CN101225051A - Preparation method of zinc glycinate - Google Patents
Preparation method of zinc glycinate Download PDFInfo
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- CN101225051A CN101225051A CNA2008100596423A CN200810059642A CN101225051A CN 101225051 A CN101225051 A CN 101225051A CN A2008100596423 A CNA2008100596423 A CN A2008100596423A CN 200810059642 A CN200810059642 A CN 200810059642A CN 101225051 A CN101225051 A CN 101225051A
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Abstract
The invention relates to a preparation method of zinc glycinate, selecting glycine and zinc sulfate as main materials and the reaction molar ration of the glycine and the zinc sulfate in the range of 1:1 to 3:1, which is characterized in that: firstly, the glycine is dissolved in water, solid caustic soda is added into the solution to react with the glycine thoroughly and glycine sodium salt is obtained after the membrane separation, and then, the zinc sulfate dissolved by a solvent is added into the glycine sodium salt solution, the pH value of the solution with the glycine sodium salt and the zinc sulfate is regulated in the range of three to eight, the solution is heated to sixty to one hundred degrees and reacts for one to four hours under agitation, and the solution is evaporated and concentrated by scraper film until the precipitation of crystal membrane on the surface, the precipitated crystal membrane is cooled slowly at the ambient temperature and is crystallized for at least 18 hours at a temperature lower than 8 degrees, at last, after the vacuum drying of the crystallized and purified crystal, the zinc glycinate product with a molecular structure form of [Zn(C2H5NO2)2SO4 x 4H2O][ZnSO4 x 6H2O] is obtained. The preparation method of zinc glycinate has the advantages of simple preparation technique, high product quality of the products produced by the preparation method and popularization convenience.
Description
Background
The invention relates to a preparation method of an amino acid nutritional additive, in particular to a preparation method of zinc glycinate.
Technical Field
Zinc is one of the most important trace elements necessary for livestock and poultry, participates in the composition andmetabolism of various enzymes in vivo and directly participates in the in vivo synthesis of proteins and vitamins in vivo, and is a food and feed additive which is recognized at home and abroad at present and has the most ideal use effect. The zinc additive is developed through three stages, the first generation is inorganic salts, such as zinc sulfate, zinc oxide and the like, and the second generation is some simple organic compounds, such as zinc lactate, zinc gluconate and the like. However, the above two products have their disadvantages, the inorganic salts not only have poor absorption and utilization rate, but also easily cause environmental pollution and resource waste, and affect other active nutrients in the feed, and the simple organic compounds also have difficulty in overcoming the defect of low absorption and utilization rate, and cannot fully meet the needs of animal growth. Since the discovery and preparation of complexes in the chemical world since the beginning of the 17 th century, the study and application of complexes has been greatly developed in many industries. In the 70 s of the 20 th century, the research on the complex of trace elements and amino acids promoted the use of the complex in animal nutrition. Glycine is one of animal nutrition sources, and animal nutrition researchers use the glycine as a complexing agent to research and develop a new generation of trace element amino acid nutritional additive, namely zinc glycinate.
A large number of experiments prove that zinc glycinate combines zinc element necessary for animals and glycine with the minimum molecular weight in amino acid in a molar ratio of 1: 1 by virtue of a unique chemical structure, has a stable molecular structure, has the highest biological value and excellent chemical stability, avoids the mutual antagonism between mineral substances, and eliminates the defect that inorganic salt oxidizes vitamins. The zinc glycinate integrates economy, high efficiency and environmental protection, has the advantages of good solubility, high digestibility, interference resistance, no irritation, no toxicity and the like, and is widely applied to industries such as feed, food and the like.
In recent years, many enterprises at home and abroad compete for research and development of zinc glycinate, but due to the problems of process design and route, the quality of each product is different, the effect is different, and meanwhile, a set of standard zinc glycinate quality inspection analysis method is not provided, so that the product cannot be objectively evaluated, and the wide application of the zinc glycinate in practice is limited.
Disclosure of Invention
The invention aims to overcome the defects and provide the preparation method of the zinc glycinate, which has the advantages of simple preparation process, stable and reliable product quality and convenient popularization and application.
The invention is achieved by the following technical scheme thatGlycine and zinc sulfate are used as main raw materials, and the method is characterized in that the reaction molar ratio of the glycine to the zinc sulfate is 1: 1-3: 1; dissolving glycine in water, andadding solid alkali to react fully, obtaining glycine sodium salt after membrane separation, dissolving zinc sulfate with solvent, adding the glycine sodium salt, adjusting pH value to 3-8, heating to 60-100 ℃, reacting for 1-4 hours under stirring, evaporating and concentrating with a scraper film until crystal film is separated out on the surface, taking out, slowly cooling at room temperature, crystallizing at least 18 hours in an environment below 8 ℃, and vacuum drying the crystal after crystallization purification to prepare [ Zn (C) with molecular structure form2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
The reaction molar ratio of glycine to zinc sulfate is 2: 1; dissolving zinc sulfate with solvent, adding glycine sodium salt, adjusting pH to 5, heating to 80 deg.C, reacting under stirring for 4 hr, evaporating and concentrating with scraper film until crystal film is separated out on surface, taking out, slowly cooling at room temperature, crystallizing at 5 deg.C or below for 24 hr, vacuum drying the crystal, and making into [ Zn (C) with molecular structure form2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
The main research content of the invention is as follows:
① research on the synthesis process of zinc glycinate, pH value of complex solution, and trace element ion concentration [ Zn]in the complex solution2+]Determining the complexing parameters of different complexes, and determining the influence factors of the complexing reaction and the optimal synthesis process conditions by taking the complexing rate as an index.
② structural characterization and analysis of zinc glycinate complex comprises infrared spectroscopy of zinc glycinate, determining characteristic groups in molecules from the spectrogram, determining infrared measurement of the molecular structure of the complex, and analyzing and measuring the crystal structure of zinc glycinate by X-ray diffractometer.
The technology breaks through the technical bottleneck of production and preparation of zinc glycinate, and establishes zinc glycinate (molecular formula is C)4H30N2O22S2Zn2The chemical structural formula: [ Zn (C)2H5NO2)2SO4·4H2O][ZnSO4·6H2O]) The structure representation and quality detection analysis method has the advantages of simple preparation process, stable product quality, convenience in popularization and the like.
Detailed Description
The invention will now be described in detail with reference to specific examples: the material selected by the invention mainly comprises zinc sulfate (ZnSO4&7H)2O), solid caustic soda, glycine, the above reagents are analytical pure, and the reagent mainly comprises:
(1) preparation of glycine sodium salt:
C2H5NO2+NaOH→C2H4NO2Na+H2O
(2) reacting sodium glycinate with zinc sulfate to prepare a finished product of zinc glycinate:
the invention selects glycine and zinc sulfate as main raw materials, and is characterized in that the reaction molar ratio of the glycine to the zinc sulfate is 1: 1-3: 1; dissolving glycine in water, adding solid alkali for full reaction, and membrane separation to obtainDissolving zinc sulfate with solvent, adding the sodium glycinate, adjusting pH to 3-8, heating to 60-100 deg.C, stirring, reacting for 1-4 hr, concentrating with scraper film evaporation to precipitate crystal film on surface, taking out, slowly cooling at room temperature, crystallizing at 8 deg.C or below for at least 18 hr, vacuum drying the crystal, and making into [ Zn (C) with molecular structure2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
The embodiments of the present invention may be arbitrarily selected and substituted within the above numerical ranges, and constitute different embodiments, and are not limited to the following three embodiments.
Example 1: glycine and zinc sulfate are selected as main raw materials, the reaction molar ratio of the glycine to the zinc sulfate is 1: 1, firstly, the glycine is dissolved in water, solid alkali is added to the glycine to enable the glycine to fully react, sodium glycine salt is obtained after membrane separation, the zinc sulfate is dissolved by a solvent and then is added into the sodium glycine salt, after the pH value is adjusted to 4.5, the glycine sodium salt is heated to 90 ℃, the glycine sodium salt reacts for 2.5 hours under stirring, a scraper film is used for evaporation and concentration until a crystal film is separated out on the surface, the crystal film is slowly cooled at room temperature after being taken out, then the crystal film is placed in a refrigerator with the temperature of 4 ℃ for crystallization for 24 hours, and the crystal after crystallization and purification is: [ Zn (C)2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
Example 2: glycine and zinc sulfate are selected as main raw materials, the reaction molar ratio of the glycine to the zinc sulfate is 1: 2, the glycine is dissolved in water, solid alkali is added to the glycine to enable the glycine to react fully, glycine sodium salt is obtained after membrane separation, zinc sulfate is dissolved by a solvent, the glycine sodium salt is added, after the pH value is adjusted to 8, the glycine sodium salt is heated to 100 ℃, the glycine sodium salt reacts for 4 hours under stirring, a scraper film is used for evaporation and concentration until a crystal film is separated out on the surface, the crystal film istaken out and slowly cooled at room temperature, then the crystal film is placed in a refrigerator at 4 ℃ to crystallize for 20 hours, and the crystallized and purified crystal is placed in a vacuum drying box to be dried to obtain a.
Example 3: glycine and zinc sulfate are selected as main raw materials, the reaction molar ratio of the glycine to the zinc sulfate is 1: 3, firstly, the glycine is dissolved in water, solid alkali is added to the glycine to enable the glycine to fully react, sodium glycine salt is obtained after membrane separation, the zinc sulfate is dissolved by a solvent, then, the sodium glycine salt is added, after the pH value is adjusted to 3, the heating is carried out to 80 ℃, the reaction is carried out for 3 hours under stirring, a scraper film is used for evaporation and concentration until a crystal film is separated out on the surface, the crystal film is slowly cooled at room temperature after being taken out, then, the crystal film is placed in a refrigerator at 4 ℃ to be crystallized for 18 hours, and the crystal after crystallization and purification is placed in.
In the above embodiment of the invention, after the zinc sulfate is dissolved by the solvent, the sodium glycinate is added, the pH value is adjusted, and after the reaction by heating and stirring, the zinc sulfate is evaporated and concentrated until crystals are precipitated on the surface. After the crystals are precipitated on the surface by evaporation and concentration, a novel additive calcium glycinate product can be produced by selectively cleaning the crystals with an organic solvent and drying the crystals. The organic solvent washing at least comprises common alcohol washing. The mother liquor can be recycled after the reaction under heating and stirring, namely can be recycled.
Claims (2)
1. A preparation method of zinc glycinate selects glycine and zinc sulfate as main raw materials, and is characterized in that the reaction molar ratio of the glycine to the zinc sulfate is 1: 1-3: 1; dissolving glycine in water, adding solid alkali to react completely, performing membrane separation to obtain glycine sodium salt, dissolving calcium chloride in solvent, adding the glycine sodium salt, adjusting pH to 3-8, heating to 60-100 deg.C, reacting under stirring for 1-4 hr, concentrating with scraper film evaporation until crystal film is separated out, taking out, slowly cooling at room temperature, crystallizing at below 8 deg.C for at least 18 hr, and vacuum drying the crystal to obtain [ Zn (C)2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
2. The method for preparing zinc glycinate according to claim 1, wherein the reaction molar ratio of the glycine to the zinc sulfate is 2: 1; dissolving calcium chloride with solvent, adding glycine sodium salt, adjusting pH to 5, heating to 80 deg.C, reacting under stirring for 4 hr, evaporating and concentrating with scraper film until crystal film is separated out, taking out, slowly cooling at room temperature, and coolingCrystallizing at below 5 deg.C for 24 hr, and vacuum drying to obtain [ Zn (C) with molecular structure2H5NO2)2SO4·4H2O][ZnSO4·6H2O]The zinc glycinate product of (1).
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100596423A CN101225051A (en) | 2008-01-30 | 2008-01-30 | Preparation method of zinc glycinate |
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| CNA2008100596423A CN101225051A (en) | 2008-01-30 | 2008-01-30 | Preparation method of zinc glycinate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922954A (en) * | 2014-04-02 | 2014-07-16 | 哈尔滨德邦鼎立生物科技有限公司 | Method for preparing glycine zinc chelate |
| CN106187796A (en) * | 2016-07-08 | 2016-12-07 | 仲恺农业工程学院 | A kind of preparation method of zinc-glycine complex |
| CN109480095A (en) * | 2019-01-03 | 2019-03-19 | 常宁德邦生物科技有限公司 | A kind of preparation method of loose non-caking feed addictive glycine zine |
-
2008
- 2008-01-30 CN CNA2008100596423A patent/CN101225051A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922954A (en) * | 2014-04-02 | 2014-07-16 | 哈尔滨德邦鼎立生物科技有限公司 | Method for preparing glycine zinc chelate |
| CN106187796A (en) * | 2016-07-08 | 2016-12-07 | 仲恺农业工程学院 | A kind of preparation method of zinc-glycine complex |
| CN109480095A (en) * | 2019-01-03 | 2019-03-19 | 常宁德邦生物科技有限公司 | A kind of preparation method of loose non-caking feed addictive glycine zine |
| CN109480095B (en) * | 2019-01-03 | 2022-04-15 | 湖南德邦生物科技有限公司 | Preparation method of loose and non-caking feed additive zinc glycinate |
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Open date: 20080723 |