A device and method for preparing vitamin A acetate by multi-stage continuous series reaction extraction

A series reaction and extraction device technology, applied in the direction of organic chemistry, can solve the problems of increased side reactions, increased vitamin A acetate synthesis yield, high labor intensity, and difficulty in continuous operation, so as to reduce the labor intensity of process operations and improve industrial production level, the effect of mild reaction conditions

Active Publication Date: 2021-12-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For reactions containing solids in the reaction system, the solids in the system will deposit at the bottom of the equipment during long-term operation, which is difficult to clean up, and the risk of blockage of the pipeline is very easy to occur, and because the solids cannot be removed from the reaction system in time, under stirring conditions Products, raw materials, intermediates and by-product solids will wrap each other, reduce the reaction rate, affect the conversion rate and yield, and increase the occurrence of side reactions
In the reactive extraction process, these problems are difficult to solve by conventional methods such as stirring, and it is not easy to achieve continuous operation. Therefore, there are few reports on the continuous liquid-solid phase reactive extraction process.
[0009] Using C15 phosphine salt and C5 aldehyde as reaction raw materials and water as the reaction solvent for the vitamin A acetate preparation process, triphenylphosphine oxide and other by-product solid particles will be generated during the reaction process. These continuously generated solid particles, on the one hand, make In fact, it is difficult to realize the continuous production of reaction extraction. On the one hand, it also increases the side reaction and affects the synthesis yield of vitamin A acetate.
The currently reported production processes for the preparation of vitamin A acetate by chemical synthesis are batch processes, which have the disadvantages of high labor intensity, low production efficiency, and large impact on the environment. Therefore, it is urgent to seek a suitable and competitive green manufacturing process. solved problem

Method used

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  • A device and method for preparing vitamin A acetate by multi-stage continuous series reaction extraction
  • A device and method for preparing vitamin A acetate by multi-stage continuous series reaction extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Preparation raw material F 1 , wherein the mass content of C15 phosphonium chloride is 30.37%, the mass content of C5 aldehyde is 8.88%, and the mass content of water is 60.75% (the molar ratio of C5 aldehyde to C15 phosphine chloride is 1.03). raw material F 1 Preheat to 40°C.

[0059] Prepare lye F 2 , wherein the sodium carbonate mass concentration is 15%, and the phase transfer aid cetyltrimethylammonium chloride mass concentration is 3% (the mol ratio of sodium carbonate and cetyltrimethylammonium chloride is 15), The rest is pure water. Lye F 2 Preheat to 40°C.

[0060] Petroleum ether was selected as the extractant E 0 . Extractant E 0 Preheat to 40°C.

[0061] Reactor such as figure 1 As shown, the raw material F 1 , lye F 2 and extractant E 0 The mass flow rates of 14.8kg / min, 7.0kg / min and 7.4kg / min are simultaneously passed into the first-stage reaction extraction stirring tank 1-1 and maintained at 40°C for the reaction extraction process. When ...

Embodiment 2

[0063] Preparation raw material F 1 , wherein the mass content of C15 phosphine chloride is 15.77%, the mass content of C5 aldehyde is 5.37%, and the mass content of water is 78.86% (the molar ratio of C5 aldehyde to C15 phosphine chloride is 1.2). raw material F 1 Preheat to 55°C.

[0064] Prepare lye F 2 , wherein the mass concentration of sodium hydroxide is 35%, the mass concentration of phase transfer aid dodecyltrimethylammonium chloride is 6.4%, and all the other are pure water (sodium hydroxide and dodecyltrimethylammonium chloride The molar ratio is 36). Lye F 2 Preheat to 55°C.

[0065] Select n-heptane as extractant E 0 . Extractant E 0 Preheat to 55°C.

[0066] As shown in the attached figure, the raw material F 1 , lye F 2 and extractant E 0The mass flow rates of 38.0kg / min, 1.9kg / min and 9.4kg / min are simultaneously passed into the first-stage reaction extraction stirring tank 1-1 and maintained at 55°C for the reaction extraction process. When the li...

Embodiment 3

[0068] Preparation raw material F 1 , wherein the mass content of chloride C15 phosphine salt is 23.19%, the mass content of C5 aldehyde is 7.24% (the molar ratio of C5 aldehyde to chloride C15 phosphine salt is 1.1), and the water mass content is 69.57%. raw material F 1 Preheat to 50°C.

[0069] Prepare lye F 2 , wherein the mass concentration of potassium carbonate is 30%, the phase transfer aid cetyltrimethylammonium bromide mass concentration is 3.2%, and all the other are pure water (mole of potassium carbonate and cetyltrimethylammonium bromide than 25). Lye F 2 Preheat to 50°C.

[0070] Select n-hexane as extractant E 0 . Extractant E 0 Preheat to 50°C.

[0071] As shown in the attached figure, the raw material F 1 , lye F 2 and extractant E 0 The mass flow rates of 21.6kg / min, 5.5kg / min and 8.7kg / min are simultaneously passed into the first-stage reaction extraction stirring tank 1-1 and maintained at 50°C for the reaction extraction process. When the liqu...

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Abstract

The invention relates to a method for preparing vitamin A acetate by multi-stage continuous series reaction extraction. The device used in the method is a multi-stage continuous series reaction extraction device, which includes a reaction extraction stirring tank, a high-speed shear mixer, a pump, and a cyclone-liquid separation device. device and oil-water separator. The process: the raw material F 1 , lye F 2 and extractant E 0 Continuously feed into a multi-stage continuous series reaction extraction device to carry out wittig reaction synthesis to obtain vitamin A acetate. The present invention has the advantages that the reaction and extraction process can be carried out simultaneously in the multi-stage continuous series reaction extraction device, and the solid phase generated in the reaction process can be separated in time, which is beneficial to reduce the occurrence of side reactions and improve the yield of vitamin A acetate ; Compared with the traditional intermittent production process, the process of the present invention has realized continuous production, shortened the production cycle, and can reduce production costs.

Description

technical field [0001] The invention relates to a device and method for preparing vitamin A acetate through multi-stage continuous series reaction extraction, and belongs to the technical field of vitamin A and its derivative production. Background technique [0002] The chemical name of vitamin A is retinol, which is the first discovered fat-soluble vitamin and one of the essential nutrients for the human body. However, vitamin A is very unstable, and it is easily destroyed when it encounters acid, air, oxidizing substances, high temperature or ultraviolet rays, and is irritating to the skin. Vitamin A ester derivatives are more stable than vitamin A and are not irritating. Therefore, commercial vitamin A is provided in the form of ester, and the most common commercial form is vitamin A acetate. Vitamin A acetate is one of the most important series of vitamin A products. Because of its better stability and better pharmacological effects, its demand is increasing day by day...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C403/12
CPCC07C403/12C07C2601/16
Inventor 林龙冯兴磊张涛吕英东黎源罗朝辉张旭程晓波王延斌朱龙龙翟文超卢福广潘亚男黄存贺其他发明人请求不公开姓名
Owner WANHUA CHEM GRP CO LTD
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