A method for continuous crystallization of vitamin C

A vitamin and crystallization technology, applied in the direction of organic chemistry, can solve problems such as difficulty in controlling cooling rate, poor crystal form, and fine vitamin C crystal particles, and achieve the effects of improving product quality, reducing production costs, and uniform crystal form

Active Publication Date: 2011-12-21
DSM JIANGSHAN PHARMACEUTICAL (JIANGSU) CO LTD
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AI Technical Summary

Problems solved by technology

The cooling crystallization and liquid-solid separation of crude vitamin C and the cooling crystallization and liquid-solid separation of high-quality vitamin C have relatively low requirements for equipment. The saturated vitamin C supersaturated solution causes the obtained vitamin C crystal particles to be fine and poor in crystal form, which cannot further improve the quality and yield of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0011] Concentrate the vitamin C aqueous solution (ion exchange liquid) with a concentration of 110mg / ml~160mg / ml into a vitamin C aqueous solution with a concentration of 25%~32% (W / V) through primary vacuum concentration, and then pass through a vacuum concentration crystallization system to obtain the solid content 20% to 40% vitamin C suspension. Alternatively, the vitamin C aqueous solution (ion exchange liquid) with a concentration of 110 mg / ml-160 mg / ml is directly passed through a vacuum concentration crystallization system to obtain a vitamin C suspension with a solid content of 20%-40%.

[0012] The primary vacuum concentration passes through the three-effect falling film evaporator, and adopts the method of decompression evaporation. During the concentration process, the evaporation temperature of the first-effect evaporator is controlled not to exceed 70°C, and the relative vacuum degree is not greater than -0.075MPa; the second-effect evaporator evaporates The tem...

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Abstract

The invention discloses a method for continuous crystallization of vitamin C. It includes the following steps: pump the ion-exchanged vitamin C aqueous solution into the first-stage crystallizer for vacuum evaporation and crystallization, and then continuously introduce the vitamin C evaporation concentrate produced in the first-stage crystallizer into the second-stage crystallizer for vacuum cooling Crystallization, after liquid-solid separation, crystal washing, centrifugation, and continuous discharge to obtain crude vitamin C crystals; after the crude vitamin C is dissolved in purified water, it is filtered and pumped into the third-stage crystallizer to realize continuous crystallization of high-quality vitamin C. After liquid-solid separation, crystal washing, centrifugation, and continuous discharge to obtain high-quality vitamin C crystals. The method adopted in the invention can realize the continuous crystallization of vitamin C and obtain coarse, uniform and neat crystal grains, which can not only improve product quality, but also reduce production cost.

Description

technical field [0001] The invention relates to the technical field of vitamin production, in particular to a method for continuous crystallization of vitamin C. Background technique [0002] The vitamin C production process of the prior art is: obtain 2-keto- L-Sodium Gulonic Acid Fermentation Broth; the protein and other impurities in the fermented liquid are removed by ultrafiltration, and sodium ions are removed by cation exchange to become 2-keto-L-gulonic acid aqueous solution, which is then concentrated, cooled and crystallized, liquid-solid The crystal 2-keto-L-gulonic acid intermediate was obtained by separation; using sulfuric acid as a catalyst, 2-keto-L-gulonic acid was subjected to methyl esterification reaction in methanol solution system to generate 2-keto-L-gulonic acid methyl Add a certain amount of sodium bicarbonate to carry out alkali conversion reaction to generate vitamin C sodium salt solution. After cooling and sedimentation, liquid-solid separation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/62
Inventor 毛煜祥葛亮刘杰秦苏东周灿芳钱海燕
Owner DSM JIANGSHAN PHARMACEUTICAL (JIANGSU) CO LTD
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