CN106824222A - A kind of nano platinum particle/cupric oxide plate composite and preparation method and application - Google Patents
A kind of nano platinum particle/cupric oxide plate composite and preparation method and application Download PDFInfo
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- CN106824222A CN106824222A CN201611184248.3A CN201611184248A CN106824222A CN 106824222 A CN106824222 A CN 106824222A CN 201611184248 A CN201611184248 A CN 201611184248A CN 106824222 A CN106824222 A CN 106824222A
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- cupric oxide
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- platinum particle
- nano platinum
- plate composite
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 217
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 229960004643 cupric oxide Drugs 0.000 title claims abstract description 109
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 75
- 239000002245 particle Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 46
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 23
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 23
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 23
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 230000009467 reduction Effects 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 13
- 230000008859 change Effects 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 150000001879 copper Chemical class 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 239000002135 nanosheet Substances 0.000 claims description 4
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 2
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 23
- 102000003992 Peroxidases Human genes 0.000 abstract description 14
- 108040007629 peroxidase activity proteins Proteins 0.000 abstract description 14
- 238000001514 detection method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 9
- 241000446313 Lamella Species 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 20
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- 102000004190 Enzymes Human genes 0.000 description 7
- 108090000790 Enzymes Proteins 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 5
- 108010001336 Horseradish Peroxidase Proteins 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000004737 colorimetric analysis Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002965 ELISA Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000002255 enzymatic effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- OHDRQQURAXLVGJ-HLVWOLMTSA-N azane;(2e)-3-ethyl-2-[(e)-(3-ethyl-6-sulfo-1,3-benzothiazol-2-ylidene)hydrazinylidene]-1,3-benzothiazole-6-sulfonic acid Chemical compound [NH4+].[NH4+].S/1C2=CC(S([O-])(=O)=O)=CC=C2N(CC)C\1=N/N=C1/SC2=CC(S([O-])(=O)=O)=CC=C2N1CC OHDRQQURAXLVGJ-HLVWOLMTSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- YRNWIFYIFSBPAU-UHFFFAOYSA-N 4-[4-(dimethylamino)phenyl]-n,n-dimethylaniline Chemical compound C1=CC(N(C)C)=CC=C1C1=CC=C(N(C)C)C=C1 YRNWIFYIFSBPAU-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011942 biocatalyst Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000005515 coenzyme Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Plasma & Fusion (AREA)
- Catalysts (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The present invention relates to nano material, a kind of nano platinum particle/cupric oxide plate composite and preparation method thereof and its application in ascorbic acid is detected are specifically disclosed.The nano platinum particle/cupric oxide plate composite has the cupric oxide nano piece of nano platinum particle for surface is dispersed；0.5~2 μm of the cupric oxide nano length of a film, it is wide 0.4~0.6 μm；10~20nm of the nano platinum particle diameter.The present invention utilizes the property of the big specific surface area of lamella cupric oxide, be supported on Pt nanoparticle in the lamellar structure of cupric oxide by one stage reduction method, obtain nano platinum particle/cupric oxide plate composite, preparation process is simple, workable, the requirement to equipment is relatively low, and the present invention not only increases the stability of Pt nanoparticle, the Catalyzed Synthesis By Peroxidase activity of material is also improve simultaneously, and then significantly improves sensitivity and the selectivity of Ascorbic Acid detection.
Description
Technical field
The present invention relates to nano material, specifically, it is related to nano platinum particle/cupric oxide plate composite.
Background technology
Enzyme linked immunosorbent assay (ELISA) (ELISA measure) has extensively in every field such as identification, retention analysis and quality controls
General application.Used as a kind of biocatalyst, enzyme is present in all of organism, participates in almost all of internal reaction, tool
There are high efficiency and specificity.Equally, enzyme is also widely used at aspects such as industry, medical science, chemistry, food, environment.But,
The structure of enzyme is highly susceptible to the influence of high temperature or chemical reagent and then causes the reduction of its catalysis activity or forfeiture.Due to enzyme
Difficult, purifying high cost is prepared, being difficult the problems such as storing causes the application of enzyme to be subject to certain restrictions.Therefore, stabilization is developed high
The analogue enztme with high catalytic activity of effect increasingly receives everybody concern and research.
2006, ferromagnetic nano material was found have close mistake with traditional horseradish peroxidase (HRP)
Peroxidase activity, since then, designs the extensive concern that the new nano material with enzymatic activity receives scientific worker.It is various
Nano material is found to have peroxidase activity, such as FeS, nanometer V2O5Nano wire and nano platinum particle etc..Compared to it
His metal material, copper source is a kind of generally the least expensive noble metal precursor body, can save and prepare Cu oxide and metal-based nano material
The expense of material.In addition, the material of Cu bases has the Fenton property similar with iron-based, and this property has peroxide with Fe sills
Compound enzymatic activity is related.Therefore, the copper-based nano material with peroxidase activity is widely studied.Additionally, cupric oxide
(CuO), a narrow band gap p-type semiconductor (1.2eV), in high-temperature superconductor, solar cell and detector aspect are obtained extensively
Research and application.However, due to relatively low Catalyzed Synthesis By Peroxidase efficiency, CuO nano materials have in terms of biology sensor
Little application.Therefore, the efficiency for improving the peroxidase activity of cupric oxide based nano-material is the task of top priority.
Because with excellent catalysis activity, Pt nano particles are widely used in catalytic field.But, Pt nanoparticles
The catalysis activity of son be easy to be aggregated or surfactant and influence.Two-dimentional (2D) lamellar graphite alkene or molybdenum bisuphide have abundant
Avtive spot and big specific surface area, can as the backing material of nano particle, improve nano particle stability.So
And, as far as we know, the preparation of cupric oxide nano lamella composite and its application in biological field are seldom reported.
Ascorbic acid (AA) is ascorbic primary biological form, and many biochemical activities are participated in as coenzyme.In recent years
Come, the detection method of AA is gradually developed, including electrochemistry, AAS, chromatography and colorimetric method etc..Colorimetric method due to
The characteristics of its is simple, quick, cheap, has caused increasing concern.
Therefore, in this area, expect to prepare the cupric oxide nano sheets of platinum layer composite with efficient peroxidase simultaneously
Use it for the colorimetric detection of Ascorbic Acid.
The content of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of nano platinum particle/cupric oxide
Piece composite and preparation method and application.
In order to realize the object of the invention, technical scheme is as follows：
In a first aspect, the invention provides a kind of nano platinum particle/cupric oxide plate composite, it is dispersed surface
There is the cupric oxide nano piece of nano platinum particle.Nano platinum particle is uniformly supported in the lamellar structure of cupric oxide nano piece, surely
It is qualitative to be enhanced.Cupric oxide nano piece of the present invention is prepared by hydro-thermal method, long 0.5~2 μm, wide 0.4~0.6 μm；It is described
10~20nm of nano platinum particle diameter.
Further, the nano platinum particle/cupric oxide plate composite is by the dispersion liquid of cupric oxide nano piece
One step reduction chloroplatinic acid is prepared.
Be supported on nano platinum particle in the lamellar structure of cupric oxide nano piece using a stage reduction method obtain platinum by the present invention
Nano-particle/cupric oxide plate composite.
The nano platinum particle/cupric oxide plate compound has efficient peroxidase activity, exists in hydrogen peroxide
In the case of, can efficiently catalyzing and oxidizing substrate molecule, the certain color change of presentation.For example, nano platinum particle/cupric oxide plate is multiple
Compound, can be with the tetramethyl benzidine (TMB) of catalytic substrate 3,3', 5,5'-, o-phenylenediamine in the presence of hydrogen peroxide
Or 2'- hydrazines (OPD)-bis- -3- ethyl benzo thiazole phenanthrolines -6- sulfonic acid (ABTS) oxidations, are presented peroxidase activity, and present
The color of corresponding oxide.
Second aspect, the invention provides a kind of preparation method of nano platinum particle/cupric oxide plate composite, including such as
Lower step：
(1) soluble copper salt and surfactant are dissolved in water, add sodium hydroxide solution, after uniform stirring, turned
Enter in reactor, 120~180 DEG C of 6~8h of reaction, centrifugation, dispersion obtains the dispersion liquid of cupric oxide nano piece；
(2) chloroplatinic acid is added in the dispersion liquid of cupric oxide nano piece, is stirred under ice bath, sodium borohydride reduction agent is added dropwise,
Drip reaction 2h；After reaction terminates, the solution 8000rpm that will obtain centrifugation 10min is washed with water, and most lower floor is again at last
It is dispersed in water, obtains nano platinum particle/cupric oxide plate compound.
Further, soluble copper salt and the molal weight ratio of surfactant are 1 in step (1):1~22:1, preferably
2:1。
Further, the mol ratio of cupric oxide nano piece and chloroplatinic acid is 1 in step (2):1~5:1, preferably 3:1.
Further, in step (2) sodium borohydride and chloroplatinic acid mol ratio >=10:1.
Alternatively, the soluble copper salt is Copper dichloride dihydrate, Salzburg vitriol, Gerhardite or a hydration
Any one in copper acetate or two or more mixtures.Preferably Copper dichloride dihydrate.
Alternatively, the surfactant is polyvinylpyrrolidone, lauryl sodium sulfate or cetyl trimethyl
Any one in ammonium bromide or two or more mixtures.Preferably cetyl trimethylammonium bromide.
Used as preferred technical scheme, the present invention provides a kind of specific nano platinum particle/cupric oxide plate composite
Preparation method, specifically includes following steps：
(1) cupric oxide nano piece is prepared
0.5g Copper dichloride dihydrates and 0.5g CTAB are dispersed in 15mL water, the NaOH of 1mL0.3g/mL is added
Solution is added, and is stirred；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h；Reaction terminate after, 8000rpm from
Heart 10min, washes with water, and the lower floor after being most centrifuged at last is dispersed in water, the cupric oxide nano piece being dispersed in water；
(2) nano platinum particle/cupric oxide plate composite is prepared
To in the aqueous solution of 660 μ L 170mg/L cupric oxide nano pieces add 2.34mL ultra-pure waters, ultrasonic 10min, then
The molar concentration of 23.5 μ L Pt is added for the H of 19.3mM2PtCl6·6H2The O aqueous solution；Under conditions of ice bath is quickly stirred by
Drop is added dropwise 1mL 4.8mM NaBH4The aqueous solution, continues to stir 2h after completion of dropwise addition；After reaction terminates, 8000rpm centrifugation 10min,
Wash with water, the lower floor after being most centrifuged at last is dispersed in water, obtain cupric oxide/nano sheets of platinum layer composite.
The third aspect, the present invention provides foregoing nano platinum particle/cupric oxide plate compound answering in ascorbic acid is detected
With.
Nano platinum particle of the present invention/cupric oxide plate compound when hydrogen peroxide and ascorbic acid are added simultaneously,
Its peroxidase activity is suppressed, and the oxidation of substrate is suppressed.Because the concentration of rejection and ascorbic acid has dependence to imitate
Should, the color of oxidation substrates is also presented different suppression situations, it is possible to the detection of Ascorbic Acid is realized with colorimetric method.
Color change weakens and the absorption of specific wavelength is presented certain concentration dependant effect.The detection range of ascorbic acid is 1 μM
~0.6mM, lowest detection is limited to 1.8 μM.
The present invention lifts the stability of platinum grain using the cupric oxide of the lamellar structure of big specific surface area, not only improves
The dispersiveness and stability of nano platinum particle/cupric oxide plate composite, the catalysis activity of its peroxidase are also improved,
And then lift the sensitivity of material resistant bad hematic acid detection.
The present invention relates to raw material or reagent be ordinary commercial products, the operation being related to is unless otherwise specified
This area routine operation.
On the basis of common sense in the field is met, above-mentioned each optimum condition can be mutually combined, and obtain specific embodiment party
Formula.
The beneficial effects of the present invention are：
The present invention utilizes the property of the big specific surface area of lamella cupric oxide, and be supported on for Pt nanoparticle by a stage reduction method
In the lamellar structure of cupric oxide, nano platinum particle/cupric oxide plate composite is obtained, preparation process is simple is workable, right
The requirement of equipment is relatively low, and the present invention not only increases the stability of Pt nanoparticle while improve the peroxide of material
Enzymatic activity, and then significantly improve sensitivity and the selectivity of Ascorbic Acid detection.
Brief description of the drawings
Fig. 1 is cupric oxide nano piece (A) and nano platinum particle/cupric oxide plate composite prepared by the embodiment of the present invention 1
(B) transmission electron microscope picture；
Fig. 2 is the element energy spectrum analysis (EDS) of nano platinum particle/cupric oxide plate compound prepared by the embodiment of the present invention 1
Figure；
Fig. 3 is the X-ray diffraction spectrogram of nano platinum particle/cupric oxide plate composite prepared by the embodiment of the present invention 1；
Fig. 4 is the feelings that nano platinum particle/cupric oxide plate composite prepared by the embodiment of the present invention 1 exists in hydrogen peroxide
To the catalysis color change (A) of zymolyte molecule under condition, and the stability kinetics of Michaelis-Menten equation fitting analyzes curve (B) and Michaelis
The contrast form (C) of constant Km and Vmax and HRP
Fig. 5 be the embodiment of the present invention 1 prepare nano platinum particle/cupric oxide plate composite with hydrogen peroxide by Bu Tong dense
TMB after degree ascorbic acid effect aoxidizes variation diagram, color change figure and absorption and the ascorbic acid of repressed UV absorption
Concentration dependant effect.
Specific embodiment
The preferred embodiment of the present invention is described in detail below in conjunction with embodiment.It will be appreciated that following real
Being given merely to play descriptive purpose for example is applied, is not used to limit the scope of the present invention.The skill of this area
Art personnel can carry out various modifications and replacement in the case of without departing substantially from spirit of the invention and spirit to the present invention.
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.
Embodiment 1
In the present embodiment, nano platinum particle/cupric oxide plate composite is prepared by the following method, is specifically included following
Step：
(1) cupric oxide nano piece is prepared
0.5g Copper dichloride dihydrates and 0.5g CTAB are dispersed in 15mL water, the NaOH of 1mL0.3g/mL is added
Solution is added, and is stirred；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h.After reaction terminates, centrifugation is washed
Wash, the cupric oxide nano piece being dispersed in water.
(2) nano platinum particle/cupric oxide plate composite is prepared
To addition 2.34mL ultra-pure waters, ultrasonic 10min in the aqueous solution of 660 μ L170mg/L cupric oxide nano pieces.Then plus
Enter 23.5 μ L H2PtCl6·6H2O (19.3mM) aqueous solution.1mL NaBH are dropwise added dropwise under conditions of ice bath is quickly stirred4
The aqueous solution of (4.8mM), continues to stir 2h after completion of dropwise addition.After reaction terminates, centrifugation, washing obtains nano platinum particle/oxidation
Copper sheet composite.
Embodiment 2
In the present embodiment, nano platinum particle/cupric oxide plate composite is prepared by the following method, is specifically included following
Step：
(1) cupric oxide nano piece is prepared
1g Copper dichloride dihydrates and 1g CTAB are dispersed in 15mL water, 1mL is added
The sodium hydroxide solution of 0.3g/mL is added, and is stirred；Reaction solution is transferred in 20mL reactors, 120 DEG C anti-
Answer 6h.After reaction terminates, centrifugation, washing, the cupric oxide nano piece being dispersed in water.
(2) nano platinum particle/cupric oxide plate composite is prepared
To addition 2.78mL ultra-pure waters, ultrasonic 10min in the aqueous solution of 220 μ L170mg/L cupric oxide nano pieces.Then plus
Enter 23.5 μ L H2PtCl6·6H2O (19.3mM) aqueous solution.1.5mL NaBH are dropwise added dropwise under conditions of ice bath is quickly stirred4
The aqueous solution of (4.8mM), continues to stir 2h after completion of dropwise addition.After reaction terminates, centrifugation, washing obtains nano platinum particle/oxidation
Copper sheet composite.
Embodiment 3
In the present embodiment, nano platinum particle/cupric oxide plate composite is prepared by the following method, is specifically included following
Step：
(1) cupric oxide nano piece is prepared
0.4g Copper dichloride dihydrates and 0.1g CTAB are dispersed in 15mL water, the NaOH of 1mL0.3g/mL is added
Solution is added, and is stirred；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h.After reaction terminates, centrifugation is washed
Wash, the cupric oxide nano piece being dispersed in water.
(2) nano platinum particle/cupric oxide plate composite is prepared
To addition 1.9mL ultra-pure waters, ultrasonic 10min in the aqueous solution of 1.1mL 170mg/L cupric oxide nano pieces.Then plus
Enter 23.5 μ L H2PtCl6·6H2O (19.3mM) aqueous solution.2mL NaBH are dropwise added dropwise under conditions of ice bath is quickly stirred4
The aqueous solution of (4.8mM), continues to stir 2h after completion of dropwise addition.After reaction terminates, centrifugation, washing obtains nano platinum particle/oxidation
Copper sheet composite.
Embodiment 4
The cupric oxide nano piece prepared to embodiment 1 using transmission electron microscope (FEI Co. of the Tecnaig2 20S-Twin U.S.)
Characterized with nano platinum particle/cupric oxide plate composite, it can be seen in fig. 1 that copper oxide particle prepared by embodiment 1
Pattern is nano-sheet, is about 0.5-2 μm, wide about 0.5 μm；Nano platinum particle is uniformly dispersed in the table of lamellar structure in Figure 1B
Face, size is 10~20nm or so, illustrates to be successfully prepared nano platinum particle/cupric oxide plate composite.
(Horiba X are penetrated to carry out EDS energy-spectrum scannings to nano platinum particle/cupric oxide plate composite prepared by embodiment 1
Line energy disperse spectroscopy, HIT), Fig. 2 is its EDS energy-spectrum scanning figure.Copper coin can be clearly found out from the result of spectrogram
The presence of plain (Cu), oxygen element (O) and platinum element (Pt), and signal intensity is very high, illustrates that nano platinum particle/cupric oxide plate is combined
There are three kinds of presence of element in material；Additionally, due to silicon chip need to be used as the substrate of material, so there is element silicon (Si) in spectrogram
Signal.
Nano platinum particle/the oxidation prepared to embodiment 1 using x-ray diffractometer (Bruker companies of D8focus Germany)
Copper sheet composite carries out X-ray diffraction measure, and Fig. 3 is the x-ray diffraction pattern for obtaining.As can be seen from the figure prepare
The characteristic diffraction peak of nano platinum particle/cupric oxide plate composite include simultaneously cupric oxide CuO (11-1), (20-2), (020),
(202) and Pt nanoparticle Pt (111), the characteristic diffraction peak of (220) and each diffraction maximum there are different intensity, show successfully
Prepare nano platinum particle/cupric oxide plate composite.
The test of the nano platinum particle/cupric oxide plate composite peroxidase activity property prepared to embodiment 1, surveys
Method for testing is as follows：
To different zymolyte molecular oxygens in the nano platinum particle/cupric oxide plate composite and hydrogen peroxide of the preparation of embodiment 1
Change, and change substrate molecule concentration, the Michaelis of the peroxidase activity for obtaining material is fitted to catalytic
Constant and maximum reaction rate.
Various concentrations ascorbic acid and TMB molecules are added in nano platinum particle/cupric oxide plate composite and hydrogen peroxide,
Inhibition of the various concentrations ascorbic acid to catalytic substrate molecule is obtained, and then relies on colorimetric method Ascorbic Acid molecular concentration
Detected, obtained detection range and test limit.
Fig. 4 is that nano platinum particle/cupric oxide plate composite prepared by embodiment 1 is right in the presence of hydrogen peroxide
The catalysis color change (A) of zymolyte molecule, and the stability kinetics of Michaelis-Menten equation fitting analyzes curve (B) and Michaelis constant Km
And the contrast form (C) of Vmax and HRP.Can see that nano platinum particle/cupric oxide plate composite is deposited in hydrogen peroxide from figure
When, substrate molecule TMB, OPD and ABTS can be aoxidized, obvious color change is presented.It is fitted by Michaelis-Menten equation
Afterwards, it is found that complex has with enzyme molecule HRP suitable catalytic capability, material is to substrate molecule TMB and H2O2Affinity slightly show
Enhancing, maximum reaction rate also has a certain degree of increase, shows the peroxidase activity of material.
Fig. 5 is the nano platinum particle/cupric oxide plate composite and hydrogen peroxide prepared using embodiment 1 by various concentrations
TMB after ascorbic acid effect aoxidizes variation diagram (Fig. 5 A), color change figure (illustration) and the absorption of repressed UV absorption
With the concentration dependant effect (Fig. 5 B) of ascorbic acid.Can clearly find out that embodiment 1 is made from spectrogram and color change is absorbed
Standby cupric oxide nano piece is suppressed to the catalysis oxidation of TMB molecules.It is inhibited effect and ascorbic acid according to inhibition level
The dependence of concentration, obtains the detection range and test limit of ascorbic acid after linear fit.The detection range of ascorbic acid is 0.6
μM~1mM, lowest detection is limited to 1.8 μM.
Embodiment 5
In the present embodiment, nano platinum particle/cupric oxide plate composite is prepared by the following method, is specifically included following
Step：
(1) cupric oxide nano piece is prepared
The nitric hydrate copper of 0.7g bis- and 0.5g CTAB are dispersed in 15mL water, the NaOH of 1mL0.3g/mL is added
Solution is added, and is stirred；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h.After reaction terminates, centrifugation is washed
Wash, the cupric oxide nano piece being dispersed in water.
(2) nano platinum particle/cupric oxide plate composite is prepared
To addition 1.9mL ultra-pure waters, ultrasonic 10min in the aqueous solution of 1.1mL 170mg/L cupric oxide nano pieces.Then plus
Enter 23.5 μ L H2PtCl6·6H2O (19.3mM) aqueous solution.2mL NaBH are dropwise added dropwise under conditions of ice bath is quickly stirred4
The aqueous solution of (4.8mM), continues to stir 2h after completion of dropwise addition.After reaction terminates, centrifugation, washing obtains nano platinum particle/oxidation
Copper sheet composite.
Embodiment 6
In the present embodiment, nano platinum particle/cupric oxide plate composite is prepared by the following method, is specifically included following
Step：
(1) cupric oxide nano piece is prepared
0.5g Copper dichloride dihydrates and 0.37g lauryl sodium sulfate are dispersed in 15mL water, 1mL0.3g/mL is added
Sodium hydroxide solution add, stir；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h.Reaction terminates
Afterwards, it is centrifuged, washing, the cupric oxide nano piece being dispersed in water.
(2) nano platinum particle/cupric oxide plate composite is prepared
To addition 1.9mL ultra-pure waters, ultrasonic 10min in the aqueous solution of 1.1mL 170mg/L cupric oxide nano pieces.Then plus
Enter 23.5 μ L H2PtCl6·6H2O (19.3mM) aqueous solution.2mL NaBH are dropwise added dropwise under conditions of ice bath is quickly stirred4
The aqueous solution of (4.8mM), continues to stir 2h after completion of dropwise addition.After reaction terminates, centrifugation, washing obtains nano platinum particle/oxidation
Copper sheet composite.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of nano platinum particle/cupric oxide plate composite, it is characterised in that it is that surface is dispersed nano platinum particle
Cupric oxide nano piece；0.5~2 μm of the cupric oxide nano length of a film, it is wide 0.4~0.6 μm；The nano platinum particle diameter 10~
20nm。
2. nano platinum particle according to claim 1/cupric oxide plate composite, it is characterised in that the platinum nanoparticle
Son/cupric oxide plate composite reduces chloroplatinic acid and prepares by a step in the dispersion liquid of cupric oxide nano piece.
3. the preparation method of a kind of nano platinum particle/cupric oxide plate composite, it is characterised in that comprise the following steps：
(1) soluble copper salt and surfactant are dissolved in water, add sodium hydroxide solution, after uniform stirring, be transferred to anti-
Answer in kettle, 120~180 DEG C of 6~8h of reaction, centrifugation, dispersion obtains the dispersion liquid of cupric oxide nano piece；
(2) chloroplatinic acid is added in the dispersion liquid of cupric oxide nano piece, is stirred under ice bath, sodium borohydride reduction agent is added dropwise, be added dropwise
Complete reaction 2h；After reaction terminates, the solution centrifugal that will be obtained, washing, dispersion obtain nano platinum particle/cupric oxide plate compound.
4. preparation method according to claim 3, it is characterised in that soluble copper salt and surfactant in step (1)
Molal weight ratio be 1:1~22:1.
5. preparation method according to claim 3, it is characterised in that cupric oxide nano piece and chloroplatinic acid in step (2)
Mol ratio is 1:1~5:1.
6. preparation method according to claim 3, it is characterised in that in step (2) sodium borohydride and chloroplatinic acid mole
Than >=10:1.
7. the preparation method according to claim 3~6 any one, it is characterised in that the soluble copper salt is two water
Any one in conjunction copper chloride, Salzburg vitriol, Gerhardite or copper acetate monohydrate or two or more mixing
Thing.
8. the preparation method according to claim 3~6 any one, it is characterised in that the surfactant is poly- second
Any one in alkene pyrrolidone, lauryl sodium sulfate or cetyl trimethylammonium bromide or two or more mixing
Thing.
9. preparation method according to claim 3, it is characterised in that comprise the following steps：
(1) cupric oxide nano piece is prepared
0.5g Copper dichloride dihydrates and 0.5g CTAB are dispersed in 15mL water, the sodium hydroxide solution of 1mL0.3g/mL is added
Add, stir；Reaction solution is transferred in 20mL reactors, 120 DEG C of reaction 6h；After reaction terminates, centrifugation, washing is obtained
To the cupric oxide nano piece being dispersed in water；
(2) nano platinum particle/cupric oxide plate composite is prepared
It is subsequently adding to 2.34mL ultra-pure waters, ultrasonic 10min is added in the aqueous solution of 660 μ L 170mg/L cupric oxide nano pieces
The molar concentration of 23.5 μ L Pt is the H of 19.3mM2PtCl6·6H2The O aqueous solution；Dropwise dripped under conditions of ice bath is quickly stirred
Plus 1mL 4.8mM NaBH4The aqueous solution, continues to stir 2h after completion of dropwise addition；After reaction terminates, centrifugation, washing, dispersion obtains oxygen
Change copper/nano sheets of platinum layer composite.
10. application of the nano platinum particle described in the claim 1 or 2/cupric oxide plate compound in ascorbic acid is detected.
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