A kind of continuous preparation method of disperse dye

A disperse dye and diazotization technology, which is applied in the field of continuous preparation of disperse dyes, can solve the problems of increasing energy consumption and material consumption in the production process, increasing production costs, and not involving the continuous system construction of downstream processes, so as to improve product quality and Effects of stability, efficiency improvement, and reaction equivalent reduction

Active Publication Date: 2021-05-11
TSINGHUA UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This inevitably brings environmental protection pressure and safety hazards, increases energy consumption and material consumption in the production process, and increases the production cost of the reaction.
At present, relevant patent documents on nitroaniline chlorination such as CN105461572B, CN104003888B, etc. all focus on the continuation of the reaction, and do not involve the construction of this process and the continuous system of the downstream process

Method used

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  • A kind of continuous preparation method of disperse dye
  • A kind of continuous preparation method of disperse dye
  • A kind of continuous preparation method of disperse dye

Examples

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Effect test

Embodiment 1

[0032] Example 1 Preparation of Disperse Violet 93:1 by Chlorination and Coupling of 2,4-Dinitroaniline

[0033] 2,4-dinitroaniline is dissolved in 98wt% sulfuric acid, and the mass ratio of 2,4-dinitroaniline to 98wt% sulfuric acid is 1:4; the solution and chlorine are continuously fed into the chlorination mixer, and then enter The chlorination reaction was carried out in a chlorination tubular reactor to obtain a 2,4-dinitro-6-chloroaniline solution; the molar ratio of 2,4-dinitroaniline to chlorine was 1:0.60, and the mixing temperature was 48°C. The temperature is controlled at 50°C, and the reaction time is 2.5 hours; 87.5% of the reaction liquid is circulated back to the chlorination mixing stage, and the remaining part is mixed with nitrosyl sulfuric acid in the diazo mixer and then sent to the diazo tubular reactor. Carry out diazotization reaction to obtain diazo solution, 85% of the diazo solution is circulated back to the diazo mixing stage, and the rest is input i...

Embodiment 2

[0035] Example 2 Preparation of Dispersed Ruby 167 by Chlorination and Coupling of p-Nitroaniline

[0036] p-nitroaniline is dissolved in 95wt% sulfuric acid, and the mass ratio of p-nitroaniline and 95wt% sulfuric acid is 1:2.5; O-chloro-p-nitroaniline solution was obtained by chemical reaction; the molar ratio of p-nitroaniline to chlorine gas was 1:0.55, the mixing temperature was 29°C, the reaction temperature was controlled at 30°C, and the reaction time was 2.5h; 89% of the reaction solution was circulated Reflux to the chlorination mixing stage, the remaining part is mixed with nitrosyl sulfuric acid in the diazo mixer and then transported to the diazo tank reactor for diazotization reaction to obtain diazonium liquid, and 86% of the diazo liquid is circulated and refluxed At the diazo mixing stage, the remaining part is input into the diazo liquid buffer tank, and the temperature is adjusted to 8°C; the molar ratio of p-nitroaniline to nitrosyl sulfuric acid is 1:1.05,...

Embodiment 3

[0038] Embodiment 3 p-Nitroaniline Chlorination Coupling Disperse Orange 30

[0039]p-Nitroaniline is dissolved in 98wt% sulfuric acid, and the mass ratio of p-nitroaniline to 98wt% sulfuric acid is 1:3; the solution and chlorine gas are continuously fed into the chlorination mixer, and enter the chlorination tubular reactor for chlorination The reaction obtained 2,6-dichloro-4-nitroaniline solution; the molar ratio of p-nitroaniline to chlorine gas was 1:1.10, the mixing temperature was 78°C, the reaction temperature was controlled at 80°C, and the reaction time was 4.5h; 92 % of the reaction solution is circulated back to the chlorination mixing stage, and the remaining part is mixed with nitrosyl sulfuric acid in the diazo mixer and then sent to the diazo tube reactor for diazotization reaction to obtain the diazo solution. 89% The diazo solution is circulated back to the diazo mixing stage, and the remaining effluent is input into the diazo solution buffer tank, and the te...

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Abstract

The invention discloses a continuous preparation method for disperse dyes, which comprises the steps of: 1) dissolving nitroaniline with sulfuric acid; 2) mixing the obtained solution with chlorine gas in a chlorination mixer and then inputting it into a chlorination reactor for chlorination reaction, The obtained chlorination reaction solution is partially recycled to step 1) to replace sulfuric acid to dissolve nitroaniline, and the remaining part flows into the diazo mixer and mixes with nitrosyl sulfuric acid after gas recovery, and then flows into the diazo reactor for diazotization reaction, and the obtained heavy Part of the nitriding reaction solution is circulated to the diazo mixer, and the remaining part is continuously mixed with the coupling solution in the coupling mixer after temperature control, and finally input into the coupling reactor for coupling reaction, and continuously discharged to obtain disperse dyes. The present invention directly continues the production process of nitroaniline chlorination and subsequent coupling, eliminates the energy and material consumption, environmental protection pressure and hidden safety hazards caused by the intermediate separation process, forms a more controllable and safe continuous reaction system, and improves product quality and stability.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a continuous preparation method of disperse dyes. Background technique [0002] Nitroaniline is chlorinated to obtain chlorinated nitroaniline, which can be further coupled with various aniline compounds to prepare disperse dyes, including disperse blue 291:2, disperse violet 93:1, disperse ruby ​​167, disperse orange 30, etc. [0003] In industrial production, the chlorination reaction of nitroaniline and the coupling reaction of chlorinated nitroaniline are completely separated, and the chlorination products of nitroaniline need to undergo cooling crystallization, separation, washing, drying and other processes before they can be used as raw materials used in the next coupling reaction. This inevitably brings environmental protection pressure and potential safety hazards, increases energy consumption and material consumption in the production process, and increases the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/01C09B29/085
CPCC09B29/0003C09B29/0834C09B29/0836
Inventor 傅伟松吕阳成徐万福兰洲黄振夫陈华祥
Owner TSINGHUA UNIV
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