CN111875490A - Preparation method of calcium gluconate - Google Patents
Preparation method of calcium gluconate Download PDFInfo
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- CN111875490A CN111875490A CN202010793387.6A CN202010793387A CN111875490A CN 111875490 A CN111875490 A CN 111875490A CN 202010793387 A CN202010793387 A CN 202010793387A CN 111875490 A CN111875490 A CN 111875490A
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- C07C51/41—Preparation of salts of carboxylic acids
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Abstract
The invention discloses a preparation method of calcium gluconate, which comprises the steps of selecting waste egg shells and crab shells as raw materials, washing with water, alkali washing, crushing, acid leaching, decoloring and alkali precipitation to obtain calcium carbonate powder, then adding distilled water to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under the water bath heating condition of 60-70 ℃, decoloring, filtering, recrystallizing filtrate with isopropanol and absolute ethyl alcohol respectively, and drying to obtain white calcium gluconate. The invention uses the kitchen waste such as egg shells, crab shells and the like as raw materials, and the superfine calcium carbonate powder is prepared by the pretreatment such as crushing, screening, acid leaching, alkali precipitation and the like, and then the superfine calcium carbonate powder reacts with gluconic acid-lactone to obtain the calcium gluconate with high yield and high purity, the production cost is low, and the requirements of industrial mass production are met.
Description
Technical Field
The invention relates to the field of preparation of calcium gluconate, and particularly relates to a preparation method of calcium gluconate.
Background
Calcium gluconate (Calcium gluconate) is Calcium salt of gluconic acid and has a molecular formula of Ca (C)6H11O7)2·H2O is white crystalline or granular powder, has melting point of 201 deg.C, is odorless and tasteless, and is soluble in cold water and hot water. It is important to haveThe organic calcium is mainly used as a calcium enhancer, a nutrient, a buffering agent, a curing agent and a chelating agent of food, and has wide application prospect.
At present, the production methods of calcium gluconate mainly comprise an electrolytic oxidation method, a chemical oxidation method, a metal catalytic synthesis method, a fermentation method, an enzyme catalysis method and the like. At present, most of domestic manufacturers adopt a fermentation method, but still have the problems of culture and separation of the melanomyces, difficult control of byproducts and the like; the electrolytic oxidation method has the defects of large equipment investment, high cost, large energy consumption, long period and the like; the metal catalytic synthesis is a novel chemical synthesis method at present, but the catalytic oxidation method needs expensive noble metal reagents, and the cost is not easy to control.
Chinese patent application CN101434532A discloses a method for preparing high-purity calcium gluconate by using oyster shell. Oyster is an important marine economic shellfish in China, and oyster shells contain more than 90% of natural calcium carbonate and are good natural calcium sources. However, oysters have strong accumulation capacity on heavy metals, and in recent years, due to marine pollution, the exceeding of lead in a biological calcium product obtained by roasting oyster shells is a common problem.
In addition to shellfish, egg shells, crab shells, etc. contain a large amount of calcium carbonate, and can also be used for preparing biological calcium. However, the existing treatment modes are direct drying, crushing and screening, the contained impurities are more, the subsequent influence on the production of calcium gluconate is larger, and a high-purity product cannot be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of calcium gluconate, which can be used for preparing a high-purity calcium gluconate product.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, cleaning, adding the raw materials into a sodium hydroxide solution with the mass fraction of 2-10%, soaking for 15-20 min at the temperature of 95-100 ℃, taking out, washing with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing the waste shells by using a crusher, and sieving the crushed powder to obtain mixed shell powder;
(3) putting 2-5 mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon after the reaction is finished, decoloring, and filtering to obtain calcium ion-containing solution;
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 1-2 mol/L bicarbonate solution for precipitation treatment; after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.0-2.6 mol/L gluconic acid-lactone solution with distilled water, heating to 60-70 ℃ in water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution while stirring under the water bath heating condition of 60-70 ℃, and stirring for 2-5 hours while keeping the temperature;
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) to the filtrate was added isopropanol, isopropanol: standing the filtrate for 5-8 hours for crystallization and centrifuging to obtain a calcium gluconate crude crystal, adding the crude crystal into absolute ethyl alcohol, wherein the volume ratio of the filtrate is 0.5-1.5: 1, and the absolute ethyl alcohol: and (3) standing the crude crystals for 3-5 hours for crystallization, centrifuging, washing calcium gluconate crystals by using absolute ethyl alcohol, and drying in vacuum to obtain the white calcium gluconate.
Preferably, in the step (1), the mass ratio of the egg shells to the crab shells is 4-6: 5 to 10.
Preferably, in the step (2), the number of the sieved screens is 300-350 meshes.
Preferably, in step (4), the bicarbonate is selected from ammonium bicarbonate or sodium bicarbonate.
Preferably, in the step (6), the solid-to-liquid ratio of the calcium carbonate powder to the distilled water is 1: 8-12, and the molar ratio of the glucono-lactone to the calcium carbonate is 2.05-2.1: 1.
Preferably, in the step (8), the temperature of the vacuum drying is 45-60 ℃; the water content of the dried calcium gluconate is less than or equal to 0.5 percent.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, kitchen waste such as egg shells and crab shells is used as raw materials, so that the production cost is saved, solid waste is treated, the utilization rate of resources is improved, and the risk that heavy metals of calcium gluconate products exceed the standard is reduced;
2. according to the invention, the egg shell and the crab shell are pretreated to prepare the superfine calcium carbonate powder with higher purity, and then the superfine calcium carbonate powder reacts with the gluconic acid-lactone, so that the reaction yield and the product purity are improved;
3. the method adopts fractional recrystallization to obtain the calcium gluconate with high yield (up to 91.2%) and high purity (up to 99.8%), and meets the requirement of industrial mass production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments.
Example 1
A preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, mixing and cleaning the raw materials according to the mass ratio of 5: 8, adding the raw materials into a sodium hydroxide solution with the mass fraction of 5%, soaking the raw materials for 18min at the temperature of 100 ℃, taking the raw materials out, washing the raw materials with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing by using a crusher, and sieving the crushed powder with a sieve of 325 meshes to obtain mixed shell powder;
(3) putting 3mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon to decolor after the reaction is finished, and filtering to obtain calcium ion-containing solution; the reaction equation is:
CaCO3+2HCl→CaCl2+H2O+CO2↑；
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 1.5mol/L sodium bicarbonate solution for precipitation treatment; the reaction equation is:
2NaHCO3+CaCl2→CaCO3↓+2NaCl+H2O+CO2↑；
after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.5mol/L gluconic acid-lactone solution by using distilled water, and heating the solution to 65 ℃ in a water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water according to the solid-to-liquid ratio of 1: 10g/L to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under stirring under the water bath heating condition of 65 ℃, and keeping the temperature and stirring for 3 hours; wherein the molar ratio of the glucono-lactone to the calcium carbonate is 2.05: 1, and the reaction equation is as follows:
2HOCH2(C4H8O4)COOH+CaCO3→
Ca[OOC(C4H8O4)CH2OH]2·H2O+CO2↑
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) to the filtrate was added isopropanol, isopropanol: and (3) standing the filtrate for 6 hours to crystallize and centrifugate to obtain a calcium gluconate crude crystal, adding the crude crystal into absolute ethyl alcohol, wherein the volume ratio of the filtrate is 1: 1, and the absolute ethyl alcohol: standing the coarse crystals at a mass ratio of 1: 1 for 4 hours for crystallization, centrifuging, washing the calcium gluconate crystals with absolute ethyl alcohol, drying at 50 ℃ in vacuum, and drying until the water content of the calcium gluconate is less than or equal to 0.5% to obtain the white calcium gluconate.
Example 2
A preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, mixing and cleaning the raw materials according to the mass ratio of 4: 5, adding the raw materials into a sodium hydroxide solution with the mass fraction of 2%, soaking the raw materials for 20min at the temperature of 100 ℃, taking the raw materials out, washing the raw materials with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing by using a crusher, and sieving the crushed powder with a sieve of 300 meshes to obtain mixed shell powder;
(3) putting 2mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon to decolor after the reaction is finished, and filtering to obtain calcium ion-containing solution; the reaction equation is:
CaCO3+2HCl→CaCl2+H2O+CO2↑；
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 1mol/L sodium bicarbonate solution for precipitation treatment; the reaction equation is:
2NaHCO3+CaCl2→CaCO3↓+2NaCl+H2O+CO2↑；
after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.0mol/L gluconic acid-lactone solution by using distilled water, and heating the solution to 60 ℃ in a water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water according to the solid-to-liquid ratio of 1: 8g/L to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under stirring under the water bath heating condition at 60 ℃, and keeping the temperature and stirring for 2 hours; wherein the molar ratio of the glucono-lactone to the calcium carbonate is 2.1: 1, and the reaction equation is as follows:
2HOCH2(C4H8O4)COOH+CaCO3→
Ca[OOC(C4H8O4)CH2OH]2·H2O+CO2↑
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) to the filtrate was added isopropanol, isopropanol: and (3) standing the filtrate for 8 hours for crystallization and centrifugation according to the volume ratio of 0.5: 1 to obtain a calcium gluconate crude crystal, and adding the crude crystal into absolute ethyl alcohol: standing the crude crystal at a mass ratio of 1.5: 1 for 3 hours for crystallization, centrifuging, washing the calcium gluconate crystal with absolute ethyl alcohol, drying at 45 ℃ in vacuum, and drying to obtain white calcium gluconate with the water content of less than or equal to 0.5%.
Example 3
A preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, mixing and cleaning the raw materials according to the mass ratio of 3: 5, adding the raw materials into a sodium hydroxide solution with the mass fraction of 10%, soaking the raw materials for 15min at the temperature of 95 ℃, taking the raw materials out, washing the raw materials with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing by using a crusher, and sieving the crushed powder with a sieve of 350 meshes to obtain mixed shell powder;
(3) adding 5mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon to decolor after the reaction is finished, and filtering to obtain calcium ion-containing solution; the reaction equation is:
CaCO3+2HCl→CaCl2+H2O+CO2↑；
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 2mol/L ammonium bicarbonate solution for precipitation treatment; the reaction equation is:
2NH4HCO3+CaCl2→CaCO3↓+2NH4Cl+H2O+CO2↑；
after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.6mol/L gluconic acid-lactone solution by using distilled water, and heating the solution to 70 ℃ in a water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water according to the solid-to-liquid ratio of 1: 10g/L to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under stirring under the water bath heating condition at 70 ℃, and keeping the temperature and stirring for 5 hours; wherein the molar ratio of the glucono-lactone to the calcium carbonate is 2.05: 1, and the reaction equation is as follows:
2HOCH2(C4H8O4)COOH+CaCO3→
Ca[OOC(C4H8O4)CH2OH]2·H2O+CO2↑
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) adding isopropanol into the filtrate, wherein the volume ratio of the isopropanol to the filtrate is 1.5: 1, standing for 5 hours for crystallization, centrifuging to obtain calcium gluconate crude crystals, adding the crude crystals into absolute ethyl alcohol, wherein the absolute ethyl alcohol: standing the crude crystal at a mass ratio of 0.5: 1 for 5 hours for crystallization, centrifuging, washing the calcium gluconate crystal with absolute ethyl alcohol, drying at 60 ℃ in vacuum, and drying until the water content of the calcium gluconate is less than or equal to 0.5% to obtain the white calcium gluconate.
Comparative example 1
A preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, mixing and cleaning the raw materials according to the mass ratio of 5: 8, adding the raw materials into a sodium hydroxide solution with the mass fraction of 5%, soaking the raw materials for 18min at the temperature of 100 ℃, taking the raw materials out, washing the raw materials with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing by using a crusher, and sieving the crushed powder with a sieve of 325 meshes to obtain mixed shell powder;
(3) putting 3mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon to decolor after the reaction is finished, and filtering to obtain calcium ion-containing solution; the reaction equation is:
CaCO3+2HCl→CaCl2+H2O+CO2↑；
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 1.5mol/L sodium bicarbonate solution for precipitation treatment; the reaction equation is:
2NaHCO3+CaCl2→CaCO3↓+2NaCl+H2O+CO2↑；
after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.5mol/L gluconic acid-lactone solution by using distilled water, and heating the solution to 65 ℃ in a water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water according to the solid-to-liquid ratio of 1: 10g/L to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under stirring under the water bath heating condition of 65 ℃, and keeping the temperature and stirring for 3 hours; wherein the molar ratio of the glucono-lactone to the calcium carbonate is 2.05: 1, and the reaction equation is as follows:
2HOCH2(C4H8O4)COOH+CaCO3→
Ca[OOC(C4H8O4)CH2OH]2·H2O+CO2↑
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) adding absolute ethyl alcohol into the filtrate, wherein the absolute ethyl alcohol: standing the filtrate for 12 hours to crystallize and centrifugate to obtain calcium gluconate crystals, drying the calcium gluconate crystals at 50 ℃ in vacuum, and drying the calcium gluconate crystals until the water content is less than or equal to 0.5 percent to obtain the white calcium gluconate.
Comparative example 2
A preparation method of calcium gluconate comprises the following steps:
(1) selecting waste egg shells and crab shells as raw materials, mixing and cleaning the raw materials according to the mass ratio of 5: 8, adding the raw materials into a sodium hydroxide solution with the mass fraction of 5%, soaking the raw materials for 18min at the temperature of 100 ℃, taking the raw materials out, washing the raw materials with water, and removing shell membranes and cuticles;
(2) drying the pretreated waste shells, then crushing by using a crusher, and sieving the crushed powder with a sieve of 325 meshes to obtain mixed shell powder;
(3) preparing 2.5mol/L gluconic acid-lactone solution by using distilled water, and heating the solution to 65 ℃ in a water bath to completely dissolve the gluconic acid-lactone solution;
(4) placing the mixed shell powder into a reaction bottle, adding distilled water according to the solid-to-liquid ratio of 1: 10g/L to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution under stirring under the water bath heating condition of 65 ℃, and keeping the temperature and stirring for 3 hours; wherein the mass ratio of the gluconic acid-lactone to the mixed shell powder is 3: 1, and the reaction equation is as follows:
2HOCH2(C4H8O4)COOH+CaCO3→
Ca[OOC(C4H8O4)CH2OH]2·H2O+CO2↑
(5) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(6) to the filtrate was added isopropanol, isopropanol: and (3) standing the filtrate for 6 hours to crystallize and centrifugate to obtain a calcium gluconate crude crystal, adding the crude crystal into absolute ethyl alcohol, wherein the volume ratio of the filtrate is 1: 1, and the absolute ethyl alcohol: standing the coarse crystals at a mass ratio of 1: 1 for 4 hours for crystallization, centrifuging, washing the calcium gluconate crystals with absolute ethyl alcohol, drying at 50 ℃ in vacuum, and drying until the water content of the calcium gluconate is less than or equal to 0.5% to obtain the white calcium gluconate.
The product quality of the calcium gluconate of the above examples and comparative examples is shown in table 1:
TABLE 1 product quality of the examples
| Purity of calcium gluconate/%) | Product yield/% | |
| Example 1 | 99.8 | 91.2 |
| Example 2 | 99.4 | 89.3 |
| Example 3 | 99.3 | 88.6 |
| Comparative example 1 | 99.0 | 83.7 |
| Comparative example 2 | 89.2 | 82.1 |
As can be seen from the above table, comparing comparative example 1 and example 1, the one-step crystallization using absolute ethanol with the fractional recrystallization using isopropanol and absolute ethanol, although the purities were all more than 99.0%, the yield was significantly reduced; comparing with comparative example 2 and example 1, the superfine calcium carbonate is prepared by acid leaching and alkali precipitation, and the purity and yield are obviously improved compared with the reaction of directly adding mixed shell powder and gluconic acid-lactone. In conclusion, the calcium gluconate product with high yield and high yield can be obtained by adopting the reaction of the superfine calcium carbonate and the gluconic acid-lactone and combining the fractional recrystallization.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (6)
1. A preparation method of calcium gluconate is characterized by comprising the following steps:
(1) selecting waste egg shells and crab shells as raw materials, cleaning, adding the raw materials into a sodium hydroxide solution with the mass fraction of 2-10%, soaking for 15-20 min at the temperature of 95-100 ℃, taking out, washing with water, and removing shell membranes and cuticles.
(2) Drying the pretreated waste shells, then crushing the waste shells by using a crusher, and sieving the crushed powder to obtain mixed shell powder;
(3) putting 2-5 mol/L hydrochloric acid solution into an acid-resistant cylinder, adding mixed shell powder while stirring to react, adding activated carbon after the reaction is finished, decoloring, and filtering to obtain calcium ion-containing solution;
(4) adjusting the pH value of the calcium ion-containing solution to 7-8, and then adding 1-2 mol/L bicarbonate solution for precipitation treatment; after the precipitation is completed, carrying out suction filtration, washing a filter cake until no chloride ion exists basically, and drying to obtain calcium carbonate powder;
(5) preparing 2.0-2.6 mol/L gluconic acid-lactone solution with distilled water, heating to 60-70 ℃ in water bath to completely dissolve the gluconic acid-lactone solution;
(6) placing calcium carbonate powder into a reaction bottle, adding distilled water to prepare uniformly dispersed suspension, adding a gluconic acid-lactone solution while stirring under the water bath heating condition of 60-70 ℃, and stirring for 2-5 hours while keeping the temperature;
(7) after the reaction is finished, carrying out suction filtration, removing filter residues, adding active carbon into filtrate for decolorization, and filtering again;
(8) adding isopropanol into the filtrate, wherein the volume ratio of the isopropanol to the filtrate is 0.5-1.5: 1, standing for 5-8 hours for crystallization, centrifuging to obtain a calcium gluconate crude crystal, adding the crude crystal into absolute ethyl alcohol, wherein the mass ratio of the absolute ethyl alcohol to the crude crystal is 0.5-1.5: 1, standing for 3-5 hours for crystallization, centrifuging, washing the calcium gluconate crystal with the absolute ethyl alcohol, and vacuum drying to obtain the white calcium gluconate.
2. The preparation method of calcium gluconate according to claim 1, wherein in the step (1), the mass ratio of the egg shell to the crab shell is 4-6: 5-10.
3. The method for preparing calcium gluconate according to claim 1, wherein in the step (2), the sieved mesh number is 300-350 meshes.
4. The method as claimed in claim 1, wherein in step (4), the bicarbonate is selected from ammonium bicarbonate or sodium bicarbonate.
5. The method for preparing calcium gluconate according to claim 1, wherein in the step (6), the solid-to-liquid ratio of the calcium carbonate powder to the distilled water is 1: 8-12, and the molar ratio of glucono-lactone to calcium carbonate is 2.05-2.1: 1.
6. The method for preparing calcium gluconate according to claim 1, wherein in the step (8), the temperature of vacuum drying is 45-60 ℃; the water content of the dried calcium gluconate is less than or equal to 0.5 percent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552167A (en) * | 2020-12-31 | 2021-03-26 | 常州兰陵制药有限公司 | Preparation method of calcium gluconate |
| CN113045409A (en) * | 2021-03-25 | 2021-06-29 | 山东新华制药股份有限公司 | Crystallization method of calcium gluconate for injection |
| CN115215363A (en) * | 2022-05-25 | 2022-10-21 | 华中农业大学 | Method for efficiently preparing eggshell source fine calcium carbonate and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552167A (en) * | 2020-12-31 | 2021-03-26 | 常州兰陵制药有限公司 | Preparation method of calcium gluconate |
| CN112552167B (en) * | 2020-12-31 | 2024-03-22 | 常州兰陵制药有限公司 | Preparation method of calcium gluconate |
| CN113045409A (en) * | 2021-03-25 | 2021-06-29 | 山东新华制药股份有限公司 | Crystallization method of calcium gluconate for injection |
| CN115215363A (en) * | 2022-05-25 | 2022-10-21 | 华中农业大学 | Method for efficiently preparing eggshell source fine calcium carbonate and application thereof |
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