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Production method for high-purity 1-aminoanthraquinone

An aminoanthraquinone, production method technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of no industrialization value and high cost, achieve good industrialization value, reduce production costs, equipment Requirements and the effect of low production costs

Inactive Publication Date: 2014-05-07
CHANGZHOU INST OF CHEM
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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, naphthoquinone method and electrochemical method to synthesize 1-aminoanthraquinone, but these methods have no industrial value due to their high cost.

Method used

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  • Production method for high-purity 1-aminoanthraquinone
  • Production method for high-purity 1-aminoanthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 2L electromagnetically stirred hydrogenation pressure reactor, add 120g of 1-nitroanthraquinone with a purity of 99.2%, 1500g of toluene, and 11.0g of Raney Ni catalyst. After replacing the air with inert gas, introduce hydrogen into the system. The hydrogenation reaction is carried out, and the reaction is stopped after the hydrogen consumption reaches the reaction stoichiometric ratio. The reducing solution was heated and filtered to remove the catalyst, and then entered the oxidation tank, fed with oxygen, heated to 105°C and stirred for 1 hour, then cooled to room temperature for crystallization. Filter and crystallize, weigh 95.4g after drying, and check its purity by liquid chromatography. The content of 1-aminoanthraquinone is 99.3%.

Embodiment 2

[0020] In a 2L electromagnetically stirred hydrogenation pressure reactor, add 120g of 1-nitroanthraquinone with a purity of 99.2%, 1200g of xylene, and 10.0g of Raney Ni catalyst, replace the air with an inert gas, and introduce hydrogen into the system. The hydrogenation reaction is carried out at ℃, and the reaction is stopped after the hydrogen consumption reaches the reaction stoichiometric ratio. After the reducing solution is heated and filtered to remove the catalyst, it enters the oxidation tank, is fed with oxygen, is heated to 135°C and stirred for 1 hour, and then cooled to room temperature for crystallization. Filter and crystallize, weigh 97.5g after drying, and check its purity by liquid chromatography. The content of 1-aminoanthraquinone is 99.2%. Apply the mother liquor and catalyst mechanically, add 112g of 1-nitroanthraquinone, repeat the above reaction and post-treatment process (among them, add 3.0g of catalyst for the seventh time of mechanical applicatio...

Embodiment 3

[0022] Raw material, solvent, catalyst consumption and hydrogenation reaction process are all with embodiment 2. Afterwards, the reducing solution was heated and filtered to remove the catalyst and then entered into the oxidation tank, where oxygen and a small amount of ammonia gas were introduced, heated to 135°C and stirred for 1 hour, then cooled to room temperature for crystallization. Filter and crystallize, weigh 98.4g after drying, and check its purity by liquid chromatography. The content of 1-aminoanthraquinone is 99.3%. Apply the mother liquor and catalyst mechanically, add 112g of 1-nitroanthraquinone, repeat the above reaction and post-treatment process (among them, add 3.0g of catalyst for the seventh time of mechanical application), and perform liquid phase analysis on each precipitated crystal obtained from 10 times of mechanical application. Chromatographic detection shows that its 1-aminoanthraquinone content is above 99.1%. The final mother liquor was distil...

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Abstract

The invention discloses a production method for high-purity 1-aminoanthraquinone. The production method is advantaged by simple devices, safe operation, low production cost and no pollution. The production method comprises: 1-nitroanthraquinone, aromatic hydrocarbon solvents and catalysts are subjected to a catalytic hydrogenation reaction in a reactor, after the catalysts are removed through filtration, the reduction solution is oxidized under certain conditions, cooling is carried out, the precipitated crystals are subjected to filtration and drying, and high-purity 1-aminoanthraquinone is obtained, the mother liquor obtained after the crystals are removed through filtration and the catalyst can be used continuously; during the catalytic hydrogenation reaction, the mass rate of the solvents to 1-nitroanthraquinone is 5-30:1, the hydrogenation reaction temperature is 60 DEG C-150 DEG C, and the oxidation reaction temperature is 70 DEG C-180 DEG C. In the production method, the one-way crystallization amount can reach above 90%, the selectivity of 1-aminoanthraquinone reaches above 99.8%, during the production process, the mother liquor can be directly recycled without processing, the total yield can reach above 98% during the recycling process, no "three wastes (waste gas,waste water and industrial residue)" are discharged in the production technology and the production technology is clean.

Description

technical field [0001] The invention relates to a production process of a type of aromatic amine, in particular to a production method of high-purity 1-aminoanthraquinone. Background technique [0002] Anthraquinone dyes are the second largest category of dyes next to azo dyes, and 1-aminoanthraquinone is an important intermediate for the synthesis of anthraquinone dyes. It has the widest application and the largest consumption. The main raw material of acid and pyrazole anthraquinone occupies an extremely important position in the dye industry. With the increasing demand for 1-aminoanthraquinone, the output of low-quality 1-aminoanthraquinone in the domestic market has exceeded the demand, while the output of high-quality products is far from meeting the needs of export. In recent years, due to the "three wastes" and other reasons, the production of anthraquinone-based intermediates, anthraquinone-based vat and disperse dyes has been reduced or stopped in North America and...

Claims

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Application Information

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IPC IPC(8): C07C225/34C07C221/00
Inventor 辛阳吴集钱贾树勇王公应
Owner CHANGZHOU INST OF CHEM
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