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 shade

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 longer, especially in the process of the intermediate potassium phenylglycinate produced, the produced waste water contains a large amount of condensation mother liquor and iron salt filtrat

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Put aniline and hydroxyacetonitrile in the condensation reactor with a molar ratio of 1:0.95, react at 65-101 degrees Celsius, after 7 hours of reaction, put all the reaction materials into the separator for static layering, Put the oil in the lower layer in the separator into the crystallization tank to solidify, until the content of aniline acetonitrile reaches more than 92%, it can be directly put into the hydrolysis reactor, and the supernatant in the separator is placed in the condensation reactor; the liquid potassium and aniline Acetonitrile is put into reactor with the metering of 1: 0.95 with molar ratio, carries out hydrolysis reaction under boiling and having reflux, and the ammonia gas that reaction discharges adopts concentration to be absorbed by the dilute sulfuric acid of 20%, until no longer in hydrolysis reactor. Until the ammonia gas is discharged, the obtained reaction materials are concentrated and dried to obtain slightly yellow powdered potassium p...

Embodiment 2

[0015] Use a metering tank to place aniline and hydroxyacetonitrile in the condensation reactor at a molar ratio of 1:1.1, react at 70-101 degrees Celsius, and after 6 hours of reaction, put all the reaction materials into the separator for static Stratification, put the lower layer oil in the separator into the crystallization tank to solidify, until the content of aniline acetonitrile reaches more than 91%, it can be directly put into the hydrolysis reactor, and then put the supernatant in the separator into the condensation reactor; The tank puts liquid potassium and aniline acetonitrile into the hydrolysis reactor in a molar ratio of 1:1:1, carries out the hydrolysis reaction under boiling and reflux, and adopts 25% dilute hydrochloric acid to absorb the ammonia gas discharged from the reaction. Until the ammonia gas is no longer discharged in the hydrolysis reactor, the obtained reaction material is finally concentrated and dried to obtain white flake potassium phenylglyci...

Embodiment 3

[0017] At normal temperature, 684 kilograms of hydroxyacetonitrile with a content of 50.1% were measured and put into a 4000 liter condensation reaction pot, then 1800 kilograms of tap water was added, and 530 kilograms of aniline with a content of 99.6% was added after stirring for 15 minutes, and after stirring for 15 minutes , open the steam valve, heat slowly, keep warm at 55-60 degrees Celsius for 1.5 hours, then raise the temperature to 85 degrees Celsius, and keep warm at this temperature for 6 hours, the condensation reaction is over, then let the reaction materials stand still for 25 minutes , put the oily aniline acetonitrile in the lower layer into the crystallization tank, break the package and measure after crystallization, and put the supernatant liquid into the storage tank to cool and use it as condensation feeding water; put 837 kilograms of aniline acetonitrile into 6000 liters of hydrolysis tank with a content of 94.5%. Reactor, and add 2000 kg of tap water, ...

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Abstract

The production method of indigo incldues the following steps: placing aniline and hydroxy-acetonitrile into a condensation reactor according to the mole ratio of 1:0.9-1:1.2, reacting for 2-8 hr. at 60-105 deg.C; placing all the reactants into separator to make stratification by standing still; placing lower layer oily material into crystallizing tank to make solidification, and when the aniline acetonitrile content is up to above 90%, directly adding the above-mentioned material into the hydrolysis reactor, placing the supernatnat fluid in the separator into the condensation reactor; placingthe liquid potassium and aniline acetonitrile into the reactor according to the mole ratio of 1:0.9-1:1.2, under the condition of boiling and refluxing making hydrolysis reaction, using acid adsorb the ammonia gas discharged by reaction.

Description

Technical field: [0001] The utility model belongs to the technical field of chemical dyes, in particular relates to an improved indigo production method, especially relates to the condensation and hydrolysis reactions of the first two parts in indigo production. 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 longer, especially in the process of the intermediate potassium phenylglycinate ...

Claims

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Application Information

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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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