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Clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid

A diaminoanthraquinone, clean production technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of wasting energy, dark color, and high COD in wastewater, and achieve the effects of reducing costs, solving high COD, and reducing waste residue discharge.

Inactive Publication Date: 2015-04-22
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The disadvantages of the above-mentioned production method are as follows: firstly, the waste residue generated by filtering and removing impurities in this method needs to be landfilled; secondly, a large amount of waste water produced after acidification treatment in this method needs to be discharged, and this part of waste water has high COD, deep color, and A large amount of water-soluble substances exist, and three, the method adopts negative pressure dehydration and wastes energy

Method used

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  • Clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid
  • Clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0037]Add 300g of o-dichlorobenzene and 40g of 1,4-diaminoanthraquinone leuco into a 500mL flask, slowly add 91g of chlorosulfonic acid at 40°C, keep the vacuum at -0.005MPa during the dropping process, and slowly raise the temperature after the dropping Incubate at 140°C for 3.5h, keep the vacuum at -0.005MPa during the reaction, use liquid chromatography to detect that the remaining amount of 1,4-diaminoanthraquinone ≤ 2% is the end point of sulfonation, cool down, and dilute with 400mL of water to obtain The material is neutralized with liquid caustic soda, and the solvent o-dichlorobenzene is evaporated by raising the temperature. The evaporated solvent can be directly reused as the reaction solvent. During the distillation process, water can be added appropriately according to the reaction system to maintain the fluidity of the material. After the condensation tube is free of oil When the beads come out, the distillation is stopped, and the impurities are filtered out whil...

Embodiment 2

[0041] Add 300g of o-dichlorobenzene and 40g of 1,4-diaminoanthraquinone leuco into a 500mL flask, slowly add 93g of chlorosulfonic acid at 40°C, keep the vacuum at -0.005MPa during the dropping, and slowly raise the temperature after the dropping Incubate at 140°C for 3.5h, keep the vacuum at -0.005MPa during the reaction, use liquid chromatography to detect that the remaining amount of 1,4-diaminoanthraquinone ≤ 2% is the end point of sulfonation, cool down, and dilute with 400mL of water to obtain The material is neutralized with liquid caustic soda, and the solvent o-dichlorobenzene is evaporated by raising the temperature. The evaporated solvent can be directly reused as the reaction solvent. During the distillation process, water can be added appropriately according to the reaction system to maintain the fluidity of the material. After the condensation tube is free of oil When the beads come out, the distillation is stopped, and the impurities are filtered out while it is...

Embodiment 3

[0045] The other conditions are the same as in Example 2, except that the system vacuum is kept at -0.002MPa during the addition of chlorosulfonic acid and the reaction process.

[0046] The total yield of the finally obtained sulfonated product filter cake is 96%, and the content is greater than 98%. 2.0% of 1,4-diaminoanthraquinone can be recovered, and 1.2% of sulfonic acid filter cake can be recovered. The amount of high-concentration wastewater obtained by stripping is reduced to 75ml, and the solvent is removed and then directly incinerated. The low-COD waste water (COD is 400mg / L, COD removal rate up to 96%) obtained by extraction can be directly used in the next-level biodegradation process without further removal of organic matters.

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Abstract

The invention discloses a clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid. The process comprises the following steps of in the presence of o-dichlorobenzene as a solvent, oxidizing and sulfonating a 1,4-diaminoanthraquinone leuco compound by virtue of chlorosulfonic acid; after the reaction is completed, neutralizing, removing the solvent and filtering to obtain waste residue; pulping the waste residue and water, filtering to obtain a filter cake and drying the filter cake for reuse; acidifying filtrate, filtering and washing the filter cake which is 1,4-diaminoanthraquinone-2-sulfonic acid; carrying out extraction and reverse extraction on the filtrate to obtain low-COD wastewater and recycling the solvent. After the implementation of the method disclosed by the invention, the waste residue is fully reused and the emissions of waste residue are greatly reduced; meanwhile, the conversion rate of the 1,4-diaminoanthraquinone leuco compound is increased and the cost of sulfonic acid is decreased. The difficult problems of high COD and dark chromaticity of acidified wastewater are solved, the obtained wastewater can be directly subjected to subsequent treatment, and discoloration and COD removal treatment are not needed.

Description

technical field [0001] The invention belongs to the technical field of production and preparation of organic dyes, and in particular relates to a clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid. Background technique [0002] C.I. Disperse Blue 60 (CAS No.: 12217-80-0) is a very important variety of disperse dyes, and its structure is shown in the following formula: [0003] [0004] C.I. Disperse Blue 60 generally uses 1,4-diaminoanthraquinone and γ-methoxypropylamine as raw materials. First, 1,4-diaminoanthraquinone is chlorinated, sulfonated, cyanated, ring-closed, and finally combined with γ- Methoxypropylamine condensation products. After filtering, grinding and drying, the finished product is obtained. [0005] In the above sulfonation process, 1,4-diaminoanthraquinone leuco body is used as raw material, o-dichlorobenzene is used as solvent, chlorosulfonic acid is used as sulfonating agent, low temperature dropwise, high temperature sulfonation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/53C07C303/08
Inventor 叶华明李茂陈庆林
Owner ZHEJIANG RUNTU INST
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