Method for preparing 2-ethylanthraquinone by continuous 2-(4-alkylbenzoyl)benzoic acid ring-closing reaction

An alkylbenzoyl, ring-closure reaction technology, applied in the preparation of quinones, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem that 2-(4-ethylbenzoyl)benzoic acid does not reach microscopic mixing, The basic parameters of jet mixing and the complex processing process are not given, so as to achieve the effect of improving the labor environment, reducing equipment investment and simple operation

Inactive Publication Date: 2013-10-23
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN101633613A (2010-01-27) patent introduces the device and process for the continuous production of 2-ethylanthraquinone in a pipeline reactor. ) Benzoic acid did not achieve microscopic mixing in sulfuric acid solution, resulting in low yield, and at the same time, the basic parameters of jet mixing that could be protected were not given in the patent requirements
The process is cumbersome, complicated, labor-intensive, and low yield, so it is necessary to improve the production process

Method used

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  • Method for preparing 2-ethylanthraquinone by continuous 2-(4-alkylbenzoyl)benzoic acid ring-closing reaction
  • Method for preparing 2-ethylanthraquinone by continuous 2-(4-alkylbenzoyl)benzoic acid ring-closing reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 6.0g / min 2-(4-alkylbenzoyl)benzoic acid at 160°C and 15ml / min concentrated sulfuric acid at room temperature into a 250ml stirring mixer and mix, and the liquid 2-(4-alkylbenzoyl) ) The ratio of benzoic acid and concentrated sulfuric acid is 1:2.5, the mixing temperature is controlled at 60°C, the mixture flows into the first stirred reactor in overflow mode, the reactor temperature is controlled at 120°C, the residence time is 5min, and then the Flow into the second stirred reactor, the residence time is 3min, the control reactor temperature is 125°C, and then flow into the third stirred reactor in overflow mode, the residence time is 3min, the control reactor temperature is 120°C ℃. The reaction liquid flowing out from the reactor directly enters the hydrolysis tank for hydrolysis, extracts with an equal amount of toluene, and the oil phase is washed with alkali, washed with water, and distilled to obtain 2-ethylanthraquinone with a yield of 80.2%.

Embodiment 2

[0029] Add 5.0g / min 2-(4-alkylbenzoyl)benzoic acid at 180°C and 11ml / min concentrated sulfuric acid at room temperature into a 250ml stirring mixer and mix, and the liquid 2-(4-alkylbenzoyl) ) The ratio of benzoic acid and concentrated sulfuric acid is 1:2.2. Control the mixing temperature at 40°C, the mixture flows into the first stirred reactor in an overflow manner, control the reactor temperature at 110°C, and the residence time is 4min, and then flow into the second stirred reactor in an overflow manner, and stay The time is 3 minutes, the temperature of the reactor is controlled at 130°C, and then it flows into the third stirred reactor in overflow mode, the residence time is 1min, and the temperature of the reactor is controlled at 140°C. The reaction liquid flowing out from the reactor directly enters the hydrolysis tank for hydrolysis, and is extracted with an equal amount of toluene. The oil phase is washed with alkali, washed with water, and distilled to obtain 2-et...

Embodiment 3

[0031]Add 4.0g / min 2-(4-alkylbenzoyl)benzoic acid at 140°C and 7.6ml / min concentrated sulfuric acid at 60°C to a 250ml stirring mixer for mixing, and the liquid 2-(4-alkylbenzene The ratio of formyl)benzoic acid to concentrated sulfuric acid is 1:1.9. Control the mixing temperature at 50°C, the mixture flows into the first stirred reactor in an overflow manner, control the reactor temperature at 110°C, and the residence time is 5min, and then flow into the second stirred reactor in an overflow manner, and stay The time is 3 minutes, and the temperature of the reactor is controlled at 130°C. The reaction liquid flowing out from the reactor directly enters the hydrolysis tank for hydrolysis, extracts with an equal amount of toluene, and the oil phase is washed with alkali, washed with water, and distilled to obtain 2-ethylanthraquinone with a yield of 82.5%.

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Abstract

The invention discloses a method for preparing 2-ethylanthraquinone by continuous 2-(4-alkylbenzoyl)benzoic acid ring-closing reaction, which comprises the following steps: mixing liquid 2-(4-alkylbenzoyl)benzoic acid and room-temperature concentrated sulfuric acid in a mixer in a mass-volume ratio of 1:1.5-1:2.5, wherein the mixing temperature is room temperature to 100 DEG C, and the retention time of the mixture in the mixer is 1-10 minutes; connecting the mixer with a stirring reactor, and carrying out ring-closing reaction, wherein the temperature of the stirring reactor is 100-140 DEG C, and the retention time of the reaction materials in the reactor is 5-30 minutes; and directly hydrolyzing the liquid after reaction, extracting, and distilling to obtain the 2-ethylanthraquinone. The detailed method is disclosed in the specification. The process is simple to operate and easy to control, lowers the labor intensity, improves the working environment, reduces the equipment investment, lowers the waste acid quantity, and enhances the product yield by 5-10% as compared with the existing production technique; and the product quality is good.

Description

technical field [0001] The invention belongs to the production process of fine chemical products, in particular to a method for preparing 2-ethylanthraquinone by continuous 2-(4-alkylbenzoyl) benzoic acid ring-closing reaction. Background technique [0002] 2-Ethylanthraquinone is a light yellow powder or bright yellow scale solid, which is an important fine chemical raw material, mainly used as a hydrogen peroxide synthesis catalyst, and also used to prepare photosensitive compounds, dyes, 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. [0003] At present, the methods for producing 2-ethylanthraquinone mainly include: (1) Direct oxidation of ethylanthracene: This method uses hydrochloric acid as a catalyst, and hydrogen peroxide is used to oxidiz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/16C07C46/00
Inventor 靳海波刘泉军郭志武杨索和何广湘
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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