A kind of preparation method of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene

A technology for hexachlorodibutene and butene is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., and can solve the problems of harsh reaction conditions, unobtainable raw materials, difficult purification, etc. The effect of low cost and simple process

Active Publication Date: 2016-04-13
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first route uses trifluorotrichloroethane as a raw material and the precious metal rhodium as a catalyst for hydrogenation reaction, which has the disadvantages of difficult raw materials, high cost, low yield and difficult purification; although the second route is cheaper Butane is used as raw material, but there will be a large amount of hydrogen chloride by-products, and the yield of the reaction is also low, and the purification is relatively difficult; the third route also has raw materials that are not easy to obtain, harsh reaction conditions, low yield, and difficult purification. Shortcomings

Method used

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  • A kind of preparation method of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene
  • A kind of preparation method of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene
  • A kind of preparation method of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene

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Experimental program
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Effect test

Embodiment 1

[0032] Add 30g (0.10mol) antimony pentachloride and 400g (20mol) hydrogen fluoride to a 1.0L autoclave respectively, stir, then add 260.8g (1.0mol) hexachlorodibutene at a rate of 2.0g / min with a metering pump . After the addition of hexachlorodibutene, react at 80°C for 6 hours, control the reaction pressure to 1.0Mpa to cool, after the reaction, pour the reaction solution into 1200g ice water, separate layers, wash the organic layer with water, and then use 200g After washing with saturated sodium bicarbonate solution and rectifying, 180.1 g (0.91 mol) of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene with a content of 99% was obtained, yield 91% .

Embodiment 2

[0034] Add 38g (0.2mol) titanium tetrachloride and 200g (10mol) hydrogen fluoride respectively in a 1.0L autoclave, stir, then add 260.8g (1.0mol) hexachlorodibutene at a speed of 2.0g / min with a metering pump . After the addition of hexachlorodibutene, react at 120°C for 8 hours, control the reaction pressure to 2.0Mpa to cool, after the reaction, add the reaction solution into 1200g ice water, separate layers, wash the organic layer with water, and then use 200g carbonic acid After washing with a saturated sodium hydrogen solution, rectification gave 184.1 g (0.93 mol) of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene with a content of 99%, with a yield of 93%.

Embodiment 3

[0036] Add 38g (0.05mol) tin tetrachloride and 600g (30mol) hydrogen fluoride respectively in a 1.0L autoclave, stir, then add 260.8g (1.0mol) hexachlorodibutene at a rate of 2.0g / min with a metering pump . After the addition of hexachlorodibutene, react at 160°C for 10 hours, control the reaction pressure to 0.5Mpa, cool down, add the reaction solution to 1200g of ice water, separate layers, wash the organic layer with water, and then use 200g of carbonic acid After washing with a saturated sodium hydrogen solution, rectification gave 182.3 g (0.92 mol) of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene with a content of 99%, with a yield of 92%.

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Abstract

The invention discloses a preparation method for 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene. The preparation method is as follows: mixing a catalyst, hydrogen fluoride and hexachlorobutadiene in a molar ratio of (0.01-0.3):(5-50):1, then, heating to 30-250 DEG C for reacting for 3-12 hours while controlling the reaction pressure to 0.1-3.0Mpa, and cooling, layering, washing, alkaline-washing and rectifying to obtain a product after the reaction is ended. The preparation method disclosed by the invention has the advantages of being simple in process, high in yield, easy in obtaining of materials and gentle in reaction condition.

Description

technical field [0001] The invention relates to a preparation method of fluoroolefins, in particular to a preparation method of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene (CF3Cl=CHCF3). Background technique [0002] 2-Chloro-1,1,1,4,4,4-hexafluoro-2-butene is an important raw material for organic synthesis. It can be oxidized to synthesize trifluoroacetic acid, and can also be synthesized by hydrogenation and dechlorination to 1 ,1,1,4,4,4-Hexafluoro-2-butene. 1,1,1,4,4,4-hexafluoro-2-butene is considered to be one of the ideal substitutes for blowing agent HCFC-141b, and it will be a key ODS substitute to be promoted in the next few years, with a good market Foreground and economic benefits, it can be used as a new type of foaming agent, refrigerant and fire extinguishing agent. 1,1,1,4,4,4-hexafluoro-2-butene as a blowing agent has the advantages of environmental protection, outstanding heat insulation properties, non-flammable, non-ozone depletion, etc., and can replace o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/35
Inventor 王宗令周强耿为利吴庆郭志毅钟俊良黄波夏林兵
Owner JUHUA GROUP TECH CENT
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