Continuous coupling and energy utilization method for dyes

A dye and energy technology, used in azo dyes, organic dyes, monoazo dyes, etc., can solve the problems of large consumption of cold and heat energy, low production efficiency, and inability to effectively use it, so as to reduce waste water discharge and improve production efficiency. , to achieve the effect of reuse and resource utilization

Active Publication Date: 2012-11-28
ZHEJIANG LONGSHENG GROUP +1
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of low production efficiency, large consumption of cold and heat energy and ineffective utilization in the existing batch coupling process, the present invention provides a method for continuous coupling production and energy comprehensive utilization

Method used

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  • Continuous coupling and energy utilization method for dyes

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Experimental program
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Effect test

Embodiment 1

[0019] See flow chart figure 1 .

[0020] Beat 995kg of 2-methoxy-5-acetylamino-N,N-diacetoxyethylaniline, 12500L of washing water cooled by heat exchanger 1, and 5kg of auxiliary agent TX-10 to obtain 7.4 % of coupling components beating fluid.

[0021] 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 folded mole ratio of diazonium salt and coupling component in the feed to 1:1.01, and add 1 to 3 Grade 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. The reaction temperature of each coupling kettle is controlled at 0-5°C.

[0022] The output of the three...

Embodiment 2

[0026] Beat 926kg of 3-acetamido-N,N-diethylaniline, 10500L of washing water cooled by heat exchanger 1, and 5kg of auxiliary agent TX-10 to obtain 8.1% beating liquid of coupling components.

[0027] Continuously pump the above-mentioned beating liquid into the first-stage coupling reactor at a flow rate of 3352kg / h, and at the same time inject 30% 2,4-dinitro-6-bromoaniline sulfuric acid into the coupling reactor at a flow rate of 1580kg / h Nitrogen salt, carry out the coupling reaction under stirring, control the molar ratio of diazonium solution and coupling solution to 1:1.03, and the ratio of diazonium solution added in the secondary coupling tank is 7:3. The output of the first-stage coupling reaction overflows to the second-stage coupling kettle, and the reaction temperature of each coupling kettle is controlled at 0-5°C.

[0028] The discharge of the secondary coupling kettle is heat-exchanged with the washing water from the washing water buffer tank 2 in the heat exch...

Embodiment 3

[0031] Embodiment 3: O61#, diazo, coupling liquid add once, yield 98%

[0032] Beat 740kg of N-ethyl-N-cyanoethylaniline, 11500L of washing water cooled by heat exchanger 1, and 5kg of auxiliary agent TX-10 to obtain a 6% beating liquid of the coupling component.

[0033] Continuously pump the above-mentioned beating liquid into the first-stage coupling reactor at a flow rate of 3140kg / h, and inject 30% 2,6-dibromo-4-nitroaniline sulfuric acid into the coupling reactor at a flow rate of 1412kg / h Nitrogen salt, carry out the coupling reaction under stirring, control the molar ratio of the diazonium solution and the coupling solution to 1:1.04, and add all the diazo solution into the first-stage coupling reaction 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. The reaction temperature of each coupling kettle is controlled at 0-5...

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Abstract

The invention provides a continuous coupling and energy utilization method for dyes. The method comprises the following steps of: respectively continuously pumping coupling component suspension liquid and diazo liquid into a coupling reaction kettle by a metering device; adjusting flow of cooling water and controlling the coupling temperature to be between -10 and 20 DEG C; performing coupling reaction on the coupling component suspension liquid and the diazo liquid under the stirring condition; and discharging after the coupling reaction is completed and enabling the mixture to enter a thermal transfer crystal pot after the mixture is subjected to the heat exchange. The continuous coupling and energy utilization method has the beneficial effects that the continuous coupling production is realized, so that the production efficiency and the yield are improved, and the product quality is improved and stabilized; the coupling product is subjected to multi-level heat exchange, so that the cold energy and the concentrated condensed water heat energy of the coupling material can be effectively utilized; mother liquid is neutralized, concentrated and crystallized, and ammonium sulfate is recovered, so that the heat energy of the concentrated condensed water is subjected to heat exchange and recovered; the condensed water subjected to temperature reduction is used for washing a filter cake; and the washing water is used for pulping the coupling component, so that the recycling and reclamation of the wastewater are realized, and the drainage of the waste water is greatly reduced.

Description

(1) Technical field [0001] The invention relates to a continuous automatic chemical production technology, in particular to a method for continuous coupling and energy utilization in dye synthesis. (2) Background technology [0002] In the process of dye production, almost all chemical reaction processes need to be controlled at a certain temperature. In order to achieve and maintain the required temperature, the reaction materials often need to be heated or cooled to a certain temperature, and the heating and cooling process consumes energy. . 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 actual production process, the couplin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/085C09B29/01
Inventor 何旭斌陶建国孟明朱敬鑫杨伟军杨日升孟福庆
Owner ZHEJIANG LONGSHENG GROUP
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