CN1861576A - Preparation process of ferrous glycine - Google Patents
Preparation process of ferrous glycine Download PDFInfo
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- CN1861576A CN1861576A CN 200610049929 CN200610049929A CN1861576A CN 1861576 A CN1861576 A CN 1861576A CN 200610049929 CN200610049929 CN 200610049929 CN 200610049929 A CN200610049929 A CN 200610049929A CN 1861576 A CN1861576 A CN 1861576A
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- ferrous sulfate
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Abstract
A process for preparing the ferrous glycinate from glycine and ferrous sulfate includes such steps as dissolving glycine in water, adding solid alkali, reaction, membrane separation to obtain sodium glycinate, adding ferrous sulfate solution and catalyst, regulating pH=3-8, heating to 80-100 deg.C, stirring while reacting, evaporation concentrating until the crystal film is educed out on the surface of scraper, slow cooling, crystallizing at 8 deg.C for at least 18 hr, and vacuum drying.
Description
Technical Field
Iron is an important component of hemoglobin, myoglobin and various enzyme systems, and plays important roles in nutrition, immunity and the like in vivo. It is one of the essential trace elements for livestock and poultry. The iron additive is developed in three stages, the first generation is inorganic salts such as ferrous sulfate, ferrous carbonate and the like, the second generation products are simple organic compounds such as ferrous citrate, ferrous fumarate and the like, but the two products have application defects, and the inorganic salts not only have poor absorption and utilization rate, but also easily cause environmental pollution, resource waste and influence other active nutrient substances in the feed. The simple organic compound is still difficult to overcome the defect of low absorption and utilization rate, and can not fully meet the requirement of animal organism growth. Therefore, for half a century, animal nutrition scientists have devoted themselves to research and develop new products of safe and efficient iron additives for feeding so as to overcome the disadvantages of the inorganic salt additives of trace elements which are used all the time.
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 the essential nutrient sources for animals, and animal nutrition researchers use the glycine as a complexing agent to research and develop a new generation of microelement amino acid nutritional additive, namely ferrous glycine.
A large number of researches show that ferrous glycinate has higher biological value, is close to a natural trace element supplement in an animal body, can be completely absorbed and utilized by animals, has good chemical stability, avoids the mutualantagonism among mineral substances, eliminates the defect of vitamin oxidation caused by inorganic salt, has the advantages of good solubility, high absorptivity, interference resistance, no irritation, no toxicity and the like, and is widely applied to the feed and food industries.
Disclosure of Invention
The invention aims to overcome the defects and provide the preparation method of the ferrous glycinate, which has the advantages of simple preparation process, stable and reliable product quality and convenient popularization and application. The method comprises the following steps: glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1-3: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate with solvent, adding the sodium glycinate, adding a little 121 of catalyst, adjusting the pH value to 3-8, heating to 80-100 ℃, and reacting for 1.5-2.5 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then placing in a refrigerator at 4 ℃ for crystallizing for at least 18 hours, and carrying out vacuum drying on the crystallized and purified crystal to prepare a ferrous glycinate product.
Glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1-2: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate with solvent, adding the sodium glycinate, adding a little 121 of catalyst, adjusting the pH value to 3-5, heating to 85-95 ℃, and reacting for 1.8-2.2 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then crystallizing for at least 20 hours in an environment below 5 ℃, and drying the crystal after crystallization and purification in vacuum to obtain a ferrous glycinate product.
Glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate in a solvent, adding the sodium glycinate, adding a small amount of 121 catalyst, adjusting the pH value to 4, heating to 90 ℃, and reacting for 2 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then crystallizing for 24 hours in a refrigerator at 4 ℃, and drying the crystal after crystallization and purification in a vacuum drying oven to obtain a ferrous glycinate product.
The invention breaks through the bottleneck of the production and preparation of the ferrous glycinate and establishes the ferrous glycinate (the molecular formula is [ Fe (C)]2H5NO2)2SO4.4H2O].[FeSO4.6H2O]Structural watch ofThe characterization and quality detection analysis method has the characteristics of simple preparation process, good quality of prepared products, convenience for popularization and application and the like.
Drawings
FIG. 1 is a block diagram of a preparation process route of the present invention.
Detailed Description
The invention will be described in detail with reference to the accompanying drawings and specific examples, wherein the selected materials mainly comprise ferrous sulfate (FeSO4&7H2O), solid alkali, glycine and a catalyst (the reagents are all analytically pure), wherein the reaction molar ratio of the glycine to the ferrous sulfate is 1: 2-3: 1, and the method mainly comprises the preparation of ① sodium glycinate: ② reacting sodium glycinate with inorganic salt to obtain the final product: 。
the specific process is shown in the attached figure 1: dissolving glycine 1 in water 2, adding solid alkali 3, heating 4, adding ferrous sulfate 5, adjusting the pH value 6, adding a catalyst 7, carrying out a synthesis reaction 8, evaporating 9, crystallizing and purifying 10, and drying 11 to obtain a product 12; the material remaining after evaporation 9 is recovered 14 by means of a solvent 13.
Example 1: glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate in a solvent, adding the sodium glycinate, adding a small amount of 121 catalyst, adjusting the pH value to 4, heating to 90 ℃, and reacting for 2 hours under stirring; evaporating and concentrating to separate crystal film on the surface by using a scraper film, taking out, slowly cooling at room temperature, crystallizing for 24 hours in a refrigerator at 4 ℃, and drying the crystal after crystallization and purification in a vacuum drying oven to obtain the crystal with the chemical structural formula of
Ferrous glycinate product (the same applies below).
Example 2: glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 2; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate in a solvent, adding the sodium glycinate, adding a small amount of 121 catalyst, adjusting the pH value to 8, heating to 100 ℃, and reacting for 1.5 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then crystallizing for 18 hours in a refrigerator at 4 ℃, and drying the crystal after crystallization and purification in a vacuum drying oven to obtain a ferrous glycinate product.
Example 3: glycine and ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 3: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate in a solvent, adding the sodium glycinate, adding a small amount of 121 catalyst, adjusting the pH value to 3, heating to 80 ℃, and reacting for 2.5 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then placing in a refrigerator at 4 ℃ for crystallizing for 20 hours, and drying the crystallized and purified crystal in a vacuum drying box to obtain a ferrous glycinate product.
Claims (3)
1. A preparation method of ferrous glycinate, it chooses glycine and ferrous sulfate as the main raw materials, characterized by that to choose glycine and ferrous sulfate to react the molar ratio to be 1: 2-3: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate with solvent, adding the sodium glycinate, adding a little 121 of catalyst, adjusting the pH value to 3-8, heating to 80-100 ℃, and reacting for 1.5-2.5 hours under stirring; evaporating with scraper filmCondensing to surface to precipitate crystal film, 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 molecular structure
The ferrous glycinate product.
2. The method for preparing ferrous glycinate according to claim 1, wherein the glycine and the ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1-2: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate with solvent, adding the sodium glycinate, adding a little 121 of catalyst, adjusting the pH value to 3-5, heating to 85-95 ℃, and reacting for 1.8-2.2 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then crystallizing for at least 20 hours in an environment below 5 ℃, and drying the crystal after crystallization and purification in vacuum to obtain a ferrous glycinate product.
3. The method for preparing ferrous glycinate according to claim 2, wherein the glycine and the ferrous sulfate are selected as main raw materials, and the reaction molar ratio of the glycine to the ferrous sulfate is 1: 1; dissolving glycine in water, adding solid alkali to react fully, and performing membrane separation to obtain glycine sodium salt; dissolving ferrous sulfate in a solvent, adding the sodium glycinate, adding a small amount of 121 catalyst, adjusting the pH value to 4, heating to 90 ℃, and reacting for 2 hours under stirring; evaporating and concentrating by using a scraper film until a crystal film is separated out on the surface, taking out and slowly cooling at room temperature, then crystallizing for 24 hours in a refrigerator at 4 ℃, and drying the crystal after crystallization and purification in a vacuum drying oven to obtain a ferrous glycinate product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610049929 CN1861576A (en) | 2006-03-19 | 2006-03-19 | Preparation process of ferrous glycine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516108A (en) * | 2011-12-31 | 2012-06-27 | 广州生产力促进中心 | Formula for preparing ferrous bisglycinate and method thereof |
| CN102578386A (en) * | 2012-01-18 | 2012-07-18 | 长沙兴加生物技术有限公司 | Compound glycine multi-mineral product as well as preparation method and application thereof |
| CN102696924A (en) * | 2012-06-21 | 2012-10-03 | 曲湘勇 | Fodder for producing iron rich green shell egg and improving laying rate, and effect measuring method |
| CN111032026A (en) * | 2017-06-30 | 2020-04-17 | 罗泽根有限责任公司 | Iron glycine sulfate compositions and uses thereof |
-
2006
- 2006-03-19 CN CN 200610049929 patent/CN1861576A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516108A (en) * | 2011-12-31 | 2012-06-27 | 广州生产力促进中心 | Formula for preparing ferrous bisglycinate and method thereof |
| CN102578386A (en) * | 2012-01-18 | 2012-07-18 | 长沙兴加生物技术有限公司 | Compound glycine multi-mineral product as well as preparation method and application thereof |
| CN102578386B (en) * | 2012-01-18 | 2016-08-31 | 长沙兴嘉生物工程股份有限公司 | Compound many ore deposits of glycine and its preparation method and application |
| CN102696924A (en) * | 2012-06-21 | 2012-10-03 | 曲湘勇 | Fodder for producing iron rich green shell egg and improving laying rate, and effect measuring method |
| CN111032026A (en) * | 2017-06-30 | 2020-04-17 | 罗泽根有限责任公司 | Iron glycine sulfate compositions and uses thereof |
| EP3644978A4 (en) * | 2017-06-30 | 2021-03-03 | Rozegen LLC | Iron glycine sulfate compositions and uses thereof |
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