CN110894199A - Preparation method of ammonium magnesium citrate - Google Patents
Preparation method of ammonium magnesium citrate Download PDFInfo
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- CN110894199A CN110894199A CN201911268416.0A CN201911268416A CN110894199A CN 110894199 A CN110894199 A CN 110894199A CN 201911268416 A CN201911268416 A CN 201911268416A CN 110894199 A CN110894199 A CN 110894199A
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- magnesium
- citric acid
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- ammonium
- ammonia water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/02—Magnesium compounds
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application discloses a preparation method of ammonium magnesium citrate, which comprises the following steps: adding a raw material containing magnesium carbonate or magnesium oxide into a citric acid solution, stirring for 0.5-1 hour for primary chelation until the solution is clear, adding ammonia water into the obtained reaction solution for the first time, and stirring for 0.5-1 hour for secondary chelation to obtain a chelated reaction solution; heating and concentrating the chelation reaction solution to 1/2 of the volume of the chelation reaction solution, cooling, and adding ammonia water until the pH value of the solution is 8-10 to obtain a solution containing ammonium magnesium citrate; the mass ratio of the citric acid to the raw materials is as follows: 1.5-5.5: 1; the volume ratio of the primarily added ammonia water to the supplemented ammonia water is 10-15: 1; the mass ratio of the total amount of the added ammonia water to the citric acid is as follows: 1.5-2: 1. The method solves the problem that magnesium citrate is insoluble in water, has simple preparation process and low cost, and widens the application range of magnesium as a medium element in medicine, food, feed, industry and agriculture.
Description
Technical Field
The application relates to a preparation method of ammonium magnesium citrate, belonging to the field of inorganic non-metallic materials.
Background
Magnesium citrate is insoluble in water, limiting the use of magnesium citrate.
At present, no preparation process of ammonium magnesium citrate exists in the market, no mature ammonium magnesium citrate product is sold, and the production and the sale of the ammonium magnesium citrate are in blank stages.
Disclosure of Invention
The present application provides a method for preparing ammonium magnesium citrate for solving the above technical problems.
The application provides a preparation method of ammonium magnesium citrate, which comprises the following steps:
adding the raw materials into a citric acid solution, stirring for 0.5-1 hour for primary chelation until the solution is clear, adding ammonia water into the obtained reaction solution for the first time, and stirring for 0.5-1 hour for secondary chelation to obtain a chelation reaction solution;
heating and concentrating the chelation reaction liquid to 1/2 of the volume of the chelation reaction liquid, cooling, and supplementing ammonia water until the pH value of the solution is 8-10 to obtain a solution containing the ammonium magnesium citrate;
the mass ratio of the citric acid to the raw materials is as follows: 2.5-5.5: 1, the raw material is magnesium carbonate or magnesium oxide;
the volume ratio of the primarily added ammonia water to the supplemented ammonia water is 10-15: 1;
the mass ratio of the total amount of the added ammonia water to the citric acid is as follows: 1.5-2: 1.
Preferably, the raw material is magnesium carbonate, and the mass ratio of the citric acid to the magnesium carbonate is as follows: 1.5-3: 1.
preferably, the raw material is magnesium oxide, and the mass ratio of the citric acid to the magnesium oxide is as follows: 2-5.5: 1.
preferably, the method further comprises the step of drying or spray drying the solution containing the magnesium ammonium citrate.
Preferably, the drying temperature is 130-150 ℃.
Preferably, the temperature of the spray drying is 200-240 ℃.
Preferably, the citric acid is citric acid monohydrate with a purity of 98%.
Preferably, the magnesium carbonate is magnesium carbonate powder with the purity of 98 percent; the magnesium oxide is magnesium oxide powder with the purity of 98 percent.
The method provided by the application comprises the following steps:
1. citric acid monohydrate (C) was added to 600ml of water6H10O8Purity 98%), stirring and dissolving to obtain citric acid solution.
2. Mixing magnesium carbonate (MgCO)3Purity 98%) was added to citric acid solution and stirred at room temperature for 45 minutes for primary chelation until the solution was clear. The mass ratio of the citric acid to the raw materials is as follows: 2.5-5.5: 1, the raw material is magnesium carbonate or magnesium oxide.
3. And (3) adding ammonia water into the solution obtained in the step (2) for the first time, and stirring at room temperature for secondary chelation for 0.5 hour.
4. Heating the reaction solution to 90-100 ℃ to concentrate the reaction solution to 1/2 of the volume of the reaction solution, stopping heating, air-cooling the reaction solution to room temperature, adding ammonia water, adjusting the pH to 8, and drying the obtained solution at 130 ℃ to obtain the magnesium ammonium citrate sample.
The beneficial effects that this application can produce include:
1) the preparation method of the magnesium ammonium citrate solves the problem that magnesium citrate is insoluble in water, has simple preparation process and lower cost, and widens the application range of the medium element magnesium in medicine, food, feed, industry and agriculture.
2) According to the preparation method of the ammonium magnesium citrate provided by the application, the ammonium magnesium citrate is a citric acid chelating salt, is pure white, slightly has ammonia smell, is dissolved in water, and is alkalescent in aqueous solution. The magnesium ammonium citrate can make up the defect that the magnesium citrate finished product is not dissolved in water, and can play various properties of the magnesium citrate after being dissolved, thereby having wide application range.
3) According to the preparation method of the ammonium magnesium citrate, magnesium carbonate or magnesium oxide is used as a raw material and reacts with citric acid to generate a magnesium citrate clear solution, and ammonia water is added to prepare the ammonium magnesium citrate which is a new substance, so that the blank of the substance in the market is made up, and a foundation is laid for mass production, market sale and popularization of the ammonium magnesium citrate.
4) According to the preparation method of the magnesium ammonium citrate, the magnesium ammonium citrate is a complex salt composed of magnesium, ammonia and citric acid, the complexing is carried out by providing lone pair electrons by nitrogen atoms in the ammonia and complexing with metal ions with empty orbits, and in the preparation process of a product, a secondary chelating technology is adopted, primary chelating is carried out on magnesium and citric acid, and ammonia water is added for secondary chelating, so that the medium-strength chelate salt is prepared.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Examples
The materials used in the following examples were all obtained commercially, unless otherwise specified.
Examples 1 to 3: preparation of ammonium magnesium citrate samples 1-3
The method comprises the following steps:
1. citric acid monohydrate (C) was added to 600ml of water6H10O8Purity 98%), stirring and dissolving to obtain citric acid solution.
2. Mixing magnesium carbonate (MgCO)3Purity 98%) was added to citric acid solution and stirred at room temperature for 45 minutes for primary chelation until the solution was clear.
3. And (3) adding ammonia water into the solution obtained in the step (2) for the first time, and stirring at room temperature for secondary chelation for 0.5 hour.
4. Heating the reaction solution to 90-100 ℃ to concentrate the reaction solution to 1/2 of the volume of the reaction solution, stopping heating, air-cooling the reaction solution to room temperature, adding ammonia water, adjusting the pH to 8, and drying the obtained solution at 130 ℃ to obtain the magnesium ammonium citrate sample.
The preparation method parameters of the magnesium ammonium citrate samples 1-3 are shown in the table 1.
TABLE 1
Examples 4 to 6: preparation of ammonium magnesium citrate samples 4-6
The differences between the preparation methods of the magnesium ammonium citrate samples 4-6 and the preparation method of the magnesium ammonium citrate sample 2 are shown in the table 2.
TABLE 2
Example 7 product detection
The products obtained in examples 1-5 were tested for appearance, magnesium content, nitrogen content and pH according to the prior art, typical results are listed in the following table, and the products obtained in other examples are the same.
TABLE 2
As can be seen from table 2, the method provided by the present application can produce magnesium ammonium citrate, which can be dissolved in water to form a solution, and effectively solves the problem that magnesium citrate is insoluble in water.
Reference throughout this specification to "one embodiment," "another embodiment," "an embodiment," "a preferred embodiment," or the like, means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described generally in this application. The appearances of the same phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the scope of the disclosure to effect such feature, structure, or characteristic in connection with other embodiments.
Although the present application has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the claims disclosed herein. In addition to variations and modifications in the component parts and/or arrangements, other uses will also be apparent to those skilled in the art.
Claims (8)
1. The preparation method of the ammonium magnesium citrate is characterized by comprising the following steps:
adding the raw materials into a citric acid solution, stirring for 0.5-1 hour for primary chelation until the solution is clear, adding ammonia water into the obtained reaction solution for the first time, and stirring for 0.5-1 hour for secondary chelation to obtain a chelation reaction solution;
heating and concentrating the chelation reaction liquid to 1/2 of the volume of the chelation reaction liquid, cooling, and supplementing ammonia water until the pH value of the solution is 8-10 to obtain a solution containing the ammonium magnesium citrate;
the mass ratio of the citric acid to the raw materials is as follows: 1.5-5.5: 1, the raw material is magnesium carbonate or magnesium oxide;
the volume ratio of the primarily added ammonia water to the supplemented ammonia water is 10-15: 1;
the mass ratio of the total amount of the added ammonia water to the citric acid is as follows: 1.5-2: 1.
2. The method for preparing ammonium magnesium citrate according to claim 1, wherein the raw material is magnesium carbonate, and the mass ratio of the citric acid to the magnesium carbonate is as follows: 1.5-3: 1.
3. the method for preparing the ammonium magnesium citrate according to claim 1, wherein the raw material is magnesium oxide, and the mass ratio of the citric acid to the magnesium oxide is as follows: 2-5.5: 1.
4. the method of claim 1, further comprising the step of drying or spray drying the solution containing the magnesium ammonium citrate.
5. The method for preparing ammonium magnesium citrate according to claim 4, wherein the drying temperature is 130-150 ℃.
6. The method for preparing magnesium ammonium citrate according to claim 4, wherein the temperature of the spray drying is 200-240 ℃.
7. The method of claim 1, wherein the citric acid is citric acid monohydrate with a purity of 98%.
8. The method for producing magnesium ammonium citrate according to claim 1, wherein the magnesium carbonate is magnesium carbonate powder having a purity of 98%; the magnesium oxide is magnesium oxide powder with the purity of 98 percent.
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| CN201911268416.0A CN110894199A (en) | 2019-12-11 | 2019-12-11 | Preparation method of ammonium magnesium citrate |
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| CN201911268416.0A CN110894199A (en) | 2019-12-11 | 2019-12-11 | Preparation method of ammonium magnesium citrate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312782A (en) * | 1998-08-21 | 2001-09-12 | 格拉基阿诺·威格纳里 | Compositions based on water-soluble gold compounds suitable for coloring ceramic articles |
| CN104311317A (en) * | 2014-10-16 | 2015-01-28 | 郑州瑞普生物工程有限公司 | Preparation method of ammonia manganese citrate |
| CN104387143A (en) * | 2014-10-16 | 2015-03-04 | 郑州瑞普生物工程有限公司 | Copper ammonium citrate preparation method |
| CN104387142A (en) * | 2014-10-16 | 2015-03-04 | 郑州瑞普生物工程有限公司 | Zinc ammonium citrate preparation method |
-
2019
- 2019-12-11 CN CN201911268416.0A patent/CN110894199A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312782A (en) * | 1998-08-21 | 2001-09-12 | 格拉基阿诺·威格纳里 | Compositions based on water-soluble gold compounds suitable for coloring ceramic articles |
| CN104311317A (en) * | 2014-10-16 | 2015-01-28 | 郑州瑞普生物工程有限公司 | Preparation method of ammonia manganese citrate |
| CN104387143A (en) * | 2014-10-16 | 2015-03-04 | 郑州瑞普生物工程有限公司 | Copper ammonium citrate preparation method |
| CN104387142A (en) * | 2014-10-16 | 2015-03-04 | 郑州瑞普生物工程有限公司 | Zinc ammonium citrate preparation method |
Non-Patent Citations (1)
| Title |
|---|
| STN: "CAS RN 68213-76-3", 《REGISTRY》 * |
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