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Method for preparing 1,1,2,2-tetrachlorofluoroethyl-2,2,3,3-tetrachlorofluoropropyl ether

A technology of tetrafluoropropyl ether and tetrafluoroethyl is applied in the field of preparation of hydrofluoroether to achieve the effects of high purity, high product yield and avoidance of separation

Inactive Publication Date: 2014-08-20
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

[0006] In order to solve the problems of complex post-treatment, low conversion rate and low yield in the synthesis of the above hydrofluoroether compounds, the present invention provides a simpler and more economical Method for preparing 1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether (HFE-458) with high cost, high yield and simple post-treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Vacuum the 10L autoclave, replace it with monomer once, and then evacuate to -0.1MPa, add 2Kg tetrafluoropropanol, 4Kg sodium tetrafluoropropoxide solution (sodium tetrafluoropropoxide mass fraction is 25%), and then add When the monomer reaches 0.4MPa, stir and raise the temperature to about 85°C, start to add the monomer in batches until the pressure of the storage tank is 0.75MPa, and control the temperature of the kettle at about 85°C. When the pressure in the kettle dropped to 0.5MPa, add monomer to the tank pressure again, and continue for 2 hours, then start to add monomer continuously, continue to react for 5 hours, cool down, discharge, weigh, and add a total of 3.75Kg of monomer. Put the released material into the rectification kettle for rectification, and collect the material with a top temperature of 93-94°C as the HFE-458 product. The product purity is 98.5%, and the product yield is 80.5%.

Embodiment 2

[0030] Vacuum the 10L autoclave, replace it with monomer once, and then evacuate to -0.1MPa, add 2Kg tetrafluoropropanol, 4Kg sodium tetrafluoropropoxide solution (sodium tetrafluoropropoxide mass fraction is 25%), and then add When the monomer reaches 0.4MPa, stir and raise the temperature to about 70°C, start to add the monomer in batches until the pressure of the storage tank is 0.75MPa, and control the temperature of the kettle at about 70°C. When the pressure in the kettle drops to 0.5MPa, add monomer to the tank pressure again, and continue for 2 hours, then start to continuously add monomer, continue to react for 5 hours, cool down, discharge, weigh, and add a total of 3.6Kg of monomer. Put the released material into the rectification kettle for rectification, and collect the material with a top temperature of 93-94°C as the HFE-458 product. The product purity is 98.1%, and the product yield is 78%.

Embodiment 3

[0032] Vacuum the 10L autoclave, replace it with monomer once, and then evacuate to -0.1MPa, add 2Kg tetrafluoropropanol, 4Kg sodium tetrafluoropropoxide solution (sodium tetrafluoropropoxide mass fraction is 25%), and then add When the monomer reaches 0.4MPa, stir and raise the temperature to about 85°C, start to add the monomer in batches until the pressure of the storage tank is 0.75MPa, and control the temperature of the kettle at about 85°C. When the pressure in the kettle dropped to 0.5MPa, add monomer to the tank pressure again, and continue for 2 hours, then start to add monomer continuously, continue to react for 9 hours, cool down, discharge, weigh, and add 3.8Kg of monomer in total. Put the released material into the rectification kettle for rectification, and collect the material with a top temperature of 93-94°C as the HFE-458 product. The product purity is 98.5%, and the product yield is 80.4%.

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PUM

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Abstract

The invention relates to a preparation method of hydrofluoride ether, and particularly relates to a method for preparing 1,1,2,2-tetrachlorofluoroethyl-2,2,3,3-tetrachlorofluoropropyl ether. The method comprises the following steps: with tetrachlorofluoropropyl alcohol as an initial raw material and sodium tetrachlorofluoro-propoxide as a catalyst, reacting with a tetrafluoroethylene monomer, and carrying out after treatment on reaction products to obtain the 1,1,2,2-tetrachlorofluoroethyl-2,2,3,3-tetrachlorofluoropropyl ether. The catalyst used by the method is a tetrachlorofluoropropyl alcohol solution containing the sodium tetrachlorofluoro-propoxide, while the tetrachlorofluoropropyl alcohol is also one of the reaction raw materials, so any other solvents need not to be added so as to avoid separation of the solvent and the reaction products, reduce the after treatment steps and lower the production cost; by using the sodium tetrachlorofluoro-propoxide as the catalyst, the product yield is high and the purity is high.

Description

technical field [0001] The present invention relates to a method for preparing hydrofluoroether, in particular to a method for preparing 1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether (HFE-458 )Methods. 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] Hydrofluoroether is a new substitute for CFCs, with zero ODP, low GWP, and short atmospheric residence time, and is considered to be one of the ideal substitutes for CFCs. [0004] The synthesis methods of hydrofluoroethers (HFEs) are divided into two categories. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/06
CPCC07C41/06C07C43/123
Inventor 何日兴张立亭吕伟平吴军
Owner 山东中氟化工科技有限公司
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