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Synthesis method of 1,4-diamino-anthraquinone leuco body

A technology of diaminoanthraquinone and synthesis method, which is applied in the field of synthesis of 1,4-diaminoanthraquinone leuco, can solve the problems of difficult treatment, dark wastewater, large ammonia consumption, etc., to reduce production costs, The effect of increasing product yield and reducing ammonia consumption

Active Publication Date: 2018-08-14
大连傲视化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this method is that the ammonia consumption is large, and a large amount of high COD, high ammonia nitrogen, and high salt wastewater is produced, and the wastewater is dark in color and difficult to treat.

Method used

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  • Synthesis method of 1,4-diamino-anthraquinone leuco body

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Experimental program
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Effect test

Embodiment 1

[0022] Add 17.7g of hydrazine hydrate (85%, 0.3mol), 120g of 1,4-dihydroxyanthraquinone (0.5mol), and 400g of ethylene glycol monomethyl ether into a 1000ml autoclave. Close the autoclave, replace with nitrogen once and once with ammonia. Turn on stirring, feed ammonia gas, and adjust the pressure to 0.3Mpa. Heat up to 80°C and keep the pressure at 0.3Mpa. React for about 3 to 4 hours, pass 28 to 32 g of ammonia in total, close the ammonia gas inlet, slowly open the exhaust port, and gradually discharge excess ammonia to absorb water until the pressure is zero. Raise the temperature to 100°C and continue to stir to remove ammonia for 1h, stir and cool, then cool down to 5-10°C for about 1h, and keep it for 1h. After filtering, the filter cake was washed with 50 g of water, and air-dried at 70-75° C. for 5 h to obtain 116 g of 1,4-dihydroxyanthraquinone leuco compound, with a purity of 99.3% by HPLC and a calculated yield of 95.7%.

Embodiment 2

[0024] Add 17.7g of hydrazine hydrate (85%, 0.3mol), 120g of 1,4-dihydroxyanthraquinone (0.5mol), and 400g of sulfolane into a 1000ml autoclave. Close the autoclave, replace with nitrogen once and once with ammonia. Turn on the stirring, feed ammonia gas, and adjust the pressure to 0.4Mpa. Heat up to 80°C and keep the pressure at 0.4Mpa. React for about 3 to 4 hours, pass 28 to 32 g of ammonia in total, close the ammonia gas inlet, slowly open the exhaust port, and gradually discharge excess ammonia to absorb water until the pressure is zero. Raise the temperature to 100°C and continue to stir to remove ammonia for 1h, stir and cool, then cool down to 5-10°C for about 1h, and keep it for 1h. After filtering, the filter cake was washed with 50 g of water, and air-dried at 70-75° C. for 5 h to obtain 113 g of 1,4-dihydroxyanthraquinone leuco compound. The purity by HPLC was 99.2%, and the calculated yield was 93.4%.

Embodiment 3

[0026] Add 23.6g of hydrazine hydrate (85%, 0.4mol), 120g of 1,4-dihydroxyanthraquinone (0.5mol), and 400g of sulfolane into a 1000ml autoclave. Close the autoclave, replace with nitrogen once and once with ammonia. Turn on the stirring, feed ammonia gas, and adjust the pressure to 0.4Mpa. Heat up to 80°C and keep the pressure at 0.4Mpa. React for about 3 to 4 hours, pass 28 to 32 g of ammonia in total, close the ammonia gas inlet, slowly open the exhaust port, and gradually discharge excess ammonia to absorb water until the pressure is zero. Raise the temperature to 100°C and continue to stir to remove ammonia for 1h, stir and cool, then cool down to 5-10°C for about 1h, and keep it for 1h. After filtering, the filter cake was washed with 50 g of water, and air-dried at 70-75° C. for 5 h to obtain 113 g of 1,4-dihydroxyanthraquinone leuco compound. The purity by HPLC was 99.2%, and the calculated yield was 94.5%.

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a synthesis method of a 1,4-diamino-anthraquinone leuco body. The synthesis method comprises the following steps:adopting 1,4-diamino-anthraquinone as a raw material to mix with hydrazine hydrate and an organic solvent; reacting with ammonia gas for 3-4 hours under the conditions of the reaction pressure being 0.2-0.5 Mpa and the reaction temperature being 50-100 DEG C; exhausting ammonia gas after finishing reaction; and cooling, crystallizing, filtering and drying a reaction product to obtain the 1,4-diamino-anthraquinone leuco body. The synthesis method has the advantages of no high-COD (chemical oxygen demand), high-ammonia nitrogen and high-salinity waste water in the synthesis process, recyclability of filtrated stock, reduction of ammonia consumption, efficient reduction of production cost and high-purity and high-yield products, and is suitable for scale production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method and product separation method of 1,4-diaminoanthraquinone leuco. Background technique [0002] 1,4-Diaminoanthraquinone leuco is an important intermediate in the synthesis of dyes. The current common synthesis method is to react the raw material 1,4-dihydroxyanthraquinone with ammonia water in the presence of hydrosulfite, and separate and purify the product by filtering and washing with water. However, the disadvantage of this method is that the ammonia consumption is large, and a large amount of high COD, high ammonia nitrogen, and high salt wastewater is produced, and the wastewater is dark in color and difficult to treat. Therefore, there is an urgent need in the art for a new method for synthesizing 1,4-diaminoanthraquinone leuco that does not produce high-COD, high-ammonia-nitrogen, and high-salt wastewater. Contents of the invention [0...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/34
CPCC07C221/00C07C2603/24C07C225/34
Inventor 张宇段玉辉
Owner 大连傲视化学有限公司
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