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Resource utilization method of tail gas from trifluoroethylene production

A technology of trifluoroethylene and chlorotrifluoroethylene, which is applied in organic chemistry, halogen addition preparation, etc., can solve problems such as incinerator corrosion, and achieve the effects of mild reaction conditions, simple process, and easy purification

Inactive Publication Date: 2013-01-09
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrogen fluoride produced during the combustion of trifluoroethylene and chlorotrifluoroethylene will cause serious corrosion to the incinerator

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Preparation of trifluoroethylene

[0028] The raw materials chlorotrifluoroethylene and hydrogen flow into the fixed-bed reactor according to a certain ratio after being measured by the flow meter to carry out the catalytic hydrodechlorination reaction. The reactor is filled with a hydrodechlorination catalyst. After the reaction, the product is washed with water, alkali and dried. Enter the low temperature condensation system to collect the product trifluoroethylene, the reaction temperature is 20~200 ℃, and the raw material space velocity is 100~1000 h -1 , Hydrogen: Chlorotrifluoroethylene 0.3~2.0, condensation temperature -60~-80 ℃. Due to the low boiling point of trifluoroethylene and the entrainment of hydrogen in the reaction system, the reaction product cannot be completely condensed and collected. The gas flowing out from the outlet of the condensation collection system is called trifluoroethylene tail gas, in which the hydrogen content is 40~60%. Tr...

Embodiment 2

[0031] Add 300 g of bromine into the three-necked flask, heat up to 50°C, stir and reflux, and continuously feed the trifluoroethylene tail gas (42% trifluoroethylene content, 6% chlorotrifluoroethylene content) in Example 1 to carry out the bromination reaction , The flow of trifluoroethylene tail gas is controlled by a flowmeter, and the reaction is stopped when the molar ratio of bromine to the total content of trifluoroethylene and chlorotrifluoroethylene accumulated is 1.1. After alkali neutralization and water washing, static layering, the organic phase after removing the upper layer of water was dried over anhydrous magnesium sulfate, filtered, and chromatographically analyzed to obtain 353.7 g of dibromotrifluoroethane and 57.7 g of dibromotrifluorochloroethane. g.

[0032] Since bromine remains in excess during the reaction, the content of trifluoroethylene and chlorotrifluoroethylene in the tail gas after the reaction is less than 1%.

[0033]

Embodiment 3

[0035] The bromination reaction was carried out using the same bromination method as in Implementation 2, adding 300 g of bromine, raising the temperature to 30 °C, and stopping the reaction when the molar ratio of bromine to the total content of trifluoroethylene and chlorotrifluoroethylene accumulated was 1.2. After alkali neutralization and water washing, static layering, the organic phase after removing the upper layer of water was dried over anhydrous magnesium sulfate, filtered, and chromatographically analyzed to obtain 297.8 g of dibromotrifluoroethane and 48.6 g of dibromotrifluorochloroethane. g.

[0036]

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Abstract

The invention discloses a resource utilization method of tail gas from trifluoroethylene production. According to the invention, addition reaction between the tail gas from the trifluoroethylene production and bromine is performed to generate dibromotrifluoroethane and dibromotrifluoro chloroethane. The preparation method has the following advantages: the technology is simple; reaction condition is mild; purification is easy; and the technology is suitable for large-scale production. The method provided by the invention has effects of energy conservation and emission reduction. The prepared dibromotrifluoroethane can be used to prepare a dry etching gas hexafluorobutadiene, novel gyroscope suspension fluorobromohydrocarbon oil, alpha, beta, beta-trifluorostyrene and an insecticide and acaricide 1,4-diaryl-2,3-difluoro-2-butene. The prepared dibromotrifluoro chloroethane can be used to prepare a plant growth regulator's intermediate ethyl bromodifluoroacetate and a chain transfer agent used as radical polymerization.

Description

technical field [0001] The invention relates to a method for utilizing tail gas in the production of trifluoroethylene, in particular to a method for preparing dibromotrifluoroethane and dibromotrifluorochloroethane by using the tail gas in the production of trifluoroethylene as raw materials. [0002] Background technique [0003] Both dibromotrifluoroethane and dibromotrifluorochloroethane are very valuable raw materials. [0004] Dibromotrifluoroethane (CF 2 BrCBrHF) dehydrobromide generated bromotrifluoroethylene (CF 2 =CBrF) can produce excellent dry etching gas perfluorobutadiene (CF 2 =CF-CF=CF 2 ) (US2008 / 0300432A1), can also prepare novel gyro suspension fluid bromide oil (US4,835,304), α,β,β-trifluorostyrene (Burton,D.et al.J.Org.Chem,1988, 53,2714) and insecticide and acaricide 1,4-diaryl-2,3-difluoro-2-butene (US6,506,800). [0005] Dibromotrifluorochloroethane (CF 2 BrCBrClF) can be used to synthesize ethyl bromodifluoroacetate (JP 11080084 A) as an inter...

Claims

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Application Information

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IPC IPC(8): C07C19/12C07C19/14C07C17/04
Inventor 徐卫国刘武灿张金柯石能富
Owner SINOCHEM LANTIAN
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