Method for preparing fluorine-containing ether

A technology of fluorine-containing ethers and trifluoromethyl methyl ethers, which is applied in the field of preparation of fluorine-containing ethers, and can solve problems such as easy decomposition, high toxicity, and difficulty in obtaining

Active Publication Date: 2019-07-12
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In the above-mentioned existing technology, the synthesis of trifluoromethyl methyl ether has the following defects: (1) the raw material trifluoronitrosomethane of the first route belongs to highly toxic and unstable gas, and it is easy to encounter light or strong alkali. Decomposition, and the total yield of synthetic trifluoromethyl methyl ether is too low; (3) the raw material trifluoromethyl hypochlorite of the third route is difficult to obtain, and the yield of trifluoromethyl methyl ether is low; (4) the raw material dimethyl sulfate of the fourth route Esters are highly toxic methylating reagents, potential carcinogens and mutagens, and the yield of trifluoromethyl methyl ether is low

Method used

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  • Method for preparing fluorine-containing ether
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  • Method for preparing fluorine-containing ether

Examples

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Embodiment 1

[0081] In a 1L autoclave, add 200 ml of acetonitrile, 0.5 mol of CsF, and 2 mol of carbonyl fluoride, react at 20 degrees for 24 hours, then separate the remaining carbonyl fluoride in the above reaction system at -40 degrees, and then add 0.01mol of water and 1mol of dimethyl carbonate were reacted at 20 degrees for 24 hours. After the reaction, distillation was carried out to obtain trifluoromethyl methyl ether (boiling point was -25.2°C / 760mmHg), with a yield of 92.8% and a purity of was 98.1%.

Embodiment 2

[0083] In a 1L autoclave, add 200 ml of propionitrile, 0.5 mol of RbF, and 2 mol of trifluoroacetyl fluoride, react at 20 degrees for 24 hours, and then separate the remaining trifluoroacetyl fluoride in the above reaction system at -40 degrees , then add 0.03mol of water and 1mol of dimethyl carbonate, react at 20 degrees for 36 hours, after the reaction ends, carry out distillation to obtain pentafluoroethyl methyl ether (boiling point is 6 ℃ / 760mmHg), and the yield is 90.3% , with a purity of 97.2%.

Embodiment 3

[0085] In a 1L autoclave, add 200 ml of butyronitrile, 0.5 mol of KF, and 2 mol of pentafluoropropionyl fluoride, react at 20 degrees for 24 hours, and then separate the remaining pentafluoropropionyl in the above reaction system at -20 degrees. Acyl fluoride, then add 0.05mol of water and 1mol of dimethyl carbonate, and react at 20 degrees for 36 hours. After the reaction is finished, distill to obtain heptafluoropropyl methyl ether (boiling point is 6°C / 760mmHg), and the yield is 83.7% with a purity of 98.4%.

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Abstract

The invention relates to a 'method for preparing fluorine-containing ether', and belongs to the field of chemical synthesis. The method comprises the steps that under a nitrile solvent condition, carbonyl fluoride, trifluoroacetyl fluoride, pentafluoropropionyl fluoride, heptafluoro-n-butyryl fluoride, heptafluoro-iso-butyryl fluoride and other acyl fluorides are taken as raw materials to have anaddition reaction with metal fluorides to obtain perfluoroalkoxide, then under water catalysis, the perfluoroalkoxide and a low-toxic or even non-toxic harmless alkylating agent are subjected to an alkylation reaction to obtain the fluorine-containing ether. The method for preparing the fluorine-containing ether has the advantages that not only is the reaction condition mild, the yield of the fluorine-containing ether is high, but also the low-toxic or even non-toxic harmless alkylating agent is taken as a safe alkylation agent, the process is safe and reliable, and effective separation can beperformed by an ordinary distillation means in the industry.

Description

technical field [0001] The present invention relates to a method for preparing fluorine-containing ethers, in particular to a kind of reaction between acid fluoride and metal fluoride to form perfluoroalkoxide, and then, under the catalysis of water, react perfluoroalkoxide with alkylating reagent to synthesize fluorine-containing ether. Fluorine method. Background technique [0002] Up to now, trifluoromethyl methyl ether (trifluoromethyl methyl ether) has the following four synthetic routes: [0003] The first is a synthetic route based on trifluoronitrosomethane. Documents "Dokl.Akad.Nauk SSSR, 1961, Volume 141, Issue 2,357–360" and "J.Gen.Chem.USSR (Engl.Transl.), 1968, vol.38, Issue4, 685-690" reported that in In methanol solvent, trifluoronitrosomethane reacts with hydroxylamine to obtain trifluoromethyl methyl ether with a yield of 35%. See reaction (1) for the equation. In addition, the document "J.Gen.Chem.USSR (Engl.Transl.), 1967, vol.37, 1026-1032" reported th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/12
CPCC07C41/16C07C29/68C07C43/12C07C43/123C07C31/40
Inventor 张呈平郭勤张文妮权恒道
Owner 泉州宇极新材料科技有限公司
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