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Method for preparation of fluorinated acrylic ester from fluorinated alcohol

A technology for fluorinating acrylates and acrylates, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems such as the need to improve the process, and achieve convenient industrial production, low reaction temperature, and product manufacturing. Simple way to effect

Active Publication Date: 2020-07-10
安徽灵达高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the residual rate of fluoroalcohol is 4.5-7%, the conversion rate is 88.7-91.9%, the yield is 86.5-89.4%, and secondary distillation is required, so the process still needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. In a 100ml four-necked bottle, add 20 grams of dodecafluoroheptanol, 20 grams of dichloromethane, and 6 grams of triethylamine, and stir well. A mixture of 2.5 g of titanium tetrachloride and 2.5 g of dichloromethane was slowly added dropwise at 5-15° C., and the temperature was raised to 25° C. and continued stirring for 4 hours. Filtration removes solid, and filtrate rotary evaporation removes dichloromethane etc., obtains 23 grams of light yellow transparent liquid catalysts [HC 6 f 12 CH 2 O] 4 Ti.

[0033] 2. In a 5-liter four-port reactor equipped with a heater, a thermometer, an agitator, a 1.2-meter packed tower, and a rectification separator, add a fluorinated alcohol—dodecafluoroheptanol (HC 6 f 12 CH 2 OH) 3000 grams, 500 grams of toluene, 2100 grams of methyl acrylate, 8 grams of hydroquinone and 9 grams of fluorine-containing catalyst obtained in step 1, start stirring and heat up to 80 ° C, reduce the heating rate, and pass through the rectifier ...

Embodiment 2

[0036] 1, by the method for embodiment 1, replace dodecafluoroheptanol with 22 grams of perfluorohexyl alcohols, make similar catalyst [C 6 f 13 CH 2 CH 2 O] 4 Ti.

[0037] 2, in the reactor with embodiment 1, add fluorinated alcohol-perfluorohexyl alcohol (C 6 f 13 CH 2 CH 2 OH) 3000 grams, 500 grams of toluene, 1900 grams of methyl acrylate, 7 grams of hydroquinone and 8 grams of fluorine-containing catalyst obtained in step 1, start stirring and heat up to 80 ° C, reduce the heating rate, and pass through the rectifier Gradually separate the azeotrope between toluene acrylate and methanol, continue the separation for 3.5 hours, no more methanol is produced, the content of fluorinated alcohol is 1.0% and the target product content is 98.1% after detection of methyl acrylate and toluene.

[0038] 3. Adjust the heating range to rectify excess methyl acrylate and toluene; control the temperature of the kettle to not exceed 135°C by adjusting the vacuum degree, and recti...

Embodiment 3

[0040] By the method for embodiment 1, replace dodecafluoroheptanol with 23 grams of perfluorohexyl propanols, make similar catalyst [C 6 f 13 CH 2 CH 2 CH 2 O] 4 Ti.

[0041] In the reactor with embodiment 2, add fluorinated alcohol-perfluorohexyl propanol (C 6 f 13 CH 2 CH 2 CH 2 OH) 3000 grams, 500 grams of toluene, 1850 grams of methyl acrylate, 7 grams of hydroquinone and 10 grams of the above-mentioned fluorine-containing catalyst; %, yield 97.6%.

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PUM

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Abstract

The invention discloses a method for preparation of fluorinated acrylic ester from fluorinated alcohol. The method includes: in a reaction kettle provided with a packed tower and a rectification separator, reacting fluorinated alcohol with acrylic ester in the presence of a self-made fluorine-containing catalyst, a solvent and an assistant, performing step-by-step rectification in the reaction process to remove generated methanol, excessive acrylic ester and the solvent, and then conducting rectification to obtain a high-purity target product. According to the method, the used self-made fluorine-containing catalyst has good compatibility with the reaction system, the reaction temperature is low, the reaction speed is high, and few impurities are generated; the product manufacturing mode issimpler, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of preparation of new fluorine-containing materials, in particular to a method for preparing fluorinated acrylates from fluorinated alcohols. Background technique [0002] Fluorinated acrylate is an important fluorine-containing chemical. Its polymer has excellent oil and water repellency. It is an important intermediate in the production of surface protective agents and is widely used in the fields of textiles, coatings and fluorine-containing surfactants. It is the key intermediate for the production of "three-defense" fabric finishing agent. [0003] At present, the manufacturing methods of fluorine-containing acrylate introduced by domestic and foreign patents mainly include: [0004] One is based on perfluoroalkyl ethyl iodide base material. Such as: CN102531889A introduces perfluoroalkyl ethyl iodide (C 2 f 5 (CF 2 CF 2 ) n CH 2 CH 2 I, n is an integer greater than 0) and alkali metal and / or a...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/653B01J31/02
CPCC07C67/08B01J31/0212B01J2231/49C07C69/653
Inventor 张立亭张秀芳蒋韶贤李文强徐宪龙
Owner 安徽灵达高新材料有限公司
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