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Preparation and purification method for 2-tert-amylanthraquinone

A technology of tert-amylanthraquinone and solvent, which is applied in the field of production and purification of 2-tert-amylanthraquinone, and can solve problems affecting the yield and purity of amylanthraquinone, affecting the reaction rate, affecting the production cost and yield of hydrogen peroxide, etc. , to achieve the effects of low incidence of side reactions, uniform reaction, and increased product purity

Active Publication Date: 2017-09-15
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of hydrogen peroxide by the anthraquinone method mainly uses 2-alkylanthraquinone as the main carrier. At present, most companies use 2-ethylanthraquinone. Compared with 2-ethylanthraquinone, 2-tert-amylanthraquinone has obvious advantages Compared with the two, the solubility of 2-tert-amylanthraquinone in the working solution is larger than that of 2-ethylanthraquinone, which affects the subsequent reaction rate, thus affecting the production cost and yield of hydrogen peroxide
[0003] The preparation of 2-tert-amyl anthraquinone is mainly obtained by dehydration of 2-(4'-tert-amylbenzoyl)benzoic acid through oleum. In patent CN104262124, ABB acid is melted and then added to oleum. This method is simple to operate and has low cost, but the yield of amyl anthraquinone is about 70-80%, and it is easy to form carbonized impurities of tar in the process of dehydration, which affects the yield and purity of amyl anthraquinone.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 5g of phosphorus pentoxide and 100g of trifluoroacetic acid into the reaction kettle and heat up to 90°C. Weigh 50g of ABB acid and dissolve it in 350g of dichloroethane for later use. When the temperature in the kettle reaches 95°C, add dichloride of ABB acid dropwise Ethane solution, dropwise time 20min, after dropwise addition, keep warm at 90°C for 1.5 hours, cool naturally after heat preservation, add the reaction solution into 350g of cold water, stir for 0.5h, let it stand for stratification, collect the solvent layer, add 17.5g of activated carbon , the temperature was raised to 60° C. for 0.5 h, the temperature was naturally lowered, the filtrate was distilled and crystallized after filtering the reaction solution to obtain 2-tert-amylanthraquinone product, the total yield was 85.5%, and the purity of amylanthraquinone quantified by liquid chromatography was 98.7%. After the recovered activated carbon was washed with dichloroethane distilled out, it was dr...

Embodiment 2

[0029] Weigh 6g of phosphorus pentoxide and 125g of trifluoroacetic acid into the reaction kettle and heat up to 90°C. Weigh 50g of ABB acid and dissolve it in 500g of dichloroethane for later use. When the temperature in the kettle reaches 90°C, add dichloride of ABB acid dropwise Ethane solution, the dropwise addition time is 30min. After the dropwise addition is completed, the temperature is kept at 90°C for 1 hour. After the heat preservation is completed, it is cooled naturally. A total of 50g of new activated carbon was added to the recovered activated carbon for adsorption, the temperature was raised to 60°C for 1 hour, and the temperature was naturally lowered. After filtering the reaction solution, the filtrate was distilled and crystallized to obtain 2-tert-amylanthraquinone. The product yield was 87.5%. Quantitatively, the purity of amyl anthraquinone is 99.0%. After the recovered activated carbon is washed with dichloroethane distilled out, it is dried and roasted t...

Embodiment 3

[0031] Weigh 5g of phosphorus pentoxide and 100g of trifluoroacetic acid into the reaction kettle and heat up to 105°C, weigh 50g of ABB acid and dissolve it in 400g of trichloroethane for later use. When the temperature in the kettle reaches 105°C, add dropwise the trichloro Ethane solution, dropwise time 20min, after dropwise addition, keep warm at 105°C for 1 hour, cool down naturally after warming up, add the reaction solution into 400g cold water, stir for 0.5h, let stand to separate and collect the solvent layer, add recovered activated carbon 32g , the temperature was raised to 55° C. for 1.5 h, and the temperature was naturally lowered. After the reaction liquid was filtered, the filtrate was distilled and crystallized to obtain 2-tert-amylanthraquinone product with a total yield of 89.5%. The purity of amylanthraquinone quantified by liquid chromatography was 98.9%. After the recovered activated carbon was washed with dichloroethane distilled out, it was dried and calc...

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Abstract

The invention discloses a preparation and purification method for 2-tert-amylanthraquinone. The method includes: subjecting phosphorus pentoxide and trifluoroacetic acid to mixed heating to certain temperature, dissolving 2-(4'-tert-amylbenzoyl)benzoic acid (called ABB acid for short) with a solvent and then adding the product dropwise into the mixed phase, performing mixing and then carrying out reaction at certain temperature, at the end of the reaction, pouring the reaction liquid into cold water, conducting standing and layering, collecting the oil layer, then adding a certain amount of an adsorbent for adsorption of tar impurities at certain temperature, then performing filtering, and subjecting the filtrate to distillation crystallization, thus obtaining a high purity 2-tert-amylanthraquinone product. The method provided by the invention has the advantages of mild reaction conditions, simple operation, few side reaction, and recyclability of adsorbent, and lowers the separation cost.

Description

technical field [0001] The invention relates to a method for producing and purifying 2-tert-amylanthraquinone, and relates to the field of chemical raw material production. Background technique [0002] Hydrogen peroxide is an important green and environmental protection chemical, which has very important uses in medical treatment, civil use and industry. At present, the main method for producing hydrogen peroxide is the anthraquinone method, which has low production cost, less energy consumption and is easy to produce on a large scale. The production of hydrogen peroxide by the anthraquinone method mainly uses 2-alkylanthraquinone as the main carrier. At present, most companies use 2-ethylanthraquinone. Compared with 2-ethylanthraquinone, 2-tert-amylanthraquinone has obvious advantages Compared with the two, the solubility of 2-tert-amylanthraquinone in the working solution is larger than that of 2-ethylanthraquinone, which affects the subsequent reaction rate, thereby aff...

Claims

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Application Information

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IPC IPC(8): C07C46/10C07C50/18
CPCC07C46/10C07C50/18
Inventor 李进王蕊王庆吉王炳春王建青
Owner CHINA CATALYST HLDG CO LTD
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