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Preparation method of calcium gluconate

A technology of calcium gluconate and gluconic acid, which is applied in the field of drug preparation, can solve problems such as low yield and unsatisfactory crystallization effect, and achieve the effects of improving crystallization efficiency, uniform and stable temperature, and improving reaction yield

Pending Publication Date: 2021-03-26
CHANGZHOU LANLING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the biggest problem in the preparation of calcium gluconate is: the yield is not high, usually only about 70%
[0007] The main reason for the low yield is: the crystallization effect is not ideal, and the crystallization mother liquor contains a large amount of product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0017] The preparation method of the calcium gluconate of the present embodiment has the following steps:

[0018] ①Put 700L of purified water into the reactor, start stirring, add 89kg (0.50kmol) glucono-δ-lactone, after stirring and dissolving completely, add 25kg (0.25kmol) of calcium carbonate, add purified water to a total volume of 850L, The temperature was raised to 85±1°C and the reaction was stirred for 1.5 hours to obtain an aqueous solution of calcium gluconate. Then add 1 kg of 50-mesh medicinal activated carbon at one time under stirring, and decolorize at 85±1°C for 30 minutes.

[0019] ②Filtrate while it is hot, cool the filtrate to 35±1°C, add 2kg of seed crystals, then cool down to 15±1°C, maintain the temperature and stir for crystallization at a frequency of 20±1Hz for 10h.

[0020] ③ After centrifugal filtration, the filter cake was pulverized and boiled and dried at 70°C for 2 hours to obtain 106.6 kg of calcium gluconate with a yield of 95.2% and a purit...

Embodiment 2～ Embodiment 3）

[0022] The preparation method of each embodiment is basically the same as that of Example 1, except that see Table 1.

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PUM

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Abstract

The invention discloses a preparation method of calcium gluconate, which comprises the following steps: (1) reacting gluconic acid-delta-lactone with calcium carbonate at 80-90 DEG C to obtain a calcium gluconate water solution, adding medicinal activated carbon, and keeping the temperature at 80-90 DEG C for 30 minutes; and (2) filtering while hot, cooling the filtrate to 30-40 DEG C, adding seedcrystals, cooling to 10-20 DEG C, and stirring and crystallizing at the frequency of 20 + / -1Hz for 8-12 hours; and (3) centrifugally filtering, and crushing and drying a filter cake to obtain a calcium gluconate finished product. It is found through a large number of experiments that by controlling the stirring crystallization temperature and the stirring frequency, it can be guaranteed that thetemperature in the crystallization kettle is uniform and stable, and therefore the problems of crystallization caking, crystallization slurry wrapping, large supersaturation degree and the like are solved, the crystallization efficiency is remarkably improved, and the reaction yield is greatly increased.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a preparation method of calcium gluconate. Background technique [0002] Calcium gluconate (also known as calcium gluconate monohydrate) is an organic calcium salt with the chemical formula C 12 h 24 o 15 Ca, appearance is white crystalline or granular powder, melting point is 201°C (decomposition), odorless, tasteless, soluble in boiling water (20g / 100mL), slightly soluble in cold water (3g / 100mL, 20°C), insoluble in Organic solvents such as ethanol or ether. The aqueous solution is neutral (pH about 6-7). Calcium gluconate is mainly used as calcium fortifier and nutrient, buffer, curing agent and chelating agent in food. [0003] At present, the method for preparing calcium gluconate mainly includes following two classes: [0004] (1) Glucose oxidation method: that is, glucose and calcium carbonate are used as starting materials to react in the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/105C07C51/41C07C51/43
CPCC07C51/412C07C51/43C07C59/105
Inventor 马斌尹文娟吴燕枫徐芳芳
Owner CHANGZHOU LANLING PHARMA