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Method and device for continuously producing dyes

A technology for dyes and detection devices, applied in azo dyes, organic dyes, monoazo dyes, etc., can solve problems such as chemical ratio deviation, process medium toxicity, corrosiveness, flammability, and explosiveness, and difficulty in stirring evenly.

Active Publication Date: 2013-06-12
ZHEJIANG DIBANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In a conventional batch reactor, it is difficult to ensure that all areas of the reactor are stirred evenly, the local chemical ratio deviates from the reaction conditions, and the temperature in the reactor is uneven, which will lead to the decomposition of the diazonium salt and the occurrence of various side reactions. Resulting in poor quality of diazonium salt, low purity of dyestuff and low yield
[0005] At present, the production methods of dyestuffs in my country are still relatively backward, automatic control technology has not been practically applied in the dyestuff production process, and the comprehensive automation level of enterprises is generally low
The reason for this is that the dye production process is complicated, the operation is complicated, the process medium is toxic, corrosive, flammable and explosive, the safety requirements for production are high, and it is difficult to automatically detect the reaction end point and quality in automatic control. Feedback and other reasons
[0006] In addition, as a traditional fine chemical industry, the dye industry has a large amount of "three wastes" (waste water, waste gas, and waste residue), especially waste water pollution, which restricts the development of the entire industry.

Method used

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  • Method and device for continuously producing dyes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Put 1980kg of N,N-diethyl-3-acetamidoaniline into the beating pot of the coupling component, and beat with 20000kg of beating liquid with a mass percentage of 3% sulfuric acid to obtain the coupling component solution J, which is ready for use.

[0076] Add 420kg of nitrosyl sulfuric acid (28% content) into the batching kettle P1, turn on the frozen brine, control the temperature in the kettle at 20°C to 30°C, and slowly twist in 2,4-dinitro-6-chloroaniline ( Diazo component) 200kg is mixed to form an initiator, and then the metering of 2,4-dinitro-6-chloroaniline (diazo component) and nitrosyl sulfuric acid are controlled at 571kg / h and 1200kg / h respectively. Automatic continuous feeding, the mixed material flows from the overflow port to the tubular diazotization reactor G1 for reaction, after the polarity voltage control system E1 detects that the reaction is completed, it flows to the transfer tank Z1, and is continuously pumped by the metering pump D5 to Batching k...

Embodiment 2

[0081] Put 700kg of N,N-diethyl-3-acetamidoaniline into the beating pot of the coupling component, and beat with 15000kg of beating liquid with a mass percent of sulfuric acid of 4.5%, to obtain the coupling component solution J, ready for use.

[0082]Add 380kg of nitrosyl sulfuric acid (28% content) and 660kg of sulfuric acid into the batching kettle P1, turn on the frozen brine, control the temperature in the kettle at 0°C to 5°C, and slowly twist in 2-cyano-4-nitro 200kg of -6-bromoaniline is mixed to form an initiator. After finishing the preparation, the metering control of 2-cyano-4-nitro-6-bromoaniline (diazo component), sulfuric acid and nitrosyl sulfuric acid is 300kg / h, 990kg / h, 570kg / h for automatic continuous feeding, the mixed material flows from the overflow port to the tubular diazotization reactor G1 for reaction, after the reaction is completed by the polarity voltage control system E1, it flows to the transfer tank Z1, and then continuously pumped to the ba...

Embodiment 3

[0087] Put 2050kg of 3-(N,N-diallyl)amino-4-methoxyacetanilide in the beating pot of the coupling component, and beat with 20000kg of sulfuric acid with a mass percentage of 6% to obtain the coupling component Divide solution J and set aside.

[0088] Add 690kg of nitrosyl sulfuric acid (28% content) into the batching kettle P1, turn on the frozen brine, control the temperature in the kettle at 20°C to 30°C, slowly twist in 330kg of 2,4-dinitro-6-bromoaniline Mix and prepare the initiator. After the preparation is completed, the metering control of 2,4-dinitro-6-bromoaniline (diazo component) and nitrosyl sulfuric acid are respectively 495kg / h and 1035kg / h for continuous feeding. The mixed material flows from the overflow port to the tubular diazotization reactor G1 for reaction. After the completion of the reaction is detected by the polarity voltage control system E1, it flows to the transfer tank Z1, and then is continuously pumped to the batching tank P2 by the metering pu...

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Abstract

The invention discloses a method and a device for continuously producing dyes. The method comprises the following steps: adding diazotization reaction raw materials into an ingredient kettle, controlling temperature in the kettle, allowing the materials to flow in a tubular reactor through an overflow orifice, detecting the reaction state through an online detection device, continuously discharging the diazotization compound solution obtained through the reaction, continuously feeding the diazotization compound solution and a coupling component solution according to a specified ratio, allowing the materials to flow into the tubular reactor through the overflow orifice, detecting the reaction state through the online detection device, transferring the coupling reaction materials into a crystal transformation kettle, performing crystal transformation, and performing filter pressing to obtain a dye filter cake, wherein the filter cake mother solution and the wash water are circulated for preparing the coupling component solution. The reaction temperature, material flow and reaction state detection device are automatically subjected to interconnected control. According to the method, automatic and continuous dye production is realized, the production capacity, the product quality and yield are improved, the labor intensity and working conditions of workers are improved, the waste water, water gas and waste residue amounts in the dye production process are greatly reduced, and circular economy and cleaner production process are realized.

Description

technical field [0001] The invention relates to a method for continuously producing dyes and a device for realizing the method. Background technique [0002] The dye industry is one of the industries with the longest history in the fine chemical industry. In recent years, with the development of my country's light textile industry, the dye industry has also developed rapidly; especially since the beginning of the new century, my country's dye industry has developed more rapidly, and its output, export volume and consumption have all ranked first in the world. [0003] The preparation of general dyes consists of batch-type diazotization reactions and coupling reactions. In the diazotization reaction, the diazonium salt is easy to decompose at high temperature, and the preparation of the diazonium salt is an exothermic reaction. Therefore, the production process requires quite high heat transfer. In the coupling reaction, the diazonium salt is also easy to decompose. If the ...

Claims

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Application Information

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IPC IPC(8): C09B29/085
Inventor 徐万福傅伟松陈华祥唐智勇徐斌
Owner ZHEJIANG DIBANG CHEM
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