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A method for continuous coupling of dyes and reducing energy consumption

A technology of energy consumption and dyes, applied in the direction of azo dyes, organic dyes, monoazo dyes, etc., can solve the problems of high energy consumption and low production efficiency in freezing, and achieve the goals of saving cold energy, improving production efficiency and preventing clogging Effect

Active Publication Date: 2017-04-19
SHAOXING UNIVERSITY +1
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Problems solved by technology

[0008] Aiming at the problems of low production efficiency and high energy consumption of freezing in the coupling process in the prior art, the object of the present invention is to provide a method for continuous coupling production and energy consumption reduction. The device is continuously pumped into the coupling reaction kettle, the cooling water flow rate is adjusted to control the coupling temperature at -10°C to 30°C, and the coupling reaction is carried out in stages under stirring. There are excessive coupling components in the first-stage coupling kettle to ensure that the diazo Salt can be quickly reacted and consumed, so it can be carried out at a moderately high temperature, reducing the requirement for chilled water and saving energy

Method used

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  • A method for continuous coupling of dyes and reducing energy consumption

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Embodiment l

[0033] As shown in Figure 1, 926 kg of 3-acetylamino-N, N-diethylaniline, 10500 L of washing water cooled by a heat exchanger, and 5 kg of auxiliary agent TX-10 were beaten to obtain 8.1% coupling components Beating fluid.

[0034] Continuously pump the above-mentioned beating liquid into the tower-type first-section reactor at a flow rate of 3352kg / h, and at the same time inject 30% 2,4-dinitro-6 into the first-section coupling kettle at a flow rate of 1106kg / h - bromoaniline sulfate diazonium salt, control the reaction temperature of the first section of the coupling tank to 10-15 ° C, and carry out the coupling reaction under stirring. The output of the coupling reaction in the first section overflows to the secondary coupling kettle, and at the same time injects 30% 2,4-dinitro-6-bromoaniline diazonium sulfate into the second coupling kettle at a flow rate of 474kg / h , control the reaction temperature of the second coupling tank at 0-5°C, and carry out the coupling reacti...

Embodiment 2

[0037] Embodiment 2: 061#, diazo, coupling solution are added at one time, the yield is 98%

[0038] Such as figure 1 , beat 740kg of N-ethyl-N-cyanoethylaniline, 11500L of washing water cooled by heat exchanger, and 5kg of auxiliary agent TX-10 to obtain 6% coupling component beating liquid.

[0039] Continuously pump the above-mentioned beating liquid into the first section of the tower reactor at a flow rate of 3140kg / h, and at the same time inject 30% 2,6-dibromo-4-nitrate into the coupling kettle at a flow rate of 424kg / h Aniline sulfate diazonium salt, control the reaction temperature of the first coupling tank at 14-18°C, and carry out the coupling reaction under stirring. The output of the coupling reaction in the first section overflows to the secondary coupling kettle, and at the same time injects 30% 2,4-dinitro-6-bromoaniline diazonium sulfate into the second coupling kettle at a flow rate of 988kg / h , control the reaction temperature of the second coupling tank ...

Embodiment 3

[0043] Such as figure 1 2-methoxy-5-acetylamino-N of 995kg, N-diacetoxyethylaniline, 12500L washing water cooled by heat exchanger 1, 5kg auxiliary agent TX-10 are beaten to obtain 7.4% coupling component beating fluid.

[0044] Continuously pump the above slurry into the first-stage coupling reactor at a flow rate of 3857kg / h, and at the same time inject 30% 2,4-dinitro-6-chloroaniline into the third-stage coupling reactor at a flow rate of 870kg / h Sulfate diazonium salt solution, carry out coupling reaction under stirring, control the molar ratio of diazonium salt and coupling component in the feeding material to be 1:1.01, wherein the diazonium solution is added in a ratio of 6:3:1 in 1- 3-stage coupling kettle. The output of the first-stage coupling reaction overflows to the second-stage coupling kettle, and the output of the second-stage coupling reactor overflows to the third-stage coupling kettle. Cool the first-stage coupling kettle with low-temperature water at 5°C,...

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Abstract

The invention relates to a method for continuous coupling of dyes and reducing energy consumption, which comprises the following steps: mixing and beating coupling components, water and auxiliary agents, and continuously pumping the obtained coupling liquid into a coupling reaction kettle through a metering device; at the same time, diazo The salt solution is continuously pumped into the multi-stage coupling reaction kettle in batches through the metering device, and the feeding diazonium salt is controlled: the molar ratio of the coupling component is 1:0.95‑1.05; the cooling medium is adjusted through the heat exchange device attached to the coupling reaction kettle The flow control coupling temperature is -10°C-30°C, and the coupling reaction is carried out under stirring. After the coupling reaction is completed, the material is discharged for subsequent processing. The invention realizes continuous coupling production, realizes segmental coupling, improves production efficiency, product yield and product quality, adopts a tower reactor, and gravity guides the reaction liquid, thereby saving power consumption such as stirring.

Description

technical field [0001] The invention relates to a continuous automatic chemical production technology, in particular to a method for continuous coupling and energy consumption reduction in dye synthesis. Background technique [0002] More than 60% of the dyes in the dye industry are azo-type structures. Diazoization and coupling are necessary steps for the synthesis of this type of dye. A large amount of heat will be released in the diazo reaction and coupling reaction. It leads to the decomposition of materials, which affects product quality and yield, so cooling is required to meet production requirements. [0003] In the dye production process, due to the low stability of the diazonium salt component, a certain acidity and low temperature are required. There are side reactions such as decomposition while the coupling reaction is going on, practice shows that as the temperature rises, the side reactions intensify. The coupling process is an exothermic reaction, in order ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/085C07C245/08C07C255/24C07C253/30
Inventor 季根忠章思怡朱红旗徐万福付伟松
Owner SHAOXING UNIVERSITY
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