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Method for preparing 2,4,6-trichloro-fluorobenzene

A technology of trichlorofluorobenzene and fluoronitrobenzene, applied in 2 fields, can solve the problems of low yield, high reaction temperature, harsh equipment conditions, etc., improve the conversion rate of raw materials, save existing resources, and solve pollution and waste Effect

Inactive Publication Date: 2008-05-14
ZHEJIANG FUSHENG HLDG GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In order to solve the problems of low yield and high reaction temperature and harsh equipment conditions in the method for preparing 2,4,6-trichlorofluorobenzene in the prior art, the present invention provides a high conversion rate, high yield and low reaction equipment requirements, Preparation method of 2,4,6-trichlorofluorobenzene with reduced cost

Method used

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  • Method for preparing 2,4,6-trichloro-fluorobenzene
  • Method for preparing 2,4,6-trichloro-fluorobenzene

Examples

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Effect test

Embodiment 1

[0032] Produce high boiler (i.e. the mixture of trichloronitrobenzene) analysis when getting p-chloronitrobenzene chlorination to produce 3,4-dichloronitrobenzene:

[0033] 3,4,5-trichloronitrobenzene accounts for 70%; 2,3,4-trichloronitrobenzene accounts for 15.7%; 2,4,5-trichloronitrobenzene accounts for 15-20%

[0034] The mixed trichloronitrobenzene and potassium fluoride (KF) after destaining are reacted with the quaternary ammonium salt catalyst at 150-190° C. for 10-20 hours in the presence of solvent DMF. The catalyst consumption of the quaternary ammonium salt catalyst is 1%, the mixed trichloronitrobenzene is 450kg, and the potassium fluoride is 232kg.

[0035]After completion of the reaction, 280 kg of 3,5-dichloro-4-fluoronitrobenzene was isolated.

[0036] Then take 3,5-dichloro 4-fluoronitrobenzene as raw material in 500mL reactor, add 84g catalyst benzoyl peroxide (by raw material weight) simultaneously, feed chlorine and carry out catalytic chlorination reacti...

Embodiment 2

[0038] 500kg of 3,5-dichloro-4-fluoronitrobenzene was put into the reactor, and at the same time, in the presence of 100g of catalyst azobisisobutyronitrile, a catalytic chlorination reaction occurred with chlorine gas, and the reaction temperature was maintained at 250°C. After reacting for 4 hours, 2,4,6-trichlorofluorobenzene was obtained with a yield of 95%, and the purity of the product was 99.5% as measured by GC.

Embodiment 3

[0040] The 3,5-dichloro-4-fluoronitrobenzene of this embodiment comes from the leftovers after rectification when preparing 2,3,4-trifluoronitrobenzene, and the leftovers are 87.5% 3,5-dichloro -4-fluoronitrobenzene, the rest is 3,4-difluoro-5-chloronitrobenzene and a small amount of sulfolane, and 99.1% of 3,5-dichloro-4-fluoronitrobenzene is obtained by conventional crystallization and centrifugation benzene.

[0041] Get 3, the 3 of 3,5-dichloro-4-fluoronitrobenzene 300kg, the 3 of 5-dichloro-4-fluoronitrobenzene drops into reaction still, under the existence of 3kg catalyst crown ethers and chlorine generation catalytic chlorination reaction simultaneously, The reaction temperature was maintained at 180°C. After reacting for 5 hours, 2,4,6-trichlorofluorobenzene was obtained with a yield of 94%, and the purity of the product was 99% as measured by GC.

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Abstract

The invention relates to a preparation method for the two, four, six-three-chlorine fluorobenzene, belonging to fluorin chemical engineering technical field. The invention is characterized in that three and five-two chlorine and four fluorin are used as the materials, which are catalyzed and chlorinated with the chlorine under the action of a catalyst in order to make the two, four and six-three-chlorine fluorobenzene; the reaction temperature ranges from one hundred and fifty and two hundred and fifty DEG C; the catalyst is chosen from oxidation benzoyl, azobisisobutyronitrile, and crown ether; the dosage accounts for zero point zero three percent to one percent of the three and five-two-chlorine-four-nitrobenzene. The invention has the advantages that the defects of the preparation method in the prior art such as low yield, high reaction temperature and the rigorous equipment condition are overcome; the preparation method enables the reaction to be completed below two hundred and twenty DEG C; the reaction equipment and the corresponding matched auxiliary equipment has low cost; the material transformation rate and the yield are increased; the purity of the products can reach ninety-nine point eight percent; the materials of the invention can be chosen from the leftovers which can be seen commonly in chemical enterprises and the rectifying remaining, which can save the prior resources with good economic benefit, environmental benefits and social benefits.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, and specifically relates to a preparation method of 2,4,6-trichlorofluorobenzene. Background technique [0002] 2,4,6-Trichlorofluorobenzene belongs to chlorofluoroorganic compounds, it can also be 2-fluoro-1,3,5-trichlorobenzene, its English name is 2,4,6-Trichlorofluorobenzene; 1,3, 5-trichloro-2-fluorobenzene; or 2-fluoro-1,3,5-trichlorobenzene; CAS registration number: 36556-33-9; the structural formula is as follows: [0003] [0004] 2,4,6-Trichlorofluorobenzene can be used as a liquid crystal material and as an intermediate in the synthesis of pesticides, and has potential market demand. [0005] In the prior art, there are few reports on the synthesis method of 2,4,6-trichlorofluorobenzene. In the European patent EP0355719 A1 "Preparation of chlorofluorobenzenes", Kumai, Seisaku et al once proposed the following The fluorobenzene compound of the structural formula ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/13C07C17/093B01J31/02
Inventor 沈志良杨茂生陈志明周智慧徐德忠
Owner ZHEJIANG FUSHENG HLDG GROUP
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