CN105883891A - Preparation method of regular-dodecahedron cuprous oxide micro/nanocrystals - Google Patents
Preparation method of regular-dodecahedron cuprous oxide micro/nanocrystals Download PDFInfo
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- CN105883891A CN105883891A CN201410746520.7A CN201410746520A CN105883891A CN 105883891 A CN105883891 A CN 105883891A CN 201410746520 A CN201410746520 A CN 201410746520A CN 105883891 A CN105883891 A CN 105883891A
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- copper oxide
- dodecahedron
- oxide micro
- regular dodecahedron
- red copper
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Abstract
The invention discloses a preparation method of regular-dodecahedron cuprous oxide nanocrystals. The method comprises the following steps: by using a copper salt and N,N-dimethylformamide (DMF) as raw materials and polyvinylpyrrolidone as a structural guide agent, carrying out solvothermal reaction in a teflon high-pressure reaction kettle at 170 DEG C for 4-8 hours, and carrying out centrifugation, washing and drying on the obtained brick red precipitate to obtain the regular-dodecahedron cuprous oxide nano material. By using the copper salt and hydroxylamine hydrochloride as the raw materials and avoiding using the surfactant, template or any other organic additive, the raw materials are cheap and accessible, thereby lowering the cost. The method has the characteristics of simple equipment and the like, is convenient to operate, and is beneficial to implementing large-scale industrial production. The prepared regular-dodecahedron cuprous oxide nanocrystals have large specific area and multiple active spots, and thus, have potential application value in the aspects of photocatalytic degradation of dyes, gas sensitivity, energy storage, lithium batteries and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of Red copper oxide, particularly relate to a kind of regular dodecahedron Red copper oxide micro nanocrystalline
Preparation method.
Background technology
Red copper oxide is a kind of important Inorganic Chemicals, in coating, glass, pottery, plastics, agricultural and Industrial Catalysis
Purposes widely is suffered from field.In numerous semiconductor light-catalyst materials, Cu2O has good photocatalysis performance,
Become the research direction that photocatalysis field is new.Micro-nano Red copper oxide can make full use of sunlight, it is not necessary to ultraviolet light, energy consumption is low,
Efficiency is high, cost-effective, and the preparation of the most micro-nano Red copper oxide becomes the focus of research at present.Due to Cu2The pattern of O and knot
Structure affects its physics and chemical property, therefore, synthesis controllable appearance and the micro-nano Cu of structure to a great extent2O has become and has ground
The emphasis studied carefully.At present, existing many about Cu2O nano material preparation process controls its pattern and size to optimize its corresponding properties
Achievement in research report, such as scientific research person has used the method systems such as solid phase method, vapour deposition process, solvent-thermal method and electrochemical deposition
For synthesizing Cu2The patterns such as O nano wire, hollow ball, thin film, octahedron and dodecahedron.But the positive dodecahedro of micro/nano level
Body Red copper oxide micro nanocrystalline seldom has been reported that.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, seek to design being layered flower-shaped cuprous nano structure a kind of preparation
Method, the invention provides with mantoquita and oxammonium hydrochloride. as raw material, and distilled water is the method that positive tetrahedron Red copper oxide prepared by solvent.
The object of the present invention is achieved like this, with copper chloride, copper sulfate or copper acetate for copper source, with N, N-dimethyl formyl
Amine (DMF) is reducing agent, with PVP as structure directing agent, carries out molten in politef autoclave
Agent thermal response, directly prepares the regular dodecahedron Red copper oxide of micro/nano level.
The present invention prepares specifically comprising the following steps that of Red copper oxide regular dodecahedron structure
(1) 2.5mmol mantoquita, 1g PVP are dissolved in 25mL DMF (DMF), stir under room temperature to
Clarification；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction certain time at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.
Further, described mantoquita is the one in copper chloride, copper sulfate and copper acetate, and the response time is 4h, 6h or 8h.
The present invention utilizes mantoquita, DMF (DMF) to be raw material, and these low in raw material price are easy to get, and reduce
Cost.The features such as it is simple that the present invention also has equipment, easy to operate, are advantageously implemented large-scale commercial production.Prior
That the present invention has obtained novel regular dodecahedron Red copper oxide and has a uniform structure, and uniformly superstructure due to have low-density,
The character such as high-ratio surface have the most wide application prospect at aspects such as wastewater pollutants absorption, hydrogen storage, catalyst carriers.
Accompanying drawing explanation
Fig. 1 is prepared scanning electron microscope (SEM) photo being layered flower-shaped cuprous nano material of example 1.
Fig. 2 is the prepared X ray diffracting spectrum being layered flower-shaped cuprous nano material of example 1.
Detailed description of the invention
Below by way of specific embodiment for further illustrating the method that the present invention describes, it is not intended that the present invention is limited to
These embodiments.
Embodiment 1:
(1) 2.5mmol Copper dichloride dihydrate (0.4262g), 1g PVP are dissolved in 25mLN, dinethylformamide (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 16h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Red copper oxide obtained by preparation
Regular dodecahedron superstructure is characterized by scanning electron microscope, as Fig. 1 (a) be gained Red copper oxide be regular dodecahedron structure,
Regular dodecahedron granularity is 1～2.5 μm.If Fig. 1 (b) is the amplification SEM spectrogram of regular dodecahedron Red copper oxide superstructure,
It can be seen that regular dodecahedron Red copper oxide structural integrity.Regular dodecahedron cuprous nano material obtained by preparation
Material, by X-ray diffraction analysis, obtains as pure cuprous oxide crystal material (Fig. 2).
Embodiment 2:
(1) 2.5mmol copper sulfate pentahydrate (0.6242g), 1g PVP are dissolved in 25mL DMF (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 16h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 2～
4μm。
Embodiment 3:
(1) 2.5mmol copper acetate dihydrate (0.4991g), 1g PVP are dissolved in 25mL DMF (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 16h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 3～
4.5μm。
Embodiment 4:
(1) 2.5mmol Copper dichloride dihydrate (0.4262g), 1g PVP are dissolved in 25mLN, dinethylformamide (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 24h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 2～
3.5μm。
Embodiment 5:
(1) 2.5mmol copper sulfate pentahydrate (0.6242g), 1g PVP are dissolved in 25mL DMF (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 24h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 2～
4.5μm。
Embodiment 6:
(1) 2.5mmol copper acetate dihydrate (0.4991g), 1g PVP are dissolved in 25mL DMF (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 24h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 2～
4.5μm。
Embodiment 7:
(1) 2.5mmol Copper dichloride dihydrate (0.4262g), 1g PVP are dissolved in 25mL DMF (DMF),
Stir to clarify under room temperature；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction 24h at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.Regular dodecahedron granularity be 2～
4.5μm。
Claims (4)
1. a preparation method for regular dodecahedron Red copper oxide micro nanocrystalline, it comprises the steps:
(1) 2.5mmol mantoquita, 1g PVP are dissolved in 25mLN, dinethylformamide (DMF), stir under room temperature to
Clarification；
(2) after above-mentioned solution poured in 50mL politef autoclave hydro-thermal reaction certain time at 170 DEG C.
(3), after reaction terminates, the brick-red precipitation obtained is taken out, then with distilled water and the washing of dehydrated alcohol alternating centrifugal,
Then it is dried in the vacuum drying oven of 60 DEG C, obtains regular dodecahedron Red copper oxide micro nanocrystalline.
The method preparing regular dodecahedron Red copper oxide micro nanocrystalline the most according to claim 1, it is characterised in that used
Mantoquita is the one in copper nitrate, copper sulfate and copper acetate.
The method preparing regular dodecahedron Red copper oxide micro nanocrystalline the most according to claim 1, it is characterised in that solvent
The heat time is 2～6h.
The method preparing regular dodecahedron Red copper oxide micro nanocrystalline the most according to claim 1, it is characterised in that made
Standby positive tetrahedron Red copper oxide micro nanocrystalline structure is homogeneous, and particle diameter is 1～4.5 μm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112093817A (en) * | 2020-10-29 | 2020-12-18 | 广西师范大学 | Preparation method of cuprous oxide dendritic crystal |
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2014
- 2014-12-05 CN CN201410746520.7A patent/CN105883891A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112093817A (en) * | 2020-10-29 | 2020-12-18 | 广西师范大学 | Preparation method of cuprous oxide dendritic crystal |
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Application publication date: 20160824 |