Method for producing indigo

A production method and technology for indigo, applied in the field of condensation and hydrolysis reaction of the first two parts in the production of indigo, can solve problems such as restricting the development of production enterprises, difficult disposal of waste residues, affecting environmental protection, etc., to simplify production processes and reduce energy consumption. , the effect of pure color light

Inactive Publication Date: 2004-01-07
上海蓝建染化有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] As can be seen from the flow chart, the flow process of indigo production is relatively long, especially in the process of making the intermediate potassium phenylglycinate, the produced waste water contains a large amount of condensation mother liquor and iron salt washing solution and a high concentration (COD in 2500-3000mg / L, producing one ton of indigo will discharge 300 tons of waste water) In addition, waste residue (iron mud) is also difficult to deal with, which affects environmental protection and restricts the development of production enterprises

Method used

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  • Method for producing indigo
  • Method for producing indigo
  • Method for producing indigo

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Put aniline and hydroxyacetonitrile in the condensation reactor with a molar ratio of 1:0.9, and react at 65 degrees Celsius. After 5 hours of reaction, all the reaction materials are put into the hydrolysis reactor, and potassium hydroxide The same molar ratio as aniline is put into the hydrolysis reactor, and the hydrolysis reaction is carried out under boiling and reflux, and the ammonia gas discharged from the reaction is absorbed by dilute sulfuric acid until the ammonia gas is no longer discharged in the hydrolysis reactor, and finally the The obtained reaction material is concentrated, dried to obtain white powdery potassium phenylglycinate, and then the potassium phenylglycinate and sodium hydroxide plus potassium hydroxide and sodium amide enter the alkali fusion oxidation reaction. About the alkali fusion oxidation reaction and the prior art The same, not described in detail here, the following

[0014] Embodiment no longer illustrates.

Embodiment 2

[0016] Use a metering tank to place aniline and hydroxyacetonitrile in the condensation reactor at a molar ratio of 1:1, react at 85 degrees Celsius, and after 4 hours of reaction, put all the reaction materials of aniline and hydroxyacetonitrile into hydrolysis Reactor, and potassium hydroxide is slowly put into the hydrolysis reactor with the same molar ratio of aniline, and the hydrolysis reaction is carried out under boiling and reflux, and the ammonia gas discharged from the reaction is absorbed by dilute hydrochloric acid until it is in the hydrolysis reactor Until the ammonia gas is no longer discharged, the obtained reaction materials are finally concentrated and dried to obtain slightly yellow powdered potassium phenylglycinate, and then the potassium phenylglycinate, sodium hydroxide, potassium hydroxide and sodium amide are put into alkali fusion oxidation reaction.

Embodiment 3

[0018] Use a metering tank to place aniline and hydroxyacetonitrile in the condensation reactor at a molar ratio of 1:1, react at 85 degrees Celsius, and after 4 hours of reaction, put all the reaction materials of aniline and hydroxyacetonitrile into hydrolysis Reactor, slowly put potassium hydroxide into the hydrolysis reactor in the same molar ratio as aniline, carry out the hydrolysis reaction under boiling and reflux, and absorb the ammonia gas discharged from the reaction with dilute phosphoric acid until it is in the hydrolysis reactor Until the ammonia gas is no longer discharged, the obtained reaction materials are concentrated and dried to obtain slightly yellow flaky potassium phenylglycinate, and then the potassium phenylglycinate, sodium hydroxide, potassium hydroxide and sodium amide are put into alkali fusion oxidation reaction.

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Abstract

The production method of indigo includes the following steps: placing aniline and hydroxyacetonitrile into condensation reactor according to the mole ratio of 1:0.9-1:1.2, reacting for 2-8 hr. at 60-105 deg.C, then placing all the materials into hydrolysis reactor, adding potassium hydroxide into the hydrolysis reactor according to the mole ratio of aniline and potassium hydroxide of 1:0.9-1:1.2,boiling and refluxing to make hydrolysis reaction, adopting acid to absorb the ammonia gas discharged by reaction, concentrating reactant material, drying to obtain white and light-yellow powder or flake potassium phenylglycinate, then making the potassium phenylglycinate, sodium hydroxide, potassium hydroxide and amino sodium undergo the process of alkali fusion oxidation reaction so as to obtain the invented product indigo.

Description

Technical field: [0001] The invention belongs to the technical field of chemical dyes, in particular to an improved production method of indigo, especially relates to the condensation and hydrolysis reactions of the first two parts in the production of indigo. Background technique: [0002] Indigo is a vat dye, mainly used for dyeing cotton and linen fabrics, especially for denim. The industrial production of indigo has a history of more than 100 years, and it has a production history of more than 30 years in my country. At present, the production of indigo in my country has been using the production process of aniline chloroacetic acid. The production method mainly includes three parts: condensation reaction, metathesis reaction and alkali fusion oxidation reaction. The process flow is as attached figure 2 . [0003] As can be seen from the flow chart, the flow process of indigo production is relatively long, especially in the process of making the intermediate potassium ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B7/00
Inventor 许寒云周娟根陈德兴
Owner 上海蓝建染化有限公司
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