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Environmentally friendly preparation method of solvent red 52 dye

A solvent red and dye technology, applied in the fields of benzo-azabenzanthrone dyes, organic chemistry, etc., can solve the problems of lower production efficiency, environmental threats, long reaction time, etc., to improve production efficiency and reduce waste acid , The effect of shortening the production cycle

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

A large amount of waste acid is produced in such a process step, which poses a serious threat to the environment, and the product yield is low and the reaction time is long, which reduces the production efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The present embodiment provides a kind of environment-friendly preparation method of solvent red 52 dyes, and it comprises the following steps:

[0018] (a) Put 80 grams of 1-methylamino-4-bromoanthraquinone into a 500ml three-necked flask, followed by 2 times the amount of p-toluidine (160g), 0.3 times the amount of potassium hydroxide (24g), and 0.01 times the amount Copper sulfate (0.8g) was heated up to 100°C for condensation reaction, reacted for 8 hours to the end, then added 1.5 times the amount (120g) of methanol for isolation, filtered, washed, and dried to obtain 79 grams of intermediate;

[0019] (b) Put the intermediate into 2 times the amount (158g) of solvent DMF, add 0.5 times the amount (39.5g) of acetic anhydride, heat up to 80°C for acylation reaction, and react for 10 hours to the end;

[0020] (c) Cool the product of step (b) to 40°C, add 0.4 times the amount (31.6g) of sodium hydroxide, then raise the temperature to 100°C for ring closure reaction, ...

Embodiment 2

[0022] The present embodiment provides a kind of environment-friendly preparation method of solvent red 52 dyes, and it comprises the following steps:

[0023] (a) Put 80 grams of 1-methylamino-4-bromoanthraquinone into a 500ml three-necked flask, followed by 4 times the amount of p-toluidine (320g), 0.6 times the amount of potassium hydroxide (48g), and 0.03 times the amount Copper sulfate (2.4g) was heated to 140°C for condensation reaction, and the reaction was carried out for 4 hours to the end, then 2.5 times the amount (200g) of methanol was added for isolation, filtered, washed, and dried to obtain 76 grams of intermediate;

[0024] (b) Put the intermediate into 4 times the amount (304g) of solvent DMF, add 1 times the amount (76g) of acetic anhydride, heat up to 130°C for acylation reaction, and react for 6 hours to the end;

[0025] (c) Cool the product of step (b) to 30°C, add 0.8 times the amount (60.8g) of sodium hydroxide, then raise the temperature to 130°C for r...

Embodiment 3

[0027] The present embodiment provides a kind of environment-friendly preparation method of solvent red 52 dyes, and it comprises the following steps:

[0028] (a) Put 80 grams of 1-methylamino-4-bromoanthraquinone into a 500ml three-necked flask, followed by 3 times the amount of p-toluidine (240g), 0.4 times the amount of potassium hydroxide (32g), 0.02 times Copper sulfate (1.6g) was heated up to 120°C for condensation reaction, reacted for 6 hours to the end, then added 2 times the amount (160g) of methanol for isolation, filtered, washed, and dried to obtain 78 grams of intermediates;

[0029] (b) Put the intermediate into 3 times the amount (234g) of solvent DMF, add 0.8 times the amount (62.4g) of acetic anhydride, heat up to 100°C for acylation reaction, and react for 8 hours to the end;

[0030] (c) Cool the product of step (b) to 50°C, add 0.5 times the amount (39g) of sodium hydroxide, then raise the temperature to 120°C for ring closure reaction, and react for 6 ho...

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Abstract

The invention relates to an environmentally friendly preparation method of a solvent red 52 dye. The preparation method comprises (a) adding 1-methylamino-4-bromoanthraquinone into a reaction vessel, orderly adding p-toluidine, alkali metal hydroxide and copper sulfate into the 1-methylamino-4-bromoanthraquinone, carrying out a condensation reaction process, and carrying out separation, filtration, washing and drying to obtain an intermediate, (b) dissolving the intermediate in an organic solvent, adding acetic anhydride into the solution and heating the solution to the end point of an acylation reaction, and (c) adding alkali metal hydroxide into the product in the step b, carrying out a ring-closure reaction process until an end point, and carrying out separation, filtration, washing and drying. The preparation method is free of sulfuric acid, reduces production of a large amount of waste acid, is free of further refining and purification, shortens a production period and improves production efficiency.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to an environment-friendly preparation method of solvent red 52 dye. Background technique [0002] Solvent Red 52, Chinese name: 3-methyl-6-(p-toluidyl)-3H-dibenzo[f,ij]isoquinoline-2,7-dione, its molecular formula is: C 24 h 18 N 2 o 2 . It is a purple-red crystal with a melting point of 269-270°C and can be dissolved in water; it is dark red in concentrated sulfuric acid and produces a red precipitate after dilution; it is widely used in the coloring of various resins and plastics, such as polyacrylic resins, ABS resins , plexiglass, polyester resin, polycarbonate, etc., have the advantages of good heat resistance and light resistance, high tinting strength and bright color. [0003] The existing production process of Solvent Red 52 is to acylate 1-methylamino-4-bromoanthraquinone and close the ring to obtain 4-bromo-anthracenopyridone, which is then refined and purified by co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/18C09B5/14
CPCC07D221/18C09B5/14
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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