CN105129835A - Hexacosahedral cuprous oxide nanometer particle preparation method - Google Patents
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- C01G3/02—Oxides; Hydroxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention discloses a hexacosahedral cuprous oxide nanometer particle preparation method, which comprises: dissolving an inorganic copper salt in a solvent, adding an additive, adding an alkaline substance, adding a reducing agent, carrying out a reaction for 0.5-6 h at a temperature of 30-90 DEG C, carrying out centrifugation separation on the obtained reaction solution by controlling the rotation speed at 6000-8000 r/min, washing the obtained precipitate with deionized water until the pH value of the washing liquid is neutral, and drying by controlling the temperature at 40-80 DEG C so as to obtain the hexacosahedral cuprous oxide nanometer particles. According to the present invention, the hexacosahedral cuprous oxide nanometer particles have the special appearance, have more crystal surface exposing for photocatalysis, and can be used for photocatalytic degradation of organic pollutants, and the preparation method has characteristics of low cost and simple and controllable synthesis pathway, and is suitable for mass production.
Description
Technical field
The invention belongs to field of inorganic nano material, relate to a kind of cuprous nano particle, specifically a kind of preparation method of 20 hexahedron cuprous nano particles.
Background technology
Nano material has the characteristic being obviously different from block materials and individual molecule: surface effects, volume effect, quantum size effect and macroscopical tunnel effect etc.No matter in theory or in the application aspect of reality, the inorganic nanoparticles with uniform particle size and shape all causes the great interest of people.The synthesis of regular shape nanostructure has great using value in fields such as photon, nanoelectronics, information storage, catalysis and biosensors.
Red copper oxide (Cu
20) be rare can by the one of excited by visible light typical case P-type semiconductor material, its bandwidth is 2.17eV.Due to the physical and chemical performance of its excellence, cause the attention of people gradually in the potential using value of every field.Cu
20 has good gas sensing property and piezoelectricity, can is the excited by visible light of 400-800nm by wavelength; Polycrystalline state Cu
20 has satisfactory stability, can Reusability and can not be reduced to Cu or be oxidized to CuO; In addition, Cu
20 is nontoxic, rich reserves, and preparation cost is lower, cheap, and its purposes in each field obtains the research and development of people gradually, and plays a part indispensable in daily life.Such as: (1) in recent years, cuprous catalysis cross-coupling reaction oneself become popular research direction, and be widely used in organic synthesis, bioactive molecules preparation and industrial production in the middle of.(2) Cu
20 because of its have that cheapness, abundance are large, easily preparation, absorb visible ray, band gap can be in harmonious proportion the characteristics such as low toxicity, has widespread use in photocatalysis field.(3) Red copper oxide is this very wide as its industrial use of important Inorganic Chemicals, and it is the antifouling paint field being applied to boats and ships that Industrial products are greater than 90%, and this coating can be used as stain control agent, reaches antifouling object by seawater to its solvency action.(4) the oxide-metal matrix material prepared based on Red copper oxide is utilized, can as the application of non-burning anode with electrolysis process.Along with the development of Red copper oxide morphology control preparation method research, its using value also result in extensive concern, in the last few years, adopts different methods to prepare pattern and the controlled Cu of size
2the 0 nanocrystalline focus having become various countries researchist and paid close attention to.
2005, Choi group is once detailed have studied electrolyte temperature, electrolysis voltage, current density, concentration of electrolyte, reaction times and protective material to Cu
2the pattern impact of 0 crystal growth.This group also reports use three-electrode system, use SDS(sodium lauryl sulphate), tensio-active agent as negatively charged ion is adsorbed in crystal face from excellent, to obtain that crystalline form is cubes, to chamfer cubes, octahedron and rescinded angle octahedra in the pH scope of the hierarchy of control in (3.4,3.5,3.7,3.9).Guo also reports in the system without template and tensio-active agent, by regulating voltage when 0.6V, can obtain cube Cu
20, voltage can obtain Cu at 0.7V
20 nanometer ball.Li etc. also once reported that ([MEIN]+[at room temperature, electrolysis obtained Cu to ESD to hydrophilic ionic liquids
20.Cubes be can finally obtain at control ionic liquid content at (0-0.08%), cubes, octahedron, the Cu such as spherical chamfered
20.
Chen etc. are reactant with ammoniacal liquor and venus crystals, in the autoclave of polytetrafluoroethylene still lining, heat 150-245 ° of C, and reaction 5-72h, can obtain long cylindrical particle, and study its mechanism of nucleation.The trolamine such as Li, acetic acid acid copper and water are raw material, in autoclave, are heated to 160 DEG C and after continuing, by creating the Cu of octahedron and octahedra nucleocapsid shape after centrifugal, washing and drying
20 particle.Zeng etc. use DMF to substitute the hydro-thermal reaction method of water, have prepared Cu in the control final reaction times
20 hollow cubic body and hollow ball.Jiao group PEG-200 is that solvent obtains the Cu of size between 50nm-200nm
20 cubes.
Zhu Haitao uses polyvinylpyrrolidone to prepare hollow sphere made from cuprous oxide.Tan Qiang uses by force etc. urea to prepare octahedra Red copper oxide.Tao Feifei etc. utilize anhydrous sodium acetate and dextrose anhydrous to prepare Emission in Cubic Red copper oxide.
Li Yadong uses cupric nitrate to be copper source, and POTASSIUM BOROHYDRIDE is reductive agent, under oil bath, obtains the nanometer ball of about 250nm, but surperficial smoother, and surface-area thus specific surface area is relatively little.
In theory, the Red copper oxide with particular crystal plane is conducive to improving its photocatalysis performance.
In sum, the Red copper oxide with different crystal face is different for the efficiency of photocatalysis to degrade organic matter, so the Red copper oxide having special crystal face has larger benefit to practical application, therefore explore that relative cost is lower, simple to operate, the cuprous nano material with special crystal face and preparation method significant.And 20 hexahedron Red copper oxide prepared by present method have multiple crystal face, specific crystal face is wherein had to have potential application prospect in photocatalysis to degrade organic matter field.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation method of 20 hexahedron cuprous nano particles, the preparation method of described this 20 hexahedron cuprous nano particles solves that the method cost of preparation 20 hexahedron cuprous nano particle of the prior art is high, the technical problem of complex process.
The invention provides a kind of preparation method of 20 hexahedron cuprous nano particles, inorganic mantoquita is dissolved in solvent, add additive, then alkaline matter is added, add after reductive agent mixes subsequently, under 30-90 DEG C of condition, carry out reaction 0.5-6h, it is that 6000-8000r/min carries out centrifugation that the reaction solution of gained is controlled rotating speed, the precipitate with deionized water washing of gained be neutrality to the pH of elutant, then control temperature is 40-80 DEG C and dries, and namely obtains 20 hexahedron cuprous nano particles;
The material ratio of above-mentioned inorganic mantoquita, solvent, additive, alkaline matter and reductive agent used is 0.001-0.1mol:5-200ml:0.005-4g:0.05-0.4g:0.05-1g;
Wherein, described inorganic mantoquita is cupric nitrate, copper sulfate or cupric chloride;
Described solvent is the mixture of a kind of of water, ethanol, methyl alcohol or ethylene glycol and two or more composition;
Described additive is the mixture of a kind of of hydrochloric acid, quadrol or Trisodium Citrate and two or more composition;
Described alkaline matter is the mixture of a kind of and two or more composition of sodium hydroxide, potassium hydroxide, ammoniacal liquor or sodium bicarbonate;
Described reductive agent is the mixture of a kind of and two or more composition of formic acid, acetaldehyde, glucose or xitix.
Further, described inorganic mantoquita is cupric nitrate, described aqueous solvent, and described additive is quadrol, and described alkaline matter is sodium bicarbonate, and described reductive agent is glucose.
Further, the preparation method of above-mentioned a kind of 20 hexahedron cuprous nano particles, comprises the steps:
(1), inorganic mantoquita is dissolved in solvent obtains Inorganic Copper salts solution;
(2), in the Inorganic Copper salts solution of step (1) gained add additive, stir 10-20min, add alkaline matter and stir 10-20min, then add reductive agent, after being uniformly mixed, under 30-90 DEG C of condition, carry out reaction 0.5-6h;
(3) after, step (2) reaction terminates, the reaction solution of gained naturally cools to room temperature, then controlling rotating speed is that 6000-8000r/min carries out centrifugation, the precipitate with deionized water washing of gained be neutrality to the pH of elutant, then control temperature is 40 DEG C-80 DEG C and dries, and obtains 26 cuprous nano particles.
Present invention also offers by above-mentioned method obtain a kind of 20 hexahedron cuprous nano particles as the purposes in photocatalyst catalyze and degrade organic pollutants.
26 cuprous nano particles of above-mentioned gained, the crystal face of exposure is many, and thus it can be used for catalyze and degrade organic pollutants.When it is for catalyze and degrade organic pollutants, the specific crystal face had due to it is high to light-catalysed efficiency comparison, therefore can improve the catalytic efficiency of Red copper oxide as photocatalyst catalyze and degrade organic pollutants.
A kind of 20 hexahedron cuprous nano particles of the present invention, because the specific crystal face had is high to light-catalysed efficiency comparison, thus, when it reacts for catalyze and degrade organic pollutants, the catalytic efficiency of Red copper oxide as photocatalyst catalyze and degrade organic pollutants is improved.Preparation method of the present invention, owing to using hydrothermal method preparation, therefore have low production cost, preparation process is simply controlled, is applicable to the feature of scale operation.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope collection of illustrative plates of a kind of 20 hexahedron cuprous nano particles of embodiment 1 gained.
Fig. 2 is the wide-angle XRD figure of a kind of 20 hexahedron cuprous nano particles of embodiment 1 gained.
Fig. 3 is that a kind of 20 hexahedron Red copper oxide of embodiment 1 gained are to the degradation capability figure of tropeolin-D.
Embodiment
Below by specific embodiment, also the invention will be further described by reference to the accompanying drawings, but the present invention is not limited to following examples.
Method described in various embodiments of the present invention if no special instructions, is ordinary method.
Raw materials used without special instruction in various embodiments of the present invention, all can buy from open commercial sources and obtain.
The model of the instrument that various embodiments of the present invention are used or equipment and the information of manufacturer as follows:
Air dry oven, model DHG-9920A, manufacturer Shanghai one is permanent;
Xenon lamp, sea blue bright Electronics Co., Ltd. on visible light source XQ350W;
X-ray diffraction (XRD), PANalytical company of XPERTPRO Holland;
Ultraviolet-visible pectrophotometer, Shimadzu Corporation of UV-3600 Japan;
Scanning electronic microscope (SEM), S-3400N HIT.
embodiment 1
A preparation method for 20 hexahedron cuprous nano particles, specifically comprises the following steps:
(1) copper nitrate solution is obtained in the solvent, formed in 9ml deionized water by 0.02mol nitrate trihydrate copper dissolution;
(2), in the copper nitrate solution of step (1) gained add 0.1g quadrol, stir 10-20min, add 0.1g sodium hydroxide, finally add 0.2g formic acid, be uniformly mixed rear control temperature and carry out reaction 2h at 50 DEG C;
(3) after, step (3) hydro-thermal reaction terminates, controlling centrifugal rotational speed after the reaction solution of gained naturally cools to room temperature is that 6000r/min carries out centrifugation, the precipitate with deionized water washing of gained is dried to the pH of elutant for control temperature after neutral is 40-60 DEG C, obtains 20 hexahedron cuprous nano particles.
(4), the catalyzer of above-mentioned preparation is carried out photocatalytic degradation reaction, take 0.1g catalyzer, add the methyl orange solution 200mL that starting point concentration is 25mg/L, 30min is stirred under dark room conditions, make in catalyzer dispersion soln, and the absorption that reaches capacity, timing sampling, centrifugal, get supernatant liquid light-intensity method and analyze.
By the cuprous nano particle of above-mentioned gained by scanning electron microscopic observation, as shown in Figure 1, as can be seen from Figure 1 obtained cuprous nano particle has 26 to result.
Characterized by X-ray diffraction (XRD) by the cuprous nano particle of above-mentioned gained, as shown in Figure 2, as can be seen from Figure 2 its relative intensity is higher for the wide-angle XRD figure of gained, and show that the degree of crystallinity of sample is higher thus, pattern is very regular.
As can be seen from Figure 3 come, under the illumination condition of visible ray, with 0.1g 20 hexahedron Red copper oxide 200mL25mg/L degraded in 30 minutes and reach more than 90%, show that this Red copper oxide has strong catalytic activity to organic photocatalytic degradation.
embodiment 2
A kind of 20 hexahedron cuprous nano particles, specifically comprise the following steps:
(1), 0.34g nitrate trihydrate copper cupric chloride is dissolved cupric chloride in the solvent of 20 deionized water compositions;
(2), in the Cupric Chloride Solution of step (1) gained add 0.5g hydrochloric acid, stir 10-20min, add 0.1g sodium hydroxide, finally add 0.2g ascorbic acid, be uniformly mixed latter 70 DEG C and carry out reaction 4h;
(3) after, step (2) hydro-thermal reaction terminates, controlling centrifugal rotational speed after the reaction solution of gained naturally cools to room temperature is that 7000r/min carries out centrifugation, the precipitate with deionized water washing of gained is dried to the pH of elutant for control temperature after neutral is 60 DEG C, obtains cuprous nano particle.
embodiment 3
A preparation method for 20 hexahedron cuprous nano particles, specifically comprises the following steps:
(1), by 0.45g nitrate trihydrate copper dissolution in 27ml ethanol and 3ml deionized water composition solvent in;
(2), add in the copper nitrate solution of step (1) gained in 0.7g citric acid, stir 10-20min, add 0.3g ammoniacal liquor, add reductive agent 0.2g xitix, after being uniformly mixed, control temperature carries out reaction 6h at 90 DEG C;
(3) after, step (2) hydro-thermal reaction terminates, controlling centrifugal rotational speed after the reaction solution of gained naturally cools to room temperature is that 8000r/min carries out centrifugation, the precipitate with deionized water washing of gained is dried to the pH of elutant for control temperature after neutral is 60-80 DEG C, obtains cuprous nano particle.
In sum, 20 hexahedron cuprous nano particles of the present invention, expose many crystal faces, it will have higher catalytic efficiency for photocatalyst catalyze and degrade organic pollutants.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification all should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for 20 hexahedron cuprous nano particles, is characterized in that:
Inorganic mantoquita is dissolved in solvent, add additive, then alkaline matter is added, add after reductive agent mixes subsequently, under 30-90 DEG C of condition, carry out reaction 0.5-6h, it is that 6000-8000r/min carries out centrifugation that the reaction solution of gained is controlled rotating speed, the precipitate with deionized water washing of gained be neutrality to the pH of elutant, and then control temperature is 40-80 DEG C and dries, and namely obtains 20 hexahedron cuprous nano particles;
The material ratio of above-mentioned inorganic mantoquita, solvent, additive, alkaline matter and reductive agent used is 0.001-0.1mol:5-200ml:0.005-4g:0.05-0.4g:0.05-1g;
Wherein, described inorganic mantoquita is cupric nitrate, copper sulfate or cupric chloride;
Described solvent is the mixture of a kind of of water, ethanol, methyl alcohol or ethylene glycol and two or more composition;
Described additive is the mixture of a kind of of hydrochloric acid, quadrol or Trisodium Citrate and two or more composition;
Described alkaline matter is the mixture of a kind of and two or more composition of sodium hydroxide, potassium hydroxide, ammoniacal liquor or sodium bicarbonate;
Described reductive agent is the mixture of a kind of and two or more composition of formic acid, acetaldehyde, glucose or xitix.
2. the preparation method of a kind of 20 hexahedron cuprous nano particles as claimed in claim 1, it is characterized in that: described inorganic mantoquita is cupric nitrate, described aqueous solvent, described additive is quadrol, described alkaline matter is sodium bicarbonate, and described reductive agent is glucose.
3. the preparation method of a kind of 20 hexahedron cuprous nano particles as claimed in claim 1, is characterized in that comprising the steps:
(1), inorganic mantoquita is dissolved in solvent obtains Inorganic Copper salts solution;
(2), in the Inorganic Copper salts solution of step (1) gained add additive, stir 10-20min, add alkaline matter and stir 10-20min, then add reductive agent, after being uniformly mixed, under 30-90 DEG C of condition, carry out reaction 0.5-6h;
(3) after, step (2) reaction terminates, the reaction solution of gained naturally cools to room temperature, then controlling rotating speed is that 6000-8000r/min carries out centrifugation, the precipitate with deionized water washing of gained be neutrality to the pH of elutant, then control temperature is 40 DEG C-80 DEG C and dries, and obtains 26 cuprous nano particles.
4. a kind of 20 hexahedron cuprous nano particles obtained by the method for claim 1 are as the purposes in photocatalyst catalyze and degrade organic pollutants.
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Cited By (8)
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| CN105836787A (en) * | 2016-05-23 | 2016-08-10 | 常州大学 | Environment-friendly preparation method of cuprous oxide |
| CN105923647A (en) * | 2016-04-14 | 2016-09-07 | 青岛大学 | Preparation method of cuprous oxide nano crystal assembly |
| CN107915249A (en) * | 2016-10-08 | 2018-04-17 | 中国科学院大连化学物理研究所 | The nanometer Cu of square core shell structure2O/Cu3The preparation method of N materials |
| CN109704387A (en) * | 2019-01-17 | 2019-05-03 | 西安理工大学 | 20 hexahedron Cu of one kind2O, which is situated between, sees the preparation method of crystal powder |
| CN110156064A (en) * | 2019-04-30 | 2019-08-23 | 南开大学 | A kind of low indices of crystallographic plane Cu2The preparation method of O Polyhedral Particles |
| CN111252800A (en) * | 2020-01-21 | 2020-06-09 | 上海电力大学 | Preparation method of nano cuprous oxide photoelectric material |
| CN112941643A (en) * | 2021-01-26 | 2021-06-11 | 南京捷纳思新材料有限公司 | Method for preparing photocatalytic fiber through microfluid electrostatic spinning |
| CN115259207A (en) * | 2022-08-30 | 2022-11-01 | 西北工业大学 | Preparation method of tetradecahedron cuprous oxide |
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| CN105923647A (en) * | 2016-04-14 | 2016-09-07 | 青岛大学 | Preparation method of cuprous oxide nano crystal assembly |
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| CN107915249A (en) * | 2016-10-08 | 2018-04-17 | 中国科学院大连化学物理研究所 | The nanometer Cu of square core shell structure2O/Cu3The preparation method of N materials |
| CN107915249B (en) * | 2016-10-08 | 2020-03-24 | 中国科学院大连化学物理研究所 | Nano Cu of square core-shell structure2O/Cu3Preparation method of N material |
| CN109704387A (en) * | 2019-01-17 | 2019-05-03 | 西安理工大学 | 20 hexahedron Cu of one kind2O, which is situated between, sees the preparation method of crystal powder |
| CN109704387B (en) * | 2019-01-17 | 2021-06-15 | 西安理工大学 | Icosahedron Cu2Preparation method of O mesoscopic crystal powder |
| CN110156064A (en) * | 2019-04-30 | 2019-08-23 | 南开大学 | A kind of low indices of crystallographic plane Cu2The preparation method of O Polyhedral Particles |
| CN111252800A (en) * | 2020-01-21 | 2020-06-09 | 上海电力大学 | Preparation method of nano cuprous oxide photoelectric material |
| CN112941643A (en) * | 2021-01-26 | 2021-06-11 | 南京捷纳思新材料有限公司 | Method for preparing photocatalytic fiber through microfluid electrostatic spinning |
| CN115259207A (en) * | 2022-08-30 | 2022-11-01 | 西北工业大学 | Preparation method of tetradecahedron cuprous oxide |
| CN115259207B (en) * | 2022-08-30 | 2024-02-23 | 西北工业大学 | Preparation method of fourteen-surface cuprous oxide |
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