A kind of method for replacing fluorine on double bond of fluorine-containing olefin into hydrogen

A technology for fluorine-containing olefins and fluorine replacement, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve problems such as harsh reaction conditions, difficult preparation of raw materials, and restrictions on industrial production, and achieve cheap raw materials and three industrial wastes The effect of less and safe synthesis process

Active Publication Date: 2020-07-03
天津航大翼安科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] As can be seen from the above, in the process of replacing the fluorine on the double bond of perfluoroalkene with hydrogen, there are disadvantages such as harsh reaction conditions and difficult preparation of raw materials, which limit the industrial production of this method

Method used

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  • A kind of method for replacing fluorine on double bond of fluorine-containing olefin into hydrogen

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Experimental program
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Effect test

Embodiment 1

[0026] (1) Preparation of the fluorine-to-chlorine catalyst used in the gas-phase fluorination reaction: the co-precipitation method is adopted, and the steps are as follows: CrCl 3 , Zn(NO 3 ) 2 , Mg(NO 3 ) 2 The solutions were mixed at a molar ratio of 70:20:10 to form a mixed solution, and then ammonia water accounting for 30% by weight of the above mixed solution was added dropwise to the above mixed solution, and the pH value of the mixed solution was adjusted to 9.0, after 48 hours of precipitation After aging, the precipitate was filtered and washed with deionized water, dried and pressed to form a Cr-Zn-Mg catalyst.

[0027] The drying process of the fluorine-to-chlorine catalyst: 20ml of Cr-Zn-Mg catalyst is loaded into the fixed-bed reactor, and then the fixed-bed reactor is heated by an open-type tube heating furnace. First, the Cr-Zn-Mg catalyst is raised to a temperature of 400°C at a rate of 10°C / min under the protection of 50ml / min of nitrogen and dried for ...

Embodiment 2

[0035] (1) Preparation of the fluorine-to-chlorine catalyst used in the gas-phase fluorination reaction: the co-precipitation method is adopted, and the steps are as follows: CrCl 3 , Mg(NO 3 ) 2 , Co(NO 3 ) 2 The solutions were mixed at a molar ratio of 70:20:10 to form a mixed solution, and then ammonia water accounting for 30% by weight of the above mixed solution was added dropwise to the above mixed solution, and the pH value of the mixed solution was adjusted to 9.0, after 48 hours of precipitation After aging, the precipitate was filtered and washed with deionized water, dried, and pressed to form a Cr-Mg-Co catalyst.

[0036] The drying process of the fluorine-to-chlorine catalyst: put 20ml of Cr-Mg-Co catalyst into the fixed-bed reactor, and then open the tube heating furnace to heat the fixed-bed reactor. First, the Cr-Cu-Zn catalyst is raised to a temperature of 400°C at a rate of 10°C / min under the protection of 50ml / min of nitrogen and dried for 10 hours, and ...

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Abstract

The invention relates to a method for replacing fluorine on double bonds of fluorinated alkene with hydrogen and belongs to the field of organic chemical synthesis. The method for replacing fluorine on the double bonds with hydrogen is characterized by comprising the following steps: reacting fluorinated alkene and carbon tetrachloride in the presence of a catalyst, and changing fluorine on the double bonds into chlorine at high selectivity; and changing the chlorine on the double bonds into hydrogen in the fluorinated alkene in the presence of a catalyst of replacing chlorine with hydrogen. The structural formula is as shown in the specification. According to the method disclosed by the invention, the raw materials are cheap and convenient in source; the product separation and purification are simple; industrialized production is easily realized; industrial three wastes are less.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, in particular to a method for replacing fluorine on a fluorine-containing olefin double bond with hydrogen. Background technique [0002] Fluorine-containing olefins have high industrial value and are widely used industrial raw materials. They have high application value in the synthesis of fluorine-containing fine chemicals such as fluorine-containing pharmaceutical intermediates. Perfluoroolefins are generally relatively stable. If the fluorine on its double bond is changed to hydrogen with high selectivity, the product fluoroolefin is a very important chemical intermediate. [0003] There are few reports on the method of replacing fluorine on the double bond of perfluoroalkene with hydrogen. The patent (US20138487144) reported a gas-phase method for generating l,1,1-trifluoro-3-monochloropropene from l,1,1,3-tetrafluoropropene and hydrogen chloride under the action of a sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/23C07C21/18C07C17/20
CPCC07C17/202C07C17/23C07C21/18
Inventor 周晓猛周彪赵洪海张青松
Owner 天津航大翼安科技发展有限公司
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