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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  • 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 hyd

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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Example Embodiment

[0025] Example 1:

[0026] The 1,4-dihydroxy steel pressure kettle is 3.00 g (0.208 mol), 600 g of industrial ammonia (25% ammonia), 10.00 g of hydrazine (0.200 mol), catalyst (TBAb) 0.50g, test After the pressure is slowly warmed by about 30 minutes, the pressure is 0.15 ~ 0.20 MPa, the pressure is 1 h, and the heat preservation ends the pressure-binding dermine (ammonia enters circulating recycling system), the material is filtered to wash to neutral, dry 1 49.84 grams of 4-diaminophyroxide nuts, HPLC was detected by 95.43%, and the reaction rate was 95.12%.

Example Embodiment

[0027] Example 2:

[0028] 1,4-dihydroxy steel pressure kettle, 500 grams of industrial ammonia (25% ammonia), 7.3 g of hydrazine (0.146 mol), catalyst (TBAB) 1.0g, slow temperature after test pressure 60min left and right at 65 ~ 70 ° C, forward pressure 0.15 ~ 0.20MPa, thermal insulation for 1 h, heat insulation end pressure-binding dermine (ammonia into circulating recovery system), material filtration washed to neutral, dry 1,4-two The amino anthraquinone was 49.69 g, HPLC detection content was 95.12%, and the reaction yield was 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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