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Synthesis method of solvent blue 122

A synthesis method and solvent technology, applied in the synthesis field of solvent blue 122, can solve problems such as difficult industrial production operation, poor water solubility of raw materials, long reaction time, etc., achieve good economic and environmental benefits, increase yield, and improve conversion rate Effect

Active Publication Date: 2019-11-26
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

During the reaction process of this process, due to the poor water solubility of the raw materials, it is easy to form agglomerates and affect the reaction.
The reaction time is long, special equipment is required, the reaction requirements are high, and it is not easy for industrial production operation

Method used

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  • Synthesis method of solvent blue 122
  • Synthesis method of solvent blue 122

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preparation example Construction

[0020] A kind of synthetic method of solvent blue 122 of the present invention comprises the steps:

[0021] (a) Add water, hydrochloric acid, and p-aminoacetanilide to the reaction vessel, and stir evenly at 40-50°C for 25-35 minutes to obtain the first mixed solution. The molar ratio of p-aminoacetanilide to hydrochloric acid is 1.05-1.25 :1;

[0022] (b) Add 1,4-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone leuco, water, and catalyst CJ to another reaction vessel to obtain a second mixed solution. Catalyst CJ is based on one or several Alumina is a carrier, and palladium is used as a catalyst for active components; the molar ratio of the total feed mole of 1,4-dihydroxy anthraquinone and 1,4-dihydroxy anthraquinone leucosome to hydrochloric acid is 1.05~1.25:1, The ratio of the total mass of 1,4-dihydroxyanthraquinone and 1,4-dihydroxyanthraquinone leuco to the mass of catalyst CJ is 100:2-6;

[0023] (c) Slowly add the first mixed solution to the second mixed soluti...

Embodiment 1

[0028] The present embodiment provides a kind of synthetic method of solvent blue 122, and it comprises the following steps:

[0029] (a) Add 30ml of hot water, 20g of 30% hydrochloric acid, and 30g of p-aminoacetanilide in sequence in a four-neck flask, heat up and stir, and maintain the temperature at 40°C to 50°C for 30min to fully dissolve the p-aminoacetanilide to obtain the first mixture solution;

[0030] (b) In another four-necked flask, add 80ml of water, 28g of 1,4-dihydroxyanthraquinone, 8g of leuco 1,4-dihydroxyanthraquinone, and 0.8g of catalyst CJ to obtain a second mixed solution;

[0031] (c) Warm up and stir the second mixed solution to 85-90°C, drop the first mixed solution therein, finish adding dropwise in 3-4 hours, keep it for 12 hours, lower the temperature, and detect the reaction end point by HPLC; Filtrate hot, wash the filtered solid with hot water until neutral, and then dry the obtained solid to obtain 53.6 g of navy blue solvent blue 122 powder, ...

Embodiment 2

[0033] The present embodiment provides a kind of synthetic method of solvent blue 122, and it is basically the same as that in embodiment 1, and difference is, in step (b), add 25.92g p-aminoacetanilide, finally after filtering, wash with hot water to neutrality, The filter cake was dried to obtain 53.1 g of solvent blue 122 powder, with a content of 93.45% and a yield of 95.16%.

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Abstract

The invention relates to a synthesis method of solvent blue 122. The method comprises the following steps: a, adding water, hydrochloric acid and p-aminoacetanilide into a reaction container, and uniformly stirring to obtain a first mixed solution; b, adding 1,4-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone leuco body, water and a catalyst CJ into another reaction container to obtain a secondmixed solution, wherein the catalyst CJ is a catalyst adopting one or more kinds of aluminum oxide as a carrier and palladium as an active ingredient; and c, slowly dropwise adding the first mixed solution to the second mixed solution for a condensation reaction to obtain the solvent blue 122. The hydrochloric acid and p-aminoacetanilide are used to prepare the balanced and stable solution, and the balanced and stable solution is dropwise added, so the reaction rate and the dissolving effect can be well controlled; water is used as a solvent, so that the operation environment is improved, thereaction period is simplified, the productivity is improved, and the cost is saved; and the novel catalyst CJ greatly reduces the pollution of sewage to water, improves the conversion rate of the product, and reduces the reaction temperature and pressure.

Description

technical field [0001] The present invention relates to a kind of synthesis method of dye, in particular to a kind of synthesis method of solvent blue 122. Background technique [0002] Solvent blue 122 is an important solvent dye, also known as transparent blue R, transparent blue 2RA, its chemical name is N-[4-[(4-hydroxyanthraquinone-1-yl)amino]phenyl]acetamide, The English name is Solvent Blue 122, and the molecular formula is C 22 h 16 N 2 o 4 , the molecular weight is 372.37, and the CAS number is 67905-17-3. The appearance of this product is purple-black powder, insoluble in water, soluble in organic solvents such as benzene, chlorobenzene, xylene, DMF, etc., it appears dark green in concentrated sulfuric acid, and produces olive to red light blue precipitate after dilution. Solvent blue 122 can be used in the coloring of various resin plastics, such as polyacrylic resin, ABS resin, polystyrene, plexiglass, polyester resin, polycarbonate, etc., to obtain red ligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/514B01J23/44
CPCB01J23/44C09B1/5145
Inventor 周利霞王伟张标来杨庆水
Owner 安徽清科瑞洁新材料有限公司
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