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Preparation method of hydrofluoroether

A hydrofluoroether and hydroxide technology, which is applied in the preparation of ether, the preparation of ether by the addition of unsaturated compounds, organic chemistry, etc., can solve the problems of difficult separation, recovery energy consumption, high cost, harsh reaction conditions, etc. Three wastes discharge, easy recycling, mild reaction conditions

Active Publication Date: 2013-08-21
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that strong polar substances such as DMF or DMSO are used as solvents, and alkali metal hydroxides are used as catalysts. However, when the difference between the boiling point of the product and the boiling point of the solvent is small, separation is difficult, and the boiling point of the solvent DMSO itself is very high. Recovering energy consumption, higher cost
No solvent or fluorine-containing catalyst is used in the reaction process, but the reaction conditions are relatively harsh, requiring higher temperature (110-180°C) and pressure (0.6-1.2MPa)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] Add 20.0g (0.5mol) of sodium hydroxide, 1.8g (0.005mol) of cetyltrimethylammonium bromide, 290g (5.0mol) of solvent acetone, and 660g (5.0mol) of tetrafluoropropanol in a 2L high-pressure reactor. ), after closing the kettle, use N 2 Replace the gas three times, heat to 60°C, add 500g of tetrafluoroethylene continuously, control the pressure at 0.25MPa and react for 1.5h, and rectify to obtain 1050g of a product with a purity of 99.2%, with a yield of 90.5%.

example 2

[0033] Add 11.2g (0.2mol) of potassium hydroxide, 3.1g (0.02mol) of tetramethylammonium bromide, 774g (9.0mol) of solvent MTHF, and 250g (2.5mol) of trifluoroethanol in a 2L autoclave, and use the N 2 The gas was replaced three times, heated to 60°C, 280g of tetrafluoroethylene was continuously added, and the pressure was controlled at 0.6MPa to react for 0.5h, and rectified to obtain 432g of a product with a purity of 99.5%, with a yield of 86.4%.

example 3

[0035] Add 8.0g (0.2mol) of sodium hydroxide, 5.45g (0.05mol) of tetramethylammonium chloride, 1185g (15.0mol) of solvent pyridine, and 115g (2.5mol) of ethanol in a 2L autoclave. The gas was replaced three times, heated to 20°C, 260g of tetrafluoroethylene was continuously added, and the pressure was controlled at 0.3MPa to react for 2.5h, and rectified to obtain 341g of a product with a purity of 99.8%, with a yield of 93.4%.

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PUM

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Abstract

The invention discloses a preparation method of hydrofluoroether. The preparation method comprises the following steps of: mixing a solvent, a catalyst, olefin and alcohol to have reaction, wherein the mole ratio of the solvent to the alcohol is (1-6):1, the mole ratio of the catalyst to the alcohol is (0.01-0.15):1, the mass ratio of the olefin to the alcohol is (0.5-5):1, the reaction temperature is 20-60 DEG C, the reaction pressure is 0.05-0.6MPa, and the reaction time is 0.5-3 hours; and rectifying after the reaction is accomplished, so as to obtain a hydrofluoroether product. The preparation method has the advantages that the reaction condition is gentle, the operation is simple, products are easy to separate, and less wastewater, waste gas and waste residue are discharged.

Description

technical field [0001] The invention relates to a preparation method of hydrofluoroether compounds, in particular to a method for preparing by reacting raw material alcohol and olefin in a low boiling point weak polar solvent under the catalytic action of a mixture of quaternary ammonium salt and alkali metal hydroxide as a catalyst Hydrofluoroether method. Background technique [0002] Hydrofluoroether (HFE) is a class of ether compounds containing fluorine, carbon, hydrogen, and oxygen elements. It does not destroy the ozone layer and has a small greenhouse effect. It is a new generation of ODS (ozone depleting substances) substitutes and can be used for refrigerants, hair Foaming agent, cleaning agent and heat conduction agent and other fields. [0003] The preparation method of existing hydrofluoroether comprises following several, (1) fluorine gas (F 2 ) or the fluorination of ether compounds by metal fluorine compounds. (2) Electrochemical fluorination of ether comp...

Claims

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Application Information

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IPC IPC(8): C07C41/06C07C43/12
Inventor 兰喜平周强胡正耿为利王树华
Owner JUHUA GROUP TECH CENT
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