A green production process of magnesium glycinate

Abstract

The application discloses a green production process of magnesium glycinate, which comprises the following steps: adding pure water into a reaction kettle, heating and adding glycine to dissolve, adding magnesium oxide after the dissolution, carrying out the reaction at 95 DEG C, keeping the temperature for 15 min, filtering out the unreacted magnesium oxide to re-input the reaction kettle, cooling and crystallizing the filtered mother liquor, centrifugally separating to obtain wet products and the mother liquor, recycling the mother liquor to re-input the reaction kettle, and drying, sieving and packaging the magnesium glycinate wet products to obtain finished products. The production process of the application has high purity of the prepared magnesium glycinate, does not need additional organic solvents, is energy-saving and environment-friendly, and realizes continuous industrial green production.

Description

Technical Field

[0001] This invention relates to the field of glycine magnesium production technology, and in particular to a green production process for glycine magnesium. Background Technology

[0002] Magnesium glycinate is a compound formed by the chelation of magnesium ions and the amino acid glycine. Its unique structure gives it several advantages over other forms of magnesium supplements. With its high absorption rate, neuromodulation, and muscle recovery benefits, magnesium glycinate is an ideal choice for preventing magnesium deficiency and improving related symptoms.

[0003] Currently, glycine magnesium is obtained by a one-step reaction of glycine and magnesium compounds. Patent document CN106478438A uses the reaction of glycine and magnesium compounds to prepare glycine magnesium with a yield of 85-97.5%. When the magnesium compound is magnesium hydroxide, the yield is 91.8-97.5%, which has a large range and the process is unstable. At the same time, the process uses alcohol precipitation, and the subsequent alcohol precipitation liquid needs to be further distilled, which is energy-intensive and costly.

[0004] Patent document CN113321592B discloses a method for preparing glycine magnesium. The method involves pretreating glycine and magnesium hydroxide or magnesium oxide, adding the glycine to a solid-phase reactor, and then adding magnesium compounds in batches. After the reaction is completed, the product is washed with ethanol and dried to obtain glycine magnesium with a yield of 94-98.8%. The pretreatment process uses a grinder for pulverization and sieving, which causes serious dust pollution. Alcohol precipitation is also used for separation, which results in high energy consumption in subsequent processing.

[0005] Patent document CN109608349B discloses a green preparation method for glycine magnesium. By optimizing the molar ratio of glycine to magnesium hydroxide raw materials through experiments, a high yield and high purity of glycine magnesium can be achieved. However, the preparation process is a small-scale production carried out in the laboratory. After scale-up experiments, the data deviates significantly and is not suitable for large-scale factory production.

[0006] How to achieve high-purity, high-yield, large-scale, and green production of magnesium glycinate is a key research focus for enterprises. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of the prior art and provide a green production process for magnesium glycinate to solve the problems of high energy consumption, pollution and low purity in the industrial production of magnesium glycinate in the prior art.

[0008] The objective of this invention is achieved through the following technical solution: a green production process for magnesium glycine, comprising the following steps, S1. Add purified water to the reaction vessel, heat it, and add glycine to dissolve it; S2. After dissolving, add magnesium oxide and react at 95℃ for 15 minutes. S3. After the reaction is complete, filter out the unreacted magnesium oxide and put it back into the reactor. Cool the filtered mother liquor to crystallize, and centrifuge to separate the wet product and the mother liquor. S4. The entire mother liquor is recycled back into the reactor. The wet glycine magnesium product is dried, sieved, and packaged to obtain the finished product.

[0009] Preferably, the process also includes step S5, where the centrifuged mother liquor is recycled to a specified number of times, then concentrated and crystallized, the wet product is separated by centrifugation and put back into the reaction vessel, and the concentrated mother liquor is treated as wastewater.

[0010] Preferably, the centrifuged mother liquor is recycled 15 times.

[0011] Preferably, the unqualified products after sieving are put into the centrifugal mother liquor for concentration and crystallization.

[0012] Preferably, the molar ratio of glycine to magnesium oxide in the reaction system is 2.5:1, and the mass ratio of glycine to purified water is 1:2.

[0013] Preferably, the concentration vacuum degree is -0.05 MPa and the concentration temperature is 70°C.

[0014] Preferably, the wet glycine magnesium product is dried at 75°C for 4 hours.

[0015] The present invention has the following advantages: 1. This invention uses a cooling crystallization method to achieve the industrial production of glycine magnesium chelate. Compared with the alcohol precipitation method, it does not introduce organic solvents and does not require energy-consuming processes such as heating distillation, making it more energy-efficient and environmentally friendly. 2. The production process of this invention optimizes the reaction temperature, precisely controls the molar ratio of the reaction raw materials, shortens the reaction time, overcomes the technical bias that the longer the reaction time, the higher the purity, and circulates the mother liquor multiple times to ensure continuous large-scale production capacity. In addition, the mother liquor is concentrated and then processed after multiple cycles, which reduces the impurity content introduced into the reaction system during the mother liquor circulation process, achieving a high purity of 99.9% for magnesium glycine, ensuring the purity of industrial production, and avoiding the impact of high impurity content and fluctuations in impurity content at the raw material end on the purity of the product. 3. The product synthesized industrially by this invention is glycine magnesium dihydrate, which meets the stringent requirements for food grade. Attached Figure Description

[0016] Figure 1 This is a simplified process flow diagram of the present invention. Detailed Implementation

[0017] The present invention will be further described in detail below with reference to the embodiments.

[0018] The reaction equation for the synthesis of magnesium glycine from magnesium oxide is as follows: 2NH2CH2COOH+MgO→Mg(NH2CH2COOH)2 A green production process for magnesium glycine, such as Figure 1 As shown, it includes the following steps: S1. Add purified water to the reaction vessel, heat it, and add glycine to dissolve it; S2. After dissolving, add magnesium oxide and react at 95℃ for 15 min. The initial molar ratio of glycine to magnesium oxide in the reaction system is 2.5:1, and the mass ratio of glycine to purified water is 1:2. S3. After the reaction is complete, filter out the unreacted magnesium oxide and put it back into the reactor. Cool the filtered mother liquor to crystallize, and centrifuge to separate the wet product and the mother liquor. S4. The mother liquor is completely recycled back into the reactor. The wet glycine magnesium product is dried at 70°C for 4 hours, sieved, and packaged to obtain the finished product. S5. After the mother liquor is recycled 15 times, it is concentrated. The concentration vacuum is -0.05 MPa and the concentration temperature is 75°C. The wet product is separated by centrifugation and put back into the reaction vessel. The concentrated mother liquor is then treated as wastewater. Example 1

[0019] Four tons of purified water were added to the reactor, and two tons of 99% pure glycine were added and dissolved. After dissolution, 0.5 tons of 96% pure magnesium oxide were added, and the reaction was carried out at 95℃ for 15 minutes. After the reaction was completed, the unreacted magnesium oxide was filtered out and returned to the reactor. The filtered mother liquor was cooled to 15℃ to crystallize, and centrifuged to obtain a wet product and a separation mother liquor. All the separation mother liquor was recycled back to the reactor. The glycine magnesium wet product was dried at 70℃ for 4 hours, sieved, and packaged to obtain the finished product. During this period, the centrifuged mother liquor was recycled up to 15 times and then concentrated. The concentration vacuum was -0.05 MPa and the concentration temperature was 75℃. The wet product was centrifuged out and returned to the reactor, and the concentrated mother liquor was treated as wastewater.

[0020] The sample was commissioned to Zhengzhou Guozhun Testing Technology Co., Ltd. for testing. The glycine magnesium produced had a purity of 99.9%, a magnesium content of 11.6%, and a nitrogen content of 13.9%, which is far superior to the standard.

[0021] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A green production process for magnesium glycinate, characterized in that: Includes the following steps, S1. Add purified water to the reaction vessel, heat it, and add glycine to dissolve it; S2. After dissolving, add magnesium oxide and react at 95℃ for 15 minutes. S3. After the reaction is complete, filter out the unreacted magnesium oxide and put it back into the reactor. Cool the filtered mother liquor to crystallize, and centrifuge to separate the wet product and the mother liquor. S4. The entire mother liquor is recycled back into the reactor. The wet glycine magnesium product is dried, sieved, and packaged to obtain the finished product.

2. The green production process for magnesium glycinate according to claim 1, characterized in that: It also includes step S5, in which the centrifuged mother liquor is circulated and concentrated after a specified number of cycles, the wet product is separated by centrifugation and put back into the reaction vessel, and the mother liquor is treated as wastewater.

3. The green production process for magnesium glycinate according to claim 2, characterized in that: The mother liquor from the crystallization centrifugation was recycled 15 times.

4. The green production process for magnesium glycinate according to claim 1, characterized in that: The sieved defective products are put into the centrifugal mother liquor for reaction and crystallization.

5. The green production process for magnesium glycinate according to claim 1, characterized in that: The molar ratio of glycine to magnesium oxide in the reaction system is 2.5:1, and the mass ratio of glycine to purified water is 1:

2.

6. The green production process for magnesium glycinate according to claim 2, characterized in that: The concentration vacuum degree is -0.05 MPa, and the concentration temperature is 70°C.

7. The green production process for magnesium glycinate according to claim 1, characterized in that: The wet glycine zinc product was dried at 75°C for 4 hours.

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