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Method for preparing beta-ionone by using pseudoionone as raw materials

A technology for pseudo-ionone and ionone, which is applied in the field of preparing high-purity β-ionone, can solve the problems of producing a large amount of sulfuric acid waste water, harsh operating conditions, difficult separation, etc., and achieves reduced requirements for cyclization reaction conditions and improved utilization. The effect of reducing the rate and separation difficulty

Active Publication Date: 2018-07-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims at the disadvantages of the prior art for preparing β-ionone, such as high equipment requirements, harsh operating conditions, difficult follow-up separation and massive production of sulfuric acid waste water, etc., and improves the production method of β-ionone

Method used

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  • Method for preparing beta-ionone by using pseudoionone as raw materials
  • Method for preparing beta-ionone by using pseudoionone as raw materials

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 600g concentrated sulfuric acid (98wt%) is added in the reaction kettle I, start stirring, pass into the circulating cold water to regulate the temperature in the reaction kettle I, then by metering pump, 600g false ionone solution, hereinafter referred to as false purple solution (50wt%, The solvent is dichloroethane) and pumped into the reaction kettle Ⅰ to carry out the cyclization reaction. During the whole process of adding the false purple solution, the temperature in the reaction kettle Ⅰ is controlled at 7-39°C. After the addition of the false purple solution, continue at 28°C React for 10 minutes, then add 240g of water to dilute and quench. After quenching in the reaction kettle I, the reaction solution was separated by separator I to obtain 594g of organic phase I and 836g of dilute acid aqueous phase I (about 520mL, concentration 70.0%). The obtained dilute acid aqueous phase I was washed with 52 mL of dichloroethane, and the washing liquid I and the washed ...

Embodiment 2

[0046] 350g sulfuric acid solution (75wt%) is joined in the reaction kettle I, start to stir, pass into the temperature in the reaction kettle I of circulating cold water adjustment, then 700g pseudopurple solution (70wt%, solvent is dichloroethane) by metering pump Pump it into the reaction kettle Ⅰ for cyclization reaction. During the whole process of adding the false violet solution, the temperature in the reaction kettle Ⅰ is controlled at 5-32°C. After the addition of the false violet solution, continue the reaction at 0°C for 30 minutes, and then add 85g water for dilution and quenching. After quenching in the reaction kettle I, the reaction solution was separated by separator I to obtain 691 g of organic phase I and 428 g of dilute acid aqueous phase I (about 290 mL, concentration 60.3%). The obtained dilute acid aqueous phase I was washed with 45 mL of dichloroethane, and the washing liquid I and the washed dilute acid aqueous phase I were obtained after washing. Add ...

Embodiment 3

[0050] 470g sulfuric acid solution (85wt%) is joined in the reaction kettle I, start to stir, pass into the temperature in the reaction kettle I of circulating cold water adjustment, then by metering pump, 800g pseudopurple solution (10wt%, solvent is dichloroethane) Pump it into the reaction kettle Ⅰ to carry out the cyclization reaction. During the whole process of adding the false violet solution, the temperature in the reaction kettle Ⅰ is controlled at 25-47°C. After the addition of the false violet solution, continue the reaction at 50°C for 2 minutes, and then add 145g water for dilution and quenching. After quenching in the reaction kettle I, the reaction liquid was separated by separator I to obtain 791g of organic phase I and 608g of dilute acid aqueous phase I (about 390mL, concentration 64.9%). The obtained dilute acid aqueous phase I was washed with 48 mL of dichloroethane, and the washing liquid I and the washed dilute acid aqueous phase I were obtained after was...

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Abstract

The invention discloses a method for preparing beta-ionone by using pseudoionone as raw materials. The pseudoionone performs cyclization reaction under the catalysis effect of sulfuric acid; quenchingis performed; nitric oxide gas is introduced into reaction liquid after the quenching; then, isomerization reaction is performed to obtain the beta-ionone. The method has the advantages that the process is simple; no harsh reaction conditions are needed; sulfuric acid and solvents can be cyclically used for many times; in addition, the purity of the beta-ionone in the obtained product is high, and is higher than 97.5 percent.

Description

technical field [0001] The invention relates to a method for preparing high-purity β-ionone by using pseudoionone as a raw material, belonging to the fields of chemical industry, medicine and spices. Background technique [0002] β-ionone [4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one, β-ionone] is a kind of precious spice, which also has certain Biological activity, showing a strong anti-cancer effect, especially the obvious inhibitory effect on the occurrence of tumors. In addition, this product is widely used in industry and is a very important pharmaceutical intermediate and an important raw material for the synthesis of vitamins A, E, β-carotene, carotenoids, retinoic acid and phytol. [0003] The synthesis of β-ionone is generally generated by cyclization reaction using pseudoionone as raw material under acidic conditions. The product of the cyclization reaction is usually a mixture of three isomers of α-ionone, β-ionone and γ-ionone, among which the two isomers o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/21C07C45/46C07C45/67
CPCC07B2200/09C07C45/46C07C45/67C07C49/21
Inventor 林龙吕英东张涛程晓波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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