CN109967077A - Nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method and application - Google Patents
Nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method and application Download PDFInfo
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- CN109967077A CN109967077A CN201910189279.5A CN201910189279A CN109967077A CN 109967077 A CN109967077 A CN 109967077A CN 201910189279 A CN201910189279 A CN 201910189279A CN 109967077 A CN109967077 A CN 109967077A
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- powder
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- porous copper
- cuprous oxide
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000010949 copper Substances 0.000 title claims abstract description 75
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 70
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 69
- 239000000843 powder Substances 0.000 title claims abstract description 68
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 239000011258 core-shell material Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 14
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 14
- 230000015556 catabolic process Effects 0.000 description 13
- 238000006731 degradation reaction Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
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- 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
- B01J23/72—Copper
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/396—
-
- B01J35/60—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
Nano porous copper disclosed by the invention/cuprous oxide nucleocapsid micro-powder preparation method, preset reaction temperature, under atmospheric environment after temperature rises to preset reaction temperature, nano porous copper powder is kept the temperature into a period of time at the reaction temperatures, it then cools to room temperature to get nano porous copper/cuprous oxide nucleocapsid micro-powder.Invention additionally discloses using nano porous copper obtained/cuprous oxide nucleocapsid micro-powder as the application of photochemical catalyst.The present invention prepares nano porous copper/cuprous oxide nucleocapsid micro-powder, preparation method is simple for this, is easy to volume production by carrying out thermal oxidation to nano porous copper micro-powder；And the micro-powder being prepared has three-dimensional co-continuous nanoporous core-shell structure and higher photocatalytic activity, and is easy to recycle after photocatalysis.
Description
Technical field
The invention belongs to metal oxide semiconductor material technical fields, and in particular to a kind of nano porous copper/oxidation is sub-
The preparation method of copper nucleocapsid micro-powder further relates to the application of the nano porous copper/cuprous oxide nucleocapsid micro-powder.
Background technique
Cuprous oxide (Cu2O p-type semiconductor material, forbidden bandwidth 2.1eV, in sensing, catalysis, battery) are important
The fields such as electrode are with important application prospects.Nano porous copper/oxidation is prepared by thermal oxide nano porous copper micro-powder
The method of cuprous nucleocapsid micro-powder is simple and easy, and prepared nano porous copper/cuprous oxide nucleocapsid micro-powder has both three
The features such as co-continuous nanoporous core-shell structure, high surface are tieed up, show preferable photocatalysis performance, and be easily recycled
It utilizes.
Summary of the invention
The purpose of the present invention is to provide a kind of nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method, systems
Standby obtained nano porous copper/cuprous oxide nucleocapsid micro-powder have apparent three-dimensional co-continuous nanoporous core-shell structure with
And higher photocatalytic activity.
Another object of the present invention, which also resides in, provides above-mentioned nano porous copper/cuprous oxide nucleocapsid micro-powder in photocatalysis
Application in agent.
A kind of technical solution of the present invention is: nano porous copper/cuprous oxide nucleocapsid micro-powder preparation side
Method is specifically implemented according to the following steps:
Reaction temperature is preset, under atmospheric environment after temperature rises to preset reaction temperature, by nano porous copper
Powder keeps the temperature a period of time at the reaction temperatures, then cools to room temperature to get nano porous copper/cuprous oxide nucleocapsid powder and micron
Body.
The features of the present invention also characterized in that
Preset reaction temperature is adjusted using warm table heating, the nano porous copper powder is placed on the warm table
Carry out isothermal holding.
The partial size of the nano porous copper powder is 300~1000 mesh.
The reaction temperature is 150~200 DEG C, and soaking time is 1~60min.
The type of cooling is natural cooling.
Another technical solution of the present invention is: the application of nano porous copper/cuprous oxide nucleocapsid micro-powder,
The nano porous copper being prepared using the above method/cuprous oxide nucleocapsid micro-powder is as the application of photochemical catalyst.
The beneficial effects of the present invention are: the present invention is by carrying out thermal oxidation, preparation to nano porous copper micro-powder
Nano porous copper/cuprous oxide nucleocapsid micro-powder out, preparation method is simple for this, is easy to volume production；And be prepared
Micro-powder has three-dimensional co-continuous nanoporous core-shell structure and higher photocatalytic activity, and recycling benefit is easy after photocatalysis
With.
Detailed description of the invention
Fig. 1 is the obtained nano porous copper of the embodiment of the present invention 1/cuprous oxide nucleocapsid micro-powder XRD spectrum；
Fig. 2 is the obtained nano porous copper of the embodiment of the present invention 1/cuprous oxide nucleocapsid micro-powder SEM photograph；
Fig. 3 is the obtained nano porous copper of the embodiment of the present invention 1/cuprous oxide nucleocapsid micro-powder in photocatalytic degradation
The absorption spectrum of methyl orange solution in experiment；
Fig. 4 is the obtained nano porous copper of the embodiment of the present invention 1/cuprous oxide nucleocapsid micro-powder in photocatalytic degradation
The degradation curve of methyl orange solution in experiment.
Specific embodiment
Nano porous copper of the invention/cuprous oxide nucleocapsid micro-powder preparation method, it is specifically real according to the following steps
It applies:
150~200 DEG C are preset on warm table, after the temperature of thermal station to be added rises to preset temperature from room temperature, by grain
Diameter is placed in 1~60min of heat preservation, cooled to room temperature on warm table for the nano porous copper powder of 300~1000 mesh and obtains
Nano porous copper/cuprous oxide nucleocapsid micro-powder.
The nano porous copper/cuprous oxide nucleocapsid micro-powder can carry out light-catalyzed reaction directly as photochemical catalyst.
Nano porous copper micro-powder is placed on warm table by preparation method of the invention, passes through thermal oxide nanoporous
Copper micro-powder prepares nano porous copper/cuprous oxide nucleocapsid micro-powder, and preparation method is simple for this, is easy to volume production；
And nano porous copper obtained/cuprous oxide nucleocapsid micro-powder has apparent three-dimensional co-continuous nanoporous nucleocapsid knot
The features such as recycling is easy after structure, higher photocatalytic activity, photocatalysis.
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Nano porous copper disclosed in the present embodiment/cuprous oxide nucleocapsid micro-powder preparation method, specifically includes step:
It is 180 DEG C that heating temperature is preset on warm table, and after the temperature of thermal station to be added rises to preset temperature from room temperature, partial size is existed
The nano porous copper powder of 300~500 mesh ranges, which is placed on warm table, keeps the temperature 60min, and cooled to room temperature can be prepared
Nano porous copper/cuprous oxide nucleocapsid micro-powder.
Fig. 1 is nano porous copper manufactured in the present embodiment/cuprous oxide nucleocapsid micro-powder XRD diagram, can from Fig. 1
Out, Cu and Cu is contained in the nano porous copper that the present invention prepares/cuprous oxide nucleocapsid micro-powder2Two kinds of object phases of O；Fig. 2 is
Nano porous copper manufactured in the present embodiment/cuprous oxide nucleocapsid micro-powder SEM figure, as can be seen from Figure 2, present invention preparation
Nano porous copper out/cuprous oxide nucleocapsid micro-powder has apparent three-dimensional co-continuous nano-porous structure.
The present embodiment be also disclosed using nano porous copper obtained/cuprous oxide nucleocapsid micro-powder as photochemical catalyst into
Row photocatalytically degradating organic dye, specific experiment process are as follows:
Using prepared nano porous copper/cuprous oxide nucleocapsid micro-powder as photochemical catalyst (0.2g/L), degradation
The methyl orange solution of 10mg/L.Light source used is 300W xenon lamp in photocatalysis experiment.Before irradiation, the methyl containing photochemical catalyst
Orange solution stirs 30min in the dark, carries out illumination after reaching adsorption equilibrium.Fig. 3 is the obtained nanoporous of the present embodiment
The absorption spectrum of copper/cuprous oxide nucleocapsid micro-powder methyl orange solution in photocatalytic degradation experiment, Fig. 4 is the present embodiment institute
The degradation curve of obtained nano porous copper/cuprous oxide nucleocapsid micro-powder methyl orange solution in photocatalytic degradation experiment.
Nano porous copper/cuprous oxide nucleocapsid micro-powder photochemical catalyst reaches the degradation rate of methyl orange solution after 15min
99.81%.
Embodiment 2
Nano porous copper disclosed in the present embodiment/cuprous oxide nucleocapsid micro-powder preparation method, specifically includes step:
It is 150 DEG C that heating temperature is preset on warm table, after the temperature of thermal station to be added rises to preset temperature from room temperature, is by partial size
The nano porous copper powder of 300~500 mesh, which is placed on warm table, keeps the temperature 30min, and cooled to room temperature can prepare nanometer
Porous Cu/cuprous oxide nucleocapsid micro-powder.
The present embodiment is also disclosed using nano porous copper produced by the present invention/cuprous oxide nucleocapsid micro-powder as light and urges
Agent carries out photocatalytically degradating organic dye, and specific experiment process is as follows:
Using prepared nano porous copper/cuprous oxide nucleocapsid micro-powder as photochemical catalyst (0.2g/L), degradation
The methyl orange solution of 10mg/L.Light source used is 300W xenon lamp in photocatalysis experiment.Before irradiation, the methyl containing photochemical catalyst
Orange solution stirs 30min in the dark, carries out illumination after reaching adsorption equilibrium, nano porous copper/cuprous oxide light is urged after 15min
Agent reaches 97.67% to the degradation rate of methyl orange solution.
Embodiment 3
Nano porous copper disclosed in the present embodiment/cuprous oxide nucleocapsid micro-powder preparation method, specifically includes step:
It is 160 DEG C that heating temperature is preset on warm table, after the temperature of thermal station to be added rises to preset temperature from room temperature, is by partial size
The nano porous copper powder of 1000 mesh, which is placed on warm table, keeps the temperature 10min, and cooled to room temperature can prepare nanoporous
Copper/cuprous oxide nucleocapsid micro-powder.
The present embodiment be also disclosed using nano porous copper obtained/cuprous oxide nucleocapsid micro-powder as photochemical catalyst into
Row photocatalytically degradating organic dye, specific experiment process are as follows:
Using prepared nano porous copper/cuprous oxide nucleocapsid micro-powder as photochemical catalyst (0.2g/L), degradation
The methyl orange solution of 10mg/L.Light source used is 300W xenon lamp in photocatalysis experiment.Before irradiation, the methyl containing photochemical catalyst
Orange solution stirs 30min in the dark, carries out illumination after reaching adsorption equilibrium, nano porous copper/cuprous oxide light is urged after 15min
Agent reaches 95.42% to the degradation rate of methyl orange solution.
Embodiment 4
Nano porous copper disclosed in the present embodiment/cuprous oxide nucleocapsid micro-powder preparation method, specifically includes step:
It is 200 DEG C that heating temperature is preset on warm table, after the temperature of thermal station to be added rises to preset temperature from room temperature, is by partial size
The nano porous copper powder of 500~700 mesh, which is placed on warm table, keeps the temperature 1min, and cooled to room temperature can prepare nanometer
Porous Cu/cuprous oxide nucleocapsid micro-powder.
The present embodiment be also disclosed using nano porous copper obtained/cuprous oxide nucleocapsid micro-powder as photochemical catalyst into
Row photocatalytically degradating organic dye, specific experiment process are as follows:
Using prepared nano porous copper/cuprous oxide nucleocapsid micro-powder as photochemical catalyst (0.2g/L), degradation
The methyl orange solution of 10mg/L.Light source used is 300W xenon lamp in photocatalysis experiment.Before irradiation, the methyl containing photochemical catalyst
Orange solution stirs 30min in the dark, carries out illumination after reaching adsorption equilibrium, nano porous copper/cuprous oxide light is urged after 15min
Agent reaches 96.58% to the degradation rate of methyl orange solution.
Embodiment 5
Nano porous copper disclosed in the present embodiment/cuprous oxide nucleocapsid micro-powder preparation method, specifically includes step:
It is 190 DEG C that heating temperature is preset on warm table, after the temperature of thermal station to be added rises to preset temperature from room temperature, is by partial size
The nano porous copper powder of 700~900 mesh, which is placed on warm table, keeps the temperature 60min, and cooled to room temperature can prepare nanometer
Porous Cu/cuprous oxide nucleocapsid micro-powder.
The present embodiment be also disclosed using nano porous copper obtained/cuprous oxide nucleocapsid micro-powder as photochemical catalyst into
Row photocatalytically degradating organic dye, specific experiment process are as follows:
Using prepared nano porous copper/cuprous oxide nucleocapsid micro-powder as photochemical catalyst (0.2g/L), degradation
The methyl orange solution of 10mg/L.Light source used is 300W xenon lamp in photocatalysis experiment.Before irradiation, the methyl containing photochemical catalyst
Orange solution stirs 30min in the dark, carries out illumination after reaching adsorption equilibrium, nano porous copper/cuprous oxide light is urged after 15min
Agent reaches 99.89% to the degradation rate of methyl orange solution.
The above-mentioned each embodiment of the present invention is prepared by the nano porous copper powder that thermal oxide partial size is 300~1000 mesh
Nano porous copper/cuprous oxide nucleocapsid micro-powder photochemical catalyst, the photochemical catalyst have significant degradation effect to methyl orange
Fruit.
Claims (6)
1. nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method, which is characterized in that specifically real according to the following steps
It applies:
Reaction temperature is preset, under atmospheric environment after temperature rises to preset reaction temperature, by nano porous copper powder
At the reaction temperatures heat preservation a period of time, then cool to room temperature to get nano porous copper/cuprous oxide nucleocapsid micro-powder.
2. nano porous copper as described in claim 1/cuprous oxide nucleocapsid micro-powder preparation method, which is characterized in that
Preset reaction temperature is adjusted using warm table heating, the nano porous copper powder is placed on the warm table and is kept the temperature
Processing.
3. nano porous copper as claimed in claim 1 or 2/cuprous oxide nucleocapsid micro-powder preparation method, feature exist
In the partial size of the nano porous copper powder is 300~1000 mesh.
4. nano porous copper as claimed in claim 1 or 2/cuprous oxide nucleocapsid micro-powder preparation method, feature exist
In the reaction temperature is 150~200 DEG C, and soaking time is 1~60min.
5. nano porous copper as claimed in claim 1 or 2/cuprous oxide nucleocapsid micro-powder preparation method, feature exist
In the type of cooling is natural cooling.
6. the application of nano porous copper/cuprous oxide nucleocapsid micro-powder, which is characterized in that as Claims 1 to 5 is prepared
Nano porous copper/application of the cuprous oxide nucleocapsid micro-powder as photochemical catalyst.
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| CN201910189279.5A CN109967077A (en) | 2019-03-13 | 2019-03-13 | Nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method and application |
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| CN201910189279.5A CN109967077A (en) | 2019-03-13 | 2019-03-13 | Nano porous copper/cuprous oxide nucleocapsid micro-powder preparation method and application |
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|---|---|---|---|---|
| US20090269269A1 (en) * | 2006-04-20 | 2009-10-29 | The Trustees Of Columbia University In City Of New York | Copper oxide nanoparticle system |
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| WO2016030753A1 (en) * | 2014-08-29 | 2016-03-03 | Sabic Global Technologies B.V. | Photocatalytic hydrogen production from water over catalysts having p-n juncations and plasmonic materials |
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| CN107986316A (en) * | 2017-11-20 | 2018-05-04 | 西安理工大学 | Nanoporous cupric oxide/cupric oxide nano line composite construction and preparation method thereof |
| CN108193255A (en) * | 2018-01-30 | 2018-06-22 | 河北工业大学 | A kind of supported porous cuprous nano piece composite material of nano porous copper and preparation method thereof |
-
2019
- 2019-03-13 CN CN201910189279.5A patent/CN109967077A/en active Pending
Patent Citations (6)
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| US20090269269A1 (en) * | 2006-04-20 | 2009-10-29 | The Trustees Of Columbia University In City Of New York | Copper oxide nanoparticle system |
| CN102350499A (en) * | 2011-09-28 | 2012-02-15 | 河北工业大学 | Cu/Cu2O core-shell composite microsphere and preparation method thereof |
| WO2016030753A1 (en) * | 2014-08-29 | 2016-03-03 | Sabic Global Technologies B.V. | Photocatalytic hydrogen production from water over catalysts having p-n juncations and plasmonic materials |
| CN106215824A (en) * | 2016-09-07 | 2016-12-14 | 南京理工大学 | A kind of Cu2the preparation method of O/Cu composite |
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| Title |
|---|
| KOU, TIANYI ET AL.: ""Nanoporous core-shell Cu@Cu2O nanocomposites with superior photocatalytic properties towards the degradation of methyl orange"", 《RSC ADVANCES》 * |
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