Preparation method of copper glycinate

A technology of copper glycinate and glycine, which is applied in the field of preparation of copper glycinate by ammonia catalysis, can solve the problems of difficult purification and long reaction time, and achieve the effects of accelerating the sedimentation speed, increasing the yield, and reducing the discharge of waste liquid

Active Publication Date: 2017-01-04
HEBEI DONGHUA JIHENG CHEM
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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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  • 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, comprises the following steps:

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

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

[0031] ②Synthesis reaction: put glycine and copper ammonium complex into the reaction according to the reaction molar ratio of 1:1~3:1, the heating temperature is 30~100°C, and the reaction is 30~200min to obtain the reaction solution;

[0032]

[0033] ③Product purification: Cool the above reaction solution to 20-50°C, centrifuge to obtain copper glycinate solid 1 and filtrate, then distill the filtrate under reduced pressure to obtain copper glycinate solid 2 and liquid fraction, the pressure of vacuum distillation is -0.08MPa, Th...

Embodiment 1

[0038] Such as figure 2 As shown, add 8g of copper oxide and 100ml of ammonia water with a mass fraction of 15% to the reaction bottle 2, dissolve completely after stirring for 40min, then add 15g of glycine and then heat slowly, at the same time, add 70ml of water and 8g of oxidation Copper, stirred with a magnetic stirrer 5 at room temperature. Along with the rising of reaction temperature, the ammonia gas that slowly produces in reaction bottle 2 and reacts with glycine, simultaneously; The ammonia gas that overflows from reaction bottle 2 enters in ammonia gas recovery bottle 3 and forms copper ammonium complex with copper oxide compound, and the residual ammonia is absorbed by the tail gas treatment device 4. By observing the liquid level difference of the U-tube differential pressure gauge 1 to judge the pressure in the system, the reaction temperature can be adjusted to control the generation rate of ammonia gas. After reacting for 90 minutes, the reaction temperatur...

Embodiment 2

[0040]Add 16g of copper oxide to the ammonia gas recovery bottle 3 in Example 1, slowly add 125ml of ammonia water with a mass fraction of 25% as a new round of reaction bottle 2, fully stir for 50min, and add 45g of glycine after the copper oxide is completely dissolved Afterwards slowly heat, simultaneously, all join the liquid fraction that obtains in the vacuum distillation in embodiment 1 in the clean ammonia recovery bottle 3 and add deionized water to 210ml, add 24g cupric oxide simultaneously, stir under normal temperature, in order to Absorb the ammonia gas produced in the reaction bottle 2, and judge the pressure in the system by observing the liquid level difference of the U-tube differential pressure gauge 1, and adjust the reaction temperature to control the generation rate of ammonia gas. After 120 minutes of reaction, the reaction temperature rose to 95°C, and there was basically no gas in the reaction bottle 2, so the reaction was stopped, and the reaction solut...

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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 method for preparing copper glycinate, in particular to a method for preparing copper glycinate by ammonia catalysis, and belongs to the technical field of copper glycinate preparation. Background technique [0002] Copper is an important trace element necessary for human body 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, and that of adults is 1.5-3.0 mg. The copper content in the human body is about 100-150 mg. 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 stable complexes rather than ions, the third-generation copper supplement amino a...

Claims

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Application Information

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Patent Type & Authority Applications(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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