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Preparation method of hexafluoropropene trimer

A technology of hexafluoropropylene trimer and hexafluoropropylene, applied in the direction of preparation of halogenated hydrocarbons, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of increasing industrial solid waste and increasing production Cost, many by-products of reaction products, etc., to achieve the effect of less by-products, high selectivity, and less catalyst consumption

Inactive Publication Date: 2019-12-17
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis process of hexafluoropropylene trimer has been reported, most of which use hexafluoropropylene (HFP) as raw material and obtain it by polymerization in different catalyst and solvent systems, but in the reaction process, a large amount of catalyst is required , and there are many by-products in the reaction product after the reaction, the use of a large amount of catalyst will increase the production cost and increase a large amount of industrial solid waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The reaction of perfluoro-2-methyl-2-pentene and hexafluoropropylene to obtain hexafluoropropylene trimer is carried out in the following steps:

[0019] a. First clean the 500ml reactor and dry it;

[0020] b. Add 1.5g of anhydrous potassium fluoride and 1.95g of 18-crown-6, cover the lid of the kettle, and seal it well; c. Vacuumize the reaction kettle to below -0.09MPa, inhale 200g of perfluoro-2-methyl- 2-pentene and 100ml acetonitrile;

[0021] d. Turn on the stirring, feed 120g of hexafluoropropylene, and the reaction temperature should not exceed 50°C;

[0022] e. After passing through, continue to keep warm for 1.5 hours;

[0023] f. After the reaction is finished, cool to room temperature, open the reaction kettle, and separate the solvent from the fluorinated liquid with a separatory funnel;

[0024] g. Sampling and analyzing the obtained fluorinated liquid after metering;

[0025] Results: The mass of the crude fluorinated liquid was 302.6 g, the content ...

Embodiment 2

[0027] The same method operation and other conditions as in Example 2 are all the same, except that the main catalyst anhydrous potassium fluoride consumption is reduced to 0.5g, and the cocatalyst 18-crown-6 consumption is reduced to 0.65g;

[0028] Results: The mass of the crude fluorinated liquid was 305.4g, the trimer content was 84.82%, the by-product content was 0.201%, the perfluoro-4-methyl-2-pentene content was 8.32%, and the perfluoro-2-methyl The -2-pentene content is: 5.83%, the residual hexafluoropropylene is 0.16334%, the conversion rate of hexafluoropropylene is 99.83666%, and the yield of trimer is 80.95%.

Embodiment 3

[0030] The same method and operation as in Example 1 and other conditions are the same, except that the feed rate of hexafluoropropylene is increased to 150 g.

[0031] Results: The mass of the crude fluorinated liquid was 334.7g, the trimer content was 85.82%, the by-product content was 0.103%, the perfluoro-4-methyl-2-pentene content was 12.32%, and the perfluoro-2-methyl-2-pentene content was 12.32%. The content of 2-pentene is: 0.83%, the residual hexafluoropropylene is 0.00261%, the conversion rate of hexafluoropropylene is 99.99739%, and the yield of trimer is 82.07%.

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Abstract

The invention discloses a preparation method of a hexafluoropropene trimer. The preparation method comprises a step of subjecting perfluoro-2-methyl-2-pentene and hexafluoropropylene to one-step addition in an aprotic polar solvent under the action of a catalyst so as to generate the hexafluoropropene trimer, wherein the catalyst is composed of a main catalyst and a cocatalyst in a mass ratio of 0.1-10: 1, and a molar ratio of perfluoro-2-methyl-2-pentene to hexafluoropropylene is (0.1-10): 1. According to the above technical scheme, perfluoro-2-methyl-2-pentene and hexafluoropropylene are used as raw materials and undergo one-step addition under the combined action of the main catalyst and the cocatalyst so as to prepare the hexafluoropropene trimer; and the method has the advantages of high selectivity, high conversion rate, high content of the obtained product, few byproducts and low catalyst consumption.

Description

technical field [0001] The invention belongs to the technical field of organic fluorine chemistry, and relates to a preparation method of a hexafluoropropylene polymer, in particular to a preparation method of a hexafluoropropylene trimer. Background technique [0002] Hexafluoropropylene trimer is an important fluorine-containing chemical. It is the main raw material for the synthesis of fluorine-containing surfactants, and it can also be used as a cleaning agent, solvent, cooling medium, etc., so it has broad market application prospects. [0003] At present, the synthesis process of hexafluoropropylene trimer has been reported, most of which use hexafluoropropylene (HFP) as raw material and obtain it by polymerization in different catalyst and solvent systems, but in the reaction process, a large amount of catalyst is required , and there are more by-products in the reaction product after the reaction, the use of a large amount of catalyst will increase the production co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/278C07C21/18B01J31/26
CPCB01J31/0204B01J31/26B01J2231/20C07C17/278C07C21/18
Inventor 周孝瑞陶杨章鑫辉
Owner 浙江诺亚氟化工有限公司
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