Method for preparing 2-alkylanthraquinone with microchannel continuous reactor

A technology of microchannel reactor and alkylanthraquinone, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, quinone preparation, etc., can solve the problem of 2-(4-alkylbenzoyl)benzoic acid Micro-mixing is not achieved, the basic parameters of jet mixing are not given, and the processing process is complicated, etc., to achieve the effect of improving the working environment, reducing equipment investment, and simple process operation

Inactive Publication Date: 2018-04-06
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] CN101633613A (2010-01-27) patent introduces the device and process of continuous production of 2-alkylanthraquinone in pipeline reactor. The patent adopts Y-type jet mixer, and there are some 2-(4-alkylbenzoyl ) 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
However, there are problems such as cumbersome process, complicated treatment process, high labor intensity and low yield in this process, and the production process needs to be improved.

Method used

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  • Method for preparing 2-alkylanthraquinone with microchannel continuous reactor

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Embodiment 1

[0028] 2-(4-ethylbenzoyl)benzoic acid at 140° C. was continuously added to the T-type mixer I at a flow rate of 6.0 g / min and concentrated sulfuric acid at room temperature at a flow rate of 15 ml / min to mix, and the liquid 2- The mass (g) of (4-ethyl benzoyl) benzoic acid and concentrated sulfuric acid: the volume (ml) ratio is 1: 2.5, and the control mixing temperature is 50 ℃, and the mixture flows into the microchannel reactor I in the plug flow mode Inside, the reactor temperature is controlled at 120°C, and the residence time is 30min; the reaction liquid flowing out from the reactor directly enters the mixer II for mixing, and directly enters the microchannel reactor II for hydrolysis, and the reaction temperature is controlled at 40°C, and the residence time is 5min; then enter the separation unit for separation, the separation unit uses an equal amount of toluene for extraction, the oil phase is washed with alkali, washed with water, and distilled to obtain 2-ethylanth...

Embodiment 2

[0030]Add 2-(4-butylbenzoyl)benzoic acid at 180°C at a flow rate of 5.0g / min and room temperature concentrated sulfuric acid at a flow rate of 11ml / min to the Y-type mixer I and mix continuously, and the liquid 2- The mass (g) of (4-butyl benzoyl) benzoic acid and concentrated sulfuric acid: the volume (ml) ratio is 1: 2.2, control mixing temperature 40 ℃, the mixture flows into the microchannel reactor I with plug-flow mode Inside, the reactor temperature is controlled at 130°C, and the residence time is 20min; the reaction liquid flowing out from the reactor directly enters the mixer II for mixing, and directly enters the microchannel reactor II for hydrolysis, and the reaction temperature is controlled at 30°C, and the residence time is 10 min; then enter the separation unit for separation, the separation unit uses an equal amount of toluene for extraction, the oil phase is washed with alkali, washed with water, and distilled to obtain 2-butylanthraquinone with a yield of 80...

Embodiment 3

[0032] Add 2-(4-propylbenzoyl)benzoic acid at 140°C at a flow rate of 4.0g / min and concentrated sulfuric acid at 60°C at a flow rate of 7.6ml / min into the T-type mixer I for mixing with a metering pump. The mass (g) of 2-(4-ethyl benzoyl) benzoic acid and concentrated sulfuric acid: the volume (ml) ratio is 1:1.9, the mixing temperature is controlled at 50°C, and the mixture flows into the microchannel reaction in a plug-flow manner In the reactor I, the temperature of the reactor is controlled at 110°C, and the residence time is 30 minutes; the reaction liquid flowing out from the reactor directly enters the mixer II for mixing, and directly enters the microchannel reactor II for hydrolysis, and the reaction temperature is controlled at room temperature, and the residence time is Then enter the separation unit for separation, the separation unit uses an equal amount of toluene for extraction, the oil phase is washed with alkali, washed with water, and distilled to obtain 2-pro...

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a method for preparing 2-alkylanthraquinone with a microchannel continuous reactor. The synthesis is carried out in a microchannel reactor, and the method comprises the following steps: (1) catalyzing phthalic anhydride and alkylbenzene by using AlCl3 as a catalyst, and performing a Friedel-Crafts acylation reaction to generate 2-(4-alkyl benzoyl) benzoic acid; and (2) continuously reacting the 2-(4-alkyl benzoyl) benzoic acid with concentrated sulfuric acid through a mixer I, a reactor I, a mixer II, a reactor II and a separation unit of the microchannel reactor to generate the 2-alkylanthraquinone in a closed loop mode. Compared with a traditional intermittent reaction, the microchannel reaction adoptedin the method has the advantages of relatively good microchannel airtightness, high safety, little pollution and simple operation; the product has a yield increased by 5-10 percent in comparison withthat of an existing production process, and has high quality.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing 2-alkylanthraquinone in a microchannel continuous reactor. Background technique [0002] Microchannel reactor is a general term for microchannel chemical equipment such as microreactors, micromixers, microheat exchangers and microcontrollers. Due to its unique advantages such as simple structure, easy control of operating conditions and no amplification effect, since the mid-1990s, it has been widely used in the research and development and production of chemical, pharmaceutical, pesticide, material, food, organic synthesis and other fine chemical industries. It has been applied more and more, and has rapidly developed into a research hotspot. Compared with the traditional reaction process, the microreactor application process has high-speed mixing, high-efficiency mass transfer and heat transfer, narrow residence time distribution, adjustable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/00C07C50/16B01J19/00
CPCB01J19/0093B01J2219/00792B01J2219/00867B01J2219/00889C07C46/00C07C51/083C07C50/16C07C65/34
Inventor 靳海波杨索和何广湘郭晓燕
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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