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Synthesis process of novel green naphthol chromophore type products

A synthetic process and green technology, which is applied in the field of synthetic process of new-type green naphthol color-based products, can solve problems such as difficult recycling, and achieve the effects of increased yield, good reproducibility, and improved purity

Inactive Publication Date: 2015-08-19
JIANGSU HUAYI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 1. Due to the use of phosphorus trichloride or thionyl chloride, new pollutants are produced, such as phosphite, hydrochloric acid, etc.;
[0009] 2. A small amount of unreacted raw materials and products are dissolved in the water phase during the reaction process, which is difficult to recover

Method used

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  • Synthesis process of novel green naphthol chromophore type products
  • Synthesis process of novel green naphthol chromophore type products
  • Synthesis process of novel green naphthol chromophore type products

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A novel green naphthenol color-based product synthesis process is characterized in that it comprises the following steps:

[0028] 1) The input material 2,3-acid and aniline compound are dissolved in a suitable solvent, and the solvent selection is generally a solvent that does not react and azeotrope with the initial raw materials and products, and forms an azeotrope with water and is immiscible with water, such as Toluene, chlorobenzene, etc.;

[0029] 2) Pass into a microwave reactor for reaction, the temperature in the microwave reactor is generally controlled at 90-150 degrees, and the reaction time is 0.5-5h;

[0030] 3) Since 1 equivalent of water will be released during the reaction process, it must be transferred in time. The coupling process of reaction and azeotropic rectification is used to continuously separate the produced water. First, the azeotropic solvent produced by rectification enters the high-level In the tank, the rapid separation of water and so...

Embodiment 2

[0034]

[0035] Dissolve 1 equivalent of 2,3-acid and 1 equivalent of 4,-chloro-2,5-dimethoxyaniline in 10 equivalents of chlorobenzene, control the reaction temperature to 110 degrees, and set the reaction time to 1h. During the process, the rectification reflux ratio R=1.2. After the reaction is completed, the bottom temperature is controlled to 150 degrees, the reflux ratio is 0.8, and the chlorobenzene is rectified. After the chlorobenzene is removed, the product is released, and the product yield is 99%. , The product purity is 99.5%.

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Abstract

The present invention discloses a synthesis process of novel green naphthol chromophore type products. The synthesis process is characterized by comprising the following steps: 1) putting and dissolving materials of 2, 3-acid and aniline compounds into a suitable solvent; 2) pumping a resulting solution into a microwave reactor for reaction; 3) transferring water in time because 1 equivalent of the water can be drained in the process of the reaction; 4) upon completion of the reaction, distilling off the solvent through rectification; and 5) discharging bottom products. The microwave reaction and the reaction rectification are combined, so that the product synthesis efficiency is improved, and zero discharge of pollutants is realized.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis process of novel green naphthenochrome-based products. Background technique [0002] Naphthol is commonly known as Naphthol and primer. Refers to the coupling component of azo dyes. [0003] When printing and dyeing, it is used as a primer, and it reacts with the diazonium salt of the color base on the cellulose fiber to form an insoluble azo dye and fix it on the fiber. A naphthol can often be coupled with different chromophore diazonium salts to form different azo dyes with different hues and fastnesses. Most varieties of naphthols are formed by condensation of 2-hydroxy-3-naphthoic acid with different aromatic amines after acyl chloride, and there are also hydroxyformamide derivatives of carbazole, oxyfluorene, and anthracene. For example, naphthol AS, naphthol AS-D, naphthol AS-LB, naphthol AS-BT, etc. [0004] Naphthalene compounds are closely relat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C235/66
Inventor 王卉李新良徐志红桂媛
Owner JIANGSU HUAYI TECH
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