CN107954463A - A kind of preparation method of cuprous nano crystalline substance cube and hollow polyhedral - Google Patents
A kind of preparation method of cuprous nano crystalline substance cube and hollow polyhedral Download PDFInfo
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- CN107954463A CN107954463A CN201711287549.3A CN201711287549A CN107954463A CN 107954463 A CN107954463 A CN 107954463A CN 201711287549 A CN201711287549 A CN 201711287549A CN 107954463 A CN107954463 A CN 107954463A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention belongs to transition metal oxide preparing technical field, it is related to a kind of preparation method of cuprous nano crystalline substance cube and hollow polyhedral, for catalysis material, anti-fouling paint, insecticide, and various mantoquitas, analytical reagent, red glass, the preparation occasion of copper facing and copper-beryllium solution；The problem of preparation of industrialization cuprous nano crystalline substance cube and hollow polyhedral is solved, the nanocrystalline of synthesis has good photocatalysis performance, can adsorb azo dyes rapidly and be easily isolated；And to Na2SO4Nitrobenzene in solution has good detection effect；First reacted using copper acetate dihydrate and sodium hydroxide first, then using lauryl sodium sulfate as surfactant and stabilizer, add different volumes than deionized water and hydrazine hydrate aqueous solution cuprous nano crystalline substance cube and hollow polyhedral is made, its preparation process is simple, and principle is reliable, and manufacturing cost is low, product purity is high, performance is good, is widely used, and use environment is friendly.
Description
Technical field：
The invention belongs to transition metal oxide preparing technical field, is related to a kind of hollow and solid using immersion method synthesis
The nanocrystalline method of different-shape, the preparation method of especially a kind of cuprous nano crystalline substance cube and hollow polyhedral,
For catalyst, catalysis material, electrocatalysis material, manufacture ship bottom anti-fouling paint, insecticide, and various mantoquitas, analytical reagent,
Red glass, is additionally operable to the preparation occasion of copper facing and copper-beryllium solution.
Background technology：
Cuprous oxide is a kind of important novel inorganic industrial chemicals, in marine anti-pollution, photoelectric conversion, catalytic degradation, biography
The fields such as sensor are widely used, due to the physics and chemical property of cuprous oxide depend greatly on its crystalline size and
Pattern, therefore, the controllable cuprous oxide of synthesis appearance and size have become the focus of the area research.The oxidation synthesized in recent years
The pattern of cuprous crystal mainly has crystalline powder, wire, polyhedron and hollow ball etc., synthetic method be generally low-temperature solid-phase method,
Electrolysis, chemical precipitation method, mechanochemical reaction, hydro-thermal method, solvent-thermal method, electrolysis are to apply more preparation method at present,
Its advantage is that flow is short, cost is low, and technique is simple, purity is big, but this method power consumption is high, low output；Chemical precipitation method is by heavy
The effect of shallow lake agent, makes the purpose ion component in solution optionally be separated out in the form of compound hard to tolerate；Liu Ruping, Du Li
East, Yue Zhao, waits Cu2The nanocrystalline preparations of O and its application [J] sensors and micro-system in alcohol gas sensor, 2013,
32(12)：138-141, with CuCl2.H2O is primary raw material, and ascorbic acid makees reducing agent, and polyethylene glycol makees surfactant, is led to
Cross chemical precipitation method and be prepared for the preferable Cu of dispersiveness2O nanocube crystal, and pH value is have studied to Cu2O nanometers of mechanisms
Influence.D Guo, L Wang, Y I Du, et al.Preparation of actahedral Cu2O nanoparticles
by a green route[J].Materials Letters,2015,160,(1):541-543. pass through green simple chemistry
Intermediate processing prepares Cu2O is octahedra, it is characterized through XRD, SEM, FTIR etc., the results showed that octahedra particle length is in 200-
Between 300nm, narrow band gap (2.26ev) is conducive to most of Cu2O blue shifts (2.17ev), Cu2O surfaces can be very good to inhale
Receive visible ray.K Zhou,Y Shi,S Jiang,et al.Facile preparation of Cu2O/carbon sphere
heterostructure with high photocatalytic activity[j].Journal of the Materials
Letters,2013,98(1):213-216. Cu is prepared by simply chemical reduction method2The photocatalysis of O/CS heterojunction structures is lived
Property is apparently higher than pure Cu2The possible cause of O.L Liu,Y Qi,J Hu,et al.Efficient visible-light
photocatalytic hydrogen evolution and enhanced photostability of core@shell
Cu2O@g-C3N4octahedra[J].Applied Surface Science,2015,351:1146-1154. pass through solvent heat
Method and absorption method have only carried on the back the Cu of octahedra core shell structure2O@g-C3N4 photochemical catalysts, Cu2The octahedral formation ratios of O { 111 }
Cu2O balls more have efficient photocatalysis performance, in addition, for H2Production, Cu2O@g-C3N4 composite material exhibits go out excellent work
Property.Due to Cu2The octahedral cooperative effects of O enhance photocatalytic activity, and mixed type nucleocapsid has higher photostability.
Therefore, the catalyst performance that prepared by cuprous nano crystalline substance cube and hollow polyhedral is excellent, but the above method is only to test
Preparation is used for theoretical research, and severe reaction conditions, product pollution environment, is not particularly suited for industrialized production, therefore, industrialization
The controllable cuprous oxide of synthesis appearance and size is still the hot spot of this area research.
The content of the invention：
It is an object of the invention to overcome shortcoming existing in the prior art, propose a kind of cuprous nano crystalline substance cube and
The preparation method of hollow polyhedral, by varying the proportioning of solvent and reducing agent in water-bath system so as to synthesized pattern,
The cuprous nano of size and structure-controllable is brilliant, solves preparation of industrialization cuprous nano crystalline substance cube and hollow polyhedral
Problem, the nanocrystalline of synthesis have good photocatalysis performance, can adsorb azo dyes rapidly and be easily isolated；It is and right
Na2SO4Nitrobenzene in solution has good detection effect.
To achieve these goals, the preparation side of cuprous nano crystalline substance cube and hollow polyhedral of the present invention
Method is：Copper acetate dihydrate (Cu (CH are used first3COO)2·H2O) first reacted with sodium hydroxide (NaOH), then with dodecane
Base sodium sulphate (C12H25SO4Na be) surfactant and stabilizer, add different volumes than deionized water and hydrazine hydrate
(N2H4·H2O) cuprous nano crystalline substance cube and hollow polyhedral is made in aqueous solution, its specific embodiment includes following step
Suddenly：
(1) dissolve：Two parts of 0.87g lauryl sodium sulfate are weighed first, are dissolved separately in 89ml and 69mL deionized waters
In solvent, it is stirred well to and is uniformly dissolved；
(2) copper acetate is added：Then 5ml 0.1mol/L Cu are separately added into solution made from step (1)
(CH3COO)2Aqueous solution, is vigorously stirred to being uniformly dissolved；
(3) NaOH is added：Then it is 34 DEG C to keep bath temperature, and 2ml is separately added into solution made from step (2)
NaOH aqueous solutions, are vigorously stirred to uniformly mixed；
(4) hydrazine hydrate is added：In 5s, add again in the mixed liquor containing 89ml deionized water solvents made from step (3)
Enter 4ml N2H4·H2O solution, 24ml is added in the mixed liquor containing 69ml deionized water solvents made from step (3)
N2H4·H2O solution, it is 100ml to keep total amount of liquid, stops stirring after being vigorously stirred 20s；
(5) water-bath；After when finally water-bath 1 is small, solid product centrifugation is collected, washs number with deionized water and ethanol respectively
It is secondary, then 60 DEG C of dry 12h.The sample being collected into is in respectively brownish red and sepia, is respectively designated as Cu2O-1、Cu2O-2,
Regular texture is presented, size is between 100nm to 300nm, Cu2O-1 is fairly regular solid cube；Fig. 1-2 and Fig. 2-2
The Cu of expression2O-2 is then the hollow polyhedral structure of rule.
Compared with prior art, the present invention the preparation method is simple, easy, stable, reliable, wherein, deionized water and water
The volume ratio for closing hydrazine aqueous solution is 89:4 synthesis are solid cubes, and volume ratio is 69:24 synthesis are hollow polyhedrals；
At ambient temperature, cuprous nano crystalline substance has good photodegradation to organic macromolecule methyl orange；In 0.2mol/L
Na2SO4The detection effect of hollow polyhedral p-nitrophenyl (NB) is more preferable than solid cube in aqueous solution；Its preparation process is simple,
Principle is reliable, and manufacturing cost is low, and product purity is high, and performance is good, is widely used, and use environment is friendly.
Brief description of the drawings：
Fig. 1 is Cu prepared by the present invention2O-1 (1) and Cu2The scanning electron microscope diagram of O-2 (2).
Fig. 2 is Cu prepared by the present invention2O-1 (1) and Cu2The transmission electron microscope figure of O-2 (2).
Fig. 3 is Cu prepared by the present invention2O-1 (1) and Cu2The X-ray diffractogram of O-2 (2).
Fig. 4 is the Cu that methyl orange solution is prepared in the present invention under normal illumination2O-1 (A) and Cu2In the presence of O-2 (B),
During by 0min, 10min, 20min, 30min, 45min, 60min, 90min, 120min, 180min, 240min, 300min
UV, visible light figure.
Fig. 5 is Cu prepared by the present invention2O-1/GCE (1) and Cu2O-2/GCE (2) is in the 0.2mol/L Na containing NB2SO4
Cyclic voltammetry curve in aqueous solution in the case where sweeping speed and being 100mV/s.
Fig. 6 is Cu prepared by the present invention2O-1/GCE (A) and Cu2O-2/GCE (B) is in the 0.2mol/ containing NB (0.4mM)
LNa2SO4Difference sweeps (a) 20 under fast (mV/s) in aqueous solution；(b)40；(c)60；(d)80；(e)100；(f)120；(g) 160
Cyclic voltammetry curve.
Embodiment：
It is described further by way of example and in conjunction with the accompanying drawings.
Embodiment：
The cuprous nano crystalline substance cube and the preparation method of hollow polyhedral that the present embodiment is related to be：One is used first
Hydrated copper acetate (Cu (CH3COO)2·H2O) first reacted with sodium hydroxide (NaOH), then with lauryl sodium sulfate
(C12H25SO4Na be) surfactant and stabilizer, add different volumes than deionized water and hydrazine hydrate (N2H4·H2O)
Cuprous nano crystalline substance cube and hollow polyhedral is made in aqueous solution, its specific embodiment comprises the following steps：
(1) dissolve：Two parts of 0.87g lauryl sodium sulfate are weighed first, are dissolved separately in 89ml and 69mL deionized waters
In solvent, it is stirred well to and is uniformly dissolved；
(2) copper acetate is added：Then 5ml 0.1mol/L Cu are separately added into solution made from step (1)
(CH3COO)2Aqueous solution, is vigorously stirred to being uniformly dissolved；
(3) NaOH is added：Then it is 34 DEG C to keep bath temperature, and 2ml is separately added into solution made from step (2)
NaOH aqueous solutions, are vigorously stirred to uniformly mixed；
(4) hydrazine hydrate is added：In 5s, add again in the mixed liquor containing 89ml deionized water solvents made from step (3)
Enter 4ml N2H4·H2O solution, 24ml is added in the mixed liquor containing 69ml deionized water solvents made from step (3)
N2H4·H2O solution, it is 100ml to keep total amount of liquid, stops stirring after being vigorously stirred 20s；
(5) water-bath；After when finally water-bath 1 is small, solid product centrifugation is collected, washs number with deionized water and ethanol respectively
It is secondary, then 60 DEG C of dry 12h.The sample being collected into is in respectively brownish red and sepia, is respectively designated as Cu2O-1、Cu2O-2。
The pattern and structure of cuprous nano crystalline substance are levied by SEM and TEM charts, and such as Fig. 1 and Fig. 2, all samples are all
Regular texture is presented, size is between 100nm to 300nm.Wherein, Cu shown in Fig. 1-1 and Fig. 2-12O-1 is fairly regular
Solid cube；The Cu that Fig. 1-2 and Fig. 2-2 is represented2O-2 is then the hollow polyhedral structure of rule.
Fig. 3 is the standard diffraction peak position of the XRD spectra of cuprous nano crystalline substance, diffraction maximum and the cuprous structure of standard oxidation
(JCPDS NO.05-0667) unanimously, their 2 θ angles are respectively 29.5,36.4,42.3,61.3,73.5 and 77.3, respectively
Corresponding ZnFe2O4(110), (111), (200), (311), (220) and (222) crystal face of spinelle.Cu2The diffraction maximum of O-1 is than it
The diffraction maximum of his sample is more sharp and narrow, illustrates Cu2The crystallite dimension of O-1 compares Cu2O-2 crystallite dimension biggers.
(A) solid cube and hollow polyhedral cuprous nano crystalline substance is to Adsorption of Methyl Orange performance study：
The Cu respectively prepared by the 10mg present invention2O-1 and Cu2O-2 adds the methyl orange aqueous solution that 50ml concentration is 50mg/L
In, the UV-visible spectrum of certain period of time in ultrasound 1min under normal lighting conditions, measure 300min.When Fig. 4 is each
The UV-visible spectrum of section, with the development of time, Cu2O-2 absworption peaks be dropped rapidly to it is very low, be one continuous decrease
Process, and Cu2The absworption peak of O-1 declines very slow, no significant change.Although Cu2O-1 and Cu2Absorption of the O-2 to methyl orange
All it is a steady decline process, but Cu2The efficiency far of O-2 is higher than Cu2O-1。
(B) the electrocatalysis characteristic research of solid cube and hollow polyhedral cuprous nano crystalline substance：
Fig. 5 utilizes the electricity of two kinds of cuprous nano crystalline substance modified electrode p-nitrophenyls (NB) of cyclic voltammetric technique study to urge
Change activity.Indicate it is identical sweep speed under, Cu2O-2/GCE and Cu2O-1/GCE has more preferable catalytic activity.
Fig. 6 is Cu2O-1/GCE (A) and Cu2O-2/GCE (B) is in the 0.2mol/L Na containing NB (0.4mM)2SO4Solution
Middle difference sweeps the CV curves under speed.From the illustration in Fig. 6 A, B as it can be seen that the catalysis peak current of cuprous nano crystalline substance modified electrode
Value is with the substantially linear increase of increase for sweeping speed.Show that the GCE electrodes of the brilliant modification of cuprous nano can effectively and delicately
Detect NB.
Claims (2)
- A kind of 1. preparation method of cuprous nano crystalline substance cube and hollow polyhedral, it is characterised in that：A water is used first Close copper acetate (Cu (CH3COO)2·H2O) first reacted with sodium hydroxide (NaOH), then with lauryl sodium sulfate (C12H25SO4Na be) surfactant and stabilizer, add different volumes than deionized water and hydrazine hydrate (N2H4·H2O) Cuprous nano crystalline substance cube and hollow polyhedral is made in aqueous solution, wherein, the volume of deionized water and hydrazine hydrate aqueous solution Than for 89:4 synthesis are solid cubes, and volume ratio is 69:24 synthesis are hollow polyhedrals, and specific embodiment includes Following steps：(1) dissolve：Two parts of 0.87g lauryl sodium sulfate are weighed first, are dissolved separately in 89ml and 69mL deionized water solvents In, it is stirred well to and is uniformly dissolved；(2) copper acetate is added：Then 5ml 0.1mol/L Cu (CH are separately added into solution made from step (1)3COO)2Water Solution, is vigorously stirred to being uniformly dissolved；(3) NaOH is added：Then it is 34 DEG C to keep bath temperature, and 2ml NaOH are separately added into solution made from step (2) Aqueous solution, is vigorously stirred to uniformly mixed；(4) hydrazine hydrate is added：In 5s, 4ml is added in the mixed liquor containing 89ml deionized water solvents made from step (3) N2H4·H2O solution, 24mlN is added in the mixed liquor containing 69ml deionized water solvents made from step (3)2H4·H2O Solution, it is 100ml to keep total amount of liquid, stops stirring after being vigorously stirred 20s；(5) water-bath；After when finally water-bath 1 is small, solid product centrifugation is collected, is washed for several times with deionized water and ethanol respectively, so 60 DEG C of dry 12h afterwards；The sample being collected into is in respectively brownish red and sepia, is respectively designated as Cu2O-1、Cu2O-2。
- 2. the preparation method of cuprous nano crystalline substance cube as claimed in claim 1 and hollow polyhedral, it is characterised in that： The product Cu of preparation2O-1 and Cu2Regular texture is presented in O-2, and size is between 100nm to 300nm, Cu2O-1 is solid cube Body；Cu2O-2 is hollow polyhedral structure, can be used in preparing catalysis material, ship bottom anti-fouling paint, insecticide, mantoquita, analysis examination Agent and red glass.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110039043A (en) * | 2019-03-15 | 2019-07-23 | 上海大学 | Three-dimensional copper@carbon core shell nanoparticles, preparation method and the application as enzyme-free glucose electrochemical sensor |
| CN114908413A (en) * | 2022-04-21 | 2022-08-16 | 微冻眠(厦门)科技有限公司 | Preparation method and application of nano cuprous oxide cubic single crystal and refrigerating fluid |
| CN115722246A (en) * | 2022-11-09 | 2023-03-03 | 华侨大学 | anti-SO suitable for medium and low temperature condition 2 Combined denitration and mercury removal catalyst and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043703A (en) * | 2013-01-05 | 2013-04-17 | 河北工业大学 | Preparation method of hollow Cu2O cubic box |
| CN105314669A (en) * | 2015-10-09 | 2016-02-10 | 重庆大学 | Technology for preparing micro-nano cuprous oxide hollow polyhedrons through reduction method |
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2017
- 2017-12-07 CN CN201711287549.3A patent/CN107954463B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043703A (en) * | 2013-01-05 | 2013-04-17 | 河北工业大学 | Preparation method of hollow Cu2O cubic box |
| CN105314669A (en) * | 2015-10-09 | 2016-02-10 | 重庆大学 | Technology for preparing micro-nano cuprous oxide hollow polyhedrons through reduction method |
Non-Patent Citations (3)
| Title |
|---|
| CHUN-HONG KUO ET AL.: "Facile Synthesis of Cu2O Nanocrystals with Systematic Shape Evolution from Cubic to Octahedral Structures", 《J.PHYS.CHEM.C》 * |
| JINYI-HO ET AL.: "Synthesis of Submicrometer-Sized Cu2O Crystals with Morphological Evolution from Cubic to Hexapod Structures and Their Comparative Photocatalytic Activity", 《J. PHYS. CHEM. C》 * |
| YA-HUEI TSAI ET AL.: "Direct formation of small Cu2O nanocubes, octahedra, and octapods for efficient synthesis of triazoles", 《NANOSCALE》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110039043A (en) * | 2019-03-15 | 2019-07-23 | 上海大学 | Three-dimensional copper@carbon core shell nanoparticles, preparation method and the application as enzyme-free glucose electrochemical sensor |
| CN110039043B (en) * | 2019-03-15 | 2021-07-06 | 上海大学 | Three-dimensional copper @ carbon core-shell nanoparticle, and preparation method and application thereof |
| CN114908413A (en) * | 2022-04-21 | 2022-08-16 | 微冻眠(厦门)科技有限公司 | Preparation method and application of nano cuprous oxide cubic single crystal and refrigerating fluid |
| CN115722246A (en) * | 2022-11-09 | 2023-03-03 | 华侨大学 | anti-SO suitable for medium and low temperature condition 2 Combined denitration and mercury removal catalyst and preparation method thereof |
| CN115722246B (en) * | 2022-11-09 | 2024-02-27 | 华侨大学 | SO resistance suitable for medium and low temperature condition 2 Combined denitration mercury-removal catalyst and preparation method thereof |
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