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Novel process for controlling waste residue and recycling resources in 1-anthraquinone production

A resource recovery and aminoanthraquinone technology, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of waste residue accumulation and no good recycling methods, so as to improve efficiency and eliminate hidden dangers of environmental pollution Effect

Active Publication Date: 2010-09-22
YANCHENG OUHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, due to the lack of good recycling methods, resulting in a large amount of waste accumulation

Method used

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  • Novel process for controlling waste residue and recycling resources in 1-anthraquinone production
  • Novel process for controlling waste residue and recycling resources in 1-anthraquinone production
  • Novel process for controlling waste residue and recycling resources in 1-anthraquinone production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A new process for 1-aminoanthraquinone production waste residue treatment and resource recovery, the method includes two steps:

[0014] A) Reacting the waste residue with an aqueous solution of sodium sulfite to convert the components containing β-nitroanthraquinone in the waste residue into water-soluble substances, which are removed by filtration. After the filter cake is dried, it is used for the next operation;

[0015] B) the dried filter cake reacts with an organic amine in N, N-dimethylformamide at high temperature and cools and crystallizes. After the crystals are collected, a product containing 88% of 1-nitroanthraquinone can be obtained, which The quality is better than crude nitroanthraquinone obtained by direct nitration of anthraquinone.

[0016] Wherein, the component containing β-nitroanthraquinone includes 2-nitroanthraquinone, 1,6-; 1,7-; 2,6-; 2,7-four dinitroanthraquinones. They can all be removed by reacting with sodium sulfite solution to generat...

Embodiment 2

[0027] A new process for 1-aminoanthraquinone production waste residue treatment and resource recovery, the method includes two steps:

[0028] A) Reacting the waste residue with an aqueous sodium sulfite solution to convert the nitroanthraquinone-containing components in the waste residue into water-soluble substances, which are removed by filtration. After the filter cake is dried, it is used for the next operation;

[0029] B) the dried filter cake reacts with an organic amine in N, N-dimethylformamide at high temperature and cools and crystallizes. After the crystals are collected, a product containing 88% of 1-nitroanthraquinone can be obtained, which The quality is better than crude nitroanthraquinone obtained by direct nitration of anthraquinone.

[0030] Wherein, the component containing β-nitroanthraquinone includes 2-nitroanthraquinone, 1,6-; 1,7-; 2,6-; 2,7-four dinitroanthraquinones. They can all be removed by reacting with sodium sulfite solution to generate wat...

Embodiment 3

[0041] A new process for 1-aminoanthraquinone production waste residue treatment and resource recovery, the method includes two steps:

[0042] A) Reacting the waste residue with an aqueous sodium sulfite solution to convert the nitroanthraquinone-containing components in the waste residue into water-soluble substances, which are removed by filtration. After the filter cake is dried, it is used for the next operation;

[0043] B) the dried filter cake is reacted with an organic amine in N, N-dimethylformamide at high temperature and crystallized by cooling. After the crystals are collected, a product containing 88% of 1-nitroanthraquinone can be obtained, which The quality is better than crude nitroanthraquinone obtained by direct nitration of anthraquinone.

[0044] Wherein, the component containing β-nitroanthraquinone includes 2-nitroanthraquinone, 1,6-; 1,7-; 2,6-; 2,7-four dinitroanthraquinones. They can all be removed by reacting with sodium sulfite solution to generat...

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Abstract

The invention discloses a process for controlling waste residue and recycling resources in 1-anthraquinone production, which comprises the following steps that: (1) waste residue, sodium sulfite and water are mixed and react so as to convert components of the waste residue which contain Beta-nitroanthraquinone into water-soluble substances to be removed by filtration, and a filter cake is dried for the next-step operation; and (2) the dried filter cake reacts with an organic amine, is cooled and crystallized in N, N-dimethylformamide, the 1,5-, 1,8-dinitro-anthraquinone components are converted into organic amines, cooled and crystallized, removed together with the unreacted anthraquinone, and the product which contains 1-mitro-anthraquinone 88 percent is obtained after the crystal is collected. The process for controlling waste residue and recycling resources in 1-anthraquinone production effectively treats a large amount of solid waste residue produced in a solvent method 1-amino-anthraquinone process, obtains high-quality 1-nitro-anthraquinone, and can further process and produce 1-anthraquinone or other products.

Description

technical field [0001] The invention belongs to the field of dye intermediate production, and in particular relates to a method for refining treatment and resource recovery of 1-aminoanthraquinone production waste residue by solvent method. Background technique [0002] 1-Aminoanthraquinone is an important dye intermediate. At present, the national annual output has exceeded 10,000 tons, which still cannot meet the market demand, and the production capacity needs to be further expanded. 1-Aminoanthraquinone is produced by the solvent method, that is, anthraquinone reacts with mixed acid in an organic solvent to form a mixture of 1-nitroanthraquinone and other nitroanthraquinones (referred to as "crude nitrate"), and the crude nitrate is passed through N, N - High-purity 1-nitroanthraquinone (referred to as "fine nitrate") is obtained after dimethylformamide (DMF) solvent recrystallization and purification. The refined nitrate is reduced by sodium sulfide to obtain the finis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/47C07C201/16
Inventor 曹阳黄都都应会荣杨思卫
Owner YANCHENG OUHUA CHEM IND
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