Novel technique for synthesizing solvent yellow 163

A synthesis process and solvent technology, applied in the field of solvent yellow 163 synthesis process, can solve the problems of complex preparation process, high production cost, large fluctuation of product appearance and content, etc.

Inactive Publication Date: 2008-02-27
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The chemical name of solvent yellow 163 is 1,8 diphenylthioanthraquinone. It is a solvent dye with excellent performance. It can also be used as a disperse dye for dyeing polyester and its blended fabrics after post-treatment and commercialization. The original production process is Using 1,8-dichloroanthraquinone as the raw material, in the solvent xylene, potassium carbonate is used as the acidic agent to react with thiophenol. After the reaction, the solvent xylene is distilled off, then filtered and washed with hot water. The unreacted thiophenol is washed and dried to obtain the finished product. The yield of this process is very high. However, since the main raw materials and reaction by-products used in the product are insoluble in water, the unreacted main raw materials and the raw materials brought in Impurities and by-products from the reaction all enter the product at the end, so the product quality is difficult to guarantee, the appearance and content of the product fluctuate greatly between batches, and the main raw material 1,8-dichloroanthraquinone used in this process The preparation process is complicated and the production cost is very high, which makes the production cost of Solvent Yellow 163 relatively high and the quality is difficult to stabilize, which limits the popularization of this variety

Method used

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  • Novel technique for synthesizing solvent yellow 163
  • Novel technique for synthesizing solvent yellow 163

Examples

Experimental program
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Effect test

Embodiment 1

[0015] In a 250ml four-neck flask, add 100ml of dimethylformamide, 30g of 1,8-dinitroanthraquinone, 24g of thiophenol, and 12g of potassium hydroxide. After the addition, slowly raise the temperature to 50°C for about one hour and keep it warm. React for two hours, after the chromatographic detection of 1,8-dinitroanthraquinone disappears, use a cold water bath to cool down to 25°C, keep stirring at this temperature for one hour, then filter, and wash the filter cake with dimethylformamide containing 20% ​​water Then wash it with hot water at about 80° C., and dry the filter cake to obtain 41 g of finished product, with a content of 99.5% and a yield of 96%.

Embodiment 2

[0017] In a 250ml four-neck flask, add 120ml of dimethylformamide, 30g of 1,8-dinitroanthraquinone, 24g of thiophenol, and 12g of potassium hydroxide. After the addition, slowly raise the temperature to 50°C for about one hour to keep the temperature React for two hours, after the chromatographic detection of 1,8-dinitroanthraquinone disappears, use a cold water bath to cool down to 25°C, keep stirring at this temperature for one hour, then filter, and wash the filter cake with dimethylformamide containing 20% ​​water Then wash it with hot water at about 80° C., and dry the filter cake to obtain 40 g of finished product, with a content of 99.8% and a yield of 93.7%.

Embodiment 3

[0019] In a 250ml four-neck flask, add 100ml of dimethylacetamide, 30g of 1,8-dinitroanthraquinone, 24g of thiophenol, and 12g of potassium hydroxide. After 1,8-dinitroanthraquinone disappears, use a cold water bath to cool down to 25°C, keep stirring at this temperature for one hour and then filter. The filter cake is washed with dimethylacetamide containing 20% ​​water and then washed with 80°C or so After washing with hot water, the filter cake was dried to obtain 41.5 g of finished product with a content of 99.4% and a yield of 97.2%.

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Abstract

The invention discloses a new synthesizing technique of solvent yellow 163, which comprises the following steps: adopting 1, 8-dinitroanthraquinone as raw material to react with thiophenol in the strongly polar solvent of dimethyl formamide or dimethyl acetamide based on potassium hydroxide as acid-attaching agent at 30-100 deg. c to make the solvent yellow 163; cooling below 30 deg. c after finishing the reaction; filtering until the product is evolved sufficiently; washing the filter pie; drying; obtaining the product. The method reduces the manufacturing cost greatly and improves the main content of the product obviously, which modifies the appearance of the product with simple operation and easy control, in order to stabilize the manufacturing and increase the economical benefit.

Description

technical field [0001] The present invention is a synthesis process of solvent yellow 163. More specifically, a more economical and readily available raw material 1,8-dinitroanthraquinone is used as a raw material to replace 1,8-dichloroanthraquinone in the original process. Produce a product with lower cost and higher quality. Background technique [0002] The chemical name of solvent yellow 163 is 1,8 diphenylthioanthraquinone. It is a solvent dye with excellent performance. It can also be used as a disperse dye for dyeing polyester and its blended fabrics after post-treatment and commercialization. The original production process is Using 1,8-dichloroanthraquinone as the raw material, in the solvent xylene, potassium carbonate is used as the acidic agent to react with thiophenol. After the reaction, the solvent xylene is distilled off, then filtered and washed with hot water. The unreacted thiophenol is washed and dried to obtain the finished product. The yield of this p...

Claims

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Application Information

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IPC IPC(8): C09B1/60
Inventor 李少文周干臣
Owner JIANGSU YABANG DYE
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