Method for synthesizing solvent green 5

A synthesis method and solvent technology, applied in the field of synthesis of solvent green 5, can solve problems such as weather resistance defects and lack of vividness

Inactive Publication Date: 2018-04-17
连云港锐华化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the pigment has such excellent application properties, it still has some drawbacks, especially the lack of sufficient vividness, and there are also certain defects in weather resistance. Therefore, it is of great significance to carry out research on vividness and weather resistance

Method used

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  • Method for synthesizing solvent green 5
  • Method for synthesizing solvent green 5
  • Method for synthesizing solvent green 5

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, a kind of synthetic method of solvent green 5, synthetic method comprises the steps:

[0030] (1) Acylation reaction

[0031] The mixture of 3,9-perylene diacid and 3,10-perylene diacid is produced by reacting 3,9-perylene dioic acid and 3,10-perylene diacid with sulfur oxychloride, and the reaction route is as follows:

[0032]

[0033] (2) Esterification reaction

[0034] 3,9-perylene diacid chloride, 3,10-perylene diacid chloride react with isobutanol to generate 3,9-diisobutyl perylene diacid and 3,10-perylene diacid isobutyl ester, the reaction scheme is as follows:

[0035]

[0036] (3) Decolorization

[0037] Product 3,9-diisobutyl perylene diacid and 3,10-diisobutyl perylene diacid are crude products of solvent chlorine 5, and two kinds of adsorbents are added in the chlorobenzene solution of this crude product: activated carbon and activated clay , so that these two adsorbents can adsorb and refine the crude product at the same time, and th...

Embodiment 2

[0040] Example 2, in the synthesis method of solvent green 5 described in Example 1: add the slag material produced in steps (3) and (4) to the recovered chlorobenzene, then add activated carbon and activated clay to adsorb and refine again, After hot filtration to remove impurities, the filtrate is a mixture of chlorobenzene and methanol, recovered according to different fractions at different distillation temperatures, then add a certain amount of methanol to the filtrate, cool down and filter, the filtrate is a mixture of filter cake and methanol, and recover by distillation , The filter cake is recovered as the secondary crude product.

Embodiment 3

[0041] Embodiment 3, in the synthetic method of a kind of solvent green 5 described in embodiment 1 or 2: the specific steps of acylation reaction are: add unused chlorobenzene in the acylation kettle, then add perylene dioic acid, DMF and triethylbenzyl ammonium chloride, close the lid of the kettle, suck in an appropriate amount of unused thionyl chloride and recover the thionyl chloride by vacuum, and carry out the acylation reaction at 60°C-95°C.

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Abstract

The invention discloses a method for synthesizing solvent green 5 with high conversion ratio and high quality. The method mainly comprises improvement and enhancement of two aspects, such as enhancement of a conversion rate in an acylation reaction (production of acyl chloride) and scientific and reasonable refining of crude solvent green 5. The acylation reaction is an initial reaction for synthesizing the product, the enhancement of the reaction conversion ratio is to enhance the utilization ratio of an initial raw material, perylene diacid from the product synthesis source, the purity of the product, namely the acyl chloride, in the acylation reaction is increased, and a foundation is preferentially laid for improving the product quality. Moreover, during refining of the crude product,the crude product is adsorbed and refined by adopting two adsorbents with different adsorption mechanisms and different adsorption capacities, so that the product quality is effectively improved.

Description

technical field [0001] The invention belongs to the field of organic solvent pigments, and relates to a method for synthesizing solvent green 5 by improving the conversion rate of the acylation reaction (formation of acid chlorides) of perylene pigments and improving the refining method of crude products, thereby improving and improving product performance. Background technique [0002] Due to its special planar structure of five-membered condensed ring molecules, the perylene pigments have consistent and regular crystal form of the pigment particles, and the regular crystal form makes the particle structure dense and firm, so that the pigment has excellent application performance and has Good weather fastness and heat resistance stability make it worthy of the name to enter the ranks of high-grade pigments and can be used in high-grade coatings, such as: automotive coatings, metal surface coatings, powder coatings, exterior wall coatings and synthetic fiber coloring and plas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B3/18C09B67/20C09B67/54
CPCC09B3/18C09B67/0065C09B67/0096
Inventor 方百红
Owner 连云港锐华化工有限公司
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