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Method for separating and purifying 2-ethyl anthraquinone from sulphuric acid

A technology of ethyl anthraquinone and sulfuric acid, applied in quinone separation/purification, organic chemistry, etc., can solve problems such as long process time, difficult process control, and poor working environment, so as to improve operational safety, improve operating environment, reduce The effect of material loss

Active Publication Date: 2011-05-11
山东门捷新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of this conventional post-treatment process are: (1) the process time is long, and the whole production process needs 32 hours; (2) the labor intensity is high, and a lot of labor is required; Because the drying process and drying process are all carried out in the open, the dust is relatively large and the working environment is poor; (4) The product quality is unstable and the process control is difficult. Problems such as color deviation, high acidity, high residue, and high content of trace impurities such as sulfur, chlorine, and iron in the product; (5) high energy consumption and high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add the measured water into the acid analysis kettle with a cooling water jacket, turn on the stirring and cooling water, and slowly put the 2-ethylanthraquinone concentrated sulfuric acid solution obtained by the ring-closing reaction into the acid analysis kettle at a uniform speed for acidification. Analysis, acid analysis into 36wt% 2-ethylanthraquinone sulfuric acid solution, the temperature is controlled between 98 ° C, after the acid analysis is completed, the cooling water is adjusted according to the temperature, and the temperature of the acid analysis solution is kept ≥ 70 ° C.

[0023] (2) Put the feed liquid after acid analysis into the extraction tower for extraction, enter the extraction tower at a constant speed from the upper entrance of the extraction tower, pass the toluene through the extraction tower at a constant speed from the bottom of the extraction tower, and the feed liquid from the top to bottom of the extraction tower After the countercur...

Embodiment 2

[0030] (1) Add the measured water into the acid analysis kettle with a cooling water jacket, turn on the stirring and cooling water, and slowly put the 2-ethylanthraquinone concentrated sulfuric acid solution obtained by the ring-closing reaction into the acid analysis kettle at a uniform speed for acidification. Analysis, acid analysis into 38wt% 2-ethylanthraquinone sulfuric acid solution, the temperature is controlled between 102 ° C, after the acid analysis is completed, the cooling water is adjusted according to the temperature, and the temperature of the acid analysis solution is kept ≥ 70 ° C.

[0031] (2) Put the material liquid after acid analysis into the extraction tower for extraction, enter the extraction tower at a constant speed from the upper inlet of the extraction tower, pass the xylene through the extraction tower at a constant speed from the bottom of the extraction tower, and mix the top-down material of the extraction tower The countercurrent extraction of...

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Abstract

The invention discloses a method for separating and purifying 2-ethyl anthraquinone from sulphuric acid. The method comprises the following steps of: slowly adding a 2-ethyl anthraquinone concentrated sulphuric acid solution obtained by a closed-loop reaction to well-measured water to carry out acid separation; carrying out countercurrent extraction to the feed liquid subjected to acid separationand an extraction solvent at a temperature of 75-80 DEG C, separating a small amount of dilute sulphuric acid contained in the extract liquor from the 2-ethyl anthraquinone obtained through extraction; then, respectively carrying out caustic washing and rinsing to separate a small amount of water contained in the feed liquid; and finally, respectively carrying out room-pressure distillation and reduced-pressure distillation in a distillation kettle to obtain product of 2-ethyl anthraquinone. The invention utilizes an extraction principle and a reduced-pressure distillation principle for the post-treatment of the 2-ethyl anthraquinone concentrated sulphuric acid solution so as to lighten the labor intensity, improve the operating environment, enhance the operation safety, decrease the production cost and shorten the production flow of the post-treatment, and the product obtained through separation has high purity and stable quality.

Description

technical field [0001] The invention relates to a post-treatment process in the production process of 2-ethylanthraquinone, in particular to a method for separating and purifying 2-ethylanthraquinone from sulfuric acid. Background technique [0002] 2-Ethylanthraquinone is an important fine chemical raw material, mainly used as a catalyst for the synthesis of hydrogen peroxide, and also used in the preparation of photosensitive compounds, fuels, optical sieve resins, pharmaceutical and pesticide intermediates and other fields. With the increasing demand for hydrogen peroxide, especially the rapid development of the paper industry, 2-ethylanthraquinone has become a fine chemical with considerable development potential. The current industrial production method of 2-ethylanthraquinone mainly includes two steps: ethylbenzene and phthalic anhydride are dissolved in anhydrous AlCl 3 or HBF 4 Under the action of , the intermediate product 2-(4-ethylbenzoyl)benzoic acid (EBA) is o...

Claims

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Application Information

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IPC IPC(8): C07C50/18C07C46/10
Inventor 赵新良刘泉军
Owner 山东门捷新材料股份有限公司
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