CN112409200B - Preparation method and application of isoleucine chelate metal - Google Patents
Preparation method and application of isoleucine chelate metal Download PDFInfo
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- CN112409200B CN112409200B CN202011354864.5A CN202011354864A CN112409200B CN 112409200 B CN112409200 B CN 112409200B CN 202011354864 A CN202011354864 A CN 202011354864A CN 112409200 B CN112409200 B CN 112409200B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/142—Amino acids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/24—Compounds of alkaline earth metals, e.g. magnesium
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of isoleucine chelate metal, which comprises the following steps: dissolving substances containing isoleucine radicals under stirring, adding a metal source, heating to react, cooling, crystallizing, filtering, separating, washing and drying a reaction system to obtain the isoleucine chelate metal. The invention also provides an application of the isoleucine chelate metal as an animal feed additive in animals, wherein the isoleucine chelate metal is prepared by the preparation method, and the animals are pigs, poultry, ruminants or aquatic animals. The preparation method has the advantages of high chemical reaction rate, high product yield, high product purity and the like.
Description
Technical Field
The invention belongs to the field of animal feed additives, and particularly relates to a preparation method and application of an amino acid chelate.
Background
The trace element zinc is one of the trace elements necessary for animals, has been compared with animal's "vital element", and it has been gradually found that zinc is a constituent of more than 200 metalloenzymes, hormones and insulin in animal bodies, and has the following effects: (1) Preventing intestinal cell chloride ion from extravasation, reducing NO secretion, protecting the compact structure of intestinal biological membrane and cell gap, accelerating wound healing, and resisting diarrhea; (2) Zinc is a nutrient for the development of thymus of immune organs, and can effectively ensure the development of thymus only when the zinc is sufficient, and can normally differentiate T lymphocytes and promote the cellular immune function; (3) Zinc is an important component of superoxide dismutase CuZn-SOD, can inhibit excessive free radical generation, maintain the antioxidant capacity of the organism, and prevent oxidative damage of protein, fat and DNA; (4) Promote secretion of pancreatic disaccharide enzyme and raise utilization rate of carbohydrate.
Manganese is a constituent of arginase, prolinase, RNA polymerase, manganese-containing superoxide dismutase (Mn-SOD), pyruvate carboxylase, etc., and is also an activator of many enzymes in the body such as phosphorylase, aldolase, transferase, hydrolase, etc. By the action of the manganese-containing enzyme, the excessive lactic acid can be prevented, and the myoglobin film can be protected, so that the meat quality can be prevented and improved; in addition, the composition can maintain normal metabolism of fat, reduce fat deposition, improve protein deposition and improve feed conversion ratio. The manganese deficiency of animals can lead to reduced feed intake, reduced growth, reduced feed utilization, abnormal bones, ataxia, abnormal reproductive function, and the like.
Magnesium is involved in many vital activities such as cellular respiration and transfer of high-energy phosphate bonds in animals. Magnesium ions form complexes with ATP, ADP and AMP during oxidative phosphorylation, and play a role in energy transfer. Magnesium can also act as an activator of various enzymes in animals such as alkaline phosphatase, glucose phosphomutase, enolpeptidase, thiamine pyrophosphate (TTP), etc., thereby affecting fat, protein and energy metabolism. Usually, the magnesium content in natural plant feed cannot meet the demand of various animals, and the supplement of magnesium should be noted in animal feed.
The amino acid chelated metal is a chelated compound with a cyclic structure generated by the action of metal elements necessary for animal growth and amino acids, and is a metal element supplement close to the natural form of an animal body. Compared with inorganic metal element salt, the compound has the advantages of good chemical stability and biochemical stability, improved biological utilization rate of metal elements, easy digestion and absorption, interference resistance, low toxicity and the like, and is a novel ideal high-efficiency feed additive at present.
Isoleucine is diamond leaf-shaped or sheet-shaped crystal, bitter in taste, water-soluble, slightly ethanol-soluble, is the second limiting amino acid of ruminants, and is one of three branched-chain amino acids. Because of its special structure and function, it plays a particularly important role in life metabolism. It can help to improve physical performance, help repair muscle tissue, control blood glucose, and provide energy to body tissue. It also increases the production of growth hormone and helps burn visceral fat. If the patient lacks, symptoms such as physical failure, coma and the like can appear. Therefore, the chelating amino acid having isoleucine as a metal element has important biological value.
Zhang Xiangdong A doctor's article on weak interaction in metal complexes reports that amino acid (dipeptide) -metal element (II) binary complexes are prepared by potentiometric titration of nitrates of metal elements and amino acids in nitric acid solution, wherein the amino acids contain isoleucine, the metal elements comprise zinc, magnesium and the like, and from the aspect of stability constants and coordination configurations of the complexes, the isoleucine zinc is mainly prepared by Zn (Ile - ) 2 In the form of magnesium isoleucine is predominantly in the form of Mg (Ile - ) 2 In the form of a gel. However, the method is only suitable for theoretical research, and is not applicable to large-scale production of feed. In addition, the introduction of nitrate ions into the feed should be avoided as much as possible, because nitrate is reduced to nitrite in the body, and has certain carcinogenicity.
Therefore, research into developing an isoleucine-chelating metal that can be used in the feed field is a difficult problem in the field of feed additives.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art, and provide a preparation method and application of isoleucine chelate metal, which have the advantages of high chemical reaction rate, high product yield, wide raw material sources, low cost and the like. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing isoleucine chelate metal, comprising the steps of: dissolving substances containing isoleucine radicals under stirring, adding a metal source, heating to react, cooling, crystallizing, filtering, separating, washing and drying a reaction system to obtain the isoleucine chelate metal.
In the above preparation method, preferably, the metal source includes a soluble metal source and an insoluble metal source, and the metal source is added in two portions, the soluble metal source is added first, and the insoluble metal source is added after reacting for 0.2 to 0.5 hours.
In the above preparation method, preferably, the metal content in the soluble metal source is 5 to 50% of the metal content in the metal source.
In the above preparation method, preferably, the metal in the metal source includes zinc, and the soluble zinc source is zinc sulfate or zinc chloride; the insoluble zinc source is one or more of zinc carbonate, basic zinc chloride, basic zinc sulfate, basic zinc carbonate, zinc hydroxide or zinc oxide; the metal in the metal source comprises manganese, and the soluble manganese source is manganese sulfate or manganese chloride; the insoluble manganese source is one or more of manganese carbonate, basic manganese chloride, basic manganese sulfate, basic manganese carbonate, manganese hydroxide or manganese monoxide; the metal in the metal source comprises magnesium, and the soluble magnesium source is magnesium sulfate or magnesium chloride; the insoluble magnesium source is one or more of magnesium carbonate, basic magnesium chloride, basic magnesium sulfate, basic magnesium carbonate, magnesium hydroxide or magnesium oxide. In the invention, the metal source can adopt produced tailings, defective products and the like, thereby reducing the cost.
The amino acid ligand is isoleucine, the structure of the amino acid ligand only contains one carboxyl group and one amino group, and does not contain hydroxyl, sulfhydryl, guanidino, carbonyl, amido bond, sulfonyl, benzene ring, heterocycle and other groups, the structure is relatively simple, but the carbon chain is longer, the amino acid ligand contains branched methyl, the property is stable, the amino group is not easy to obtain electrons, and the hydroxyl group is not easy to lose electrons; and because of the branching, there is some steric hindrance. When the isoleucine participates in the reaction, the equilibrium isoelectric point needs to be broken, and the target product is the isoleucine chelate metal, and alkali is generally adopted to break the equilibrium isoelectric point. In this case, if a soluble metal source is used as the metal source, the metal first reacts with the base to form a hydroxide, resulting in a slow reaction rate. If the metal source adopts an insoluble metal source, the isoleucine and the insoluble zinc salt can only react on the two-phase interface, the contact reaction area is small, the reaction rate is slow, the product is easy to deposit on the surface of the insoluble zinc salt, and the insoluble zinc salt is coated, so that the residual raw materials in the product are caused. Therefore, based on the characteristics of isoleucine, the effect of independently adopting the soluble metal source or the insoluble metal source is poor, and the defects of independent use are avoided by combining the soluble metal source and the insoluble metal source, so that the reaction rate can be improved, and the purity of a product is improved. The specific analysis is as follows:
in the present invention, the principle of the present invention is illustrated as follows by taking a metal source as a zinc source: ionization of isoleucine to H in solution + And C 6 H 12 NO 2 - When a soluble zinc source (such as zinc sulfate or zinc chloride) is singly adopted, zinc ions can react with the isoleucyl acid radical to generate isoleucine zinc, and part of hydrogen ions are accumulated in a reaction system. The acid concentration of the solution is increased after the soluble zinc source is adopted to react with the isoleucine, but after the acid solubility is increased to a certain value, the reaction tends to be in an equilibrium state, and the conversion rate is low. In this case, alkali is added, but if zinc chloride, zinc sulfate and alkali are directly mixed, zinc hydroxide is firstly generated, and zinc hydroxide is insoluble and reacts with isoleucine at a low speed. In addition, the zinc hydroxide powder generated in the solution is thinner, so that the generated finished product is thinner, solid-liquid separation is not facilitated, the specific gravity of the product is lighter, the specific surface area is large, the product is fluffy, and dust is easy to raise. In addition, when heated at a high alkali concentration, other side reactions such as isoleucine dehydration condensation reaction and the like occur.
In the invention, insoluble zinc sources are used for replacing soluble zinc sources such as zinc sulfate, zinc chloride and the like, and isoleucine is used for reacting with one or more of zinc oxide, zinc hydroxide, zinc carbonate or basic zinc carbonate in the insoluble zinc sources, so that byproducts are not generated, and the product purity is high. In addition, when the insoluble zinc source is zinc carbonate or basic zinc carbonate, carbon dioxide small bubbles released in the reaction process can temporarily change the viscosity of the reaction system, the distribution of materials in the reaction system is looser, the reaction rate is more uniform, and the particle size of the generated product tends to be consistent. At this time, the zinc source cannot be added too quickly, otherwise the solution is liable to pop. When the insoluble zinc source is active zinc oxide, the active zinc oxide particles are smaller, the specific surface area is larger, the active zinc oxide particles are easier to react with isoleucine, and the reaction time is shorter. However, if insoluble zinc sources are used in their entirety, the reaction rate is relatively slow.
In the invention, the research discovers that based on the characteristics of the reaction of a soluble zinc source and an insoluble zinc source with isoleucine, the combination of the soluble zinc source and the insoluble zinc source is preferably adopted, and the zinc source is added in two steps, namely, the soluble zinc source is added firstly, and the insoluble zinc source is added after the reaction is carried out for 0.2-0.5 h. The zinc ions in the soluble zinc salt added first react with the isoleucyl acid radical to generate zinc isoleucine, and part of hydrogen ions are accumulated in the reaction system. After 0.2-0.5h of reaction, adding an insoluble zinc source, wherein a certain acid concentration exists in the reaction system, and the proper acid concentration can accelerate the reaction rate of the insoluble zinc source, so that the reaction is carried out forward. Thus, the defects of independently adopting the soluble zinc source and the insoluble zinc source are overcome, the advantages of the soluble zinc source and the insoluble zinc source are fully exerted, and the reaction rate, the product purity and the like are higher.
However, if too many soluble zinc sources are adopted, the accumulated acid concentration in the reaction system is too high, and the reaction gradually tends to be in an equilibrium state after a certain period of reaction, so that the zinc content in the soluble zinc sources accounts for 5-50% of the zinc content in the zinc sources.
Further research shows that when the insoluble zinc source adopts the combination of zinc carbonate and/or basic zinc carbonate and active zinc oxide and the ratio of zinc oxide is controlled, the two insoluble zinc sources are matched through specific gravity, reaction activity, action effect and the like, the time required by the reaction process is shorter, the temperature required by the reaction is lower, the solution bumping phenomenon is also inhibited to the greatest extent, and finally the obtained product is purer and byproducts are fewer. In addition, when the zinc source is a mixed sample of zinc carbonate and/or basic zinc carbonate and active zinc oxide, the specific gravity is proper, the zinc source is not easy to sink, the zinc source is more similar to the specific gravity of other components in the feed, and layering phenomenon is not easy to occur during transportation.
It should be noted that other amino acids containing a heterocycle or a benzene ring have too large steric hindrance, and even if the preparation method of the present invention is adopted, the improvement of the reaction rate and the reaction conversion rate is not obvious. Other amino acids with simpler structures, such as glycine and the like, have small steric hindrance, do not need to consider the influence of the steric hindrance, and have faster reaction rates with different raw materials. The other amino acids containing acidic amino acid and basic amino acid are not neutral amino acid, and the equilibrium isoelectric point is different from that of isoleucine, so that the preparation method adopted by the invention is not applicable.
In the above preparation method, preferably, the isoleucine-containing substance is isoleucine or isoleucine hydrochloride. More preferably, isoleucine hydrochloride is used, which reacts faster with the insoluble zinc source. In the invention, substances containing isoleucine can adopt fermentation liquor, mother liquor, leftovers and the like for producing isoleucine, and the substances do not need to be refined, purified and dried, thereby saving the cost and expanding the range of raw materials.
In the above production method, preferably, the molar ratio of isoleucine in the isoleucine-containing substance to the metal in the metal source is (1.9-2.1): 1. more preferably, the molar ratio of isoleucine in the isoleucine-containing material to the metal in the metal source is (1.94-2.06): 1.
in the preparation method, preferably, when the temperature is raised for reaction, the reaction temperature is controlled to be 50-85 ℃, the reaction time is controlled to be 1-2.5 hours, and the pH value of a reaction system is controlled to be 5.5-8.5. In the invention, isoleucine contains amino and carboxyl, and dehydration and condensation can occur under the conditions of higher temperature, longer reaction time and strong alkalinity to generate peptide bonds, so that the product is impure and the yield is affected. The reaction temperature is too low, the reaction time is too short, the reaction conversion rate is low, and the yield is affected. If the reaction pH is too low, the reaction equilibrium shifts to the left (product-forming raw material) direction, resulting in incomplete reaction. If the pH is too high, a large amount of zinc ions will generate fine particles of zinc hydroxide under stirring, resulting in finer product particles. Therefore, it is necessary to select an appropriate reaction temperature, reaction time and reaction pH.
In the above preparation method, preferably, when the substance containing isoleucine radical is dissolved under stirring, the solvent is water or an aqueous solution of an organic solvent, the organic solvent is one or more of isopropanol, ethanol and glycerol, and the volume ratio of the organic solvent to water in the aqueous solution of the organic solvent is (0.05-0.2): 1. in the invention, the solubility of the isoleucine zinc in water is large, and the solubility of the isoleucine zinc in partial organic solvents is small. The organic solvent-water solution is used as the solvent, so that the materials in the reaction system are more loosely distributed, the reaction rate is more uniform, the sizes of the produced product particles tend to be consistent, and the product particles are uniformly dispersed and crystallized in the reaction system. Considering the factors of cost, crystallization efficiency, volume of the reaction kettle and the like, the volume ratio of the added organic solvent to water is (0.05-0.2): 1 is more suitable.
In the above preparation method, preferably, the filtrate obtained by filtration and separation is used as mother liquor for dissolving isoleucine in the next reaction. The preparation method provided by the invention has no byproducts, no wastewater is required to be discharged, the mother solution can be recycled, and the preparation method is of great benefit to factories with tighter environmental protection control and no wastewater discharge permission. In addition, the mother liquor is recycled, the material loss is almost avoided except in the drying and transferring process, and the yield of the multi-batch product can be more than 99.8%.
The invention also provides an application of the isoleucine chelate metal as an animal feed additive in animals, wherein the isoleucine chelate metal is prepared by the preparation method, and the animals are pigs, poultry, ruminants or aquatic animals.
In the above applications, preferably, the isoleucine chelating metal includes zinc isoleucine, manganese isoleucine and magnesium isoleucine chelating; the addition amount of the isoleucine zinc in each ton of ruminant feed is 30-80ppm calculated by zinc element; the addition amount of the isoleucine manganese in each ton of ruminant feed is 30-60ppm calculated by manganese element; the addition amount of the isoleucine magnesium in each ton of pig feed is 100-400ppm calculated by magnesium element; the addition amount of the magnesium element in each ton of poultry feed is 200-500ppm; the addition amount of the magnesium element in each ton of ruminant feed is 1000-3000ppm; the addition amount of the magnesium element in each ton of water active material is 200-600ppm.
The chemical reaction equation and the reaction principle related by the invention are described as follows by taking a metal source as a zinc source:
in the first step, isoleucine is ionized to form H + And C 6 H 12 NO 2 - ；
Second step, H + Reacting with a zinc source; and with H + Is consumed to make the first step reaction proceed forward;
2H + +ZnO＝Zn 2+ +H 2 O；
2H + +Zn(OH) 2 ＝Zn 2+ +2H 2 O；
2H + +ZnCO 3 ＝Zn 2+ +H 2 O+CO 2 ↑；
8H + +Zn 5 (OH) 8 Cl 2 ＝5Zn 2+ +8H 2 O+2Cl - ；
6H + +Zn 4 (OH) 6 SO 4 ＝4Zn 2+ +6H 2 O+SO 4 2- ；
xZnCO 3 ·yZn(OH) 2 +2(x+y)H + ＝(x+y)Zn 2+ +(x+2y)H 2 O+xCO 2 ↑；
third step, zn 2+ And C 6 H 12 NO 2 - Binding to form Zn (C) 6 H 12 NO 2 ) 2 ；
Zn 2+ +2C 6 H 12 NO 2 - ＝Zn(C 6 H 12 NO 2 ) 2 ；
Fourth step, redundant H + With OH - Combines to produce water.
H + +OH - ＝H 2 O。
Wherein the basic zinc carbonate is amorphous powder, the components are not fixed, and the molecular formula is xZnCO 3 ·yZn(OH) 2 ；x、y≥0。
The chemical reaction equation related in the invention is described as follows with a metal source as a magnesium source:
in the first step, isoleucine is ionized to form H + And C 6 H 12 NO 2 - ；
Second step, H + Reacting with a magnesium source; and with H + Is consumed to make the first step reaction proceed forward;
2H + +MgO＝Mg 2+ +H 2 O；
2H + +Mg(OH) 2 ＝Mg 2+ +2H 2 O；
2H + +MgCO 3 ＝Mg 2+ +H 2 O+CO 2 ↑；
8H + +Mg 5 (OH) 8 Cl 2 ＝5Mg 2+ +8H 2 O+2Cl - ；
6H + +Mg 4 (OH) 6 SO 4 ＝4Mg 2+ +6H 2 O+SO 4 2- ；
xMgCO 3 ·yMg(OH) 2 +2(x+y)H + ＝(x+y)Mg 2+ +(x+2y)H 2 O+xCO 2 ↑；
third step, mg 2+ And C 6 H 12 NO 2 - Binding to Mg (C) 6 H 12 NO 2 ) 2 ；
Mg 2+ +2C 6 H 12 NO 2 - ＝Mg(C 6 H 12 NO 2 ) 2 ；
Fourth step, redundant H + With OH - Combines to produce water.
H + +OH - ＝H 2 O。
Wherein basic carbon magnesium is amorphous powder, the components are not fixed, and the molecular formula is xMgCO 3 ·yMg(OH) 2 ；x、y≥0。
Compared with the prior art, the invention has the advantages that:
1. compared with other metal element products, the isoleucine chelate metal is a limited amino acid zinc product, animals can absorb the zinc product preferentially, and the yield and the utilization rate are higher, so that the zinc product has good application prospect.
2. In the invention, the sources of raw materials are wide, and the composition of the raw materials can be adjusted according to the cost to save the cost.
3. The preparation method has the advantages of high chemical reaction rate, high product yield, high product purity and the like.
4. The method of the invention also can reduce energy consumption, simplify the process and has no waste liquid discharge and environmental pollution.
Detailed Description
The present invention will be described more fully hereinafter with reference to the preferred embodiments for the purpose of facilitating understanding of the present invention, but the scope of protection of the present invention is not limited to the specific embodiments described below.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The content of metal elements in the products of the following examples is determined by atomic spectrophotometry, the content of isoleucine is determined by nitrogen determination, water loss is caused by loss of crystal water at 180 ℃ and water loss is caused by loss of free water at 104 ℃.
Example 1:
a method for preparing zinc isoleucine, comprising the following steps: starting stirring, adding 535.4Kg of isoleucine with the purity of 98% into 2.5t of water, dissolving, heating to 50 ℃, slowly adding 278.3Kg of zinc chloride with the zinc content of 47%, controlling the pH value to be 5.5, reacting for 2.5h, cooling the reaction system to below 40 ℃ after the reaction is finished, crystallizing, centrifugally filtering, separating, washing with water for 3 times, and drying in a drying room to obtain 604.8Kg of isoleucine zinc.
In this example, the isoleucine content of the zinc isoleucine product was 77.0%, zn 2+ 19.3%, a water loss of 3.6% at 104 ℃, i.e. a purity of 96.3%, a yield of 89.4% calculated as isoleucine, i.e. a molar ratio of isoleucine to zinc of about 2:1, molecular formula is Zn (C) 6 H 12 NO 2 ) 2 。
Example 2:
a method for preparing isoleucine manganese, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, then the temperature is raised to 85 ℃, 354Kg of manganese sulfate monohydrate with the manganese content of 31% is slowly added, 100L of glycerol is added, the pH value is controlled to be 6.0, the reaction is carried out for 2.5h, the reaction system is cooled to below 40 ℃, centrifugal filtration and separation are carried out, water is used for washing for 3 times, and 643Kg of isoleucine manganese is obtained after drying in a drying room.
In this example, the isoleucine content of the zinc isoleucine product was measured to be 75.7%, mn 2+ 16.0%, a water loss of 8.2% at 104 ℃, i.e., a purity of 91.7%, and a yield of 93.5% calculated as isoleucine, i.e., a molar ratio of isoleucine to manganese of about 2:1 of the formula Mn (C) 6 H 12 NO 2 ) 2 。
Example 3:
a method for preparing zinc isoleucine, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, 185L of isopropanol is added, the temperature is raised to 78 ℃, 226Kg of basic zinc chloride with the zinc content of 58% is slowly added, the pH value is controlled to be 8.0, the reaction is carried out for 1.5h, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, the reaction system is centrifugally filtered and separated, washed with water for 3 times, and a drying room is dried, thus obtaining 609Kg of isoleucine zinc.
In this example, the isoleucine content of the zinc isoleucine product was measured to be 76.9%, zn 2+ 19.3%, a water loss of 3.8% at 104 ℃, i.e. a purity of 96.2%, a yield of 89.9% calculated as isoleucine, i.e. a molar ratio of isoleucine to zinc of about 2:1, molecular formula is Zn (C) 6 H 12 NO 2 ) 2 。
Example 4:
a method for preparing zinc isoleucine, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, 410L of ethanol is added, the temperature is raised to 55 ℃, 233.6Kg of basic zinc carbonate with the zinc content of 56% is slowly added, the pH value is controlled to be 8.5, the reaction is carried out for 2.5h, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, the reaction system is centrifugally filtered and separated, then washed with water for 3 times, and a drying room is dried, thus obtaining 623.2Kg of isoleucine zinc.
In this example, the isoleucine content of the zinc isoleucine product was 75.4%, zn 2+ 19.0%, a water loss of 5.5% at 104 ℃, i.e. a purity of 94.4%, a yield of 90.3% calculated as zinc, i.e. a molar ratio of isoleucine to zinc of about 2:1, molecular formula is Zn (C) 6 H 12 NO 2 ) 2 。
Example 5:
a method for preparing zinc isoleucine, comprising the following steps:
93.5Kg of basic zinc carbonate with the zinc content of 56 percent and 101.9Kg of active zinc oxide with the zinc content of 77 percent are uniformly mixed for standby (the zinc content in the zinc oxide accounts for about 60 percent of the total zinc ratio).
Stirring is started, 2.3t of mother liquor in the embodiment 4 is added into a reaction kettle, 519.3Kg of isoleucine with the purity of 98 percent is added into the mother liquor for dissolution, then the temperature is raised to 60 ℃, 195.4Kg of standby zinc carbonate and zinc oxide mixture is slowly added, the pH value is controlled to 7.5, the reaction is carried out for 2.0h, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, the crystallization is carried out after centrifugal filtration and separation, water is used for washing for 3 times, and the isoleucine zinc 700Kg is obtained after flash evaporation and drying.
In this example, the isoleucine content of the isoleucine zinc product was 73.2%, zn 2+ 18.4%, a water loss of 8.3% at 104 ℃, i.e., a purity of 91.6%, a yield of over 100% on isoleucine basis, i.e., a molar ratio of isoleucine to zinc of about 2:1, molecular formula is Zn (C) 6 H 12 NO 2 ) 2 . In addition, the bumping phenomenon in the embodiment is not obvious, the speed of adding the zinc source is obviously faster than that of the group of the embodiment 4, the bumping phenomenon is also obviously better than that of the embodiment 4, and the yield is increased after the mother solution is circulated.
Example 6:
a method for preparing zinc isoleucine, comprising the following steps: stirring is started, 2.1t of mother liquor in the embodiment 5 is added into a reaction kettle, 535.3Kg of isoleucine with the purity of 98% is added into the mother liquor for dissolution, then the temperature is raised to 75 ℃, 14Kg of zinc chloride with the zinc content of 47% is slowly added for reaction for 0.2h, 264.3Kg of zinc carbonate with the zinc content of 47% is slowly added, the pH value is controlled to 7.0, the reaction is carried out for 1.3h, after the reaction is finished, the reaction system is cooled to below 40 ℃ for crystallization, the reaction system is centrifugally filtered and separated, then washed with water for 3 times, and a drying room is dried, thus obtaining 693.9Kg of zinc isoleucine.
In this example, the isoleucine content of the zinc isoleucine product was 75.0%, zn 2+ 18.8%, a water loss of 6.1% at 104 ℃, i.e., a purity of 93.8%, a yield of 99.9% calculated as isoleucine, i.e., a molar ratio of isoleucine to zinc of about 2:1, molecular formula is Zn (C) 6 H 12 NO 2 ) 2 . The reaction time was shortened as compared with examples 1, 2, 4 and 5, but the yield was not lowered.
Example 7:
a method for preparing isoleucine manganese, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, 200L of glycerol is added, the temperature is raised to 55 ℃, 125.6Kg of manganese chloride with the manganese content of 42% is slowly added for reaction for 0.5h, 105.8Kg of basic manganese chloride with the manganese content of 54% is then added, the pH value is controlled to 7.3, the reaction is carried out for 1h, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, the reaction system is centrifugally filtered and separated, water is used for washing for 3 times, and a drying room is used for drying, so that 625.2Kg of isoleucine manganese is obtained.
In this example, the isoleucine content of the isoleucine manganese product was measured to be 78.5%, mn 2+ 16.6%, a water loss of 4.8% at 104 ℃, i.e., a purity of 95.1%, and a yield of 94.3% calculated as isoleucine, i.e., a molar ratio of isoleucine to zinc of about 2:1 of the formula Mn (C) 6 H 12 NO 2 ) 2 . Compared with example 2, the reaction time was shortened and the yield was increased.
Example 8:
a method for preparing magnesium isoleucine, comprising the following steps: stirring is started, 514.2Kg of isoleucine with the purity of 98 percent is added into 2.5t of water to be dissolved, then the temperature is raised to 50 ℃, 196.0Kg of magnesium chloride with the magnesium content of 25 percent is added, the pH value is controlled to be 7.5, the reaction is carried out for 2.5 hours, the reaction system is cooled to below 40 ℃ after the reaction is finished, crystallization, centrifugal filtration and separation are carried out, water washing is carried out for 3 times, and 520.8Kg of isoleucine magnesium is obtained after drying in a drying room.
In this example, the isoleucine content of the magnesium isoleucine product was measured to be 79.1%, mg 2+ 7.4%, 10.9% at 180 ℃, 2.5% at 104 ℃, i.e. 97.4% purity, and 79.1% yield calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O。
Example 9:
a method for preparing magnesium isoleucine, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25 percent is added into a reaction kettle, then the temperature is raised to 85 ℃, 285.9Kg of magnesium sulfate monohydrate with the magnesium content of 17 percent is added, the pH value is controlled to be 8.5, the reaction is carried out for 2.0h, 135L of diethyl ether is added after the reaction is finished, crystallization is carried out, the reaction system is cooled to below 40 ℃, centrifugal filtration and separation are carried out, water is used for washing for 3 times, and the 591.0Kg of isoleucine magnesium is obtained after drying in a drying room.
In this example, the isoleucine content of the isoleucine magnesium product was measured to be 76.6%, mg 2+ 7.2%, 10.6% at 180 ℃, 5.6% at 104 ℃, i.e. 94.3% purity, 86.9% yield calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O。
Example 10:
a method for preparing magnesium isoleucine, comprising the following steps: stirring is started, 2.76t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, the temperature is raised to 55 ℃, 121.5Kg of magnesium hydroxide with the magnesium content of 40% is added, the pH value is controlled to be 5.5, the reaction is carried out for 2.0h, 520L of glycerol is added after the reaction is finished, crystallization is carried out, the reaction system is cooled to below 40 ℃ for crystallization, centrifugal filtration and separation are carried out, water is used for washing for 3 times, and 622.8Kg of isoleucine magnesium is obtained after drying in a drying room.
In this example, the isoleucine content of the isoleucine magnesium product was measured to be 76.2%, mg 2+ 7.1%, 10.5% at 180 ℃, 6.1% at 104 ℃, i.e. 93.8% purity, 91.1% yield calculated as magnesium, i.e. isoleucine to magnesium molar ratio of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O。
Example 11:
a method for preparing magnesium isoleucine, comprising the following steps:
81Kg of tetrahydrated basic magnesium carbonate with the magnesium content of 24% and 121.5Kg of magnesium carbonate with the magnesium content of 24% are uniformly mixed for later use (the magnesium content in the magnesium carbonate accounts for about 60% of the total magnesium ratio).
2.3t of mother liquor in the embodiment 3 is added into a reaction kettle, 498.8Kg of isoleucine with the purity of 98 percent is added into the mother liquor for dissolution, then the temperature is raised to 60 ℃, 202.5Kg of standby basic magnesium carbonate and magnesium carbonate mixture is slowly added, the pH value is controlled to be 5.5, the reaction is carried out for 1.5 hours, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, the crystallization is carried out for 3 times after centrifugal filtration and separation, and the magnesium isoleucine 639.3Kg is obtained after flash evaporation and drying.
In this example, the isoleucine content of the isoleucine magnesium product was 80.3%, mg 2+ 7.5%, 11.2% at 180 ℃, 1.0% at 104 ℃, i.e. 98.9% purity, and yields of over 100% on isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O. In addition, the bumping phenomenon in this example is not obvious, and the yield increases after the mother liquor is circulated.
Example 12:
a method for preparing magnesium isoleucine, comprising the following steps: stirring is started, 2.1t of mother solution in the embodiment 4 is added into a reaction kettle, 514.2Kg of isoleucine with the purity of 98 percent is added into the mother solution for dissolution, then the temperature is raised to 74 ℃, 29.2Kg of magnesium chloride with the magnesium content of 25 percent is slowly added for reaction for 0.2h, 137.7Kg of basic magnesium chloride with the magnesium content of 30 percent (the magnesium content in the magnesium chloride accounts for about 15 percent of the total magnesium), the pH value is controlled to be 7.0, the reaction is carried out for 1.2h, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, water is used for washing 3 times after centrifugal filtration and separation, and 683.7Kg of isoleucine magnesium is obtained after drying in a drying room.
In this example, the isoleucine content of the isoleucine magnesium product was measured to be 76.1%, mg 2+ 7.1%, 10.5% at 180 ℃, 6.2% at 104 ℃, i.e. 93.7% purity, 99.9% yield calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O. The reaction time was shortened as compared with examples 1 to 5, but the yield was not lowered.
Example 13:
a method for preparing magnesium isoleucine, comprising the following steps: stirring is started, 2.7t of isoleucine hydrochloride water solution with the concentration of 25% is added into a reaction kettle, the temperature is raised to 55 ℃, 128.7Kg of magnesium sulfate monohydrate with the magnesium content of 17% is slowly added for reaction for 0.5h, 95.5Kg of basic magnesium sulfate with the magnesium content of 28% (the magnesium content in the magnesium sulfate monohydrate accounts for about 45% of the total magnesium ratio) is added, the pH value is controlled to be 6.3, the reaction is carried out for 1h, 300L of ethanol is added for crystallization, the reaction system is cooled to below 40 ℃ for crystallization after the reaction is finished, centrifugal filtration is carried out, water is used for washing 3 times after separation, and the drying room is dried, thus obtaining 639.9Kg of isoleucine magnesium.
In this example, the isoleucine content of the isoleucine magnesium product was 77.0%, mg 2+ 7.2%, 10.7% at 180 ℃, 5.1% at 104 ℃, i.e. 94.8% purity, 94.6% yield calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2:1, molecular formula is Mg (C) 6 H 12 NO 2 ) 2 ·2H 2 O. Compared with examples 1 to 5, the reaction time was shortened and the yield was increased.
Application example 1: application of zinc isoleucine as cow feed additive
The zinc isoleucine prepared in example 1 was added to Holstein cow stock and its effect on milk yield and invisible mastitis of cows was observed. 40 Holstein cows with similar ages, gestation times, milk yield and lactation period are selected and randomly divided into 4 groups, 10 cows in each group, one group is a control group, and the other three groups are test groups. The control group was fed with a basal diet supplemented with 80ppm zinc sulfate monohydrate as zinc, and the test group was fed with a basal diet supplemented with 30, 50, 80ppm zinc isoleucine as zinc, respectively. The test period was 90 days, and the milk yield of each cow was recorded and the number of somatic cells in the milk was measured. The effects are shown in table 1 below.
Table 1: effect of zinc isoleucine on milk yield and somatic cell count in cows
The data in table 1 above indicate that: compared with the control group, the daily milk yield of the dairy cows is obviously improved by adding 80ppm of isoleucine zinc in the daily ration (P < 0.05), and the daily milk yield is improved by adding 50ppm of isoleucine zinc in the daily ration, but the difference is not obvious (P > 0.05). The addition of 80ppm zinc isoleucine in daily ration significantly reduces the somatic cell number in milk by 25.02% (P < 0.05), and 30 and 50ppm zinc isoleucine group also has the tendency of reducing the somatic cell number. The number of somatic cells in milk reflects the occurrence probability of cow invisible mastitis, and cows with the number of somatic cells in milk of 50 ten thousand to 100 ten thousand per ml in pastures are generally treated with the invisible mastitis. Therefore, the daily milk yield of the dairy cows can be effectively improved by adding the isoleucine zinc into the daily ration, the occurrence probability of the invisible mastitis of the dairy cows can be reduced, and the health level of the dairy cows can be improved.
Application example 2: application of magnesium isoleucine as fattening pig feed additive
The magnesium isoleucine prepared in example 8 was used as an animal feed additive for feeding fattening pigs. 120 fattening pigs with the same variety (Du x length x big) and similar weight (80.0+/-4.5 Kg) are selected in the test, and randomly divided into a blank control group and 2 test groups according to the principle of uniform average weight, wherein each group is 5 times of the test groups, and 8 times of the test groups are 8 times of the test groups. The blank group is fed with basic ration, 150 ppm of isoleucine magnesium and 400ppm of isoleucine magnesium are added into the basic ration respectively, and the test period is 28 days. The effect of magnesium isoleucine as a feed additive on growth performance, pH value of muscle and drip loss of fattening pigs was studied, and the effect is shown in Table 2 below.
Table 2: effect of magnesium isoleucine on growing and fattening pig growth Properties, muscle pH and drip loss
The data in table 2 above indicate that: compared with a blank control group, the average daily gain and average daily feed intake of fattening pigs are not obviously influenced by adding the isoleucine magnesium in the daily ration (P is more than 0.05), but the average daily gain and average daily feed intake tend to be improved along with the increase of the concentration, and the feed-to-meat ratio of fattening pigs can be obviously reduced by adding 400ppm of isoleucine magnesium in the daily ration (P is less than 0.05); the pH value is a core index for measuring the pork quality, and is often used as a standard for evaluating poor-quality pork, and the pH value of the muscle can be remarkably improved by 5.33 percent (P is less than 0.05) by adding 400ppm of isoleucine magnesium in daily ration; drip loss is a first important index considered by meat processors, and the addition of 400ppm of isoleucine magnesium calculated by magnesium to ration can obviously reduce 11.52 percent (P < 0.05) of pork drip loss. Experiments show that the addition of isoleucine magnesium in daily ration of fattening pigs can improve the feed utilization rate, improve the meat quality and improve the water retention capacity, wherein the addition amount of 400ppm calculated by magnesium has the best effect.
Application example 3: application of magnesium isoleucine as feed additive for white feather broiler chickens
The isoleucine magnesium prepared in example 9 was used as an animal feed additive for feeding Evien broiler chickens, and the influence of the isoleucine magnesium on the growth performance of the broiler chickens was observed. 180 Evieine broilers at 1 day of age were randomly selected into 3 groups of 5 replicates of 12 chickens each. One group is a blank control group, the basic ration is fed, the rest 2 groups are test groups, and 250 ppm of isoleucine magnesium and 500ppm of isoleucine magnesium are additionally added into the basic ration. Weighing at 42 days old, and calculating daily gain, feed intake and feed conversion ratio of each group. The effects are shown in table 3 below.
Table 3: effect of magnesium isoleucine on the growth performance of Ewei-cause broiler chickens
The data in table 3 above indicate that: compared with a control group, the average daily gain of broilers can be obviously improved by 9.48 percent (P < 0.05) by adding 500ppm of isoleucine magnesium in daily ration, the daily feed intake is slowly increased but does not reach obvious difference along with the increase of the addition amount of the isoleucine magnesium, the feed conversion ratio is obviously reduced, and the feed conversion ratio can be obviously reduced by 5.49 percent (P < 0.05) by adding 500ppm of isoleucine magnesium in daily ration; the addition of 300 and 500ppm of isoleucine magnesium in the daily ration obviously reduces the mortality rate by 36.28 percent and 47.86 percent (P < 0.05) respectively. The result shows that the addition of isoleucine magnesium in daily ration can effectively improve the productivity of the broiler chickens and obviously reduce the death rate of the broiler chickens, wherein the addition amount of 500ppm calculated by magnesium has the best effect.
Application example 4: application of magnesium isoleucine as dairy cow feed additive
The magnesium isoleucine prepared in example 10 was added to a Holstein cow feed and its effect on milk yield and apparent digestibility of nutrients of the cows was observed. 30 Holstein cows with similar ages, gestation, milk yield and lactation period are selected and randomly divided into 3 groups, 10 cows are selected in each group, one group is a control group, the other two groups are test groups, the control group is fed with basic ration added with 4000ppm magnesium oxide calculated by magnesium, and the test groups are respectively added with 1500 ppm magnesium isoleucine and 3000ppm magnesium isoleucine calculated by magnesium in the basic ration. The test period was 80 days, and the milk yield of each cow was recorded and the apparent digestibility of the nutrients was measured. The effects are shown in table 4 below.
Table 4: effect of magnesium isoleucine on milk yield and apparent digestibility of nutrients in cows
The data in table 4 above indicate that: compared with a control group, the daily milk yield of the dairy cows can be obviously improved by 16.36 percent (P is less than 0.05) by adding 3000ppm of isoleucine magnesium in the daily ration; 1500 and 3000ppm of isoleucine magnesium calculated by magnesium are added into the daily ration to respectively and remarkably improve the digestibility of crude protein of the dairy cow by 6.39 percent and 4.98 percent (P < 0.05), 2000ppm of isoleucine magnesium calculated by magnesium is added into the daily ration to remarkably improve the apparent digestibility of crude fat of the dairy cow by 4.12 percent (P < 0.05), and 1500 and 3000ppm of isoleucine magnesium are added into the daily ration to respectively and remarkably improve the digestibility of calcium of the dairy cow by 19.58 percent and 11.33 percent (P < 0.05). The result shows that the addition of the isoleucine magnesium in the daily ration can improve the milk yield of the dairy cows, and simultaneously improve the apparent digestibility of the daily ration of the dairy cows and the utilization rate of the feed.
Application example 5: application of magnesium isoleucine as additive for megalobrama amblycephala
The magnesium isoleucine prepared in example 12 was added to the megalobrama amblycephala feed, and its effect on the growth performance and blood index of megalobrama amblycephala was observed. The test selects 30 healthy megalobrama amblycephala, and is divided into 3 treatment groups, 10 fishes in each group are divided into 1 control group and 2 test groups, the control group is fed with basic ration added with 600ppm magnesium chloride calculated by magnesium, and the test groups are respectively added with 250 ppm magnesium isoleucine and 550ppm magnesium isoleucine calculated by magnesium in the basic ration. And (5) recording the growth performance index of the megalobrama amblycephala in the test period 56d, and measuring the blood index of tail veins. The effects are shown in table 5 below.
Table 5: effect of magnesium isoleucine on the growth Performance and blood of megalobrama amblycephala
The data in table 5 above indicate that: compared with a control group, the addition of 550ppm of isoleucine magnesium in daily ration can obviously improve the powder weight of the megalobrama amblycephala by 12.12 percent (P is less than 0.05), has no obvious influence on the bait coefficient of the megalobrama amblycephala, but has a decreasing trend along with the increase of the concentration of the isoleucine magnesium; under the condition of stress, the synthesis and release of adrenocortical hormone COR of the animal are increased, so that the concentration of COR in blood is the first choice index for measuring the stress degree of the animal, and the mass concentration of cortisol can be obviously reduced by 35.94 percent (P < 0.05) by adding 550ppm of isoleucine magnesium in daily ration in the test; glutamic-oxaloacetic transaminase is an important transaminase of fish, when liver cells are damaged, the glutamic-oxaloacetic transaminase can be released into blood, the activity is increased, and the activity of 54.97 percent (P < 0.05) of the glutamic-oxaloacetic transaminase can be obviously reduced by adding 550ppm of isoleucine magnesium calculated by magnesium into daily ration in the test. The result shows that the addition of isoleucine magnesium in the daily ration of the megalobrama amblycephala can improve the growth performance of the megalobrama amblycephala and the stress capability of the fish.
Application example 6: application of manganese isoleucine as beef cattle feed additive
The isoleucine manganese prepared in example 7 was added to a fattening cattle feed, and the effect of the addition of isoleucine manganese to the ration on the growth performance of the fattening cattle was investigated. Siemens hybrid beef cattle with similar weight and about 60 heads and 17 months of age are selected and randomly divided into 3 groups of 20 heads. The control group was fed with a basal diet supplemented with 60ppm manganese sulfate monohydrate based on manganese, and the test group was fed with a basal diet supplemented with 30 and 55ppm manganese isoleucine based on manganese, respectively. The effects are shown in table 6 below.
Table 6: effect of manganese isoleucine on growth Property of fattening cattle
As can be seen from table 6, the initial weight of the control group, 30ppm manganese isoleucine group and 55ppm manganese isoleucine group test cattle before the start of the test and the weight after the end of the test were not significantly different (P > 0.05); the difference of the dry matter feed intake of the three groups of test animals in the test period is not obvious (P > 0.05); the average daily gain of the 30ppm manganese isoleucine group was 0.94kg/d, higher than the control group but the difference was not significant (P > 0.05), the average daily gain of the 55ppm manganese isoleucine group was 1.02kg/d, significantly higher than the control group (P < 0.05); the 30ppm isoleucine manganese group had a lower weight ratio than the control group, but the difference was not significant (P > 0.05), and the 55ppm isoleucine manganese group had a significantly lower weight ratio than the control group (P < 0.05). Therefore, the daily gain of the fattening cattle can be obviously increased by adding 55ppm of isoleucine manganese into daily ration of the fattening cattle, and the feed-to-weight ratio can be reduced.
Claims (3)
1. A method for preparing isoleucine chelate metal, comprising the steps of: dissolving substances containing isoleucine radicals under stirring, adding a metal source, heating to react, cooling, crystallizing, filtering, separating, washing and drying a reaction system to obtain the isoleucine chelate metal;
the metal source is added in two times, firstly, soluble metal source is added, and after 0.2-0.5h of reaction, insoluble metal source is added;
the metal content in the soluble metal source accounts for 5-50% of the metal content in the metal source;
when the metal in the metal source is zinc, the soluble zinc source is zinc sulfate or zinc chloride; the insoluble zinc source is one or more of zinc carbonate, basic zinc chloride, basic zinc sulfate, basic zinc carbonate, zinc hydroxide or zinc oxide; when the metal in the metal source is manganese, the soluble manganese source is manganese sulfate or manganese chloride; the insoluble manganese source is one or more of manganese carbonate, basic manganese chloride, basic manganese sulfate, basic manganese carbonate, manganese hydroxide or manganese monoxide; when the metal in the metal source is magnesium, the soluble magnesium source is magnesium sulfate or magnesium chloride; the insoluble magnesium source is one or more of magnesium carbonate, basic magnesium chloride, basic magnesium sulfate, basic magnesium carbonate, magnesium hydroxide or magnesium oxide;
when in heating reaction, the reaction temperature is controlled to be 50-85 ℃, the reaction time is controlled to be 1-2.5h, and the pH value of a reaction system is controlled to be 5.5-8.5;
when the substance containing isoleucine radical is dissolved under stirring, the solvent adopts water or aqueous solution of organic solvent, the organic solvent is one or more of isopropanol, ethanol and glycerol, and the volume ratio of the organic solvent to water in the aqueous solution of the organic solvent is (0.05-0.2): 1.
2. the method according to claim 1, wherein the isoleucine-containing substance is isoleucine or isoleucine hydrochloride.
3. The method according to claim 1, wherein the molar ratio of isoleucine in the isoleucine-containing substance to the metal in the metal source is (1.9-2.1): 1.
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