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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 the problems of solid waste pollution, high requirements on equipment corrosion, etc.

Active Publication Date: 2015-04-15
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 Radix japonica oil) and 1200g / h acetone 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 100 g / h of 0.4% NaOH aqueous solution pressurized to the same pressure through a static mixer, and then entered into a tubular reactor for condensation reaction. The reaction residence time was 10 minutes, and the reaction solution was analyzed by gas chromatography. The reaction solution was decompressed to normal pressure and then entered into a flash tower. The recovered acetone containing 8% water was obtained from the top of the tower. The oil layer was recovered under reduced pressure to obtain a pseudo-ionone crude product of 202.6g / h, which was tested and analyzed by gas chromatography. The crude product was further subjected to high vacuum rectification to separate unreacted light components, citral and ps...

Embodiment 2

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

Embodiment 3

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

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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 a vitamin A intermediate pseudoionone. Background technique [0002] Pseudo-ionone, chemical name 6,10-dimethyl-3,5,9-undecanotrien-2-one, pale 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 spice in the spice industry; the β-ionone synthesized at the same time is an important intermediate for the synthesis of vitamin A and β-carotene. [0003] For a long time, scholars at home and abroad have been continuing to improve the synthesis process of pseudoionone. Its main synthesis method is obtained from Aldol condensation of citral separated from Radix japonica oil under alkaline conditions with acetone. [0004] PL147748 describ...

Claims

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Application Information

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Patent Type & Authority Patents(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