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

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...

Examples

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...

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...

Examples

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...