Method for synthesizing vitamin C crude product by adopting L-gulonic acid

A vitamin and gulonic acid technology, applied in the direction of organic chemistry, can solve the problems of high labor intensity, long centrifugation time, and long process flow, and achieve the effects of improving the production environment, environmental protection of the production process, and simple process production

Inactive Publication Date: 2011-08-03
山东润鑫投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Adopting the cooling centrifugation process can bring the following problems: the technological process of the above-mentioned method is long, and the equipment that adopts is many; Secondly, part VC-Na is contained in the mother liquor that centrifuges out, causes the yield of vitamin C to

Method used

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  • Method for synthesizing vitamin C crude product by adopting L-gulonic acid
  • Method for synthesizing vitamin C crude product by adopting L-gulonic acid
  • Method for synthesizing vitamin C crude product by adopting L-gulonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Add 1.0mol of L-gulonic acid and 850ml of industrial methanol into a 2000ml reaction flask, add 4.85g of concentrated sulfuric acid at room temperature, raise the temperature to 66°C, and perform esterification for 2 hours. After the esterification reaction, the temperature was lowered to 55° C., an appropriate amount of baking soda (sodium bicarbonate) was added to adjust the pH value of the reaction solution to 9.0, the temperature was raised to 68° C., and the lactonization reaction was carried out for 3 hours. After the lactonization reaction, the temperature of the solution was lowered to 40° C., 55% dilute sulfuric acid was added until the pH of the reaction solution was 1.95, and the acidification reaction was carried out by keeping warm for 2 hours. Finally, the acidified solution is decolorized and filtered with activated carbon, and the filtrate is concentrated and crystallized, and the filtered white crystal is the crude vitamin C product. In Example 1, the p...

Embodiment 2

[0059] Add 1.0mol of L-gulonic acid and 870ml of industrial methanol into a 2000ml reaction flask, add 5.00g of concentrated sulfuric acid at room temperature, raise the temperature to 66°C, and perform esterification for 2 hours. After the esterification reaction, the temperature was lowered to 55° C., an appropriate amount of sodium bicarbonate was added to adjust the pH value of the reaction solution to 8.3, the temperature was raised to 68° C., and the lactonization reaction was carried out for 3 hours. After the lactonization reaction, the temperature of the solution was lowered to 40° C., 55% dilute sulfuric acid was added until the pH of the reaction solution was 1.90, and the acidification reaction was carried out by keeping warm for 2 hours. Finally, the acidified solution is decolorized and filtered with activated carbon, and the filtrate is concentrated and crystallized, and the filtered white crystal is crude vitamin C. In Example 2, the purity detected by HPLC was...

Embodiment 3

[0061] Add 1.0mol of L-gulonic acid and 890ml of industrial methanol into a 2000ml reaction flask, add 5.5g of concentrated sulfuric acid at room temperature, raise the temperature to 65°C, and perform esterification for 2 hours. After the esterification reaction, the temperature was lowered to 53° C., an appropriate amount of sodium bicarbonate was added to adjust the pH value of the reaction solution to 9.3, the temperature was raised to 69° C., and the lactonization reaction was carried out for 3 hours. After the lactonization reaction, the temperature of the solution was lowered to 40° C., 55% dilute sulfuric acid was added until the pH of the reaction material was 1.98, and the acidification reaction was carried out by keeping warm for 2 hours. The acidified solution is decolorized and filtered with activated carbon, the filtrate is concentrated and crystallized, and the filtered white crystal is crude vitamin C. In Example 3, the purity detected by HPLC was 99.5%, the de...

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Abstract

The invention provides a method for synthesizing vitamin C crude product by adopting L-gulonic acid, which comprises the following steps: the L-gulonic acid and a reaction solvent are added to a reaction vessel, and esterification reaction is carried out on the L-gulonic acid and the reaction solvent in the condition of strong acid catalyst so as to generate an L-gulonic acid methyl ester solution; internal esterification reaction is directly carried out on the L-gulonic acid methyl ester solution in alkalinity condition so as to generate a vitamin C sodium salt solution; after the vitamin C sodium salt solution cools down, dilute sulphuric acid is added directly for acidification reaction so as to generate an acidification solution; activated carbon decoloration filtration and concentration filtration are carried out on the acidification solution so as to obtain the vitamin C crude product, wherein esterification reaction, internal esterification reaction and acidification reaction are carried out in the same reaction vessel. The method provided by the invention has simple process, improves production efficiency, reduces labor intensity of workers and improves production environment.

Description

technical field [0001] The invention relates to the technical field of vitamin synthesis, in particular to a method for synthesizing crude vitamin C by using L-gulonic acid. Background technique [0002] As we all know, L-gulonic acid is generally used in the industry to prepare vitamin C. The preparation method that usually adopts in the prior art has following three steps: [0003] Step 1. Esterification conversion process: First, L-gulonic acid and methanol solvent are first subjected to esterification reaction in the presence of a strong acid catalyst to generate a methanol solution of L-gulonic acid methyl ester, and then the lactone is completed under alkaline conditions The chemical reaction produces a methanol solution of vitamin C sodium salt (VC-Na). [0004] Step 2, cooling centrifugation process: pump the methanol solution of VC-Na above into the cooling tank for cooling down, after reaching a certain temperature, put it into the centrifuge for centrifugal sepa...

Claims

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Application Information

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IPC IPC(8): C07D307/62
Inventor 米超杰宋道淮张忠庆
Owner 山东润鑫投资有限公司
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