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Disperse red 356 preparation method

A technology of disperse red and mass ratio, which is applied in the direction of chemical instruments and methods, organic dyes, azo dyes, etc., can solve the problems of low yield and high production cost, achieve purity and yield improvement, reduce the production of by-products, The effect of increasing productivity

Inactive Publication Date: 2014-08-06
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the above synthesis process, there is the generation of highly toxic gas hydrocyanic acid, which is a high-risk reaction, and the yield of this route is low, and the generation cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The synthesis of step 1 p-propoxybenzaldehyde:

[0042] In a 1000ml four-neck bottle with mechanical stirring and a thermometer, add toluene 250, DMF200 mixed solvent, start stirring, and then add 50g of p-hydroxybenzaldehyde, 50g of bromopropane, 2g of auxiliary chlorine-type strong alkali ion exchange resin, hydrogen Potassium oxide 20g, the temperature was raised to 85°C for 1 hour, and after the reaction was completed, the temperature was lowered to 10°C, water was added, stirred for 30 minutes, and allowed to stand for stratification. The upper toluene layer was washed twice with water to obtain 66.5 g of p-propoxybenzaldehyde with a content of 99% and a yield of 98%.

Embodiment 2

[0044] The synthesis of step 1 p-propoxybenzaldehyde:

[0045] In a 1000ml four-neck bottle with mechanical stirring and a thermometer, add toluene 400, DMF300 mixed solvent, start stirring, and then add 50g of p-hydroxybenzaldehyde, 60g of bromopropane, 4g of auxiliary agent chlorine-type strong alkali ion exchange resin, hydrogen Potassium oxide 25g, the temperature was raised to 95°C for 1 hour reaction, after the reaction was completed, the temperature was lowered to 15°C, water was added, stirred for 30 minutes, and allowed to stand for stratification. The upper toluene layer was washed twice with water, and 66.8 g of p-propoxybenzaldehyde was obtained by precipitation, with a content of 98.5% and a yield of 98%.

Embodiment 3

[0047] The synthesis of step 1 p-propoxybenzaldehyde:

[0048]In a 1000ml four-necked bottle with mechanical stirring and a thermometer, add toluene 500, DMF250 mixed solvent, start stirring, and then add 50g of p-hydroxybenzaldehyde, 65g of bromopropane, 3g of auxiliary chlorine-type strong alkali ion exchange resin, hydrogen Potassium oxide 30g, the temperature was raised to 110°C to react for 1 hour, and after the reaction was completed, the temperature was lowered to 25°C, water was added, stirred for 30 minutes, and allowed to stand for stratification. The upper toluene layer was washed twice with water to obtain 66.8 g of p-propoxybenzaldehyde with a purity of 97.5% and a yield of 97%.

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Abstract

The present invention discloses a disperse red 356 preparation method, which comprises five reaction units such as alkylation, cyanation, condensation, cyclization and oxidation. Comparison with the method in the prior art, the method of the present invention has the following significant advantages that: 1, alkylation adopts a DMF and toluene mixed solvent and a chlorine type strong base anion exchange resin to replace the original quaternary ammonium salt phase transfer catalyst so as to significantly increase the reaction rate, the purity and the yield; 2, in the cyanation process, the generation of toxic hydrogen cyanide during the reaction process is avoided, and the yield is improved; 3, in the cyclization process, a perphosphoric acid and concentrated sulfuric acid mixed acid is adopted as a catalyst, and a reaction of p-propoxy phenyl glycolonitrile and 3-phenyl-6-hydroxy-benzofuran-2-one is adopted to replace the original process so as to reduce the production of the byproduct; and 4, the oxidation experiment results of different oxidants are different, wherein sodium perborate is screened, and the total yield of cyclization and oxidation can achieve 80%.

Description

technical field [0001] The invention relates to a preparation method of disperse red 356, which belongs to the technical field of manufacturing chemical dyes and chemicals. Background technique [0002] The chemical name of Disperse Red 356 is 3-phenyl-7(4-propoxyphenyl)-benzodifuran-2,6-dione, which is the largest variety of benzodifuranone disperse dyes, benzodifuranone Furanone disperse dyes have been widely valued for their bright color, high color strength and good dyeing performance, especially in the application of polyester microfibers. [0003] Its molecular formula is C 26 h 20 o 5 , relative molecular mass 412.43. The mechanism formula of Disperse Red 356 is: [0004] [0005] The existing production method synthetic route is as follows: [0006] [0007] In the above synthesis process, the generation of highly toxic gas hydrocyanic acid is a high-risk reaction, and the yield of this route is low, and the generation cost is relatively high. Therefore,...

Claims

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Application Information

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IPC IPC(8): C09B57/00
Inventor 徐松刘学峰郭维成汪港孙中华
Owner JIANGSU DAOBO CHEM
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