Environmentally friendly preparation method of solvent blue 63 dye

A dye and solvent technology is applied in the field of environmental protection preparation of solvent blue 63 dye, which can solve the problems of long reaction time, large amount of washing wastewater and low reaction purity in the production process, and achieve short reaction time, high reaction purity and obvious crystallization. Effect

Active Publication Date: 2017-05-31
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 environment-friendly preparation method of solvent blue 63 dyestuff, and it comprises the following steps:

[0013] (a) Add 120g of m-toluidine 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 raise the temperature 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; after stirring, cool down to 30°C, filter and wash (use 100ml methanol to wash the filter cake 2~5 times, then use 500ml, Washing with hot water at about 60°C,) and drying to obtain 59.2g of the product, with a yield of 92%, a purity of 99%, and a washing wastewater volume of 600mL.

Embodiment 2

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

[0017] (a) Add 160g of m-toluidine 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 raise the temperature to 130°C, and react 4 hours to the end;

[0018] (b) Cool the product of step (a) to 70°C, then add 150ml methanol for isolation; after stirring, cool down to 50°C, filter and wash (use 160ml methanol to wash the filter cake 2~5 times, then use 500ml, Washing with hot water at about 60°C), and drying to obtain 58.5 g of the product, 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 environment-friendly preparation method of solvent blue 63 dyestuff, and it comprises the following steps:

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

[0022] (b) Cool the product of step (a) to 65°C, then add 120ml methanol for isolation; after stirring, cool down to 35°C, filter and wash (use 150ml methanol to wash the filter cake 2~5 times, then use 300ml, Washing with hot water at about 60°C,) and drying to obtain 58.5g of the product, with a yield of 91%, a purity of 99%, and a washing wastewater volume of 600mL.

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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 preparation method of a dye, in particular to an environment-friendly preparation method of 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 an environmentally friendly 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 solution adopted in the present invention is: a kind of environment-friendly preparation method of solvent blue 63 dye, it comprises the following steps: [000...

Claims

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Application Information

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Patent Type & Authority Applications(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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