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Device and method for continuously producing beta-ionone by using microchannel

A technology of ionone and pseudo-ionone, which is applied in the field of microchannel continuous production of β-ionone, can solve the problems of high price of phase transfer catalyst and anti-translocation agent, high energy consumption of ultrasonic equipment, and low production efficiency. , to achieve the effects of high yield, saving operating costs and convenient operation

Pending Publication Date: 2017-05-17
SHANGHAI FLUKO TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 1109462A has introduced the addition of 2-hydroxy-4-octyloxybenzophenone compound as translocation preventive agent in the cyclization reaction, but the phase transfer catalyst and transposition preventive agent used are expensive and cannot be recycled. conducive to industrialization
German patent DE.3328440 proposed a method of producing β-ionone by instant contact between pseudoionone and sulfuric acid at room temperature, but this method requires special equipment and difficult condition control, so it has not been widely used
Chinese patent CN1129209A introduces a method of completing the cyclization reaction under the action of ultrasonic waves, but the ultrasonic device consumes a lot of energy, and it is difficult to realize industrial production
In Chinese patent CN02155069.7, dry ice is added in batches in the cyclization reaction to prevent local overheating, but the processing capacity is small and the production efficiency is not high

Method used

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  • Device and method for continuously producing beta-ionone by using microchannel
  • Device and method for continuously producing beta-ionone by using microchannel
  • Device and method for continuously producing beta-ionone by using microchannel

Examples

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Effect test

Embodiment 1

[0022] A method for the continuous production of beta-ionone with a microchannel reactor, see figure 2 , including the following steps:

[0023] (1) Use the above-mentioned device for continuously producing β-ionone with a microchannel reactor;

[0024] (2) the false ionone solution (stored in the false violet solution storage tank 1) of 50% volume fraction is made into pseudo-ionone with acetone, the pseudo-ionone solution and the vitriol oil (the concentrated sulfuric acid is stored in sulfuric acid In storage tank 2) pass in the microchannel reactor by two entrances of microchannel reactor 3 respectively, the flow of false ionone solution is 9L / h, the flow of vitriol oil is 18L / h, reacts at 30 ℃ (cooling 10 DEG C of water are passed into the microchannel reactor), after the product flows out of the microchannel reactor, the phase separator 4 is used to carry out the phase separation process to obtain the water phase recycling, and the oil phase containing β-ionone is succ...

Embodiment 2

[0027] A method for continuously producing β-ionone with a microchannel reactor, comprising the steps of:

[0028] (1) Use the above-mentioned device for continuously producing β-ionone with a microchannel reactor;

[0029] (2) Pseudo-ionone is made into a volume fraction of 70% pseudo-ionone solution with dichloromethane, and pseudo-ionone solution and vitriol oil are passed into the micro-channel reactor by two inlets of the micro-channel reactor respectively , the flow rate of pseudoionone solution is 9L / h, the flow rate of vitriol oil is 36L / h, reacts at 25 ℃ (cooling is passed into microchannel reactor with 5 ℃ of water), after the product flows out of microchannel reactor, separate The phase device (4) carries out the phase separation treatment to obtain the water phase recycling, and the oil phase containing β-ionone is washed with water, 2% sodium carbonate aqueous solution and water successively, and the dichloromethane is removed by distillation under reduced pressur...

Embodiment 3

[0032] A method for continuously producing β-ionone with a microchannel reactor, comprising the steps of:

[0033] (1) Use the above-mentioned device for continuously producing β-ionone with a microchannel reactor;

[0034] (2) Pseudo-ionone is made into a volume fraction of 30% pseudo-ionone solution with a mixed solvent (the mixed solvent is chloroform, carbon tetrachloride and 1,2-dichloride with a volume ratio of 1:1:1 Ethane composition), pseudo ionone solution and the vitriol oil pass in the micro channel reactor through two entrances of microchannel reactor (3) respectively, the flow of pseudo ionone solution is 9L / h, the flow of the vitriol oil is 9L / h, react at 28 DEG C (cooling is passed into microchannel reactor with 8 DEG C of water), after the product flows out of microchannel reactor, carry out phase separation treatment with phase separator (4) to obtain water phase recycling, obtain the - The oily phase of the ionone is washed with water, an aqueous sodium car...

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PUM

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Abstract

The invention discloses a device and method for continuously producing beta-ionone by using microchannel. The method comprises the following steps: preparing a pseudoionone organic solvent into a pseudoionone solution in volume percentage of 30-70%, adding the pseudoionone solution and concentrated sulfuric acid into a microchannel reactor respectively through two inlets of the microchannel reactor, reacting at a temperature of 25-30 DEG C, enabling reactant to flow out of the microchannel reactor, carrying out phase splitting treatment on the reactant by using a phase splitter to obtain a water phase and an oil phase containing beta-ionone, and treating the oil phase containing beta-ionone to obtain beta-ionone oily liquid. The method is convenient to operate and easily controllable in condition; the produced beta-ionone is high in yield and high in purity; the large-scale industrial production is facilitated; the microchannel reactor has extremely high heat exchange efficiency and is capable of preventing local temperature from excessively high, eliminating hot-spot temperature and improving the purity of the product which is beta-ionone; the continuous product is achieved; the production efficiency is improved; the copious cooling condition is avoided; the energy consumption is reduced; the cost is reduced.

Description

technical field [0001] The invention relates to a device and method for continuously producing β-ionone by using a microchannel. Background technique [0002] β-ionone is an important synthetic spice and an important intermediate for the synthesis of vitamin A in the pharmaceutical industry. It can be cyclized under acidic conditions after condensing citral and acetone to generate pseudo-ionone. According to the position of the double bond of ionone, there are three isomers of α, β and γ. The product of cyclization synthesis is usually a mixture of α-, β-ionone. In the synthesis of vitamin A in the pharmaceutical industry, the purity of β-ionone has a great influence on the product. Therefore, it is the key to the development of β-ionone preparation technology to be able to prepare high-purity β-ionone simply and in large quantities. [0003] [0004] At present, the synthesis of ionone mainly revolves around how to increase the content of β-ionone in the cyclization pr...

Claims

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Application Information

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IPC IPC(8): C07C45/67C07C49/21B01J19/00
CPCB01J19/0093C07C45/67B01J2219/00873C07C49/21
Inventor 张金利杨超李韡韩优周鸣亮
Owner SHANGHAI FLUKO TECH DEV
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