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Method for preparing water-soluble azo dye continuously by chaos mixing of spiral tube

A technology of chaotic mixing and azo dyes, applied in the direction of mixing methods, azo dyes, monoazo dyes, etc., can solve the problems of unseen coupling and continuous reaction of spiral tube reactors, and achieve enhanced chaotic mixing effect and residence time Short, low energy consumption effect

Active Publication Date: 2012-08-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the chaotic mixer is mainly a straight tube type sudden expansion and contraction structure, and there is no reactor with a helical tube type sudden expansion and contraction structure, and there are no relevant reports on the coupling and continuous reaction in this reactor.

Method used

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  • Method for preparing water-soluble azo dye continuously by chaos mixing of spiral tube
  • Method for preparing water-soluble azo dye continuously by chaos mixing of spiral tube
  • Method for preparing water-soluble azo dye continuously by chaos mixing of spiral tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation of coupling component solution: in the 250ml flask that fills 20ml water, add 3.41g 1-amino-8-hydroxyl-3,6-naphthalene disulfonic acid, add the sodium carbonate solution that concentration is 20% under stirring, Adjust the pH to 6.0-6.5, add water to dilute the coupling component solution to a total volume of 200ml, and a pH of 6.0-6.5 to obtain a solution containing the coupling component of 1-amino-8-hydroxy-3,6-naphthalene disulfonic acid for use. Prepare an aniline diazonium salt solution with the same molar concentration as the coupling component solution for later use.

[0021] Utilize the calibration constant flow pump, the flow rate of regulating aniline diazonium salt solution and coupling component solution is 30ml / min, aniline diazonium salt solution and above-mentioned coupling component solution are transported respectively in the helical tube chaos continuous reactor (the The number of connections between the thick spiral tube and the thin ...

Embodiment 2-22

[0023] Use p-methoxyaniline diazonium salt solution, o-chloroaniline diazonium salt solution, 1-naphthylamine diazonium salt solution, aniline 2,5 disulfonic acid diazonium salt solution, p-nitroaniline diazonium salt solution, m- Nitroaniline diazonium salt solution, o-nitroaniline diazonium salt solution, p-cyanoaniline diazonium salt solution, p-aminobenzenesulfonic acid diazonium salt solution, o-aminobenzenesulfonic acid diazonium salt solution, 1-amino- 4-Naphthalenesulfonic acid diazonium salt solution and structure are respectively the diazonium salt solution of 1-10#, replaces aniline diazonium salt solution, respectively with 1-amino-8-hydroxyl-3 , 6-naphthalene disulfonic acid solution reaction to prepare the corresponding water-soluble azo dye solution, other conditions are consistent with Example 1.

[0024]

Embodiment 23-33

[0026] With 1-naphthylamine-6-sulfonic acid, 2-amino-8-hydroxy-6-naphthalenesulfonic acid, 2-amino-5-hydroxy-7-naphthalenesulfonic acid, 2-amino-8-hydroxy-3,6 -Naphthalene disulfonic acid, 1-amino-8-hydroxy-4-naphthalenesulfonic acid, 1-amino-8-hydroxy-2,4-naphthalene disulfonic acid, 1-anilino-8-naphthalenesulfonic acid solution and structure The coupling component solutions of 11-14# respectively replace 1-amino-8-hydroxyl-3,6-naphthalene disulfonic acid solution, and react with aniline diazonium salt solution in a spiral tube chaotic continuous reactor to obtain the corresponding The water-soluble azo dye solution, other conditions are consistent with embodiment 1.

[0027]

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Abstract

The invention provides a method for preparing a water-soluble azo dye continuously by the chaos mixing of a spiral tube. The core is that a spiral tube sudden-expansion and sudden-contraction structure is adopted; compared with pure straight tube sudden-expansion and sudden-contraction mixed reaction, the method has the advantages that a mixed effect of a transverse secondary flow generated by fluid in a curved pipeline is far stronger than that of pure diffusion of a straight tube part; compared with the conventional spiral tube, the sudden-expansion and sudden-contraction part has the advantages that the motion trail of the fluid can be changed, the superficial area of a mixed interface can be increased and a chaos mixing effect can be enhanced; and the mixer has the advantages of quick and uniform mixing, stirring prevention, short retention time, high quality stability of the product, high speed of removing reaction heat by a tube wall and the like of a microreactor, and also overcomes the defects of small internal diameter and high possibility of blockage of the microreactor, so that the dye can be produced quickly and continuously, and the method is wide in industrial prospect.

Description

technical field [0001] The invention relates to a continuous preparation method of spiral tube chaotic mixing of water-soluble azo dyes. Background technique [0002] There are many kinds of azo dyes, including acid, direct, reactive, and disperse dyes. Its annual output accounts for more than half of the world's dyes, and it is an extremely important class of dyes. In the production process, it involves the coupling reaction process, that is, the reaction of diazonium salt and aromatic amine or phenol and other coupling components to form azo compound, which is an important step in the production of azo dyes. However, the coupling reaction is an exothermic reaction, and the diazonium salt is unstable to heat. Therefore, the conventional batch synthesis process must be carried out under cooling. Generally, it is cooled with an ice-water bath, and the temperature is maintained at 0-5°C for the coupling reaction. Cause energy waste, and in the coupling reaction process, due t...

Claims

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Application Information

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IPC IPC(8): C09B29/30C09B31/08B01J19/00B01F5/00B01F3/08
Inventor 张淑芬梁栋吕荣文唐炳涛
Owner DALIAN UNIV OF TECH
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