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Continuous production method and system of heterogeneous system azo disperse dye

A disperse dye and heterogeneous technology, applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., can solve problems such as difficult, difficult to ensure uniformity, and azo disperse dyes have not yet appeared, and achieve advanced The effect of reducing the difficulty of materials, reducing the coupling reaction time, achieving stability and simplicity

Inactive Publication Date: 2020-06-19
ZHEJIANG DIBANG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in continuous production, it is necessary to ensure that two or more strands of reaction materials are uniformly fed and contacted evenly, but continuous feeding of solid-liquid heterogeneous systems is difficult, and it is not easy to ensure uniformity. Production system for azo disperse dyes that realizes continuous and stable feeding of solid-liquid heterogeneous systems

Method used

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  • Continuous production method and system of heterogeneous system azo disperse dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] (1) Coupling component beating

[0059] Weigh 20kg of N-cyanoethyl-N-benzylaniline, add 400kg of water, add 0.04kg of dispersant MF and stir to premix, add the obtained premix to a grinder for grinding, and adjust the grinding particle size to 4-8 μm by a grinding disc. Add the ground material into the beating kettle, open the beating kettle and stir, add 50 kg of water and 30 kg of sulfuric acid, turn on the temperature control system, and control the temperature of the beating liquid to about 20-30 ° C to obtain milky white N-cyanoethyl-N-benzylaniline suspension.

[0060] (2) Coupling reaction

[0061] Prepare 53.55kg of p-nitroaniline diazonium salt solution by diazotization equipment, keep the temperature for 25~

[0062] 30 ℃, keep stirring; again, the diazonium salt solution is pumped into the supergravity rotating bed through the metering pump to adjust the flow rate to be 350g / min, and the coupling component slurry prepared in step (1) is adjusted to the flow...

Embodiment 2

[0064] (1) Coupling component beating

[0065] Using the beating method of Example 1, 2-methoxy-5-acetamido-(N,N-diallyl)aniline, water and dispersant MF were ground and pulped to obtain milky white 2-methoxy- 5-Acetylamino-(N,N-diallyl)aniline suspension.

[0066] (2) Coupling reaction

[0067] Using the coupling reaction method of Example 1, 2,4-dinitro-6-bromoaniline diazonium salt solution and 2-methoxy-5-acetamido-(N,N-diallyl)aniline were added to The slurry was pumped into a supergravity rotating bed, and reacted to obtain a coupled product, which was heated up, crystallized, filtered by pressure, and washed with water to obtain Disperse Blue 291 dye with a yield of 97.7% and a sample purity of 94.8%.

Embodiment 3

[0069] (1) Coupling component beating

[0070] Using the beating method of Example 1, grinding and beating 3-acetamido-(N,N-diethyl)aniline, water and dispersant MF to obtain milky white 3-acetamido-(N,N-diethyl) ) aniline suspension.

[0071] (2) Coupling reaction

[0072] Using the coupling reaction method of Example 1, the 2,4-dinitro-6-bromoaniline diazonium salt solution and 3-acetamido-(N,N-diethyl)aniline slurries were pumped into the hypergravity rotating bed , carry out the reaction to obtain the coupling product, carry out heating, crystallization, pressure filtration, and water washing to obtain the disperse violet 93 dye, the yield is 95.4%, and the sample purity is 93.6%.

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Abstract

The invention provides a continuous production method and system of a heterogeneous system azo disperse dye, and the method comprises the following steps: grinding and pulping a coupling intermediateinsoluble in water or an acid aqueous solution, a dispersing agent, and the water or the acid aqueous solution to obtain a coupling pulping solution, continuously pumping the coupling pulping solutionand a diazonium salt solution into a supergravity machine for coupling reaction, enabling a reaction material to flow into a receiving kettle, forming a circulating system by the receiving kettle, aheat exchanger and the supergravity machine, controlling the liquid level or weight of the receiving kettle, continuously extracting the reaction material into a crystal transformation kettle, and carrying out heating crystal transformation, filter pressing and washing to obtain the azo disperse dye. According to the method, through combination of intermediate grinding, dispersant adding and supergravity machine enhanced reaction, sulfuric acid or hydrochloric acid needing to be added during pulping in a traditional process is reduced or even eliminated, the wastewater amount can be effectively reduced, the reaction efficiency is improved, and the method has obvious advantages in the aspects of reaction retention time, product purity and yield.

Description

technical field [0001] The invention relates to the field of preparation of azo disperse dyes, in particular to a continuous production method and system for azo disperse dyes in a heterogeneous system. Background technique [0002] Disperse dyes can be divided into three types: azo type, anthraquinone type and heterocyclic type according to their molecular structure. Disperse dyes can be produced by general azo dye synthesis methods, with simple process and low cost. [0003] In industry, the production of azo disperse dyes is generally carried out in a stirred tank reactor in batch operation. However, due to the complexity of organic reactions and the large volume of the stirred tank reactor, even liquid-liquid homogeneous system materials The temperature and mixing effect are difficult to achieve uniformity in local areas. Therefore, it is more difficult to achieve uniformity of materials in the solid-liquid heterogeneous system, and the production efficiency of dyes pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/01C09B29/085C09B67/38C09B67/54
CPCC09B29/0003C09B29/08C09B67/008C09B67/0096
Inventor 徐万福邹海魁唐智勇张亮亮李勇陈建峰周海斌罗勇徐斌初广文孙宝昌
Owner ZHEJIANG DIBANG CHEM
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