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Method for preparing vitamin A palmitate by supercritical method

A technology of palmitate and methyl palmitate, applied in the field of preparation of VA palmitate, can solve the problems of long production cycle of VA palmitate, cumbersome process operation steps, low conversion rate and the like, and improve the transesterification reaction rate. , the effect of improving the reaction rate and conversion rate, and reducing the mass transfer resistance

Active Publication Date: 2021-03-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Repeated filtration and vacuum distillation in the reaction, the process operation steps are cumbersome
[0005] The existing VA palmitate preparation method also has problems such as long production cycle and low conversion rate. Preparation method makes good commercial sense

Method used

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  • Method for preparing vitamin A palmitate by supercritical method
  • Method for preparing vitamin A palmitate by supercritical method
  • Method for preparing vitamin A palmitate by supercritical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Such as figure 1 As shown, 5730 gVa alcohol (20 mol) and 6480 g of palmitate (24 mol) were placed in the raw material can be selected from 1: 1.2 molar ratio of the raw material Va alcohol and palmitate. Open the methanol pressure reducing valve and methanol gas tank pressure reducing valve, a mixture of volumetric flow rate of 12 l / min supercritical methanol and trifluorometise (supercritical methanol and trifluorometise bromochiome is 20: 1) In the mixer, the mixture temperature was 239.1 ° C, and the pressure was 8.1 MPa. Further, the formulated raw material liquid was mixed by a volumetric flow of 60 ml / min and the supercritical mixture was transferred to the reactor, and the temperature was 239.1 ° C, the pressure was 8.1 MPa, and the reactor was filled with a quantity of non-metallic glass springs. It is an object to increase the liquid contact area, strengthen the mass transfer, and the glass spring fill is 5 g, the filler is 0.5 ml. The reaction process is stab...

Embodiment 2

[0042] Such as figure 1 As shown, 5270 gVa alcohol (20 mol) and 5940 g of palmitate (22 mol) were placed in the raw material tank according to the raw material Va alcohol and the palmitate molar ratio of 1: 1.1. Open the methanol pressure reducing valve and methanol gas tank pressure reducing valve, a mixture of volumetric flow rate of 13 l / min supercritical methanol and trifluorometise (supercritical methanol and trifluorometheramethiometry) is 25: 1). In the mixer, the mixed gas temperature was 245 ° C, and the pressure was 8.93 MPa. The formulated raw material liquid is delivered to the reactor after mixing by volume flow of 78 ml / min and supercritical methanol, and the temperature is 245 ° C, the pressure is 7.8 MPa, and the glass spring is filled with a glass spring fill amount of 4.5 g, and the filler volume is 3ml. . The reaction process is stabilized by the back pressure valve. After the reaction is completely (sampling at intervals, the content is stabilized to the r...

Embodiment 3

[0044] Such as figure 1 As shown, 2860 gVa alcohol (10 mol) and 3510 g of palmitate (13 mol) were added to the raw material can be measured according to the raw material Va alcohol and the palmitate molar ratio of 1: 1.3. Open the methanol pressure reducing valve and methanol gas tank pressure reducing valve, a mixture of volumetric flow rate of 14 l / min supercritical methanol and trifluorometise (supercritical methanol and trifluorometiocene bromochiome is 30: 1) In the mixer, the mixture temperature was 250 ° C, and the pressure was 9.67 MPa. The formulation mixed raw material liquid is mixed with a volumetric flow of 98 ml / min and the supercritical mixture is transferred to the reactor, and the temperature is 250 ° C, the pressure is 9.67 MPa, and the glass spring is filled with 3.5 g, and the filler volume is 2ml. The reaction process is stabilized by the back pressure valve. After the reaction is completely (sampling at intervals, the content is stabilized to the reactio...

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Abstract

The invention discloses a method for preparing vitamin A palmitate by a supercritical method, which utilizes the strong solubility of supercritical fluid to strengthen mass transfer, and liquid-phasemethanol generated by continuous analysis of supercritical methanol in the reaction process to promote transesterification to be carried out in the positive direction, thereby enhancing the reaction conversion rate. According to the process, a trifluoromethylthio compound is entrained in supercritical methanol, so that the formation of carbocation of methyl palmitate is effectively promoted, and the reaction yield is increased.

Description

Technical field [0001] The present invention belongs to the preparation of Va palmitates, and a method of preparing vitamin A palmitate is prepared by supercritical methods. Background technique [0002] Vitamin A palmitate (Va palmitate) has the advantages of carbon chain length, low melting point, good oil solubility, low temperature stability, is an indispensable substance of normally metabolism in humans and animals, has been widely used in cosmetics. Pharmaceutical, feed and other fields. [0003] Va palmitate is primarily made of chemical synthesis and biomease. The chemical synthesis method mainly controls the Va alcohol with palm chloride to form Va palmitate and HCl gas. The synthesis reaction conditions are harsh, producing more acidic by-products, and high requirements for corrosionability of production equipment, which is not conducive to industrial production. The biomease method is a prouse ester that occurs in the presence of lipase. [0004] Patent CN104673870A di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/12
CPCC07C403/12Y02P20/54
Inventor 罗朝辉林龙翟文超吕英东黎源
Owner WANHUA CHEM GRP CO LTD
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