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Method for separating and purifying anthraquinone

A technology for separation and purification of anthraquinone, applied in the field of anthraquinone, can solve the problems of excessive waste, low yield, poor color quality, etc., and achieve the effect of cost reduction

Inactive Publication Date: 2008-03-12
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The common disadvantages of these purification methods are that there are many wastes, poor color quality of anthraquinone, low yield, and cumbersome treatment process.

Method used

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  • Method for separating and purifying anthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 200 g of crude anthraquinone with a content of about 60% in a three-neck flask, add 100 g of N,N-dimethylformamide, and stir at -5°C for 0.5 h. Then, filter with suction and wash the filter cake three times with 100 g of N, N-dimethylformamide, then wash with water, filter with suction and dry to obtain 115 g of anthraquinone, and distill the mother liquor for mechanical use. The measured melting point of anthraquinone is 283°C-284°C.

Embodiment 2

[0013] Add 200 g of crude anthraquinone with a content of about 60% in a three-necked flask, add 100 g of N,N-dimethylformamide, and stir at 60° C. for 2 h. Then, filter with suction and wash the filter cake three times with 400g N, N-dimethylformamide, then wash with water, filter with suction and dry to obtain 110g of anthraquinone, and distill the mother liquor for mechanical use. The melting point of anthraquinone was measured to be 284°C to 284.6°C.

Embodiment 3

[0015] Add 200 g of crude anthraquinone with a content of about 60% into a three-neck flask, add 600 g of N,N-dimethylformamide, and stir at -5°C for 0.5 h. Then, filter with suction and wash the filter cake three times with 100 g of N, N-dimethylformamide, then wash with water, filter with suction and dry to obtain 112 g of anthraquinone, and distill the mother liquor for mechanical use. The melting point of anthraquinone was measured to be 284.3°C to 284.8°C.

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Abstract

The present invention discloses a separation and purification method of the anthraquinone, comprising the following steps: a. the rough anthraquinone is put into the organic solvent; the amount of the organic solvent is 0.5 to 3 times as much as the weight of the rough anthraquinone; the temperature is controlled between minus 5 DEG C and 60 DEG C; the mixture is stirred and the temperature is maintained for 0.5 to 2 hours; b. the mixture is taken out and filtered, and washed by the organic solvent and filtered once to three times after stopping the stirring; the amount of the organic solvent is 0.5 time to twice as much as the weight of the rough anthraquinone; the filter cake is washed by any type of water; the anthraquinone of high purity can be got after pumping and drying; the mother solution is decompressed and distilled; the organic solvent can be recycled and reused. The present invention proposes a simple and highly efficient separation and purification method of the anthraquinone; the anthraquinone made in the present invention is of the high purity; the measured melting point is between 284.3 and 285 DEG C; the reclamation rate of the anthraquinone can reach above 90 percent.

Description

technical field [0001] The present invention relates to anthraquinones, i.e. C 14 h 8 o 2 separation and purification method. Background technique [0002] Anthraquinone is a dye intermediate and can also be used as a cooking agent for paper pulping. The anthraquinone obtained by the gas-phase catalytic oxidation method of refined anthracene, the liquid-phase oxidation method of refined anthracene chromic acid, the hydrogenation oxidation method of crude anthracene, the phthalic anhydride method, the naphthoquinone method and the styrene method is not high in purity and needs to be separated and purified before it can be put into use. . At present, the commonly used purification methods are (1) alkali washing, acid washing, water washing or light oil washing. (2) Rectification under reduced pressure. (3) Recrystallization or sublimation. The common disadvantages of these purification methods are many wastes, poor color quality of anthraquinone, low yield and cumbersom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/18C07C46/10
Inventor 金东元姜荫陶建伟张兴龙
Owner SHANGHAI INST OF TECH