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Method for continuously synthesizing 4-oxoisophorone in microchannel reactor

A microchannel reactor, oxoisophorone technology, applied in chemical instruments and methods, chemical/physics/physicochemical reactors, preparation of organic compounds, etc., can solve the problem of lack of industrialization and expensive transition metal catalysts , the problem of high cost of the reaction process, to reduce the abnormal working conditions that block the microchannel reactor, improve the experimental stability and operability, and improve the stability and operability.

Pending Publication Date: 2019-09-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has a high yield, the porphyrin or phthalocyanine transition metal catalyst is quite expensive, and is easily destroyed in the reaction, making the reaction process cost higher
In addition, ethylene glycol dimethyl ether and triethylamine are very dangerous under operating conditions, and currently do not have the conditions for industrialization
[0008] Patent US4046813 describes a method for preparing KIP by catalytic oxidation of β-isophorone using vanadium, iron, cobalt, and manganese acetylacetonate complexes in the presence of pyridine, although the method has a conversion rate of about 100%. During the reaction process, a large amount of waste gas containing pyridine will be produced, and there is a risk of flash explosion in the reaction system. In the actual operation process, some catalysts will also be slagged.
[0009] These two approaches for the above-mentioned preparation of 4-oxoisophorone have their own defects: the direct oxidation of α-IP to KIP takes a long time, the conversion rate is not high, and the selectivity is low; while β-IP can be easily Oxygen oxidation is used to prepare KIP, but a large amount of three wastes will be generated in the catalytic oxidation of homogeneous catalysts, and the treatment of three wastes and the avoidance of safety risks will increase the production cost

Method used

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  • Method for continuously synthesizing 4-oxoisophorone in microchannel reactor
  • Method for continuously synthesizing 4-oxoisophorone in microchannel reactor
  • Method for continuously synthesizing 4-oxoisophorone in microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Material preparation:

[0048] Weigh 2.00g of molybdenum acetylacetonate, 8.00g of ammonia water (25%), and 990g of tetrahydrofuran, and mix them uniformly in a 2L glass jar; weigh 400g of β-isophorone and put them into a 500mL glass jar. Put the β-isophorone and catalyst solution into the ultrasonic generator for 30 minutes to remove the dissolved gas in the material.

[0049] System preparation:

[0050] Turn on the microchannel reaction system, set the temperature of the heat transfer oil in the preheating zone to 50°C, set the temperature of the heat transfer oil in the reaction zone to 60°C, and set the temperature of the heat transfer oil in the cooling zone to 20°C, and wait for the temperature to balance.

[0051] Preparation of 4-oxoisophorone:

[0052] After the temperature of the heat transfer oil is stable, take out the β-isophorone and the catalyst solution from the ultrasonic generator, inject the catalyst solution into the microchannel system at a rate ...

Embodiment 2

[0054] Material preparation:

[0055] Weigh 2.50g of vanadyl acetylacetonate, 3.50g of triethylamine, and 994g of tetrahydrofuran, and mix them uniformly in a 2L glass jar; weigh 400g of β-isophorone into a 500mL glass jar. Put the β-isophorone and catalyst solution into the ultrasonic generator for 30 minutes to remove the dissolved gas in the material.

[0056] System preparation:

[0057] Turn on the microchannel reaction system, set the temperature of the heat transfer oil in the preheating zone to 50°C, set the temperature of the heat transfer oil in the reaction zone to 60°C, and set the temperature of the heat transfer oil in the cooling zone to 20°C, and wait for the temperature to balance.

[0058] Preparation of 4-oxoisophorone:

[0059] After the temperature of the heat transfer oil is stable, take out the β-isophorone and catalyst solution from the ultrasonic generator, inject the catalyst solution into the microchannel system at a rate of 8 g / min with an advection...

Embodiment 3

[0061] Material preparation:

[0062] Weigh 3.00g of nickel acetylacetonate, 3.00g of diethylamine, and 994g of 2-methyltetrahydrofuran, and mix them uniformly in a 2L glass jar; weigh 400g of β-isophorone into a 500mL glass jar. Put the β-isophorone and catalyst solution into the ultrasonic generator for 30 minutes to remove the dissolved gas in the material.

[0063] System preparation:

[0064] Turn on the microchannel reaction system, set the temperature of the heat transfer oil in the preheating zone to 65°C, set the temperature of the heat transfer oil in the reaction zone to 75°C, and set the temperature of the heat transfer oil in the cooling zone to 25°C, and wait for the temperature to balance.

[0065] Preparation of 4-oxoisophorone:

[0066] After the temperature of the heat transfer oil is stable, take out the β-isophorone and catalyst solution from the ultrasonic generator, inject the catalyst solution into the microchannel system at a rate of 2g / min with an ad...

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Abstract

The invention discloses a method for continuously synthesizing 4-oxoisophorone in a microchannel reactor. The method comprises the following steps: feeding a metered catalyst solution, oxygen and beta-isophorone into the microchannel reactor in proportion, fully mixing and then reacting to obtain the 4-oxoisophorone. According to the process method disclosed by the invention, the microchannel reactor is utilized, so that the reaction mass-transfer efficiency is high, the reaction temperature is stable, and the experimental operability is greatly improved; the metered oxygen is used as an oxidant, the reactor volume is small, no waste gas is generated, the flash-explosion risk of a traditional kettle type gas-liquid two-phase reaction is effectively avoided, and the safety performance of the reaction is improved; a special system is adopted, so that a homogeneous catalyst is prevented from slagging during the reaction so as to plug the reactor, and the efficient continuous production of the 4-oxoisophorone becomes possible.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for continuously synthesizing 4-oxoisophorone in a microchannel reactor, in particular to a gas-liquid two-phase catalytic oxidation of β-isophorone to prepare 4-oxoisophorone The pherone method. Background technique [0002] 4-Oxoisophorone (KIP for short) is an important chemical intermediate product, which can be used not only in cosmetics and fragrances, but also in the synthesis of carotenoids and vitamins. Due to the importance of 4-oxoisophorone in chemical products, the synthesis of 4-oxoisophorone has been a research hotspot for a long time. [0003] At present, there are mainly two methods for synthesizing KIP commonly used, namely, oxidizing β-isophorone (abbreviated as β-IP) or α-isophorone (abbreviated as α-IP) to synthesize KIP. [0004] Patent CN101417936A describes a method for preparing KIP by catalytic oxidation of α-IP under a metal-free cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/34C07C49/603
CPCB01J19/0093C07C45/34C07C2601/16C07C49/603
Inventor 程晓波张鹏飞张涛郭劲资黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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