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Preparation method of substituted p-phenylenediamine hydrochlorides

A technology for the chemical reaction of phenylenediamine hydrochloride and phenylenediamine hydrochloride, which is applied in the field of fine chemicals, can solve the problems of limited viability and large waste water, and achieve the effects of reducing environmental protection costs, improving purity, and reducing environmental protection treatment

Active Publication Date: 2017-09-26
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method of this product in the current market: using water as a solvent, this method produces a large amount of waste water, and the viability is severely limited in today's increasingly stringent environmental protection requirements

Method used

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  • Preparation method of substituted p-phenylenediamine hydrochlorides
  • Preparation method of substituted p-phenylenediamine hydrochlorides
  • Preparation method of substituted p-phenylenediamine hydrochlorides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present invention provides a kind of preparation method of substituted p-phenylenediamine hydrochloride, comprising the following steps:

[0025] Dissolve the substituted p-phenylenediamine in the acetonitrile solvent, continuously inject hydrogen chloride gas into the acetonitrile solvent at -20-80°C for 30 minutes, and then filter to obtain the product;

[0026] Wherein, the volume molar ratio of the acetonitrile to the first substituted p-phenylenediamine hydrochloride is 200ml:1mol; the molar ratio of p-phenylenediamine to hydrogen chloride is 1:3;

[0027] The chemical reaction formula of the substituted p-phenylenediamine hydrochloride is shown in the following formula:

[0028]

[0029] A1, A2, A3, A4 represent (1), halo-Cl, -F or -Br(2), alkyl C n h 2n+1 n=0, 1, 2...9.

Embodiment 2

[0031] The substituted p-phenylenediamine was dissolved in acetonitrile solvent, hydrogen chloride gas was continuously passed into the acetonitrile solvent at 0°C for 60 minutes, and then the product was obtained by cooling and filtering.

[0032] The volume molar ratio of the acetonitrile to the first substituted p-phenylenediamine hydrochloride is 600ml:1mol.

[0033] The molar ratio of p-phenylenediamine to hydrogen chloride is 1:2.

[0034] The chemical reaction formula of the substituted p-phenylenediamine hydrochloride is shown in the following formula:

[0035]

[0036] A1, A2, A3, A4 represent (1), halo-Cl, -F or -Br(2), alkyl C n h 2n+1 n=0, 1, 2...9.

Embodiment 3

[0038] The substituted p-phenylenediamine was dissolved in acetonitrile solvent, hydrogen chloride gas was continuously passed into the acetonitrile solvent at 55°C for 120 minutes, and then the product was obtained by cooling and filtering.

[0039] The volume molar ratio of the acetonitrile to the first substituted p-phenylenediamine hydrochloride is 1000ml:1mol.

[0040] The molar ratio of p-phenylenediamine to hydrogen chloride is 1:4.

[0041] The chemical reaction formula of the substituted p-phenylenediamine hydrochloride is shown in the following formula:

[0042]

[0043] A1, A2, A3, A4 represent (1), halo-Cl, -F or -Br(2), alkyl C n h 2n+1 n=0, 1, 2...9.

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PUM

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Abstract

The invention discloses a preparation method of substituted p-phenylenediamine hydrochlorides. The method comprises the step of enabling p-phenylenediamine and hydrogen chloride to be subjected to a reaction in an acetonitrile solvent in presence of a catalyst so as to produce the substituted p-phenylenediamine hydrochlorides. The method adopts acetonitrile as the solvent, so that waste water is not produced, the recycling of the solvent is facilitated, and the manpower and the water resource are further greatly saved. The method also can improve the purity of products.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of substituted p-phenylenediamine hydrochloride. Background technique [0002] As an intermediate, substituted p-phenylenediamine hydrochloride is mainly used in the synthesis of isocyanates. The synthesis method of this product in the current market: using water as a solvent, this method produces a large amount of waste water, and the viability is severely limited in today's increasingly stringent environmental protection requirements. [0003] Based on the above shortcomings, the present invention proposes more reasonable process conditions and provides a more environmentally friendly preparation method by changing the solvent of the product. Contents of the invention [0004] It is an object of the present invention to solve at least the above-mentioned problems and to provide at least the advantages which will be described later. [0005] Still...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/52C07C211/51
CPCC07C209/00C07C211/52C07C211/51
Inventor 纪传武骆志才朱新江曾磊李欣
Owner XINYI AGRI CHEM PLANT JIANGSU PROV