heating to 70° C. and stirring for 4 h under the protection of inert gas, then adding 0.5 wt% of the total mass of the aforementioned five reactants, and heating to 90-130° C. for reaction for 1.5-3 h;

[0035] S5. Under the protection of inert gas, add 0.2 wt% of the total mass of the above five reactants into a Karstedt catalyst, keep the temperature at 100°C and stir to react for 4 hours. After the reaction is completed, continue to heat to 150°C and keep warm for 90 minutes. Under the conditions of relative vacuum degree of -0.10 MPa and temperature of 170°C, vacuum treat for 40 minutes to remove low-boiling substances, and obtain modified silicone oil for high-temperature resistant lubricating oil.

[0036] Example 2

[0037] A method for preparing modified silicone oil for high temperature resistant lubricating oil comprises the following steps:

[0038] S1. Add 130 g of perfluorooctylethanol and 25 g of itaconic acid into toluene for esterification reaction to obtain perfluoroalkylethanol organic acid ester, and then react the perfluoroalkylethanol organic acid ester with aminosilicone oil in a mass ratio of 2:1 to obtain perfluoroalkyl modified aminosilicone oil;

[0039] S2, 150g of hexamethylcyclotrisiloxane was mixed with an equal amount of xylene, 19g of methyl lithium and 16g of methyl lithium alkoxide were added to carry out anionic ring-opening polymerization at 25-30°C, and then 2.5g of end-capping agent trimethylchlorosilane was added to react to obtain single-terminated hydrogen-containing silicone oil;

[0040] S3, after 100g of single-ended hydrogen-containing silicone oil and 80g of methylphenylcyclotetrasiloxane are uniformly mixed, an inert gas is introduced, and then isopropanol, 1.7g of vanadium trichloride-tetrahydrofuran complex, and 0.8g of metallocene complex are added, heated to 80°C and mixed and stirred for 2h, and then cooled to 55°C, and isopropanol is removed by vacuum distillation to obtain a polyalkylphenyl silicone oil mixture;

[0041] S4, mixing the polyalkylphenyl silicone oil mixture obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane in a mass ratio of 6:3:2, adding cyclohexene and α-methylstyrene (mass ratio of 1:1), wherein the total mass of cyclohexene and α-methylstyrene is 1.5 times the total mass of the aforementioned three reactants, heating to 100° C. and stirring for 2 h under the protection of an inert gas, then adding 0.95 wt% of the total mass of the aforementioned five reactants, and heating to 130° C. for reaction for 1.5 h;

[0042] S5. Under the protection of inert gas, add 0.11 wt% of the total mass of the above five reactants into a Karstedt catalyst, keep the temperature at 120°C and stir to react for 2 hours. After the reaction is completed, continue to heat to 160°C and keep warm for 45 minutes. Under the conditions of relative vacuum degree of -0.06Mpa and temperature of 200°C, vacuum treat for 20 minutes to remove low-boiling substances, and obtain modified silicone oil for high-temperature resistant lubricating oil.

[0043] Example 3

[0044] A method for preparing modified silicone oil for high temperature resistant lubricating oil comprises the following steps:

[0045] S1. Add 125 g of perfluoroheptylethanol and 20 g of itaconic acid into toluene for esterification to obtain perfluoroalkylethanol organic acid ester, and then react the perfluoroalkylethanol organic acid ester with aminosilicone oil in a mass ratio of 3:1 to obtain perfluoroalkyl modified aminosilicone oil;

[0046] S2, 150g of hexamethylcyclotrisiloxane was mixed with an equal amount of toluene, 15g of methyl lithium and 20g of methyl lithium alkoxide were added to carry out anionic ring-opening polymerization at 20-30°C, and then 1.5g of end-capping agent dimethyldichlorosilane was added to react to obtain single-terminal hydrogen-containing silicone oil;

[0047] S3, after 100g of single-end hydrogen-containing silicone oil and an equal amount of methylphenylcyclotetrasiloxane are mixed evenly, an inert gas is introduced, and then isopropanol, 1.5g of vanadium trichloride-tetrahydrofuran complex, and 1.2g of metallocene complex are added, heated to 75°C and mixed and stirred for 3.5h, and then cooled to 45°C, and isopropanol is removed by vacuum distillation to obtain a polyalkylphenyl silicone oil mixture;

[0048] S4, after mixing the polyalkylphenyl silicone oil mixture obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane in a mass ratio of 5:2.5:3, cyclohexene and α-methylstyrene (mass ratio 1:1.5) are added, the total mass of cyclohexene and α-methylstyrene is 1.2 times the total mass of the above three reactants, heating to 80°C and stirring for 3.5h under the protection of inert gas, then adding 0.45wt% of the total mass of the above five reactants Karstedt catalyst, heating to 90-130°C and reacting for 1.5-3h;

[0049] S5. Under the protection of inert gas, add 0.18 wt% of the total mass of the above five reactants, Karstedt catalyst, keep the temperature at 105°C and stir to react for 3.5 hours. After the reaction is completed, continue to heat to 155°C and keep warm for 60 minutes. Under the conditions of relative vacuum degree of -0.07 MPa and temperature of 180°C, vacuum treat for 30 minutes to remove low-boiling substances, and obtain modified silicone oil for high-temperature resistant lubricating oil.

[0050] Example 4

[0051] A method for preparing modified silicone oil for high temperature resistant lubricating oil comprises the following steps:

[0052] S1. Add 120 g of perfluorooctylethanol and 25 g of itaconic acid into toluene for esterification reaction to obtain perfluoroalkylethanol organic acid ester, and then react the perfluoroalkylethanol organic acid ester with aminosilicone oil at a mass ratio of 2.5:1 to obtain perfluoroalkyl modified aminosilicone oil;

[0053] S2, 150g of hexamethylcyclotrisiloxane and 180g of cyclohexane were mixed, 17g of methyl lithium and 18g of methyl lithium alkoxide were added to carry out anionic ring-opening polymerization at 20-23°C, and then 2g of end-capping agent methyltrichlorosilane was added to react to obtain single-terminated hydrogen-containing silicone oil;

[0054] S3, after 100g of single-end hydrogen-containing silicone oil and an equal amount of methylphenylcyclotetrasiloxane are mixed evenly, an inert gas is introduced, and then isopropanol, 2.1g of vanadium trichloride-tetrahydrofuran complex, and 0.8g of metallocene complex are added, heated to 70°C and mixed and stirred for 3h, and then cooled to 50°C, and isopropanol is removed by vacuum distillation to obtain a polyalkylphenyl silicone oil mixture;

[0055] S4, mixing the polyalkylphenyl silicone oil mixture obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane in a mass ratio of 4:1.5:4, adding cyclohexene and α-methylstyrene (mass ratio 1.5:1), the total mass of cyclohexene and α-methylstyrene is 1.4 times the total mass of the above three reactants, heating to 90°C and stirring for 3h under the protection of inert gas, then adding 0.7wt% of the total mass of the above five reactants, Karstedt catalyst, heating to 90-130°C and reacting for 1.5-3h;

[0056] S5. Under the protection of inert gas, add 0.15wt% of the total mass of the above five reactants into a Karstedt catalyst, keep the temperature at 110°C and stir to react for 3 hours. After the reaction is completed, continue to heat to 150°C and keep warm for 80 minutes. Under the conditions of relative vacuum degree of -0.07Mpa and temperature of 190°C, vacuum treat for 30 minutes to remove low-boiling substances, and obtain modified silicone oil for high-temperature resistant lubricating oil.

[0057] Example 5

[0058] A method for preparing modified silicone oil for high temperature resistant lubricating oil comprises the following steps:

[0059] S1. Add 120 g of perfluorohexylethanol and 25 g of itaconic acid into toluene for esterification reaction to obtain perfluoroalkylethanol organic acid ester, and then react the perfluoroalkylethanol organic acid ester with aminosilicone oil at a mass ratio of 2.5:1 to obtain perfluoroalkyl modified aminosilicone oil;

[0060] S2, 150g of hexamethylcyclotrisiloxane was mixed with 100g of cyclohexane and 50g of toluene, 17g of methyl lithium and 18g of methyl lithium alkoxide were added to carry out anionic ring-opening polymerization at 22-25°C, and then 2g of end-capping agent dimethyldichlorosilane was added to react to obtain single-terminated hydrogen-containing silicone oil;

[0061] S3, after 100g of single-ended hydrogen-containing silicone oil and 120g of methylphenylcyclotetrasiloxane are uniformly mixed, an inert gas is introduced, and then isopropanol, 2g of vanadium trichloride-tetrahydrofuran complex, and 0.75g of metallocene complex are added, heated to 75°C and mixed and stirred for 3h, and then cooled to 45°C, and isopropanol is removed by vacuum distillation to obtain a polyalkylphenyl silicone oil mixture;

[0062] S4, mixing the polyalkylphenyl silicone oil mixture obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane in a mass ratio of 9:4:7, adding cyclohexene and α-methylstyrene (mass ratio of 1:1), the total mass of cyclohexene and α-methylstyrene being 1.3 times the total mass of the aforementioned three reactants, heating to 85° C. and stirring for 3 h under the protection of inert gas, then adding 0.6 wt% of the total mass of the aforementioned five reactants, Karstedt catalyst, heating to 90-130° C. and reacting for 1.5-3 h;

[0063] S5. Under the protection of inert gas, add 0.15wt% of the total mass of the above five reactants into a Karstedt catalyst, keep the temperature at 110°C and stir to react for 3 hours. After the reaction is completed, continue to heat to 155°C and keep warm for 60 minutes. Under the conditions of relative vacuum degree of -0.08Mpa and temperature of 185°C, vacuum treat for 30 minutes to remove low-boiling substances, and obtain modified silicone oil for high-temperature resistant lubricating oil.

[0064] Comparative Example 1

[0065] Step S1 is omitted, and the rest is the same as in Embodiment 5.

[0066] Comparative Example 2

[0067] Steps S2 and S3 are omitted, and the rest is the same as in Example 5.

[0068] Comparative Example 3

[0069] Steps S4 and S5 are combined into one step. In step S4, all the Karstedt catalyst is directly added, the temperature is raised to 90-130° C. for reaction for 3.5-7 hours, and after the reaction is completed, the temperature is further raised to 150-160° C. for preservation for 45-90 minutes. The rest is the same as in Example 5.

[0070] Comparative Example 4

[0071] The cyclohexene and α-methylstyrene were removed, and the rest was the same as in Example 5.

[0072] The performance of the modified silicone oils obtained in Examples 1-5 and Comparative Examples 1-3 was compared, and the results are shown in Table 1:

[0073] Table 1

[0074] Heat resistant temperature Friction coefficient Example 1 546 0.028 Example 2 538 0.027 Example 3 554 0.025 Example 4 557 0.026 Example 5 561 0.023 Comparative Example 1 454 0.053 Comparative Example 2 437 0.049 Comparative Example 3 405 0.058 Comparative Example 4 417 0.056

[0075] As can be seen from the data in Table 1, the modified silicone oil provided by the present invention has excellent high temperature resistance and lubrication performance. Perfluoroalkyl modified amino silicone oil (Comparative Example 1), polyalkylphenyl silicone oil mixture (Comparative Example 2), catalyst added in batches (Comparative Example 3), olefin (Comparative Example 4) will affect the high temperature resistance and lubrication performance of the modified silicone oil obtained. In the present invention, each reactant and catalyst work together to obtain a modified silicone oil for high temperature resistant lubricating oil. In particular, the effect of the catalyst added in batches is the greatest, which may be because more side reactions will be produced when the catalyst is added once, affecting the performance of the final product. The present invention adds the catalyst in two batches to control the reaction process and reduce side reactions; the second olefin (cyclohexene, α-methylstyrene) has a greater impact, and the addition of olefins can increase the reaction coupling between the polyalkylphenyl silicone oil mixture, perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane, improve the strength of the product molecular structure, and finally form a modified silicone oil for high temperature resistant lubricating oil.

[0076] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing modified silicone oil for high temperature resistant lubricating oil, characterized in that: The following steps are involved: S1, adding perfluoroalkylethanol and an alkenyl-containing organic acid into a solvent for esterification to obtain perfluoroalkylethanol organic acid ester, and then reacting the perfluoroalkylethanol organic acid ester with aminosilicone oil to obtain perfluoroalkyl-modified aminosilicone oil; S2, mixing hexamethylcyclotrisiloxane with a solvent, adding a first catalyst to carry out anionic ring-opening polymerization, and then adding a capping agent to react to obtain a single-terminal hydrogen-containing silicone oil; S3, after the single-end hydrogen-containing silicone oil and methylphenylcyclotetrasiloxane are evenly mixed, an inert gas is introduced, and then isopropanol, vanadium trichloride-tetrahydrofuran complex, and metallocene complex are added, and the mixture is heated to 70-80° C. and stirred for 2-4 hours, and then the temperature is lowered and the isopropanol is removed by distillation under reduced pressure; S4, mixing the product obtained in step S3 with perfluoroalkyl modified amino silicone oil and olefin trimethoxysilane, adding cyclohexene and α-methylstyrene, heating to 70-100° C. and stirring under the protection of inert gas, then adding a portion of the second catalyst, heating to 90-130° C. and reacting for 1.5-3 hours; S5. Add the remaining second catalyst under the protection of inert gas, maintain the temperature at 100-120°C and stir to react for 2-4 hours. After the reaction is completed, continue to heat to 150-160°C and keep warm for a period of time. Vacuum treatment is performed to remove low-boiling substances to obtain modified silicone oil for high-temperature resistant lubricating oil.

2. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: In step S1: The perfluoroalkylethanol includes at least one of perfluorohexylethanol, perfluoroheptylethanol and perfluorooctylethanol; The alkenyl-containing organic acid includes at least one of 3-decenoic acid and itaconic acid.

3. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The temperature of the anionic ring-opening polymerization reaction in step S2 is 20-30°C.

4. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The solvent in step S2 includes at least one of n-hexane, cyclohexane, ethylcyclohexane, toluene, xylene, and trimethylbenzene, the first catalyst includes alkyl lithium and alkyl lithium alcohol, and the end-capping agent includes at least one of dimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, and trimethylchlorosilane.

5. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The cooling temperature in step S3 is 40-55° C., and the mass ratio of the perfluoroalkyl modified amino silicone oil, the polyalkylphenyl silicone oil mixture, and the olefin trimethoxy silane in step S4 is 1-3:3-6:2-5.

6. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The total amount of cyclohexene and α-methylstyrene used in step S4 is 1 to 1.5 times the total mass of perfluoroalkyl modified amino silicone oil, polyalkylphenyl silicone oil mixture, and olefin trimethoxysilane, and the second catalyst is a Karstedt catalyst.

7. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The stirring time in step S4 is 2 to 4 hours, and the amount of the second catalyst added is 70 to 90 wt % of the total amount of the catalyst.

8. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: In step S5, the amount of the remaining second catalyst added is 10-30wt% of the total amount of the catalyst, and the insulation time is 45-90 minutes.

9. The method for preparing a modified silicone oil for high temperature resistant lubricating oil according to claim 1, characterized in that: The relative vacuum degree of the vacuum treatment in step S5 is -0.10 to -0.06 MPa, the temperature is 170 to 200° C., and the time is 20 to 40 minutes.

10. A modified silicone oil for high temperature resistant lubricating oil, characterized in that: Prepared according to the preparation method described in any one of claims 1 to 9.