Preparation method of high-purity magnesium orotate

Abstract

The invention discloses a preparation method of high-purity magnesium orotate, which comprises the following steps: (1) sequentially adding orotic acid, sodium hydroxide and water into a reaction kettle, heating to reflux, reacting for 1-6 hours, and after the reaction is finished, filtering, cooling, crystallizing, centrifuging and drying the reaction liquid while the reaction liquid is hot to obtain sodium orotate; (2) preparing a magnesium solution; (2) mixing the sodium orotate solid prepared in the step (1) with water in proportion, then pumping the mixture into a reaction kettle for heating, filtering the magnesium solution, slowly dropwise adding the filtered magnesium solution into the reaction kettle in batches for reaction, and after the reaction is finished, cooling and centrifuging to obtain a solid A and a filtrate A; and (3) repeatedly washing the solid A prepared in the step (2) with water for multiple times, and drying to obtain the high-purity magnesium orotate. According to the preparation method, no organic solvent is used in the production process, the preparation method is suitable for industrial production, the process is simple, and the obtained magnesium orotate is high in purity.

Description

Technical Field

[0001] The invention belongs to the technical field of orotic acid series products, and particularly relates to a method for preparing high-purity magnesium orotate. Background Art

[0002] At present, there are few literature reports on the synthesis of magnesium orotate. Some literature reports that magnesium orotate is generated by reacting orotate with magnesium acetate in a molar ratio. This technology has the following disadvantages: (1) there are residual acetate ions in the magnesium orotate obtained after the reaction, and the product has an acetic acid taste; (2) the solution system obtained after the reaction is a mixture of orotate, magnesium acetate, and orotate magnesium acetate, and it is difficult to obtain high-purity magnesium orotate.

[0003] Therefore, it is necessary to develop a high-purity magnesium orotate preparation process suitable for industrialization. Summary of the invention

[0004] The inventors conducted experiments using orotic acid and magnesium metal oxides (magnesium oxide, magnesium hydroxide, magnesium carbonate) and found that no matter how the reaction conditions were controlled, the feed liquid would solidify in about 15 minutes of the reaction, causing the agitator to be unable to rotate, which was not conducive to industrialization.

[0005] In order to solve the above technical problems, the present invention provides a method for preparing high-purity magnesium orotate, which is easy to realize industrialization.

[0006] The present invention adopts the following technical scheme: a method for preparing high-purity magnesium orotate, which uses orotic acid as a raw material to first prepare sodium orotate, and then continues to react with a magnesium solution to obtain high-purity magnesium orotate. The present invention is suitable for industrial production, has a simple process and the obtained magnesium orotate has high purity.

[0007] The present invention provides a method for producing high-purity magnesium orotate, comprising the following steps:

[0008] Step (1) adding orotic acid, sodium hydroxide and water to a reaction kettle in sequence, heating to reflux, reacting for 1-6 hours, and after the reaction is completed, filtering the reaction solution while hot, cooling, crystallizing, centrifuging, and drying to obtain sodium orotate.

[0009] Step (2) mixing sodium orotate and water in proportion, then pumping into a reactor to heat up, filtering the magnesium solution and slowly dropping it into the reactor in batches to react, cooling after the reaction, centrifuging to obtain solid A and filtrate A;

[0010] Step (3), washing the solid prepared in step (2) repeatedly with water, and drying to obtain high-purity magnesium orotate.

[0011] In the above technical solution, preferably, the step (3) comprises:

[0012] Step (3.1) solid A is added with water in proportion, stirred for 30 min and then centrifuged to obtain solid B and filtrate B;

[0013] Step (3.2) adding water to the solid B in proportion, stirring for 30 minutes and then centrifuging to obtain a solid C and a filtrate C;

[0014] In step (3.3), the solid C is added with water in proportion, stirred for 30 minutes and then centrifuged to obtain a solid D and a filtrate D; and then the solid D is dried to obtain magnesium orotate with high purity.

[0015] Preferably, in step (2), the magnesium solution is any one of a magnesium chloride solution and a magnesium sulfate solution, and the concentration of the magnesium solution is prepared according to the following requirements: the mass ratio of magnesium chloride or magnesium sulfate to water is 50-80:100 and 40-55:100 respectively.

[0016] Preferably, in step (2), the dropping speed of the magnesium solution is controlled to be 3 ml-9 ml / min.

[0017] Preferably, in step (2), the reaction temperature of the magnesium orotate is 60-100° C. and the reaction time is 2-6 h.

[0018] Preferably, in step (3), the temperature of the washing water is 5-10°C, and the mass ratio of the washing water to the solid is 3-5:1.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] (1) The present invention uses orotic acid as a starting material, first prepares sodium orotate, and then converts it to obtain high-purity magnesium orotate without using any organic solvent;

[0021] (2) The process of the present invention does not cause the liquid to solidify during the reaction, which results in the agitator being unable to rotate, and is more suitable for industrialization;

[0022] (3) The present invention makes full use of the replacement reaction and the solubility characteristics of sodium orotate, sodium chloride, magnesium sulfate, magnesium chloride, magnesium orotate, and sodium hydroxide. Even if soluble salts are present in the product, the product is stirred and washed with ice water for multiple times, and almost no impurity ions are contained, and the purity is high. DETAILED DESCRIPTION

[0023] In order to better understand the content of the present invention, further description is given below in conjunction with specific embodiments. It should be understood that these embodiments are only used to further illustrate the present invention, and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content described in the present invention, those skilled in the art make some non-essential changes or adjustments to the present invention, which still belong to the protection scope of the present invention.

[0024] Example 1

[0025] (1) Anhydrous orotic acid (156 g, 1.0 mol), sodium hydroxide (40 g, 1.0 mol) and 280 ml of water were added to a reaction kettle in sequence, and the temperature was raised and refluxed for 1 h until the reaction was completed. The reaction solution was filtered while hot, cooled, crystallized, centrifuged, and dried to obtain 178 g of sodium orotic acid with a yield of 100%.

[0026] (2) Sodium orotate (178 g, 1.0 mol) and 350 ml of water were mixed, then pumped into a reactor and heated to 75° C. Magnesium chloride (47.6 g, 0.5 mol) was dissolved in 68 ml of water, filtered, and added dropwise to the reactor at a rate of 3 ml / min, and reacted for 4 h while stirring. After the reaction was completed, the temperature was lowered and centrifuged to obtain solid A and filtrate A;

[0027] (3) adding solid A to 5°C ice water in a ratio of 1:5, stirring for 30 min and centrifuging to obtain solid B and filtrate B;

[0028] (4) adding solid B to 5°C ice water in a ratio of 1:4, stirring for 30 min and centrifuging to obtain solid C and filtrate C;

[0029] (5) Solid C was added to ice water at 5°C in a ratio of 1:5, stirred for 30 min and then centrifuged to obtain solid D and filtrate D, and then solid D was dried to obtain 161.3 g of magnesium orotate, with a yield of 96.42%, a magnesium content of 7.172%, a total magnesium orotate content of 99.97%, and chloride <0.02%.

[0030] Example 2

[0031] (1) Anhydrous orotic acid (156 g, 1.0 mol), sodium hydroxide (40 g, 1.0 mol) and 280 ml of water were added to a reaction kettle in sequence, and the temperature was raised and refluxed for 1.5 h until the reaction was completed. The reaction solution was filtered while hot, cooled, crystallized, centrifuged, and dried to obtain 178 g of sodium orotic acid with a yield of 100%.

[0032] (2) Sodium orotate (178 g, 1.0 mol) and 350 ml of water were mixed, then pumped into a reactor and heated to 75° C. Magnesium chloride (47.6 g, 0.5 mol) was dissolved in 79 ml of water, filtered, and added dropwise to the reactor at a rate of 4 ml / min, and reacted for 4 h while stirring. After the reaction was completed, the temperature was lowered and centrifuged to obtain solid A and filtrate A;

[0033] (3) adding solid A to 7°C ice water in a ratio of 1:4, stirring for 30 min and centrifuging to obtain solid B and filtrate B;

[0034] (4) adding solid B to 7°C ice water in a ratio of 1:4, stirring for 30 min and centrifuging to obtain solid C and filtrate C;

[0035] (5) Solid C was added to ice water at 7° C. in a ratio of 1:5, stirred for 30 min and centrifuged to obtain solid D and filtrate D, and then solid D was dried to obtain 162.7 g of magnesium orotate with a yield of 97.28%, a magnesium content of 7.173%, a total content of 99.98%, and a chloride content of <0.02%.

[0036] Example 3

[0037] (1) Anhydrous orotic acid (156 g, 1.0 mol), sodium hydroxide (40 g, 1.0 mol) and 280 ml of water were added to a reaction kettle in sequence, and the temperature was raised and refluxed for 1 h until the reaction was completed. The reaction solution was filtered while hot, cooled, crystallized, centrifuged, and dried to obtain 178 g of sodium orotic acid with a yield of 100%.

[0038] (2) Sodium orotate (178 g, 1.0 mol) and 350 ml of water were mixed, then pumped into a reactor and heated to 75° C. Magnesium sulfate (60.1 g, 0.5 mol) was dissolved in 90 ml of water, filtered, and added dropwise to the reactor at a rate of 3 ml / min. The mixture was stirred and reacted for 4 h. After the reaction was completed, the temperature was lowered and centrifuged to obtain solid A and filtrate A;

[0039] (3) adding solid A to 5°C ice water in a ratio of 1:3, stirring for 30 min and centrifuging to obtain solid B and filtrate B;

[0040] (4) adding solid B to 5°C ice water in a ratio of 1:5, stirring for 30 min and centrifuging to obtain solid C and filtrate C;

[0041] (5) Solid C was added to ice water at 5°C in a ratio of 1:5, stirred for 30 min and then centrifuged to obtain solid D and filtrate D, and then solid D was dried to obtain 162 g of magnesium orotate with a yield of 96.87%, a magnesium content of 7.165%, a magnesium orotate content of 99.95%, and a sulfate content of <0.05%.

[0042] Comparative Example

[0043] Anhydrous orotic acid (156 g, 1.0 mol) and 418 ml of water were mixed, and then pumped into a reactor. The temperature was raised to 75° C. Magnesium oxide (20.1 g, 0.5 mol) was slowly added into the reactor in batches while stirring to react. After about 5 minutes of reaction, the feed liquid gradually became viscous and began to solidify. The agitator blades were stuck and could not rotate. The feed liquid was broken up with a tool and 300 ml of water was added until the feed liquid reached a stirrable state. The reaction was continued for 4 hours. After the reaction was completed, the temperature was lowered and centrifuged to obtain solid A and filtrate A. Solid A was dried to obtain 173.6 g of a powder product with a magnesium content of 6.90% and a magnesium orotate content of 72.32%.

[0044] The above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the invention has been described in detail with reference to the aforementioned embodiments, it is still possible for a person skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent replacements for some of the technical features therein. Such modifications or replacements also fall within the scope of protection defined by the claims attached to this application.

Claims

1. A method for preparing high-purity magnesium orotate, characterized in that, include: Step (1), adding orotic acid, sodium hydroxide and water to a reactor in sequence, heating to reflux, reacting for 1-6 hours, filtering the reaction solution while hot, cooling, crystallizing, centrifuging and drying after the reaction is completed to obtain sodium orotate; step (2), preparing a magnesium solution; mixing the sodium orotate solid prepared in the step (1) with water in proportion, then pumping it into the reactor for heating, filtering the magnesium solution and slowly dropping it into the reactor in batches for reaction, cooling after the reaction is completed, centrifuging to obtain solid A and filtrate A; step (3), repeatedly washing the solid A prepared in the step (2) with water for multiple times, and drying to obtain high-purity magnesium orotate.

2. A method for preparing high-purity magnesium orotate as claimed in claim 1, characterized in that, In the step (2), the magnesium solution is any one of a magnesium chloride solution and a magnesium sulfate solution, and the mass ratio of the solute to water is 50-80:100 and 40-55:100 respectively.

3. A method for preparing high-purity magnesium orotate according to claim 1, characterized in that, In the step (2), the dropping speed of the magnesium solution is controlled to be 3 ml-9 ml / min.

4. A method for preparing high-purity magnesium orotate according to claim 1, characterized in that, In the step (2), the reaction temperature of the magnesium orotate is 60-100° C. and the reaction time is 2-6 hours.

5. A method for preparing high-purity magnesium orotate according to claim 1, characterized in that, In the step (3), the temperature of the washing water is 5-10°C, and the mass ratio of the washing water to the solid is 3-5:

1.

6. A method for preparing high-purity magnesium orotate according to claim 1, characterized in that, In the step (3), the step (3) includes: Step (3.1), adding water according to a proportion to the solid A prepared in step (2), stirring for 30 minutes and then centrifuging to obtain a solid B and a filtrate B; Step (3.2), adding water to the solid B in proportion, stirring for 30 minutes and then centrifuging to obtain a solid C and a filtrate C; Step (3.3), adding water to the solid C in proportion, stirring for 30 minutes and then centrifuging to obtain solid D and filtrate D; then drying the solid D to obtain high-purity magnesium orotate.