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Fluorinated silicone lube oil synthetic method

A synthesis method and technology of lubricating oil, applied in lubricating compositions, petroleum industry, additives, etc., can solve the problems affecting product quality control and production process, affecting the storage stability of silicone oil products, affecting the catalytic efficiency of catalysts, etc., and achieve excellent comprehensive The effect of performance, short response time and simple post-processing

Inactive Publication Date: 2003-11-19
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages. First, the terminal hydroxyl groups in the co-hydrolyzed product generate a large amount of water in the polycondensation reaction, which affects the catalytic efficiency of the catalyst; secondly, the HCl generated during the hydrolysis process will break some Si-C bonds and form trifunctional The components of fluorosilicone oil products synthesized by hydrolysis polycondensation method are relatively dispersed, and the existence of residual hydroxyl groups affects the storage stability of silicone oil products, so it is advisable to use fluorine-containing ring Siloxane ring-opening polymerization preparation
In addition, a large amount of strongly acidic wastewater is produced in the production of co-hydrolysis, which needs to be neutralized
[0008] When the traditional co-hydrolysis method produces polysiloxane, the existence of hydroxyl groups affects the quality control and production process of the product. The production of polysiloxane by ring-opening polymerization of cyclosiloxane can overcome the above shortcomings, but some cyclosiloxanes It is not easy to obtain, and the preparation of mixed cyclosiloxane by dechlorination of metal oxide and then ring-opening polymerization to produce polysiloxane overcomes the shortcomings of the first two methods at the same time

Method used

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  • Fluorinated silicone lube oil synthetic method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The three-necked reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and water bath, and the fluorine-containing mixed cyclosiloxane (R 1 , R 2 Methyl, X=2, Y=6) 16g, end-capping agent divinyltetramethyldisiloxane 2.4g (15% of mixed cyclosiloxane weight) and 95% sulfuric acid 1.92g were added to the reaction flask in sequence After stirring for 30 minutes, the temperature was raised to 30°C; after 40 hours of reaction, it was cooled to room temperature, 20ml of n-hexane was added, washed with water until neutral, and then the solvent and low fraction were evaporated to obtain 13.5g of fluorine-containing polysiloxane with a yield of 73.5% . The product is a colorless transparent liquid with a viscosity (-40°C) of 1536.6mm 2 / s, the fluorine content is 44.3%.

Embodiment 2

[0031] The three-necked reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and water bath, and the fluorine-containing mixed cyclosiloxane (R 1 is methyl, R 2 Ethyl, X=2, Y=0) 16g, end-capping agent divinyltetramethyldisiloxane 3.2g (20% of the weight of the mixed cyclosiloxane) and 0.8g perchloric acid were added to the reaction flask in sequence After stirring for 30 minutes, the temperature was raised to 30°C; after 30 hours of reaction, it was cooled to room temperature, 20ml of n-hexane was added, washed with water until neutral, and then the solvent and low fraction were evaporated to obtain 15.6g of fluorine-containing polysiloxane with a yield of 80.9% . Product viscosity (-40°C) is 605.9mm 2 / s, the fluorine content is 20.7%.

Embodiment 3

[0033] The three-necked reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and water bath, and the fluorine-containing mixed cyclosiloxane (R 1 , R 2 is methyl, X=2, Y=10) 20g, end-capping agent divinyltetramethyldisiloxane 3g and 0.8g95%H 2 SO 4 Add it to the reaction flask in turn, stir for 30 minutes and then heat up to 30°C; react for 30 hours and cool to room temperature, add 20ml of n-hexane, wash with water until neutral, then distill off the solvent and low fractions to obtain 17g of fluorine-containing polysiloxane solid. The rate is 73.5%. The fluorine content of the product was 56.6%.

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Abstract

A F-Si lubricating oil is prepared from the mixture of fluoric alkylmethyl dichlorosilane and dihydroxy dichlorosilane through dechlorimating by metallic oxide, synthesizing multiple elements mixed fluoric cyclosilane, and opening-loop polymerizing under trigger of strong acid. Its advantage is high performance.

Description

technical field [0001] The invention relates to a new method for synthesizing fluorine-silicon lubricating oil from fluorine-containing alkylmethyldichlorosilane, which is to prepare fluorine-containing lubricating oil from a mixture of fluorine-containing alkylmethyldichlorosilane and dihydrocarbyl dichlorosilane through metal oxide dechlorination Mixed rings, followed by ring-opening polymerization catalyzed by strong acid, controlled molecular weight and molecular weight distribution to obtain fluorosilicone lubricating oil with excellent comprehensive performance. Background technique [0002] Synthetic lubricating oil is the preparation of lubricating oil through chemical synthesis. Its research and development started from the Second World War. At that time, France and Japan, which lacked oil resources, developed such products at any cost for the urgent needs of the war. It is much higher than the mineral oil used in large quantities, so it is currently limited to use ...

Claims

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Application Information

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IPC IPC(8): C10M155/02
Inventor 唐松青李战雄刘金涛钱国兴
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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