Preparation method of 1-amino-4(ethylamino) anthraquinone-2-carbonitrile

A technology of ethyl amino and amino, which is applied in the field of dye preparation, can solve the problems of difficult product quality stability, many side reactions, and three wastes, etc., and achieve the effect of improving utilization rate, shading and dyeing performance

Active Publication Date: 2017-12-22
宁波德欣科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The existing technology includes four reaction steps of sulfonation, chlorination, amination, and cyanation. The process is long, with many side reactions and many wastes. However, bromine is produced by bromination, and then through amination and cyanation, although it reduces According to the reaction steps, the quality of bromic acid, such as impurity content, solubility in water and the content of insoluble matter, etc. have a great influence on the yield of condensation reaction; the impurities brought in bromic acid also enter the product together, making the product The quality is difficult to be stable, and generally speaking, the brilliance of the prepared Disperse Blue 359 is generally low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing 1-amino-4(ethylamino)anthraquinone-2-carbonitrile. The preparation steps include: (1) Preparation of rare earth adsorbent: in parts by weight, 100 parts of silica gel are washed and dried, and 7 Parts of mercaptopropyltriethoxysilane, 0.04 parts of 2,5-bis(4-bromophenyl)-1,1-dimethyl-3,4-diphenylsilole, 2 parts of triethylamine, 500 Parts of toluene, reacted at 70°C for 18 hours, filtered, washed, and dried to obtain mercaptosilanized silica gel, then added 500 parts of water, added 2 parts of cerous chloride, 1 part of n-butyl mercaptopropionate, and 0.03 parts of o-phenanthroline , refluxed under mechanical stirring for 28 hours; after stopping the reaction, filter, wash and dry to obtain the rare earth adsorbent.

[0027] (2) Purification of bromic acid

[0028] According to parts by weight, put 100 parts of rare earth adsorbent into the adsorption column, and add the bromic acid aqueous solution with a mass percentage concentration of 8 at a ...

Embodiment 2

[0034] A method for preparing 1-amino-4(ethylamino)anthraquinone-2-carbonitrile. The preparation steps include: (1) Preparation of rare earth adsorbent: in parts by weight, 100 parts of silica gel are washed and dried, and 5 Parts of mercaptopropyltriethoxysilane, 0.01 part of 2,5-bis(4-bromophenyl)-1,1-dimethyl-3,4-diphenylsilole, 1 part of triethylamine, 300 Parts of toluene, reacted at 50°C for 10 hours, filtered, washed, and dried to obtain mercaptosilanized silica gel, then added 300 parts of water, added 1 part of cerous chloride, 0.5 part of n-butyl mercaptopropionate, and 0.01 part of o-phenanthroline , refluxed under mechanical stirring for 24 hours; after stopping the reaction, filtered, washed and dried to obtain the rare earth adsorbent.

[0035] (2) Purification of bromic acid

[0036] According to parts by weight, put 100 parts of rare earth adsorbent into the adsorption column, add the aqueous solution of bromic acid with a mass percentage concentration of 5 at...

Embodiment 3

[0042] A method for preparing 1-amino-4(ethylamino)anthraquinone-2-carbonitrile. The preparation steps include: (1) Preparation of rare earth adsorbent: in parts by weight, 100 parts of silica gel are washed and dried, and 15 Parts of mercaptopropyltriethoxysilane, 0.1 part of 2,5-bis(4-bromophenyl)-1,1-dimethyl-3,4-diphenylsilole, 5 parts of triethylamine, 1000 Parts of toluene, reacted at 80°C for 24 hours, filtered, washed, and dried to obtain mercaptosilanized silica gel, then added 1000 parts of water, added 5 parts of cerous chloride, 2 parts of n-butyl mercaptopropionate, and 0.1 part of o-phenanthroline , refluxed under mechanical stirring for 36 hours; after stopping the reaction, filter, wash and dry to obtain the rare earth adsorbent.

[0043] (2) Purification of bromic acid

[0044] According to parts by weight, put 100 parts of rare earth adsorbent into the adsorption column, and add the bromic acid aqueous solution with a mass percentage concentration of 20 at a...

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PUM

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Abstract

The invention provides a preparation method of 1-amino-4(ethylamino) anthraquinone-2-carbonitrile. The method comprises steps as follows: purified bromamine acid, copper sulfate, ethylamine and sodium carbonate in a certain ratio are subjected to a reaction at the temperature of about 60-90 DEG C for 4-10 h, a 1-amino-4 ethylamino-anthraquinone-2-sodium sulfonate solution is obtained, excessive ethylamine is recovered through distillation, water and activated carbon are added, bromine-containing impurities are adsorbed with a rare earth adsorbent, and a filtrate containing 1-amino-4 ethylamino-anthraquinone-2-sodium sulfonate is pumped into a cyaniding kettle. In the cyaniding kettle provided with a tail gas absorption device, sodium carbonate with a certain proportion and a sodium cyanide water solution with the mass percentage concentration being 20%-40% are subjected to a reaction at the temperature of 85-105 DEG C for 4-10 hours, filtration, washing and drying are performed, and 1-amino-4(ethylamino) anthraquinone-2-carbonitrile is obtained.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to a preparation method of 1-amino-4(ethylamino)anthraquinone-2-carbonitrile. Background technique [0002] Disperse Blue 359, whose chemical name is 1-amino-4(ethylamino)anthraquinone-2-carbonitrile, is a disperse dye with anthraquinone structure, with red and blue shades, and is mainly used for thermal transfer printing of polyester fabrics. [0003] CN106748902A discloses a synthesis method of 1-amino-4 (ethylamino)-9,10-anthraquinone-2-sulfonic acid, the steps are as follows: first, water, 1,4-dihydroxyanthraquinone-2-sulfonic acid 1. Concentrated hydrochloric acid is put into the container, stirred and heated up, and zinc powder is added for reduction reaction. After the reaction, 70wt% ethylamine and 30wt% ammonia water are respectively added dropwise. After that, the temperature is lowered to release the pressure, air is introduced to carry out the oxidation reaction, and fin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/00C07C255/58C07C303/44C07C309/53B01J20/22B01J20/30
Inventor 杨卫统郭志毅屠仁华颜福池赵汉安谷灿波
Owner 宁波德欣科技有限公司
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