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Method for preparing 1, 4-diaminoanthraquinone-2-sulfonic acid by using supergravity reactor

A high-gravity reactor, diaminoanthraquinone technology, applied in chemistry/physics/physicochemical fixed reactor, sulfonic acid preparation, organic chemistry, etc., can solve the problem of difficult waste liquid treatment, complex temperature control, system Problems such as low pH, to achieve the effect of solving uneven temperature distribution and temperature monitoring, high yield and purity, and improving product yield

Pending Publication Date: 2022-03-11
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of this method are: a large amount of acid-base solution needs to be used, the pH of the system is too low after the reaction, and the waste liquid treatment is difficult; the temperature control in the reaction process is relatively complicated, and the requirements for equipment are high, which increases the production cost. , not conducive to the industrial production of 1,4-diamino-2-sulfonic acid anthraquinone

Method used

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  • Method for preparing 1, 4-diaminoanthraquinone-2-sulfonic acid by using supergravity reactor

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Effect test

Embodiment 1

[0023] In the high-gravity reactor, 1,4-diaminoanthraquinone leuco is used as the raw material, o-dichlorobenzene is used as the solvent, and the temperature is raised under negative pressure to remove trace moisture in the system. , the weight ratio of 4-diaminoanthraquinone leuco is 8:1, the supergravity level of the supergravity reactor is 600g, and the feed rate of 1,4-diaminoanthraquinone leuco is 30kg / h; Oxidize and sulfonate 1,4-diaminoanthraquinone leuco with chlorosulfonic acid, the molar ratio of chlorosulfonic acid to 1,4-diaminoanthraquinone leuco is 3.5:1, and the sulfonation temperature is 90°C , the sulfonation time is 3h; in the later stage of sulfonation, the auxiliary agent thionyl chloride is also added, and the ratio of its dosage to the weight of 1,4-diaminoanthraquinone leuco body is 1:50; the obtained material is neutralized and distilled to remove After solvent, filtration, and acidification treatment, the precipitated material was drained and washed to...

Embodiment 2

[0025] In the high-gravity reactor, 1,4-diaminoanthraquinone leuco is used as the raw material, and nitrobenzene is used as the solvent, and the temperature is raised under negative pressure to remove trace moisture in the system, and the o-dichlorobenzene solvent and 1, The weight ratio of 4-diaminoanthraquinone leuco is 8:1, the supergravity level of the supergravity reactor is 500g, and the feed rate of 1,4-diaminoanthraquinone leuco is 25kg / h; Chlorosulfonic acid oxidizes and sulfonates 1,4-diaminoanthraquinone leuco, the molar ratio of chlorosulfonic acid to 1,4-diaminoanthraquinone leuco is 3.5:1, and the sulfonation temperature is 90°C. The sulfonation time is 3 hours; in the later stage of sulfonation, the auxiliary agent thionyl chloride is added, and the ratio of its dosage to the weight of 1,4-diaminoanthraquinone leuco body is 1:50; the obtained material is neutralized and distilled to remove the solvent , filtration to remove impurities, and acidification treatmen...

Embodiment 3

[0027] In the high-gravity reactor, 1,4-diaminoanthraquinone leuco is used as the raw material, o-dichlorobenzene is used as the solvent, and the temperature is raised under negative pressure to remove trace moisture in the system. , the weight ratio of 4-diaminoanthraquinone leuco is 10:1, the supergravity level of the supergravity reactor is 600g, and the feed rate of 1,4-diaminoanthraquinone leuco is 30kg / h; Oxidize and sulfonate 1,4-diaminoanthraquinone leuco with chlorosulfonic acid, the molar ratio of chlorosulfonic acid to 1,4-diaminoanthraquinone leuco is 3.5:1, and the sulfonation temperature is 100°C , the sulfonation time is 3h; in the later stage of sulfonation, the auxiliary agent thionyl chloride is also added, and the ratio of its dosage to the weight of 1,4-diaminoanthraquinone leuco body is 1:50; the obtained material is neutralized and distilled to remove After solvent, filtration, and acidification treatment, the precipitated material was drained and washed ...

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Abstract

The invention discloses a method for preparing 1, 4-diamino-anthraquinone-2-sulfonic acid by using a supergravity reactor, which comprises the following steps: in the supergravity reactor, reacting a 1, 4-diamino-anthraquinone leuco body with chlorosulfonic acid at a certain feeding speed under a specific supergravity level to obtain a target product. The method solves the problem of overhigh local concentration of sulfonic acid, and can effectively strengthen mixing in the sulfonation process, thereby improving the product yield; meanwhile, the problems of uneven temperature distribution in the kettle and temperature monitoring can be effectively solved; the preparation method is simple in process, mild in condition and convenient to operate, the product has high yield and purity, and industrial production of the 1, 4-diaminoanthraquinone-2-sulfonic acid is facilitated.

Description

technical field [0001] The invention belongs to the technical field of synthesis of dye intermediates, and in particular relates to a method for preparing 1,4-diaminoanthraquinone-2-sulfonic acid in a high-gravity reactor. Background technique [0002] Disperse Turquoise GL, also known as Disperse Blue 60, has a molecular formula of C 20 h 17 N 3 o 5 , with a molecular weight of 379.3661, is an important variety in the field of dyes. [0003] 1,4-diaminoanthraquinone-2-sulfonic acid is the key intermediate of disperse blue, and its synthesis is usually prepared by sulfonating 1,4-diaminoanthraquinone leuco with chlorosulfonic acid in the kettle to prepare 1,4-diaminoanthraquinone Aminoanthraquinone-2-sulfonic acid, the process can be divided into oxidation and sulfonation. Among them, the sulfonation reaction requires heating and rapid heat release, and the temperature and heat transfer distribution in the kettle is uneven. When the local temperature is too high, side r...

Claims

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Application Information

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IPC IPC(8): C07C303/22C07C309/53B01J19/18
CPCC07C303/22B01J19/18C07C309/53
Inventor 姬书亮周坚彪王登兵臧君娇詹国青
Owner JIANGSU YABANG DYE
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