CN112409200A - Preparation method and application of isoleucine chelated metal - Google Patents
Preparation method and application of isoleucine chelated metal Download PDFInfo
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- CN112409200A CN112409200A CN202011354864.5A CN202011354864A CN112409200A CN 112409200 A CN112409200 A CN 112409200A CN 202011354864 A CN202011354864 A CN 202011354864A CN 112409200 A CN112409200 A CN 112409200A
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- C07—ORGANIC CHEMISTRY
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- 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
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- A23K20/142—Amino acids; Derivatives thereof
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
The invention discloses a preparation method of isoleucine chelated metal, which comprises the following steps: dissolving the substance containing isoleucine roots under stirring, adding a metal source, heating for reaction, cooling the reaction system, crystallizing, filtering, separating, washing and drying to obtain the isoleucine chelated metal. The invention also provides application of the isoleucine chelated metal as an animal feed additive in animals, wherein the isoleucine chelated 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 essential trace elements of animals, is compared with 'vital elements' of animals, and is gradually found to be a component of more than 200 metalloenzymes, hormones and insulin in animal bodies, and has the following functions: (1) preventing the chloride ions of intestinal cells from exosmosis, reducing NO secretion, protecting intestinal biomembranes and compact structures of intercellular spaces, accelerating wound healing and having the function of resisting diarrhea; (2) the zinc is a nutrient for thymus development of immune organs, and the development of thymus can be effectively guaranteed only if the zinc is sufficient, T lymphocytes are normally differentiated, and the cellular immune function is promoted; (3) zinc is an important component of superoxide dismutase CuZn-SOD, and can inhibit the generation of excessive free radicals, maintain the oxidation resistance of organisms, and prevent the oxidative damage of protein, fat and DNA; (4) promote the secretion of pancreatic diglycosidase and improve the utilization rate of carbohydrate.
Manganese is a component of arginase, prolidase, 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, and hydrolase. The enzyme containing manganese can prevent the excess of lactic acid and protect the myoglobin membrane, thereby preventing the meat quality from being improved; in addition, the normal metabolism of fat can be maintained, fat deposition is reduced, protein deposition is improved, and the feed conversion ratio is improved. Manganese deficiency in animals can lead to decreased feed intake, slower growth, decreased feed utilization, bone abnormalities, ataxia, and reproductive dysfunction.
Magnesium is involved in many vital activities in animals, such as cellular respiration and the transfer of high-energy phosphate bonds. In oxidative phosphorylation, magnesium ions form complexes with ATP, ADP and AMP, and play a role in energy transfer. Magnesium also acts as an activator of various enzymes in the animal body, such as alkaline phosphatase, phosphoglucomutase, enolpeptidase, thiamine pyrophosphate (TTP), etc., thereby affecting fat, protein and energy metabolism. The magnesium content in natural plant feed usually cannot meet the requirements of various animals, and the supplement of magnesium in animal feed needs to be paid attention.
The amino acid chelated metal is a chelated compound with a ring structure generated by the action of metal elements essential for animal growth and amino acid, and is a metal element supplement close to the natural form in the animal body. Compared with inorganic metal element salt, the compound feed additive has good chemical stability and biochemical stability, can improve the biological utilization rate of metal elements, has the characteristics of easy digestion and absorption, interference resistance, small toxicity and the like, and is an ideal novel high-efficiency feed additive at present.
Isoleucine is a rhombic foliate or lamellar crystal, bitter in taste, soluble in water, slightly soluble in ethanol, a second limiting amino acid for ruminants, and one of three branched chain amino acids. Due to its special structure and function, it plays a particularly important role in the metabolism of life. It can help improve physical performance, help repair muscle tissue, control blood glucose, and provide energy to body tissues. It also increases growth hormone production and helps burn visceral fat. If the patient is lack of the traditional Chinese medicine, symptoms such as physical failure and coma can appear. Therefore, a chelated amino acid having isoleucine as a metal element has an important biological value.
The doctor's academic paper "Weak interaction research in Metal complexes" by Zhang east reports that an amino acid (dipeptide) -metal element (II) binary complex is prepared from nitrate of metal elements and amino acid in a nitric acid solution by potentiometric titration, wherein the amino acid contains isoleucine, the metal elements comprise zinc, magnesium and the like, and the zinc isoleucine is mainly Zn (Ile) from the aspects of stability constant and coordination configuration of the complex-)2In the form of isoleucine magnesium predominantly Mg (Ile)-)2The form exists. However, the method is only suitable for theoretical research and cannot be applied to large-scale production of feeds. In addition, the introduction of nitrate ions into the feed should be avoided as much as possible, because nitrate ions are reduced into nitrite in the body and have certain carcinogenicity.
Therefore, the research and development of isoleucine chelated metal which can be used in the feed field is a problem in the feed additive field.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and defects mentioned in the background technology, and provide a preparation method of isoleucine chelated metal and application thereof, wherein the preparation method has the advantages of high chemical reaction rate, high product yield, wide raw material source, low cost and the like. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of isoleucine chelated metal comprises the following steps: dissolving the substance containing isoleucine roots under stirring, adding a metal source, heating for reaction, cooling the reaction system, crystallizing, filtering, separating, washing and drying to obtain the isoleucine chelated metal.
In the above preparation method, preferably, the metal source comprises a soluble metal source and an insoluble metal source, and the metal source is added in two times, the soluble metal source is added firstly, and the insoluble metal source is added after the reaction is carried out for 0.2-0.5 h.
In the above production method, preferably, the metal content in the soluble metal source accounts for 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 the amino acid ligand does not contain hydroxyl, sulfydryl, guanidyl, carbonyl, amido bond, sulfuryl, benzene ring, heterocycle and other groups, the structure is relatively simple, but the carbon chain of the amino acid ligand is longer, contains branched chain methyl, has relatively stable property, the amino group is not easy to obtain electrons, and the hydroxyl group is not easy to lose electrons; and because of the branched chain, a certain steric hindrance exists. Namely, when isoleucine participates in the reaction, equilibrium isoelectric points need to be broken, the target product is isoleucine chelated metal, and alkali is generally adopted to break the equilibrium isoelectric points. In this case, if a soluble metal source is used as the metal source, the metal first reacts with the base to form hydroxide, resulting in a slow reaction rate. If the metal source is an insoluble metal source, isoleucine and the insoluble zinc salt can only react on a two-phase interface, the contact reaction area is small, the reaction rate is slow, and the product is easy to deposit on the surface of the insoluble zinc salt, so that the insoluble zinc salt is coated, and the raw material is remained in the product. Therefore, based on the characteristics of isoleucine, the effect of the metal source which is a soluble metal source or an insoluble metal source is not good, the defect of single use is avoided by combining the soluble metal source and the insoluble metal source, the reaction rate can be improved, and the purity of the product can be improved. The specific analysis is as follows:
in the invention, the principle of the invention is illustrated by taking a metal source as a zinc source as an example as follows: ionization of isoleucine to H in solution+And C6H12NO2 -When a soluble zinc source (such as zinc sulfate or zinc chloride) is adopted independently, zinc ions can react with an isoleucate radical to generate isoleucine zinc, and part of hydrogen ions are accumulated in a reaction system. Namely, the acid concentration of the solution is increased after the soluble zinc source is adopted to react with isoleucine, but the reaction tends to be in an equilibrium state after the acid solubility is increased to a certain value, and the conversion rate is low. At this time, alkali is added, but if zinc chloride, zinc sulfate and alkali are directly mixed, zinc hydroxide is generated firstly, and the reaction speed of zinc hydroxide and isoleucine is slow because zinc hydroxide is insoluble. In addition, the zinc hydroxide powder generated in the solution is fine, so that the generated finished product is also fine, solid-liquid separation is not facilitated, the specific gravity of the product is also light, the specific surface area is large, and the product is fluffy and is easy to fly dust. In addition, other side reactions such as isoleucine dehydrating condensation reaction and the like may occur by heating at a higher alkali concentration.
In the invention, the insoluble zinc source is 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 source, so that no by-product is generated, and the product purity is high. And when the insoluble zinc source is zinc carbonate or basic zinc carbonate, the carbon dioxide bubbles released in the reaction process can temporarily change the viscosity of the reaction system, the materials in the reaction system are distributed more loosely, the reaction rate is more uniform, and the particle size of the generated product tends to be consistent. At this point, the zinc source cannot be added too quickly, otherwise the solution would be prone to bumping. When the insoluble zinc source is active zinc oxide, the active zinc oxide has smaller particles, larger specific surface area, easier reaction with isoleucine and shorter reaction time. However, if an insoluble zinc source is used throughout, the reaction rate will be relatively slow.
In the invention, the research finds that based on the characteristics of the reaction of the soluble zinc source, the insoluble zinc source and isoleucine, the combination of the soluble zinc source and the insoluble zinc source is preferably adopted, the zinc source is added in two times, the soluble zinc source is firstly added, 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 firstly react with the isoleucid radical to generate isoleucine zinc, and part of hydrogen ions are accumulated in the reaction system. After the reaction is carried out for 0.2-0.5h, adding the insoluble zinc source, wherein a certain acid concentration exists in the reaction system, and the reaction rate of the insoluble zinc source can be accelerated by proper acid concentration, so that the reaction can be carried out in the forward direction. Therefore, the defects of independently adopting a soluble zinc source and an 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 much soluble zinc source is used, the concentration of acid accumulated in the reaction system is too high, and the reaction gradually tends to be in an equilibrium state until a certain stage, so that the content of zinc in the soluble zinc source is more suitable to be 5-50% of the content of zinc in the zinc source.
Further research shows that when the insoluble zinc source adopts the combination of zinc carbonate and/or basic zinc carbonate + active zinc oxide and the proportion 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, the finally obtained product is purer, and the byproducts are less. And when the zinc source is a mixed sample of zinc carbonate and/or basic zinc carbonate and active zinc oxide, the specific gravity is appropriate, the zinc source is not easy to sink, the zinc source is closer to the specific gravity of other components in the feed, and the layering phenomenon is not easy to occur during transportation.
It should be noted that other amino acids containing heterocyclic ring or benzene ring have too large steric hindrance, and even if the preparation method of the present invention is adopted, the improvement of reaction rate and 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 higher reaction rates with different raw materials. Other acidic amino acid and basic amino acid are contained, the neutral amino acid is not contained, the equilibrium isoelectric point is different from isoleucine, and the preparation method is not suitable for the preparation method adopted by the invention.
In the above preparation method, preferably, the isoleucine root-containing substance is isoleucine or isoleucine hydrochloride. More preferably, isoleucine hydrochloride is used, which reacts faster with the insoluble zinc source. In the invention, the matters containing isoleucine roots can adopt fermentation liquor, mother liquor, leftovers and the like for producing isoleucine, and are not required to be refined, purified and dried, so that the cost can be saved and the raw material range can be enlarged.
In the above production method, it is preferable that the molar ratio of isoleucine in the isoleucine root-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 root-containing substance to the metal in the metal source is (1.94-2.06): 1.
in the above preparation method, preferably, the reaction temperature is controlled to be 50-85 ℃, the reaction time is 1-2.5h, and the pH value of the reaction system is 5.5-8.5 during the temperature rising reaction. 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, and peptide bonds are generated, so that the product is impure and the yield is influenced. The reaction temperature is too low, the reaction time is too short, the reaction conversion rate is low, and the yield is influenced. If the reaction pH is too low, the reaction equilibrium is shifted to the left (product-forming starting material), resulting in incomplete reaction. If the pH is too high, a large amount of zinc ions will be stirred to form fine zinc hydroxide particles, which will result in a product of finer particle size. 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 roots is dissolved under stirring, the solvent is water or an aqueous solution of an organic solvent, the organic solvent is one or more of isopropyl alcohol, 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, isoleucine zinc has high solubility in water and low solubility in part of organic solvents. The organic solvent-water solution is used as a solvent, so that the materials in the reaction system are distributed more loosely, the reaction rate is more uniform, the particle size of the generated product tends to be consistent, and the crystals are uniformly dispersed in the reaction system. Considering the factors of cost, crystallization efficiency, volume size of a reaction kettle and the like, the volume ratio of the added organic solvent to water is (0.05-0.2): 1 is preferred.
In the above production method, preferably, the filtrate obtained by filtration separation is used as a mother liquor for the dissolution of isoleucine in the next reaction. The preparation method provided by the invention has no by-product, does not need to discharge waste water, can recycle the mother liquor, and is greatly beneficial to plant areas which are strictly controlled by environmental protection and do not allow waste water to be discharged. In addition, the mother liquor is recycled, except the drying and transferring process, almost no material loss exists, and the yield of the multi-batch product can be more than 99.8 percent.
As a general technical concept, the invention also provides an application of the isoleucine chelated metal as an animal feed additive in animals, wherein the isoleucine chelated metal is prepared by the preparation method, and the animals are pigs, poultry, ruminants or aquatic animals.
In the above application, preferably, the isoleucine chelating metal includes isoleucine zinc, isoleucine manganese and isoleucine chelating magnesium; the adding amount of isoleucine zinc in each ton of ruminant animal material is 30-80ppm calculated by zinc element; the addition amount of the isoleucine manganese in each ton of ruminant animal material is 30-60ppm calculated by manganese element; the adding amount of the isoleucine magnesium in each ton of pig feed is 100-400ppm calculated by magnesium element; the addition amount of the magnesium-containing additive in each ton of poultry feed is 200-500ppm calculated by magnesium element; the addition amount of the magnesium element in each ton of ruminant material is 1000-3000 ppm; the addition amount of the magnesium element in each ton of water power generation material is 200-600 ppm.
The chemical reaction equation and the reaction principle related to the invention are explained by taking a metal source as a zinc source as follows:
in the first step, isoleucine ionizes out H+And C6H12NO2 -；
Second step, H+Reacting with a zinc source; and with H+Consumed to ensure that the reaction of the first step is carried out positively;
2H++ZnO＝Zn2++H2O；
2H++Zn(OH)2＝Zn2++2H2O；
2H++ZnCO3＝Zn2++H2O+CO2↑；
8H++Zn5(OH)8Cl2＝5Zn2++8H2O+2Cl-；
6H++Zn4(OH)6SO4＝4Zn2++6H2O+SO4 2-；
xZnCO3·yZn(OH)2+2(x+y)H+＝(x+y)Zn2++(x+2y)H2O+xCO2↑；
third step, Zn2+And C6H12NO2 -Combine to form Zn (C)6H12NO2)2；
Zn2++2C6H12NO2 -＝Zn(C6H12NO2)2；
Fourth, excess H+With OH-The combination produces water.
H++OH-＝H2O。
Wherein the basic zinc carbonate is amorphous powder with unfixed component and molecular formula of xZnCO3·yZn(OH)2；x、y≥0。
The chemical reaction equation involved in the present invention is described below with a metal source as a magnesium source:
in the first step, isoleucine ionizes out H+And C6H12NO2 -；
Second step, H+Reacting with a magnesium source; and with H+Consumed to ensure that the reaction of the first step is carried out positively;
2H++MgO＝Mg2++H2O；
2H++Mg(OH)2＝Mg2++2H2O；
2H++MgCO3＝Mg2++H2O+CO2↑；
8H++Mg5(OH)8Cl2＝5Mg2++8H2O+2Cl-；
6H++Mg4(OH)6SO4＝4Mg2++6H2O+SO4 2-；
xMgCO3·yMg(OH)2+2(x+y)H+＝(x+y)Mg2++(x+2y)H2O+xCO2↑；
third step, Mg2+And C6H12NO2 -Combined to form Mg (C)6H12NO2)2；
Mg2++2C6H12NO2 -＝Mg(C6H12NO2)2；
Fourth, excess H+With OH-The combination produces water.
H++OH-＝H2O。
Wherein the basic magnesium carbonate is amorphous powder, the components are not fixed, and the molecular formula is xMgCO3·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 chelated metal is a product of limiting amino acid zinc, animals can preferentially absorb the isoleucine chelated metal, and the yield utilization rate is higher, so that the isoleucine chelated metal has a good application prospect.
2. In the invention, the raw materials are wide in source, 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 can also reduce energy consumption, simplify the process and avoid waste liquid discharge and environmental pollution.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art 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 limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The contents of metal elements in the products of the following examples were measured by atomic spectrophotometry, and the isoleucine content was measured by the azotometry method, and water loss at 180 ℃ was lost as crystal water, and water loss at 104 ℃ was lost as free water.
Example 1:
a preparation method of isoleucine zinc comprises the following steps: stirring is started, 535.4Kg of isoleucine with the purity of 98 percent is added into 2.5t of water for dissolving, the temperature is raised to 50 ℃, 278.3Kg of zinc chloride with the zinc content of 47 percent is slowly added, the pH value is controlled to be 5.5, the reaction is carried out for 2.5h, after the reaction is finished, the reaction system is cooled to below 40 ℃, the crystallization is carried out, the water is used for washing 3 times after the centrifugal filtration and separation, and the drying room is dried to obtain 604.8Kg of isoleucine zinc.
In this example, isoleucine content of the isoleucine zinc product was 77.0%, Zn was measured2+19.3%, a water loss at 104 ℃ of 3.6%, 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 Zn (C)6H12NO2)2。
Example 2:
a preparation method of isoleucine manganese comprises the following steps: starting stirring, adding 2.7t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, heating to 85 ℃, slowly adding 354Kg of manganese sulfate monohydrate with the manganese content of 31%, adding 100L of glycerol, controlling the pH value to be 6.0, reacting for 2.5h, cooling a reaction system to below 40 ℃ after the reaction is finished, centrifugally filtering, separating, washing with water for 3 times, and drying in a drying room to obtain 643Kg of isoleucine manganese.
In this example, isoleucine content of 75.7% in the isoleucine zinc product was determined, and Mn was determined2+16.0%, a water loss at 104 ℃ of 8.2%, i.e. a purity of 91.7%, a yield of 93.5% calculated as isoleucine, i.e. a molar ratio of isoleucine to manganese of about 2: 1, molecular formula Mn (C)6H12NO2)2。
Example 3:
a preparation method of isoleucine zinc comprises the following steps: starting stirring, adding 2.7t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, adding 185L of isopropanol, heating to 78 ℃, slowly adding 226Kg of basic zinc chloride with 58% zinc content, controlling the pH value to be 8.0, reacting for 1.5h, cooling a reaction system to below 40 ℃ after the reaction is finished, crystallizing, washing for 3 times by using water after centrifugal filtration and separation, and drying in a drying room to obtain 609Kg of isoleucine zinc.
In this example, isoleucine content of isoleucine-zinc product was found to be 76.9%, Zn2+19.3%, a water loss at 104 ℃ of 3.8%, 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 Zn (C)6H12NO2)2。
Example 4:
a preparation method of isoleucine zinc comprises the following steps: starting stirring, adding 2.7t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, adding 410L ethanol, heating to 55 ℃, slowly adding 233.6Kg of basic zinc carbonate with 56% zinc content, controlling the pH value to be 8.5, reacting for 2.5h, cooling a reaction system to below 40 ℃ after the reaction is finished, crystallizing, washing with water for 3 times after centrifugal filtration and separation, and drying in a drying room to obtain 623.2Kg of isoleucine zinc.
In this example, isoleucine content of 75.4% in isoleucine-zinc product was determined, Zn2+19.0%, a water loss at 104 ℃ of 5.5%, i.e. a purity of 94.4%, a yield calculated on zinc of 90.3%, i.e. a molar ratio of isoleucine to zinc of about 2: 1, molecular formula Zn (C)6H12NO2)2。
Example 5:
a preparation method of isoleucine zinc comprises the following steps:
93.5Kg of basic zinc carbonate with 56% of zinc content and 101.9Kg of active zinc oxide with 77% of zinc content are mixed uniformly for standby (the zinc content in the zinc oxide accounts for about 60% 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 to be dissolved, the temperature is raised to 60 ℃, 195.4Kg of the mixture of zinc carbonate and zinc oxide for later use is slowly added, the pH value is controlled to be 7.5, the reaction is carried out for 2.0h, the reaction system is cooled to below 40 ℃ after the reaction is finished, crystallization is carried out, water is used for washing for 3 times after centrifugal filtration and separation, and 700Kg of isoleucine zinc is obtained after flash evaporation and drying.
In this example, isoleucine content of the isoleucine zinc product was found to be 73.2%, Zn2+18.4%, a water loss at 104 ℃ of 8.3%, i.e. a purity of 91.6%, a yield of over 100% with respect to isoleucine, i.e. a molar ratio of isoleucine to zinc of about 2: 1, molecular formula Zn (C)6H12NO2)2. Moreover, the bumping phenomenon in this example is not obvious, the speed of adding the zinc source is obviously faster than that in the example 4 group, the bumping phenomenon is also obviously better than that in the example 4, and the yield is increased after the mother liquor is circulated.
Example 6:
a preparation method of isoleucine zinc comprises the following steps: starting stirring, adding 2.1t of the mother liquor in the embodiment 5 into a reaction kettle, adding 535.3Kg of isoleucine with the purity of 98% into the mother liquor for dissolving, heating to 75 ℃, slowly adding 14Kg of zinc chloride with the zinc content of 47% for reaction for 0.2h, adding 264.3Kg of zinc carbonate with the zinc content of 47%, controlling the pH value to be 7.0, reacting for 1.3h, cooling the reaction system to below 40 ℃ after the reaction is finished, crystallizing, centrifuging, filtering, separating, washing with water for 3 times, and drying in a drying room to obtain 693.9Kg of isoleucine zinc.
In this example, isoleucine content of 75.0% and Zn in isoleucine-zinc product was determined2+18.8%, a water loss at 104 ℃ of 6.1%, 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 Zn (C)6H12NO2)2. Although the reaction time was shortened, the yield was not reduced as compared with examples 1, 2, 4 and 5.
Example 7:
a preparation method of isoleucine manganese comprises the following steps: starting stirring, adding 2.7t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, adding 200L of glycerol, heating to 55 ℃, slowly adding 125.6Kg of manganese chloride with the manganese content of 42% for reaction for 0.5h, adding 105.8Kg of basic manganese chloride with the manganese content of 54%, controlling the pH value to be 7.3, reacting for 1h, 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 625.2Kg of isoleucine manganese.
In this example, isoleucine content of the isoleucine manganese product was determined to be 78.5%, Mn2+16.6%, a water loss at 104 ℃ of 4.8%, i.e. a purity of 95.1%, a yield calculated as isoleucine of 94.3%, i.e. a molar ratio of isoleucine to zinc of about 2: 1, molecular formula Mn (C)6H12NO2)2. The reaction time was shortened and the yield was increased as compared with example 2.
Example 8:
a preparation method of isoleucine magnesium comprises the following steps: stirring is started, 514.2Kg of isoleucine with the purity of 98 percent is added into 2.5t of water for dissolving, 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 2.5h, after the reaction is finished, the reaction system is cooled to below 40 ℃, the crystallization is carried out, the water is used for washing 3 times after the centrifugal filtration and separation, and the room is dried to obtain 520.8Kg of isoleucine magnesium.
In this example, isoleucine content of the isoleucine magnesium product was determined to be 79.1%, Mg2+7.4%, a water loss of 10.9% at 180 ℃, 2.5% at 104 ℃, i.e. a purity of 97.4%, a yield of 79.1% calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2: 1, molecular formula of Mg (C)6H12NO2)2·2H2O。
Example 9:
a preparation method of isoleucine magnesium comprises the following steps: starting stirring, adding 2.7t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, heating to 85 ℃, adding 285.9Kg of magnesium sulfate monohydrate with the magnesium content of 17%, controlling the pH value to be 8.5, reacting for 2.0h, adding 135L of diethyl ether after the reaction is finished, crystallizing, cooling the reaction system to below 40 ℃, washing with water for 3 times after centrifugal filtration and separation, and drying in a drying room to obtain 591.0Kg of isoleucine magnesium.
In this example, isoleucine content of isoleucine magnesium product was found to be 76.6%, Mg2+7.2%, 10.6% water loss at 180 ℃, 5.6% water loss 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 of Mg (C)6H12NO2)2·2H2O。
Example 10:
a preparation method of isoleucine magnesium comprises the following steps: starting stirring, adding 2.76t of 25% isoleucine hydrochloride aqueous solution into a reaction kettle, heating to 55 ℃, adding 121.5Kg of magnesium hydroxide with the magnesium content of 40%, controlling the pH value to be 5.5, reacting for 2.0h, adding 520L of glycerol after the reaction is finished, crystallizing, cooling the reaction system to below 40 ℃ for crystallizing, washing with water for 3 times after centrifugal filtration and separation, and drying in a drying room to obtain 622.8Kg of isoleucine magnesium.
In this example, isoleucine content of isoleucine magnesium product was found to be 76.2%, Mg2+7.1%, a water loss of 10.5% at 180 ℃, 6.1% at 104 ℃, i.e. a purity of 93.8%, a yield of 91.1% calculated on magnesium, i.e. a molar ratio of isoleucine to magnesium of about 2: 1, molecular formula of Mg (C)6H12NO2)2·2H2O。
Example 11:
a preparation method of isoleucine magnesium comprises the following steps:
81Kg of basic magnesium carbonate tetrahydrate with the magnesium content of 24 percent and 121.5Kg of magnesium carbonate with the magnesium content of 24 percent are evenly mixed for later use (the magnesium content in the magnesium carbonate accounts for about 60 percent of the total magnesium ratio).
Stirring is started, 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 to be dissolved, 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 1.5h, after the reaction is finished, the reaction system is cooled to below 40 ℃ for crystallization, water is used for washing for 3 times after centrifugal filtration and separation, and 639.3Kg of isoleucine magnesium is obtained after flash evaporation and drying.
In this example, isoleucine content of the isoleucine magnesium product was determined to be 80.3%, Mg2+7.5%, a water loss of 11.2% at 180 ℃, 1.0% at 104 ℃, i.e. a purity of 98.9%, a yield of more than 100% in terms of isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2: 1, molecular formula of Mg (C)6H12NO2)2·2H2And O. Moreover, the bumping phenomenon in this example was not significant, and the yield was increased after the mother liquor was circulated.
Example 12:
a preparation method of isoleucine magnesium comprises the following steps: stirring is started, 2.1t of mother liquor 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 liquor to be dissolved, the temperature is raised to 74 ℃, 29.2Kg of magnesium chloride with the magnesium content of 25 percent is slowly added to react for 0.2h, 137.7Kg of basic magnesium chloride with the magnesium content of 30 percent is added (the magnesium content in the magnesium chloride accounts for about 15 percent of the total magnesium ratio), 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 ℃ after the reaction is finished to crystallize, water is used for washing 3 times after centrifugal filtration and separation, and the isoleucine magnesium 683.7Kg is obtained after drying in a room.
In this example, isoleucine content of isoleucine magnesium product was found to be 76.1%, Mg2+7.1%, a water loss of 10.5% at 180 ℃, 6.2% at 104 ℃, i.e. a purity of 93.7%, a yield of 99.9% calculated as isoleucine, i.e. a molar ratio of isoleucine to magnesium of about 2: 1, molecular formula of Mg (C)6H12NO2)2·2H2And O. Although the reaction time was shortened, the yield was not reduced as compared with examples 1 to 5.
Example 13:
a preparation method of isoleucine magnesium comprises the following steps: starting stirring, adding 2.7t of isoleucine hydrochloride aqueous solution with the concentration of 25% into a reaction kettle, heating to 55 ℃, slowly adding 128.7Kg of magnesium sulfate monohydrate with the magnesium content of 17% for reaction for 0.5h, adding 95.5Kg of basic magnesium sulfate with the magnesium content of 28% (the magnesium content in the magnesium sulfate monohydrate accounts for about 45%), controlling the pH value to be 6.3, reacting for 1h, adding 300L of ethanol for crystallization, cooling the reaction system to below 40 ℃ for crystallization after the reaction is finished, washing with water for 3 times after centrifugal filtration and separation, and drying in a drying room to obtain 639.9Kg of isoleucine magnesium.
In this example, isoleucine content of isoleucine magnesium product was 77.0%, Mg2+7.2%, 10.7% water loss at 180 ℃, 5.1% water loss at 104 ℃, i.e. 94.8% purity, yield 94.6% calculated as isoleucine, i.e. molar ratio of isoleucine to magnesium about 2: 1, molecular formula of Mg (C)6H12NO2)2·2H2And O. The reaction time was shortened and the yield was increased as compared with examples 1 to 5.
Application example 1: application of isoleucine zinc as cow feed additive
Isoleucine zinc prepared in example 1 was added to the holstein cow feed and its effect on the milk yield of cows and on stealth mastitis was observed. Selecting 40 Holstein cows with similar ages, fetal times, milk yield and lactation period, randomly dividing into 4 groups, 10 cows in each group, one group as a control group and the other three groups as test groups. The control group was fed a basal diet supplemented with 80ppm zinc sulfate monohydrate calculated as zinc, and the test groups were fed basal diets supplemented with 30, 50, 80ppm isoleucine zinc calculated 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 determined. The effects are shown in table 1 below.
Table 1: effect of isoleucine Zinc on milk production and somatic cell count in Dairy cows
The data in table 1 above show that: compared with a control group, the daily milk yield of the cow is improved by 7.11% by adding 80ppm isoleucine zinc calculated by zinc into the daily ration (P <0.05), and the milk yield is improved by adding 50ppm isoleucine zinc calculated by zinc into the daily ration, but the difference is not obvious (P > 0.05). Addition of 80ppm isoleucine zinc in terms of zinc to the ration significantly reduced the number of somatic cells in milk by 25.02% (P <0.05), and the groups with 30 and 50ppm isoleucine zinc in terms of zinc also had a tendency to reduce the number of somatic cells. The number of somatic cells in milk reflects the occurrence probability of cow recessive mastitis, and a pasture generally treats cows with 50 to 100 ten thousand/ml of somatic cells in milk. Therefore, the daily milk yield of the dairy cow can be effectively improved by adding the isoleucine zinc into the daily ration, the occurrence probability of the invisible mastitis of the dairy cow is reduced, and the health level of the dairy cow is improved.
Application example 2: application of isoleucine magnesium as feed additive for fattening pigs
Isoleucine magnesium prepared in example 8 was used as an animal feed additive for feeding of fattening pigs. 120 fattening pigs of the same breed (Du multiplied by length multiplied by big) and the similar weight (80.0 +/-4.5 Kg) are selected in the test, and are randomly divided into a blank control group and 2 test groups according to the principle of the uniform average weight, wherein each group has 5 repetitions, and each repetition has 8 pigs. The blank group is fed with basic daily ration, and the test group is additionally added with 150 ppm isoleucine magnesium and 400ppm isoleucine magnesium respectively in the basic daily ration, and the test period is 28 days. The effects of isoleucine magnesium as a feed additive on the growth performance, muscle pH and drip loss of fattening pigs were studied, and the effects are shown in table 2 below.
Table 2: effect of isoleucine magnesium on growth performance, muscle pH value and drip loss of fattening pig
The data in table 2 above show that: compared with a blank control group, the addition of isoleucine magnesium in the daily ration does not have obvious influence on the average daily gain and the average daily feed intake of the fattening pigs (P is more than 0.05), but the addition of isoleucine magnesium has the tendency of improving the average daily gain and the average daily feed intake along with the increase of the concentration, and the addition of isoleucine magnesium accounting for 400ppm of magnesium in the daily ration can obviously reduce the feed conversion ratio of the fattening pigs by 7.45 percent (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 meat quality, and the addition of 400ppm isoleucine magnesium calculated by magnesium in daily ration can obviously improve the pH value of the muscle by 5.33 percent (P < 0.05); drip loss is the first important index considered by meat processors, and the addition of 400ppm isoleucine magnesium in terms of magnesium in the ration can significantly reduce drip loss of pork by 11.52% (P < 0.05). Experiments show that isoleucine magnesium is added into daily ration of fattening pigs, so that the utilization rate of feed can be improved, the meat quality is improved, and the water retention is improved, wherein the adding amount of 400ppm in terms of magnesium has the best effect.
Application example 3: application of isoleucine magnesium as white feather broiler feed additive
The isoleucine magnesium prepared in example 9 was used as an animal feed additive for feeding avidine broiler chickens, and the effect on the growth performance of broiler chickens was observed. 180 1-day-old avid broilers are randomly divided into 3 groups, each group has 5 repetitions, and each repetition has 12 chickens. One group was a blank control group and fed a basal diet, and the remaining 2 groups were test groups fed with isoleucine magnesium at 500ppm in addition to the basal diet measured as magnesium. 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: influence of isoleucine magnesium on growth performance of avidine broiler
The data in table 3 above show that: compared with a control group, the average daily gain of the broiler chicken can be remarkably improved by 9.48% (P <0.05) by adding 500ppm isoleucine magnesium calculated by magnesium into the daily ration, the daily feed intake is slowly increased along with the increase of the addition amount of the isoleucine magnesium, but the difference is not achieved, the feed-meat ratio is remarkably reduced, and the feed-meat ratio can be remarkably reduced by 5.49% (P <0.05) by adding 500ppm isoleucine magnesium calculated by magnesium into the daily ration; the addition of 300 ppm and 500ppm of isoleucine magnesium calculated by magnesium in daily ration respectively and obviously reduces the death rate of 36.28% and 47.86% (P < 0.05). The result shows that isoleucine magnesium is added into daily ration, so that the production performance of the broiler chicken can be effectively improved, the death rate of the broiler chicken can be obviously reduced, and the addition amount of 500ppm in terms of magnesium has the best effect.
Application example 4: application of isoleucine magnesium as cow feed additive
The magnesium isoleucine prepared in example 10 was added to the holstein cow feed and its effect on the milk yield and apparent nutrient digestibility of cows was observed. Selecting 30 Holstein cows with similar ages, fetal times, milk yields and lactation periods, randomly dividing the Holstein cows into 3 groups, wherein each group comprises 10 cows, one group is a control group, the other two groups are test groups, the control group feeds basic daily ration added with magnesium oxide of 4000ppm, and the test groups respectively add isoleucine magnesium of 1500 ppm and 3000ppm in terms of magnesium into the basic daily ration. The test period is 80 days, the milk yield of each cow is recorded and the apparent digestibility of nutrients is measured. The effects are shown in table 4 below.
Table 4: effect of isoleucine magnesium on milk production and apparent nutrient digestibility of cows
The data in table 4 above show that: compared with a control group, the daily ration added with 3000ppm isoleucine magnesium calculated by magnesium can obviously improve the daily milk yield of the dairy cow by 16.36 percent (P < 0.05); the addition of 1500 ppm of magnesium isoleucine and 3000ppm of magnesium isoleucine in daily ration can respectively and obviously raise the crude protein digestibility of milk cow by 6.39% and 4.98% (P <0.05), the addition of 2000ppm of magnesium isoleucine and daily ration can respectively and obviously raise the apparent digestibility of crude fat of milk cow by 4.12% (P <0.05), and the addition of 1500 ppm of magnesium isoleucine and 3000ppm of magnesium isoleucine and daily ration can respectively and obviously raise the calcium digestibility of milk cow by 19.58% and 11.33% (P < 0.05). The result shows that the addition of isoleucine magnesium in the daily ration can improve the milk yield of the dairy cow, improve the apparent digestibility of the daily ration of the dairy cow and improve the utilization rate of the feed.
Application example 5: application of isoleucine magnesium as megalobrama amblycephala additive
Isoleucine magnesium prepared in example 12 was added to the megalobrama amblycephala feed, and the influence thereof on the growth performance and blood index of megalobrama amblycephala was observed. In the test, 30 healthy megalobrama amblycephala are selected and 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 daily ration added with 600ppm magnesium chloride calculated by magnesium, and the test groups are respectively added with 250 ppm isoleucine magnesium calculated by magnesium and 550ppm isoleucine magnesium calculated by magnesium. And in the test period of 56d, recording the growth performance index of the megalobrama amblycephala, and measuring the blood index by using the tail vein. The effects are shown in table 5 below.
Table 5: influence of isoleucine magnesium on growth performance and blood of megalobrama amblycephala
The data in table 5 above show that: compared with a control group, the addition of 550ppm magnesium isoleucine in terms of magnesium into the daily ration can obviously improve the final body weight of the megalobrama amblycephala by 12.12% (P <0.05), has no obvious influence on the bait coefficient of the megalobrama amblycephala, but the bait coefficient has a decreasing trend along with the increase of the concentration of the magnesium isoleucine; under the stress condition of animals, the synthesis and release of corticoid COR are increased, so that the concentration of COR in blood is the first index for measuring the stress degree of the animals, and the addition of 550ppm isoleucine magnesium calculated by magnesium in the daily ration in the test can obviously reduce the quality concentration of cortisol 35.94% (P < 0.05); the glutamic-oxaloacetic transaminase is an important transaminase of fishes, when liver cells are damaged, the glutamic-oxaloacetic transaminase is released into blood, the activity is increased, and in the test, when 550ppm of isoleucine magnesium calculated by magnesium is added into daily ration, the activity of the glutamic-oxaloacetic transaminase can be obviously reduced by 54.97% (P is less than 0.05). The result shows that the growth performance of the megalobrama amblycephala can be improved and the stress capacity of the fish can be improved by adding the isoleucine magnesium into the daily ration of the megalobrama amblycephala.
Application example 6: application of isoleucine manganese as beef cattle feed additive
The isoleucine manganese prepared in example 7 was added to a feed for fattening cattle, and the influence of the addition of isoleucine manganese in a daily ration on the growth performance of the fattening cattle was studied. Selecting Simmental hybrid beef cattle with similar weight about 60 years of 17 months, randomly dividing the beef cattle into 3 groups, and 20 cattle in each group. The control group was fed a basal diet supplemented with 60ppm manganese sulfate monohydrate, calculated as manganese, and the test groups were fed a basal diet supplemented with 30, 55ppm isoleucine manganese, calculated as manganese, respectively. The effects are shown in table 6 below.
Table 6: influence of isoleucine manganese on growth performance of fattening cattle
As can be seen from table 6, the initial body weights of the control group, the 30ppm isoleucine-manganese group and the 55ppm isoleucine-manganese group of the test cattle before the start of the test and the body weights after the end of the test were not significantly different (P > 0.05); the differences in dry matter feed intake were not significant (P >0.05) for the three groups of experimental animals during the experimental period; the average daily gain of the 30ppm isoleucine-manganese group is 0.94kg/d, which is higher than that of the control group but has no significant difference (P >0.05), and the average daily gain of the 55ppm isoleucine-manganese group is 1.02kg/d, which is significantly higher than that of the control group (P < 0.05); the weight ratio of the 30ppm isoleucine manganese group material is lower than that of the control group, but the difference is not significant (P >0.05), and the weight ratio of the 55ppm isoleucine manganese group material is significantly lower than that of the control group (P < 0.05). Therefore, the addition of 55ppm of isoleucine manganese in the daily ration of the fattening cattle can obviously increase the daily weight of the fattening cattle and reduce the feed-weight ratio.
Claims (10)
1. A preparation method of isoleucine chelated metal is characterized by comprising the following steps: dissolving a substance containing isoleucine roots under stirring, adding a metal source, heating for reaction, cooling a reaction system, crystallizing, filtering, separating, washing and drying to obtain the isoleucine chelated metal.
2. The method according to claim 1, wherein the metal source comprises 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 the reaction for 0.2 to 0.5 hours.
3. The method of claim 2, wherein the metal content of the soluble metal source is 5-50% of the metal content of the metal source.
4. The method of claim 2, wherein the metal in the metal source comprises 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.
5. The production method according to any one of claims 1 to 4, wherein the isoleucine root-containing substance is isoleucine or isoleucine hydrochloride.
6. The production method according to any one of claims 1 to 4, wherein the molar ratio of isoleucine in the isoleucine root-containing substance to the metal in the metal source is (1.9-2.1): 1.
7. the production process according to any one of claims 1 to 4, wherein the reaction temperature is controlled to 50 to 85 ℃, the reaction time is 1 to 2.5 hours, and the pH of the reaction system is 5.5 to 8.5 at the time of the temperature-increasing reaction.
8. The method according to any one of claims 1 to 4, wherein when the substance containing isoleucine roots is dissolved under stirring, the solvent is water or an aqueous solution of an organic solvent, the organic solvent is one or more selected from 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 to 0.2): 1.
9. use of isoleucine chelated metal as an animal feed additive in animals, wherein the isoleucine chelated metal is prepared by the preparation method of any one of claims 1 to 8, and the animals are pigs, birds, ruminants or aquatic animals.
10. The use according to claim 9, wherein the isoleucine chelating metals include isoleucine zinc, isoleucine manganese, and isoleucine chelating magnesium; the addition amount of the isoleucine zinc in each ton of ruminant animal material is 30-80ppm calculated by zinc element; the addition amount of the isoleucine manganese in each ton of ruminant animal material is 30-60ppm calculated by manganese element; the adding amount of the isoleucine magnesium in each ton of pig feed is 100-400ppm calculated by magnesium element; the addition amount of the magnesium-containing additive in each ton of poultry feed is 200-500ppm calculated by magnesium element; the addition amount of the magnesium element in each ton of ruminant material is 1000-3000 ppm; the addition amount of the magnesium element in each ton of water power generation material is 200-600 ppm.
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