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Method for synthesizing 2-ethylanthraquinone by taking heteropoly acid intercalated hydrotalcite as catalyst

A technology of ethyl anthraquinone and heteropoly acid, applied in the field of preparation of 2-ethyl anthraquinone, can solve equipment and environmental hazards, the production scale and product quality cannot be satisfied, and restrict the industrial production scale of 2-ethyl anthraquinone Normal development and other problems, to achieve the effect of improving separation efficiency and less dosage

Inactive Publication Date: 2018-06-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the rapid development of the hydrogen peroxide industry, the demand for 2-ethylanthraquinone has increased rapidly, but its production scale and product quality cannot meet the demand for 2-ethylanthraquinone in my country's hydrogen peroxide industry
[0003] The traditional production process of 2-ethylanthraquinone uses oleum as a catalyst, and a large amount of waste acid will be produced during the production process. The by-product of 1 ton of 2-ethylanthraquinone is 8-10 tons of waste acid with a concentration of 30-50%. , the waste acid contains a large amount of organic matter, which not only causes serious harm to equipment and the environment, but also the cost of harmless treatment of the waste acid is extremely high, which seriously restricts the industrial production scale of 2-ethylanthraquinone and the normal development of enterprises, so The development of new catalytic processes to replace traditional production processes has become the focus and hotspot of research in this field
[0007] The synthesis of 2-ethylanthraquinone by dehydration and ring closure of 2-(4'-ethylbenzoyl)benzoic acid adopts the Friedel-Crafts acylation reaction catalyzed by proton acid or Lewis acid, and its reaction mechanism is similar to that of esterification reaction. Differently, the application of heteropoly acid intercalated hydrotalcite to Friedel-Crafts acylation reaction has not been reported yet.

Method used

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  • Method for synthesizing 2-ethylanthraquinone by taking heteropoly acid intercalated hydrotalcite as catalyst
  • Method for synthesizing 2-ethylanthraquinone by taking heteropoly acid intercalated hydrotalcite as catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Catalyst preparation: prepare 15mmol MgCl 2 and 7.5mmol AlCl 3 75 mL of the mixed salt solution, and then prepare 0.5M 75ml tris solution, add the tris solution into the mixed salt solution, mix and stir for 0.5 hours, and conduct a hydrothermal reaction at 80°C for 12 hours. Gel material was obtained by centrifugation, in 0.5M Na 2 CO 3 dispersed in the solution, ion-exchanged for 1 hour, centrifuged and washed, and vacuum-dried to obtain magnesium-aluminum carbonate hydrotalcite for future use. Prepare 100mL of phosphotungstic acid sodium salt solution with a concentration of 1.1mM, add 2.3g of magnesium aluminum carbonate hydrotalcite to it, stir for 12 hours under the protection of no nitrogen, centrifuge, wash, and vacuum dry to obtain phosphotungstic acid intercalated trihydroxy Methyl hydrotalcite, the chemical formula is Mg 9 Al 3 (OH) 15 (C 4 h 8 NO 3 )(PW 12 o 40 ).

[0024] A. Catalytic synthesis of 2-ethylanthraquinone: Add 5.0g of 2-(4'-ethylben...

Embodiment 2

[0027]Catalyst preparation: change phosphotungstic acid sodium salt solution to silicotungstic acid sodium salt solution, and other conditions are the same as the catalyst preparation in Example 1 to obtain silicotungstic acid intercalated trimethylol hydrotalcite, the chemical formula is Mg 9 al 3 (OH) 14 (C 4 h 8 NO 3 )(SiW 12 o 40 ).

[0028] A. Catalytic synthesis of 2-ethylanthraquinone: Add 5.0g 2-(4′-ethylbenzoyl)benzoic acid into the reactor, add 50mL chloroform to fully dissolve, add 7.0g silicotungstic acid to intercalate trihydroxy Methyl hydrotalcite catalyst, after stirring for 15 minutes, the temperature was raised to 70°C to dechloroform, and the temperature was raised to 130°C to make the BE acid into a molten state, so that the molten BE acid was evenly adsorbed on the surface and layer of the catalyst. Then the temperature was raised to 180° C., and the reaction was carried out for 2.0 hours. Cool to room temperature, add 50mL of toluene to fully diss...

Embodiment 3

[0031] Catalyst preparation: change phosphotungstic acid sodium salt solution to phosphomolybdic acid sodium salt solution, and other conditions are the same as the catalyst preparation in Example 1 to obtain phosphomolybdic acid intercalated trimethylol hydrotalcite, the chemical formula is Mg 9 al 3 (OH) 15 (C 4 h 8 NO 3 ) (PMo 12 o 40 ).

[0032] A. Catalytic synthesis of 2-ethylanthraquinone: Add 5.0g 2-(4'-ethylbenzoyl)benzoic acid into the reactor, add 50mL chloroform to fully dissolve, add 5.0g phosphomolybdic acid to intercalate trihydroxy Methyl hydrotalcite catalyst, after stirring for 15 minutes, heat up to 70°C to remove the solvent chloroform, then heat up to 130°C to make the BE acid into a molten state, so that the molten BE acid is evenly adsorbed on the surface and layer of the catalyst, then heat up to 180°C, and react 2.0 hours. Cool to room temperature, add 50mL of toluene to fully dissolve the product, separate by filtration to obtain catalyst and ...

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Abstract

The invention discloses a method for synthesizing 2-ethylanthraquinone by taking heteropoly acid intercalated hydrotalcite as a catalyst. According to the method, the 2-ethylanthraquinone is producedin a closed-loop manner through enabling 2-(4'-ethylbenzoyl)benzoic acid, which serves as a raw material, to react for 1.0 to 4.0 hours at the temperature of 180 DEG C to 250 DEG C in the presence ofthe heteropoly acid intercalated trihydroxymethyl hydrotalcite, which serves as the catalyst. The adopted heteropoly acid intercalated trihydroxymethyl hydrotalcite catalyst is prepared through takingtrihydroxymethyl modified magnalium hydrotalcite as a precursor and carrying out ion exchange with heteropoly acid. According to the method, the defect in the prior art that a large volume of unmanageable waste acid is generated due to fuming sulfuric acid is avoided.

Description

technical field [0001] The invention belongs to the technical field of synthetic chemical engineering, and in particular relates to a preparation method of 2-ethylanthraquinone. technical background [0002] 2-Ethylanthraquinone (2-EAQ) is an important organic intermediate widely used in the preparation of hydrogen peroxide, optical sieve resins, photosensitive polymerizers and dye intermediates. With the rapid development of the hydrogen peroxide industry, the demand for 2-ethylanthraquinone has increased rapidly, but its production scale and product quality cannot meet the demand for 2-ethylanthraquinone in my country's hydrogen peroxide industry. [0003] The traditional production process of 2-ethylanthraquinone uses oleum as a catalyst, and a large amount of waste acid will be produced during the production process. The by-product of 1 ton of 2-ethylanthraquinone is 8-10 tons of waste acid with a concentration of 30-50%. , the waste acid contains a large amount of orga...

Claims

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Application Information

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IPC IPC(8): C07C50/18C07C46/00B01J31/34B01J27/188B01J27/19B01J37/10B01J37/30
CPCB01J27/188B01J27/19B01J31/34B01J37/10B01J37/30C07C46/00C07C50/18
Inventor 冯拥军谢浩杰李殿卿李宏宇唐平贵
Owner BEIJING UNIV OF CHEM TECH
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