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Preparation method of 1, 1, 2, 2,-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether

A technology of trifluoroethyl ether and tetrafluoroethyl, applied in 1 field, can solve the problems of difficult separation of product and catalyst, difficult catalyst recovery, and high slag content, and achieves easy separation, comprehensive alkalinity enhancement, and good catalyst activity. Effect

Inactive Publication Date: 2015-11-18
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The catalysts used in the above patents and literature technologies are mainly alkali metal compounds, which have disadvantages such as difficulty in catalyst recovery, high slag content, and difficulty in separating the product from the catalyst due to fine solid particles. At the same time, it is easy to cause environmental pollution due to the use of a large amount of solvents.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of 1,1,2,2,-tetrafluoroethyl-2,2,2-trifluoroethyl ether, comprising the following steps:

[0025] Step 1: in 500L reactor, add D201 strongly basic anion exchange resin 100Kg, 300Kg water, the N-hydroxyethyl perfluorooctane sulfonamide of 0.3Kg, the 1 of 10Kg, 8-diazabicyclo (5,4 , 0) Undec-7-ene (DBU), 0.2Kg of disodium ethylenediaminetetraacetic acid (EDTA), stirred and reacted at 60°C for 15h to prepare a composite catalyst for future use.

[0026] Step 2: In a 1000L stainless steel autoclave, add 100Kg trifluoroethanol at one time, the composite catalyst obtained in the above step (1) of 70Kg, close the feeding port, replace the air in the still with nitrogen, and then feed tetrafluoroethylene monomer , the temperature rises to start the reaction, the reaction temperature is controlled at 60°C, the tetrafluoroethylene is metered into the reactor, and the reaction is completed when 400Kg of tetrafluoroethylene monomer is passed through, the compos...

Embodiment 2

[0028] A preparation method of 1,1,2,2,-tetrafluoroethyl-2,2,2-trifluoroethyl ether, comprising the following steps:

[0029] Step 1: add D201 strongly basic anion exchange resin 100Kg in 500L reactor, the N-hydroxyethyl perfluorooctane sulfonamide of 200Kg water, 0.1Kg, the 1 of 5Kg, 8-diazabicyclo (5,4 , 0) Undec-7-ene (DBU), 0.05Kg of disodium ethylenediaminetetraacetic acid (EDTA), stirred and reacted at 40°C for 20h to prepare a composite catalyst for future use.

[0030] Step 2: In a 1000L stainless steel autoclave, add 100Kg trifluoroethanol at one time, the composite catalyst obtained in the above step (1) of 30Kg, close the feeding port, replace the air in the still with nitrogen, and then feed tetrafluoroethylene monomer , the temperature rises to start the reaction, the reaction temperature is controlled at 40°C, the tetrafluoroethylene is metered into the reactor, and the reaction is completed when 300Kg of tetrafluoroethylene monomer is passed through, the composi...

Embodiment 3

[0032] A preparation method of 1,1,2,2,-tetrafluoroethyl-2,2,2-trifluoroethyl ether, comprising the following steps:

[0033] Step 1: add D201 strongly basic anion exchange resin 100Kg, 400Kg water, 0.5Kg of N-hydroxyethyl perfluorooctane sulfonamide, 20Kg of 1,8-diazabicyclo (5, 4,0) Undec-7-ene (DBU), 0.5Kg of disodium ethylenediaminetetraacetic acid (EDTA), stirred and reacted at 80° C. for 10 h to prepare a composite catalyst, which was set aside.

[0034] Step 2: In a 1000L stainless steel autoclave, add 100Kg trifluoroethanol at one time, the composite catalyst obtained in the above step (1) of 100Kg, close the feeding port, replace the air in the still with nitrogen, and then feed tetrafluoroethylene monomer , the temperature rises to start the reaction, the reaction temperature is controlled at 80°C, the tetrafluoroethylene is metered into the reactor, and the reaction is completed after feeding 500Kg of tetrafluoroethylene monomer, the composite catalyst is recovered ...

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PUM

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Abstract

The invention discloses a preparation method of 1, 1, 2, 2,-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether. The method comprises the steps of: (a) by weight, reacting 100 parts of strongly basic anion exchange resin, 200-400 parts of water, 0.1-0.5 part of N-hydroxyethyl perfluorooctane sulfonamide, 5-20 parts of 1, 8-diazabicyclo (5, 4, 0)undec-7-ene, and 0.05-0.5 part of ethylenediamine tetraacetic acid disodium at 40DEG C-80DEG C for 10-20h to obtain a composite catalyst for standby use; and (b) by weight, adding 100 parts of trifluoroethanol and 30-100 parts of the composite catalyst prepared in step (1) into a reaction kettle, then introducing a tetrafluoroethylene monomer to carry out reaction at 40-80DEG C, after introduction of 300-500 parts of the tetrafluoroethylene monomer, ending the reaction, performing filtering and recovering the composite catalyst, and subjecting the filtrate to washing and refining, thus obtaining 1, 1, 2, 2,-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether. The 1, 1, 2, 2,-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether prepared by the method provided by the invention has the advantages of good activity, recyclability, few three wastes, green and environmental protection.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing ether compounds, in particular to a preparation method of 1,1,2,2,-tetrafluoroethyl-2,2,2-trifluoroethyl ether. Background technique [0002] Both Japan's Daikin and Asahi Glass have launched the molecular formula CF 3 CH 2 0CF 2 CHF 2 Daikin’s commercial name is HFE-S7, Asahi Glass’s commercial name is AE3000, and the commercial name after dilution with ethanol is AE3100 (also known as HFE347pc-f). Many properties of HFE-347pc-f are similar to those of CFC-113, and there is no need for major adjustments in the method of use. However, because its KB value is smaller than that of CFC-113 and its solubility is slightly worse, it is different when used. HFE-347pc The KB value of -f is small and the solvency is weak, so ultrasonic assistance is required for cleaning. At the same time, the appropriate KB value makes it have good compatibility with most materials, easy to recycle and u...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/06B01J31/08
CPCC07C41/06B01J31/0224B01J31/0238B01J31/0244B01J31/08B01J2231/32B01J35/19C07C43/123
Inventor 王金明马利勇徐峰林晓云
Owner JUHUA GROUP TECH CENT
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