CN115850057A - Preparation method of calcium gluconate monohydrate - Google Patents
Preparation method of calcium gluconate monohydrate Download PDFInfo
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- CN115850057A CN115850057A CN202211680604.6A CN202211680604A CN115850057A CN 115850057 A CN115850057 A CN 115850057A CN 202211680604 A CN202211680604 A CN 202211680604A CN 115850057 A CN115850057 A CN 115850057A
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- calcium gluconate
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- gluconate monohydrate
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Abstract
The invention discloses a preparation method of calcium gluconate monohydrate, which takes gluconic acid-delta-lactone, calcium carbonate and water as initial raw materials and obtains the calcium gluconate monohydrate through hydrolysis, decoloration, crystallization and drying; wherein: the weight ratio of the gluconic acid-delta-lactone to the calcium carbonate is 10: 3-10: 5; the hydrolysis reaction temperature is 95-105 ℃, and the decolorization reaction temperature is 65-75 ℃; the temperature of adding the seed crystal is 55-65 ℃; the crystallization temperature is 5-15 ℃, and the crystallization time is 5-10 h; the drying is boiling drying, the time is 60-180 min, the air inlet temperature is 70 +/-10 ℃, and the frequency of an induced draft fan is 40 +/-10 Hz. According to the method, the content of the calcium gluconate monohydrate with higher purity can be obtained by properly increasing the temperature of adding the seed crystal; the method of the invention can effectively improve the reaction yield by properly increasing the temperature of the hydrolysis reaction and simultaneously properly reducing the temperature of the decolorization reaction.
Description
Technical Field
The invention belongs to the technical field of medicine preparation, and particularly relates to a preparation method of calcium gluconate monohydrate.
Background
Calcium gluconate (Calcium gluconate) is an organic Calcium salt, is white crystalline or granular powder in appearance, odorless, tasteless, dry without loss of water, not decomposed, and stable in air. The water solution is neutral, soluble in water, and insoluble in ethanol, diethyl ether, and other organic solvents. The main applications of the calcium supplement comprise a buffering agent, a chelating agent, a curing agent, a food additive, a calcium enhancer, a nutrient medicine and the like.
The calcium gluconate has anhydrous calcium gluconate (CAS number is 299-28-5, molecular formula is C 12 H 22 CaO 14 Molecular weight of 430.37) and calcium gluconate monohydrate (CAS number 18016-24-5, molecular formula C 12 H 22 CaO 14 ·H 2 O, molecular weight 448.39), and calcium gluconate monohydrate is required in large market quantity.
The main problems existing in the prior art are as follows: the calcium gluconate monohydrate prepared by the existing method contains more anhydrous calcium gluconate, so that the purity of the calcium gluconate monohydrate is low. Therefore, the technical problem to be solved in the field is to provide the calcium gluconate monohydrate with higher purity.
Known from the United states Pharmacopeia: the infrared spectrograms of the anhydrous calcium gluconate and the monohydrate gluconic acid have certain differences. The characteristic peak wave number of the former is 766cm -1 (middle) 865cm -1 (Weak) 948cm -1 (middle) 1007cm -1 1263-1250cm -1 (Strong), 1329cm -1 (middle), 1618cm -1 (strong); the characteristic peak wave number of the latter is mainly 878cm -1 (Weak) 972cm -1 (Weak), 1045cm -1 (middle) 1236cm -1 (middle) 1305cm -1 (middle) 1595cm -1 (Strong), the standard infrared spectrogram of calcium gluconate monohydrate is shown in figure 1.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of calcium gluconate monohydrate with higher purity.
The technical scheme for realizing the purpose of the invention is as follows: a preparation method of calcium gluconate monohydrate takes gluconic acid-delta-lactone, calcium carbonate and water as starting raw materials, and the calcium gluconate monohydrate is obtained by hydrolysis, decoloration, crystallization and drying.
In the crystallization step, the temperature of adding seed crystals is 55-65 ℃.
In the prior art, the temperature of adding the seed crystal does not exceed 45 ℃, and the applicant finds that: the temperature of adding the seed crystal is properly increased, and the calcium gluconate monohydrate with higher purity can be obtained.
Further, the hydrolysis reaction temperature is 95-105 ℃, and the decolorization reaction temperature is 65-75 ℃.
In the prior art, the hydrolysis reaction temperature is basically below 90 ℃ (for example CN106565460A, CN109608328A, CN112552167A, CN113045409A, CN111875490A and the like); the decolorization reaction temperature is usually the same as the hydrolysis reaction temperature (for example, CN106565460A, CN112552167A, CN113045409A, etc.), that is, no heating or cooling operation is performed after the hydrolysis reaction.
The applicant has found through a large number of experiments that: the hydrolysis reaction temperature is properly increased, and the decoloring reaction temperature is properly reduced, so that the reaction yield can be effectively improved.
The weight ratio of the gluconic acid-delta-lactone to the calcium carbonate is 10: 3-10: 5.
The crystallization temperature is 5-15 ℃, and the crystallization time is 5-10 h.
The drying is boiling drying, the time is 60-180 min, the air inlet temperature is 70 +/-10 ℃, and the frequency of an induced draft fan is 40 +/-10 Hz.
The invention has the following positive effects:
(1) The method can obtain the content of the calcium gluconate monohydrate with higher purity by properly increasing the temperature of adding the seed crystal.
(2) The method of the invention can effectively improve the reaction yield by properly increasing the temperature of the hydrolysis reaction and simultaneously properly reducing the temperature of the decolorization reaction.
Drawings
FIG. 1 is a standard infrared spectrum of calcium gluconate monohydrate.
FIG. 2 is an infrared spectrum of calcium gluconate monohydrate prepared in example 1.
FIG. 3 is an infrared spectrum of calcium gluconate monohydrate prepared in example 2.
FIG. 4 is an infrared spectrum of calcium gluconate monohydrate prepared in comparative example 1.
Detailed Description
(example 1)
The preparation method of calcium gluconate monohydrate of the embodiment comprises the following steps:
(1) and (4) hydrolyzing.
Adding 400kg of purified water into a reaction kettle, adding 50kg of gluconic acid-delta-lactone and 15kg of calcium carbonate into the reaction kettle under stirring, then heating to 100 +/-2 ℃, and carrying out hydrolysis reaction for 2h at the temperature to obtain the calcium gluconate aqueous solution.
(2) And (6) decoloring.
After the reaction is finished, cooling the reaction system obtained in the step (1) to 70 +/-2 ℃, adding 1kg of activated carbon, and carrying out a decoloring reaction for 30min at the temperature.
(3) And (4) crystallizing.
And (3) carrying out suction filtration on the reaction system obtained in the step (2) while the reaction system is hot, adding 2kg of seed crystal when the filtrate is naturally cooled to 60 +/-2 ℃, then cooling to 10 +/-2 ℃, and stirring for crystallization for 8 hours.
(4) And (5) drying.
And (4) carrying out suction filtration on the reaction system obtained in the step (3), and carrying out boiling drying on a filter cake for 70min, wherein: the temperature of an air inlet of the dryer is 70 ℃, the frequency of an induced draft fan is 40Hz, after the boiling drying is finished, discharging and cooling are carried out, 100kg of calcium gluconate monohydrate is obtained, the yield is 79.5%, and an infrared spectrogram is shown in figure 2.
As can be seen from fig. 2: the infrared spectrogram of calcium gluconate monohydrate obtained in this example is very close to fig. 1, which shows that the purity of calcium gluconate monohydrate obtained in this example is high.
(example 2)
This embodiment is substantially the same as embodiment 1 except that: in the step (1), the hydrolysis reaction temperature is 85 +/-2 ℃; in the step (2), the decoloring reaction temperature is 85 +/-2 ℃.
85kg of calcium gluconate monohydrate is finally obtained, the yield is 67.5%, and an infrared spectrogram is shown in figure 3.
As can be seen from fig. 3: the infrared spectrum of calcium gluconate monohydrate obtained in example 2 is very similar to that of fig. 1, which shows that the purity of calcium gluconate monohydrate obtained in example 2 is also higher, but the reaction yield is reduced compared with that of example 1.
Comparative example 1
This comparative example is essentially the same as example 1, except that: in the step (3), 2kg of seed crystal is added when the filtrate is naturally cooled to 40 +/-2 ℃.
97kg of calcium gluconate monohydrate is finally obtained, the yield is 77.1 percent, and an infrared spectrogram is shown in figure 4.
As can be seen from fig. 4: the infrared spectrogram of calcium gluconate monohydrate obtained in comparative example 1 has a certain difference from that in FIG. 1, and particularly has a characteristic peak wave number of 948cm of anhydrous calcium gluconate -1 It is shown that the calcium gluconate monohydrate obtained in the comparative example 1 contains more anhydrous calcium gluconate and has lower purity.
Claims (5)
1. A method for preparing calcium gluconate monohydrate uses glucono-delta-lactone, calcium carbonate and water as initial raw materials, and obtains the calcium gluconate monohydrate through hydrolysis, decoloration, crystallization and drying; the method is characterized in that: in the crystallization step, the temperature of adding seed crystals is 55-65 ℃.
2. The method for preparing calcium gluconate monohydrate according to claim 1, wherein the method comprises the following steps: the hydrolysis reaction temperature is 95-105 ℃, and the decoloration reaction temperature is 65-75 ℃.
3. The method of preparing calcium gluconate monohydrate according to claim 1 or 2, wherein: the weight ratio of the gluconic acid-delta-lactone to the calcium carbonate is 10: 3-10: 5.
4. The method of preparing calcium gluconate monohydrate according to claim 1 or 2, wherein: the crystallization temperature is 5-15 ℃, and the crystallization time is 5-10 h.
5. The method for preparing calcium gluconate monohydrate according to claim 1 or 2, wherein: the drying is boiling drying, the time is 60-180 min, the air inlet temperature is 70 +/-10 ℃, and the frequency of an induced draft fan is 40 +/-10 Hz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211680604.6A CN115850057A (en) | 2022-12-27 | 2022-12-27 | Preparation method of calcium gluconate monohydrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211680604.6A CN115850057A (en) | 2022-12-27 | 2022-12-27 | Preparation method of calcium gluconate monohydrate |
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| CN115850057A true CN115850057A (en) | 2023-03-28 |
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| CN202211680604.6A Pending CN115850057A (en) | 2022-12-27 | 2022-12-27 | Preparation method of calcium gluconate monohydrate |
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- 2022-12-27 CN CN202211680604.6A patent/CN115850057A/en active Pending
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