Preparation method of stable amino acid-ferrous complex

A technology of amino acid ferrous and complexes, applied in the preparation of sulfide, organic chemistry, etc., can solve the problem of removing impurity ions and dissolved oxygen in water, stability control of amino acid ferrous products, and increasing ferrous Difficulty and workload of anti-oxidation, to reduce the risk of ferrous oxidation, ensure high ferrous quality, and ensure the effect of anti-oxidation function

Active Publication Date: 2019-08-16
LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (1) The preparation process of using water as a solvent does not consider the removal of impurity ions and dissolved oxygen in water, which increases the difficulty and workload of ferrous anti-oxidation in the subsequent preparation process
[0012] (2) There are problems in the selection or use of antioxidants, such as: the use of heterogeneous antioxidants such as hydroxylamine hydrochloride and ascorbic acid to bring into the final product affects product quality; when iron powder is used as a reducing agent, there is a need to filter out unreacted iron powder and recycle iron The iron powder is difficult to use or the iron powder is preferentially contacted with acid or stronger acid to cause consumption without actual reduction; the above problems directly affect the quality and stability of the final product
[0013] (3) The stability control of subsequent links such as storage, transportation and use of amino acid ferrous products is not considered (Chinese patent CN107118115 adds maltodextrin with 10-50% glycine weight to prevent moisture absorption during storage and transportation, but there are problems described above , and it does not help the stability when used as a feeding material)
[0014] (4) Some product preparation methods also produce salty wastewater

Method used

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  • Preparation method of stable amino acid-ferrous complex
  • Preparation method of stable amino acid-ferrous complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of ferrous methionine complex: Add 602.02kg of industrial desalted water (conductivity 2.8us / cm) into a 2000L reactor, then raise the temperature to 95°C, keep it warm for 30~60min, and then inject nitrogen gas for 5~15min at the same time, analyze The residual amount of oxygen in the water was not detected. Then add 301.01kg of DL-methionine crystals (2000 moles) with a content of 99wt% and 310.02kg (2000 moles) of anhydrous ferrous sulfate with a content of 98wt%, stir and dissolve completely, add reduced iron powder 0.448kg (8 moles), and Keep warm at 40~95°C for 20~60min, add 3.41kg (20mol) of additive 2-hydroxy-4-methylthiobutyric acid, adjust the pH of the reaction solution to 2~5, digest the residual reduced iron powder, and stir for 10~30min , to obtain DL-methionine complex ferrous salt aqueous solution, the concentration of DL-methionine complex ferrous salt in the aqueous solution is 49.7wt%.

[0038] Spray drying treatment of ferrous methionine ...

Embodiment 2

[0040] Preparation of ferrous glycinate complex: add 451.52kg of industrial desalted water (conductivity 3.2us / cm) into a 2000L reactor, then raise the temperature to 95°C, keep it warm for 30~60min, and pass nitrogen gas for 5~15min at the same time in the later stage, and analyze the water Residual amount of oxygen, not detected. Then add 151.66kg of glycine crystals (2000 moles) with a content of 99wt% and 573.22kg (2000 moles) of ferrous sulfate heptahydrate with a content of 97wt%, stir and dissolve completely, add reduced iron powder 0.448kg (8 moles), at 40~ Insulate at 95°C for 20-60 minutes, add 2.56 kg (15 moles) of auxiliary agent 2-hydroxy-4-methylthiobutyric acid, adjust the pH of the reaction solution to 2-5, digest the residual reduced iron powder, and stir for 10-30 minutes to obtain The aqueous solution of the ferrous glycinate complex, the concentration of the ferrous glycinate complex in the aqueous solution is 45.53wt%.

[0041] Spray drying treatment of f...

Embodiment 5

[0047] Stability Test 1:

[0048] When ferrous ions exist as stable complexes and chelates, they are not easily oxidized whether in solid state or in aqueous solution, but the free ferrous ions are easily oxidized to ferric iron by air or oxygen in solution. , ferrous iron is oxidized and consumed, which further promotes the analysis to go forward, resulting in the consumption of ferrous iron complexes and the conversion of ferrous iron to unusable ferric iron. The experiment mainly tracks the analysis reaction of the product to judge its stability by measuring the content of ferric iron in the solution.

[0049] Take 20g of the ferrous complexes obtained in Examples 1, 2, 3, and 4 and transfer them into 100ml beakers, add 20ml of normal temperature deoxidized deionized water, stir and dissolve them, record them as groups A, B, C, and D, and place them on the operating table , respectively at 10min, 60min, and 90min, sample and analyze the content of ferric iron in each group...

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Abstract

The invention discloses a preparation method of a stable amino acid-ferrous complex. The amino acid-ferrous complex is prepared from optimized amino acid and a ferrous salt according to a molar ratioof 1:1 in the presence of iron powder under the condition of a water system. An auxiliary agent is used to achieve the effects of regulating the pH value, digesting the iron powder, and carrying out secondary complexation or chelating on free ferrous, so that after the obtained reaction liquid is subjected to spray drying, the stable amino acid-ferrous complex is obtained. A high-level ferrous content and a low-level oxidation rate (ferric iron content) are achieved, and relatively good antioxidant capacity is achieved in a water solution, so that excellent stability is exhibited, oxidation resistance of a ferrous complex product in a storage and transportation process is improved, and efficient utilization of the ferrous product is facilitated. According to the preparation process of themethod, the steps of filtering the iron powder and digesting the iron powder by adding inorganic acid are optimized, no three wastes (waste gas, waste water and industrial residue) are generated, cleaning can be carried out continuously, and in addition, the used auxiliary agent can also provide favorable nutritional ingredients.

Description

technical field [0001] The invention belongs to the field of organic compound synthesis, and in particular relates to a preparation method of a stable ferrous amino acid complex. Background technique [0002] Ferrous iron is an essential trace element for humans and animals. It is a component of hemoglobin. If it is deficient in food or feed, it will cause iron deficiency anemia in animals. Traditionally, inorganic salts of ferrous iron are used as feed additives, which are unstable during the addition process and are easily oxidized. Animals need to pass through various biological barriers for absorption and utilization. The absorption efficiency is low, the addition amount is large, and the biological potency is low. Most of them are excreted through feces, which has the disadvantages of polluting the environment. [0003] Amino acid ferrous complexes or chelates are single five-membered ring ferrous complexes formed by ferrous ions forming coordination bonds with amino g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C323/58
CPCC07C319/20C07C323/58
Inventor 周荣超廖常福彭启明
Owner LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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