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Method for preparing 1-amino-anthraquinone from 1-nitro-anthraquinone by catalytic hydrogenation

A technology of nitroanthraquinone catalysis and aminoanthraquinone, applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as retention, high production cost, and no industrial value, and achieve Less investment in equipment, improved catalytic performance, and environmentally friendly effects

Inactive Publication Date: 2016-12-21
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, there are some green processes, such as hydrazine hydrate method and electrochemical method, but these methods are still in the laboratory stage due to high production costs, and have no industrial value.

Method used

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  • Method for preparing 1-amino-anthraquinone from 1-nitro-anthraquinone by catalytic hydrogenation
  • Method for preparing 1-amino-anthraquinone from 1-nitro-anthraquinone by catalytic hydrogenation
  • Method for preparing 1-amino-anthraquinone from 1-nitro-anthraquinone by catalytic hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Catalyst preparation:

[0028] In the presence of organic modifier polyethylene glycol 600, copper nitrate trihydrate, nickel acetate tetrahydrate and hydrazine hydrate were used as raw materials to prepare nano-copper / nickel binary alloy catalysts by wet chemical reduction method.

[0029] First take by weighing 3.2g of copper nitrate trihydrate and 1.3g of nickel acetate tetrahydrate and dissolve them in 50ml of absolute ethanol respectively, and mix 20ml of aqueous solution with 0.32g of polyethylene glycol 600 and the ethanol solution of copper and nickel; Under stirring, at a constant temperature of 60° C., 1.5 mol / L NaOH ethanol solution was added dropwise to adjust the pH value of the solution to 13. Then measure 20ml of hydrazine hydrate with a mass fraction of 85% and dilute it to 100ml with absolute ethanol, add dropwise to the above solution, and prepare nano-copper-nickel binary alloy Cu / Ni after reacting at 80°C for 4h, and cool to room temperature and sto...

Embodiment 2

[0033] Adopt the same catalyst preparation method of Example 1, only change the organic modifier to be polyvinylpyrrolidone K-30 or sodium dodecylsulfonate or D-sorbitol or sodium dodecylbenzenesulfonate to prepare nano-copper-nickel di Elemental alloy Cu / Ni. The catalytic hydrogenation reaction of 1-nitroanthraquinone adopts the same method as in Example 1 to obtain the influence of different organic modifiers on the catalytic hydrogenation reaction of 1-nitroanthraquinone prepared by nano-copper-nickel catalysts. The results are shown in Table 1.

[0034] Table 1 Effect of Cu / Ni nanocatalysts prepared by different organic modifiers on the catalytic hydrogenation of 1-nitroanthraquinone

[0035]

Embodiment 3

[0037] Using the same method as in Example 1 to prepare nano-Cu / Ni catalysts, catalyze the hydrogenation of 1-nitroanthraquinone, and only change the reaction temperature in the kettle to 60 ° C, 80 ° C and 120 ° C respectively, the reaction temperature can be obtained. The influence of nitroanthraquinone catalytic hydrogenation reaction, the results are shown in Table 2.

[0038] The influence of table 2 reaction temperature on 1-nitroanthraquinone catalytic hydrogenation reaction

[0039]

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PUM

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Abstract

The invention provides a method for preparing 1-amino-anthraquinone from 1-nitro-anthraquinone by catalytic hydrogenation. The method comprises the following steps: step 1, placing 1-nitro-anthraquinone and N,N-dimethylformamide into a high pressure reaction kettle; adding a certain amount of nano-copper / nickel binary alloy catalyst; mounting a reacting device well; feeding N2 to exhaust air; feeding high-purity hydrogen to exhaust the N2; and starting a stirring device; step 2, feeding a certain pressure of hydrogen into a system obtained in step 1 under a constant temperature condition for reacting; after the reaction is ended, reducing the temperature to be below 45 DEG C; diluting the reacting product 1-amino-anthraquinone; and finally analyzing and calculating a result by using high performance liquid chromatography. During a preparation procedure of a catalyst disclosed by the invention, different organic modifiers are used for controlling the size of particles; the nano-copper / nickel binary alloy catalyst of different structures and shapes is prepared; the catalytic performance of the catalyst is effectively improved.

Description

technical field [0001] The invention relates to a method for preparing 1-aminoanthraquinone by catalytic hydrogenation of 1-nitroanthraquinone, belonging to the technical field of organic chemical synthesis. Background technique [0002] 1-aminoanthraquinone (C 14 h 9 NO 2 ), also known as 1-amino-9,10 anthracenedione, is a red to brown crystalline powder, and is mainly an important intermediate for the synthesis of anthraquinone dyes. Anthraquinone dyes are the second largest category of dyes after azo dyes, but because azo dyes use aromatic amines as intermediates in the production process, some aromatic amines are carcinogenic, and may be produced after the production of azo dyes Purification is not clean and there is a small amount of residue, so the application of azo dyes is subject to certain restrictions. Therefore, 1-aminoanthraquinone occupies an extremely important position in the dye industry. [0003] Traditionally, 1-aminoanthraquinone is produced by sulfo...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/34B01J23/755
CPCC07C221/00B01J23/755C07C225/34
Inventor 卢志鹏殷恒波薛武平王爱丽
Owner JIANGSU UNIV
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