Synthesis process of dimido dipheny compound

A technique for the synthesis of diaminobenzene, which is applied in the preparation of amino compounds, the preparation of organic compounds, and organic chemistry, and can solve problems such as low industrial safety, many side reactions, and easy coking of products

Inactive Publication Date: 2015-08-19
ANHUI SHENGYUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in traditional tank reactors, especially in high-risk chemical reactions such as nitration (including continuous nitration) and catalytic hydrogenation reduction, there are many instantaneously reacted materials, large heat generation, many side reactions, and industrial safety accidents are prone to occur
[0005] The reaction on the microreactor platform has the advantages of suff

Method used

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  • Synthesis process of dimido dipheny compound
  • Synthesis process of dimido dipheny compound
  • Synthesis process of dimido dipheny compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Preparation of nitration reaction solution:

[0040] Reaction solution-1: weigh 78.8g (99%) benzene (I) as reaction solution-1;

[0041] Reaction solution-2: Weigh 128.5g (98%) nitric acid and 390g (98%) concentrated sulfuric acid and mix, keeping the temperature during the mixing process not exceeding 15°C, as reaction solution-2;

[0042] (2) Synthesis of dinitrobenzene compound (II):

[0043]Keep the temperature of the microreactor at 70°C, and add the reaction solution-1 and the reaction solution-2 into the microreactor through the syringe pumps-1 and -2 respectively, the flow rate of the reaction solution-1 is 20mL / min, and the flow rate of the reaction solution-2 The flow rate is 44mL / min. At this time, the molar ratio of nitric acid and benzene (I) added is 2.1:1, and the reaction is completed in about 5 minutes. The conversion rate of raw material benzene is 100%, and 162.1g (99.8%) of mixed dinitrobenzene products are obtained. (II, wherein the content of...

Embodiment 2

[0053] (1) Preparation of nitration reaction solution:

[0054] Reaction solution-1: weigh 788g (99%) benzene (I) as reaction solution-1;

[0055] Reaction solution-2: Weigh 1285.7g (98%) nitric acid and 2364g (98%) concentrated sulfuric acid and mix, keeping the temperature during the mixing process not exceeding 15°C, as reaction solution-2;

[0056] (2) Synthesis of dinitrobenzene compound (II):

[0057] Keep the temperature of the micro-reactor at 90°C, add the reaction liquid-1 and the reaction liquid-2 into the micro-reactor through the syringe pumps-1 and -2 respectively, the flow rate of the reaction liquid-1 is 20mL / min, the flow rate of the reaction liquid-2 The flow rate is 44mL / min. At this time, the molar ratio of nitric acid and benzene (I) added is 2.1:1, and the reaction is completed in about 50 minutes. The conversion rate of raw material benzene (I) is 100%, and 1646g (99.9%) of mixed dinitro Benzene compound (II, wherein the content of mononitrobenzene is ...

Embodiment 3～6

[0059] (1) Preparation of reduction reaction solution

[0060] Weigh 200 g of the mixed dinitrobenzene compound (II) synthesized in Example 2 and mix them with different solvents and different catalysts respectively, as reduction reaction solution-3.

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Abstract

The invention discloses a synthesis process of a dimido dipheny compound. The synthesis process disclosed by the invention comprises the following steps: by taking benzene(I) as a raw material, carrying out continuous nitration on a micro reactor platform to obtain a mixed nitrobenzene compound (II); then obtaining a mixed diaminobenzene compound (III) by carrying out catalytic hydrogenation reduction under a mild condition with temperature of 50~70 DEG C and hydrogen gas pressure not higher than 1.0MPa; and purifying to obtain o-phenylenediamine, p-phenylenediamine and m-phenylenediamine. The synthesis process disclosed by the invention has the benefits that: the use level of nitric acid is low, so that the waste acid is easy to concentrate and apply mechanically; the heat release is less, the product dinitrobenzene compound (II) is quickly transferred, the reaction phenomenon is stable without intense heat release and even punch of a common autoclave nitration reaction, so that the safety of nitration reaction is improved; the rate in nitrification reaction is fast, and the energy consumption is reduced; the reaction phenomenon is stable, so that the safety of catalytic hydrogenation reduction reaction is improved; the synthesis process is a new technique which is high in safety, easy to industrialize and less in environment protection.

Description

technical field [0001] The invention relates to a synthesis process of organic compounds, in particular to a synthesis process of diaminobenzene compounds. Background technique [0002] Diaminobenzene compound (III), including three compounds of o-, m-, and p-phenylenediamine, is widely used in the manufacture of various dyes. In Japan, m-phenylenediamine consumed by azo dye intermediate dyes accounts for 90% of the total consumption. %. At the same time, it is also widely used in the curing agent of epoxy resin, coagulant of cement, hair dye, mordant, color developer, and petroleum additives, and can be used as a raw material for the manufacture of pharmaceuticals and for the photometric determination of nitrite and reagents for active chlorine in water. [0003] The method of synthesizing diaminobenzene compound (III): (1) benzene (I) obtains dinitrobenzene compound (II) through continuous nitration, and then through reduction (divided into iron powder one-step reduction...

Claims

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Application Information

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IPC IPC(8): C07C211/51C07C209/36
Inventor 韩君邱宇飞邵玉田
Owner ANHUI SHENGYUAN CHEM
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