A kind of method of gas phase catalytic synthesis 3,4,4-trifluorocyclobutene

A trifluorocyclobutene, gas phase technology, applied in the field of gas phase catalytic synthesis of 3,4,4-trifluorocyclobutene, can solve the problems of harsh reaction conditions, long technical route, expensive raw materials, etc., and achieve high product yield , the effect of reducing risk and convenient source

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

The synthetic methods in the existing literature have disadvantages such as long technical routes, harsh reaction conditions, and extremely expensive raw materials, which severely limit the industrial production of 3,4,4-trifluorocyclobutene

Method used

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  • A kind of method of gas phase catalytic synthesis 3,4,4-trifluorocyclobutene
  • A kind of method of gas phase catalytic synthesis 3,4,4-trifluorocyclobutene

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 75:5:20 3 , Co(NO 3 ) 2 , In(NO 3 ) 3 The solutions are mixed, 30 wt% ammonia water is added dropwise to the mixed solution, the pH is adjusted to 9.0, the precipitate is filtered, washed with deionized water, dried, and press-molded to obtain the ring fluorination catalyst precursor Cr-Co-In;

[0028] Put 50ml of ring fluorination catalyst Cr-Co-In 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 catalyst wi...

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 80:5:15 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=9.0. Precipitation is filtered, washed with deionized water, dried, and pressed to obtain ring fluorination catalyst precursor Cr-Mg-Cu.

[0039] Pass 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.

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

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Abstract

The invention relates to a method for gas phase catalytic synthesis of 3,4,4-trifluorocyclobutene, and belongs to the field of organic chemical synthesis. According to the method, 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-trichloro-3,4,4-trifluorocyclobutene(the molecular formula is Cyclo-CF2-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-trichloro-3,4,4-trifluorocyclobutene and hydrogen generate 3,4,4-trifluorocyclobutene (the molecular formula is Cyclo-CF2-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 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 3,4,4-trifluorocyclobutene, and relates to an easy industrial method for synthesizing 3,4,4-trifluorocyclobutene. Background technique [0002] 3,4,4-Trifluorocyclobutene is a widely used fluorine-containing olefin compound, which is mainly used in the fields of refrigerants, gas etching, and synthesis of fluorine-containing fine chemicals. At the same time, because of its carbon-carbon double bond And four-membered ring structure, unstable in the atmosphere, easy to degrade, with low global warming potential (GWP) and zero ozone depletion potential (ODP), is a very important class of ODP substitutes and reaction intermediates , has high economic value and industrial value, and has a large market demand. [0003] There are few reports about the synthesis route of 3,4,4-trifluorocyclobutene. Literature (Journal of Molecular Structure, 1990, 223, p.45-61) reported a kind of perfluorocyclobu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/23C07C23/06B01J23/656B01J27/132
CPCB01J23/6562B01J27/132B01J35/1019B01J35/1023C07C17/23C07C17/35C07C2601/04C07C23/06
Inventor 柯巍周彪
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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