Method for continuous crystallisation of vitamin C

A vitamin and crystallization technology, applied in organic chemistry and other directions, can solve the problems of small vitamin C crystal particles, difficult to control cooling speed, poor crystal form, etc., to achieve uniform crystal form, improve product quality, and reduce production costs.

Active Publication Date: 2009-04-01
DSM JIANGSHAN PHARMACEUTICAL (JIANGSU) CO LTD
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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 equipm

Method used

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Examples

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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 vitamin-C continuous crystallization method, including the following steps: a vitamin-C aqueous solution after ion-exchange is pumped into a first-stage crystallizing device for crystallization by vacuum evaporation; then the vitamin-C evaporated concentrated solution generated in the first-stage crystallizing device is continuously guided into a second-stage crystallizing device for crystallization by vacuum cooling; after the liquid and solid are separated, the crystals are washed and processed by centrifugation and then are continuously discharged to obtain the crude vitamin-C crystals; the crude vitamin-C crystals are dissolved by purified water and then pumped into a third-stage crystallizing device through a filter pump so as to realize the continuous crystallization of refined vitamin-C; after the liquid and solid are separated, the crystals are washed and processed by centrifugation and then are continuously discharged to obtain the refined vitamin-C crystals. The method adopted by the invention can realize the continuous crystallization of vitamin-C and obtain the large, even and well-shaped grains, which not only can enhance the quality, but also can reduce the manufacturing 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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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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