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Method of preparing fluorine-containing olefin

A technology for fluorine-containing olefins and fluorochloroalkanes, applied in the field of organic fluorine chemistry, can solve problems such as hidden safety hazards, easy agglomeration, poor dispersion of metal dechlorination agents, etc., and achieves both reaction yield and efficiency, low toxicity, and solubility. Capable effect

Inactive Publication Date: 2014-07-16
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] 3. The use of alcohol solvents has great potential safety hazards, and the use of water as a solvent without a catalyst reacts very slowly, and the metal dechlorination agent is not well dispersed and easy to agglomerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a jacketed, anchored stirrer equipped with 1m 3 In the stirred tank, add 200kg of zinc powder with a specification of 200 mesh (average particle size of about 80 microns), 100kg of N,N-dimethylformamide (DMF), 350kg of deionized water, and the jacket is passed into circulating hot water to wait for the kettle When the internal temperature rises to 50°C, the flow meter starts to feed difluorotetrachloroethane in a controlled manner at a feeding rate of about 200 kg / h. As soon as difluorotetrachloroethane is added to the reaction kettle, dechlorination reaction will occur, and the heat will be released strongly. At this time, the temperature of the circulating water must be lowered so that the temperature of the kettle will not rise too much. The cumulative amount of difluorotetrachloroethane added is 600kg. The generated difluorodichloroethylene is a mixture of several isomers (b.p18.9~22°C) passing through the rectification column set on the kettle to control the ref...

Embodiment 2

[0027] Replace 200 mesh zinc powder in embodiment 1 with zinc powder of 100 mesh (average particle diameter about 150 microns), all the other are the same as embodiment 1. 345kg of the product was collected, the total content of the two isomers of difluorodichloroethylene in the product was 96.17%, and the yield of the dechlorination reaction was 91.1%.

Embodiment 3

[0029] DMF and deionized water in Example 1 were replaced by 100kg N,N-dimethylacetamide (DMAC) and 350kg deionized water, and the rest were the same as in Example 1. The raw material difluorotetrachloroethane was 587kg, and the collected product was 355kg. The total content of the two isomers of difluorodichloroethylene in the product was 98.54%, and the yield of the dechlorination reaction was 98.2%.

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Abstract

The invention relates to a method of preparing fluorine-containing olefin, and belongs to the technical field of organofluorine chemistry. The method comprises the following steps: firstly adding non-alcohol organic solvents, water and a metal dechlorinating agent with grain size of 40-150 microns into a container for stirring and mixing, and then rising the container temperature to 45 DEG C-65 DEG C; then, adding the chlorine-fluorine alkane material and keeping the temperature at 50 DEG C-80 DEG C; finally, rectifying to obtain the fluorine-containing olefin product. The method disclosed by the invention ensures that the dechloridation reaction can be kept at a certain reaction speed from beginning to end, has the advantages of being safer and more efficient, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing chemical intermediates, more specifically, the invention relates to a method for preparing fluorine-containing olefins, which belongs to the technical field of organic fluorine chemistry. Background technique [0002] Fluorinated olefins are a class of industrially important chemical intermediates, which are usually prepared by reacting chlorofluoroalkanes with metal dechlorinating agents in organic solvents. [0003] Chinese patent CN1980874 discloses a method for preparing halogenated olefins by minimizing one or more side reactions that form at least one impurity. Specifically, trifluorotrichloroethane reacts with zinc powder with an average particle size of 5-9 microns to prepare chlorotrifluoroethylene, and suitable solvents are methanol and ethanol. Generally speaking, smaller particle size of zinc powder has larger specific surface area and higher reactivity, but at the same time, it is easier to ...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C21/20C07C17/23
Inventor 黎爽罗凯吴勇陈彬彬罗生乔赖碧红杨晓勇
Owner CHINA BLUESTAR CHENGRAND CO LTD
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