Method for catalytically synthesizing 2, 4-dichloronitrobenzene by adopting tetraphenylphosphine iodide

A technology of tetraphenylphosphine iodide and dichloronitrobenzene is applied in the field of preparation of 2,4-dichloronitrobenzene, and can solve the problem of low synthesis rate, low reaction activity, large consumption of ice water, etc. problem, to achieve the effect of improving selectivity and improving reactivity

Pending Publication Date: 2021-07-09
YUNNAN YUNTIANHUA +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for catalyzing the synthesis of 2,4-dichloronitrobenzene using tetraphenylphosphine iodide, which solves the problem that the e

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  • Method for catalytically synthesizing 2, 4-dichloronitrobenzene by adopting tetraphenylphosphine iodide
  • Method for catalytically synthesizing 2, 4-dichloronitrobenzene by adopting tetraphenylphosphine iodide
  • Method for catalytically synthesizing 2, 4-dichloronitrobenzene by adopting tetraphenylphosphine iodide

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[0021] Example 1

[0022] HNO according to quality ratio 3 : H 2 SO 4 : H 2 O = 31: 62: 7, a mass fraction of 90.5% sulfuric acid, 92.3% of nitric acid were prepared in the reaction vessel for 2 hours at 22 to 25 ° C for 2 hours.

[0023] 600 g of dichlorobenzene was taken into a reaction vessel, and the reaction vessel was added to 70 ° C, and the reaction container was heated to 70 ° C, and the mixed acid was added dropwise over the stirring, and the mixed acid of 500 ml was dripped within 1.5 hours. The reaction vessel was allowed to continue to be stirred at 70 ° C for 2 hours. After the reaction was completed, it was allowed to stand for 2 h, and the tetraenzyl iodide nano particles were retained, and the filtrate was rinsed with ice water to obtain a white product. After drying 554g 2,4-dichlorobenzene.

[0024] The preparative 2,4-dichlorozene chlorobenzene was prepared by a 102G gas chromatograph and a CDMC-1 chromatographic data processor of the Shanghai Analytical Instru...

Example Embodiment

[0025] Example 2

[0026] HNO according to quality ratio 3 : H 2 SO 4 : H 2 O = 31: 62: 7, a mass fraction of 90.5% sulfuric acid, 92.3% of nitric acid were prepared in the reaction vessel for 2 hours at 22 to 25 ° C for 2 hours.

[0027] 400 g of dichlorobenzene, a particle size of 20 nm was added to the reaction vessel to the reaction vessel, and the reaction vessel was heated to 70 ° C, and the mixed acid was added dropwise on the stirring, and 300 ml of mixed acid was dripped within 2 hours. The reaction vessel was allowed to continue to stir at 70 ° C for 2.5 hours, and after the reaction was completed, it was allowed to stand for 1.5 h, and the tetraparaphenyl iodide nano particles were recovered, and the filtrate was rinsed with ice water to give 366 g. 2,4-dichlorobenzene.

[0028] The preparative 2,4-dichlorozene chlorobenzene was prepared by a 102G gas chromatograph and a CDMC-1 chromatographic data processor of the Shanghai Analytical Instrument Factory. The column spec...

Example Embodiment

[0029] Example 3

[0030] HNO according to quality ratio 3 : H 2 SO 4 : H 2 O = 31: 62: 7, a mass fraction of 90.5% sulfuric acid, 92.3% of nitric acid were prepared in the reaction vessel for 2 hours at 22 to 25 ° C for 2 hours.

[0031] 800 g of dichlorobenzene was taken into a reaction vessel, and the reaction vessel was added to 70 ° C, and the mixed acid was added to 70 ° C, and the mixed acid was added dropwise over 2 hours. The reaction vessel was allowed to continue to stir at 70 ° C for 2.5 hours, and after the reaction was completed, it was stratified, and the tetraparaphenyl iodide nanophenyl, the filtrate was recovered, and the filtrate was rinsed to obtain a white product, 741 g 2,4-dichlorobenzene.

[0032] The preparative 2,4-dichlorozene chlorobenzene was prepared by a 102G gas chromatograph and a CDMC-1 chromatographic data processor of the Shanghai Analytical Instrument Factory. The column specification is 2.2m × 2.9m stainless steel column, which is used as a fi...

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Abstract

The invention discloses a method for catalytically synthesizing 2, 4-dichloronitrobenzene by adopting tetraphenylphosphine iodide, and relates to the technical field of preparation of 2, 4-dichloronitrobenzene. The method specifically comprises the following steps: adding m-dichlorobenzene and tetraphenylphosphine iodide into a reaction container, uniformly mixing, heating the reaction container, and keeping the temperature of the reaction container at 70 DEG C; then dropwise adding mixed acid into the reaction container at a constant speed, continuously stirring for 2-2.5 hours after dropwise adding is completed within 1.5-2 hours, keeping the temperature at 70 DEG C, and standing for 1.5-2 hours after the reaction is completed; and after layered filtration, washing with cooling water, and drying to obtain the 2, 4-dichloronitrobenzene. Tetraphenylphosphine iodide is added in the nitration reaction process of m-dichlorobenzene, the selectivity of nitration reaction is greatly improved by using the tetraphenylphosphine iodide, the reaction activity is greatly improved, the nitration reaction efficiency is improved to 95% or above, the total reaction efficiency is improved to 92% from 63%, and the standard addition recovery rate of 2, 4-dichloronitrobenzene detected by gas chromatography is 98.9% on average.

Description

technical field [0001] The invention relates to the technical field of 2,4-dichloronitrobenzene preparation, in particular to a method for catalytically synthesizing 2,4-dichloronitrobenzene by using tetraphenylphosphine iodide. Background technique [0002] 2,4-Dichloronitrobenzene is an important basic organochlorine intermediate, which can synthesize more than 20 kinds of chlorine-containing intermediates and more than 100 kinds of chlorine-containing fine chemicals, such as dichlorobenzene, trichlorobenzene, fluorochlorophenol , Fluorochlorophenol, chlorofluoronitrobenzene, nitrochloroaniline, etc. Most of 2,4-dichloronitrobenzene is prepared by dropping mixed acid of sulfuric acid and nitric acid in m-dichlorobenzene for nitration reaction, but its reactivity is not high and the synthesis rate is not high, so the reaction temperature needs to be strictly controlled. Such as patent CN101700997A discloses a kind of synthetic method of 2,4-dichloronitrobenzene, carries ou...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/12B01J31/02
CPCC07C201/08B01J31/0268C07C205/12Y02P20/584
Inventor 李骥马航陈伟王鹏宝宗世荣李灿缪明志
Owner YUNNAN YUNTIANHUA
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