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A kind of gas-phase catalytic synthesis method of 4,4-difluorocyclobutene

A technology of difluorocyclobutene and gas phase, which is applied in the field of gas-phase catalytic synthesis of 4,4-difluorocyclobutene, can solve the problems of non-compliance with chemical synthesis green environmental protection, long synthesis route, harsh conditions, etc., and achieves less industrial waste , The effect of high product yield and production safety

Active Publication Date: 2021-03-23
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As can be seen from the above, the disadvantages of the reported routes for the synthesis of 4,4-difluorocyclobutene are that the synthetic route is long, the conditions are harsh, and the raw materials are very expensive, which does not meet the requirements of green environmental protection for chemical synthesis.
These all limit the industrial production of 4,4-difluorocyclobutene

Method used

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  • A kind of gas-phase catalytic synthesis method of 4,4-difluorocyclobutene
  • A kind of gas-phase catalytic synthesis method of 4,4-difluorocyclobutene

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) adopt co-precipitation method to prepare ring fluorination catalyst, the steps are as follows:

[0028] CrCl with a molar ratio of 70:15:15 3 , Mg(NO 3 ) 2 , Cu(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. Precipitating and filtering, washing with deionized water, drying, and pressing to obtain the ring fluorination catalyst precursor Cr-Mg-Cu;

[0029] Put 50ml of ring fluorination catalyst Cr-Mg-Cu 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.

[0030] Heat the reactor to 300°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 10 hours; activate the catalys...

Embodiment 2

[0038] (1) adopt co-precipitation method to prepare ring fluorination catalyst, the steps are as follows:

[0039] CrCl with a molar ratio of 80:10:10 3 , Zn(NO 3 ) 2 , Mg(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-Zn-Mg;

[0040] Put 50ml of ring fluorination catalyst Cr-Zn-Mg 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.

[0041] Heat the reactor to 300°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 10 hours; activate the cataly...

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Abstract

The invention relates to a method for synthesizing 4,4-difluorocyclobutene through gas phase catalysis, and belongs to the field of organic chemical synthesis. The method is characterized in that: hexachlorobutadiene (the molecular formula is CCl2=CCl-CCl=CCl2), chlorine (the molecular formula is Cl2) and anhydrous hydrogen fluoride (the molecular formula is HF) generate 1,2,3,3-tetrachloro-4,4-difluorocyclobutene (the molecular formula is Cyclo-CF2-CCl2-CCl=CCl-) in a gas phase manner under the action of a cyclofluorination catalyst. Then, under the action of a hydrodechlorination catalyst, the 1,2,3,3-tetrachloro-4,4-difluorocyclobutene and hydrogen are subjected to a gas phase reaction to generate the 4,4-difluorocyclobutene (the molecular formula is Cyclo-CF2-CH2-CH=CH-). The raw materials are cheap and convenient to obtain; the product separation and purification are simple; the industrial production is easy; industrial three wastes are reduced.

Description

technical field [0001] The invention is a method for synthesizing 4,4-difluorocyclobutene by gas phase catalysis, and relates to an easy industrial method for synthesizing 4,4-difluorocyclobutene. Background technique [0002] Since CFCs and HCFCs widely used in refrigerants, fire extinguishing agents, blowing agents and other industries have a destructive effect on the ozone layer and produce a greenhouse effect, the production of zero ozone depletion potential (ODP) and low global warming potential (GWP) ) of hydrofluorocarbons has become an increasingly important topic in the world. 4,4-Difluorocyclobutene, with the characteristics of zero ozone depletion potential (ODP) and low global warming potential (GWP), is a very economically valuable intermediate, and its downstream products can be used in precision electronics Cleaning agent for circuit boards has high application value in the synthesis of fluorine-containing fine chemicals such as fluorine-containing pharmaceut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/23C07C23/06C07C17/20B01J23/26B01J23/89
CPCB01J23/26B01J23/8906C07C17/204C07C17/23C07C2601/04C07C23/06
Inventor 周彪柯巍孙绪坤
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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