Synthesis process of solvent violet 59

A synthesis process, solvent violet technology, applied in the direction of amino-hydroxy anthraquinone dyes, anthracene dyes, organic dyes, etc., can solve the problems of low purity, low product yield, long reaction time, etc., to shorten the reaction time, yield The effect of high rate and reduction of insoluble matter

Inactive Publication Date: 2018-10-16
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problems of low product yield, low purity and long reaction time in the above-mentioned process, the present invention proposes a synthesis process of 1,4-dinitro-2,3-dichloroanthraquinone

Method used

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  • Synthesis process of solvent violet 59
  • Synthesis process of solvent violet 59
  • Synthesis process of solvent violet 59

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1: Synthesis of 1,4-dinitro-2,3-diphenoxyanthraquinone

[0019] In a 500mL four-necked flask equipped with an electric stirrer, add 67.5g of sodium phenolate, 100g of 1,4-dinitro-2,3-dichloroanthraquinone and 185mL of o-dichlorobenzene, stir and heat up to 194℃, keep the temperature for reaction 5h. After the reaction, the temperature is lowered to 180°C, and the o-dichlorobenzene is desolvated. After the desolvation is completed, add 40ml NaOH (30%) and 100ml of water, stir at 100°C for 1h, filter, wash the filter cake with hot water, and dry . The product is 115.58 g, the yield is 88.2%, and the purity is 96.7%.

Embodiment 2

[0021] Other conditions are the same as in Example 1, and the experiment for detecting the mass ratio of different sodium phenolate / 1,4-dinitro-2,3-dichloroanthraquinone. The experimental results are shown in Table 1.

[0022] Table 1 Experiment of different mass ratios of sodium phenolate / 1,4-dinitro-2,3-dichloroanthraquinone

[0023]

[0024] From the above results, it can be seen that the mass ratio of sodium phenolate / 1,4-dinitro-2,3-dichloroanthraquinone is preferably 0.675 (Example 1).

Embodiment 3

[0026] Other conditions are the same as in Example 1, the experiment for detecting the mass ratio of different o-dichlorobenzene / 1,4-dinitro-2,3-dichloroanthraquinone, and the experimental results are shown in Table 2.

[0027] Table 2 Experiments on the mass ratio of different o-dichlorobenzene / 1,4-dinitro-2,3-dichloroanthraquinone

[0028]

[0029]

[0030] From the above results, it can be seen that the mass ratio of o-dichlorobenzene / 1,4-dinitro-2,3-dichloroanthraquinone is preferably 2.2 (Example 1).

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Abstract

The invention discloses a synthesis process of solvent violet 59. The synthesis process of the solvent violet 59 comprises the following steps: taking 1,4-binitro-2,3-dichloroanthraquinone and sodiumphenoxide as raw materials, performing condensation reaction under the existence of an organic solvent orthodichlorobenzene to generate 1,4-binitro-2,3-diphenoxyanthraquinone, and reducing the 1,4-binitro-2,3-diphenoxyanthraquinone to generate 1,4-diamido-2,3-diphenoxyanthraquinone. The activity of the 1,4-binitro-2,3-dichloroanthraquinone is higher than the activity of the 1,4-diamido-2,3-dichloroanthraquinone, and the reaction is easier to conduct, so the reaction time is greatly shortened; furthermore, the reaction has little side reactions, the yield is high and undissolved substances aregreatly reduced; moreover, the synthesis route avoids generation of a large amount of salt-containing waste water, and the process is relatively clean and environment-friendly.

Description

Technical field [0001] The invention relates to a synthesis process of solvent dyes, in particular to a synthesis process of 1,4-diamino-2,3-diphenoxyanthraquinone, and belongs to the field of chemical preparation. Background technique [0002] Solvent Violet 59, also known as 1,4-diamino-2,3-diphenoxyanthraquinone, is a solvent dye with excellent performance. It is mainly used for the coloring of ABS, PC, HIPS, PMMS and other resins. It can be used as a disperse dye to dye polyester and its blended fabrics. Chemical formula: C 26 H 18 N 2 O 4 , The relative molecular mass is 422.43, and the structural formula is: [0003] [0004] At present, the most commonly used synthetic route for the synthesis of this product in China is: 1,4-diaminoanthraquinone is used as a raw material, and the product is obtained by condensation with phenol after chlorination. Add 1,4-diamino-2,3-dichloroanthraquinone, phenol, potassium hydroxide aqueous solution, benzyltriethylammonium chloride and wat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/54
CPCC09B1/547
Inventor 刘学峰徐松陈路云汪港
Owner JIANGSU DAOBO CHEM
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