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A kind of preparation method of 3,3,3-trifluoropropene

A technology of trifluoropropene and ethylene, which is applied in the field of preparation of trifluoropropene, can solve problems such as unsafe production, complicated process, and high price, and achieve the effects of low cost, safe process, and easy control

Active Publication Date: 2014-10-22
衢州环新氟材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the problems of complex process, high price, unsafe production, and environmental protection, the purpose of the present invention is to provide a kind of low-cost and easy-to-obtain raw materials, low reaction temperature, low requirements for reaction production equipment, good catalytic activity, and easy industrial production. A kind of preparation method of 3,3,3-trifluoropropene with advantages such as

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: In a 100L stainless steel reactor, add 90kg of carbon tetrachloride and 20g of organic peroxide catalyst benzoyl peroxide, replace the oxygen in the reaction vessel with nitrogen, then heat up to 50°C, and then continuously pass 16.24 kg of ethylene was added, the pressure in the still was 0.3 MPa, and the reaction was completed in 2 hours, and the selectivity was 90-95% to obtain 1,1,1,3-tetrachloropropane.

[0029] The second step: 60 kg of the prepared 1,1,1,3-tetrachloropropane is added to the reaction kettle equipped with the mixture of the catalyst difluorotin dichloride and the polymerization inhibitor cyclobutanone, and the temperature is raised to 40° C. Then add 19.8 kg of anhydrous hydrogen fluoride continuously within 6-8 hours, and control the pressure at 0.2 MPa to obtain 1,1,1-trifluoro-3-chloropropane with a selectivity of 90-99%.

[0030] The third step: In a 100L enamel reaction kettle, 70kg of sodium hydroxide aqueous solution, 0.6kg of dodecy...

Embodiment 2

[0032] The first step: In a 100L stainless steel reactor, add 90kg of carbon tetrachloride and 15g of organic peroxide di-tertbutyl peroxide, replace the oxygen in the reaction vessel with nitrogen, then heat up to 150°C, and then continuously pass Add 0.54kg of ethylene, the pressure in the kettle is 1.5 MPa, and the reaction is completed in 3 hours, and the selectivity can be 90-99% of 1,1,1,3-tetrachloropropane.

[0033]The second step: 12 kg of the prepared 1,1,1,3-tetrachloropropane is added to the reactor containing the mixture of the catalyst difluorotin dichloride and the polymerization inhibitor cyclobutanone, and the temperature is raised to 70° C. Then add 66 kg of anhydrous hydrogen fluoride continuously within 6-8 hours, and control the pressure at 0.7 MPa to obtain 1,1,1-trifluoro-3-chloropropane with a selectivity of 90-96%.

[0034] The third step: In a 100L enamel reaction kettle, 70kg of sodium hydroxide aqueous solution, 1kg of dodecyltrimethylammonium chlor...

Embodiment 3

[0036] Step 1: In a 100L stainless steel reactor, add 90kg of carbon tetrachloride and 5g of organic peroxide catalyst 1,1-di-tert-butylperoxycyclohexane, replace the oxygen in the reaction vessel with nitrogen, and then heat up When the temperature reaches 150°C, 16.24 kg of ethylene is continuously fed in, the pressure in the kettle is 1.5 MPa, and the reaction is completed in 3 hours, and 1,1,1,3-tetrachloropropane with a selectivity of 80-85% can be obtained.

[0037] The second step: 60kg of the prepared 1,1,1,3-tetrachloropropane is added to the reaction kettle equipped with the mixture of the catalyst difluorotin dichloride and the polymerization inhibitor cyclobutanone, and the temperature is raised to 70°C. Then add 19.8 kg of anhydrous hydrogen fluoride continuously within 6-8 hours, and control the pressure at 0.7 MPa to obtain 1,1,1-trifluoro-3-chloropropane with a selectivity of 90-99%.

[0038] The third step: in a 100L enamel reaction kettle, 70kg of sodium hydr...

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Abstract

The invention discloses a preparation method for 3,3,3-trifluoropropene, and the preparation method comprises the following steps of: (1) taking carbon tetrachloride and ethylene as a raw material and organic peroxides as a catalyst, and reacting to prepare 1,1,1,3-tetrachloropropane, wherein the molar ratio of carbon tetrachloride and ethylene is (1:1)-(30:1), the reaction pressure is 0.3-1.5MPa, the reaction temperature is 50-150DEG C, and the reaction time is 2-5 hours; (2) taking the prepared 1,1,1,3-tetrachloropropane and anhydrous hydrogen fluoride as a raw material, and preparing 1,1,1-trifluoro-3-chloropropane in a reactor under the action of the catalyst and a polymerization inhibitor, wherein the molar ratio of 1,1,1,3-tetrachloropropane and anhydrous hydrogen fluoride is (1:3)-(1:50), the reaction pressure is 0.2-0.7MPa, the reaction temperature is 40-70DEG C, and the reaction time is 6-8 hours; and (3) carrying out dehydrochlorination on the prepared 1,1,1-trifluoro-3-chloropropane so as to prepare 3,3,3-trifluoropropene.

Description

technical field [0001] The invention relates to a preparation method of trifluoropropene, in particular to a preparation method of 3,3,3-trifluoropropene. Background technique [0002] Trifluoropropene is an important fluorine-containing chemical intermediate, an intermediate for the production of fluorine-containing pesticides and fluorine-containing pharmaceuticals. 3,3,3-Trifluoropropene is also the basic raw material for preparing high-performance polymer materials such as fluorosilicone rubber, fluorosilicone oil and fluorine-containing lubricating oil. [0003] 3,3,3-trifluoropropene and methyldichlorosilane can be added under the action of catalyst to obtain 3,3,3-trifluoropropylmethyldichlorosilane, which can be obtained after hydrolysis, ring closure and other reactions Important fluorosilicone monomer: trifluoropropylmethylcyclotrisiloxane. Fluorosilicone monomers are polymerized to make fluorosilicone raw rubber, and then mixed to produce fluorosilicone rubber. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/25
Inventor 方海滔应永安谢福钦陈伟倪一峰李国杰杨新华吴志筐王志强
Owner 衢州环新氟材料有限公司
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