Phenol and hydrogen peroxide hydroxylation microchannel reaction method

A micro-channel reaction, micro-channel reactor technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of cumbersome intermittent operation, affecting competitiveness, large reactor volume, etc. And the effect of fast heat transfer, short reaction residence time and low catalyst cost

Inactive Publication Date: 2016-05-11
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Enichem method also has many shortcomings. ① The preparation cost of titanium-silicon molecular sieve TS-1 is high, and the synthesis conditions are harsh and complicated.
②Catalyst performance is unstable
③ The internal pore size of titanium-silicon molecular sieve is small, and the effect is not good when used for macromolecular reactants. A certain amount of tar is inevitably produced in the hydroxylation reaction of phenol. Therefore, the titanium-silicon molecular sieve catalyst needs acetone as a solvent and is often regenerated, which is difficult for continuous production.
④ The reaction speed of phenol hydroxylation is slow, forcing the slurry bed reactor to be large in volume, cumbersome to operate intermittently, and the working environment is harsh, which seriously affects the competitiveness of this technology
[0011] Although there are phenol hydrogen peroxide hydroxylation production technologies in China, the production processes have obvious shortcomings. Therefore, it is necessary to research and develop a clean and efficient phenol hydrogen peroxide hydroxylation technology

Method used

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  • Phenol and hydrogen peroxide hydroxylation microchannel reaction method
  • Phenol and hydrogen peroxide hydroxylation microchannel reaction method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] At a temperature of 40°C, 47.5g of phenol, 300mL of water and 4.45g of water-soluble catalyst were added into the reaction flask and stirred evenly, and then 51mL of 30% hydrogen peroxide was quickly added dropwise to make a raw material solution. When the temperature of the microchannel reactor rose to 90° C., the raw material solution was continuously input into the microchannel reactor at a flow rate of 50 mL / min for hydroxylation reaction. The measurement results are shown in Table 2.

Embodiment 2

[0035] At a temperature of 40°C, 48.7g of phenol, 300mL of water and 4.45g of water-soluble catalyst were added into the reaction flask and stirred evenly, and then 71mL of 30% hydrogen peroxide was quickly added dropwise to make a raw material solution. When the temperature of the microchannel reactor rose to 100° C., the raw material solution was continuously input into the microchannel reactor at a flow rate of 60 mL / min for hydroxylation reaction. The measurement results are shown in Table 2.

Embodiment 3

[0037] At a temperature of 40°C, 47.8g of phenol, 300mL of water and 4.45g of water-soluble catalyst were added into the reaction flask and stirred evenly, and then 91mL of 30% hydrogen peroxide was quickly added dropwise to make a raw material solution. When the temperature of the microchannel reactor rose to 110° C., the raw material solution was continuously input into the microchannel reactor at a flow rate of 70 mL / min for hydroxylation reaction. The measurement results are shown in Table 2.

[0038]

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a phenol and hydrogen peroxide hydroxylation microchannel reaction method. The method comprises the steps of mixing the raw materials phenol, water, hydrogen peroxide and a water-soluble catalyst according to certain proportions to prepare a raw material solution, adding the raw material solution into a mixing tank, setting the reaction temperature of a microchannel reactor to be 30-150 DEG C, and inputting the raw material solution into the microchannel reactor at the flow rate of 5-150 mL/min through continuous charging and discharging for hydroxylation reaction, so that catechol and hydroquinone are obtained. The method is simple, operation is convenient, the conversion rate is high, selectivity is high, efficiency is high, and the content of tar in reaction liquid is low.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a microchannel reaction method for hydroxylation of phenol hydrogen peroxide. Background technique [0002] Hydroquinone (including catechol, hydroquinone), catechol is an important fine chemical, and it is a basic organic raw material or intermediate in industries such as rubber, medicine, pesticides, dyes, photosensitive materials, and spices. Body, mainly used as photographic developer, antioxidant, color developer for fur dyeing, etc. In the pesticide industry, catechol is an important intermediate of the carbamate pesticides carbofuran (carbofuran), propoxur, and diethofencarb; Catechol can also be used to synthesize a series of spices, such as vanillin, safrole, piperonal, etc.; in the oil field industry, catechol ether is a commonly used drilling mud stabilizer. Hydroquinone is an important raw material, auxiliary agent and intermediate for rubber, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C37/60
Inventor 杨怀青王菡黄伟
Owner CHINA PETROLEUM & CHEM CORP
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