Method for synthesizing fluorine halogenated ether

A synthesis method and technology of fluorohalogenated ethers, which are applied in the field of synthesis of fluorohalogenated ethers, can solve the problems of long reaction time, difficult storage, harsh reaction conditions, etc., and achieve stable product quality, short process flow and low reaction pressure Effect

Active Publication Date: 2012-10-03
JUHUA GRP
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The disadvantage is that the reaction principle perfluoropolyether diacyl fluoride is difficult to obtain and expensive; the reaction needs to be carried out at a very low temperature, the reaction time is long, and the reaction conditions are harsh; the product selectivity is low
The disadvantage is that the reaction raw material sulfuryl fluoride (SO2F2) has a boiling poin

Method used

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  • Method for synthesizing fluorine halogenated ether

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Embodiment 1

[0031] Add 800g of ethylene glycol, 600g of sulfolane, and 40g of potassium hydroxide into a 2L stainless steel autoclave with mechanical stirring. After the raw materials are added, close the feeding port and replace the gas in the kettle with high-purity nitrogen. When the oxygen content in the kettle is less than 50ppm, start stirring, and feed tetrafluoroethylene through the gas mass flow meter until the pressure in the kettle reaches 0.8MPa. Raise the temperature to 60°C to start the reaction, continuously feed tetrafluoroethylene during the reaction, keep the reaction pressure at 0.8-0.9MPa, and control the reaction temperature at 60-65°C. After feeding 400g of tetrafluoroethylene, stop passing through tetrafluoroethylene, cool, discharge, and rectify to obtain 492g of 2-(1,1,2,2-tetrafluoroethoxy)ethanol, 2-(1,1,2, The purity of 2-tetrafluoroethoxy)ethanol is 99.6%. Yield 75.0%.

[0032] In a 500ml four-neck flask with mechanical stirring and a reflux condenser, add 2...

Embodiment 2

[0034] Add 800g of ethylene glycol, 400g of N,N-methylformamide, and 80g of sodium hydroxide into a 2L stainless steel autoclave with mechanical stirring. After the oxygen content in the kettle is less than 50ppm, start stirring, and feed tetrafluoroethylene through the gas mass flowmeter until the pressure in the kettle reaches 0.5MPa, then raise the temperature to 10°C to start the reaction, and continuously feed tetrafluoroethylene during the reaction process to make the reaction The pressure is kept at 0.5-0.6 MPa, and the reaction temperature is controlled at 10-20°C. After feeding 200g of tetrafluoroethylene, stop passing through tetrafluoroethylene. Cool, discharge, and rectify to obtain 259g of 2-(1,1,2,2-tetrafluoroethoxy)ethanol with a purity of 99.2% and a yield of 79.9%.

[0035]In a 500ml four-neck flask with mechanical stirring and a reflux condenser, add 250g of 2-(1,1,2,2-tetrafluoroethoxy)ethanol prepared by the above method, stir, and cool the flask with an ...

Embodiment 3

[0037] Add 400g ethylene glycol, 1200g sulfolane, and 80g potassium hydroxide to a 2L stainless steel autoclave with mechanical stirring. After the raw materials are added, close the feeding port and replace the gas in the kettle with high-purity nitrogen. When the oxygen content in the kettle is less than 50ppm, start stirring, and feed tetrafluoroethylene through the gas mass flow meter until the pressure in the kettle reaches 1.0MPa. Raise the temperature to 90°C to start the reaction, continuously feed tetrafluoroethylene during the reaction, keep the reaction pressure at 1.0-1.1MPa, and control the reaction temperature at 90-95°C. After feeding 100g of tetrafluoroethylene, stop passing through tetrafluoroethylene, cool, discharge, and rectify to obtain 129g of 2-(1,1,2,2-tetrafluoroethoxy)ethanol, with a purity of 99.5% and a yield of 79.6% .

[0038] In a 500ml four-necked flask with mechanical stirring and a reflux condenser, add 125g of 2-(1,1,2,2-tetrafluoroethoxy)et...

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Abstract

The invention discloses a method for synthesizing fluorine halogenated ether. The method comprises the following steps of: 1) adding ethylene glycol, solvent and catalyst into a reaction kettle, introducing tetrafluoroethylene with stirring and starting to react, wherein the mass ratio of tetrafluoroethylene to ethylene glycol is 1:(2-8), the mass ratio of the solvent to the ethylene glycol is (0.25-4.5):1, the mass ratio of the catalyst to the ethylene glycol is 1:(5-27), controlling reaction temperature to be 10 to 125 DEG C and reaction pressure to be 0.1 to 1.5MPa, stopping introducing tetrafluoroethylene, then cooling, discharging, and rectifying to obtain 2-(1,1,2,2-tetrafluoroethoxy) ethanol; and 2) reacting the 2-(1,1,2,2-tetrafluoroethoxy) ethanol which is obtained in the step 1) and a halogenating agent in a mass ratio of 1:(0.5-2) at the temperature of between 50 and 100 DEG C for 1 to 5 hours, cooling a reaction solution, washing, layering, and rectifying to obtain a product. The method is mild in reaction condition, low in cost, and in yield; and the product is high in quality.

Description

technical field [0001] The invention relates to a method for synthesizing fluorohalogenated ethers. Background technique [0002] Fluorohalogenated ethers, especially fluorohalogenated ethers whose end groups are substituted by halogen atoms, not only have the active groups of the end groups, but also have the advantages of low surface tension and high stability of fluorine-containing chemicals, and play an important role in organic synthesis. The important role is an important medicine, pesticide intermediate and substitute Freon compound. Because fluorohalogenated ethers whose end groups are substituted by halogen atoms are widely used in organic chemical and pharmaceutical synthesis, a lot of research has been done on their synthesis at home and abroad, but there are few literature reports. The synthesis method is as follows: [0003] For example, Chinese Patent Publication No. CN1660740A, date of publication August 31, 2005, title of invention: method for preparing fluo...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/01
Inventor 叶立峰张万宏王树华周强姜永清应赢理余燕
Owner JUHUA GRP
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