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A method for continuously preparing azo dye in micro-reactors

A micro-reactor, azo dye technology, applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., can solve the problem that the diazotization reaction temperature is difficult to control, the yield of diazonium salts is not high, and the reaction cycle To avoid decomposition and other side reactions, shorten the residence time, and shorten the reaction period

Active Publication Date: 2017-12-19
深圳智微通科技有限公司
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Problems solved by technology

[0006] In order to solve the problems of difficult control of diazotization reaction temperature, low yield of diazonium salt, cumbersome flow process and long reaction cycle in the existing method for continuously synthesizing azo dyes, the present invention proposes a continuous preparation method in a microreactor. The method of azo dye, concrete technical scheme is as follows:

Method used

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  • A method for continuously preparing azo dye in micro-reactors
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  • A method for continuously preparing azo dye in micro-reactors

Examples

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Embodiment 1

[0030] Embodiment 1: the concrete steps of continuous preparation azo dye product 1# are as follows (as figure 1 and figure 2 ):

[0031] (1) At room temperature (25°C), take 0.930g of aniline in a 100mL beaker, add 15mL of DMF (N,N-dimethylformamide), 2.5mL of concentrated hydrochloric acid (37%), and 32.5mL of deionized water, Stir evenly to obtain material liquid A;

[0032] (2) Take 0.731g of solid sodium nitrite in a 100mL beaker, add 15mL of DMF (N,N-dimethylformamide), 35mL of deionized water, stir until the solid of sodium nitrite is completely dissolved, and obtain feed liquid B;

[0033] (3) At room temperature (25°C), take 2.54 g of the coupling component 1-(4-sulfophenyl)-3-methyl-5-pyrazolone in a beaker, add 60 mL of water, 30 mL of DMF ( N,N-dimethylformamide) and shake well, add sodium hydroxide solution to adjust the pH of the coupling component to 9.95-10.05, stir until the coupling component is completely dissolved, and obtain material liquid C;

[0034...

Embodiment 2

[0037] Embodiment 2: the concrete steps of continuous preparation azo dye product 2-12# are as follows (as figure 1 and figure 2 ):

[0038] Use p-methoxyaniline, o-chloroaniline, p-nitroaniline, m-nitroaniline, o-nitroaniline, 1-naphthylamine, p-cyanoaniline, N, N-dimethylaniline, p-aminobenzenesulfonic acid , o-aminobenzenesulfonic acid, 1-amino-4-naphthalenesulfonic acid instead of the diazo component aniline in Example 1, and coupling component 1-(4-sulfonic acid phenyl)-3-methyl-5 -Pyrazolone is used for the continuous synthesis of azo dyes, and other conditions are consistent with Example 1 to obtain the azo dyes of 2-12# structure (see Table 1 for the structural formula).

Embodiment 3

[0039] Embodiment 3: the concrete steps of continuous preparation azo dye product 13# are as follows (as figure 1 and figure 2 ):

[0040] (1) At room temperature (25°C), put 0.930kg of aniline into a 100L container, add 15LDMF (N,N-dimethylformamide), 2.5L concentrated hydrochloric acid (37%), and 32.5L deionized water, and stir Evenly, the material liquid A is obtained;

[0041] (2) Take 0.731kg of solid sodium nitrite in a 100L container, add 15LDMF (N,N-dimethylformamide) and 35L of deionized water, and stir until the solid sodium nitrite is completely dissolved to obtain feed liquid B;

[0042] (3) At room temperature (25°C), take 3.68kg of monosodium H acid, the coupling component, into a container, add 60L of water, 30LDMF (N,N-dimethylformamide) and shake well, then add sodium hydroxide solution Adjust the pH of the coupling components to 9.95-10.05, stir until the coupling components are completely dissolved, and obtain feed liquid C;

[0043] (4) The micro-react...

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Abstract

The invention discloses a method for continuously preparing azo dye in micro-reactors in the field of dye synthesis. The azo dye is prepared by firstly subjecting a sodium nitrite solution, an aromatic primary amine and an inorganic acid to a diazotization reaction at room temperature in a first micro-reactor to generate an aromatic primary amine diazonium salt; and then subjecting the aromatic primary amine diazonium salt and a coupling component to a coupling reaction in a second micro-reactor to generate the azo dye. Continuous preparation of the azo dye is achieved by utilizing the micro-reactors, a process is simple, a reaction period is short, and a reaction process can be easily monitored and controlled. Addition of an excessive amount of the sodium nitrite and the coupling agent to increase the reaction speed is not required so that raw materials are saved and the method is environmentally friendly. Reaction liquid in the micro-reactors achieves high-speed collision mixing, a uniform reaction environment is formed immediately, the reaction efficiency is high, and the yield and quality of a reaction product are greatly improved.

Description

technical field [0001] The invention belongs to the field of dye synthesis, in particular to a method for continuously preparing azo dyes in a microreactor. technical background [0002] Azo dyes refer to a class of synthetic dyes containing azo groups (Ar-N=N-Ar) in their molecules. The annual output of this type of dyes accounts for more than half of the world's total dye production and is widely used in textile printing and dyeing. It is one of the most important categories of synthetic dyes in the fields of printing, cosmetics and so on. Compared with other dyes, azo dyes have the following advantages: (1) low cost of raw materials (2) simple synthesis method (3) complete colors (4) stable chemical properties (5) wide range of substrates. [0003] The production process of azo dyes mainly involves two-step reactions: diazotization reaction and coupling reaction. At present, the production of azo dyes in the industry is mostly carried out in batch reactors. Since the co...

Claims

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Application Information

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IPC IPC(8): C09B29/08C09B29/15C09B29/30C09B29/50
CPCC09B29/08C09B29/103C09B29/30C09B29/366
Inventor 徐建鸿王法军黄晋培桑富宁
Owner 深圳智微通科技有限公司
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