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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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  • Summary
  • 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 existing synthesis method consumes a lot of ice water and is difficult to apply to large-scale industrial production, and the reaction activity The problem of not high synthesis rate is not high

Method used

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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

Examples

Experimental program
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Effect test

Embodiment 1

[0022] HNO by mass ratio 3 :H 2 SO 4 :H 2 O=31:62:7, take 90.5% sulfuric acid and 92.3% nitric acid in a reaction vessel and stir for 2 hours at 22-25°C to prepare a mixed acid.

[0023] Take 600g of m-dichlorobenzene and 200g of nano-tetraphenylphosphine iodide with a particle size of 50nm into the reaction vessel, heat the reaction vessel to 70°C, add the mixed acid dropwise while stirring, and drop the 500ml mixed acid within 1.5 hours. Keep the reaction vessel at 70°C and continue to stir the reaction for 2 hours. After the reaction is completed, let it stand for 2 hours, filter through layers, and recover tetraphenylphosphine iodide nanoparticles. The filtrate is washed with ice water to obtain a white product, and after drying, 554 g of 2,4-Dichloronitrobenzene.

[0024] The prepared 2,4-dichloronitrobenzene was detected by gas chromatography using 102G gas chromatograph and CDMC-1 chromatographic data processor from Shanghai Analytical Instrument Factory. The chrom...

Embodiment 2

[0026] HNO by mass ratio 3 :H 2 SO 4 :H 2 O=31:62:7, take 90.5% sulfuric acid and 92.3% nitric acid in a reaction vessel and stir for 2 hours at 22-25°C to prepare a mixed acid.

[0027] Take 400g of m-dichlorobenzene and 140g of nano-tetraphenylphosphine iodide with a particle size of 20nm into the reaction vessel, heat the reaction vessel to 70°C, add the mixed acid dropwise while stirring, and drop the 300ml mixed acid within 2 hours. Keep the reaction vessel at 70°C and continue to stir the reaction for 2.5 hours. After the reaction is completed, let it stand for 1.5 hours, filter through layers, recover tetraphenylphosphine iodide nanoparticles, wash the filtrate with ice water to obtain a white product, and dry it to obtain 366g of 2,4-dichloronitrobenzene.

[0028] The prepared 2,4-dichloronitrobenzene was detected by gas chromatography using 102G gas chromatograph and CDMC-1 chromatographic data processor from Shanghai Analytical Instrument Factory. The chromatogr...

Embodiment 3

[0030] HNO by mass ratio 3 :H 2 SO 4 :H 2 O=31:62:7, take 90.5% sulfuric acid and 92.3% nitric acid in a reaction vessel and stir for 2 hours at 22-25°C to prepare a mixed acid.

[0031] Take 800g of m-dichlorobenzene and 280g of nano-tetraphenylphosphine iodide with a particle size of 80nm into the reaction vessel, heat the reaction vessel to 70°C, add the mixed acid dropwise while stirring, and drop the 660ml mixed acid within 2 hours. Keep the reaction vessel at 70°C and continue to stir the reaction for 2.5 hours. After the reaction is completed, let it stand for 1.5 hours, filter through layers, recover tetraphenylphosphine iodide nanoparticles, wash the filtrate with ice water to obtain a white product, and dry it to obtain 741g of 2,4-dichloronitrobenzene.

[0032] The prepared 2,4-dichloronitrobenzene was detected by gas chromatography using 102G gas chromatograph and CDMC-1 chromatographic data processor from Shanghai Analytical Instrument Factory. The chromatogr...

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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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