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Method for synthesizing vitamin C sodium salt

A synthetic method and vitamin technology, applied in the direction of organic chemistry, can solve problems such as low esterification rate, unsatisfactory product color and quality, and long reaction time, so as to increase yield, shorten conversion reaction time, and prolong equipment service life Effect

Active Publication Date: 2010-06-16
HEBEI WELCOME PHARMACEUTICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a new synthetic method of vitamin C sodium salt, to solve the problems of low esterification rate, long reaction time, unsatisfactory product color and quality in the existing process as a whole

Method used

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  • Method for synthesizing vitamin C sodium salt
  • Method for synthesizing vitamin C sodium salt

Examples

Experimental program
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Embodiment 1

[0021] according to figure 1 As shown in the flow process, (1) take 300g of pure gulong acid with a content of 90.82% and place it in a reaction flask, add 900ml of 99.50% industrial methanol to dissolve the material, and then pass through the granular activated carbon column decolorization and SQD- 67 cation-exchange resin columns to remove metal impurities; (2) the treated methanol solution of guronic acid was filtered through a drying column filled with erionite (commercially available) with an adsorption critical diameter of 3A. (3) Preheating the strongly acidic styrene-based cation-exchange resin column to 50° C. to keep it at a constant temperature, passing the methanol solution of guronic acid through the resin column to circulate the material, and performing an esterification reaction for 3 hours to obtain an esterification reaction solution; (4) The esterification reaction solution was injected into the normal pressure reactor, and 110.4 grams of sodium bicarbonate w...

Embodiment 2

[0023] The technical process is the same as in Example 1, (1) get 91.51% gulong acid pure 300g and place it in a reaction flask, add 99.50% industrial methanol 1200ml to dissolve the material, then pass through the granular activated carbon column at 1 times speed at normal temperature for decolorization and SQD-67 cation exchange resin column removes metal impurities; (2) Guronic acid methanol solution after treatment is filtered through a drying column filled with 3A molecular sieve adsorbent (available from the market); (3) (732) 001× 7 Preheat the strongly acidic cation exchange resin column to 55°C, keep it at a constant temperature, pass the treated guaronic acid methanol solution through the resin column, and circulate the material, and perform esterification reaction for 3.5 hours to obtain an esterification reaction solution; (4) esterification The reaction solution was injected into the normal pressure reactor, and 103.9 g of sodium bicarbonate was added for conversio...

Embodiment 3

[0025] (1) Take 92.28% gulong acid pure 300g and place it in a reaction flask, add 99.50% industrial methanol 1500ml to dissolve the material, and then pass through the granular activated carbon column decolorization and SQD-67 cation exchange resin column at room temperature with a flow rate of 1 times speed Remove metal impurities; (2) the treated gulong acid methanol solution is passed through a drying column filled with 3A molecular sieve adsorbent; (3) the strongly acidic cation exchange resin column is preheated to 60°C to keep it at a constant temperature, and the treated cologne The acid methanol solution was circulated through the resin column to feed, and the esterification reaction was carried out for 4 hours to obtain the esterification reaction solution; (4) the esterification reaction solution was injected into the normal pressure reactor, and 90.9 grams of sodium bicarbonate was added for conversion reaction for 1 hour, and then added 28.7 grams of sodium carbona...

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Abstract

The invention discloses a method for synthesizing vitamin C sodium salt which comprises the steps of: (a) mixing Gulonic acid with methanol solution, and orderly passing through a granular active carbon column and a cation resin column, (b) passing the treating fluid through a dry filter, (c) performing a recycle esterification reaction by passing the treating fluid acquired from the step b through the resin column so as to acquire esterified liquid, (d) pouring the esterified liquid into a constant pressure reactor and performing conversion reaction, and (e) cooling the liquid material B to room temperature after finishing the reaction and centrifuging so as to acquire the vitamin C sodium salt. The method of the invention efficiently promotes the esterifying ratio of products and the yield of the vitamin C sodium salt, shortens the conversion reaction time, simplifies the process, lowers the energy consumption and producing cost, decreases the environmental pollution and prolongs the service life of the device.

Description

technical field [0001] The invention relates to a synthesis method of organic compounds, in particular to a synthesis method of vitamin C sodium salt. Background technique [0002] Vitamin C sodium salt (referred to as Vc-Na) is an important intermediate for the production of vitamin C by two-step fermentation. Its English name is Sodium L-Ascorbate, molecular formula: C 6 h 7 NaO 6 , molecular weight: 198.11. At present, the process of synthesizing vitamin C by the two-step fermentation method is usually to mix gulong acid and methanol according to a certain ratio, use concentrated sulfuric acid as a catalyst, and carry out methylation reaction at 60-70°C under normal pressure. After the methylation reaction is finished, cool the methylation reaction solution to 50-55°C, and add sodium bicarbonate which is the sum of the moles of gulonic acid and 1 / 2 the moles of concentrated sulfuric acid or 1 / 2 the moles of gulonic acid and 1 / 4 sodium carbonate of the sum of moles of...

Claims

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Application Information

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IPC IPC(8): C07D307/62
Inventor 米造吉崔永涛王宏民张红艳宋海英章志峰王乐
Owner HEBEI WELCOME PHARMACEUTICAL CO LTD
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