Preparation method of 1-hydroxy-4-(p-toluidino)anthraquinone

A technology of toluidine anthracene and p-toluidine, which is applied in the field of preparation of 1-hydroxy-4-p-toluidine anthraquinone, which can solve the problem of difficult removal of anionic surfactants, additional burden of sewage treatment, harsh condensation reaction conditions, etc. problem, achieve the effect of avoiding difficult separation, stable reaction and avoiding side reactions

Inactive Publication Date: 2017-12-22
宁波德欣科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, boric acid is used as the condensation reaction catalyst in the prior art, the product purity is low, no boric acid or other condensing agents are used, the

Method used

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  • Preparation method of 1-hydroxy-4-(p-toluidino)anthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of 1-hydroxyl-4-p-toluidino anthraquinone, characterized in that the preparation steps include:

[0024] (1) Preparation of condensation catalyst: In parts by weight, swell 100 parts of thiourea resin in 700 parts of boric acid, soak for 3 hours, filter, wash with deionized water until PH = 7, add 3 parts of 2-hydroxy-5-sulfo Benzoic acid, 0.04 parts of neodymium acetate, 0.03 parts of 5,6-diamino-1,10-phenanthroline, 2 parts of 2-fluoroisonicotinic acid, stirred and reacted at 30°C for 7h, the reaction was completed, filtered , dried to obtain the condensation catalyst;

[0025] (2) Preparation of 1-hydroxy-4-p-toluidine anthraquinone:

[0026] In parts by weight, 100 parts of 1,4-dihydroxyanthraquinone, 90 parts of p-toluidine, 500 parts of diethylene glycol dibutyl ether, and 70 parts of condensation catalyst are put into the reactor, and the system gradually heats up to carry out the reaction. The reaction temperature is 110°C, and the reactio...

Embodiment 2

[0028] A preparation method of 1-hydroxyl-4-p-toluidino anthraquinone, characterized in that the preparation steps include:

[0029] (1) Preparation of condensation catalyst: In parts by weight, swell 100 parts of thiourea resin in 500 parts of boric acid, soak for 1 hour, filter, wash with deionized water until pH = 7, add 1 part of 2-hydroxy-5-sulfo Benzoic acid, 0.01 part of neodymium acetate; 0.01 part of 5,6-diamino-1,10-phenanthroline, 1 part of 2-fluoroisonicotinic acid, stirred and reacted at 20°C for 10h, the reaction was completed, filtered, drying to obtain a condensation catalyst;

[0030] (2) Preparation of 1-hydroxy-4-p-toluidine anthraquinone:

[0031] In parts by weight, 100 parts of 1,4-dihydroxyanthraquinone, 80 parts of p-toluidine, 300 parts of tetraglyme, and 30-100 parts of condensation catalyst are put into the reactor, and the system gradually heats up to react. The temperature is 100°C, and the reaction time is 20h. After the reaction, the product i...

Embodiment 3

[0033] A preparation method of 1-hydroxyl-4-p-toluidino anthraquinone, characterized in that the preparation steps include:

[0034] (1) Preparation of condensation catalyst: In parts by weight, swell 100 parts of thiourea resin and soak in 1000 parts of boric acid for 5 hours, filter, wash with deionized water until PH = 7, add 10 parts of 2-hydroxy-5-sulfo Benzoic acid, 0.1 parts of neodymium acetate; 0.1 parts of 5,6-diamino-1,10-phenanthroline, 5 parts of 2-fluoroisonicotinic acid, stirred and reacted at 50°C for 5h, the reaction was completed, filtered, drying to obtain a condensation catalyst;

[0035] (2) Preparation of 1-hydroxy-4-p-toluidine anthraquinone:

[0036] In parts by weight, 100 parts of 1,4-dihydroxyanthraquinone, 150 parts of p-toluidine, 800 parts of diphenyl ether, and 100 parts of condensation catalyst are put into the reactor, and the system gradually heats up to react, and the reaction temperature is 150°C , the reaction time is 10h. After the react...

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Abstract

The invention provides a preparation method of 1-hydroxy-4-(p-toluidino)anthraquinone. 1,4-dihydroxy anthraquinone, p-toluidine, ether solvents and a condensation catalyst are added to a reaction kettle, a system is gradually heated for a reaction, a product is filtered after the reaction ends, a filter cake is washed, dried and treated with a refining process, and a finished product, namely, 1-hydroxy-4-(p-toluidino)anthraquinone is obtained.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to a preparation method of 1-hydroxy-4-p-toluidine anthraquinone. Background technique [0002] Chinese name: 1-hydroxy-4-(p-toluidine)-anthraquinone, Chinese aliases: boron reagent; transparent violet B; oil-soluble violet 13; oil-soluble violet B; English name: 1-hydroxy-4-(p -toluidino) anthraquinone, used as a reagent for the determination of boron. It is mainly used for the coloring of polyester fibers, and can also be used for the preparation of masterbatches for polyester. [0003] CN104341790B relates to a new method for preparing 1-hydroxyl-4-arylamino anthraquinone. The mixture of quinazine and its leucosome, and a slight excess of aromatic amine are condensed in water containing an anionic surfactant, and the reaction is not Using boric acid or other condensing agents, the condensation product is purified by DMF aqueous solution to obtain 1-hydroxy-4-arylaminoanthraquinon...

Claims

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Application Information

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IPC IPC(8): C09B1/514B01J31/22
CPCC09B1/5145B01J31/22B01J2231/4277B01J2531/38
Inventor 郭志毅杨卫统屠仁华颜福池赵汉安谷灿波
Owner 宁波德欣科技有限公司
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