Method for preparing hexachlorobutadiene

A technology of hexafluorobutadiene and trifluorovinyl zinc bromide, which is applied to the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of limiting the industrial production scale of hexafluorobutadiene, and achieve The synthetic route is short, the equipment requirements are not high, and the process is simple

Inactive Publication Date: 2009-09-09
HENAN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the industrial production s

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  • Method for preparing hexachlorobutadiene

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Embodiment 1

[0034] Step 1: In a 250ml three-necked flask under nitrogen atmosphere, add 0.23mol of activated zinc powder with a particle size of 400 mesh, add 0.35mol of N-methylpyrrolidone (moisture content 34ppm), heat to 70°C, Add 0.10 mol of 1,1-dibromotetrafluoroethane dropwise, the dropping time is 1h, adjust the dropping speed, keep the reaction temperature lower than 90°C during the dropwise addition, keep the reaction at 90°C for 2.5h after the dropwise addition, and then drop to to room temperature.

[0035]The second step: the above-mentioned solution down to room temperature is added dropwise to a 500ml three-necked flask containing a solution of anhydrous ferric chloride (0.12mol) dissolved in N-methylpyrrolidone (0.40mol), and the dropping time lasts 1.5h. Control the rate of addition so that the reaction temperature does not exceed 40°C during the dropwise addition, and react at 40°C for 2.5 hours after the dropwise addition is completed. After the generated gas was conden...

Embodiment 2

[0037] Step 1: In a 250ml three-necked flask under nitrogen atmosphere, add 0.23mol of activated zinc powder with a particle size of 450 mesh, add 0.40mol of N-methylpyrrolidone (moisture content 169ppm), heat to 70°C, Add 0.1 mol of 1,1-dibromotetrafluoroethane dropwise, the time for the dropwise addition is 1.5h, adjust the dropping speed, the reaction temperature cannot exceed 90°C during the dropwise addition, keep the reaction at 90°C for 6h after the dropwise addition, and then Bring to room temperature.

[0038] The second step: under stirring, add the above solution dropwise to a 500ml three-necked flask containing a solution of anhydrous ferric chloride (0.14mol) dissolved in N-methylpyrrolidone (0.35mol) at 15°C, and the dropping time is 1.2 h, after the dropwise addition, reacted at 20°C for 4h; the generated gas was condensed at -30°C, and collected with liquid nitrogen as a cold trap. The actual collection obtained 4.70g of liquid, and the actual yield of hexafluo...

Embodiment 3

[0040] Step 1: In a 250ml three-necked flask under nitrogen atmosphere, add 0.2mol of activated zinc powder, the particle size of which is 400 mesh, and 0.30mol of N-methylpyrrolidone (moisture content: 70ppm), heat to 60°C, drop Add 0.1mol of 1,1-dibromotetrafluoroethane, the dropping time is 0.8h, adjust the dropping speed, keep the reaction temperature at 80-90°C during the dropping process, and keep the reaction at 90°C for 3.0h after the dropping is completed , and then cooled to room temperature.

[0041] The second step: the above-mentioned solution cooled to room temperature was added dropwise to a 500ml three-necked flask containing anhydrous copper bromide (0.42mol) dissolved in N-methylpyrrolidone (1.20mol), and the dropwise addition lasted 1.5h, controlled The rate of addition is such that the reaction temperature during the dropping process does not exceed 30°C. After the dropwise addition, react at 30°C for 3 hours. After the generated gas is condensed at -30°C, ...

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Abstract

The invention provides a method for preparing hexachlorobutadiene by using 1, 1- dibromo-tetrafluoroethane, comprising: zinc powder and aprotic polar solvent are added into a reactor I protected by inert gas to lead the temperature to reach 50-90 DEG C; the 1, 1- dibromo-tetrafluoroethane is added into the reactor I within 0.5-3.5h and then reacts for 1.5-5h at the temperature of 50-120 DEG C; after that, the zinc powder reacts with the 1, 1- dibromo-tetrafluoroethane to produce trifluoro-ethylene zinc bromide; the reactor I is cooled to be room temperature, and the solution in the reactor I is added into a reactor II containing catalyst and solvent at the temperature below 1-40 DEG C within 0.5-3h and then reacts for 1-7h at the temperature of 0-60 DEG C; after the reaction, the obtained product is collected by a liquid nitrogen cold trap. The invention has the advantages of short synthetic route, simple technique, high raw material conversion rate, high yield of product and high purity of crude product, so that the product is simple to separate and purify, and the environmental pollution is reduced.

Description

Technical field: [0001] The invention relates to a method for preparing hexafluorobutadiene, in particular to a method for preparing hexafluorobutadiene by using 1,1-dibromotetrafluoroethane as a raw material. Background technique: [0002] Hexafluorobutadiene is a perfluorinated compound containing two double bonds (CF 2 =CF-CF=CF 2 ), the boiling point is 6°C, and the density is 1.4g / ml (15°C). In the synthesis of fluorine-containing polymers, it can be used as a polymer monomer to prepare polyhexafluorobutadiene, and it can also be used with other monomers to synthesize fluorine-containing elastomers and resins with excellent electrical properties. [0003] However, in recent years, the research on hexafluorobutadiene has mainly focused on the dry etching of ultra-large-scale integrated circuits. Studies have shown that it is a dry etching gas with excellent performance, which can perform dry etching on a width smaller than 100nm or even narrower. High accuracy and sel...

Claims

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Application Information

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IPC IPC(8): C07C21/20C07C17/263
Inventor 何伟春
Owner HENAN UNIVERSITY OF TECHNOLOGY
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