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A process for preparing 2,3,5-trimethyl-p-benzoquinone by catalytic oxidation

A catalytic oxidation and trimethylation technology, applied in the preparation of oxidized quinone, organic chemistry, etc., can solve the problems of slow oxidation reaction, low oxygen utilization rate, and immature

Active Publication Date: 2020-09-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although solid-state catalysts have shown unique advantages in product separation, quality control, and catalyst recovery and recycling, most of this direction is still in the laboratory exploration stage, immature, and there are not many practical industrial applications
[0005] Through relevant technical research in this field, it is found that the current methods for preparing 2,3,5-trimethyl-p-benzoquinone by catalytic oxidation of 2,3,6-trimethylphenol have the following common points: firstly, most of them are Gas-liquid or gas-liquid-liquid reaction process, so it has high requirements for liquid-liquid mixing and gas-liquid mass transfer; the second point is that the whole reaction process is carried out in a traditional stirred tank reactor, and the liquid-liquid is promoted by stirring. liquid mixing and oxygen absorption; the third point is that due to the slow oxidation reaction, most of the oxygen leaves the system without sufficient reaction, and the oxygen utilization rate is not high; the last point is that although a higher yield can be achieved in the end, the reaction time is generally Longer, less productive

Method used

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  • A process for preparing 2,3,5-trimethyl-p-benzoquinone by catalytic oxidation
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  • A process for preparing 2,3,5-trimethyl-p-benzoquinone by catalytic oxidation

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preparation example Construction

[0022] According to above narration, the present invention proposes the preparation method of a set of 2,3,5-trimethyl-p-benzoquinone matched with the preparation technology of 2,3,5-trimethyl-p-benzoquinone of the present invention, now In conjunction with the preparation process of the above-mentioned 2,3,5-trimethyl-p-benzoquinone to understand the idea of ​​the preparation method of 2,3,5-trimethyl-p-benzoquinone, see figure 2 . The preparation technology of this 2,3,5-trimethyl-p-benzoquinone comprises the following steps:

[0023] S1: Turn on the temperature control device and raise all reactors and pipelines to the specified temperature.

[0024]S2: Turn on the supergravity reactor 7 and the stirred tank reactor 2, and adjust to the required speed.

[0025] S3: Open the gas pipeline and the liquid pipeline, the gas enters the stirred tank reactor 2 after passing through the supergravity reactor 7, and finally discharges from the condensation device 9; the liquid circ...

Embodiment 1

[0034] Embodiment 1: Effect experiment of supergravity level

[0035] The reaction temperature is 73°C, the volume fraction of the water phase in the liquid phase is 0.83, the rotation speed of the stirred tank reactor is 600rpm, the concentration of 2,3,6-trimethylphenol in the oil phase is the same as that of CuCl in the water phase 2 The concentration ratio is 1:2, the above refers to the molar concentration ratio, CuCl 2 The concentration of the aqueous solution is 1mol / L, the gas-liquid volume flow ratio is 2.6, and the result of reaction for 10 minutes is as follows:

[0036] Hypergravity level (g) Yield of quinone (%) 30 14.14 120 15.34 270 15.62 480 16.9 750 15.06 Stirred tank reactors are used separately under the same conditions 5.64

[0037] The above results show that, compared with using the stirred tank reactor alone, the yield of 2,3,5-trimethyl-p-benzoquinone can be increased by about 10% after adding the high gra...

Embodiment 2

[0038] Example 2: Gas volume influence experiment

[0039] The reaction temperature is 75°C, the volume fraction of the water phase in the liquid phase is 0.83, the rotation speed of the stirred tank reactor is 600rpm, the supergravity level of the supergravity reactor is 270g, the liquid flow rate is 20L / h, and 2,3,6-trimethanone in the oil phase Base phenol concentration and CuCl in aqueous phase 2 The concentration ratio is 1:2, the above refers to the molar concentration ratio, CuCl 2 The concentration of the aqueous solution is 1mol / L, and the result of reacting for 10 minutes is as follows:

[0040]

[0041]

[0042] The above results show that, compared with using the stirred tank reactor alone, the yield of 2,3,5-trimethyl-p-benzoquinone can be increased by about 9-13% after adding the high gravity reactor.

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Abstract

The invention relates to a process for preparing 2,3,5-trimethyl p-benzoquinone by means of catalytic oxidation, belonging to the technical field of preparation of the 2,3,5-trimethyl p-benzoquinone.A new process for preparing the 2,3,5-trimethyl-p-benzoquinone is formed by combining a supergravity reactor with the conventional stirred tank reactor. The process uses pure-oxygen or oxygen-rich gasas an oxidant and takes an aqueous solution of a metal halide as a catalyst, a reactant, i.e., 2,3,6-trimethylphenol is dissolved in an organic solvent, and the whole reaction process is carried outin the supergravity reactor and the stirred tank reactor. The supergravity reactor has an ability to enhance liquid-liquid mixing and gas-liquid mass transfer, so that the process can enhance the catalytic effect of the catalyst, increase the reaction rate and shorten the production time; in addition, due to the introduction of the supergravity reactor, the utilization rate of oxygen is increased,an oxidation reaction of the 2,3,6-trimethylphenol is promoted, and the yield of the product per unit time is increased.

Description

technical field [0001] The invention relates to a method for preparing 2,3,5-trimethyl-p-benzoquinone, belonging to the technical field of 2,3,5-trimethyl-p-benzoquinone preparation. Background technique [0002] 2,3,5-Trimethyl-p-benzoquinone is an important intermediate in the synthesis of vitamin E. At present, there are many methods for preparing 2,3,5-trimethyl-p-benzoquinone by oxidation of 2,3,6-trimethylphenol. The traditional method is to sulfonate 2,3,6-trimethylphenol with sulfuric acid, and then oxidize it with manganese ore powder as an oxidant. This traditional preparation method has a low yield, and produces a large amount of industrial wastewater and waste residue, causing environmental pollution, and is gradually being eliminated. At present, the method of preparing 2,3,5-trimethyl-p-benzoquinone by catalyzing the oxidation of 2,3,6-trimethylphenol with green oxidants such as oxygen or hydrogen peroxide has received extensive attention, and the resulting y...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/08C07C50/02
CPCC07C46/08C07C2601/16C07C50/02
Inventor 邵磊陈嘉南宋云华初广文
Owner BEIJING UNIV OF CHEM TECH
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