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2-(4-pentylbenzoyl)benzoic acid and 2-pentylanthraquinone and preparation method thereof

A technology of amyl benzoyl and amyl anthraquinone, applied in the field of fine chemicals, can solve the problems of affecting yield, cumbersome operating conditions, increasing separation cost, etc., and achieve the effect of improving tertiary-secondary ratio and good economic value

Active Publication Date: 2020-11-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of adding an acid-binding agent to the reaction system needs to add new substances, which increases the cost of separation; and the operating conditions are cumbersome and affect the yield

Method used

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  • 2-(4-pentylbenzoyl)benzoic acid and 2-pentylanthraquinone and preparation method thereof
  • 2-(4-pentylbenzoyl)benzoic acid and 2-pentylanthraquinone and preparation method thereof

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preparation example Construction

[0017] The embodiment of the present invention provides a kind of preparation method of 2-(4-pentylbenzoyl) benzoic acid, comprising: phthalic anhydride, solvent, Friedel-Crafts reaction catalyst and tert-amylbenzene in high gravity reactor During the reaction, a working gas that does not participate in the reaction is introduced during the reaction.

[0018] The inventor creatively adopts a high-gravity reactor to carry out the reaction, and introduces working gas during the reaction process, which significantly increases the tertiary-secondary ratio of ABB acid. This may be due to the fact that the reactant can be torn into micron or nano-scale micelles in the hypergravity device, and the distance of the liquid phase body through which hydrogen chloride is transferred to the gas phase body is short and the mass transfer speed is fast; The renewal speed of the gas-liquid phase interface is fast, and the mass transfer driving force is strong, so that the isomerization effect o...

Embodiment 1

[0033] The present embodiment provides a kind of preparation method of 2-(4-pentylbenzoyl)benzoic acid, comprises the steps:

[0034]In a 120L container, add 8kg of phthalic anhydride to 33L of o-dichlorobenzene, stir and control the temperature to 20°C. Add 19.3 kg of anhydrous aluminum trichloride to the mixture of phthalic anhydride and o-dichlorobenzene three times, and keep the temperature of 8.8 kg of tert-amylbenzene at 20°C. Turn on the supergravity device, maintain the supergravity factor of the supergravity device at 80G, and pass the mixture of phthalic anhydride, aluminum trichloride and o-dichlorobenzene at a speed of 5.95L / min and tert-amylbenzene at 1L / min. The liquid inlet of the supergravity device is fed in, and at the same time, 30L / min of dry nitrogen is countercurrently fed into the gas inlet of the supergravity device, and the inner diameter of the supergravity reactor is 50cm.

[0035] Pour the reaction mixture into an appropriate amount of dilute sulfu...

Embodiment 2

[0037] The present embodiment provides a kind of preparation method of 2-(4-pentylbenzoyl)benzoic acid, comprises the steps:

[0038] In a 120L container, add 8kg of phthalic anhydride to 33L of o-dichlorobenzene, stir and control the temperature to 0°C. Add 19.3 kg of anhydrous aluminum trichloride to the mixture of phthalic anhydride and o-dichlorobenzene three times, and keep the temperature of 8.8 kg of tert-amylbenzene at 0°C. Turn on the supergravity device, maintain the supergravity factor of the supergravity device at 60G, and pass the mixture of phthalic anhydride, aluminum trichloride and o-dichlorobenzene at a speed of 5.95L / min and tert-amylbenzene at 1L / min. The liquid inlet of the supergravity device is fed in, and at the same time, 20L / min of dry nitrogen is countercurrently fed into the gas inlet of the supergravity device, and the inner diameter of the supergravity reactor is 50cm.

[0039] Pour the reaction mixture into an appropriate amount of dilute sulfur...

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Abstract

The invention discloses 2-(4-pentylbenzoyl)benzoic acid and 2-pentylanthraquinone and preparation methods thereof, and relates to the technical field of fine chemicals. The preparation method of the 2-(4-pentylbenzoyl)benzoic acid with the high tert-sec ratio comprises the following steps: reacting phthalic anhydride, a solvent, a Friedel-Crafts reaction catalyst and tert-pentylbenzene in a supergravity reactor, and introducing a working gas in the reaction process. After the reaction, the tertiary-to-secondary ratio of the ABB acid is remarkably increased, so that the prepared 2-pentylanthraquinone also has high tertiary-to-secondary ratio. This may be caused by that reactants can be torn into micron-scale or nano-scale micelles in the supergravity device, the distance of the liquid-phasemain body through which hydrogen chloride is transferred to the gas-phase main body is short, hydrogen chloride gas generated in the reaction process can be effectively removed and the isomerizationreaction amount is reduced, and therefore, the tertiary-secondary ratio of the product is increased.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, and in particular to 2-(4-pentylbenzoyl)benzoic acid and 2-pentylanthraquinone and a preparation method thereof. Background technique [0002] 2-(4-Pentylbenzoyl)benzoic acid (ABB acid for short) is a white solid powder, which is an intermediate in the synthesis of 2-pentylanthraquinone from phthalic anhydride and tert-amylbenzene, 2-pentyl Anthraquinone is mainly used as a catalyst for the synthesis of hydrogen peroxide. The by-product HCl produced in the process of catalyzing the synthesis of ABB acid from phthalic anhydride and tert-amylbenzene can catalyze the isomerization reaction of tert-amyl groups to generate sec-pentyl groups, and then form 2-(4-sec-pentyl Benzoyl) benzoic acid further forms 2-sec-amylanthraquinone. Compared with 2-tert-amylanthraquinone, 2-sec-amylanthraquinone has lower solubility and lower hydrogenation efficiency in the working solution of synthetic hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/083C07C65/34C07C46/00C07C50/16
CPCC07C51/083C07C46/00C07C65/34C07C50/16
Inventor 师新阁左世伟胡汉国尚尔顺李克文
Owner CHINA PETROLEUM & CHEM CORP