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Method for preparing 2,2,2-trifluoroethyl methacrylate

A technology of methacrylic acid and trifluoroethyl ester, applied in the chemical field, can solve the problems of difficult storage and transportation of raw materials, harsh reaction system requirements, expensive raw materials, etc., and achieves the effects of high yield, low price and good purity

Inactive Publication Date: 2008-04-30
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Purpose of the invention: To provide a method for preparing 2,2,2-trifluoroethyl methacrylate, to overcome the high price of raw materials in the prior art, the difficulty of storage and transportation of raw materials; the harsh requirements of the reaction system, and the corrosion of equipment, etc. insufficient

Method used

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  • Method for preparing 2,2,2-trifluoroethyl methacrylate

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 120g (1mol) of thionyl chloride and 0.8g of phenothiazine into a reactor equipped with a heater, a stirrer, a thermometer, and a reflux condenser, and slowly add methacrylic acid and DMF dropwise under stirring at 20-25°C. The mixed solution (prepared by mixing 93g of 1.1mol methacrylic acid and 1ml of DMF) was heated to 50±2°C and kept for 2 hours for reaction. Then slowly drop the mixed solution of 2,2,2-trifluoroethanol and 4-dimethylaminopyridine (DMAP) (90g 0.9mol 2,2,2-trifluoroethanol is mixed with 0.4g DMAP), control After reacting at 60±5°C for 4 hours, cool the reaction liquid to room temperature, and add 20wt% NaOH solution for neutralization, adjust the pH of the reaction liquid to 7, separate the organic layer, wash with saturated brine, add anhydrous MgSO 4 Dry, then distill under reduced pressure, collect the cut of 45-47 ℃ / 140mmHg, obtain 143.8g colorless transparent liquid product, be the product -2,2,2-trifluoroethyl methacrylate, the productive ra...

Embodiment 2

[0025] Add 120g (1mol) of thionyl chloride and 1g of hydroquinone into a reactor equipped with a heater, stirrer, thermometer, and reflux condenser, and add a mixture of methacrylic acid and DMF dropwise under stirring at 20-25°C solution (prepared by mixing 84.5g of 1.0mol methacrylic acid and 1ml of DMF), heated to 50±2°C and incubated for 3 hours. Then slowly drop the mixture of 2,2,2-trifluoroethanol and DMAP (80g 0.8mol2,2,2-trifluoroethanol mixed with 0.5g DMAP), and control the temperature at 60±5°C for 4.5 hours Afterwards, the reaction solution was cooled to room temperature, neutralized by adding 20wt% NaOH solution, and the pH of the reaction solution was adjusted to 7, and the organic layer was separated, washed with saturated brine, and added with anhydrous MgSO 4 Dry, then distill under reduced pressure, collect the cut of 45-47 ℃ / 140mm Hg, obtain 143.5g colorless transparent liquid product, be product methacrylic acid-2,2,2-trifluoroethyl ester, productive rate ...

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Abstract

The invention discloses a method for preparing methylacrylic acid-2, 2, 2-ethyl trifluoroacetate. The method adopts methylacrylic acid as the raw material, and the methylacrylic acid is reacted with thionyl chloride under the existence of DMF and polymerization retarder; the obtained methacrylic chloride is reacted with 2, 2, 2-ethyl trifluoroacetate under the existence of catalytic agent, then the target product of the invention-methylacrylic acid-2, 2, 2-ethyl trifluoroacetate-can be collected from the reaction product, the purity rate reaches more than 98 percent (GC), and the production rate is more than 95 percent. The reaction process condition of the invention is bland, the operation is secure and simple, the raw material sources are extensive, and the price is low; compared with the prior technology, the invention overcomes the deficiencies that the raw material price is expensive, the preservation and the transportation of the raw material are difficult, the reaction system request is harsh, the equipment corrosiveness is strong, the product quality is steady, the purity rate is good, the production rate is high, and the invention is suitable for large-scale industrialization production.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing 2,2,2-trifluoroethyl methacrylate. Background technique [0002] 2,2,2-trifluoroethyl methacrylate, the English name is 2,2,2-Trifluoro Ethylmethacry-late, referred to as TFEMA, is a kind of CF 3 The methacrylate-based monomer, as an important organic fluorine-containing polymer monomer, is mainly used in different types of coating formulations. The general-purpose monomer and the monomer with high fluorine content have excellent compatibility and can be applied In copolymerization system, adjustment of fluorine content and modification of resin functionalization, the polymer has a higher degree of hydrophobicity and lower refractive index than other acrylate polymers. Its structural formula is as follows: [0003] [0004] At present, the patent report-2,2,2-trifluoroethyl methacrylic acid preparation method mainly contains the following several kinds...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08
Inventor 何扣宝廖本仁
Owner SHANGHAI CHEM REAGENT RES INST
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