Preparation method of calcium glycinate complex

A technology of calcium glycinate and complexes, which is applied in the field of preparation of calcium glycinate complexes, can solve problems affecting the purity of calcium glycinate complex products, complicated process steps, and large energy loss, so as to reduce resource input and improve product quality. Purity, the effect of reducing production costs

Pending Publication Date: 2021-10-22
浙江善救日健健康产业有限公司
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Problems solved by technology

The second generation of traditional organic salt calcium, such as calcium lactate, calcium gluconate, calcium citrate, etc., compared with inorganic calcium salt, has better solubility and less irritation to the gastrointestinal tract. The disadvantage is that the calcium content is relatively low. There are also certain side effects
This method has the following disadvantages: on the one hand, glycine first reacts with solid alkali in the first step, and then reacts in the second step with calcium chloride solution. Generally, 1 molar mass of glycine requires at least 1 molar mass of solid alkali to Complete the first step reaction, namely be equivalent to 100kg glycine need 53kg solid alkali consumption at least, thus it can be seen that the preparation method process step is comparatively complicated, and raw material cost is also higher; On the other hand, the sodium ion in the solid alkali is in the first In the first step reaction, it is combined with glycine to be glycine sodium salt. If the amount of solid base is high, in the second step reaction, glycine sodium salt and calcium chloride solution are mixed to generate glycine calcium complex. In the reaction solution, there will still be Part of the free-moving sodium ions and hydroxide ions usually use hydrochloric acid (HCl) for subsequent pH adjustments, which will cause sodium ions to react with chloride ions in hydrochloric acid to form sodium chloride, which will be cooled and crystallized later. The formation of sodium chloride crystals mixed in the calcium glycinate complex crystals, thus affecting the final product purity of calcium glycinate complex
But this method needs to obtain reaction product by ultrasonic radiation under organic solvent-absolute ethanol condition, and reaction product also needs through organic solvent (preferably absolute ethanol) repeatedly washing and then just can obtain calcium glycinate by centrifugation and vacuum drying process, Therefore, this method needs to use a large amount of ethanol, and there are also problems such as the recycling and utilization of ethanol and the hidden dangers it brings to the production process. Only the medium in the cleaning tank can be transferred to the reactants, the energy loss is large, and it is affected by various factors such as the amount of water in the cleaning tank, the position of the reaction bottle in the tank, etc., and the repeatability is poor

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  • Preparation method of calcium glycinate complex
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preparation example Construction

[0030] see figure 1 , a preparation method of calcium glycinate complex, comprising the steps:

[0031] Step S100, put glycine and anhydrous calcium chloride in a reaction kettle with a molar ratio of 2:0.8-1.5, and dissolve them in a solvent, then stir and mix, the solvent is water or mother liquor, heated to 60-100° C. After the complexation reaction process, a reaction solution is obtained. The pH value of the reaction solution obtained by dissolving an appropriate proportion of glycine and anhydrous calcium chloride in a solvent is in the range of 4 to 5, which can meet the requirements of complexation reaction.

[0032] According to the complexation reaction process, the reaction formula of the complexation reaction includes the following:

[0033] Ca 2+ +6H 2 O+ heat → [Ca(H 2 O) 6 ] 2+

[0034] [Ca(H 2 O) 6 ] 2+ +2C 2 H 5 NO 2 →[Ca(C 2 H 5 NO 2 ) 2 ·4H 2 O] 2+ +2H 2 O

[0035] In step S200, the reaction solution is cooled to stand still, and the pr...

Embodiment 1

[0058] Get food-grade content and be 98.5% glycine 1000kg, get food-grade content 98% anhydrous calcium chloride 740kg, drop into slowly to add 1500kg (1.5m 3 ) water in a reaction kettle, stirring and mixing, while gradually heating the reaction solution until the reaction temperature is 90°C, so that the solid matter in the reaction solution is completely dissolved, and the reaction is completed after maintaining the reaction temperature for 2 hours, and the reaction solution with a pH value of 4.8 is obtained.

[0059] Pour the reaction solution into the crystallization tank, cool down with circulating cooling water, and at the same time stir slowly to balance the temperature of each part of the reaction solution. When the temperature of the reaction solution is close to room temperature (25°C), sprinkle a small amount of white powder of calcium glycinate complex as a crystal. species to facilitate crystallization. A large number of crystals were precipitated in the reactio...

Embodiment 2

[0063] Get 500kg of glycine with a food grade content of 98.5%, and 370kg of anhydrous calcium chloride with a food grade content of 98%. 3 In the reaction kettle of the mother liquor, stir and mix, and gradually heat the reaction solution until the reaction temperature is 90° C. to completely dissolve the solid matter in the reaction solution, keep the reaction temperature for 2 hours, and the reaction ends to obtain a reaction solution with a pH value of 4.76.

[0064] Pour the reaction solution into the crystallization tank, cool it down with circulating cooling water, and at the same time stir slowly to balance the temperature of each part of the reaction solution. When the temperature of the reaction solution is close to room temperature (26°C), sprinkle a small amount of white powder of calcium glycinate complex as a crystal. species to facilitate crystallization. A large number of crystals were precipitated in the reaction solution, and its temperature was very close to...

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Abstract

The invention discloses a preparation method of a glycine calcium complex. The preparation method comprises the following steps: step S100, adding glycine and anhydrous calcium chloride into a solvent, stirring and mixing, heating to 60-100 DEG C, and carrying out complexation reaction to obtain a reaction solution, wherein the solvent is water or mother liquor, and the molar ratio of glycine to anhydrous calcium chloride being 2: (0.8-1.5); step S200, cooling and standing the reaction solution, adding the prepared calcium glycinate complex as a seed crystal, and carrying out a crystallization process to obtain a crystal mixed solution; step S300, performing centrifugal separation on the crystal mixed solution to obtain a crystal substance and liquid, wherein the crystal substance is a calcium glycinate tetrahydrate complex; and step S400, carrying out a drying process on the calcium glycinate complex tetrahydrate to obtain the calcium glycinate complex, wherein the drying process is divided into three sections and is carried out in a negative pressure environment or a vacuum environment. According to the invention, glycine and anhydrous calcium chloride are used as raw materials, and the process flow is improved and optimized, so that the product purity and yield can be improved, the production efficiency can be improved, and the resource and energy consumption can be reduced.

Description

technical field [0001] The invention relates to a calcium supplement preparation, in particular to a preparation method of a calcium glycinate complex. Background technique [0002] The development of calcium supplements has gone through three generations: inorganic calcium salt, traditional organic calcium salt and soluble organic calcium. Solid calcium carbonate is more commonly used in the first generation of inorganic salt calcium, which has high requirements on the quality and secretion of gastric acid, and is more likely to cause stones in the body and gastrointestinal irritation symptoms. The second generation of traditional organic salt calcium, such as calcium lactate, calcium gluconate, calcium citrate, etc., compared with inorganic calcium salt, has better solubility and less irritation to the gastrointestinal tract. The disadvantage is that the calcium content is relatively low. There are also certain side effects. The third-generation soluble organic calcium, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/04C07C227/18C07C229/76
CPCC07F3/003C07C227/18C07B2200/13C07C229/76
Inventor 洪作鹏蔡学英章亦武张玉红徐清华
Owner 浙江善救日健健康产业有限公司
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