Recycling method for waste sulfuric acid of dye intermediate product

A dye intermediate, waste sulfuric acid technology, applied in the direction of sulfur trioxide/sulfuric acid, etc., to achieve the effect of simple method

Inactive Publication Date: 2011-10-19
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a large amount of waste sulfuric acid with a mass fraction of about 40% is produced after hydrolysis, and the main impurities are organic matter containing N, O, and S, substances with anthraquinone structure, ammonium bisulfate, tar, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Use 1,4-diamino-2,3-dicyanoanthraquinone as a raw material, oxidize it with sulfuric acid, add water and hydrolyze it to prepare the dye intermediate 1,4-diaminoanthraquinone-2,3-dicarboxyimine , filtered through a filter press, the outflowing mother liquor is dye intermediate waste sulfuric acid (mass fraction is 40 ± 2% sulfuric acid), the appearance is red and black, it is pumped into the settling tank for natural cooling and sedimentation, after overnight , the inorganic salt (mainly ammonium bisulfate) dissolved in the waste sulfuric acid is precipitated, and the settled waste sulfuric acid solution is pumped into the suction filter tank for filtration, and the precipitated inorganic salt is removed to obtain orange-red clear waste sulfuric acid, which is then used Pump it into the sulfuric acid high-efficiency concentration device for vacuum dehydration and concentration until sulfuric acid with a mass fraction of 90-95% is obtained. The concentrated sulfuric acid ...

Embodiment 2

[0018] It is basically the same as in Example 1, except that: at a temperature of 150-160° C., 30% hydrogen peroxide is added dropwise to the oxidation kettle until the material in the oxidation kettle becomes colorless, clear and transparent.

Embodiment 3

[0020] It is basically the same as in Example 1, the difference is: feed ozone into the oxidation kettle until the material in the oxidation kettle becomes colorless, clear and transparent.

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PUM

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Abstract

The invention relates to a recycling method for waste sulfuric acid of a dye intermediate product, which comprises the following steps of: recovering waste sulfuric acid with a mass fraction of 40+ / -2%, settling, filtering, dewatering and concentrating, then oxidizing with an oxidant (oxyful or ozone) at 80-200 DEG C to obtain colorless transparent sulfuric acid, removing exhaust gases generated during the oxidation process under negative pressure, cooling to room temperature, storing, and directly using for producing an inorganic fertilizer, a sulfate, or a water treatment agent; or mixing the oxidized sulfuric acid with fuming sulfuric acid or sulfur trioxide to obtain 98wt% sulfuric acid, storing, and reusing for synthesizing a dye intermediate product or producing a sulfate. The waste sulfuric acid is acquired by oxidizing 1,4-diamino-2,3-dicyano anthraquinone as a raw material with sulfuric acid, then hydrolyzing to obtain a dye intermediate product namely 1,4-diaminoanthraquinone-2,3-dicarboxyl imine and hydrolyzing the dye intermediate product. The recycling method is simple and practical, the recovery rate of the waste sulfuric acid of the dye intermediates is up to 96.9%, and the recovered sulfuric acid can be used as fresh industrial sulfuric acid.

Description

technical field [0001] The invention relates to a method for recycling waste sulfuric acid used as a dye intermediate. Specifically, the invention relates to a method for using 1,4-diamino-2,3-dicyanoanthraquinone as a raw material, which is oxidized with sulfuric acid and then hydrolyzed. A method for recycling waste sulfuric acid formed from the preparation of dye intermediate 1,4-diaminoanthraquinone-2,3-dicarboxyimine. Background technique [0002] Disperse Blue 60 is a very important blue disperse dye. 1,4-diaminoanthraquinone-2,3-dicarboxyimine is a dye intermediate of disperse blue 60, and its chemical formula is shown in formula I. The dye intermediate for preparing disperse blue 60 is usually prepared from 1,4-diamino-2,3-dicyanoanthraquinone as raw material, oxidized with sulfuric acid, and then hydrolyzed with water. The disadvantage of this method is that a large amount of waste sulfuric acid with a mass fraction of about 40% is produced after hydrolysis, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/90
Inventor 吴传龙
Owner JIANGSU YABANG DYE
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