Method for synthesizing hydrofluoroether by gas phase method

A technology of hydrofluoroether and gas phase method is applied in the field of synthesis of hydrofluoroether, which can solve the problems of difficult product quality assurance, serious environmental pollution and high preparation cost, and achieves the effects of low equipment requirements, production cost reduction and reaction cost reduction.

Active Publication Date: 2021-01-22
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a large amount of organic solvents are used in the production process, which will cause great environmental pollution.
CN107353184A uses gas-phase catalyzed product 1,1,2-trifluoroethylene and methanol as precursors, acetonitrile etc. as solvents to generate 1,1,2-trifluoroethyl methyl ether under a certain pressure of alkali catalysis, although avoiding Separation of trifluoroethylene, but with a lot of alkali solvent pollution
[0006] Therefore, the above-mentioned process for preparing hydrofluoroether has problems such as serious environmental pollution, high preparation cost, and difficulty in guaranteeing product quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 The synthetic method of 1,1,2,2-tetrafluoroethyl methyl ether

[0021] In a fixed bed reactor with GC-MS on-line detection system, first charge 2g MgF 2 Catalyst, then feed 10ml / min of N 2 Raise the temperature to 150°C for activation, after the temperature rises to 150°C, turn off the N 2 , after the activation is completed, the mixed gas of methanol and tetrafluoroethylene is introduced, wherein the flow rate of methanol is 0.1mol / h, the flow rate of tetrafluoroethylene is 0.1mol / h, and the molar ratio of methanol to tetrafluoroethylene is 1:1 , the reaction pressure is normal pressure, and after 20 hours of reaction, the conversion rate of tetrafluoroethylene is 50% and the selectivity of 1,1,2,2-tetrafluoroethyl methyl ether is 100% after online detection by GC-MS.

Embodiment 2

[0022] Example 2 The synthetic method of 1,1,2,3,3,3-hexafluoropropyl methyl ether

[0023] In a fixed bed reactor with an online detection system of GC-MS, first charge 5g BaF 2 Catalyst, then feed 10ml / min of N 2 Raise the temperature to 200°C for activation, after the temperature rises to 200°C, turn off the N 2 . The mixed gas of methanol and hexafluoropropylene is fed, the flow rate of methanol is 2mol / h, the flow rate of hexafluoropropylene is 0.5mol / h, the molar ratio of methanol to hexafluoropropylene is 4:1, and the reaction pressure is normal pressure . After reacting for 25 hours, the conversion rate of hexafluoropropylene was 45% and the selectivity of 1,1,2,3,3,3-hexafluoropropyl methyl ether was 100% after online detection by GC-MS.

Embodiment 3

[0024] Example 3 The synthetic method of 2-trifluoromethyl-1,1,3,3,3-pentafluoropropyl methyl ether

[0025] In a fixed-bed reactor with an online detection system of GC-MS, first load 10g of MgO catalyst, and then feed 10ml / min of N 2 Raise the temperature to 250°C for activation, after the temperature rises to 250°C, turn off the N 2 . The mixed gas of methanol and perfluoroisobutylene is introduced, wherein the flow rate of methanol is 6mol / h, the flow rate of perfluoroisobutylene is 1mol / h, the molar ratio of methanol to perfluoroisobutylene is 6:1, and the reaction pressure is normal pressure. After 30 hours of reaction, the conversion rate of perfluoroisobutene was 60% and the selectivity of 2-trifluoromethyl-1,1,3,3,3-pentafluoropropyl methyl ether was 100% after online detection by GC-MS %.

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Abstract

The invention discloses a method for synthesizing hydrofluoroether by a gas phase method, which comprises the following steps: putting a catalyst into a fixed bed reactor, heating to a specified temperature, introducing a mixed gas of methanol and fluorine-containing olefin in a molar ratio of 1-10: 1, controlling the reaction temperature to be 150-350 DEG C, the reaction pressure is normal pressure, the whole reaction process is monitored on line by GC-MS, and the product is cooled and rectified to obtain the corresponding hydrofluoroether product. According to the method for synthesizing theseries of hydrofluoroethers, a fixed bed reactor is adopted, use of strong base, organic solvents and the like is avoided, the method has good effect on reaction equipment, the cost is greatly reduced, and the method is simple in process, free of solvent pollution, mild in reaction condition, low in cost, good in product quality and very good in industrial application prospect.

Description

technical field [0001] The invention relates to a series of synthesis methods of hydrofluoroethers that can be used as cleaning agents for precision electronic devices, in particular to a method for synthesizing hydrofluoroethers by a gas phase method. Background technique [0002] As the problem of global warming worsens day by day, the protection of the ozone layer in the atmosphere is also increasingly strengthened by various countries. In order to improve the global environmental protection requirements, the traditional fluorine-containing cleaning agent HCFC has been banned. As an alternative product of HCFCs, hydrochlorofluorocarbons also have a high ozone depletion potential (ODP), global warming potential (GWP) and hydrochlorofluorocarbons have a long atmospheric residence time, so Hydrochlorofluorocarbons have been gradually restricted and phased out. [0003] As a new type of high-efficiency fluorine-containing product, hydrofluoroether has an ODP value of 0 and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/06C07C43/12
CPCC07C41/06C07C43/12
Inventor 韩文锋刘兵陈爱明陶杨龙梅
Owner 浙江诺亚氟化工有限公司
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