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Clean process for synthesizing 1, 4-diamino-anthraquinone leuco body

A technology of diaminoanthraquinone and dihydroxyanthraquinone, which is applied in the clean process field of synthesizing 1,4-diaminoanthraquinone leuco, which can solve the problems of loss and high production cost, achieve process safety and reduce reaction temperature And pressure, shorten the effect of reaction time

Active Publication Date: 2021-07-06
JIANGSU HUAER CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The Chinese invention patent with the publication number CN109776339A discloses a green synthesis method of 1,4-diaminoanthraquinone, which uses toluene as a solvent and palladium carbon as a catalyst to replace the traditional one-step ammoniation process of hydrosulfite and hydrazine hydrate It is two steps of hydrogenation and ammoniation, which is more environmentally friendly; but it still needs to use organic solvents and expensive catalysts. Although it can be reused, there is still loss in the production process, and the overall production cost is high

Method used

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  • Clean process for synthesizing 1, 4-diamino-anthraquinone leuco body
  • Clean process for synthesizing 1, 4-diamino-anthraquinone leuco body

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 1000ml stainless steel autoclave, drop into 1,4-dihydroxyanthraquinone 50.00 grams (0.208mol), industrial ammonia 600 grams (ammonia content 25%), hydrazine hydrate 10.00 grams (0.200mol), catalyst (TBAB) 0.50g, test After pressing, slowly raise the temperature for about 30 minutes at 60-65°C, with a positive pressure of 0.15-0.20Mpa, keep warm for 1 hour, and release the pressure to remove ammonia (ammonia enters the recycling and recovery system) at the end of the heat preservation. The material is filtered and washed until neutral, and dried to 1 , 49.84 grams of 4-diaminoanthraquinone leuco, the content detected by HPLC was 95.43%, and the reaction yield was 95.12%.

Embodiment 2

[0028] 1000ml stainless steel autoclave, put 50.00g of 1,4-dihydroxyanthraquinone, 500g of industrial ammonia water (25% ammonia content), 7.3g of hydrazine hydrate (0.146mol), 1.0g of catalyst (TBAB), and slowly heat up after pressure test About 60min at 65-70°C, positive pressure 0.15-0.20Mpa, heat preservation for 1h, pressure release and deamination at the end of heat preservation (ammonia enters the recycling system), the material is filtered and washed until neutral, and dried to obtain 1,4-di Aminoanthraquinone leuco is 49.69 g, the content detected by HPLC is 95.12%, and the reaction yield is 94.53%.

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Abstract

The invention relates to the technical field of dye production, and especially relates to a clean process for synthesizing a 1, 4-diamino-anthraquinone leuco body. The clean process comprises the following steps: sequentially adding 1, 4-dihydroxy-anthraquinone, hydrazine hydrate, ammonia water and a catalyst into a pressure reaction container, heating to a preset temperature, and carrying out heat preservation reaction; and after the reaction is completed, performing pressure relief and deamination, enabling ammonia gas to enter an ammonia water recovery system for reuse, carrying out suction filtration and washing on the obtained the material until the material becomes neutral, and drying to obtain the 1, 4-diamino-anthraquinone leuco body. According to the clean process for synthesizing the 1, 4-diamino-anthraquinone leuco body, provided by the invention, the hydrazine hydrate is used for replacing sodium hydrosulfite, the ammonia water is used for replacing an organic solvent, and the phase transfer catalyst is used, so that the reaction time is shortened, the reaction temperature and pressure are reduced, and the process is safer; reaction byproducts are water and nitrogen, so that generation of a large amount of salt is reduced, the environment-friendly treatment cost is reduced, and the goal of clean production is achieved.

Description

technical field [0001] The invention relates to the technical field of dye production, in particular to a cleaning process for synthesizing 1,4-diaminoanthraquinone leuco. Background technique [0002] 1,4-diaminoanthraquinone leuco is one of the commonly used raw materials in the dye industry. It has a wide range of uses and can be used to produce 2,3-dichloro-1,4-diaminoanthraquinone, Or it can be used directly as a dye. [0003] The traditional main production process of 1,4-diaminoanthraquinone leuco is to prepare the product by reacting 1,4-dihydroxyanthraquinone and ammonia water under positive pressure under the action of hydrosulfite. The biggest disadvantage of this process is that the amount of sodium hydrosulfite is large, the waste water produced has high inorganic salt content, high chroma, high COD, and high cost of waste water treatment. [0004] The Chinese invention patent with the publication number CN108395381A discloses a synthesis method and product se...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/34
CPCC07C221/00C07C225/34
Inventor 胡影影宋谷
Owner JIANGSU HUAER CHEM
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