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Improved refining process of 1, 4-dihydroxy anthraquinone

A technology for crude dihydroxyanthraquinone and hydroxyanthraquinone, which can be used in quinone separation/purification, organic chemistry, etc., and can solve the problems of ineffective removal of mechanical impurities, high safety hazards, and low productivity.

Active Publication Date: 2021-06-08
JIANGSU HUAER CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]②Sublimation process: This process utilizes the sublimation characteristics of 1,4-dihydroxyanthraquinone to produce 1,4-dihydroxyanthraquinone products at high temperature. Through this process, relatively pure products can be obtained, but the process requires high equipment, low production capacity, high energy consumption, and low yield, generally no more than 85%, and the internal standard content is 98-99%. Moreover, there is no Proven equipment capable of large-scale application
[0005]③Solvent refining process: generally use DMF to dissolve the crude product 1,4-dihydroxyanthraquinone at high temperature, then precipitate most of the product at low temperature, filter and wash to obtain the product , the process can obtain products of different purity by adjusting the ratio of 1,4-dihydroxyanthraquinone to DMF solvent, but the yield is inversely proportional to the content, the removal rate of tar is also inversely proportional to the yield, and mechanical impurities cannot Effective removal; since high-temperature filtration has great operational difficulty and high safety hazards in the mass production process, this method cannot remove mechanical impurities by filtering DMF solution at high temperature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 50 grams of crude 1,4-dihydroxyanthraquinone and 1,000 grams of p-xylene to a 2000 ml flask, heat to 80°C with stirring and keep it warm for 1 hour, add 200 grams of 1% carbonic acid at 80°C prepared in advance Sodium solution, stirred for another 10 minutes, transferred to an insulated separatory funnel, left to stand for 30 minutes, separated from the lower layer to separate the clear water layer, the water layer containing the suspended matter layer, and the xylene layer was transferred to the flask, and the xylene was distilled from the water vapor , filtered the aqueous solution, washed, and dried to obtain the product 1,4-dihydroxyanthraquinone, with an internal standard content of 98.5%, a product yield of 48.2 grams (equivalent to 100% purity), a yield of 96.4%, an ash content of 0.07%, and a tar content of 0.12%. Meet the requirements for the use of solvent dyes.

Embodiment 2

[0025] Add 1000 grams of mixed xylene (a mixture of p-xylene, o-xylene, and m-xylene) and 40 grams of crude product 1,4-dihydroxyanthraquinone into a 2000 ml flask, heat to 70°C under stirring and keep it warm for 1.5 hours, add Pre-configured 200 grams of 0.8% potassium carbonate solution at 70°C, stirred for 10 minutes, transferred to an insulated separatory funnel, and stood for 30 minutes to separate the clear water layer from the lower layer, and the water layer containing the suspended matter layer , the mixed xylene layer was transferred to a flask, water vapor was distilled to remove xylene, the aqueous solution was filtered, washed, and dried to obtain the product 1,4-dihydroxyanthraquinone, the internal standard content was 98.2%, and the product yield was 38.7 grams (equivalent to 100% purity) , the yield is 96.8%, the ash content is 0.09%, and the tar content is 0.10%, which meets the requirements for the use of solvent dyes.

Embodiment 3

[0027] Add 1000kg of mixed xylene (a mixture of p-xylene, o-xylene, and m-xylene) and 100kg of crude product 1,4-dihydroxyanthraquinone into a 3000L reactor, heat it to 65°C under stirring and keep it warm for 1.5 hours, add the pre- 1000 kg of 0.5% potassium carbonate solution at 65°C was prepared, then stirred for 10 minutes, transferred to an insulated separatory kettle, left to stand for 30 minutes, and the clear water layer and the water layer containing the suspended matter layer were separated from the lower layer. The mixed xylene layer was transferred to the still, and the xylene was distilled by water vapor. The aqueous solution was filtered, washed, and dried to obtain the product 1,4-dihydroxyanthraquinone. The internal standard content was 98.6%, and the product yield was 97.0kg (equivalent to 100% purity) , the yield is 97.0%, the ash content is 0.07%, and the tar content is 0.08%, which meets the requirements for the use of solvent dyes.

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Abstract

The invention relates to the technical field of fine chemical engineering, in particular to an improved refining process of 1, 4-dihydroxy anthraquinone. The process comprises the following steps: adding xylene into a reaction container to dissolve a 1, 4-dihydroxy anthraquinone crude product until solids are not reduced any more to obtain a 1, 4-dihydroxy anthraquinone crude product solution; adding an aqueous alkali solution into the 1, 4-dihydroxy anthraquinone crude product solution to extract phthalic acid and p-chlorophenolsulfonic acid, and carrying out settling separation to obtain an aqueous alkali layer and an insoluble substance layer so as to obtain a xylene layer; carrying out water vapor distillation on the xylene layer, recycling the obtained xylene solvent, and filtering and washing the remaining aqueous solution to obtain a refined product of 1, 4-dihydroxy anthraquinone. The product treated by the process disclosed by the invention can effectively meet the raw material requirement of solvent dye, basically has no waste, and the yield can reach 95-97%, and even 98-99% according to the internal standard.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to an improved refining process of 1,4-dihydroxyanthraquinone. Background technique [0002] 1,4-Dihydroxyanthraquinone is an important dye intermediate, which can be used in disperse dyes such as disperse blue 60, disperse blue 3, disperse blue 14, disperse blue 72, etc., and can also be used in solvent violet 13 and solvent violet 38 , Solvent Blue 35, Solvent Blue 36, Solvent Blue 104, Solvent Blue 105, Solvent Blue 128, Solvent Blue 132, etc. The synthesis process of 1,4-dihydroxyanthraquinone on the market is phthalic anhydride and p-chlorophenol under the protection of boric acid Condensate in fuming sulfuric acid, and then hydrolyze to obtain the product. The impurities in the product mainly include: phthalic acid, p-chlorophenolsulfonic acid, 1,2,4-trihydroxyanthraquinone, 1-hydroxyanthraquinone, 2-hydroxy Anthraquinone, and tar polymer, ash (such as dust, etc.). As...

Claims

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Application Information

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IPC IPC(8): C07C46/10C07C50/34
CPCC07C46/10C07C50/34
Inventor 许芸霞詹国青
Owner JIANGSU HUAER CHEM
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