Preparation method for fluorochlorobenzene

A chlorobenzene and fluorine substitution technology is applied in the field of preparation of aromatic fluorine-containing organic compounds, which can solve problems such as catalyst failure to catalyze, waste water pollution, etc., and achieve the effects of high conversion rate and yield, simple product separation, and obvious economic benefits.

Active Publication Date: 2008-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This also causes additional wastewater pollution and the catalysts added often do not catalyze in a satisfactory manner

Method used

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  • Preparation method for fluorochlorobenzene
  • Preparation method for fluorochlorobenzene

Examples

Experimental program
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Effect test

Embodiment 1

[0046] A kind of preparation of fluoropentachlorobenzene, put 500ml there-necked bottle and stir, add 0.04mol hexachlorobenzene, 0.28mol anhydrous potassium fluoride, 150ml ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate, The reactants were mixed and stirred.

[0047] React at 160°C to 230°C for 16 hours. During the reaction, the temperature increases gradually. Starting from 160°C, the temperature gradually rises until it reaches 230°C at the end of the reaction. Then, it is separated by vacuum distillation to obtain 9.12 grams of fluoropentachloro Benzene C 6 Cl 5 F, productive rate is 85% (in hexachlorobenzene); Obtain 1.1 grams of difluorotetrachlorobenzene C simultaneously 6 Cl 4 f 2 , and the yield was 11% (calculated as hexachlorobenzene).

Embodiment 2

[0049] A preparation of fluoropentachlorobenzene, put a 500ml three-necked bottle on it and stir, add 0.04mol hexachlorobenzene, 0.28mol anhydrous potassium fluoride, 180ml ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate , and the reactants were mixed and stirred.

[0050] React for 12 hours at 160°C to 230°C. During the reaction, the temperature rises gradually, and the heating rate can be roughly uniform, but it is not necessary to strictly follow the constant rate of temperature rise; vacuum rectification and separation obtain 8.63 grams of fluoropentachlorobenzene C 6 Cl 5 F, productive rate is 80% (in hexachlorobenzene); Obtain a small amount of difluorotetrachlorobenzene C simultaneously 6 Cl 4 f 2 (<1%).

Embodiment 3

[0052] A kind of preparation of fluoropentachlorobenzene, put 500ml there-necked bottle and stir, add 0.04mol hexachlorobenzene, 0.28mol anhydrous potassium fluoride, 200ml ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate, The reactants were mixed and stirred.

[0053] Reacted at 210°C for 10 hours, and separated by vacuum distillation to obtain 9.04 grams of fluoropentachlorobenzene C 6 Cl 5 F, productive rate is 84% ​​(in hexachlorobenzene); Obtain 0.8 gram of difluorotetrachlorobenzene C simultaneously 6 Cl 4 f 2 , and the yield was 8% (calculated as hexachlorobenzene).

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Abstract

The invention relates to organic chemistry, in particular to a preparation of aromatic fluorine organic compound, which uses hexachlorobenzene as material, uses alkali metal fluoride as fluorizating agent, and uses ion liquid as medium, to be mixed, reacted, and distilled and separated in vacuum, to prepare fluoro-chlorobenzene. The inventive preparation can avoid catalyst and simplify productionprocess, with warm reaction condition, high conversion rate and yield, reduced energy consumption, reduced pollution, significant economic benefit, and large-scale industrial application. The invention can be applied in medical and chemical technical fields.

Description

technical field [0001] The present invention relates to organic chemistry, in particular to the preparation of aromatic fluorine-containing organic compounds. Background technique [0002] Aromatic fluorine-containing organic compounds are widely used, involving medicine, pesticides, dyes and other industries. These compounds can be used to synthesize herbicides, fungicides, antineoplastic drugs, antipsychotic drugs, anti-senile dementia drugs, functional dyes and other products . Such as pentafluorobenzoic acid is the raw material for the synthesis of quinolone antibacterial drug sparfloxacin; hexafluorobenzene is the raw material for the synthesis of tri(pentafluorophenyl)boron, and tri(pentafluorophenyl)boron is a new cocatalyst. A generation of olefin polymerization catalysts are gradually being applied in industrial production. [0003] At present, the synthesis of polyfluorinated benzene in industry mostly adopts halogen exchange reaction, which mainly refers to the ...

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C25/13B01J31/02
Inventor 李勇王大文
Owner CHINA PETROLEUM & CHEM CORP
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