Method for cleaner production of vitamin C

A clean production and vitamin technology, applied in the direction of nitrogen fertilizer, ammonium salt fertilizer, fertilization equipment, etc., can solve the problems of huge production equipment, waste of resources, high acid consumption, etc., to reduce the pressure of environmental protection treatment, reduce production costs, and reduce emissions volume effect

Pending Publication Date: 2018-06-22
ZHENGZHOU TUOYANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the whole process, cation exchange resin is used twice to convert sodium salt into acid. The demand for resin is large, the production equipment is relatively large, and the operating system is complicated; and the regeneration process consumes a lot of acid and alkali, and discharges a large amount of high-salt wastewater.
Because in the conversion process of 2-keto-L-gulonic acid methyl ester, sodium carbonate is used as an alkali source to convert

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for clean production of vitamin C. Add 2-keto-L-gulonic acid, methanol and concentrated sulfuric acid into a reaction kettle and stir evenly. The temperature is raised to 55°C and refluxed for 5 hours to obtain a methyl gulonate solution. To 65°C, then pass ammonia gas at a rate of 0.18mL / min until the pressure in the reactor rises to 0.008MPa, then increase the ammonia gas flow rate to 0.38mL / min until the pressure of the reactor is 0.018MPa , Obtain the vitamin C ammonium salt methanol solution, cool to 5° C. and filter to obtain the vitamin C ammonium salt solid, and then dissolve the solid in deionized water, and then process the hydrogen type ion exchange resin to obtain vitamin C and ammonium sulfate. The molar ratio of 2-keto-L-gulonic acid to ammonia gas is 1:1.2; the molar ratio of 2-keto-L-gulonic acid to methanol is 1:30.

Embodiment 2

[0023] A method for clean production of vitamin C. Add 2-keto-L-gulonic acid, methanol and concentrated sulfuric acid into a reaction kettle and stir evenly, heat up to 50°C, reflux for 3 hours, and obtain methyl gulonate solution. To 63℃, then feed ammonia at a rate of 0.2mL / min until the pressure in the reactor rises to 0.01MPa, and then increase the feed rate of ammonia to 0.4mL / min until the pressure of the reactor is 0.02MPa , Obtain the vitamin C ammonium salt methanol solution, cool to 2° C. to filter to obtain the vitamin C ammonium salt solid, then dissolve the solid with deionized water, and process the hydrogen type ion exchange resin to obtain vitamin C and ammonium sulfate. The molar ratio of 2-keto-L-gulonic acid to ammonia is 1:1.03, and the molar ratio of 2-keto-L-gulonic acid to methanol is 1:25.

Embodiment 3

[0025] A method for the clean production of vitamin C. Add 2-keto-L-gulonic acid, methanol and concentrated hydrochloric acid into a reaction kettle and stir evenly. The temperature is raised to 60°C and refluxed for 4 hours to obtain a methyl gulonate solution. To 68°C, then pass ammonia gas at a rate of 0.22mL / min until the pressure in the reactor rises to 0.012MPa, then increase the ammonia gas flow rate to 0.42mL / min until the pressure of the reactor is 0.02MPa , Obtain the vitamin C ammonium salt methanol solution, cool to 0° C. and filter to obtain the vitamin C ammonium salt solid, and then dissolve the solid with deionized water, and then process the hydrogen type ion exchange resin to obtain vitamin C and ammonium sulfate. The molar ratio of 2-keto-L-gulonic acid to ammonia is 1:1.33, and the molar ratio of 2-keto-L-gulonic acid to methanol is 1:28.

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Abstract

The invention provides a method for cleaner production of vitamin C. The method comprises the following steps: adding 2-keto-L-gulonic acid, methanol and a catalyst into a reaction kettle and uniformly stirring; raising the temperature to 50 DEG C to 60 DEG C; after reflowing for 2 to 5h, obtaining a gulonate methyl ester solution; raising the temperature to 60 DEG C to 68 DEG C; then introducingammonia gas at a speed of 0.18 to 0.22mL/min until pressure in the reaction kettle is raised to 0.008 to 0.012MPa; then improving the speed of the introduced ammonia gas to 0.38 to 0.42mL/min until the pressure of the reaction kettle is 0.018 to 0.02MPa, so as to obtain a vitamin C ammonium salt methanol solution; cooling to 0 to 5 DEG C and filtering to obtain a vitamin C ammonium salt solid; after dissolving the solid with de-ionized water, treating through hydrogen type ion exchange resin to obtain the vitamin C and ammonium sulfate. The method provided by the invention has moderate reaction temperature; the yield of the vitamin C is improved and the reaction time of conversion is shortened; a byproduct ammonium sulfate fertilizer is produced and wastes are changed into valuable things;meanwhile, the production cost is reduced and economic and environment-friendly benefits are realized.

Description

Technical field [0001] The invention belongs to the technical field of vitamin C preparation, and specifically relates to a method for cleanly producing vitamin C. Background technique [0002] Vitamin C, commonly known as ascorbic acid, is a catalyst in the oxidation-reduction reaction of cells. It has strong activity and can participate in various metabolisms of the human body. It can reduce the fragility of capillaries, increase the body’s resistance and prevent the occurrence of scurvy. Essential nutrients, most animals can synthesize vitamin C by themselves, but humans, apes, guinea pigs, etc. must be taken from outside. In addition, it has strong reducing ability and can be used as an antioxidant. It has been widely used in medicine and food industry. [0003] With the increase of the experimental application scope of vitamin C, the market demand is increasing day by day, and people continue to conduct research on the experimental production technology of vitamin C. The pro...

Claims

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Application Information

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IPC IPC(8): C07D307/62C05C3/00
CPCC07D307/62C05C3/00
Inventor 崔凤霞胡景辉曹琳青张抗周俊俊高莉龚舒李月番史小利闫世梁刘银霞张生克肖媛勾丽莉王敬臣秦天苍
Owner ZHENGZHOU TUOYANG IND
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