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Method for gas phase catalytic synthesis of 3,4-difluorocyclobutene

A technology of difluorocyclobutene and gas phase, which is applied in the field of gas phase catalytic synthesis of 3,4-difluorocyclobutene, which can solve the problems of expensive raw materials, harsh conditions, and long routes, and achieve convenient sources, safe production, and raw material sources wide range of effects

Active Publication Date: 2020-04-10
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported route for preparing 3,4-difluorocyclobutene from dichlorocyclobutene has long routes, harsh conditions, and expensive raw materials, which limit the industrial production of 3,4-difluorocyclobutene

Method used

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  • Method for gas phase catalytic synthesis of 3,4-difluorocyclobutene
  • Method for gas phase catalytic synthesis of 3,4-difluorocyclobutene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) adopt co-precipitation method to prepare ring fluorination catalyst, the steps are as follows:

[0027] CrCl with a molar ratio of 65:20:15 3 , Co(NO 3 ) 2 , Zn(NO 3 ) 2 The solutions were mixed, and 30 wt% ammonia water was added dropwise to the mixed solution to adjust the pH to 10.0. Precipitation and filtration, washing with deionized water, drying, and pressing to obtain the ring fluorination catalyst precursor Cr-Co-Zn;

[0028] Put 50ml of ring fluorination catalyst Cr-Co-Zn precursor into the fixed bed reactor, and the fixed bed reactor is heated by an open tube heating furnace. Under the protection of 100ml / min nitrogen, the catalyst was first dried at a rate of 1°C / min to 400°C for 10 hours, and then the temperature was lowered to 200°C. This completes the drying process of the ring fluorination catalyst.

[0029] Heat the reactor to 300°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 10 hours; activate the cataly...

Embodiment 2

[0037] (1) adopt co-precipitation method to prepare ring fluorination catalyst, the steps are as follows:

[0038] CrCl with a molar ratio of 80:10:10 3 , Co(NO 3 ) 2 , Fe(NO 3 ) 3 The solutions were mixed, and 30 wt% ammonia water was added dropwise to the mixed solution to adjust the pH to 8.0. Precipitation and filtration, washing with deionized water, drying, and pressing to obtain the ring fluorination catalyst precursor Cr-Co-Fe;

[0039] Put 50ml of ring fluorination catalyst Cr-Co-Fe precursor into the fixed bed reactor, and the fixed bed reactor is heated by an open tube heating furnace. Under the protection of 100ml / min nitrogen, the catalyst was first dried at a rate of 1°C / min to 400°C for 10 hours, and then the temperature was lowered to 200°C. This completes the drying process of the ring fluorination catalyst.

[0040] Heat the reactor to 300°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 10 hours; activate the catalys...

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Abstract

The invention relates to a method for synthesizing 3,4-difluorocyclobutene through gas phase catalysis, and belongs to the field of organic chemical synthesis. According to the method, hexachlorobutadiene (the molecular formula is CCl2=CCl-CCl=CCl2), chlorine gas (the molecular formula is Cl2) and anhydrous hydrogen fluoride (the molecular formula is HF) generate 1,2,3,4-tetrachloro-3,4-difluorocyclobutene (the molecular formula is Cyclo-CFCl-CFCl-CCl=CCl-) in a gas phase manner under the action of a cyclofluorination catalyst; and under the action of a hydrodechlorination catalyst, the 1,2,3,4-tetrachloro-3, 4-difluorocyclobutene and hydrogen generate 3,4-difluorocyclobutene (the molecular formula is Cyclo-CFH-CFH-CH=CH-) in a gas phase manner. According to the invention, the method has characteristics of cheap and easily-available raw materials, simple separation and purification of the product and less industrial three-waste, and is suitable for industrial production.

Description

technical field [0001] The invention is a gas-phase catalytic method for synthesizing 3,4-difluorocyclobutene, and relates to an easy industrial method for synthesizing 3,4-difluorocyclobutene. Background technique [0002] 3,4-Difluorocyclobutene is a kind of fluorine-containing olefin compound, its molecule does not contain chlorine atoms, its ozone depletion potential (ODP) is 0, and its global warming potential (GWP) is also low. It is widely used in grain fumigation, foaming agent, electronic etching, refrigerant and other fields. It is reported that 3,4-difluorocyclobutene is a very important tire rubber additive. With the gradual increase of the automobile market, the industrial demand for 3,4-difluorocyclobutene has risen sharply, and the market demand is strong. [0003] There are few related reports on the synthesis route of 3,4-difluorocyclobutene. The literature (Spectrochimica Acta, Part A: Molecular and Biomolecular Spectroscopy, 1994, 50(2), p.191-202) repo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/23C07C17/35C07C23/06
CPCC07C17/23C07C17/35C07C2601/04C07C23/06
Inventor 柯巍周彪
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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