Method for producing vitamin C by esterification reaction-infiltration evaporation barrier separation integral process

A technology of pervaporation membrane and methyl esterification reaction, which is applied in the application field of pervaporation membrane technology, can solve the problems that have not yet involved the esterification synthesis reaction of solid raw materials, long reaction time, and the combined membrane technology not involved in esterification reaction, etc., reaching The effect of stable reaction, small membrane area and easy production

Inactive Publication Date: 2008-03-12
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] M.T.Sanz and Jurgen Gmehling successively in "Esterification of acetic acid with isopropanol coupled with pervaporation Part I: Kinetics and pervaporationstudies" ("Chemical Engineering Journal". 2006, 123: 1-8) and "Esterification of acetic acid with isopropanol coupled with pervaporation Part II : Study of apervaporation reactor" ("Chemical Engineering Journal" 2006, 123: 9-14) shows that the use of PERVAP  The 2201 membrane selectively removes the water produced in the isopropanol / acetic acid esterification reaction. With the increase of the molar ratio of isopropanol / acetic acid, the ratio of the membrane area to the volume of the reaction solution, the operating temperature and the amount of catalyst added, The yields of esters were all increased to varying degrees, but the reaction time was too long, and the equilibrium of the conventional esterification reaction was not broken until 10 hours later.
[0010] The esterification reaction-pervaporation membrane integration technology mentioned in the above-mentioned documents is all used for either n-butyl acetate or ethyl lactate at a higher reaction temperature or under the condition of a high membrane area to reaction liquid volume ratio. The esterification reaction of liquid raw materials such as esters or isopropyl acetate has not yet involved the esterification synthesis reaction of solid raw materials in the reactants, let alone V C Application of Esterification Reaction Combined Membrane Technology in Production Process

Method used

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  • Method for producing vitamin C by esterification reaction-infiltration evaporation barrier separation integral process
  • Method for producing vitamin C by esterification reaction-infiltration evaporation barrier separation integral process

Examples

Experimental program
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Effect test

Embodiment 1

[0027] See Figure 1. The integrated process flow of 2-KLG methyl esterification reaction-pervaporation membrane separation is as follows:

[0028] Preparation of binary reaction solution of 2-KLG and methanol → esterification reaction-pervaporation membrane separation → termination of methyl esterification reaction. The inventive method starts from 2-KLG raw material, through esterification reaction-pervaporation membrane separation integration process, finally obtains for V C Production of highly pure 2-keto-L-gulonic acid methyl ester liquid.

[0029] The esterification reaction-pervaporation membrane separation was carried out in the experimental setup of the integrated process shown in Figure 2. Get 400mL methanol (density 0.792g / mL), inject in the there-necked flask that has stirrer, reflux condenser, open stirrer, then inject 120.43g purity and be 91% 2-KLG (methanol and 2-KLG mass ratio are 2.89), the temperature of the reaction solution was kept constant at 50°C, aft...

Embodiment 2

[0034] According to the operation of embodiment 1, wherein, only changing the ratio of the effective membrane area of ​​the pervaporation membrane to the volume of the reaction solution is 0.083cm -1 , the vacuum on the downstream side of the membrane was 600Pa, and at the end of the methyl esterification reaction, HPLC analysis showed that 93.86% of 2-KLG in the reaction solution was converted into 2-Me-KLG, and 479 mL of light yellow 2-keto-L-cologne was obtained methyl ester solution.

Embodiment 3

[0036] According to the operation of Example 1, wherein only the mass ratio of methanol to 2-KLG is changed to 1.74, the vacuum on the downstream side of the membrane is 670Pa, HPLC analysis shows that 98.17% of the 2-KLG in the reaction solution is converted into 2-Me-KLG , Obtain 516mL light yellow 2-keto-L-gulonic acid methyl ester liquid.

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Abstract

The present invention provides a method of synthesizing the vitamin C (V C ) through the esterification, the pervaporation (PV) membrane separation and integration technology, comprising the process of the methyl esterification between the methanol and the 2-ketone-L-gulonic acid (2-KLG) to produce the 2-ketone-L-gulonic methyl ester (2-Me-KLG). The process comprises the following steps: (1) the solid or liquid 2-KLG is dissolved in the methanol; the temperature is then raised and the catalyst is added; (2) the reaction solution prepared in the first step is pumped into the PV membrane separation device; the reaction solution after the membrane dehydration circulates into the esterification reactor; (3) the product 2-Me-KLG or the reaction solution is directly provided for the later production of the VC. In the method of the present invention, the area of the used membrane is small; the ratio between the alcohol and acid of the raw material liquid and the reaction temperature are relatively low; the invention greatly improves the purity and collection rate of the 2-Me-KLG; the technology is simple and the process is stable; the present invention is suitable for the industrial production-line.

Description

technical field [0001] The invention relates to the application of pervaporation membrane technology in the esterification industry, in particular to a method for producing vitamin C by adopting an esterification reaction-pervaporation membrane separation integration process. Background technique [0002] V C V C The production scale and output are constantly expanding. [0003] V C One of the important links in the production process of methanol is the methyl esterification reaction of methanol and 2-keto-L-gulonic acid (hereinafter referred to as: 2-KLG) to generate 2-keto-L-gulonic acid methyl ester (hereinafter referred to as: 2-KLG) -Me-KLG). Currently, traditional processes for V C Most of the produced esterification reactions are maintained in a liquid system in which the weight ratio of methanol to 2-KLG is 1-1.5. Its reaction formula is as follows: [0004] [0005] The 2-Me-KLG obtained by the above methylation reaction reacts with sodium bicarbonate to g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/08C07D307/62
Inventor 蔡邦肖邸天梅
Owner ZHEJIANG GONGSHANG UNIVERSITY
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