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Recycling production process for nigrosine

A production process and nigrosine technology, applied in the field of dyes, can solve the problems of not fully utilizing the latent heat of the gas phase and wasting heat, and achieve the effects of protecting the environment, saving steam costs, and preventing volatilization

Active Publication Date: 2015-05-13
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of an air cooler to condense does not make full use of the gas-phase latent heat of the aniline vapor and water vapor at the top of the tower, resulting in a large amount of wasted heat

Method used

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  • Recycling production process for nigrosine
  • Recycling production process for nigrosine
  • Recycling production process for nigrosine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1) Aniline and nitrobenzene are carried out condensation reaction in condensation reactor 16 under the condition that catalyst exists, obtain the nigrosine product containing excess aniline, wherein the mass ratio of aniline and nitrobenzene is 4:1, the condensation reaction The temperature is 160°C, the condensation reaction time is 4 hours, and the catalyst is FeCl 3 ;

[0061] 2) In the presence of hydrochloric acid and hot water, the nigrosine product containing excess aniline obtained in step 1) is acidified in the acidification reaction kettle 17, and then the product obtained is centrifuged by a centrifuge 18 to obtain the nigrosine product and the nigrosine product containing Aniline wastewater, wherein the reaction temperature of the acidification reaction is 90°C, and the acidification reaction time is 1 hour;

[0062] 3) if image 3 As shown, the lye and the aniline-containing wastewater with an aniline content of 4wt% are mixed by the static mixer 7, and t...

Embodiment 2

[0067] 1) Aniline and nitrobenzene are carried out condensation reaction in condensation reactor 16 under the condition that catalyst exists, obtain the nigrosine product containing excess aniline, wherein the mass ratio of aniline and nitrobenzene is 6:1, the condensation reaction The temperature is 200°C, the condensation reaction time is 6 hours, and the catalyst is FeCl 3 ;

[0068] 2) In the presence of hydrochloric acid and hot water, the nigrosine product containing excess aniline obtained in step 1) is acidified in the acidification reaction kettle 17, and then the product obtained is centrifuged by a centrifuge 18 to obtain the nigrosine product and the nigrosine product containing Aniline wastewater, wherein the reaction temperature of the acidification reaction is 100°C, and the acidification reaction time is 2 hours;

[0069] 3) if image 3 As shown, after the lye and the aniline-containing wastewater with an aniline content of 3wt% are mixed by the static mixer ...

Embodiment 3

[0074] 1) Aniline and nitrobenzene are carried out condensation reaction in condensation reactor 16 under the condition that catalyst exists, obtain the nigrosine product containing excess aniline, wherein the mass ratio of aniline and nitrobenzene is 5:1, the condensation reaction The temperature is 180°C, the condensation reaction time is 5 hours, and the catalyst is FeCl 3 ;

[0075]2) In the presence of hydrochloric acid and hot water, the nigrosine product containing excess aniline obtained in step 1) is acidified in the acidification reaction kettle 17, and then the product obtained is centrifuged by a centrifuge 18 to obtain the nigrosine product and the nigrosine product containing Aniline wastewater, wherein the reaction temperature of the acidification reaction is 95°C, and the acidification reaction time is 1.5 hours;

[0076] 3) if image 3 As shown, the lye and the aniline-containing wastewater with an aniline content of 8wt% are mixed by the static mixer 7, and...

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Abstract

The invention relates to a recycling production process for nigrosine. The recycling production process comprises the following steps: 1) condensing aniline and nitrobenzene in a condensation reaction kettle to obtain a nigrosine product containing excessive aniline; 2) acidifying the nigrosine product in an acidification reaction kettle, and centrifuging through a centrifugal machine to obtain nigrosine and aniline-containing wastewater; 3) mixing alkaline liquor and the aniline-containing wastewater through a static mixer to obtain a mixture, feeding the mixture at the tower-top of a rectifying tower, introducing steam from the tower-bottom, performing steam stripping on the aniline-containing wastewater, and processing in a sewage plant after exchanging heat of the tower-bottom wastewater through a heat exchanger; 4) introducing a gas-phase mixture of tower-top aniline water into a lithium bromide set condenser to condense; introducing 12-DEGC circulating water into the lithium bromide set condenser to form 7-DEG C circulating water for refrigerating, and converting into 12-DEG C circulating water for use after refrigerating; 5) changing the condensed gas-phase mixture into a liquid-phase mixture, condensing through the condenser, layering through a layering device, and performing the operation of step 3) on a little aniline in an upper-layer water phase in a circulating manner, and performing operation of the step 1) on lower-layer aniline phase in the circulating manner.

Description

technical field [0001] The invention relates to the technical field of dyes, in particular to a cyclic production process of nigrosine. Background technique [0002] Nigrosine is a chemical dye with strong tinting power, low dispersion, good light absorption and high color stability. Therefore, nigrosine can be used for plastic resin coloring, ink coloring, wood decoration coloring, leather, cotton, linen dyeing And finishing, metal product coloring and paint coloring and other fields. [0003] At present, the technology for preparing nigrosine is generally as follows: after aniline and nitrobenzene are catalyzed and condensed by ferric chloride, the alcohol-soluble nigrosine is obtained through acidification, water washing, filtration, and drying; the obtained alcohol-soluble nigrosine is sulfonated, isolated, Washing with water, neutralizing and drying to prepare water-soluble nigrosine; the method for preparing water-soluble nigrosine has a long production process period...

Claims

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Application Information

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IPC IPC(8): C07D241/46C09B17/02C07C211/46C07C209/86C02F9/08F25B15/06F25B27/02
CPCY02A30/274Y02B30/625C07D241/46C02F9/00C07C209/86C07C211/46C09B17/02F25B15/06F25B27/02
Inventor 陈安源王守满史红叶
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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