Preparation method and application of amino acid complex iron

Through the method of instant pressure relief of the autoclave and pretreatment of ferrous chloride tetrahydrate by sodium stearate, the odor emission and oxidation problems in the production process of amino acid complex iron are solved, and high chelation rate and low trivalent iron ion content are achieved, and the production environment friendliness and product stability is improved.

CN120441394AInactive Publication Date: 2025-08-08XINGJIA BIO ENG CO LTD
View PDF 9 Cites 0 Cited by

Patent Information

Application Number
CN202510960657.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-11
Publication Date
2025-08-08
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

There are problems of odor emission and environmental pollution in the production process of existing amino acid complex iron, and ferrous chloride is prone to oxidation, affecting the chelation rate and stability.

Method used

The method of instantaneous pressure relief of the autoclave and pretreatment of ferrous chloride tetrahydrate by sodium stearate is used to form porous particles, reducing the odor emission and improving chelation rate and stability.

Benefits of technology

The high chelation rate and low trivalent iron ion content of amino acid complex iron are achieved, which reduces odor pollution in the production process, and improves production environment friendship and product stability.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120441394A_ABST
    Figure CN120441394A_ABST
Patent Text Reader

Abstract

The invention discloses a preparation method and application of amino acid complex iron, pressure in a reaction kettle I is instantaneously relieved, steam in reaction product particles is instantaneously flushed out, due to instantaneous pressure relief, the steam position in the particles is not filled, mesopores are formed, porous particles are obtained, and if the pressure relief time is too long, the particles are not filled with the mesopores. Steam in the particles cannot instantly overflow, and pore structures in the particles collapse along with slow reduction of pressure and temperature in the reaction kettle I, so that porous particles cannot be obtained. According to the preparation method of the amino acid complex iron, sodium stearate is added in the high-pressure reaction process, steam can be formed along with water and enters product particles, and in the subsequent instant pressure relief process, the sodium stearate can reduce the surface tension of the water, so that ferrous chloride tetrahydrate particles are stably dispersed in the water; the formation of support product particle mesopores is facilitated, and the collapse of pore structures in the particles is prevented, so that the porous particles are obtained.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention belongs to the technical field of cell biology, and particularly relates to a preparation method of amino acid complexed iron and application thereof. Background Art

[0002] Amino acid iron complex (AACI) is a ring-shaped complex formed between a ligand (amino acid) and a metal ion (trace element). Common chelate rings include five-membered and six-membered rings. α-AACI iron chelates are five-membered, while β-AACI iron chelates are six-membered. When amino acids chelate trace elements, they form chelates with moderate stability constants. These chelates utilize amino acid absorption pathways in the small intestine, avoiding competition and antagonism with other mineral elements that flow through mineral ion absorption pathways. Furthermore, the chelates are biochemically more stable, effectively resisting adverse reactions with other nutrients in the diet. They are well soluble in the body, easily absorbed, and have high bioavailability. AACI iron chelates also possess certain antibacterial and immunomodulatory properties.

[0003] Currently, there are various methods for preparing synthetic amino acid chelated iron, and the main preparation methods include liquid phase method, microwave solid phase method and room temperature solid phase method.

[0004] For example, CN201010117932.6 discloses a method for producing amino acid chelated iron, comprising the following steps: a. hydrolyzing keratin with a strong acid to produce an amino acid solution; b. reacting a carbonate and / or bicarbonate with a strong acid ferrous salt solution to obtain a precipitate, adding an appropriate amount of iron powder, and then adding the amino acid solution prepared in step a to react, adjusting the solution pH to 2.5-5.5; c. filtering, concentrating, and drying the filtrate to produce amino acid chelated iron.

[0005] For example, CN201210391260.7 discloses a method for preparing a modified amino acid chelated iron feed additive, which adopts the acid enzyme method. Feather powder is first hydrolyzed with 20% to 35% sulfuric acid at 100°C to 105°C for 1h to 2h to completely dissolve the feather powder; after cooling, ferrous chloride tetrahydrate is added, and then sodium hydroxide solution is added to neutralize, and the pH value is adjusted to 6.0 to 6.5. The mixture is reacted at 100°C to 105°C for 5h to 6h; after the reaction, the mixture is cooled to 45°C, an appropriate amount of biological enzyme is added, and the mixture is reacted for 10h to 12h, and vinegar, montmorillonite powder, polyethylene glycol 4000 and poplar bark powder are added to the reaction solution. Finally, the mixture is concentrated and dried to obtain a modified amino acid chelated iron feed additive.

[0006] Iron has physiological functions in plants, such as participating in the body's redox reaction, synthesizing chlorophyll and respiration. Iron deficiency in plants will lead to growth stunting. It is generally believed that Fe 2+ It is the main form of plant absorption, but when Fe is sprayed directly on the leaves 2+When Fe 2+ Chelating with amino acids to form a stable complex can achieve better application results. If amino acid chelated iron fertilizers are not fully chelated, the superiority of this type of fertilizer will be affected to a certain extent. Furthermore, the body can only absorb divalent iron, so iron supplements are all divalent iron. However, since divalent iron is easily oxidized to trivalent iron, it is more susceptible to oxidation during the production process than other trace elements, which is also a difficult problem to deal with in production. Summary of the Invention

[0007] In view of the problem that most amino acids used in the production of amino acid complexes in the prior art are plant or animal by-product protein hydrolysates, which are hydrolyzed into small-molecule peptides and amino acids, but the protein hydrolysates generally have an unpleasant smell, and it is inevitable that odor will be emitted during the production process, polluting the air, and often accompanied by waste liquid discharge, which seriously pollutes the environment, the present invention provides a preparation method and application of amino acid complex iron. By studying the main influencing factors affecting the odor emission during the preparation of the complex, the complexation rate is used as an indicator to screen out the optimal complexation process conditions, so as to improve the complexation rate of the composite amino acid and iron and avoid the cost increase caused by unnecessary production processes in production, thereby providing a reference basis for the production of composite amino acid complex micro-fertilizers.

[0008] The technical solutions of the present invention are as follows: The preparation method of amino acid complex iron of the present invention comprises four steps: preparation of mixed amino acid liquid, preparation of ferrous chloride tetrahydrate reaction liquid, preparation of amino acid complex iron, and drying and crushing.

[0009] The purpose of the present invention is achieved through the following technical solutions: A method for preparing amino acid complexed iron comprises the following steps: S1. Preparation of mixed amino acid liquid: First, the composite amino acid and pure water are mixed according to a solid-liquid ratio of 1: (8-10), the pH is adjusted to neutral, and a high-pressure reaction is performed. The mass ratio of the composite amino acid to pure water is 1: (1.5-2.0), the pressure of the high-pressure reaction is controlled at 0.3MPa-0.8MPa, the reaction temperature is controlled at 120°C-130°C, and the reaction time is 0.5h-1.0h; after the high-pressure reaction is completed, the reactor I of the high-pressure reaction is instantly depressurized for 1s-3s to obtain a mixed amino acid dissolved liquid. The dissolved liquid is passed through a filter to remove impurities, and then sent to a concentration tank for concentration, and concentrated to a solid content of the amino acid liquid of 20%-28% to obtain a mixed amino acid liquid; S2. Preparation of ferrous chloride tetrahydrate reaction solution: Mix ferrous chloride tetrahydrate and purified water and place them in a reactor I, then add sodium stearate equivalent to 0.5%-1.0% of the mass of purified water, heat to 30°C-32°C, and react for 1h-2h to obtain a ferrous chloride tetrahydrate reaction solution; S3, preparation of amino acid complex iron: the ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 are placed in a reactor II and mixed, stirred, the temperature of the mixed liquid in the reactor II is raised to 75°C-85°C, the mass ratio of the solid content of ferrous chloride tetrahydrate and the mixed amino acid liquid is 1:(2.5-3.5), the pH value of the liquid in the reactor II is controlled to be 5.5-6.5, the reaction time is 1.5h-2h, and after the reaction is completed, the temperature is cooled to room temperature; S4, drying and crushing: the reactants in the S3 reactor II are sent to a concentration reactor for concentration. The concentrated material is dried and then crushed to obtain amino acid complexed iron with a porous particle size of 300 μm-600 μm and a porosity of 60%-70%. The obtained amino acid complexed iron has a chelation rate of 97.24%-98.86% and a trivalent iron ion content of 0.15%-0.22%.

[0010] In the present invention: Furthermore, the mass ratio of the composite amino acid described in S1 to pure water is 1:2.0.

[0011] The pressure of the high-pressure reaction in S1 is controlled at 0.3-0.8 MPa. Controlling the appropriate pressure increases the reaction speed and is also beneficial for the water in the container to form steam and enter the product particles. If the pressure is too low, the steam cannot smoothly enter the interior of the particles. If the pressure is too high, it is not conducive to the formation of particles, the particle size of the product particles is reduced, and the performance of the product is reduced. Preferably, the pressure is controlled at 0.4 MPa, 0.5 MPa, or 0.6 MPa.

[0012] As described in S1, the reactor I of the high-pressure reaction is instantly depressurized. By instantly releasing the pressure in the closed reaction vessel, the steam in the reaction product particles is instantly rushed out. Due to the instantaneous pressure relief, the steam positions in the particles are not filled, forming mesopores, thereby obtaining porous particles. If the pressure relief time is too long, the steam in the particles cannot overflow instantly. As the pressure and temperature in the reaction vessel slowly decrease, the pore structure in the particles collapses, and porous particles cannot be obtained.

[0013] Furthermore, the solid-liquid ratio described in S1 is 1:8, and the solid content of the concentrated amino acid liquid is 25%.

[0014] The complex amino acids in S1 are purchased from the market, and their components and contents are as follows:

[0015] In S2, the mass ratio of ferrous chloride tetrahydrate to pure water is controlled to be 1:(1.5-2.0). Adding an appropriate amount of water, on the one hand, reduces the viscosity of the reactants, facilitates the uniform mixing of the reactants, and helps to improve the yield. On the other hand, the reaction in reactor I provides sufficient steam pressure, which is conducive to the formation of mesopores. If the amount of water added is too low, the mixing effect is reduced and sufficient steam cannot be provided. If the amount of water added is too high, the concentration of the reactants is reduced, which will reduce the reaction speed. Moreover, if the amount of water is too much, the steam generated is large, which is not conducive to the control of the reaction pressure and is even more unfavorable for the subsequent instantaneous pressure relief.

[0016] Furthermore, the mass ratio of the solid content of the ferrous chloride tetrahydrate and the mixed amino acid liquid described in S3 is 1:3.0.

[0017] Furthermore, the drying in S4 is carried out by oven drying at a temperature of 70° C.-80° C. and a reaction time of 8 h-12 h.

[0018] The amino acid complex iron described in S4 has a porous particle size of 300μm-600μm and a porosity of 60%-70%. The high-pressure reaction is instantaneously depressurized to control the particle size of the porous particles to 300μm-600μm, thereby increasing the particle size of the product particles, which is beneficial to improving the fluidity of the product and reducing the wall adhesion of the product. At the same time, it can effectively reduce the amount of dust during production and use, and provide a clean working environment. Further preferably, the particle size is 400μm-600μm.

[0019] At the same time, the present invention also relates to the application of the amino acid complex iron obtained by the above-mentioned method for preparing amino acid complex iron, specifically for preparing amino acid complex iron nanoassemblies. The prepared amino acid complex iron nanoassemblies have good biocompatibility and stability and can be efficiently internalized by cells. For example, certain amino acid-iron nanoassemblies can simulate the activity of peroxidase (POD) and glutathione oxidase (GSHOx) to generate reactive oxygen species (ROS) to enhance the therapeutic effect.

[0020] Compared with the prior art, the present invention has the following beneficial effects: 1. The preparation method of the amino acid complex iron described in the present invention is to instantly release the pressure in the reactor I, so that the steam in the reaction product particles rushes out instantly. Due to the instantaneous pressure relief, the steam position in the particles is not filled, forming mesopores, thereby obtaining porous particles. If the pressure relief time is too long, the steam in the particles cannot overflow instantly. As the pressure and temperature in the reactor I slowly decrease, the pore structure in the particles collapses, and porous particles cannot be obtained.

[0021] 2. The preparation method of the amino acid complex iron described in the present invention comprises the following steps: by adding sodium stearate during the high-pressure reaction, sodium stearate will form steam with water and enter the product particles. During the subsequent instantaneous pressure relief process, sodium stearate will reduce the surface tension of water, so that the ferrous chloride particles are stably dispersed in the water, which is beneficial to supporting the formation of mesopores in the product particles and preventing the collapse of the pore structure in the particles, thereby obtaining porous particles. The chelation rate of the obtained amino acid complex iron is 97.24%-98.86%, and the trivalent iron ion content is 0.15%-0.22%.

[0022] 3. Currently, most amino acids used in the production of amino acid complexes are plant or animal by-product protein hydrolysates, which are hydrolyzed into small-molecule peptides and amino acids. However, protein hydrolysates generally have an unpleasant smell. In the subsequent production process, the protein hydrolysates will emit an odor, polluting the air, and are often accompanied by waste liquid discharge, which seriously pollutes the environment. The present invention uses composite amino acids to obtain porous particles of ferrous chloride by pre-treating ferrous chloride tetrahydrate. The ferrous chloride particles have abundant mesopores. During the preparation of amino acid complex iron, the amino acids in the mixed amino acid liquid of the porous particles can fully wrap the ferrous chloride, thereby reducing the odor during the production of the mixed amino acid liquid and making the production environment more friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings are used to provide further understanding of the present invention and constitute a part of the specification. They are used to explain the present invention together with the embodiments of the present invention and do not constitute a limitation of the present invention.

[0024] Figure 1 This is a surface micrograph of the amino acid complexed iron prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0025] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0026] Example 1: A method for preparing amino acid complexed iron comprises the following steps: S1. Preparation of mixed amino acid liquid: First, the composite amino acid and purified water were mixed at a solid-liquid ratio of 1:8, the pH was adjusted to neutral, and the mixture was heated to 30°C and reacted for 2 hours to obtain a dissolved solution. The dissolved solution was filtered to remove impurities, and then sent to a concentration tank for concentration until the solid content of the amino acid liquid reached 20%. The solution was then sent to a decolorization reactor for decolorization to obtain a mixed amino acid liquid. The components and contents of the composite amino acids are shown in Table 1: Table 1: Components and contents of complex amino acids

[0027] S2, preparation of ferrous chloride tetrahydrate reaction solution: ferrous chloride tetrahydrate and pure water are mixed and put into reactor 1, and then sodium stearate equivalent to 0.5% of water mass is added, and high pressure reaction is carried out, the mass ratio of described ferrous chloride tetrahydrate and pure water is 1:2.0, the pressure of high pressure reaction is controlled at 0.3MPa, the reaction temperature is controlled at 120 ℃, and the reaction time is 1.0h; after the high pressure reaction is completed, the reactor 1 of high pressure reaction is instantly depressurized for 1s-3s to obtain ferrous chloride tetrahydrate reaction solution;

[0028] S3, preparation of amino acid complex iron: the ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 were placed in a reactor II and mixed, stirred, and the temperature of the mixed liquid in the reactor II was raised to 75 ° C. The mass ratio of the solid content of ferrous chloride tetrahydrate and the mixed amino acid liquid was 1:2.5. The pH value of the liquid in the reactor II was controlled to be 5.5, the reaction time was 1.5 h, and after the reaction was completed, the temperature was cooled to room temperature; S4, drying and crushing: the reactants in the reactor II of S3 are sent to a concentration reactor for concentration, and the concentrated materials are dried and then crushed to obtain amino acid complexed iron with porous particles having a particle size of 300 μm-600 μm and a porosity of 60%-70%.

[0029] Figure 1 This is a surface micrograph of the amino acid complexed iron prepared in Example 1.

[0030] Example 2: A method for preparing amino acid complexed iron comprises the following steps: S1. Preparation of mixed amino acid liquid: First, the composite amino acid and purified water were mixed at a solid-liquid ratio of 1:10, the pH was adjusted to neutral, and the mixture was heated to 30°C and reacted for 1 hour to obtain a dissolved solution. The dissolved solution was filtered to remove impurities, and then sent to a concentration tank for concentration until the solid content of the amino acid liquid reached 28%. The solution was then sent to a decolorization reactor for decolorization to obtain a mixed amino acid liquid. The components and contents of the composite amino acid are the same as those in Example 1; S2, preparation of ferrous chloride tetrahydrate reaction solution: ferrous chloride tetrahydrate and pure water were mixed and placed in a reactor 1, and then sodium stearate equivalent to 1.0% of the water mass was added to carry out high-pressure reaction, the mass ratio of the ferrous chloride tetrahydrate to the pure water was 1:1.5, the pressure of the high-pressure reaction was controlled at 0.8MPa, the reaction temperature was controlled at 130°C, and the reaction time was 0.5h; after the high-pressure reaction was completed, the reactor 1 of the high-pressure reaction was instantly depressurized for 1s-3s to obtain a ferrous chloride tetrahydrate reaction solution; S3, preparation of amino acid complex iron: the ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 were placed in a reactor II and mixed, stirred, and the temperature of the mixed liquid in the reactor II was raised to 85° C., the mass ratio of the solid content of ferrous chloride tetrahydrate and the mixed amino acid liquid was 1:3.5, the pH value of the liquid in the reactor II was controlled to be 6.0, the reaction time was 2 h, and after the reaction was completed, the temperature was cooled to room temperature; S4, drying and crushing: the reactants in the reactor II of S3 are sent to a concentration reactor for concentration, and the concentrated materials are dried and then crushed to obtain amino acid complexed iron with porous particles having a particle size of 300 μm-600 μm and a porosity of 60%-70%.

[0031] Example 3: A method for preparing amino acid complexed iron comprises the following steps: S1. Preparation of mixed amino acid liquid: First, the composite amino acid and purified water were mixed at a solid-liquid ratio of 1:9, the pH was adjusted to neutral, and the mixture was heated to 31° C. and reacted for 1.5 hours to obtain a dissolved solution. The dissolved solution was filtered to remove impurities, and then sent to a concentration tank for concentration until the solid content of the amino acid liquid reached 25%. The solution was then sent to a decolorization reactor for decolorization to obtain a mixed amino acid liquid. The components and contents of the composite amino acid are the same as those in Example 1; S2, preparation of ferrous chloride tetrahydrate reaction solution: ferrous chloride tetrahydrate and pure water are mixed and put into reactor 1, and then sodium stearate equivalent to 0.6% of water mass is added, and high pressure reaction is carried out, the mass ratio of described ferrous chloride tetrahydrate and pure water is 1:1.8, the pressure of high pressure reaction is controlled at 0.4MPa, the reaction temperature is controlled at 125 DEG C, and the reaction time is 1.0h; after the high pressure reaction is completed, the reactor 1 of high pressure reaction is instantly depressurized for 1s-3s to obtain ferrous chloride tetrahydrate reaction solution; S3, preparation of amino acid complex iron: the ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 were placed in a reactor II and mixed, stirred, and the temperature of the mixed liquid in the reactor II was raised to 80° C., the mass ratio of the solid content of ferrous chloride tetrahydrate and the mixed amino acid liquid was 1:3.0, the pH value of the liquid in the reactor II was controlled to be 6.5, the reaction time was 1.5 h, and after the reaction was completed, the temperature was cooled to room temperature; S4, drying and crushing: the reactants in the reactor II of S3 are sent to a concentration reactor for concentration, and the concentrated materials are dried and then crushed to obtain amino acid complexed iron with porous particles having a particle size of 300 μm-600 μm and a porosity of 60%-70%.

[0032] Example 4: A method for preparing amino acid complexed iron comprises the following steps: S1. Preparation of mixed amino acid liquid: First, the composite amino acid and purified water were mixed at a solid-liquid ratio of 1:8, the pH was adjusted to neutral, and the mixture was heated to 30°C and reacted for 2 hours to obtain a dissolved solution. The dissolved solution was filtered to remove impurities, and then sent to a concentration tank for concentration until the solid content of the amino acid liquid reached 28%. The solution was then sent to a decolorization reactor for decolorization to obtain a mixed amino acid liquid. The components and contents of the composite amino acid are the same as those in Example 1; S2, preparation of ferrous chloride tetrahydrate reaction solution: ferrous chloride tetrahydrate and pure water were mixed and placed in a reactor 1, and then sodium stearate equivalent to 1.0% of the water mass was added to carry out high-pressure reaction, the mass ratio of the ferrous chloride tetrahydrate to the pure water was 1:2.0, the pressure of the high-pressure reaction was controlled at 0.6 MPa, the reaction temperature was controlled at 120 ° C, and the reaction time was 0.5 h; after the high-pressure reaction was completed, the reactor 1 of the high-pressure reaction was instantly depressurized for 1s-3s to obtain a ferrous chloride tetrahydrate reaction solution; S3, Preparation of amino acid complex iron: The ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 were placed in a reactor II and mixed, stirred, and the temperature of the mixed liquid in the reactor II was raised to 75° C. The mass ratio of the solid content of the ferrous chloride tetrahydrate and the mixed amino acid liquid was 1:3.5. The pH value of the liquid in the reactor II was controlled to be 5.5, the reaction time was 2 h, and after the reaction was completed, the temperature was cooled to room temperature; S4, drying and crushing: the reactants in the reactor II of S3 are sent to a concentration reactor for concentration, and the concentrated materials are dried and then crushed to obtain amino acid complexed iron with porous particles having a particle size of 300 μm-600 μm and a porosity of 60%-70%.

[0033] Comparative Example 1: The difference between Comparative Example 1 and Example 1 is that sodium stearate is not added to S2, and the other conditions are the same as those of Example 1; The prepared amino acid complex iron has a particle size of 600-1000 μm and a porosity of 20-30%.

[0034] Comparative Example 2: The difference between Comparative Example 2 and Example 1 is that the preparation of the ferrous chloride tetrahydrate reaction solution in S2 is omitted, and the ferrous chloride tetrahydrate is directly mixed with the mixed amino acid liquid prepared in S1. Other differences are the same as in Example 1; Since the mixed amino acid liquid of S1 generally has an unpleasant smell, the protein hydrolyzate will emit an odor during the subsequent production process. If ferrous chloride tetrahydrate is directly added to the mixed amino acid liquid for a mixed reaction, the ferrous chloride tetrahydrate cannot encapsulate the amino acids in the mixed amino acid liquid, and a strong odor will be emitted during the production process.

[0035] Performance testing: The obtained products were tested for total iron content and free iron ion content, and the chelation rate / %=[(total iron content-free iron ion content) / total iron content]×100.

[0036] Table 2: Chelation rate of amino acid chelated iron in Examples and Comparative Examples

[0037] Table 3: Content of trivalent iron ions in amino acid chelated iron of Examples and Comparative Examples

[0038] Results and Discussion 1. By comparison of the embodiment and comparative example 1, in comparative example 1, sodium stearate was not added in the pretreatment of ferrous chloride tetrahydrate, and sodium stearate was not added during the high-pressure reaction. In the subsequent instantaneous pressure relief process, the lack of sodium stearate formed steam with water and entered the product particles, and could not reduce the surface tension of water, resulting in an unstable distribution of ferrous chloride particles in water, which is not conducive to supporting the formation of mesopores in the product particles, nor is it conducive to preventing the collapse of the pore structure in the particles, and no porous particles are obtained.

[0039] 2. By comparison of the embodiment and comparative example 2, the amino acids currently used for the production of amino acid complexes are mostly plant or animal by-product protein hydrolysates, which are hydrolyzed into small molecule peptides and amino acids. However, the protein hydrolysate generally has an unpleasant smell. In the subsequent production process, the protein hydrolysate will emit an odor, polluting the air, and is often accompanied by waste liquid discharge, which seriously pollutes the environment. The present invention obtains porous particles of ferrous chloride by pre-treating ferrous chloride tetrahydrate. The porous particles of ferrous chloride have abundant mesopores. In the preparation process of amino acid complex iron, the ferrous chloride of the porous particles can fully wrap the amino acids in the mixed amino acid liquid, thereby reducing the odor in the production process of the mixed amino acid liquid, and the production environment is more friendly.

[0040] 3. As can be seen from Table 3, by comparing the examples and the comparative examples, the trivalent iron ion content of the amino acid chelated iron in the examples is lower than that of the amino acid chelated iron in the comparative example, indicating that the amino acid chelated iron prepared in the examples is not easily oxidized and has good product stability.

[0041] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing amino acid complexed iron, characterized in that: The following steps are involved: S1. Preparation of mixed amino acid liquid: first, the composite amino acid and purified water are mixed at a solid-liquid ratio of 1:(8-10), the pH is adjusted to neutral, and a high-pressure reaction is performed. The mass ratio of the composite amino acid to purified water is 1:(1.5-2.0), the pressure of the high-pressure reaction is controlled at 0.3MPa-0.8MPa, the reaction temperature is controlled at 120°C-130°C, and the reaction time is 0.5h-1.0h; after the high-pressure reaction is completed, the high-pressure reaction reactor I is instantly depressurized for 1s-3s to obtain a mixed amino acid dissolved liquid; the dissolved liquid is filtered to remove impurities, and then sent to a concentration tank for concentration, and concentrated to a solid content of the amino acid liquid of 20%-28% to obtain a mixed amino acid liquid; S2. Preparation of ferrous chloride tetrahydrate reaction solution: Mix ferrous chloride tetrahydrate and purified water and place them in a reactor I, then add sodium stearate equivalent to 0.5%-1.0% of the mass of purified water, heat to 30°C-32°C, and react for 1h-2h to obtain a ferrous chloride tetrahydrate reaction solution; S3, preparation of amino acid complex iron: the ferrous chloride tetrahydrate reaction solution obtained in S2 and the mixed amino acid liquid obtained in S1 are placed in a reactor II and mixed, stirred, the temperature of the mixed liquid in the reactor II is raised to 75°C-85°C, the mass ratio of the solid content of ferrous chloride tetrahydrate and the mixed amino acid liquid is 1:(2.5-3.5), the pH value of the liquid in the reactor II is controlled to be 5.5-6.5, the reaction time is 1.5h-2h, and after the reaction is completed, the temperature is cooled to room temperature; S4, drying and crushing: the reactants in the S3 reactor II are sent to a concentration reactor for concentration. The concentrated material is dried and then crushed to obtain amino acid complexed iron with a porous particle size of 300 μm-600 μm and a porosity of 60%-70%. The obtained amino acid complexed iron has a chelation rate of 97.24%-98.86% and a trivalent iron ion content of 0.15%-0.22%.

2. The method for preparing an amino acid complexed iron according to claim 1, wherein: The mass ratio of the composite amino acid to pure water described in S1 is 1:2.0, and the pressure of the high-pressure reaction is controlled at 0.4 MPa, 0.5 MPa, and 0.6 MPa.

3. The method for preparing an amino acid complexed iron according to claim 1, wherein: The components and contents of the complex amino acids described in S1 are as follows: Asp is 5.71%, Ile is 0.14%, Thr is 4.37%, Leu is 0.12%, Ser is 7.90%, Tyr is 0.38%, Glu is 8.61%, Phe is 0.21%, Gly is 4.65%, His is 0.58%, Ala is 3.43%, Lys is 1.97%, Cys is 1.06%, Arg is 0.38%, Val is 2.57%, Pro is 6.17%, and Met is 0.22%.

4. The method for preparing an amino acid complexed iron according to claim 1, wherein: The solid-to-liquid ratio in S1 is 1:8, and the solid content of the concentrated amino acid liquid is 25%.

5. The method for preparing an amino acid complexed iron according to claim 1, wherein: The mass ratio of the solid content of the ferrous chloride tetrahydrate and the mixed amino acid liquid described in S3 is 1:3.

0.

6. The method for preparing an amino acid complexed iron according to claim 1, wherein: The drying in S4 is carried out by oven drying at a temperature of 70° C. to 80° C. and a reaction time of 8 h to 12 h.

7. The method for preparing an amino acid complexed iron according to claim 1, wherein: The amino acid complexed iron described in S4 has a particle size of 400 μm-600 μm.

8. Use of the amino acid complex iron obtained by the preparation method of the amino acid complex iron according to any one of claims 1 to 7, characterized in that: Used to prepare amino acid complexed iron nanoassemblies.

Citation Information

Patent Citations

  • Method for producing amino acid chelate iron

    CN101786962B

  • Method for preparing modified amino acid chelated iron feed additive

    CN102948609B

  • Method for producing amino acid chelate iron

    CN101786962A

  • Method for preparing modified amino acid chelated iron feed additive

    CN102948609A

  • Preparation method of amino acid chelated iron for fertilizers

    CN106747868A