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A kind of preparation method of copper glycinate

A technology of copper glycinate and glycine, applied in the field of preparing copper glycinate by ammonia catalysis method, can solve the problems of difficult purification and long reaction time, and achieve the effects of accelerating sedimentation speed, increasing yield and speeding up separation speed.

Active Publication Date: 2018-04-13
HEBEI DONGHUA JIHENG CHEM
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AI Technical Summary

Problems solved by technology

[0003] At present, the technology of synthesizing copper glycine in industry mainly includes liquid-phase method and solid-phase method. Anion impurities, so the method is difficult to purify; the solid-phase method mainly uses glycine and copper acetate as raw materials to volatilize the acetic acid generated in the reaction process in time, but because the raw materials are difficult to mix very uniformly, the reaction time of this process longer
Therefore, there is a lack of a method for preparing copper glycinate that can not only avoid the interference of introducing new impurity ions but also improve the reaction rate in the market now.

Method used

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  • A kind of preparation method of copper glycinate
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  • A kind of preparation method of copper glycinate

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preparation example Construction

[0028] The preparation method of copper glycinate in the present invention is described in further detail below, including the following steps:

[0029] ① Dissolution of copper oxide: According to the ratio of the reaction molar ratio of copper oxide to ammonia of 1:2 to 1:10, the copper oxide is dissolved in ammonia water with a mass fraction of 5% to 50% to form a copper-ammonia complex;

[0030] CuO+4NH 3 ·H 2 O→Cu(NH 3 ) 4 (OH) 2 +3H 2 O

[0031] ② Synthesis reaction: Put the glycine and copper ammonia complex into the reaction according to the reaction molar ratio of 1:1 to 3:1, the heating temperature is 30 to 100 ℃, and the reaction is 30 to 200 min to obtain the reaction liquid;

[0032]

[0033] ③Product purification: the above reaction solution was cooled to 20-50℃, centrifuged to obtain copper glycinate solid 1 and filtrate, and then the filtrate was distilled under reduced pressure to obtain copper glycinate solid 2 and liquid fraction. The pressure of vacuum distillation w...

Embodiment 1

[0038] Such as figure 2 As shown, add 8g of copper oxide and 100ml of 15% ammonia water to the reaction flask 2, stir for 40 minutes and then completely dissolve, then add 15g of glycine and slowly heat it. At the same time, add 70ml of water and 8g of oxidation to the ammonia recovery flask 3. Copper, stir with magnetic stirrer 5 at room temperature. As the reaction temperature rises, the ammonia gas that is slowly generated in the reaction flask 2 reacts with glycine, and at the same time; the ammonia that overflows from the reaction flask 2 enters the ammonia recovery flask 3 to form cupric ammonia complexes with copper oxide The residual ammonia gas is absorbed by the tail gas treatment device 4. By observing the liquid level difference of the U-tube differential pressure gauge 1 to determine the pressure in the system, the reaction temperature can be adjusted to control the ammonia generation rate. After the reaction for 90 minutes, the reaction temperature rose to 90°C...

Embodiment 2

[0040] Add another 16g of copper oxide to the ammonia recovery bottle 3 in Example 1, and slowly add 125ml of 25% ammonia water as a new round of reaction flask 2. Stir fully for 50 minutes to completely dissolve the copper oxide and add 45g of glycine Then slowly heat up, and at the same time, add all the liquid fractions obtained by distillation under reduced pressure in Example 1 to the clean ammonia recovery bottle 3 and add deionized water to 210ml. At the same time, add 24g of copper oxide and stir at room temperature for Absorb the ammonia generated in the reaction flask 2, and observe the liquid level difference of the U-tube differential pressure gauge 1 to determine the pressure in the system. The reaction temperature can be adjusted to control the ammonia generation rate. After reacting for 120 minutes, the reaction temperature rose to 95°C, and there was almost no gas generation in the reaction flask 2, the reaction was stopped, the reaction solution was cooled to ro...

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Abstract

The invention discloses a preparation method of copper glycinate. The preparation method comprises the following steps: (1) dissolving copper oxide: dissolving the copper oxide into ammonia water to form a copper-ammonia complex; (2) carrying out a synthetic reaction: adding glycine and the copper-ammonia complex into a reaction kettle according to a certain ratio and reacting; heating and reacting for a period of time to obtain reaction liquid; (3) purifying a product: cooling the reaction liquid and centrifuging to obtain a copper glycinate solid 1 and filtrate; decompressing and distilling the filtrate to obtain a copper glycinate solid 2 and a liquid fraction; drying the copper glycinate solid 1 and the copper glycinate solid 2 to obtain a product; (4) recycling ammonia: absorbing ammonia gas generated in a reaction process by an absorbent, so as to obtain recycling liquid; using the recycling liquid to the step (1) to replace ammonia water for dissolving copper oxide. The invention provides the preparation method of the copper glycinate, which can avoid interference of foreign ions and can also improve the reaction speed.

Description

Technical field [0001] The invention relates to a preparation method of copper glycinate, in particular to a method for preparing copper glycinate by an ammonia catalysis method, and belongs to the technical field of preparation of copper glycinate. Background technique [0002] Copper is an important trace element necessary for humans and animals. It plays an important role in the body's hematopoietic function, metabolism, body resistance and reproductive performance. Under normal circumstances, the intake of copper in infants and young children is 0.4-1.0 mg per day, 1.5-3.0 mg for adults, the content of copper in the human body is about 100-150 mg, and the normal value of serum copper is 100-120 μg / dl, which is among the highest The second essential trace element. Copper deficiency can cause anemia, osteoporosis, coronary heart disease, vitiligo, infertility and other diseases. Since most of the absorption and utilization of copper in the digestive tract is in the form of st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/18C07C227/40C07C229/76
CPCC07C227/18C07C227/40C07C229/76
Inventor 徐志伟冯辉王秀茹王立辉马宁宁赵红梅高金辉宋铁犇李兴强宋秋月赫旭欢苏杰
Owner HEBEI DONGHUA JIHENG CHEM
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