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Method for continuously preparing pseudo ionone of vitamin A intermediate

A technology for pseudo-ionone and vitamin, which is applied in the field of continuous preparation of vitamin A intermediate pseudo-ionone, can solve problems such as high requirements on equipment corrosion and solid waste pollution.

Active Publication Date: 2013-04-17
ANHUI BBCA FERMENTATION TECH ENG RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses an excessive amount of high-concentration alkali metal hydroxide aqueous solution, which requires high equipment corrosion and causes a large amount of solid waste pollution

Method used

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  • Method for continuously preparing pseudo ionone of vitamin A intermediate
  • Method for continuously preparing pseudo ionone of vitamin A intermediate
  • Method for continuously preparing pseudo ionone of vitamin A intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Citral 145g / h (content 97.3%, obtained by high vacuum fractionation and purification of litsea cubeba oil) and acetone 1200g / h with a water content of 10% are mixed evenly, pressurized to 8MPa by a pump, and heated to 100 in a preheater ℃, and then mixed with 0.4% NaOH aqueous solution 100g / h pressurized to the same pressure through a static mixer, and then entered a tubular reactor for condensation reaction. The reaction residence time is 10 minutes, and the reaction liquid is analyzed by gas chromatography. The reaction liquid is decompressed to normal pressure and enters the flash tower, and the recovered acetone with a water content of 8% is obtained from the top of the tower. The oil layer was recovered under reduced pressure to obtain 202.6g / h of pseudo-ionone crude product, which was tested and analyzed by gas chromatography, and the crude product was further separated by high-vacuum rectification to separate unreacted light components, citral and pseudo-ionone fi...

Embodiment 2

[0038] According to the method of Example 1, the difference is that citral is mixed uniformly with 150g / h (content 97.3%) and acetone 1000g / h with a water content of 15% (the mol ratio of acetone to citral is 15:1), and other conditions are not changed. Change. 177.3g / h of the pseudo-ionone fine product was obtained, the content was 94.9% (the sum of the contents of the two isomers), the conversion rate of citral was 96.41%, and the selectivity was 98.9%, which was relative to the yield of citral pseudo-ionone It is 91.23%.

Embodiment 3

[0040] According to the method of Example 1, the difference is that citral is mixed uniformly with 120g / h (content 97.3%) and acetone 1500g / h with a water content of 10% (the molar ratio of acetone to citral is 30:1), and other conditions are not changed. Change. 142.2g / h of pseudo-ionone was obtained, with a content of 95.5% (the sum of the contents of the two isomers), and a yield of 91.44% relative to that of citral pseudo-ionone.

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Abstract

The invention discloses a method for continuously preparing pseudo ionone of a vitamin A intermediate. The method evenly mixes acetone, citral and catalyst under the continuous operation condition and introduces in a tubular reactor. The reaction mixture is continuously reacted for 1-120 minutes at the reaction temperature of 20-150 DEG C under the pressure of 0-10 MPa; reaction liquid is relieved pressure to enter a flash column; recovered acetone is obtained from the top of the column; tower bottoms are introduced in a layering machine for layering; after being neutralized, oil layers are relieved pressure and recovered to obtain pseudo ionone crude products, and are further distilled in high vacuum and separated out unreacted citral and pseudo ionone competitive products; and the recovered light-component by-products and the unreacted citral are mixed with the recovered acetone to enter the reactor again. The method has the advantages of low catalyst concentration, low corrosion to equipment, short reaction time and fewer side effects; and part by-products can be recycled.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for continuously preparing vitamin A intermediate pseudoionone. Background technique [0002] Pseudo-ionone, chemical name 6,10-dimethyl-3,5,9-undecatrien-2-one, light yellow liquid. Pseudo-ionone is an important intermediate in the synthesis of ionone, which is widely used in the industries of spices, medicine, and food additives. Ionone is a kind of precious spice with woody aroma, which is one of the largest and most important spices in the perfume industry; at the same time, the synthesized β-ionone is an important intermediate for the synthesis of vitamin A and β-carotene. [0003] For a long time, scholars at home and abroad have continued to improve the synthesis process of pseudoionones. The main synthesis method is to condense citral separated from litsea cubeba oil with acetone through Aldol condensation under alkaline conditions. [0004] PL147748 describe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/74
Inventor 李荣杰尚海涛杨为华邓远德张飞
Owner ANHUI BBCA FERMENTATION TECH ENG RES
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