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, and can solve problems that have not yet involved in the esterification synthesis reaction of solid raw materials, the application of combined membrane technology that has not involved VC esterification reaction, and long reaction time, etc. , to achieve the effect of stable reaction, easy production and small membrane area
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Embodiment 1
[0027] see figure 1 , 2-KLG methyl esterification-pervaporation membrane separation integrated process flow is:
[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] exist figure 2 The esterification reaction-pervaporation membrane separation is performed in the experimental setup of the shown integrated process. 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, after 20 minutes 2-KLG was...
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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