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Crystallization method of calcium gluconate

A technology of calcium gluconate and glucose, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate, etc., can solve the problems of increasing operation time and easy generation of impurities, and achieve reduction of production energy consumption, The effect of shortening production time and reducing cost

Inactive Publication Date: 2019-11-15
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In patent CN101033189, 12% ethanol aqueous solution is used for crystallization, and the crystallization time is as long as 24 hours; in patent CN106365983A, the solution needs to be concentrated at 50°C before crystallization, which increases the operating time, and long-term high-temperature distillation is easy to produce impurities

Method used

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  • Crystallization method of calcium gluconate
  • Crystallization method of calcium gluconate
  • Crystallization method of calcium gluconate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 20g of glucose into the reaction bottle, add 200mL of purified water and stir to dissolve, add 1.0g of palladium-carbon alloy Pd-Pt / C catalyst, control the temperature at 55±5°C, pass air into the reaction solution, and add calcium carbonate in batches to adjust pH to 7.0, and then pass air until the pH value of the reaction solution no longer drops.

[0031] Filter with a 0.45 μm filter, add 0.4 g of activated carbon, stir and decolorize at 70° C. for 1 hour, and filter with a 0.45 μm filter.

[0032] Measure the volume of the filtrate to be 132mL, add 70mL of methanol, cool to 10°C, heat and crystallize for 5 hours, filter, and dry the filter cake at 60°C to obtain 21.2g of calcium gluconate monohydrate, with a yield of 85.2% and a purity of 98.41%. .

Embodiment 2

[0034] Put 20g of glucose into the reaction bottle, add 200mL of purified water and stir to dissolve, add 1.0g of palladium-carbon alloy Pd-Pt / C catalyst, control the temperature at 55±5°C, pass air into the reaction solution, and add calcium carbonate in batches to adjust pH to 7.0, and then pass air until the pH value of the reaction solution no longer drops.

[0035] Filter with a 0.45 μm filter, add 0.8 g of activated carbon, stir and decolorize at 70° C. for 1 hour, and filter with a 0.45 μm filter.

[0036] Measure the volume of the filtrate to be 170mL, add 150mL of absolute ethanol, cool to 20°C, heat and crystallize for 3 hours, filter, and dry the filter cake at 70°C to obtain 21.6g of calcium gluconate monohydrate, with a yield of 86.8%, a purity of 99.43%.

Embodiment 3

[0038] Put 50g of glucose into the reaction bottle, add 600mL of purified water and stir to dissolve, add 2.5g of palladium-carbon alloy Pd-Pt / C catalyst, control the temperature at 55±5°C, pass air into the reaction solution, and add calcium carbonate in batches to adjust pH to 7.0, and then pass air until the pH value of the reaction solution no longer drops.

[0039] Filter with a 0.45 μm filter, add 2.5 g of activated carbon, stir and decolorize at 70° C. for 1 hour, and filter with a 0.45 μm filter.

[0040] Measure the volume of the filtrate to be 490mL, add 735mL of isopropanol, cool to 20°C, keep warm and crystallize for 2 hours, filter, and dry the filter cake at 65°C to obtain 57.0g of calcium gluconate monohydrate, with a yield of 91.6%, purity 99.88%.

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Abstract

The invention belongs to the technical field of medicine production and particularly relates to a crystallization method of calcium gluconate. The crystallization method of the calcium gluconate comprises the following steps: (1) oxidizing glucose into gluconic acid at 50 to 60 DEG C by taking palladium carbon alloy Pd-Pt / C as a catalyst and taking air as an oxidizing agent, and adding calcium carbonate until the pH is 6 to 7 to obtain oxidizing reaction liquid of the glucose; (2) filtering the reaction liquid, adding activated carbon to perform decolorization and filtering; (3) adding an alcohols solvent; (4) cooling to 10 to 20 DEG C and performing crystallization for 2 to 5 hours; and (5) centrifuging and drying to obtain calcium gluconate monohydrate. Operation of concentrating the reaction liquid is omitted, so production time is greatly shortened and production energy consumption is reduced; and high yield (capable of reaching to 91.6 percent) and purity (capable of reaching to 99.88 percent) can be realized by cooling to 10 to 20 DEG C and performing crystallization for 2 to 5 hours, and centrifugal mother liquid can be reused after simple distillation, so cost is effectively reduced.

Description

technical field [0001] The invention belongs to the technical field of medicine production, and in particular relates to a crystallization method of calcium gluconate. Background technique [0002] Calcium gluconate is the calcium salt monohydrate of D-gluconic acid, the molecular formula is C 12 h 22 CaO 14 ·H 2 O, white granular powder, odorless and tasteless. As a drug, calcium gluconate can reduce capillary permeability, increase density, maintain normal excitability of nerves and muscles, strengthen myocardial contractility, and help bone formation. It is suitable for allergic diseases, such as urticaria, eczema, pruritus, contact dermatitis and serum sickness; it can also be used as an adjuvant treatment for angioedema; it is also suitable for convulsions and magnesium poisoning caused by hypocalcemia, prevention of and treatment of calcium deficiency. As a food additive, it can be used as a buffer, curing agent, chelating agent, and nutritional supplement. Acco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/235C07C51/41C07C51/47C07C51/43C07C59/105
CPCC07C51/235C07C51/412C07C51/43C07C51/47C07C59/105
Inventor 任继波杨学谦刘印孔令金郑亮李宗涛马晓红原江涛
Owner SHANDONG QIDU PHARMA
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