CN112174844B - Preparation method and application of ferrous alanine chelate - Google Patents
Preparation method and application of ferrous alanine chelate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/10—Feeding-stuffs specially adapted for particular animals for ruminants
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Abstract
The invention relates to a preparation method of ferrous alanine chelate, which comprises the following steps: adding ferrous salt solution into alanine solution, chelating under the protection of acid condition and inert gas, adding seed crystal for crystallization, concentrating, separating and drying to obtain ferrous alanine chelate. The preparation method has the advantages of high chelation rate, simple and convenient operation, obviously shortened production period and obviously reduced production cost, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method and application of a ferrous alanine chelate.
Background
Essential trace elements (such as iron, ferrous iron, copper, manganese, zinc, etc.) play a very important role in animal growth and meeting its nutritional requirements. The trace element content in the feed is low or not comprehensive enough, and the feed is difficult to meet the requirement of the growth of livestock and poultry and needs to be manually added. The amino acid metal chelate is a chelate product of metal ions and amino acids, methionine, tyrosine, tryptophan, leucine, glycine, hydrolyzed protein and the like are often used as ligands, and the cyclic structure of the chelate ensures that the metal amino acid chelate has higher chemical stability than the complex and has the effects of resisting interference, relieving antagonism competition among minerals and the like. The chelate has neutral intramolecular charge, good solubility under the condition of the environment in the organism, easy release of metal ions, direct digestion and absorption by intestinal tracts, and improved utilization rate and bioavailability of trace elements. The amino acid metal chelate becomes a novel microelement feed additive and is praised as a third generation product of essential microelements. However, the preparation method of the amino acid metal chelate has the defects of low chelation rate, low resource utilization rate and the like. For this reason, development of a more efficient method for producing an amino acid metal chelate is desired.
Iron is an important component of hemoglobin, myoglobin and various enzyme systems, plays important roles in nutrition, immunity and the like in vivo, and is one of important microelements necessary for human bodies and livestock and poultry. The amino acid chelated ferrous salt is prepared by utilizing amino acid and ferrous salt, but the ferrous salt is extremely easy to oxidize and hydrolyze, so that the amino acid chelated ferrous salt has low chelation rate, more byproducts and relatively longer reaction period. For this reason, a preparation process with a higher chelation rate is required to be studied.
Disclosure of Invention
The invention aims to provide a preparation method of ferrous alanine chelate, which comprises the following steps: adding ferrous salt solution into alanine solution, chelating under the protection of acid condition and inert gas, adding seed crystal for crystallization, concentrating, separating and drying to obtain ferrous alanine chelate.
In a preferred embodiment of the present invention, the alanine is selected from any one of L-alanine, D-alanine, alpha-alanine, beta-alanine, DL-alanine, or a combination thereof.
In a preferred embodiment of the present invention, the ferrous salt is selected from any one of ferrous sulfate, ferrous chloride, ferrous oxide, and ferrous hydroxide, or a combination thereof.
In a preferred embodiment of the present invention, alanine is: the molar ratio of the ferrous salt is 1-5:1, preferably 1-4:1, more preferably 1-3:1.
in a preferred embodiment of the present invention, the chelating reaction solution has a pH of 5.0 to 6.0.
In a preferred embodiment of the present invention, the acid-base regulator for regulating the pH of the reaction solution is selected from any one of sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, potassium bicarbonate, potassium carbonate, ammonia water, triethylamine, or a combination thereof.
In a preferred embodiment of the present invention, the inert gas is any one of nitrogen and argon or a combination thereof.
In a preferred embodiment of the present invention, the chelation reaction temperature is 60 ℃ to 100 ℃, preferably 70 ℃ to 90 ℃.
In a preferred embodiment of the present invention, the chelation reaction time is 1 to 5 hours, preferably 2 to 4 hours.
In a preferred embodiment of the present invention, an antioxidant may be added to the chelation reaction.
In a preferred embodiment of the present invention, the chelation reaction is performed with a ferrous salt: the molar ratio of the antioxidant is 1: (0.01-0.2), preferably 1: (0.02-0.1).
In a preferred embodiment of the present invention, the antioxidant is selected from any one of vitamin C, citric acid, iron powder, zinc powder, or a combination thereof.
In the preferred technical scheme of the invention, 0.001% -0.2% of ferrous alaninate chelate, preferably 0.002% -0.1% of seed crystal is added into the reaction solution.
In the preferred technical scheme of the invention, the prepared ferrous alanine chelate is subjected to crystallization and purification treatment.
In a preferred embodiment of the present invention, the number of crystallization and purification is not less than 1, preferably 1 to 4.
In a preferred embodiment of the present invention, the concentration is selected from any one of vacuum concentration, membrane concentration, normal pressure concentration, ultrafiltration concentration, and centrifugal concentration, or a combination thereof.
In a preferred embodiment of the present invention, the concentration temperature is 40-90 ℃, preferably 45-80 ℃, more preferably 50-70 ℃, most preferably 55-65 ℃.
In a preferred embodiment of the present invention, the concentrated solution is selected from any one of a saturated solution of a ferrous alaninate chelate and a supersaturated solution of a ferrous alaninate chelate.
In a preferred embodiment of the present invention, the sedimentation ratio of the concentrate is not less than 50%, preferably not less than 60%, more preferably not less than 70%, still more preferably not less than 80%.
In the preferred technical scheme of the invention, the prepared concentrated solution is naturally cooled to normal temperature, preferably subjected to standing crystallization for 0.5-10 hours, more preferably subjected to standing crystallization for 1-8 hours, and even more preferably subjected to standing crystallization for 2-5 hours.
In the preferred technical scheme of the invention, the crystallization is cooling crystallization, preferably cooling standing crystallization, more preferably gradient cooling standing crystallization.
In the preferred technical scheme of the invention, the cooling times of the gradient cooling are not less than 2 times.
In the preferable technical scheme of the invention, the first cooling condition of gradient cooling is that the crystallization system is cooled to 35-55 ℃ in 0.5-3h, and the temperature is kept for 1-10h; preferably cooling to 40-50deg.C in 1.0-2.5 hr, and maintaining for 2-5 hr.
In the preferable technical scheme of the invention, the second cooling condition of gradient cooling is that the crystallization system is cooled to 5-35 ℃ in 0.5-24h, and the temperature is kept for 0.5-4h; preferably cooling to 10-30deg.C in 1.0-2.5 hr, and maintaining for 1-12 hr; more preferably 1.2-2.0h, cooling to 15-25 ℃, and preserving heat for 1.5-6h.
In a preferred technical scheme of the invention, the cooling is selected from any one or combination of natural cooling and forced cooling.
In the preferred technical scheme of the invention, the forced cooling adopts a cooling medium to realize forced cooling of the crystal system.
In a preferred embodiment of the present invention, the cooling medium is selected from any one of condensed water, ice water, ethanol, ethylene glycol, or a combination thereof.
In a preferred embodiment of the present invention, the separation is selected from any one of filtration, centrifugation, membrane treatment, or a combination thereof.
In the preferred technical scheme of the invention, after the separated concentrated mother liquor and the ferrous alanine chelate solution to be purified are uniformly mixed, the required amount of seed crystal is added and then the mixture is concentrated again to prepare ferrous alanine chelate crystals, wherein the volume ratio of the concentrated mother liquor to the treated clear liquid is 1:3-1:5.
in the preferred technical scheme of the invention, the concentrated mother solution obtained by separation is concentrated again to a sedimentation ratio of 50-60%, and then is stood for crystallization, so that the ferrous alanine chelate crystal is prepared.
In the preferred technical scheme of the invention, the concentrated mother liquor obtained by separation is concentrated again for at least 2 times.
In a preferred embodiment of the present invention, the collected solid is dried after washing, preferably the solvent used for the washing is water.
In a preferred embodiment of the present invention, the drying is selected from any one of vacuum drying, reduced pressure drying, normal pressure drying, spray drying, and boiling drying, or a combination thereof.
In a preferred embodiment of the present invention, the drying temperature is 25 to 80 ℃, preferably 35 to 70 ℃, more preferably 40 to 60 ℃.
In the preferred technical scheme of the invention, the bulk density of the prepared ferrous alanine chelate crystal is more than or equal to 0.70g/mL, preferably more than or equal to 0.80g/mL.
In a preferred embodiment of the present invention, the purity of the obtained ferrous alaninate chelate crystal is not less than 99.0%, preferably not less than 99.5%, more preferably not less than 99.7%.
In the preferred technical scheme of the invention, the water content of the prepared ferrous alanine chelate crystal is not more than 0.10%, preferably not more than 0.03%.
It is another object of the present invention to provide the use of ferrous alaninate chelates for the preparation of animal feed.
In a preferred embodiment of the present invention, the animal feed is selected from any one of chicken feed, duck feed, goose feed, pig feed, cow feed, rabbit feed, sheep feed, deer feed, camel feed.
In the preferred technical scheme of the invention, the animal feed is obtained by adding 0.01% -0.2% of ferrous alanine chelate in basic ration, and the addition amount of the ferrous alanine chelate in the animal feed is preferably 0.02% -0.06%.
In the preferred technical scheme, the basic ration is selected from any one of chicken basic ration, duck basic ration, goose basic ration, pig basic ration, cow basic ration, rabbit basic ration, sheep basic ration, deer basic ration and camel basic ration.
1. Unless otherwise indicated, the method for detecting chelation rate of the present invention
The chelation rate was determined by EDTA (disodium edetate) standard titration, as follows:
(1) Extracting inorganic metal ions in the sample by using methanol, and centrifugally separating supernatant and precipitate;
(2) 1g of precipitate was weighed, extracted with 25ml of absolute methanol, filtered, 0.1ml of filtrate was taken and 3ml of dithizone chloroform solution was added, and the sample was bluish green (dithizone color) and no red color was observed. If a red color appears, it indicates that free metal ions exist in the chelate;
(3) Titration of metal ions in the supernatant with EDTA solution, recording the volume of EDTA solution consumed by the titration as V 1 . After ashing the sample, titrating the total metal element in the sample by using EDTA solution, and recording the volume of the EDTA solution consumed by titration as V 2 。
(4) Sample chelation rate calculation formula:
wherein, the liquid crystal display device comprises a liquid crystal display device,
concentration of C-Standard EDTA (mol/L)
V 1 Titration of the volume (ml) of EDTA solution consumed by the free metallic element
V 2 -volume of EDTA solution (ml) consumed by titration of total amount of metallic elements
2. Unless otherwise indicated, the method for detecting rumen volatile fatty acids of the present invention
Taking 1mL of rumen fluid filtered by 4 layers of gauze, placing the rumen fluid into a 2mL centrifuge tube, adding 200uL of 25% metaphosphoric acid, uniformly mixing by vortex, centrifuging for 10min at 1000r/min, and loading the supernatant into a sample injection small bottle through a 0.45um filter membrane to be tested. The chromatographic conditions were as follows: chromatographic column: agilent DB-FFAP capillary column; column temperature: programming, namely raising the temperature to 190 ℃ at the initial temperature of 60 ℃ at the speed of 12.5 ℃/min, and keeping for 1min; sample inlet temperature: 220 ℃; detector temperature: 280 ℃; the carrier gas is high-purity nitrogen; constant pressure: 100Kpa; air flow rate: 400mL/min; nitrogen flow rate: 40mL/min; tail blow flow rate: 25mL/min; split sample injection mode, split ratio 30:1, sample injection amount: 1ul.
3. Unless otherwise indicated, the method for detecting the disappearance rate of cellulose according to the present invention
The test sample is dried and crushed and then passes through a 2mm sieve, a 3X 3 Latin square design is adopted, 10g of sample is accurately weighed, the sample is carefully put into a nylon bag with constant weight after drying, the nylon bag is fastened by nylon wires, one end of a soft plastic tube (50 cm in length) is tied, the rubber band is used for fixing, and the other end is tied and fixed on a rumen fistula so as to prevent falling. Each sample was taken out, rinsed with clear water, soaked until water clarified, then baked to constant weight at 65 ℃ and tested for dry matter a.
Accurately weighing 0.5-1.0g of the sample, putting into 100ml of neutral detergent (3% sodium dodecyl sulfate, PH=7), boiling for 1-2 hours, sleeving a glass funnel with 100-150 mesh nylon spun yarn, carrying out suction filtration, transferring filter residues into a weighed glass filter pot, washing for several times with hot water, carrying out vacuum suction filtration, removing part of water, putting into a 100 ℃ oven for drying, cooling in a dryer, and keeping constant weight to obtain the content B of neutral washed cellulose.
Accurately weighing 2.0-5.0g of the sample (crushed and passed through a 1 mm sieve opening), adding 100ml of acid detergent (20 g of hexadecyl trimethyl alkylated ammonia in 1L1.00N sulfuric acid) into a reflux container, heating to boiling within 5-10 minutes, refluxing for 1 hour, sleeving a glass funnel with 100-150 meshes of nylon spun yarn for suction filtration, transferring filter residues into a weighed glass filter pot (100-120 meshes of aperture), flushing with 50ml of hot water for several times each time, vacuum suction filtration, finally washing with acetone for 1-2 times, drying in a 100 ℃ oven, cooling, and keeping constant weight to obtain the content C of the acid washed cellulose.
Cellulose disappearance = (a-B-C)/a × 100%
Unless otherwise indicated, when the invention relates to a percentage between liquids, the percentages are volume/volume percentages; the invention relates to the percentage between liquid and solid, said percentage being volume/weight percentage; the invention relates to the percentage between solids and liquids, the percentage being weight/volume percentage; the balance being weight/weight percent.
Compared with the prior art, the invention has the following beneficial technical effects:
1. according to the invention, the antioxidant is added into the chelation system of the alanine and the ferrous salt, and the amino acid ferrous chelate is added as the seed crystal, so that the crystal quality, purity and chelation rate of the ferrous alanine chelate are obviously improved, and the production cost is obviously reduced.
2. The preparation method of the invention has the advantages of simple operation, obviously shortened production period and production cost, and suitability for large-scale industrialized production.
Drawings
FIG. 1 total volatile fatty acid content comparison;
fig. 2 cellulose disappearance ratio comparison.
Detailed Description
The present invention is described below with reference to examples, but the present invention is not limited to the examples.
Example 1Preparation of ferrous alanine chelate
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: ferrous sulfate: adding ferrous sulfate and Vc into the prepared alanine solution at a molar ratio of Vc of 1:1:0.04, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 5.0, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 2 hours at 70 ℃ to obtain a reaction solution;
(3) Adding 0.05% of ferrous alanine chelate into the reaction solution under the stirring condition;
(4) Adding 1L of ethanol with the concentration of 95% into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa < -0.095 > MPa) at 70 ℃ until a large amount of crystals are precipitated;
(5) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 70 ℃ to obtain ferrous alanine chelate.
The chelation rate is 93% when the detection method is adopted for detection.
Example 2Preparation of ferrous alanine chelate
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: ferrous sulfate: adding ferrous sulfate and citric acid into the prepared alanine solution according to the molar ratio of 2:1:0.06, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 5.5, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 3 hours at 80 ℃ to obtain a reaction solution;
(3) Adding 0.05% ferrous alanine chelate to the reaction solution under stirring;
(4) Adding 1L of 95% ethanol into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa < -0.095 > MPa) at 80 ℃ until a large amount of crystals are precipitated;
(5) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 80 ℃ to obtain ferrous alanine chelate.
The chelation rate is 95% when the detection method is adopted for detection.
Example 3Preparation of ferrous alanine chelate
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: ferrous sulfate: adding ferrous sulfate and iron powder into the prepared alanine solution according to the molar ratio of 3:1:0.04, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 6.0, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 3 hours at 90 ℃ to obtain a reaction solution;
(3) Adding 0.05% ferrous alanine chelate to the reaction solution under stirring;
(4) Adding 1L of 95% ethanol into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa-0.095 MPa) at 90 ℃ until a large amount of crystals are precipitated;
(5) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 90 ℃ to obtain ferrous alanine chelate.
The chelation rate is 97% when the detection method is adopted for detection.
Comparative example 1
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: adding ferrous sulfate and iron powder into the prepared alanine solution according to the molar ratio of ferrous sulfate of 3:1, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 6.0, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 3 hours at 90 ℃ to obtain a reaction solution;
(3) Adding 1L of 95% ethanol into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa-0.095 MPa) at 90 ℃ until a large amount of crystals are precipitated;
(4) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 90 ℃ to obtain ferrous alanine chelate.
The chelation rate is 80% when the detection method is adopted for detection.
Comparative example 2
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: adding ferrous sulfate and iron powder into the prepared alanine solution according to the molar ratio of ferrous sulfate to ascorbic acid of 3:1:0.04, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 6.0, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 3 hours at 90 ℃ to obtain a reaction solution;
(3) Adding 1L of ethanol with the concentration of 95% into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa < -0.095 > MPa) at 90 ℃ until a large amount of crystals are precipitated;
(4) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 90 ℃ to obtain ferrous alanine chelate.
The chelation rate is 87% when the detection method is adopted for detection.
Comparative example 3
(1) 267.3g alanine was dissolved in 3L water to prepare an alanine solution;
(2) According to alanine: adding ferrous sulfate and iron powder into the prepared alanine solution according to the molar ratio of ferrous sulfate of 3:1, adding an ammonia water solution under the stirring condition, adjusting the pH value of the reaction solution to be 6.0, placing the reaction solution in a nitrogen protection environment, and stirring and reacting for 3 hours at 90 ℃ to obtain a reaction solution;
(3) Adding 0.05% ferrous alanine chelate to the reaction solution under stirring;
(4) Adding 1L of ethanol with the concentration of 95% into the reaction solution prepared in the step (3), and vacuum concentrating (-0.085 MPa < -0.095 > MPa) at 90 ℃ until a large amount of crystals are precipitated;
(5) Pouring the crystallization solution prepared in the step (4) into a centrifuge, centrifuging for 1h, leaching with distilled water for 2 times, centrifuging for 1h, collecting wet product, and drying at 90 ℃ to obtain ferrous alanine chelate.
The chelation rate is 89% when the detection method is adopted for detection.
Example 4Alanine chelate ferrous chelateApplication in feed
The basic ration consists of the following components: 46% of corn, 15% of bean cake, 38.5% of bran, 5% of salt, 5% of stone powder and 0.02% of alanine chelated ferrous chelate prepared in example 2.
Example 5Application of alanine chelated ferrous chelate in feed
The basic ration consists of the following components: 46% of corn, 15% of bean cake, 38.5% of bran, 5% of salt, 5% of stone powder and 0.04% of alanine chelated ferrous chelate prepared in example 2.
Example 6Application of alanine chelated ferrous chelate in feed
The basic ration consists of the following components: 46% of corn, 15% of bean cake, 38.5% of bran, 5% of salt, 5% of stone powder and 0.06% of alanine chelated ferrous chelate prepared in example 2.
Example 7Application of alanine chelated ferrous chelate in feed
1. Materials and methods
1.1 laboratory animals and groups
The experiment uses 20 beef cattle (male 10, female 10, age 2 years, average weight 200 kg) with consistent health condition, and the beef cattle are divided into two groups at random. 10 heads of experimental group, male and female halves; control group 10 heads, male and female halves.
1.2 experimental period: for a total of 15 days.
1.3 Experimental feed
The experimental groups were fed daily the basal diet of examples 4-6. The control group was fed basal daily ration daily.
1.4 feeding management
Experiments were performed on beef cattle breeding bases in Bayan city. The temperature, humidity, ventilation intensity, carbon dioxide and ammonia concentration in the cowshed are automatically controlled, the temperature in the cowshed is gradually reduced from 37 ℃ to 24-26 ℃ during the test, and the experimental beef cattle eat and drink water freely. And cleaning the feces regularly and continuously illuminating. The cattle are sterilized once in two weeks during the feeding period, and the environment outside the cowshed is sterilized once.
1.5 sampling method and detection index
Samples were withdrawn every two hours from 8:00 to 20:00 per day at ruminal balloon sites during the experiment, and the results are shown in figures 1-2.
The above description of the embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various changes or modifications according to the present invention without departing from the spirit of the present invention, and shall fall within the scope of the claims of the present invention.
Claims (12)
1. The preparation method of the ferrous alanine chelate is characterized by comprising the following steps of: adding ferrous salt solution into alanine solution, chelating under the protection of acidic condition and inert gas, adding seed crystal for crystallization, concentrating, separating, and drying to obtain ferrous alanine chelate;
wherein, an antioxidant is also added in the chelation reaction; ferrous salt: the molar ratio of the antioxidant is 1:0.01-0.2; the antioxidant is selected from any one or combination of vitamin C, citric acid and iron powder;
the ferrous salt is selected from any one or a combination of more of ferrous sulfate, ferrous chloride, ferrous oxide and ferrous hydroxide;
the pH value of the chelation reaction is 5.0-6.0, and the temperature of the chelation reaction is 60-100 ℃.
2. The method of claim 1, wherein the alanine is selected from any one of L-alanine, D-alanine, a-alanine, β -alanine, DL-alanine, or a combination thereof.
3. The method of claim 1, wherein the chelating reaction is one of alanine: the molar ratio of the ferrous salt is 1-5:1.
4. the method of claim 1, wherein the pH of the chelation reaction is adjusted using an acid-base modifier selected from any one of sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, potassium bicarbonate, potassium carbonate, aqueous ammonia, or a combination thereof.
5. The method of claim 1, wherein the inert gas is any one of nitrogen, argon, or a combination thereof.
6. The method of claim 1, wherein the chelation reaction is for a period of 1 to 5 hours.
7. The method of claim 1, wherein the reaction solution is seeded with 0.001% to 0.2% ferrous alaninate chelate.
8. The method of claim 1, wherein the concentrating is selected from any one of vacuum concentrating, membrane concentrating, atmospheric concentrating, ultrafiltration concentrating, centrifugal concentrating, or a combination thereof.
9. The method of claim 1, wherein the separation is selected from any one of filtration, centrifugation, membrane treatment, or a combination thereof.
10. The method of claim 1, wherein the collected isolated solid is washed and dried.
11. The method of claim 1, wherein the drying is selected from any one of vacuum drying, reduced pressure drying, atmospheric pressure drying, spray drying, ebullient drying, or a combination thereof.
12. The method according to claim 1, wherein the obtained ferrous alaninate chelate is subjected to crystallization and purification treatment.
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