A kind of continuous cooling rapid crystallization method of calcium gluconate

Abstract

The invention discloses a continuous cooling and rapid crystallization method of calcium gluconate. The steps are as follows: add 7500-12000kg of glucose and 2100-3400kg of heavy calcium carbonate into a reaction tank, and use water to set the volume to 47000-48000L; add glucose Oxidase and catalase, add air, react for 10-12 hours; heat up the reacted solution to 80-100°C, keep warm for 30-40min, filter and add activated carbon for decolorization, control the content of activated carbon at 17-30%; decolorize After the final feed liquid is filtered, it is cooled by the cooling coil, and added to the motion crystallization tank at 30-50°C; the seed crystal is added under low-speed stirring, and the cooling circulating water is turned on to cool the feed liquid to 15-35°C at a uniform speed or gradient. Supernatant, when the calcium content is controlled at 3-10%, the crystallization ends. The kinematic crystallization method proposed by the present invention, the crystallization process continues to exchange heat, the temperature change remains uniform and constant, the crystal uniformity is good, and the continuous cooling process can better control the supersaturation of the mother liquid, so that the feed liquid is in the first metastable zone, effectively controlling Secondary nucleation has the advantages of shorter crystallization time and higher yield.

Description

Technical field [0001] The present invention relates to the field of preparation of calcium gluconate, and more particularly to a continuous cooling and rapid crystallization method of calcium gluconate. Background technique [0002] Calcium gluconate is a calcium salt of gluconic acid, and the molecular formula is CA (C 6 Hide 11 O 7 ) 2 · H 2 O, for white crystalline or particulate powder, melting point 201 ° C, odorless taste, slightly soluble in cold water (3 g / 100 mL, 20 ° C), is soluble in hot water (20 g / 100 mL). It is an important organic calcium, which is used for calcium in the clinic, and is also a raw material for other gluconate and gluconate, which is an important chemical export product in my country. [0003] At present, all domestic companies have a calcium gluconate crystallization section, which is basically used to stand crystallization. In patent CN106399404A, a method of producing calcium gluconate, glucose and glucose oxidase, and a hydrogenide enzyme m...

AI Technical Summary

Problems solved by technology

In this process, the static crystallization method mainly has the following disadvantages: ① After the crystallization is completed, the static crystallization needs to pump out the mother liquor in the crystallization tank and then manually shovel it out, which is labor-intensive and low-efficiency.

②The traditional static crystallization method, because the crystallization process requires heat dissipation, the crystallizer usually has a large specific surface area, which limits the volume of the equipment, and the crystallization equipment occupies a large area, so it is greatly disturbed by environmental factors, poor process stability, and poor product quality uniformity

③The product obtained by the traditional static crystallization method is prone to high water content due to the serious phenomenon of water in the crystal, and the finished product faces the risk of being unqualified

[0004] In the patent CN201710407823.X, a dynamic crystallization method of calcium gluconate is disclosed. The dynamic crystallization method in this invention has the following disadvantages: ①The dynamic crystallization described in this patent only has the nucleation process and the discharge process It is dynamic, and the process of nourishing essence is still static

Therefore, it cannot solve the problem that the heat of crystallization can only rely on radiation heat dissipation instead of convective heat transfer, so it cannot solve the problem of uneven crystallization conditions in the static crystallization method, nor can it fundamentally solve the problem of patina

②Because the crystallization process cannot effectively exchange heat and the crystallization speed is slow, it needs to stand still for 16-20h, and the production cycle is long

③In order to avoid excessive supersaturation after cooling down, this process is only applicable to the crystallization process of lower concentration, and the primary yield is low

[0005] Aiming at a series of defects in the above existing crystallization process of calcium gluconate production, such as long crystallization time, poor process stability, high labor intensity, and poor product quality uniformity, we proposed a new kinematic crystallization method for calcium gluconate