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Production process of 2-keto-L-gulonic acid methyl ester

A technology of methyl guronate and gulon acid, which is applied to the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve the problems of large production equipment, high labor intensity, and large consumption of concentrated sulfuric acid. Achieve the effect of reducing the occupied area, reducing the workload of workers and shortening the reaction time

Active Publication Date: 2019-12-20
石药集团维生药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101735183A discloses a method for synthesizing vitamin C sodium salt. Gulonic acid and methanol solution are mixed according to the ratio of mass volume ratio of 1:3 to 5, heated and dissolved, followed by granular activated carbon column for decolorization and cationic resin column for impurity removal. , dry filter to remove water; the treatment solution is heated to 40-60°C through the resin column to circulate the esterification reaction; the esterification solution is then converted to obtain vitamin C sodium salt, although compared with the traditional esterification reaction, it is replaced by resin Concentrated sulfuric acid is used as a catalyst, and there is no sodium sulfate residue in the crude Vc-Na produced, and the yield is high, but the process increases, the operation is cumbersome, and it takes a long time
[0004] The preparation of 2-keto-L-gulonic acid methyl ester in the above vitamin C production process belongs to intermittent production process, normal pressure reaction, long reaction time, Generally more than 3h, the production efficiency is low, and the traditional 2-keto-L-gulonic acid methyl ester preparation process uses a large amount of concentrated sulfuric acid, and the mass volume ratio of the concentrated sulfuric acid consumption to 2-keto-L-gulonic acid is 0.027 The above not only increases the production cost, but also affects the quality of the finished product; in addition, the production equipment occupies a large area and the labor intensity of the workers is high, which is also one of the problems to be solved in the existing 2-keto-L-gulonic acid methyl ester production process

Method used

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  • Production process of 2-keto-L-gulonic acid methyl ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Production equipment: Three heat exchangers (A1, A2, A3) are used in series to form a feed heat exchanger. After the feed heat exchanger is connected to the tubular reactor B as an esterification reaction device, the material outlet of the tubular reactor B is The heat medium inlet of the primary heat exchanger formed by the countercurrent flow setting of the first heat exchanger A1 before the feed heat exchanger is connected, and the heat medium outlet of the primary heat exchanger of the feed heat exchanger is used as the production of 2-keto-L -The outlet of methyl guronate equipment, the last two heat exchangers (A2, A3) of the feed heat exchanger are connected in series and each heat exchanger is the second stage of the feed heat exchanger composed of countercurrent flow combination The heat exchanger adopts an external heat source;

[0024] Specific operation:

[0025] In the batching tank, add 2-keto-L-gulonic acid and methanol according to the mass volume ratio...

Embodiment 2

[0027] Production equipment: with embodiment 1

[0028] Specific operation:

[0029] In the batching tank, add 2-keto-L-gulonic acid and methanol according to the mass volume ratio of 2-keto-L-gulonic acid and methanol at a ratio of 1:6, and then add 2-keto-L-gulonic acid according to the The mass volume ratio of acid to concentrated sulfuric acid is 1:0.01. Slowly add concentrated sulfuric acid, start stirring, and the uniformly mixed feed liquid T1 is continuously added to the feed heat exchanger for heating, so that the feed liquid temperature rises to 76°C, and then enters the tube React in reactor B, keep the temperature in the reactor at 76°C, the pressure at 0.3MPa, control the residence time of the feed liquid in tubular reactor B to 40min, and flow out of tubular reactor B, that is, the ester after esterification As a heat source, the chemical liquid T2 is passed into the primary heat exchanger formed by the countercurrent flow of the first heat exchanger A1 in front...

Embodiment 3

[0031] Production equipment: with embodiment 1

[0032] Specific operation:

[0033] In the batching tank, add 2-keto-L-gulonic acid and methanol according to the mass volume ratio of 2-keto-L-gulonic acid and methanol at a ratio of 1:5, and then add 2-keto-L-gulonic acid according to the The mass volume ratio of acid to concentrated sulfuric acid is 1:0.004. Slowly add concentrated sulfuric acid, start stirring, and the uniformly mixed feed liquid T1 is continuously added to the feed heat exchanger for heating, so that the feed liquid is heated to 90°C, and then enters the tube React in reactor B, keep the temperature in the reactor at 90°C, the pressure at 0.45MPa, control the residence time of the feed liquid in tube reactor B to 20min, and flow out of tube reactor B, that is, the ester after esterification As a heat source, the chemical liquid T2 is passed into the primary heat exchanger formed by the countercurrent flow of the first heat exchanger A1 in front of the feed...

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Abstract

The invention discloses a method for continuously producing 2-keto-L-gulonic acid methyl ester by taking 2-keto-L-gulonic acid as a raw material. A plurality of heat exchangers are connected in seriesto form a feeding heat exchanger; the back of the feeding heat exchanger is connected to a tubular reactor to form an esterification reaction device; a material outlet of the tubular reactor is connected to a thermal medium inlet of a primary heat exchanger formed by combining the first M heat exchangers of the feeding heat exchanger; a thermal medium outlet of the primary heat exchanger of the feeding heat exchanger is used as a discharging port of equipment for producing the 2-keto-L-gulonic acid methyl ester; and a secondary heat exchanger formed by combining the last N heat exchangers ofthe feeding heat exchanger adopts an external heat source. The production method comprises the following steps: blending, heating and continuous esterifying. The method has the beneficial effects that: the reaction time is remarkably shortened, the energy consumption is reduced, the workload of workers is reduced, the use amount of sulfuric acid is remarkably reduced, byproducts are reduced, the product quality is further improved, the use amount of conversion reaction alkali can be further reduced, the production cost can be further reduced, and the like.

Description

technical field [0001] The invention relates to a production process of 2-keto-L-gulonic acid methyl ester, in particular to a method for continuously producing 2-keto-L-gulonic acid methyl ester with 2-keto-L-gulonic acid as raw material The invention belongs to the technical field of vitamin C preparation. Background technique [0002] Vitamin C, also known as L-ascorbic acid, is a common raw material, which can be used to prevent and treat diseases. Diseases such as mental depression can also be used in a large amount in the food industry as fortifiers and antioxidants. [0003] The production method of vitamin C mainly adopts two-step fermentation to prepare gulong acid, and then produces vitamin C through chemical transformation. At present, the current conversion process in China is mainly an alkali conversion process, that is, 2-keto-L-gulonic acid and methanol under the action of sulfuric acid to generate 2-keto-L-gulonic acid methyl ester, and then add NaHCO 3 or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H7/027C07H1/00
CPCC07H7/027C07H1/00Y02P20/10
Inventor 翁喜军杨剑宇王清格朱英刚贾慧卿张晓卿彭广存杨斌李会然董霞
Owner 石药集团维生药业(石家庄)有限公司
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