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Method for synthesizing 1, 5-dinitroanthraquinone by continuous flow micro-channel reactor

A technology of microchannel reactor and channel reactor, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, preparation of nitro compounds, etc., can solve unstable reaction process, high production risk and long reaction time and other problems, to achieve the effect of convenient intelligent production, excellent heat transfer performance and rapid response

Active Publication Date: 2021-02-23
XUZHOU COLLEGE OF INDAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, in the batch reactor, the nitrification reaction is inevitably dangerous due to local overheating due to local uneven mixing, and the reaction time is long, the reaction process is unstable, the risk of explosion is high, and the production risk is high

Method used

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  • Method for synthesizing 1, 5-dinitroanthraquinone by continuous flow micro-channel reactor
  • Method for synthesizing 1, 5-dinitroanthraquinone by continuous flow micro-channel reactor
  • Method for synthesizing 1, 5-dinitroanthraquinone by continuous flow micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Refer to figure 2 To determine the connection mode, the channel structure of the reactor is figure 1 a, The molar ratio is determined according to the channel volume and the set flow rate, and the heat transfer medium of the heat exchanger is heat transfer oil.

[0027] (2) Mix and stir 150g of anthraquinone and 900g of sulfuric acid to form anthraquinone-sulfuric acid saturated solution; prepare 92.5g of nitric acid, 370g of sulfuric acid and 4.5g of mercury sulfate to make a mixed acid nitration solution of mercury sulfate, and the solvent is dichloroethane. After preheating, the three systems were pumped in respectively through metering pumps, wherein the anthraquinone-sulfuric acid saturated solution was pumped into the micrometer at a flow rate of 14ml / min, the mixed acid nitration solution of mercuric sulfate was 10ml / min, and dichloroethane was pumped at a flow rate of 15ml / min. In the channel reactor, the molar ratio of anthraquinone to nitric acid is 1:2....

Embodiment 2

[0029] refer to figure 2 To determine the connection mode, the channel structure of the reactor is figure 1 b, The molar ratio is determined according to the channel volume and the set flow rate, and the heat transfer medium of the heat exchanger is heat transfer oil.

[0030] 150g of anthraquinone and 600g of sulfuric acid were mixed and stirred to form an anthraquinone-sulfuric acid saturated solution; 92.5g of nitric acid, 370g of sulfuric acid and 7.5g of mercuric sulfate were prepared into a mixed acid nitration solution of mercuric sulfate, and the solvent was dichloroethane. After the three systems were preheated, they were pumped in respectively through metering pumps, wherein the anthraquinone-sulfuric acid saturated solution was pumped into the micrometer at a flow rate of 14ml / min, the mixed acid nitration solution of mercuric sulfate was 14ml / min, and dichloroethane was pumped in at a flow rate of 15ml / min. In the channel reactor, the molar ratio of anthraquinone...

Embodiment 3

[0032] refer to figure 2 To determine the connection mode, the channel structure of the reactor is figure 1 a, The molar ratio is determined according to the channel volume and the set flow rate, and the heat transfer medium of the heat exchanger is heat transfer oil.

[0033] 150g of anthraquinone and 600g of sulfuric acid were mixed and stirred to form an anthraquinone-sulfuric acid saturated solution; 92.5g of nitric acid, 277.5g of sulfuric acid and 7.5g of mercuric sulfate were prepared into a mixed acid nitration solution of mercuric sulfate, and the solvent was dichloroethane. After the three systems were preheated, they were pumped in by metering pumps respectively, wherein the anthraquinone-sulfuric acid saturated solution was pumped into the micrometer at a flow rate of 14ml / min, the mixed acid nitration solution of mercuric sulfate was 15ml / min, and dichloroethane was pumped in at a flow rate of 15ml / min. In the channel reactor, the molar ratio of anthraquinone to...

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a method for synthesizing 1, 5-dinitroanthraquinone by a continuous flow micro-channel reactor. Specifically, anthraquinone is used as a substrate, and continuous nitrification is carried out in a continuous flow micro-channel reactor to generate 1, 5-dinitryl.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for synthesizing 1,5-dinitroanthraquinone with a continuous flow microchannel reactor. Background technique [0002] 1. 5-Dinitroanthraquinone is one of the most important anthraquinone derivatives. It is an important intermediate for the synthesis of anthraquinone dyes. Acidic and reactive dyes are also used in the production of inks, coatings, polymer pigments and other uses. Although there are many ways to prepare 1,5-dinitroanthraquinone, the most competitive method is the nitration of anthraquinone to prepare 1,5-dinitroanthraquinone. [0003] At present, the nitration of anthraquinone mainly includes pure nitric acid nitration method, mixed acid nitration method and solvent nitration method. In the pure nitric acid nitration method, the molar ratio of anthraquinone to nitric acid is about 1:19, the purity is not high, and the yield is 73%. The yield ...

Claims

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Application Information

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IPC IPC(8): C07C205/47C07C201/08C07C201/16B01J19/00
CPCC07C201/08C07C201/16B01J19/0093B01J2219/00873B01J2219/00894C07C2603/24C07C205/47
Inventor 李想吴祥林李兵窦艳徐宁杜辉陈君孙传益丁宗元王德堂
Owner XUZHOU COLLEGE OF INDAL TECH
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