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Synthesis process of 1,4-diamino-2-anthraquinone sulfonate

A technology of sulfonic acid anthraquinone and diaminoanthracene, which is applied in the field of synthesis improvement process of 1,4-diamino-2-sulfonic acid anthraquinone, can solve the problem of large amount of chlorosulfonic acid, difficult treatment of three wastes, and many by-products, etc. question

Inactive Publication Date: 2018-12-07
JIANGSU HUAER CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This leads to a large amount of chlorosulfonic acid, many by-products, and difficult disposal of the three wastes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] In a 500 ml four-neck flask, add 200 grams of o-dichlorobenzene, add 11.9 grams of 1,4-diaminoanthraquinone oxide under stirring, slowly add 6 grams of chlorosulfonic acid, and maintain the dropping temperature at 30-50 degrees Celsius. After the dropwise addition was completed, the temperature was raised to 138° C. in 2 hours. Insulate for 6 hours, cool down to 75°C, transfer to water pre-installed with 450 ml of water and 2.6 grams of soda ash, stir for 0.5 hours, adjust the pH to 7.3, distill off o-dichlorobenzene, then adjust the pH to 1.1 with sulfuric acid, and cool down to 82°C, filter, drain as much as possible, and wash with a small amount of water to obtain the product 1,4-diamino-2-sulfonic acid filter cake. The chromatographic content is 98.5%, and it can be directly used in the next process reaction without drying.

Embodiment 2

[0010] In a 500 ml four-neck flask, add 220 grams of o-dichlorobenzene, add 11.9 grams of 1,4-diaminoanthraquinone oxide under stirring, slowly add 6.1 grams of chlorosulfonic acid, and maintain the dropping temperature at 30-50 degrees Celsius. After the dropwise addition was completed, the temperature was raised to 134° C. in 2 hours. Insulate for 6.5 hours, cool down to 78°C, transfer to water pre-installed with 450 ml of water and 2.8 grams of soda ash, stir for 0.5 hours, adjust the pH to 7.5, distill off o-dichlorobenzene, then adjust the pH to 0.95 with sulfuric acid, and cool down to 80°C, filter, drain as much as possible, and wash with a small amount of water to obtain the product 1,4-diamino-2-sulfonic acid filter cake. The chromatographic content is 98.1%, and it can be directly used in the next process reaction without drying.

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PUM

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Abstract

The invention discloses a synthesis process of 1,4-diamino-2-anthraquinone sulfonate, belonging to the field of organic synthesis. The process comprises the steps of adding a 1,4-diamino-anthraquinoneoxysome and o-dichlorobenzene into a container, dropwise adding chlorosulfonic acid while holding the temperature at 30-50 DEG C, heating to 140+ / -3 DEG C, holding the temperature for 6+ / -1 hours, cooling to 60-80 DEG C, transferring to water containing sodium carbonate, stirring for a period of time, adjusting the pH to 7.5+ / -0.1, steam distilling the solvent, cooling to 80+ / -5 DEG C, adjustingthe pH to 1+ / -0.2 with sulfuric acid so as to separate out 1,4-diamino-2-anthraquinone sulfonate, and filtering, so as to obtain the 1,4-diamino-2-anthraquinone sulfonate product. The use amount of chlorosulfonic acid in the process is one third of that of an original process, and the amount of byproduct hydrochloric acid is one third of that of the original process, and no sulfur dioxide gas is produced.

Description

technical field [0001] The invention relates to an improved synthesis process of 1,4-diamino-2-sulfonic acid anthraquinone, which belongs to the technical field of organic synthesis. Background technique [0002] 1,4-diamino-2-sulfonic acid anthraquinone is an important intermediate, which can be used to synthesize dyes such as disperse blue 60 and disperse blue 359. The 4-diaminoanthraquinone leuco can be obtained by sulfonation with chlorosulfonic acid in a solvent. It can be seen from the reaction equation that to obtain one part of 1,4-diamino-2-sulfonic acid anthraquinone needs to consume 3 parts of chlorosulfonic acid, one part of which is used to oxidize 1,4-diaminoanthraquinone leuco One part is used to sulfonate 1,4-diaminoanthraquinone, and one part of water will be generated during sulfonation, and this water will consume one part of chlorosulfonic acid. At the same time, three parts of hydrochloric acid and one part of sulfur dioxide are produced. This leads t...

Claims

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Application Information

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IPC IPC(8): C07C303/08C07C303/44C07C309/53
CPCC07C303/08C07C303/44C07C309/53
Inventor 詹国青
Owner JIANGSU HUAER CHEM
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