WO2022215983A1 - Structure nano-composite d'oxyde métallique et son procédé de formation - Google Patents

Structure nano-composite d'oxyde métallique et son procédé de formation Download PDF

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WO2022215983A1
WO2022215983A1 PCT/KR2022/004817 KR2022004817W WO2022215983A1 WO 2022215983 A1 WO2022215983 A1 WO 2022215983A1 KR 2022004817 W KR2022004817 W KR 2022004817W WO 2022215983 A1 WO2022215983 A1 WO 2022215983A1
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metal oxide
nanocomposite structure
solution
aqueous solution
precursor
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Korean (ko)
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현택환
김영건
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서울대학교산학협력단
기초과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0072—Mixed oxides or hydroxides containing manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224—Oxides or hydroxides of lanthanides
    • C01F17/235—Cerium oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0054—Mixed oxides or hydroxides containing one rare earth metal, yttrium or scandium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
    • C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
    • C07K14/76—Albumins
    • C07K14/765—Serum albumin, e.g. HSA
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/08—Ingredients agglomerated by treatment with a binding agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L89/00—Compositions of proteins; Compositions of derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • the present invention relates to a metal oxide nanocomposite structure and a method for forming the same.
  • the present invention provides a metal oxide nanocomposite structure having excellent performance.
  • the present invention provides a method of forming a metal oxide nanocomposite structure.
  • the metal oxide nanocomposite structure includes a metal oxide nanostructure and a ligand compound coupled to the metal oxide nanostructure.
  • the metal oxide nanostructure may include at least one of metal oxide nanoclusters and metal oxide nanoparticles.
  • the metal oxide nanostructure may include at least one of a single metal oxide nanostructure and a multimetal oxide nanostructure.
  • the single metal oxide nanostructure may include one of cerium, manganese, and iron
  • the multimetal oxide nanostructure may include two or more of cerium, manganese, and iron.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be dispersed in the polymer compound.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be surrounded by the polymer compound.
  • the ligand compound may include at least one of polysaccharide and albumin.
  • the ligand compound may include at least one of a hydroxyl group and a carboxyl group.
  • the type of the ligand compound may be determined according to the type of the metal oxide.
  • a method of forming a metal oxide nanocomposite structure includes forming a precursor solution including a metal precursor and a ligand compound, and adding a base to the precursor solution to form a metal oxide nanocomposite structure includes
  • the metal oxide nanocomposite structure includes a metal oxide nanostructure and a ligand compound bonded to the metal oxide nanostructure.
  • the metal of the metal precursor may be precipitated by the addition of the base to form the metal oxide nanostructure.
  • the metal oxide nanostructure may include at least one of metal oxide nanoclusters and metal oxide nanoparticles.
  • the metal precursor may include at least one of a cerium precursor, a manganese precursor, and an iron precursor.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be dispersed in the polymer compound.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be surrounded by the polymer compound.
  • the ligand compound may include at least one of polysaccharide and albumin.
  • the ligand compound may include at least one of a hydroxyl group and a carboxyl group.
  • the type of the ligand compound may be determined according to the type of the metal oxide.
  • the method of forming the metal oxide nanocomposite structure may further include separating the metal oxide nanocomposite structure from the precursor solution using a membrane filter.
  • the precursor solution may be an aqueous solution.
  • the base may include at least one of NH 4 OH and KOH.
  • Metal oxide nanocomposite structures according to embodiments of the present invention may have excellent performance.
  • the metal oxide nanocomposite structure may have excellent biocompatibility and antioxidant performance.
  • the metal oxide nanocomposite structure can be formed in large quantities in a simple method in water without using an organic solvent.
  • FIG 1 and 2 are views for explaining a method of forming a metal oxide nanocomposite structure according to embodiments of the present invention.
  • 3 to 5 show the results of analyzing the performance of the metal oxide nanocomposite structure (CeMn/HSA) according to an embodiment of the present invention.
  • 6 to 8 show the results of analyzing the performance of the metal oxide nanocomposite structure according to embodiments of the present invention.
  • the metal oxide nanocomposite structure may be expressed as A/B.
  • A represents a metal oxide nanostructure
  • B represents a ligand compound bound to A.
  • Ce/HSA Ce represents a cerium oxide nanostructure
  • HSA albumin, which is a ligand compound bound to the cerium oxide nanostructure.
  • Mn/DEX Mn represents a manganese oxide nanostructure
  • DEX dextran, which is a ligand compound bound to the manganese oxide nanostructure.
  • Fe/HSA-DEX Fe represents an iron oxide nanostructure
  • HSA-DEX represents albumin and dextran, which are ligand compounds bound to the manganese oxide nanostructure.
  • CeMn/HSA CeMn represents a double metal oxide nanostructure including Ce and Mn
  • HSA albumin, which is a ligand compound bound to the double metal oxide nanostructure.
  • MnFe/DEX MnFe represents a double metal oxide nanostructure including Mn and Fe
  • DEX dextran, which is a ligand compound bonded to the double metal oxide nanostructure.
  • CeFe/HSA-DEX represents a double metal oxide nanostructure including Ce and Fe
  • HSA-DEX represents albumin and dextran, which are ligand compounds bound to the double metal oxide nanostructure.
  • FIG 1 and 2 are views for explaining a method of forming a metal oxide nanocomposite structure according to embodiments of the present invention.
  • the method of forming a metal oxide nanocomposite structure includes forming a precursor solution (S10), forming a metal oxide nanocomposite structure (S20), and separating the metal oxide nanocomposite structure It may include a step (S30).
  • a precursor solution including a metal precursor and a ligand compound is formed (S10).
  • the metal precursor may include at least one of a Ce precursor, a Mn precursor, and an Fe precursor.
  • the type of the metal precursor included in the precursor solution may be determined according to the type of metal oxide included in the metal oxide nanocomposite structure to be formed. For example, when the metal oxide nanocomposite structure includes cerium oxide and manganese oxide, the metal precursor may include a Ce precursor and a Mn precursor, and when the metal oxide nanocomposite structure includes cerium oxide and iron oxide
  • the metal precursor may include a Ce precursor and an Fe precursor.
  • the Ce precursor may include CeCl 3 or CeNO 3
  • the Mn precursor may include MnCl 2
  • the Fe precursor may include FeCl 2 .
  • the ligand compound may include a polymer compound.
  • the high molecular compound may include at least one of polysaccharide and albumin.
  • the polysaccharide may include dextran (DEX)
  • the albumin may include human serum albumin (HSA).
  • the ligand compound may include at least one of a hydroxyl group and a carboxyl group.
  • the type of the ligand compound included in the precursor solution may be determined according to the type of metal oxide included in the metal oxide nanocomposite structure to be formed.
  • a base is added to the precursor solution to form a metal oxide nanocomposite structure (S20).
  • the metal of the metal precursor may be precipitated by the addition of the base to the precursor solution to form a metal oxide nanostructure, and finally a metal oxide nanocomposite structure may be formed.
  • the base may include at least one of NH 4 OH and KOH.
  • the metal oxide nanocomposite structure is separated from the precursor solution using a membrane filter (S30).
  • washing may be performed using a centrifugal filter.
  • the metal precursor, ligand compound, and base remaining in the precursor solution (precursor solution after washing) are removed using the membrane filter, and only the metal oxide nanocomposite structure can be easily extracted.
  • the metal oxide nanocomposite structure includes a metal oxide nanostructure and a ligand compound bonded to the metal oxide nanostructure.
  • the metal oxide nanostructure may include at least one of metal oxide nanoclusters and metal oxide nanoparticles.
  • the metal oxide nanostructure may exist in an amorphous state, a crystalline state, or a mixed state of amorphous and crystalline.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be dispersed in the polymer compound.
  • the ligand compound may include a polymer compound, and the metal oxide nanostructure may be surrounded by the polymer compound.
  • the metal oxide nanocomposite structure may include one or more metal oxide nanostructures, and the metal oxide nanostructure and the ligand compound may have various bonding forms. The bonding form of the metal oxide nanostructure and the ligand compound may be controlled by the type and concentration of the metal precursor, the type and concentration of the ligand compound, the type and concentration of the base, the reaction time, and the like.
  • the metal oxide nanostructure may include at least one of a single metal oxide nanostructure and a multimetal oxide nanostructure.
  • the metal oxide nanocomposite structure may include a single metal oxide nanostructure, and when the precursor solution includes two or more metal precursors, the metal oxide nanocomposite structure includes multiple It may include a metal oxide nanostructure.
  • the metal oxide nanocomposite structure may include a double metal oxide nanostructure including Ce and Mn, and when the precursor solution includes a Ce precursor and a Fe precursor The metal oxide nanocomposite structure may include a double metal oxide nanostructure containing Ce and Fe, and when the precursor solution includes a Mn precursor and an Fe precursor, the metal oxide nanocomposite structure includes Mn and Fe It may include a double metal oxide nanostructure.
  • the metal oxide nanocomposite structure may include a triple metal oxide nanostructure including Ce, Mn, and Fe.
  • the multi-metal oxide nanostructure may be formed by co-precipitating two or more metals in Ce, Mn, and Fe.
  • the multi-metal oxide formed through the co-precipitation reaction has various oxidation states (Oxygen state), unlike when only one type of metal is precipitated, and the oxygen vacancy increases so that electron movement is active. happens to happen That is, the multi-metal oxide nanostructure may have improved active oxygen decomposition performance and improved antioxidant performance through co-precipitation of two or more of Ce, Mn, and Fe.
  • the degree of dispersion is important. Even when high-performance nanomaterials are synthesized, if agglomeration occurs in PBS, serum, and blood used in actual clinical practice other than distilled water, the active site on the surface of the nanomaterial is reduced, thereby reducing commercial value. In the metal oxide nanocomposite structure, a ligand compound is defective in the metal oxide nanostructure, thereby preventing aggregation of the metal oxide nanostructure and increasing dispersibility.
  • the metal oxide nanocomposite structure has an electron repulsion force and a steric interference effect to maintain the dispersion degree of the metal oxide nanostructure in an aqueous solution having various ionic strengths.
  • it may have biocompatibility.
  • polysaccharides such as dextran can effectively prevent aggregation of metal oxide nanostructures by increasing the steric interference effect even with respect to multi-metal oxides (CeMnO x , CeFeO x , MnFeO x , CeMnFeO x ).
  • CeCl 3 ⁇ 7H 2 O aqueous solution.
  • CeNO 3 ⁇ 6H 2 O may be used.
  • Albumin Human Serum Albumin, HSA
  • HSA Human Serum Albumin
  • Ce/HSA includes cerium oxide nanostructures and albumin bound to the cerium oxide nanostructures.
  • the cerium oxide nanostructure may include at least one of cerium oxide nanoclusters and cerium oxide nanoparticles.
  • the solution containing Ce/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate Ce/HSA.
  • CeCl 3 ⁇ 7H 2 O aqueous solution instead of CeCl 3 ⁇ 7H 2 O, CeNO 3 ⁇ 6H 2 O may be used.
  • Dextran (DEX) powder 200mg is dissolved in 5ml of distilled water to form an aqueous solution of dextran.
  • CeCl 3 ⁇ 7H 2 O aqueous solution and dextran aqueous solution are mixed to form a precursor aqueous solution.
  • Ce/DEX includes cerium oxide nanostructures and dextran bound to the cerium oxide nanostructures.
  • the cerium oxide nanostructure may include at least one of cerium oxide nanoclusters and cerium oxide nanoparticles.
  • the solution containing Ce/DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate Ce/DEX.
  • CeCl 3 ⁇ 7H 2 O aqueous solution instead of CeCl 3 ⁇ 7H 2 O, CeNO 3 ⁇ 6H 2 O may be used. 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution. CeCl 3 ⁇ 7H 2 O aqueous solution and albumin-dextran aqueous solution are mixed to form a precursor aqueous solution.
  • Ce/HSA-DEX contains cerium oxide nanostructures and albumin and dextran bound to the cerium oxide nanostructures.
  • the cerium oxide nanostructure may include at least one of cerium oxide nanoclusters and cerium oxide nanoparticles.
  • the solution containing Ce/HSA-DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate Ce/HSA-DEX.
  • aqueous solution Prepare 0.1M MnCl 2 ⁇ 4H 2 O aqueous solution. 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution. A precursor aqueous solution is formed by mixing an aqueous solution of MnCl 2 ⁇ 4H 2 O and an aqueous albumin solution.
  • Mn/HSA metal oxide nanocomposite structure
  • Mn/HSA includes manganese oxide nanostructures and albumin bound to the manganese oxide nanostructures.
  • the manganese oxide nanostructure may include at least one of manganese oxide nanoclusters and manganese oxide nanoparticles.
  • the solution containing Mn/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate Mn/HSA.
  • aqueous solution Prepare 0.1M MnCl 2 ⁇ 4H 2 O aqueous solution. Dissolve 200 mg of dextran powder in 5 ml of distilled water to form an aqueous solution of dextran. A precursor aqueous solution is formed by mixing an aqueous MnCl 2 ⁇ 4H 2 O solution and an aqueous dextran solution.
  • Mn/DEX metal oxide nanocomposite structure
  • the solution containing Mn/DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate Mn/DEX.
  • MnCl 2 ⁇ 4H 2 O aqueous solution 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution. MnCl 2 ⁇ 4H 2 O aqueous solution and albumin-dextran aqueous solution are mixed to form a precursor aqueous solution.
  • Mn/HSA-DEX metal oxide nanocomposite structure
  • Mn/HSA-DEX includes manganese oxide nanostructures and albumin and dextran bound to the manganese oxide nanostructures.
  • the manganese oxide nanostructure may include at least one of manganese oxide nanoclusters and manganese oxide nanoparticles.
  • Mn/HSA-DEX The solution containing Mn/HSA-DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter. Mn/HSA-DEX is separated by filtering the washed solution with a 0.22 ⁇ m membrane filter.
  • aqueous solution Prepare 0.1M FeCl 2 ⁇ 4H 2 O aqueous solution. 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution. A precursor aqueous solution is formed by mixing an aqueous solution of FeCl 2 ⁇ 4H 2 O and an aqueous albumin solution.
  • Fe/HSA includes iron oxide nanostructures and albumin bound to the iron oxide nanostructures.
  • the iron oxide nanostructure may include at least one of iron oxide nanoclusters and iron oxide nanoparticles.
  • the solution containing Fe/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate Fe/HSA.
  • Fe/DEX includes iron oxide nanostructures and dextran bound to the iron oxide nanostructures.
  • the iron oxide nanostructure may include at least one of iron oxide nanoclusters and iron oxide nanoparticles.
  • the solution containing Fe/DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate Fe/DEX.
  • Fe/HSA-DEX includes manganese oxide nanostructures and albumin and dextran bound to the iron oxide nanostructures.
  • the iron oxide nanostructure may include at least one of iron oxide nanoclusters and iron oxide nanoparticles.
  • the solution containing Fe/HSA-DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate Fe/HSA-DEX.
  • the amounts of the CeCl 3 ⁇ 7H 2 O aqueous solution and the MnCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Mn can be adjusted.
  • 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution.
  • An aqueous solution of CeMn and an aqueous solution of albumin are mixed to form a precursor aqueous solution.
  • CeMn/HSA includes a double metal oxide nanostructure including Ce and Mn and albumin bound to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeMn/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate CeMn/HSA.
  • the amounts of the CeCl 3 ⁇ 7H 2 O aqueous solution and the MnCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Mn can be adjusted.
  • An aqueous solution of CeMn and an aqueous solution of dextran are mixed to form a precursor aqueous solution.
  • CeMn/DEX includes a double metal oxide nanostructure including Ce and Mn and dextran bonded to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeMn/DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate CeMn/DEX.
  • the amounts of the CeCl 3 ⁇ 7H 2 O aqueous solution and the MnCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Mn can be adjusted.
  • 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution.
  • An aqueous solution of CeMn and an aqueous solution of albumin-dextran are mixed to form an aqueous precursor solution.
  • CeMn/HSA-DEX includes a double metal oxide nanostructure including Ce and Mn, and albumin and dextran bound to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeMn/HSA-DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate CeMn/HSA-DEX.
  • the amounts of the MnCl 2 ⁇ 4H 2 O aqueous solution and the FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Mn contained in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution.
  • a precursor aqueous solution is formed by mixing an aqueous MnFe solution and an aqueous albumin solution.
  • MnFe/HSA metal oxide nanocomposite structure
  • MnFe/HSA includes a double metal oxide nanostructure including Mn and Fe, and albumin bound to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing MnFe/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate MnFe/HSA.
  • the amounts of the MnCl 2 ⁇ 4H 2 O aqueous solution and the FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Mn contained in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • a precursor aqueous solution is formed by mixing an aqueous MnFe solution and an aqueous dextran solution.
  • MnFe/DEX metal oxide nanocomposite structure
  • MnFe/DEX includes a double metal oxide nanostructure including Mn and Fe and dextran bonded to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • MnFe/DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter. MnFe/DEX is separated by filtering the washed solution with a 0.22 ⁇ m membrane filter.
  • the amounts of the MnCl 2 ⁇ 4H 2 O aqueous solution and the FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted, and Mn contained in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution.
  • a precursor aqueous solution is formed by mixing an aqueous MnFe solution and an aqueous albumin-dextran solution.
  • MnFe/HSA-DEX metal oxide nanocomposite structure
  • MnFe/HSA-DEX includes a double metal oxide nanostructure including Mn and Fe, and albumin and dextran bonded to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing MnFe/HSA-DEX is washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate MnFe/HSA-DEX.
  • the amount of CeCl 3 ⁇ 7H 2 O aqueous solution and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted in consideration of the ratio of Ce 3+ and Fe 2+ in the CeFe aqueous solution, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution.
  • An aqueous solution of CeFe and an aqueous solution of albumin are mixed to form an aqueous precursor solution.
  • CeFe/HSA includes a double metal oxide nanostructure including Ce and Fe, and albumin bound to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeFe/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate CeFe/HSA.
  • the amount of CeCl 3 ⁇ 7H 2 O aqueous solution and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted in consideration of the ratio of Ce 3+ and Fe 2+ in the CeFe aqueous solution, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • a precursor aqueous solution is formed by mixing the CeFe aqueous solution and the dextran aqueous solution.
  • CeFe/DEX includes a double metal oxide nanostructure including Ce and Fe, and dextran bonded to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeFe/DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate CeFe/DEX.
  • the amount of CeCl 3 ⁇ 7H 2 O aqueous solution and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted in consideration of the ratio of Ce 3+ and Fe 2+ in the CeFe aqueous solution, and Ce included in the metal oxide nanocomposite structure formed thereby The amount and ratio of and Fe can be adjusted.
  • 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution.
  • An aqueous solution of the precursor is formed by mixing an aqueous solution of CeFe and an aqueous albumin-dextran solution.
  • CeFe/HSA-DEX includes a double metal oxide nanostructure including Ce and Fe, and albumin and dextran bonded to the double metal oxide nanostructure.
  • the double metal oxide nanostructure may include at least one of double metal oxide nanoclusters and double metal oxide nanoparticles.
  • the solution containing CeFe/HSA-DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate CeFe/HSA-DEX.
  • CeMnFe aqueous solution is formed by mixing 167 ⁇ l of CeCl 3 ⁇ 7H 2 O aqueous solution, 167 ⁇ l of MnCl 2 ⁇ 4H 2 O aqueous solution, and 167 ⁇ l of FeCl 2 ⁇ 4H 2 O aqueous solution.
  • the amounts of CeCl 3 ⁇ 7H 2 O aqueous solution, MnCl 2 ⁇ 4H 2 O aqueous solution, and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted by considering the ratio of Ce 3+ , Mn 2+ , and Fe 2+ in the CeMnFe aqueous solution, , it is possible to control the amount and ratio of Ce, Mn, and Fe included in the metal oxide nanocomposite structure formed by this.
  • 200 mg of albumin powder is dissolved in 5 ml of distilled water to form an aqueous albumin solution.
  • a precursor aqueous solution is formed by mixing an aqueous solution of CeMnFe and an aqueous albumin solution.
  • CeMnFe/HSA includes a triple metal oxide nanostructure including Ce, Mn, and Fe, and albumin bound to the triple metal oxide nanostructure.
  • the triple metal oxide nanostructure may include at least one of a triple metal oxide nanocluster and a triple metal oxide nanoparticle.
  • the solution containing CeMnFe/HSA was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution was filtered with a 0.22 ⁇ m membrane filter to separate CeMnFe/HSA.
  • CeMnFe aqueous solution is formed by mixing 167 ⁇ l of CeCl 3 ⁇ 7H 2 O aqueous solution, 167 ⁇ l of MnCl 2 ⁇ 4H 2 O aqueous solution, and 167 ⁇ l of FeCl 2 ⁇ 4H 2 O aqueous solution.
  • the amounts of CeCl 3 ⁇ 7H 2 O aqueous solution, MnCl 2 ⁇ 4H 2 O aqueous solution, and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted by considering the ratio of Ce 3+ , Mn 2+ , and Fe 2+ in the CeMnFe aqueous solution, , it is possible to control the amount and ratio of Ce, Mn, and Fe included in the metal oxide nanocomposite structure formed by this.
  • An aqueous solution of a precursor is formed by mixing an aqueous solution of CeMnFe and an aqueous solution of dextran.
  • CeMnFe/DEX includes a triple metal oxide nanostructure including Ce, Mn, and Fe, and dextran bonded to the triple metal oxide nanostructure.
  • the triple metal oxide nanostructure may include at least one of a triple metal oxide nanocluster and a triple metal oxide nanoparticle.
  • the solution containing CeMnFe/DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered through a 0.22 ⁇ m membrane filter to separate CeMnFe/DEX.
  • CeMnFe aqueous solution is formed by mixing 167 ⁇ l of CeCl 3 ⁇ 7H 2 O aqueous solution, 167 ⁇ l of MnCl 2 ⁇ 4H 2 O aqueous solution, and 167 ⁇ l of FeCl 2 ⁇ 4H 2 O aqueous solution.
  • the amounts of CeCl 3 ⁇ 7H 2 O aqueous solution, MnCl 2 ⁇ 4H 2 O aqueous solution, and FeCl 2 ⁇ 4H 2 O aqueous solution can be adjusted by considering the ratio of Ce 3+ , Mn 2+ , and Fe 2+ in the CeMnFe aqueous solution, , it is possible to control the amount and ratio of Ce, Mn, and Fe included in the metal oxide nanocomposite structure formed by this.
  • 100 mg of albumin powder and 100 mg of dextran powder are dissolved in 5 ml of distilled water to form an albumin-dextran aqueous solution.
  • a precursor aqueous solution is formed by mixing an aqueous solution of CeMnFe and an aqueous albumin-dextran solution.
  • CeMnFe/HSA-DEX includes a triple metal oxide nanostructure including Ce, Mn, and Fe, and albumin and dextran bonded to the triple metal oxide nanostructure.
  • the triple metal oxide nanostructure may include at least one of a triple metal oxide nanocluster and a triple metal oxide nanoparticle.
  • the solution containing CeMnFe/HSA-DEX was washed 4 times with distilled water at 5,000 rpm for 10 minutes using a 100 kDa centrifugal filter.
  • the washed solution is filtered with a 0.22 ⁇ m membrane filter to separate CeMnFe/HSA-DEX.
  • 3 to 5 show the results of analyzing the performance of the metal oxide nanocomposite structure (CeMn/HSA) according to an embodiment of the present invention.
  • 3 shows the results of the cytotoxicity analysis of CeMn/HSA
  • FIG. 4 shows the results of the antioxidant performance analysis of CeMn/HSA
  • FIG. 5 shows the results of the biodegradability analysis of CeMn/HSA.
  • CM75 represents a double metal oxide nanocomposite structure having a Ce:Mn content ratio of 75:25
  • CM50 represents a double metal oxide nanocomposite structure having a Ce:Mn content ratio of 50:50
  • CM25 is A double metal oxide nanocomposite structure having a Ce:Mn content ratio of 25:75 is shown.
  • the cytotoxicity of the double metal oxide nanocomposite structure containing Ce and Mn is similar to or smaller than the cytotoxicity of the single metal oxide nanocomposite structure containing only Ce or Mn.
  • the antioxidant performance of the double metal oxide nanocomposite structure containing Ce and Mn is superior to the antioxidant performance of the single metal oxide nanocomposite structure containing only Ce or Mn.
  • the biodegradability of the double metal oxide nanocomposite structure containing Ce and Mn is higher than that of the single metal oxide nanocomposite structure containing only Ce.
  • CM50 represents a double metal oxide nanocomposite structure having a Ce:Mn content ratio of 50:50
  • MF50 represents a double metal oxide nanocomposite structure having a Mn:Fe content ratio of 50:50
  • CF50 is a Ce:Fe content ratio
  • a 50:50 double metal oxide nanocomposite structure is shown.
  • the double metal oxide nanocomposite structure has higher SOD activity than the single metal oxide nanocomposite structure, and the double metal oxide nanocomposite structure containing Ce and Mn is CAT than the single metal oxide nanocomposite structure containing only Ce. activity is high. Overall, the double metal oxide nanocomposite structure has better antioxidant performance than the single metal oxide nanocomposite structure.
  • albumin can further increase the dispersibility of the single metal oxide nanocomposite structure than the double metal oxide nanocomposite structure, and dextran shows the dispersibility of the double metal oxide nanocomposite structure than the single metal oxide nanocomposite structure. can be raised further.
  • dextran having both a hydroxyl group and a carboxyl group may further increase the dispersibility of the metal oxide nanocomposite structure than dextran having only a hydroxyl group.
  • Metal oxide nanocomposite structures according to embodiments of the present invention may have excellent performance.
  • the metal oxide nanocomposite structure may have excellent biocompatibility and antioxidant performance.
  • the metal oxide nanocomposite structure can be formed in large quantities in a simple method in water without using an organic solvent.

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Abstract

L'invention concerne une structure nano-composite d'oxyde métallique et son procédé de formation. La structure nano-composite d'oxyde métallique comprend une nanostructure d'oxyde métallique et un composé ligand lié à la nanostructure d'oxyde métallique. Le procédé de formation de la structure nano-composite d'oxyde métallique comprend les étapes consistant à : former une solution de précurseur contenant un précurseur de métal et un composé de ligand ; et former une structure nano-composite d'oxyde métallique par addition d'une base à la solution de précurseur.
PCT/KR2022/004817 2021-04-09 2022-04-04 Structure nano-composite d'oxyde métallique et son procédé de formation WO2022215983A1 (fr)

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Citations (4)

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US8333993B1 (en) * 2006-12-29 2012-12-18 University Of Central Florida Research Foundation, Inc. Synthesis of polymer coated ceria nanoparticles for biomedical applications
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