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Clean production method for hydrofluoroester

A clean production and hydrofluoroether technology, applied in the field of hydrofluoroether production, to achieve the effects of saving production costs, high reaction yield, and avoiding separation

Active Publication Date: 2014-09-17
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of complex post-treatment, low conversion rate and yield in the synthesis of the above hydrofluoroether compounds, and the need for a large amount of solvents to cause environmental pollution, the present invention Provides a method for preparing hydrofluoroether with clean production, cost saving, high yield and simple post-treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Add 4610g of trifluoroethanol into a 5L four-necked flask, protect it with nitrogen, and stir mechanically (rotating speed: 500r / min). Add the treated sodium metal into the flask, add sodium metal in 10 batches, and add 23g each time. Wait until the sodium metal has completely disappeared before adding the next batch. The reaction temperature is 60-70°C, and the sodium metal is consumed after 23 hours of reaction to obtain a sodium trifluoroethoxide solution. By detecting the concentration of the solution is about 25%;

[0029] (2) Vacuumize the 10L autoclave, replace it with monomer once, and then evacuate to -0.1MPa, add 2Kg trifluoroethanol, 4Kg sodium trifluoroethoxide solution, then add monomer to 0.4MPa, stir and heat up to 105°C Around this time, start adding tetrafluoroethylene in stages until the pressure of the storage tank is 0.90MPa, while controlling the temperature of the kettle at about 105°C. When the pressure in the kettle drops to 0.7MPa, add tet...

Embodiment 2

[0031] Vacuum the 10L autoclave, replace it once with tetrafluoroethylene, and then evacuate to -0.1MPa, add 2Kg trifluoroethanol, 3Kg sodium trifluoroethoxide solution with a concentration of 25%, then add tetrafluoroethylene to 0.4MPa, and stir Raise the temperature to about 105°C, and start adding tetrafluoroethylene in stages until the pressure of the storage tank is 0.90MPa, while controlling the temperature of the kettle at about 105°C. When the pressure in the kettle drops to 0.7MPa, add tetrafluoroethylene to the tank pressure again, and continue for 2 hours, then start to add tetrafluoroethylene continuously, continue to react for 5 hours, cool down, discharge, weigh, and add tetrafluoroethylene 3.6 Kg. Put the released material into the rectification kettle for rectification, and collect the material with a top temperature of 55-56°C as the hydrofluoroether product. The product purity is 99.6%, and the product yield is 78%.

Embodiment 3

[0033] Vacuum the 10L autoclave, replace it once with tetrafluoroethylene, and then evacuate to -0.1MPa, add 2Kg trifluoroethanol, 5.2Kg sodium trifluoroethoxide solution with a concentration of 25%, and then add tetrafluoroethylene to 0.4MPa, Stir and heat up to about 105°C, start adding tetrafluoroethylene in portions until the pressure of the storage tank is 0.90MPa, while controlling the temperature of the kettle at about 105°C. When the pressure in the kettle drops to 0.7MPa, add tetrafluoroethylene to the tank pressure again, and continue for 2 hours, then start to add tetrafluoroethylene continuously, continue to react for 5 hours, cool down, discharge, weigh, and add tetrafluoroethylene 5.15 Kg. Put the released material into the rectification kettle for rectification, and collect the material with a top temperature of 55-56°C as the hydrofluoroether product. The product purity is 99.4%, and the product yield is 80.2%.

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Abstract

The invention relates to the technical field of hydrofluoroester production and particularly relates to a clean production method for hydrofluoroester. The method is as follows: adding fluorine-containing sodium alkoxide catalyst into fluorine-containing alcohol liquor, adding fluorinated olefin, heating and stirring for reacting to obtain mixed liquor; carrying out after-treatment onto the mixed liquor to obtain hydrofluoroester, wherein the fluorine-containing sodium alkoxide catalyst is sodium trifluoroalkoxide, and the corresponding fluorine-containing alcohol is trifluoroalcohol or pentafluoroalcohol. The catalyst used by the method is fluorine-containing alkanol liquor of the fluorine-containing sodium alkoxide, and the fluorine-containing sodium alkoxide is one of reaction materials, so that any other solvent is not needed to be added, and therefore, separation of the solvent and reaction products is avoided, after-treatment steps are reduced, production cost is saved, reaction yield is high, product purity is high, and economic benefits are very high.

Description

technical field [0001] The invention relates to the technical field of hydrofluoroether production, in particular to a method for clean production of hydrofluoroether. Background technique [0002] Chlorofluorocarbons (CFCs) have excellent chemical stability and are widely used as refrigerants, blowing agents, propellants and industrial cleaning agents. However, CFCs are one of the main substances that destroy ozone, with high ozone depletion potential (ODP), long residence time in the atmosphere, and high greenhouse effect potential (GWP). Therefore, the development of alternatives to CFCs has become one of the very active fields in academia and industry. [0003] In recent years, hydrofluoroethers have attracted more and more attention as a substitute for chlorofluorocarbons. They have the advantages of short atmospheric residence time, no damage to the ozone layer and low greenhouse effect. [0004] At present, there are many methods for preparing hydrofluoroethers, a...

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 何日兴张立亭吕伟平
Owner 山东中氟化工科技有限公司
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