CN114570425B - Modified CuFe 2 O 4 Synthesis method and application thereof - Google Patents
Modified CuFe 2 O 4 Synthesis method and application thereof Download PDFInfo
- Publication number
- CN114570425B CN114570425B CN202210331176.XA CN202210331176A CN114570425B CN 114570425 B CN114570425 B CN 114570425B CN 202210331176 A CN202210331176 A CN 202210331176A CN 114570425 B CN114570425 B CN 114570425B
- Authority
- CN
- China
- Prior art keywords
- cufe
- modified
- abei
- synthesis method
- lysine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000001308 synthesis method Methods 0.000 title claims abstract description 26
- LEOJISUPFSWNMA-UHFFFAOYSA-N ABEI Chemical compound O=C1NNC(=O)C=2C1=CC(N(CCCCN)CC)=CC=2 LEOJISUPFSWNMA-UHFFFAOYSA-N 0.000 claims abstract description 28
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000004472 Lysine Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 20
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 20
- 239000001632 sodium acetate Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 150000001879 copper Chemical class 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 238000007885 magnetic separation Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 17
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 14
- 239000012498 ultrapure water Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 30
- 239000000463 material Substances 0.000 abstract description 26
- 230000015572 biosynthetic process Effects 0.000 abstract description 12
- 238000003786 synthesis reaction Methods 0.000 abstract description 12
- 239000002077 nanosphere Substances 0.000 abstract description 8
- 239000003381 stabilizer Substances 0.000 abstract description 7
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 34
- 230000003197 catalytic effect Effects 0.000 description 15
- 238000004458 analytical method Methods 0.000 description 14
- 230000004048 modification Effects 0.000 description 12
- 238000012986 modification Methods 0.000 description 12
- 125000003277 amino group Chemical group 0.000 description 8
- 230000002349 favourable effect Effects 0.000 description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 4
- 206010028400 Mutagenic effect Diseases 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
- 230000000711 cancerogenic effect Effects 0.000 description 4
- 231100000315 carcinogenic Toxicity 0.000 description 4
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 231100000243 mutagenic effect Toxicity 0.000 description 4
- 230000003505 mutagenic effect Effects 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 231100000378 teratogenic Toxicity 0.000 description 4
- 230000003390 teratogenic effect Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000007112 amidation reaction Methods 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 229910002480 Cu-O Inorganic materials 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0254—Nitrogen containing compounds on mineral substrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0244—Nitrogen containing compounds with nitrogen contained as ring member in aromatic compounds or moieties, e.g. pyridine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
- C09K11/07—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials having chemically interreactive components, e.g. reactive chemiluminescent compositions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1044—Heterocyclic compounds characterised by ligands containing two nitrogen atoms as heteroatoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Biomedical Technology (AREA)
- Electrochemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention relates to the technical field of ferrite material synthesis, in particular to a modified CuFe 2 O 4 The synthesis process and application includes dissolving copper salt and ferric salt in reducing solvent, adding sodium acetate to regulate pH, adding lysine, high temperature and high pressure reaction, magnetic separation, washing and drying to obtain CuFe 2 O 4 The method comprises the steps of carrying out a first treatment on the surface of the Then HAuCl is added 4 ·4H 2 O, magnetically stirring and adding ABEI, magnetically separating, and washing to obtain CuFe 2 O 4 @ ABEI-Au composite. The application uses lysine as an electrostatic stabilizer and a surface active molecule, uses a reducing solvent as a reducing agent to provide a stable solvent environment, uses sodium acetate as an auxiliary stabilizer, assembles into nanospheres at high temperature, and synthesizes CuFe with uniform particles, good dispersibility and superparamagnetism 2 O 4 ；CuFe 2 O 4 CuFe modified by ABEI and Au 2 O 4 The @ ABEI-Au composite material has good monodispersity and excellent chemiluminescent performance; and the synthesis method adopts a one-step method, and has the advantages of simple steps, high efficiency, low cost and the like.
Description
Technical Field
The invention relates to the technical field of ferrite material synthesis, in particular to a modified CuFe 2 O 4 A synthesis method and application thereof.
Background
Spinel type ferrite belongs to a multifunctional semiconductor material, and particularly relates to an important magnetic material. Thin films of spinel ferrites exhibit many novel characteristics in many respects, including optical, electrical, magnetic, etc. So that the more intensive research on such ultra-fine powder and the development and utilization thereof are of considerable importance.
CuFe 2 O 4 Belongs to spinel type ferrite, is composed of nontoxic and cheap elements, and has good light absorption, proper band gap and structural stability. At present, the CuFe 2 O 4 Synthesis has been increasingly reported, e.g., yuyang Wu et al (Analytical and Bioanalytical Chemistry,2022, 414:367-375) for synthesizing CuFe by solvothermal method 2 O 4 In CuCl 2 ·2H 2 O and FeCl 3 ·6H 2 O is used as raw material, na 3 Cit·2H 2 O is an electrostatic stabilizer, naAc is a pH regulator, glycol is a solvent, and after stirring for 2 hours, cuFe is prepared by high-temperature reaction for 16 hours 2 O 4 But synthesized CuFe 2 O 4 The particle size was not uniform and the self-aggregation was severe.
Maiyong Zhu et al (ACS Applied Materials)&Interfaces 2013,5 (13): 6030-6037) CuFe is synthesized by hydrothermal method 2 O 4 By combining CuCl 2 ·2H 2 O、FeCl 3 ·6H 2 O, naAc, PVP is evenly dispersed in glycol and then is placed in a reaction kettle for high-temperature reaction for 24 hours to prepare CuFe 2 O 4 Although the synthesized CuFe 2 O 4 The particle size is relatively uniform and there is still a serious problem of self-aggregation.
Existing CuFe 2 O 4 Most of the synthesis methods have the problems of uneven particle size, serious self-aggregation of materials and the like, and the method is applied to the traditional CuFe 2 O 4 The synthesis method is improved, and a one-step method is adopted to synthesize CuFe with uniform size, good material dispersibility and superparamagnetism 2 O 4 。
Disclosure of Invention
The technical problem to be solved by the invention is how to provide a modified CuFe 2 O 4 The synthesis method adopts a one-step synthesis method, and has the advantages of simple steps, high efficiency, low cost and the like; and the prepared CuFe 2 O 4 The particles are uniform and have good dispersibility, and the particles also have superparamagnetism so as to improve the performance advantage of the particles serving as a catalyst, an adsorbent or a sensitive electrode.
The invention solves the technical problems by the following technical means:
in one aspect, the invention provides a modified CuFe 2 O 4 The synthesis method comprises the following steps:
s1, synthesizing CuFe 2 O 4 ：
Dissolving copper salt and ferric salt in a reducing solvent, and adding sodium acetate after complete dissolution, so as to adjust the pH of the solution to 4-6; adding lysine (Lys) into the mixed solution, uniformly stirring, and transferring to a high-temperature high-pressure reaction kettle for reaction for 15-20h; after the reaction is finished, the reaction product is cooled to room temperature, and is alternately washed by ethanol and water after magnetic separation, and finally is dried to constant weight in an oven to prepare the CuFe 2 O 4 ；
S2, modified CuFe 2 O 4
CuFe 2 O 4 Dispersing with ultrapure water, and then adding HAuCl 4 ·4H 2 O, magnetic stirring to make them fully react, adding N- (4-aminobutyl) -N-ethyl isoluminol (ABEI) into the above-mentioned mixed solution, stirring to fully react, magnetic separating, washing with water to obtain CuFe 2 O 4 The @ ABEI-Au composite is stored in an environment of 3-4 ℃.
The beneficial effects are that: according to the method, copper salt and ferric salt are used as raw materials, sodium acetate is added as a pH regulator, lysine is used as an electrostatic stabilizer and a surface active molecule, a reducing solvent is used as a reducing agent to provide a stable solvent environment, and the nanospheres are assembled at a high temperature. During the synthesis, lysine is attached to CuFe 2 O 4 The surface of the nano-sphere is enabled to have electrostatic repulsion, the material can be better dispersed, the size of the nano-sphere is relatively uniform due to the addition of lysine, and meanwhile, the sodium acetate is used as a stabilizer to assist in adjusting the size and uniformity of the material particles, so that CuFe with uniform particles and good dispersibility is synthesized 2 O 4 。
Lysine-enabled CuFe in the present application 2 O 4 Amino groups are present on the surface of (a) CuFe containing amino groups on the surface 2 O 4 Is favorable for the uniform loading of Au particles through Au-N bonds, and CuFe 2 O 4 After modification by ABEI and Au, the obtained CuFe 2 O 4 The @ ABEI-Au composite material has good monodispersity.
The application uses classical ABEI-H 2 O 2 The chemiluminescent system is taken as a research object, and CuFe is added 2 O 4 The chemiluminescent intensity of the system after the ABEI-Au composite material is enhanced because of CuFe 2 O 4 Has peroxidase-like catalytic activity and can catalyze H 2 O 2 The chemical luminescence kinetic curve obtained by the method contains 2 luminescence peaks and has excellent chemical luminescence performance.
In addition, carboxyl groups in lysine molecules can perform amidation reaction with amino groups on chemiluminescent reagent ABEI to connect ABEI to CuFe 2 O 4 Surface to CuFe is reduced 2 O 4 The modification step improves the preparation efficiency and realizes one-step synthesis; and CuFe 2 O 4 The method also has superparamagnetism, is favorable for realizing rapid separation of materials from complex sample matrixes, and has the advantages of simple steps, high efficiency, low cost and the like.
Preferably, the copper salt in the step S1 is one or more of copper chloride, copper nitrate and copper sulfate.
Preferably, the iron salt in the step S1 is one or more of ferric chloride, ferric nitrate and ferric sulfate.
Preferably, in the step S1, the molar ratio of copper salt, iron salt, sodium acetate and lysine is 2-4:5-7:24-32:10-15.
Preferably, the stirring speed of the mixed solution in the step S1 after lysine is added is 800-1200r/min, and the stirring time is 1.5-2.5h.
Preferably, the reaction temperature of the mixed solution in the step S1 in the high-temperature high-pressure reaction kettle is 150-250 ℃ and the pressure is 2-10MPa.
Preferably, the drying temperature of the mixed solution in the step S1 in the oven is 50-80 ℃.
Preferably, the reducing solvent in the step S1 is any one or more of ethylene glycol, methylene chloride, methanol, ethanol and isopropanol.
Preferably, cuFe in the step S2 2 O 4 The mass ratio of the ultra-pure water to the ultra-pure water is 1:800-1000; HAuCl 4 ·4H 2 The volume ratio of O to ultrapure water is 1:1-3.
Preferably, HAuCl is used in the step S2 4 ·4H 2 The concentration of O is 2-4mmol/L; the concentration of the ABEI is 3-5mmol/L, and the volume ratio of the ABEI to the mixed solution is 1:4-9.
Preferably, the magnetic stirring speed in the step S2 is 1200-1800r/min and the time is 20-40min.
In another aspect, the present invention provides a modified CuFe 2 O 4 Is used for the modification of CuFe 2 O 4 Used as a catalyst, adsorbent or sensitive electrode.
The beneficial effects are that: cuFe 2 O 4 The catalyst has good catalytic effect, can catalyze and remove soot, and is environment-friendly; in chemiluminescence, cu itself has a catalytic effect, cuFe 2 O 4 After being modified by ABEI and Au, the intensity of chemiluminescence is further catalyzed and enhanced; cuFe 2 O 4 When used as an adsorbent, the organic matters of polycyclic aromatic hydrocarbon with carcinogenic, teratogenic and mutagenic effects can be adsorbed; cuFe 2 O 4 When used as a sensitive electrode, the potential sensor can be prepared for NH 3 Is detected.
The invention has the advantages that:
1. during the synthesis process, lysine is attached to CuFe 2 O 4 The surface of the nano-sphere is enabled to have electrostatic repulsion, the material can be better dispersed, the size of the nano-sphere is relatively uniform due to the addition of lysine, and meanwhile, the sodium acetate is used as a stabilizer to assist in adjusting the size and uniformity of the material particles, so that CuFe with uniform particles and good dispersibility is synthesized 2 O 4 。
2. Lysine in this application causes CuFe 2 O 4 Amino groups are present on the surface of (a) CuFe containing amino groups on the surface 2 O 4 Is favorable for the uniform loading of Au particles through Au-N bonds, and CuFe 2 O 4 After modification by ABEI and Au, the obtained CuFe 2 O 4 The @ ABEI-Au composite material has good monodispersity.
3. The application uses classical ABEI-H 2 O 2 The chemiluminescent system is taken as a research object, and CuFe is added 2 O 4 The chemiluminescent intensity of the system after the ABEI-Au composite material is enhanced because of CuFe 2 O 4 Has peroxidase-like catalytic activity and can catalyze H 2 O 2 Decomposition generation · OH improves the efficiency of the chemiluminescent reaction, and further enhances the chemiluminescent intensity, so that the obtained chemiluminescent kinetic curve contains 2 luminescent peaks and has excellent chemiluminescent performance.
4. In the application, carboxyl in lysine molecule can perform amidation reaction with amino on chemiluminescent reagent ABEI to connect ABEI to CuFe 2 O 4 On the surface, reduce CuFe 2 O 4 The modification step improves the preparation efficiency and realizes one-step synthesis; and CuFe 2 O 4 The method also has superparamagnetism, is favorable for realizing rapid separation of materials from complex sample matrixes, and has the advantages of simple steps, high efficiency, low cost and the like.
5. CuFe of the present application 2 O 4 The catalyst has good catalytic effect, can catalyze and remove soot, and is environment-friendly; in chemiluminescence, cu itself has a catalytic effect, cuFe 2 O 4 After Au modification, the intensity of chemiluminescence is further catalyzed and enhanced; cuFe 2 O 4 When used as an adsorbent, the organic matters of polycyclic aromatic hydrocarbon with carcinogenic, teratogenic and mutagenic effects can be adsorbed; cuFe 2 O 4 When used as a sensitive electrode, the potential sensor can be prepared for NH 3 Is detected.
Drawings
FIG. 1 is a view of CuFe in example 3 of the present application 2 O 4 FTIR spectra of (c).
FIG. 2 is a view of CuFe in comparative example 3 of the present application 2 O 4 Is a XRD spectrum of (C).
FIG. 3 is a view of CuFe in example 4 of the present application 2 O 4 TEM analysis of (c).
FIG. 4 is a view of CuFe in example 5 of the present application 2 O 4 Magnetic susceptibility analysis results of (c) are shown.
FIG. 5 is a view of CuFe in example 6- (1) of the present application 2 O 4 TEM analysis of the @ ABEI-Au composite.
FIG. 6 is a view of CuFe in example 6- (2) of the present application 2 O 4 TEM analysis of the @ ABEI-Au composite.
FIG. 7 is a graph showing the results of the chemiluminescent performance test conducted in example 7- (1) of the present application.
FIG. 8 is a graph showing the results of the chemiluminescent performance test conducted in example 7- (2) of the present application.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Modified CuFe 2 O 4 The synthesis method comprises the following steps:
s1, synthesizing CuFe 2 O 4 ：
Dissolving 2-4mmol of copper salt and 5-7mmol of ferric salt in a reducing solvent, and adding 24-32mmol of sodium acetate after complete dissolution, so as to adjust the pH of the solution to 4-6; adding 10-15mmol of lysine (Lys) into the mixed solution, stirring at a rotating speed of 800-1200r/min for 1.5-2.5h, uniformly stirring, transferring into a high-temperature high-pressure reaction kettle, and reacting for 15-20h at a temperature of 150-250 ℃ and a pressure of 2-10MPa; after the reaction is completed, the reaction product is cooled to room temperature, and is subjected to magnetic separation and then is subjected to ethanol and water exchangeWashing, and drying in an oven at 50-80deg.C to constant weight to obtain CuFe 2 O 4 。
Wherein the copper salt is one or more of copper chloride, copper nitrate and copper sulfate; the ferric salt is one or more of ferric chloride, ferric nitrate and ferric sulfate; the reducing solvent is any one or more of ethylene glycol, dichloromethane, methanol, ethanol and isopropanol.
S2, modified CuFe 2 O 4
CuFe 2 O 4 Dispersing with ultrapure water, cuFe 2 O 4 The mass ratio of the ultra-pure water to the ultra-pure water is 1:800-1000; then adding HAuCl with the concentration of 2-4mmol/L into the mixed solution 4 ·4H 2 O, and HAuCl 4 ·4H 2 The volume ratio of O to ultrapure water is 1:1-3; magnetically stirring at 1200-1800r/min for 20-40min, and adding 3-5mmol/L N- (4-aminobutyl) -N-ethyl isoluminol (ABEI) into the mixed solution after full reaction, wherein the volume ratio of the ABEI to the mixed solution is 1:4-9, stirring to make them fully react, after magnetic separation washing with water to obtain CuFe 2 O 4 The @ ABEI-Au composite is stored in an environment of 3-4 ℃.
Modified CuFe prepared by the method 2 O 4 The catalyst has good catalytic effect, can be used as a catalyst for catalyzing and removing soot, and is environment-friendly; in chemiluminescence, cu itself has a catalytic effect, cuFe 2 O 4 After modification by ABEI and Au, the intensity of chemiluminescence is further enhanced by catalysis. Modified CuFe prepared by the method 2 O 4 Used as adsorbent, can adsorb polycyclic aromatic hydrocarbon organic matters with carcinogenic, teratogenic and mutagenic effects. Modified CuFe prepared by the method 2 O 4 Can be used as a sensitive electrode to prepare a potential sensor for NH 3 Is used as a catalyst.
Example 1
Modified CuFe 2 O 4 The synthesis method comprises the following steps:
s1, synthesizing CuFe 2 O 4 ：
3mmol of CuCl 2 ·2H 2 O and 6mmol FeCl 3 ·6H 2 O is dissolved in glycol, 32mmol of sodium acetate is added after the O is completely dissolved, and the pH of the solution is adjusted to 5.5; adding 12mmol of lysine (Lys) into the mixed solution, stirring at a rotating speed of 1000r/min for 2h, uniformly stirring, transferring into a high-temperature high-pressure reaction kettle, and reacting for 16h at a temperature of 200 ℃ and a pressure of 2 MPa; after the reaction is finished, the reaction product is cooled to room temperature, after magnetic separation, ethanol and water are used for washing alternately, and finally the reaction product is dried to constant weight in a baking oven at 60 ℃ to prepare the CuFe 2 O 4 。
S2, modified CuFe 2 O 4
Weigh 6mg of CuFe 2 O 4 Dispersing with 6ml of ultra pure water, and then adding 3ml of HAuCl with the concentration of 4mmol/L to the mixed solution 4 ·4H 2 O, magnetically stirring at 1500r/min for 30min, adding 3ml of N- (4-aminobutyl) -N-ethyl isoluminol (ABEI) with concentration of 4mmol/L into the mixed solution after full reaction, stirring for 6h to fully react the two, magnetically separating, and washing with water for three times to obtain CuFe 2 O 4 The @ ABEI-Au composite was stored at 4 ℃.
Example 2
Modified CuFe 2 O 4 The synthesis method comprises the following steps:
s1, synthesizing CuFe 2 O 4 ：
3mmol of CuCl 2 ·2H 2 O and 6mmol FeCl 3 ·6H 2 O is dissolved in glycol, and 24mmol of sodium acetate is added after the O is completely dissolved, so that the pH of the solution is adjusted to 5.4; adding 12mmol of lysine (Lys) into the mixed solution, stirring at a rotating speed of 1000r/min for 2h, uniformly stirring, transferring into a high-temperature high-pressure reaction kettle, and reacting for 16h at a temperature of 200 ℃ and a pressure of 2 MPa; after the reaction is finished, the reaction product is cooled to room temperature, after magnetic separation, ethanol and water are used for washing alternately, and finally the reaction product is dried to constant weight in a baking oven at 60 ℃ to prepare the CuFe 2 O 4 。
S2, modified CuFe 2 O 4
Weigh 6mg of CuFe 2 O 4 Dispersing with 6ml of ultra pure water, and then adding 3ml of HAuCl with the concentration of 4mmol/L to the mixed solution 4 ·4H 2 O, magnetically stirring at 1500r/min for 30min, adding 3ml of N- (4-aminobutyl) -N-ethyl isoluminol (ABEI) with concentration of 4mmol/L into the mixed solution after full reaction, stirring for 6h to fully react the two, magnetically separating, and washing with water for three times to obtain CuFe 2 O 4 The @ ABEI-Au composite was stored at 4 ℃.
Comparative example 1
Modified CuFe 2 O 4 The synthesis process differs from example 1 in that the concentration of sodium acetate is 16mmol.
Comparative example 2
Modified CuFe 2 O 4 The synthesis process differs from example 1 in that the concentration of sodium acetate is 8mmol.
Example 3
FTIR (infrared spectroscopy) and XRD analysis were performed on the materials synthesized in step 1 of examples 1-2 and comparative examples 1-2, and the analysis results are shown in fig. 1 and 2.
Fig. 1 is an infrared spectrum analysis chart in which example 1, example 2, comparative example 1, comparative example 2 correspond to A, B, C, D in fig. 1, respectively. As can be seen from the figure, the four curves are at 430cm -1 Cu-O characteristic absorption peaks are arranged nearby and 590cm -1 Near the Fe-O absorption peak, 1630cm -1 N-H characteristic absorption peaks were found nearby, indicating that the materials synthesized in step 1 of examples 1-2 and comparative examples 1-2 all contained Cu-O, fe-O, N-H.
Fig. 2 is an XRD spectrum analysis chart in which example 1, example 2, comparative example 1, comparative example 2 correspond to A, B, C, D in fig. 2, respectively. As can be seen from the figure, four curves are associated with CuFe 2 O 4 Further illustrating that the materials synthesized in step 1 of examples 1-2 and comparative examples 1-2 are CuFe 2 O 4 The method comprises the steps of carrying out a first treatment on the surface of the And as can be seen in conjunction with FIG. 1, the synthesized CuFe 2 O 4 Amino groups are present on each.
Example 4
CuFe synthesized in step 1 of examples 1-2 and comparative examples 1-2 2 O 4 TEM analysis was performed and the analysis results are shown in FIG. 3. Among these, example 1, example 2, comparative example 1, and comparative example 2 correspond to A, B, C, D in fig. 3, respectively.
It can be seen that the particles of A, B in fig. 3 are uniform and have good dispersibility, while the particles of C are not uniform in size, the particles of D are not uniform in size, and have poor dispersibility. From this, it was found that when the amount of sodium acetate was 24 to 32mmol, cuFe was prepared 2 O 4 Has the advantages of uniform particles and good dispersibility.
Example 5
CuFe synthesized in step 1 of examples 1-2 and comparative examples 1-2 2 O 4 Susceptibility analysis was performed and the analysis results are shown in fig. 4. Among them, example 1, example 2, comparative example 1, comparative example 2 correspond to A, B, C, D in fig. 4, respectively.
As can be seen from the figures, the CuFe synthesized in example 1, example 2, comparative example 1, comparative example 2 2 O 4 The saturation magnetic susceptibility of the material is 68.39emu/g, 58.01emu/g, 54.5emu/g and 54.2emu/g respectively, and hysteresis loops are not generated, so that the synthesized material has superparamagnetism; in the studies of the prior art Yuyang Wu et al (Analytical and Bioanalytical Chemistry,2022, 414:367-375), however, it synthesized CuFe 2 O 4 The magnetic susceptibility of the alloy is only 39.01emu/g, which indicates that the CuFe synthesized by the method of the application 2 O 4 The material has stronger magnetism, and the superparamagnetism of the material is better when the dosage of sodium acetate is 24-32mmol, thereby being beneficial to realizing the rapid separation of the material from complex sample matrixes.
Comparative example 3
Modified CuFe 2 O 4 The synthesis method differs from example 2 in that HAuCl 4 ·4H 2 The concentration of O was 2mmol/L.
Comparative example 4
Modified CuFe 2 O 4 The synthesis method differs from example 2 in that HAuCl 4 ·4H 2 The concentration of O was 8mmol/L.
Comparative example 5
Modified CuFe 2 O 4 The synthesis method differs from example 2 in that HAuCl 4 ·4H 2 The concentration of O was 12mmol/L.
Comparative example 6
Modified CuFe 2 O 4 The synthesis method differs from example 2 in that HAuCl 4 ·4H 2 The concentration of O was 16mmol/L.
Comparative example 7
Modified CuFe 2 O 4 The synthesis method differs from example 2 in that HAuCl 4 ·4H 2 The concentration of O was 20mmol/L.
Example 6
(1) CuFe prepared in step 2 of examples 1-2 and comparative examples 1-2 2 O 4 TEM analysis was performed on the @ ABEI-Au composite, and the analysis results are shown in FIG. 5. Among them, example 1, example 2, comparative example 1, comparative example 2 correspond to A, B, C, D in fig. 5, respectively.
As can be seen from FIG. 5, cuFe in A, B 2 O 4 The size of the particles is uniform, and gold particles can be uniformly loaded on the particles; whereas C, D CuFe 2 O 4 The size of the particles is not uniform and the gold particles are not well supported thereon. The above results illustrate CuFe 2 O 4 The uniformity of the particles of (a) affects the loading capacity of the gold particles on the surface thereof, thereby affecting the modification effect.
(2) CuFe prepared in step 2 of example 2 and comparative examples 3 to 7 2 O 4 TEM analysis was performed on the @ ABEI-Au composite, and the analysis results are shown in FIG. 6. Among them, comparative example 3, example 2, comparative example 4, comparative example 5, comparative example 6, comparative example 7 correspond to A, B, C, D, E, F in fig. 6, respectively.
As can be seen from FIG. 6, the gold particles in A, B are uniformly supported on CuFe 2 O 4 On the other hand, the gold particles in C, D, E, F self-aggregate, are not uniformly dispersed, and are formed in CuFe 2 O 4 The upper load is less. Indicating that HAuCl with concentration of 2-4mmol/L is adopted 4 Modified CuFe 2 O 4 When in use, the method is favorable for preventing CuFe 2 O 4 Self-aggregation occursA situation; and when HAuCl 4 At a concentration of 4mmol/L, the gold particles are in CuFe 2 O 4 The loading on is the greatest.
Example 7
(1) By ABEI-H 2 O 2 The system was the subject of investigation, and the CuFe prepared in step 2 of examples 1-2 and comparative examples 1-2 2 O 4 The chemiluminescent performance test was performed on the @ ABEI-Au composite and the ABEI-Au material, and the test results are shown in FIG. 7.
As can be seen from FIG. 7, the CuFe prepared in example 2 2 O 4 The luminous intensity of the @ ABEI-Au composite material is more than one hundred times that of the ABEI-Au material, which shows that the CuFe prepared by the method 2 O 4 ABEI-Au composite pair ABEI-H 2 O 2 The system has good catalytic effect. In addition, when the sodium acetate dosage is 32mmol and 24mmol, cuFe 2 O 4 The luminous intensity of the @ ABEI-Au composite material is stronger than that of the sodium acetate with the dosage of 16mmol and 8mmol, which shows that the sodium acetate with the dosage of 24mmol to 32mmol is beneficial to enhancing the CuFe 2 O 4 Catalytic effect of the @ ABEI-Au composite.
(2) By ABEI-H 2 O 2 The system was the subject of investigation, and the CuFe prepared in step 2 of example 2, comparative examples 3-7 2 O 4 The chemiluminescent performance test of the @ ABEI-Au composite and the ABEI-Au composite was performed and the test results are shown in FIG. 8.
As can be seen from FIGS. 7 and 8, the addition of CuFe is compared with the addition of ABEI-Au material 2 O 4 ABEI-H after ABEI-Au composite 2 O 2 The chemiluminescent intensity of the system is significantly enhanced because of the CuFe 2 O 4 Has peroxidase-like catalytic activity and can catalyze H 2 O 2 Decomposition generation · OH improves the efficiency of the chemiluminescent reaction, and further enhances the chemiluminescent intensity, so that the obtained chemiluminescent kinetic curve contains 2 luminescent peaks and has excellent chemiluminescent performance.
In addition, when HAuCl 4 ·4H 2 When the concentration of O is 4mmol/L, cuFe 2 O 4 The luminous intensity of the @ ABEI-Au composite material is strongest, namelyHAuCl with concentration of 4mmol/L 4 ·4H 2 O modified CuFe 2 O 4 When in use, the CuFe is beneficial to improving 2 O 4 Is a catalytic effect of (a).
The use principle and the advantages are that: during the synthesis process, lysine is attached to CuFe 2 O 4 The surface of the nano-sphere is enabled to have electrostatic repulsion, the material can be better dispersed, the size of the nano-sphere is relatively uniform due to the addition of lysine, and meanwhile, the sodium acetate is used as a stabilizer to assist in adjusting the size and uniformity of the material particles, so that CuFe with uniform particles and good dispersibility is synthesized 2 O 4 . Lysine to CuFe 2 O 4 Amino groups are present on the surface of (a) CuFe containing amino groups on the surface 2 O 4 Is favorable for the uniform loading of Au particles through Au-N bonds, and CuFe 2 O 4 After modification by ABEI and Au, the obtained CuFe 2 O 4 The @ ABEI-Au composite material has good monodispersity.
The application uses classical ABEI-H 2 O 2 The chemiluminescent system is taken as a research object, and CuFe is added 2 O 4 The chemiluminescent intensity of the system after the ABEI-Au composite material is enhanced because of CuFe 2 O 4 Has peroxidase-like catalytic activity and can catalyze H 2 O 2 Decomposition generation · OH improves the efficiency of the chemiluminescent reaction, and further enhances the chemiluminescent intensity, so that the obtained chemiluminescent kinetic curve contains 2 luminescent peaks and has excellent chemiluminescent performance.
In the application, carboxyl in lysine molecule can perform amidation reaction with amino on chemiluminescent reagent ABEI to connect ABEI to CuFe 2 O 4 On the surface, reduce CuFe 2 O 4 The modification step improves the preparation efficiency and realizes one-step synthesis; and CuFe 2 O 4 The method also has superparamagnetism, is favorable for realizing rapid separation of materials from complex sample matrixes, and has the advantages of simple steps, high efficiency, low cost and the like.
CuFe of the present application 2 O 4 Has good catalytic effect and can catalyze and remove carbonThe smoke is environment-friendly; in chemiluminescence, cu itself has a catalytic effect, cuFe 2 O 4 After Au modification, the intensity of chemiluminescence is further catalyzed and enhanced; cuFe 2 O 4 When used as an adsorbent, the organic matters of polycyclic aromatic hydrocarbon with carcinogenic, teratogenic and mutagenic effects can be adsorbed; cuFe 2 O 4 When used as a sensitive electrode, the potential sensor can be prepared for NH 3 Is detected.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. Modified CuFe 2 O 4 The synthesis method is characterized in that: the method comprises the following steps:
s1, synthesizing CuFe 2 O 4
Dissolving copper salt and ferric salt in a reducing solvent, and adding sodium acetate after complete dissolution, so as to adjust the pH of the solution to 4-6; adding lysine (Lys) into the mixed solution, uniformly stirring, and transferring to a high-temperature high-pressure reaction kettle for reaction for 15-20h; after the reaction is finished, the reaction product is cooled to room temperature, and is alternately washed by ethanol and water after magnetic separation, and finally is dried to constant weight in an oven to prepare the CuFe 2 O 4 ；
S2, modified CuFe 2 O 4
CuFe 2 O 4 Dispersing with ultrapure water, and then adding HAuCl 4 ·4H 2 O, magnetic stirring to make them fully react, adding N- (4-aminobutyl) -N-ethyl isoluminol (ABEI) into the above-mentioned mixed solution, stirring to fully react, magnetic separating, washing with water to obtain CuFe 2 O 4 The @ ABEI-Au composite is stored in an environment of 3-4 ℃.
2. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: the copper salt in the step S1 is one or more of copper chloride, copper nitrate and copper sulfate; the ferric salt is one or more of ferric chloride, ferric nitrate and ferric sulfate.
3. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: in the step S1, the molar ratio of copper salt to ferric salt to sodium acetate to lysine is 2-4:5-7:24-32:10-15.
4. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: the stirring speed of the mixed solution in the step S1 after lysine is added is 800-1200r/min, and the stirring time is 1.5-2.5h.
5. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: the reaction temperature of the mixed solution in the step S1 in a high-temperature high-pressure reaction kettle is 150-250 ℃ and the pressure is 2-10MPa; the drying temperature in the oven is 50-80 ℃.
6. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: the reducing solvent in the step S1 is any one or more of ethylene glycol, methylene dichloride, methanol, ethanol and isopropanol.
7. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: cuFe in the step S2 2 O 4 The mass ratio of the ultra-pure water to the ultra-pure water is 1:800-1000; HAuCl 4 ·4H 2 The volume ratio of O to ultrapure water is 1:1-3.
8. A modified CuF as defined in claim 1e 2 O 4 The synthesis method is characterized in that: HAuCl in step S2 4 ·4H 2 The concentration of O is 2-4mmol/L; the concentration of the ABEI is 3-5mmol/L, and the volume ratio of the ABEI to the mixed solution is 1:4-9.
9. A modified CuFe according to claim 1 2 O 4 The synthesis method is characterized in that: the magnetic stirring speed in the step S2 is 1200-1800r/min, and the time is 20-40min.
10. A modified CuFe as claimed in any one of claims 1 to 9 2 O 4 Is characterized in that: the modified CuFe 2 O 4 Used as a catalyst, adsorbent or sensitive electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210331176.XA CN114570425B (en) | 2022-03-31 | 2022-03-31 | Modified CuFe 2 O 4 Synthesis method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210331176.XA CN114570425B (en) | 2022-03-31 | 2022-03-31 | Modified CuFe 2 O 4 Synthesis method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114570425A CN114570425A (en) | 2022-06-03 |
| CN114570425B true CN114570425B (en) | 2023-05-30 |
Family
ID=81777955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210331176.XA Active CN114570425B (en) | 2022-03-31 | 2022-03-31 | Modified CuFe 2 O 4 Synthesis method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114570425B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108295904A (en) * | 2018-02-02 | 2018-07-20 | 陕西科技大学 | A kind of cu ferrite/Cellulose nanocrystal catalyst and preparation method thereof |
| CN110660414A (en) * | 2018-06-29 | 2020-01-07 | 昭和电工株式会社 | Heat-assisted magnetic recording medium and magnetic storage device |
| CN112452301A (en) * | 2020-11-06 | 2021-03-09 | 东北师范大学 | Copper ferrite-metal organic framework structure composite material and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10948484B2 (en) * | 2016-04-11 | 2021-03-16 | Veravas, Inc. | Sample depletion and enrichment to improve the quality of diagnostic test results |
-
2022
- 2022-03-31 CN CN202210331176.XA patent/CN114570425B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108295904A (en) * | 2018-02-02 | 2018-07-20 | 陕西科技大学 | A kind of cu ferrite/Cellulose nanocrystal catalyst and preparation method thereof |
| CN110660414A (en) * | 2018-06-29 | 2020-01-07 | 昭和电工株式会社 | Heat-assisted magnetic recording medium and magnetic storage device |
| CN112452301A (en) * | 2020-11-06 | 2021-03-09 | 东北师范大学 | Copper ferrite-metal organic framework structure composite material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114570425A (en) | 2022-06-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110215900B (en) | Metal chelating magnetic microsphere and preparation method thereof | |
| Zhao et al. | Magnetic N-doped Co–carbon composites derived from metal organic frameworks as highly efficient catalysts for p-nitrophenol reduction reaction | |
| CN104722276A (en) | Magnetic cucurbit urils/grapheme oxide composite material and preparation method thereof | |
| Banaei et al. | Synthesis and characterization of new modified silica coated magnetite nanoparticles with bisaldehyde as selective adsorbents of Ag (I) from aqueous samples | |
| CN114409913B (en) | Magnetic metal organic framework material and preparation method and application thereof | |
| CN112934164A (en) | Magnetic phosphorus removal adsorbent and preparation method and application thereof | |
| CN109453762B (en) | Preparation method and application of modified clay mineral supported palladium catalyst | |
| CN105854887A (en) | Cobalt-cerium double-metal oxide nanosphere and preparation method thereof | |
| Mohapatra et al. | Boronic acid functionalized superparamagnetic iron oxide nanoparticle as a novel tool for adsorption of sugar | |
| Patriarca et al. | Biomimetic Cu, Zn and Cu2 complexes inserted in mesoporous silica as catalysts for superoxide dismutation | |
| CN108854938A (en) | Amino modified magnetism CoFe2O4The preparation method and application of composite material | |
| CN111377443B (en) | Copper-doped activated carbon composite material and preparation method thereof | |
| CN114570425B (en) | Modified CuFe 2 O 4 Synthesis method and application thereof | |
| Zheng et al. | Simultaneous detection and speciation of mono-and di-valent copper ions with a dual-channel fluorescent nanoprobe | |
| CN112958041B (en) | Core-shell structure nano composite resin, preparation method and application in electroplating wastewater treatment | |
| CN111715289B (en) | In-situ synthesis of FeOOH/Fe 3 O 4 Method for preparing/cellulose composite material and application thereof | |
| Liu et al. | Metal ion-induced chemiluminescence recovery for highly intensive chemiluminescence bifunctionalized polydopamine nanospheres | |
| CN110026155B (en) | MOFs (metal-organic frameworks) -coated carbon microsphere adsorbent as well as preparation method and application thereof | |
| Dakova et al. | Cysteine modified silica submicrospheres as a new sorbent for preconcentration of Cd (II) and Pb (II) | |
| CN113967471B (en) | Preparation method and application of surface-modified magnetic mesoporous silica microspheres | |
| CN113731419B (en) | Application and preparation of oxygen carrier in chemical looping hydrogen production | |
| CN112844335B (en) | Acid-resistant magnetic nano adsorbent and preparation method thereof | |
| CN114011376A (en) | Metal oxidation affinity chromatography magnetic mesoporous nano material, preparation method and application | |
| CN114409957A (en) | Me-MOF @ activated carbon composite material, preparation method and application thereof in fluorescent recognition of Fe3+In (1) | |
| CN112156784A (en) | Layered composite material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |