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Novel technique for synthesizing solvent yellow 189

A new process and solvent technology, which is applied in the new process field of solvent yellow 189 synthesis, can solve the problems of large fluctuations in product appearance and content, high production costs, and high production costs of solvent yellow 189

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 189 is 1,5-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 treatment. The original production process is 1 , 5-dichloroanthraquinone as raw material, in the solvent xylene, using potassium carbonate as the acid agent and thiophenol to react, after the reaction, the solvent xylene is removed by distillation, then filtered, washed with hot water to remove unreacted The thiophenol is washed and dried to obtain the finished product. The yield of this process is very high, but because the product, the main raw materials used and the by-products of the reaction are all insoluble in water, the main raw materials that have not been completely reacted, the impurities brought in by the raw materials, and The by-products produced by the reaction all enter the product at the end, so the product quality is difficult to be guaranteed, the appearance and content of the product fluctuate greatly between batches, and the main raw material 1,5-dichloroanthraquinone used in the process is prepared by Complex, high production cost, making the production cost of solvent yellow 189 high, and the quality is difficult to stabilize

Method used

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  • Novel technique for synthesizing solvent yellow 189
  • Novel technique for synthesizing solvent yellow 189

Examples

Experimental program
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Effect test

Embodiment 1

[0015] In a 250ml four-necked flask, add 100ml of dimethylformamide, 30g of 1,5-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 1,5-nitroanthraquinone disappears, use a cold water bath to cool down to 25°C, keep stirring at this temperature for one hour, filter, and wash the filter cake with dimethylformamide containing 20% ​​water. Wash it with hot water at about 80°C, and dry the filter cake to obtain 41g of finished product, with a content of 99.7% and a yield of 96%.

Embodiment 2

[0017] In a 250ml four-neck flask, add 120ml of dimethylformamide, 30g of 1,5-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 1,5-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 99.7% and a yield of 93.7%.

Embodiment 3

[0019] In a 250ml four-neck flask, add 100ml of dimethylacetamide, 30g of 1,5-dinitroanthraquinone, 24g of thiophenol, and 12g of potassium hydroxide. After 1,5-dinitroanthraquinone disappears, use a cold water bath to cool down to 25°C, keep stirring at this temperature for one hour and then filter, wash the filter cake with dimethylacetamide containing 20% ​​water, and then wash it with about 80°C 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 189, which comprises the following steps: adopting 1, 5-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 189; 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 new process for the synthesis of solvent yellow 189. More specifically, a more economical and readily available raw material 1,5-dinitroanthraquinone is used as a raw material to replace 1,5-dichloroanthraquinone in the original process , to produce a product of lower cost and better quality. Background technique [0002] The chemical name of solvent yellow 189 is 1,5-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 treatment. The original production process is 1 , 5-dichloroanthraquinone as raw material, in the solvent xylene, using potassium carbonate as the acid agent and thiophenol to react, after the reaction, the solvent xylene is removed by distillation, then filtered, washed with hot water to remove unreacted The thiophenol is washed and dried to obtain the finished product. The yield of this process is ...

Claims

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Application Information

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IPC IPC(8): C09B1/58
Inventor 李少文王继昌牟忠丽
Owner JIANGSU YABANG DYE
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