A kind of preparation method of solvent blue 63 dyestuff

A dye and solvent technology, applied in the field of preparation of solvent blue 63 dye, can solve the problems of long reaction time, large amount of washing waste water, low reaction purity in the production process, and achieve the effects of short reaction time, high reaction purity and obvious crystallization

Active Publication Date: 2018-08-03
安徽清科瑞洁新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing solvent blue 63, the production process of reaction time is long, and reaction purity is low, and the amount of washing wastewater for production is large, and it is easy to cause pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The present embodiment provides a kind of preparation method of solvent blue 63 dyes, and it comprises the following steps:

[0013] (a) Add m-toluidine 120g to a 250ml reaction vessel, add 60g of 1-methylamino-4-bromoanthraquinone, 30g of sodium hydroxide and 0.4g of copper sulfate successively under stirring conditions, then heat up to 100°C, and react 7 hours to the end;

[0014] (b) Cool the product of step (a) to 60°C, then add 100ml methanol for isolation; cool to 30°C after stirring, filter and wash (wash the filter cake 2 to 5 times with 100ml methanol, then use 500ml, Washing in hot water at about 60° C.), and drying to obtain 59.2 g of the product, the yield is 92%, the purity is 99%, and the amount of washing wastewater is 600 mL.

Embodiment 2

[0016] The present embodiment provides a kind of preparation method of solvent blue 63 dyes, and it comprises the following steps:

[0017] (a) Add m-toluidine 160g to a 250ml reaction vessel, add 60g of 1-methylamino-4-bromoanthraquinone, 40g of sodium hydroxide and 0.8g of copper sulfate successively under stirring conditions, then heat up to 130°C, and react 4 hours to the end;

[0018] (b) The product of step (a) is cooled to 70°C, and then 150ml of methanol is added for isolation; after stirring, the temperature is lowered to 50°C, filtered and washed (washing the filter cake 2 to 5 times with 160ml of methanol, and then with 500ml, Washing in hot water at about 60°C, drying, and 58.5 g of the product are obtained, with a yield of 91%, a purity of 99%, and a washing wastewater volume of 650 mL.

Embodiment 3

[0020] The present embodiment provides a kind of preparation method of solvent blue 63 dyes, and it comprises the following steps:

[0021] (a) Add 150 g of m-toluidine to a 250 ml reaction vessel, add 60 g of 1-methylamino-4-bromoanthraquinone, 35 g of sodium hydroxide and 0.5 g of copper sulfate in sequence under stirring, then heat up to 120° C., and react 5 hours to the end;

[0022] (b) The product of step (a) is cooled to 65°C, and then 120ml of methanol is added for isolation; after stirring, the temperature is lowered to 35°C, filtered and washed (washing the filter cake 2 to 5 times with 150ml of methanol, and then with 300ml, Washing in hot water at about 60°C, drying, and 58.5 g of the product were obtained, with a yield of 91%, a purity of 99%, and a washing wastewater volume of 600 mL.

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PUM

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Abstract

The invention relates to an environmentally friendly preparation method of a solvent blue 63 dye. The preparation method comprises (a) adding m-toluidine into a reaction container, orderly adding 1-methylamino-4-bromoanthraquinone, an alkali metal hydroxide and a copper salt into the reaction container along with stirring, heating the mixture to 100 to 130 DEG C and carrying out a reaction process for 4 to 7 hours until a terminal point, wherein a mass ratio of 1-methylamino-4-bromoanthraquinone, m-toluidine, alkali metal hydroxide to copper salt is 6: 12-16: 3-4: 0.04-0.08, and (b) cooling the product obtained by the step a to 60-70 DEG C, then adding methanol into the product, carrying out separation, carrying out stirring, carrying out cooling to 30-50 DEG C, and carrying out filtration, washing and drying. The method has the advantages of high reaction purity, few side reactions, short reaction time, obvious crystallization, washing easiness and less washing wastewater.

Description

technical field [0001] The invention relates to a method for preparing a dye, in particular to a method for preparing a solvent blue 63 dye. Background technique [0002] Solvent blue 63, Chinese name: 1-(methylamino)-4-[(3-methylphenyl)amino]anthraquinone, its molecular formula is: C 22 h 18 N 2 o 2 , CAS No. 6408-50-0. The production process of the existing solvent blue 63 has a long reaction time, low reaction purity, and a large amount of washing wastewater for production, which is easy to cause pollution to the environment. Contents of the invention [0003] The object of the invention is to provide a kind of preparation method of solvent blue 63 dye in order to overcome the deficiencies in the prior art. [0004] In order to achieve the above object, the technical scheme adopted in the present invention is: a kind of preparation method of solvent blue 63 dye, it comprises the following steps: [0005] (a) Add m-toluidine to the reaction vessel, add 1-methylamin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C221/00C07C225/34C09B1/32
CPCC07C221/00C09B1/325C07C225/34
Inventor 陶一敏周利霞杨庆水
Owner 安徽清科瑞洁新材料有限公司
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