CN111777523A - Preparation method of glycine iron chelate - Google Patents
Preparation method of glycine iron chelate Download PDFInfo
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- CN111777523A CN111777523A CN202010512873.6A CN202010512873A CN111777523A CN 111777523 A CN111777523 A CN 111777523A CN 202010512873 A CN202010512873 A CN 202010512873A CN 111777523 A CN111777523 A CN 111777523A
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- glycine
- ferrous sulfate
- iron
- crystalline solid
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- 239000013522 chelant Substances 0.000 title claims abstract description 22
- LPOSZYSKJWFIQH-UHFFFAOYSA-N 2-aminoacetic acid;iron Chemical compound [Fe].NCC(O)=O LPOSZYSKJWFIQH-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 29
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 29
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 29
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 29
- 239000004471 Glycine Substances 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000008394 flocculating agent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 29
- 229910052742 iron Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- GIPOFCXYHMWROH-UHFFFAOYSA-L 2-aminoacetate;iron(2+) Chemical compound [Fe+2].NCC([O-])=O.NCC([O-])=O GIPOFCXYHMWROH-UHFFFAOYSA-L 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 17
- 239000013078 crystal Substances 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000011573 trace mineral Substances 0.000 abstract description 4
- 235000013619 trace mineral Nutrition 0.000 abstract description 4
- 239000003337 fertilizer Substances 0.000 abstract description 3
- 238000001953 recrystallisation Methods 0.000 abstract description 3
- 238000005189 flocculation Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract description 2
- AKLSSKNRPSKJBO-UHFFFAOYSA-K 2-aminoacetate;iron(3+) Chemical compound [Fe+3].NCC([O-])=O.NCC([O-])=O.NCC([O-])=O AKLSSKNRPSKJBO-UHFFFAOYSA-K 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 235000015097 nutrients Nutrition 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000004255 Butylated hydroxyanisole Substances 0.000 description 3
- 235000019282 butylated hydroxyanisole Nutrition 0.000 description 3
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical group COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 3
- 229940043253 butylated hydroxyanisole Drugs 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of a glycine iron chelate, which is used for improving the preparation method of the glycine iron chelate, belongs to the technical field of trace element fertilizers, and comprises the following steps: (1) dissolving ferrous sulfate in distilled water, adding antioxidant, and filtering with semipermeable membrane; (2) dissolving glycine in distilled water, adding a filtered ferrous sulfate solution and a catalyst, reacting, cooling and crystallizing to obtain a crystalline solid; (3) dissolving the crystallized solid, adding a flocculating agent, stirring, standing and collecting supernatant; (4) carrying out gradient cooling on the supernatant to obtain a crystalline solid, and drying to obtain a glycine iron chelate; according to the invention, impurities in the raw materials can be removed by filtering the raw materials through the semipermeable membrane, the influence on the uniformity of the formed crystal form and the purity of the product is avoided, and meanwhile, the ferric glycinate crystal is obtained by flocculation sedimentation and gradient cooling recrystallization, so that the purity is high, the impurity content is low, the crystal form uniformity is good, and the product stability and quality are high.
Description
Technical Field
A preparation method of glycine iron chelate belongs to the technical field of trace element fertilizers, and particularly relates to preparation of iron-containing chelate.
Background
During the growth of plants, in order to maintain the metabolic process of the plants, a certain amount of nutrient elements need to be continuously absorbed from the outside to maintain the normal operation of the organism, and the nutrient elements can be divided into a large amount of nutrient elements and trace nutrient elements according to the absorption amount of the plants. The micronutrients mainly comprise iron, manganese, boron, zinc, copper, molybdenum, chlorine and nickel, wherein the iron plays an important role in chlorophyll synthesis, oxidation reduction and electron transfer in plants and respiration of the plants, so that a proper amount of iron nutrition supplement is necessary for ensuring the requirement of cell tissues of the plants on iron, particularly for the plants growing on iron-deficient soil.
Fe3+The solubility is very low under the condition of high pH value, most plants are difficult to utilize, and Fe2+The chelated iron is a main form absorbed by plants and is easy to be absorbed by the plants, and particularly, the iron glycinate chelate is prepared by chelating iron elements by taking amino acid as a carrier and is used as a trace element fertilizer, so that the plants can better absorb iron, the utilization rate of the iron elements is improved, and accurate and efficient supplement of the trace elements is realized.
However, in the existing production process of iron glycinate chelate, ferrous sulfate is usually used as an iron source, the raw material usually contains more impurities, such as some insoluble substances, metals such as lead, bismuth, thallium and titanium, and toxic organic substances such as polychlorinated biphenyl and dioxin, which seriously affect the purity, safety, stability and crystal uniformity of the produced product, and meanwhile, in the production process of iron glycinate chelate, divalent iron is very easily oxidized in aqueous solution to generate Fe (OH)3Precipitation, which causes yellowing of the product, seriously affects the appearance and quality of the product, reduces the yield of the product and increases the content of impurities, and in order to solve the problems, the preparation method of the ferrous glycinate chelate is provided.
Disclosure of Invention
The invention aims to: the preparation method of the iron glycinate chelate is provided, impurities in the raw materials can be removed by filtering the raw materials through a semipermeable membrane, the influence on the uniformity of the formed crystal form and the purity of the product is avoided, and meanwhile, the iron glycinate crystal is obtained through flocculation sedimentation and gradient cooling recrystallization, so that the purity is high, the impurity content is low, the uniformity of the crystal form is good, and the product stability and quality are high.
The technical scheme adopted by the invention is as follows:
in order to achieve the above object, the present invention provides a method for preparing an iron glycinate chelate, comprising the steps of:
(1) dissolving ferrous sulfate in distilled water, adding antioxidant, and filtering with semipermeable membrane;
(2) dissolving glycine in distilled water, adding a filtered ferrous sulfate solution and a catalyst, adjusting the pH to 3.5-5.0, reacting at 50-70 ℃ for 0.8-1.2 h, cooling for crystallization, and separating to obtain a crystalline solid;
(3) adding the crystallized solid into distilled water at 50-70 ℃ for dissolving, adding a flocculating agent, stirring for 30-60 min, standing, and collecting a supernatant; wherein, the flocculating agent can be any one or more of polyacrylamide, polyoxyethylene and lignin;
(4) and (4) carrying out gradient cooling on the supernatant to recrystallize the supernatant to obtain a crystalline solid again, and drying the crystalline solid to obtain the glycine iron chelate.
Preferably, the catalyst is acetic acid.
Preferably, the antioxidant is BHA (butylated hydroxyanisole).
Preferably, the molar ratio of the ferrous sulfate to the antioxidant is (1.5-3) to 1.
Preferably, the molar ratio of the glycine to the ferrous sulfate is (1-3) to 1.
Preferably, the molar ratio of the glycine to the catalyst is 1 (0.002-0.01).
Preferably, the gradient temperature reduction in the step (4) is that: and under the condition of stirring, cooling at the speed of 1 ℃ every 5 minutes until the temperature is reduced to 5-10 ℃, and then stopping cooling.
Preferably, in the step (4), the crystalline solid is washed with anhydrous ethanol at least 2 times after obtaining the crystalline solid. The impurities are removed by washing with ethanol, so that the product purity is higher, the dispersibility is better, the water content is reduced, the energy consumption is saved for the subsequent drying process, the washed washing liquid is rectified by a rectifying tower, and the ethanol is separated and recovered for recycling, therefore, the invention has the beneficial effects that by adopting the technical scheme:
1. the invention firstly dissolves ferrous sulfate in distilled water and adds antioxidant, and then filters the solution through a semipermeable membrane, and the addition of the antioxidant can prevent ferrous iron from being oxidized in aqueous solution to generate Fe (OH)3The deposition, the semipermeable membrane can play the effect of filtration edulcoration to the ferrous sulfate raw materials, gets rid of insoluble substance, heavy metal, the organic matter of big group etc. that contains in the raw materials, avoids influencing the stability of follow-up crystallization process, avoids influencing crystal form homogeneity and the product purity that forms.
2. According to the invention, the crystallized solid is dissolved in water, then the flocculating agent is added, the impurities are settled out, and the obtained supernatant is recrystallized again, so that the purity of the product can be greatly improved.
3. According to the invention, the recrystallization is carried out by adopting a gradient cooling mode, so that the stability of the crystal in the forming process is increased, the uniformity of the crystal form is favorably improved, and the forming quality is better.
4. According to the invention, the impurities are further removed by washing the crystals with ethanol, so that the product purity is higher, the dispersibility is better, the water content is reduced, and the energy consumption is saved for the subsequent drying process.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of an iron glycinate chelate, which comprises the following steps:
(1) dissolving ferrous sulfate in distilled water and adding into antioxidant BHA, and filtering through semipermeable membrane; wherein the molar ratio of the ferrous sulfate to the antioxidant is 1.5: 1;
(2) dissolving glycine in distilled water, adding a filtered ferrous sulfate solution and a catalyst acetic acid, adjusting the pH to 3.5-5.0, reacting at 50-70 ℃ for 0.8-1.2 h, cooling for crystallization, and separating to obtain a crystalline solid; wherein, the mol ratio of the glycine to the ferrous sulfate is 1: 1, and the mol ratio of the glycine to the catalyst is 1: 0.005;
(3) adding the crystallized solid into distilled water at 50-70 ℃ for dissolving, adding a flocculating agent, stirring for 30-60 min, standing, and collecting a supernatant; wherein, the flocculating agent can be any one or more of polyacrylamide, polyoxyethylene and lignin;
(4) and (3) carrying out gradient cooling on the supernatant, namely cooling the supernatant at a cooling speed of 1 ℃ every 5 minutes under the stirring condition until the temperature is reduced to 5-10 ℃, stopping cooling, obtaining a crystalline solid again, washing the crystalline solid for 3 times by using absolute ethyl alcohol, and drying to obtain the glycine iron chelate.
Example 2
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 2: 1; the mol ratio of the glycine to the ferrous sulfate is 2: 1, and the mol ratio of the glycine to the catalyst is 1: 0.002.
Example 3
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 2.5: 1; the molar ratio of the glycine to the ferrous sulfate is 3: 1, and the molar ratio of the glycine to the catalyst is 1: 0.008.
Example 4
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 3: 1; the mol ratio of the glycine to the ferrous sulfate is 2: 1, and the mol ratio of the glycine to the catalyst is 1: 0.01.
Example 5
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 2: 1; the molar ratio of the glycine to the ferrous sulfate is 3: 1, and the molar ratio of the glycine to the catalyst is 1: 0.01.
Example 6
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 2.5: 1; the mol ratio of the glycine to the ferrous sulfate is 2: 1, and the mol ratio of the glycine to the catalyst is 1: 0.005.
Example 7
The difference between the present example and example 1 is that the molar ratio of ferrous sulfate to antioxidant in the present example is 3: 1; the mol ratio of the glycine to the ferrous sulfate is 2: 1, and the mol ratio of the glycine to the catalyst is 1: 0.005.
The components of the product are detected, and the product of the invention is iron (Fe)2+Calculated) is more than or equal to 27.2 percent; the total glycine is more than or equal to 57.8 percent; free glycine is less than or equal to 0.7 percent, Fe3+The product quality is not more than 0.08%, and other detection data are shown in the table I.
Table one, product inspection data of the present invention
As can be seen from the table I, the product prepared by the invention has the advantages of low impurity content, high purity and Fe3+Low content, high quality, low water content and high quality.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; these modifications and substitutions do not cause the essence of the corresponding technical solution to depart from the scope of the technical solution of the embodiments of the present invention, and are intended to be covered by the claims and the specification of the present invention.
Claims (8)
1. The preparation method of the glycine iron chelate is characterized by comprising the following steps of:
(1) dissolving ferrous sulfate in distilled water, adding antioxidant, and filtering with semipermeable membrane;
(2) dissolving glycine in distilled water, adding a filtered ferrous sulfate solution and a catalyst, adjusting the pH to 3.5-5.0, reacting at 50-70 ℃ for 0.8-1.2 h, cooling for crystallization, and separating to obtain a crystalline solid;
(3) adding the crystallized solid into distilled water at 50-70 ℃ for dissolving, adding a flocculating agent, stirring for 30-60 min, standing, and collecting a supernatant;
(4) and (4) carrying out gradient cooling on the supernatant to recrystallize the supernatant to obtain a crystalline solid again, and drying the crystalline solid to obtain the glycine iron chelate.
2. The method of claim 1, wherein the catalyst is acetic acid.
3. The method of claim 1, wherein the antioxidant is BHA.
4. The method for preparing the iron glycinate chelate according to claim 1, wherein the molar ratio of the ferrous sulfate to the antioxidant is (1.5-3) to 1.
5. The method for preparing the iron glycinate chelate according to claim 1, wherein the molar ratio of the glycine to the ferrous sulfate is (1-3) to 1.
6. The method for preparing the iron chelate of glycine according to claim 1, wherein the molar ratio of glycine to the catalyst is 1 (0.002-0.01).
7. The method for preparing the iron glycinate chelate according to claim 1, wherein the gradient temperature reduction in the step (4) is as follows: and under the condition of stirring, cooling at the speed of 1 ℃ every 5 minutes until the temperature is reduced to 5-10 ℃, and then stopping cooling.
8. The method of claim 1, wherein in the step (4), the crystalline solid is washed at least 2 times with absolute ethanol after obtaining the crystalline solid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115786045A (en) * | 2022-12-02 | 2023-03-14 | 量准（上海）医疗器械有限公司 | Laboratory nucleic acid pollution scavenger and application thereof |
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