Preparation method of hydrofluoroether

A technology of hydrofluoroethers and fluorine-containing alkanols, which is applied in the field of preparation of hydrofluoroethers, can solve the problems of harsh reaction conditions and difficult availability of raw materials, and achieve easy recycling and reuse, suppress the generation of double bond impurities, and reduce costs Effect

Inactive Publication Date: 2014-04-23
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] People have also done some research on controlling the reaction to control the formation of double bond by-products, but each has its own shortcomings, such as harsh reaction conditions and unavailable raw materials.

Method used

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  • Preparation method of hydrofluoroether

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Step A

[0028] Evacuate the 10L high-pressure reactor, replace with nitrogen for 3 times, dissolve potassium hydroxide in trifluoroethanol, add it into the reactor after it is completely dissolved, then add dichloromethane, stir, keep at a certain temperature, and introduce hexafluoropropylene under vacuum , keeping the pressure inside the kettle constant.

[0029] Step B

[0030] When the added amount of hexafluoropropylene was 1 time of the molar number of trifluoroethanol added, stop inputting hexafluoropropylene. When the pressure in the reactor drops to negative pressure, add pure water, continue to stir for 0.5 hours, stop stirring, vent and discharge.

[0031] Step C

[0032] Divided into two layers, the upper layer is water, dichloromethane, potassium hydroxide and unreacted trifluoroethanol are dissolved in the water, and the lower organic layer is separated. The purity of the target product hydrofluoroether in the organic layer was 86%, and the proportion...

Embodiment 2

[0036] Steps A to D were implemented as in Example 1, except that dichloromethane was changed to DMF in step A, and the results are listed in Table 1.

Embodiment 3

[0038] Steps A to D were carried out as in Example 1, except that dichloromethane was changed to DMSO in step A. The results are listed in Table 1.

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Abstract

The invention relates to a preparation method of hydrofluoroether. The preparation method comprises the following steps: (1), dissolving an alkali compound in fluorine-containing alkanol, adding a solvent, adding fluorinated olefin, and heating and stirring for reaction to obtain a mixed solution; (2), washing the mixed solution obtained in the step (1) by using water, standing for demixing, collecting an organic phase solution of a lower layer, and rectifying to obtain a hydrofluoroether product. According to the preparation method, the generation of double-bond impurities can be inhibited, and a reaction product from which a target product is easily purified can be obtained; the reaction temperature and the reaction pressure are relatively mild, the safety coefficient is high, and more satisfactory reaction speed can be obtained; the solvent is easily recycled, the cost is lowered, and a plurality of wastes are prevented from polluting the environment.

Description

technical field [0001] The invention relates to a preparation method of hydrofluoroether. Background technique [0002] In recent years, hydrofluoroethers have attracted more and more attention as a substitute for chlorofluorocarbons, which have the advantages of short atmospheric life, no damage to the ozone layer and low greenhouse effect. [0003] There are many methods for preparing hydrofluoroethers, including many preparation processes involving solvents. In the presence of solvents and basic compounds such as alkali metal hydroxides, hydrofluoroethers are prepared by reacting fluorine-containing alkanols with fluorinated olefins. However, in these preparation methods, the target product hydrofluoroether will undergo dehydrohalogenation reaction, thereby generating double bond by-products, accounting for about 0.1% to 10% of the total product. The problem is that this type of by-product has a boiling point close to the target product, so it is difficult to separate by...

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 王军马慧荣王汉利
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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