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Synthesis method of 2-ethylanthraquinone

A technology for the synthesis of ethyl anthraquinone, which is applied in chemical instruments and methods, preparation of quinones, preparation of organic compounds, etc., can solve the problems of high labor intensity, complicated processing, cumbersome process, etc., and achieve stable product quality, Simple operation and easy transition effects

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

AI Technical Summary

Problems solved by technology

[0004] CN 1315768C (2007-05-16) and CN 1879965A (2006-12-20) patents introduce the use of solid acid as a catalyst to catalyze the dehydration and ring closure of 2-(4-ethylbenzoyl)benzoic acid to generate 2-alkylanthraquinone The method is a liquid phase reaction, the physical properties of which directly affect the catalytic effect of the catalyst, and the regeneration of the catalyst is difficult
[0005] CN101633613A (2010-01-27) patent and Luo Zhi et al. (Science and Technology Information, 2009, vol 19, 11-12) respectively introduced the device and process for the continuous production of 2-ethylanthraquinone in a pipeline reactor, which is still the original The transformation of some technological processes cannot eliminate waste sulfuric acid
The process is cumbersome, complicated, labor-intensive, and low-yield, which requires the process to be reformed to achieve the purpose of clean production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 30g of 2-(4-alkylbenzoyl)benzoic acid into a 250ml vaporization chamber, control the temperature at 300°C, add 5g of hydrogen-type mordenite catalyst into the fixed-bed reactor, and control the reactor temperature at 280°C. The system vacuum is controlled at 8mmHg. After the raw material is gasified, it enters the fixed-bed reactor for reaction. After the reaction time is controlled at 20s, the material flowing out from the fixed-bed reactor directly enters the condensation tube to condense to obtain the crude product. Then it was extracted with an equal amount of toluene, and the oil phase was washed with alkali, washed with water and distilled to obtain 2-ethylanthraquinone with a yield of 84.3%. The deactivated catalyst was calcined at 500°C for 3 hours in a fixed bed and reused.

Embodiment 2

[0018] Add 30g of 2-(4-alkylbenzoyl)benzoic acid into a 250ml vaporization chamber, control the temperature at 330°C, add 4g of Hβ catalyst into the fixed bed reactor, and control the temperature of the reactor at 300°C. The system vacuum is controlled at 10mmHg. After the raw material is gasified, it enters the fixed bed reactor for reaction. After the reaction time is controlled at 60s, the material flowing out from the fixed bed reactor directly enters the condenser tube to condense to obtain the crude product. Then it was extracted with an equal amount of toluene, and the oil phase was washed with alkali, washed with water and distilled to obtain 2-ethylanthraquinone with a yield of 86.7%. The deactivated catalyst was calcined at 500°C for 3 hours in a fixed bed and reused.

Embodiment 3

[0020] Add 30g of 2-(4-alkylbenzoyl)benzoic acid into a 250ml vaporization chamber, control the temperature at 350°C, add 4g of HY catalyst into the fluidized bed reactor, and control the temperature of the reactor at 320°C. The system vacuum is controlled at 9mmHg. After the raw material is gasified, it enters the fluidized bed reactor for reaction. After the reaction time is controlled at 120s, the material flowing out from the fluidized bed reactor directly enters the condenser tube to condense to obtain the crude product. Then it was extracted with an equal amount of toluene, and the oil phase was washed with alkali, washed with water and distilled to obtain 2-ethylanthraquinone with a yield of 85.8%. The deactivated catalyst was calcined at 500°C for 3 hours in a fluidized bed and reused.

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Abstract

The invention discloses a synthesis method of 2-ethylanthraquinone, which comprises the following steps: gasifying 2-(4-alkylbenzoyl)benzoic acid in a gasification chamber under reduced pressure while controlling the temperature at 230-370 DEG C; carrying out gasification reaction on the 2-(4-alkylbenzoyl)benzoic acid reactant in the gaseous form through a catalyst bed composed of acidic molecular sieves, wherein the temperature of the reactor is controlled at 220-350 DEG C, the reaction time is 10-240 seconds, and the reaction pressure is 5-20 mmHg; and cooling the reaction product, extracting, washing with alkali, washing with water, and distilling to obtain the 2-ethylanthraquinone. The detailed method is disclosed in the specification. The invention has the advantages of clean production, no generation of waste acid and pollutants, high yield and stable product quality, and is simple to operate; and the conversion rate of the reactant 2-(4-alkylbenzoyl)benzoic acid can reach 90% above, and the purity of the product 2-ethylanthraquinone can reach 98.5% above.

Description

technical field [0001] The invention belongs to the production process of fine chemical products, and in particular relates to a synthesis method of 2-ethylanthraquinone. 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. In this method, hydrochloric acid is used as a catalyst, and hydrogen peroxide is used to oxidize 2-ethylanthracene in liquid phase to generate 2...

Claims

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Application Information

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IPC IPC(8): C07C50/16C07C46/00
Inventor 靳海波孔岩郭志武杨索和何广湘
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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