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Mixed fluorinated cyclosiloxane, preparing method and use thereof

A technology of siloxane and mixed rings, applied in the direction of silicon organic compounds, etc., can solve the problems of poor stability and achieve the effect of excellent performance, good heat resistance and small molecular weight

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

AI Technical Summary

Problems solved by technology

[0004] The introduction of chlorophenyl into dimethyl silicone oil can significantly improve the lubricating performance of silicone oil, but the stability is poor

Method used

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  • Mixed fluorinated cyclosiloxane, preparing method and use thereof

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Experimental program
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Effect test

Embodiment 1

[0021] The three-neck reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and addition funnel. Add 0.35mol of calcium oxide and 150ml of ethyl acetate into the reaction flask and stir to form a suspension. Add dropwise 0.15mol of the pre-mixed solution under cooling in a water bath at 20°C. f 3 C(CF 2 ) Y (CH 2 ) x Si(CH 3 ) Cl 2 (X=2; Y=0) and 0.2mol dimethyldichlorosilane mixture; after adding the dichlorosilane mixture, continue to react for 1h; filter out the insoluble calcium salt, wash the filtrate with water 100ml×2 times, and then wash 100ml with distilled water × 2 times; dried with anhydrous sodium sulfate, filtered, distilled off ethyl acetate to obtain 28.5 g of fluorine-containing mixed cyclosiloxane, and the yield (based on the total amount of dichlorosilane) was 79.4%. product 19 F NMR (δ) - 70.57 ppm, 21.18% fluorine content.

Embodiment 2

[0023] The three-neck reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and addition funnel. Add 0.35mol of magnesium oxide and 150ml of ethyl acetate into the reaction flask and stir to form a suspension, and dropwise add 0.15mol of the pre-mixed solution under cooling in a water bath at 20°C. f 3 C(CF 2 ) Y (CH 2 ) x Si(CH 3 ) Cl 2 (X=2; Y=0) and 0.2mol dimethyldichlorosilane mixture; after adding the dichlorosilane mixture, continue to react for 1h; filter off the insoluble magnesium salt, wash the filtrate with water 100ml×2 times, and then wash 100ml with distilled water × 2 times; dried with anhydrous sodium sulfate, filtered, distilled off ethyl acetate to obtain 24.5 g of fluorine-containing mixed cyclosiloxane, and the yield (based on the total amount of dichlorosilane) was 68.8%. product 19 F NMR (CDCl 3 , δ): -70.59ppm, the fluorine content is 21.21%.

Embodiment 3

[0025] The three-neck reaction flask is equipped with electromagnetic stirring, reflux condenser, thermometer and addition funnel. Add 0.6mol of zinc oxide and 250ml of ethyl acetate into the reaction flask and stir to form a suspension, then add the pre-mixed 0.1mol dropwise under cooling in a water bath at 20°C. f 3 C(CF 2) Y (CH 2 ) x Si(CH 3 ) Cl 2 (X=2; Y=10) and 0.5mol ethylmethyldichlorosilane mixture; after adding the dichlorosilane mixture, continue to react for 2h; wash the reaction solution with water 150ml×2 times, then wash 150ml×2 times with distilled water; After drying with anhydrous sodium sulfate, filter, distill off ethyl acetate to obtain 82.2 g of fluorine-containing mixed cyclosiloxane, and the yield (based on the total amount of dichlorosilane) is 71.0%. The fluorine content of the product is 34.26%.

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Abstract

A mixed fluoric cyclosiloxane is prepared through mixing fluoric alkylmethyl dichlorosilane with dihydroxy dichlorosidane and reacting on metallic oxide or carbonate of alkali metal for dechlorination. It can be used to cynthesize fluoric polysiloxane for preparing F-Si lubricant, F-Si rubber, or hydroxy F-Si oil.

Description

technical field [0001] The invention relates to a fluorine-containing mixed cyclosiloxane, a preparation method and application thereof. The fluorine-containing mixed cyclosiloxane is directly prepared by dechlorinating the mixed raw materials of fluorine-containing alkylmethyl dichlorosilane and dihydrocarbyl dichlorosilane, metal oxide and alkali metal carbonate. The compound can be used for synthesizing fluorine-containing polysiloxane as fluorine silicon lubricating oil. 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 under some special conditions where mineral lubricating oil cannot meet the requirements of us...

Claims

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Application Information

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IPC IPC(8): C07F7/21C08G77/24C08G77/385
Inventor 唐松青李战雄刘金涛
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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