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Separating and purifying method for 2-(4-ethyl benzene formyl) benzoic acid

A technology of ethyl benzoyl and purification method, which is applied in the field of separation of 2-benzoic acid, can solve the problems of large water consumption, high energy consumption, and low purity of BE acid, and achieve the effect of saving resources and reducing energy consumption

Inactive Publication Date: 2016-07-20
北京恒石尚德科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. The solubility of aluminum trichloride in water is limited, and aluminum trichloride cannot be completely back-extracted into the water phase, resulting in the final BE acid still containing a certain amount of aluminum salt, resulting in low purity of BE acid, which affects the subsequent reaction 2 - Yield and purity of ethyl anthraquinone, and need to consume a lot of water in the washing process;
[0007] 2. Due to the high boiling point of the solvent chlorobenzene, the method of removing the solvent by evaporation requires high temperature heating, which consumes a lot of energy and does not meet the requirements of energy saving and emission reduction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Add 500g (about 4.6mol) of chlorobenzene into a four-necked flask with a stirrer, then add 148g (about 1.0mol) of phthalic anhydride and 270g (about 2.03mol) of anhydrous aluminum chloride in sequence, start stirring, and control the stirring rate 180r / min, keep the temperature at 25°C, slowly and evenly add 117g (about 1.1mol) of ethylbenzene at a rate of 5ml / min, after adding ethylbenzene, raise the liquid temperature of the material to 60°C, and react At the beginning, hydrochloric acid vapor escaped, and the hydrogen chloride gas escaped was absorbed by alkali. The reaction time was 3 hours. After no hydrogen chloride gas escaped, the reaction stopped, and a reaction solution containing BE acid was obtained.

Embodiment 2

[0048] Take 100ml of the reaction solution obtained in Example 1, add the reaction system to 110ml of hydrochloric acid aqueous solution with a molar concentration of 0.1mol / L, stir at 60°C for 30min and then let stand for 10 minutes to separate layers, after layering, the water phase is colorless and transparent , the organic phase was reddish-brown, and then separated using a separatory funnel. The separated organic phase was placed in a -15°C environment and frozen for 1 hour. A large number of white and slightly yellow granular crystals were precipitated, and the precipitated BE was centrifuged. acid crystals and dried at 80 °C for 1 hour to obtain dry, pure BE acid crystals. Reclaim the supernatant chlorobenzene clear liquid to continue to be used in the reaction of synthetic BE acid.

[0049] In the present invention, Elit E3100 high-performance liquid chromatography is used to detect the product purity, and the yield is calculated to obtain a product purity of 98.5% and...

Embodiment 3

[0051] Get 100ml of the reaction solution obtained in Example 1, add the reaction system to 80ml of aqueous hydrochloric acid solution with a molar concentration of 0.3mol / L, stir at 90°C for 45min and then let stand for 5 minutes. After layering, the aqueous phase is colorless and transparent, organic The phase is reddish-brown, and then use a separatory funnel to separate the liquid, and freeze the separated organic phase at -5°C for 2 hours, and a large number of white slightly yellow granular crystals are precipitated, and the precipitated BE acid crystals are separated by centrifugation , and dried at 80 °C for 1.5 h to obtain dry, pure BE acid crystals. Reclaim the supernatant chlorobenzene clear liquid to continue to be used in the reaction of synthetic BE acid.

[0052] Use Elite E3100 high performance liquid chromatography to detect the product purity, and calculate the yield, the product purity is 98%, and the BE acid yield is 96%.

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Abstract

The invention discloses a separating and purifying method for 2-(4-ethyl benzene formyl) benzoic acid (BE acid for short).An aqueous hydrochloric acid solution is adopted as a stripping agent, a reaction system with chlorobenzene as solvent for synthesizing the BE acid is washed at certain temperature, separated liquid stands after washing, organic phases obtained through separation are put at the low temperature to be cooled and crystallized, and by means of centrifugation and drying, BE acid crystals with high purity are obtained.The method is simple, operation is easy, alchlor in chlorobenzene can be completely removed, selectivity precipitation of the BE acid is achieved, the method can replace a traditional evaporation technology, the product yield and purity are high, the energy consumption is low, and the method is an ideal technology for separating and purifying the BE acid.

Description

technical field [0001] The invention relates to the technical field of compound separation and purification, in particular to a separation method of 2-(4-ethylbenzoyl)benzoic acid. Background technique [0002] 2-Ethylanthraquinone (2-EAQ) is an important intermediate in organic synthesis. It is the carrier for the production of hydrogen peroxide by anthraquinone method. It is also an important raw material for the production of photosensitive compounds, dyes and degradable resins. It is widely used in the manufacture of hydrogen peroxide, Vat dyes, disperse dyes, reactive dyes, etc. [0003] At present, large-scale hydrogen peroxide manufacturers at home and abroad use the anthraquinone method to manufacture hydrogen peroxide. The output and quality of 2-ethylanthraquinone greatly affect the development of hydrogen peroxide production and related industries. The annual demand growth rate of hydrogen peroxide in the North American paper industry is 18%, and the annual deman...

Claims

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Application Information

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IPC IPC(8): C07C51/083C07C51/42C07C51/43C07C65/34
CPCC07C51/083C07C51/42C07C51/43
Inventor 丁溪锋刘志勇武昉王树忠闫福顺闫明生李雪萍
Owner 北京恒石尚德科技有限公司
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