CN107098375B - A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure - Google Patents
A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure Download PDFInfo
- Publication number
- CN107098375B CN107098375B CN201710303765.6A CN201710303765A CN107098375B CN 107098375 B CN107098375 B CN 107098375B CN 201710303765 A CN201710303765 A CN 201710303765A CN 107098375 B CN107098375 B CN 107098375B
- Authority
- CN
- China
- Prior art keywords
- cuprous sulfide
- solution
- nano material
- similar
- sulfide nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 67
- 241000510091 Quadrula quadrula Species 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000007146 photocatalysis Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 15
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 14
- 239000001119 stannous chloride Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 68
- 238000013019 agitation Methods 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 7
- 150000002171 ethylene diamines Chemical class 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 22
- 239000013049 sediment Substances 0.000 description 20
- 239000002105 nanoparticle Substances 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000001027 hydrothermal synthesis Methods 0.000 description 10
- 239000004408 titanium dioxide Substances 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 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 6
- 229940012189 methyl orange Drugs 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- 239000010949 copper Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 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 2
- 239000000126 substance Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000011787 zinc oxide Substances 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of preparation methods of the cuprous sulfide nano material of similar maple leaf structure, stannous chloride is dissolved in ethylenediamine, the first solution is made, thiocarbamide is added into the first solution again, the second solution is made, second solution is reacted using solvent-thermal method, material after reaction is subjected to purification process up to the cuprous sulfide nano material of similar maple leaf structure, wherein, the cuprous concentration of the first Chlorine in Solutionization is 0.02~0.1mol/L.The additional amount that the present invention passes through control raw material, by above-mentioned steps to prepare the cuprous sulfide nanostructure with similar maple leaf structure, the nanostructure makes the large specific surface area of cuprous sulfide nano material, with higher photocatalysis efficiency, while the catalytic effect that cuprous sulfide nano material is generated using visible light is more preferable.
Description
Technical field
The present invention relates to photochemical catalyst fields, and in particular to a kind of similar maple leaf structure with visible light photocatalysis effect
Cuprous sulfide preparation method of nano material.
Background technique
From the end of the eighties, people start photocatalytic applications in field of environment pollution control, since the technology can be effectively
The Recalcitrant chemicals of many stable structure are destroyed, therefore are led in purification of sewage treatment, restraining and sterilizing bacteria and environment etc.
Domain obtains widely studying and applying.Compared with traditional water treatment technology, with apparent energy conservation, efficient, contaminant degradation is thorough
The advantages that bottom, and photocatalysis technology is easy to operate, without secondary pollution, it has become a kind of environmental improvement side for having important application prospect
Method causes the most attention of domestic and foreign scholars.However, the majority being related to is wide in the research of semiconductor light-catalyst
The semiconductor material of forbidden band, such as zinc oxide, titanium dioxide, stannic oxide, these semiconductor materials have big due to itself
Band-gap energy, therefore they are not high to the utilization rate of solar energy, and due to the composite attribute of light induced electron and hole, make list
One semiconductor light-catalyst is restricted in terms of development and utilization.Therefore it needs to carry out single semiconductor light-catalyst
Modification improves the active purpose of conductor photocatalysis to reach.Cuprous sulfide (Cu2It S) is a kind of low energy gap (forbidden bandwidth
=1.2~1.24eV) p-type semiconductor material, have good chemical and thermal stability energy, be a kind of good photoelectricity material
Material the fields such as utilizes to have huge application potential in solar energy.
It is well known that the micron or nanostructure of material have a significant impact its performance, in order to improve urging for cuprous sulfide
Change, the performance in terms of optics and electricity, research prepares novel micron or nanometer cuprous sulfide structure also increasingly by people
Concern.However, the cuprous sulfide structure prepared at present is limited only to the dull particle of comparison, sheet and spherical shape,
Show the absorbing wavelength response range better than traditional titanium dioxide to light.However, these cuprous sulfide structure specific surface areas
Smaller, photocatalysis efficiency is lower, and poor to visible light catalytic effect.
Summary of the invention
In order to solve the deficiencies in the prior art, the vulcanization that an object of the present invention is to provide a kind of similar maple leaf structure is sub-
The preparation method of copper nano material, the large specific surface area of the cuprous sulfide nano material of this method preparation, there is higher light to urge
Change efficiency, and more preferable using the catalytic effect that the cuprous sulfide nano material can be generated using visible light.
To achieve the goals above, the technical solution of the present invention is as follows:
A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure, stannous chloride is dissolved in ethylenediamine
The first solution is made, then thiocarbamide is added into the first solution, the second solution is made, the second solution is carried out instead using solvent-thermal method
It answers, the material after reaction is subjected to purification process up to cuprous sulfide nano material, wherein cuprous dense of the first Chlorine in Solutionization
Degree is 0.02~0.1mol/L.
The present invention has been prepared by above-mentioned steps with similar maple leaf structure by the additional amount of control raw material
Cuprous sulfide nanostructure, the nanostructure make the large specific surface area of cuprous sulfide nano material, have higher photocatalysis
Efficiency, while the catalytic effect that cuprous sulfide nano material is generated using visible light is more preferable.
The second object of the present invention is to provide a kind of cuprous sulfide nano material of above-mentioned preparation method preparation.The vulcanization is sub-
Copper nano material have unique similar maple leaf shape nanostructure, enable nanometer cuprous sulfide preferably utilize visible light into
Row photocatalysis, to improve the utilization to sunlight.
The third object of the present invention is to provide a kind of application of above-mentioned cuprous sulfide nano material in visible light photocatalysis.
The fourth object of the present invention is to provide a kind of photochemical catalyst, using above-mentioned cuprous sulfide nano material.
Beneficial effects of the present invention:
(1) the cuprous sulfide nano material of similar maple leaf structure prepared by the present invention has effectively widened the response to sunlight
Range, realizing has excellent photocatalysis effect under visible light, so as to improve photocatalysis effect.
(2) present invention prepares the cuprous sulfide nano material similar to maple leaf structure by hydro-thermal method, and two with single structure
Titanium dioxide nanoparticle is compared with cuprous sulfide nano particle, the cuprous sulfide nanometer material of the similar maple leaf structure of this method preparation
Material has widened the response range to sunlight, effectively increases the utilization rate to sunlight.With independent titania nanoparticles
Compared with cuprous sulfide nano particle, this method similar to maple leaf structure cuprous sulfide nano material under visible light to methyl orange
Photocatalysis efficiency with higher effectively increases the utilization rate to sunlight.
(3) operation of the present invention process is simple, and production cost is low, easy to spread, and cuprous sulfide is greatly facilitated in practical light
The application of catalytic field.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the scanning electron microscope (SEM) photograph of cuprous sulfide nano material obtained in embodiment 2；
Fig. 2 is cuprous sulfide nano material, commercial titanium dioxide nano particle and business sulphur obtained in Examples 1 to 5
Change cuprous nano particle respectively under visible light illumination to the change curve of the photocatalytic activity of methyl orange solution and time.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Heretofore described first, second is not to define tandem, and be only the restriction carried out to title.
Heretofore described solvent-thermal method refers in enclosed system such as autoclave, is molten with organic matter or non-aqueous solvent
Agent, under the self-generated pressure of certain temperature and solution, a kind of synthetic method that original stock is reacted.
Heretofore described purification process refers to the process of takes out solid product from solvent, can be filtering, wash
The process wash, dried, or centrifuge separation, dry process.
As background technique is introduced, the cuprous sulfide structure specific surface area of prior art preparation exists in the prior art
Deficiency smaller, poor to the catalytic effect generated using visible light, in order to solve technical problem as above, present applicant proposes
A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure.
In a kind of exemplary embodiment of the application, a kind of cuprous sulfide nano material of similar maple leaf structure is provided
Stannous chloride is dissolved in ethylenediamine and the first solution is made by preparation method, then thiocarbamide is added into the first solution and is made second
Second solution is reacted using solvent-thermal method, the material after reaction is carried out purification process and is received up to cuprous sulfide by solution
Rice material, wherein the cuprous concentration of the first Chlorine in Solutionization is 0.02~0.1mol/L.
The present invention has been prepared by above-mentioned steps with similar maple leaf structure by the additional amount of control raw material
Cuprous sulfide nanostructure, the nanostructure make the large specific surface area of cuprous sulfide nano material, have higher photocatalysis
Efficiency, while the catalytic effect that cuprous sulfide nano material is generated using visible light is more preferable.
In order to guarantee that stannous chloride is uniformly dispersed in ethylenediamine, it is preferred that take 10~50 milliliters of ethylenediamines and 1 mM
Stannous chloride was sufficiently mixed solution uniformly by magnetic agitation 30 minutes, and the first solution is made.
It is further preferred that the additional amount of the ethylenediamine is 30 milliliters.The cuprous sulfide nano material of condition preparation
Visible light photocatalytic degradation is more efficient.
Preferably, the additional amount of the thiocarbamide is 2.5~3.5 mMs.
In order to dissolve thiocarbamide sufficiently, it is preferred that be added after thiocarbamide magnetic agitation 30 minutes.
Preferably, the reaction condition of the solvent-thermal method is 80~200 DEG C of reaction temperature, and the reaction time is 8~24 small
When.
It is further preferred that the reaction condition of the solvent-thermal method is, 120 DEG C of reaction temperature, the reaction time is 12 hours.
The cuprous sulfide nano material visible light photocatalytic degradation of condition preparation is more efficient.
Preferably, the process of the purification process is filtering, cleaning, drying.
It is further preferred that the drying condition is, drying temperature is 60 DEG C, and drying time is 10 hours.
In another exemplary embodiment of the application, a kind of cuprous sulfide nanometer of above-mentioned preparation method preparation is provided
Material.The cuprous sulfide nano material has unique similar maple leaf shape nanostructure, enables nanometer cuprous sulfide more preferable
Using visible light carry out photocatalysis, to improve the utilization to sunlight.
Preferably, the cuprous sulfide nano material with a thickness of 100~200 nanometers, width is 5~8 microns.
Present invention also provides a kind of application of above-mentioned cuprous sulfide nano material in visible light photocatalysis.
Present invention also provides a kind of photochemical catalysts, using above-mentioned cuprous sulfide nano material.
In order to enable those skilled in the art can clearly understand the technical solution of the application, below with reference to tool
The technical solution of the application is described in detail in the embodiment and comparative example of body.
The surface topography test of 2 mixed powder of embodiment is carried out using scanning electron microscope, specific test result is shown in
Fig. 1.
The raw material that following embodiments 1 are used into embodiment 5 is ethylenediamine, stannous chloride, thiocarbamide, ethyl alcohol and deionization
Water.
Used equipment has for mixed beaker, magnetic stirring apparatus, hydrothermal reaction kettle, baking oven etc..
Step 1: after a certain amount of stannous chloride is dissolved into ethylenediamine mixing, abundant magnetic agitation prepares the first solution.
Step 2: after a certain amount of thiocarbamide is dissolved into the mixing of the first solution, abundant magnetic agitation prepares the second solution.
Step 3: the second solution being placed in hydrothermal reaction kettle, is sufficiently prepared into product filtering, cleaning, drying after reaction
Similar maple leaf structure cuprous sulfide nano material.
When producing the cuprous sulfide nano material of similar maple leaf structure, stannous chloride and ethylenediamine are sufficiently mixed system first
Then standby first solution adds thiocarbamide to the first solution and stirs the second solution of preparation；The second solution is subsequently put into hydro-thermal
Third solution is produced in reaction in reaction kettle；Then sediment is obtained by filtration in third solution, the sediment being separated to first is used into second
The cuprous sulfide nano material of similar maple leaf structure is made to neutrality in the drying of obtained sediment by pure and mild ion washing.It takes out
The cuprous sulfide nano material of similar maple leaf structure obtained also needs to carry out by scanning electron microscope and photocatalysis effect test macro
Observation analysis.
A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure provided by the invention, specific steps are such as
Under:
Step 1: taking 1 mM of 3 parts of stannous chlorides, it is added in not same amount ethylenediamine, preparation the in magnetic agitation 30 minutes
One solution.
Step 2: being added 3 mMs of thiocarbamide to 3 part of first solution, 30 minutes the second solution of preparation is sufficiently stirred.
Step 4: the second solution is placed in hydrothermal reaction kettle, sufficiently reacted under the conditions of 120 DEG C 12 hours, preparation the
Three solution.
Step 5: filtering third solution obtains sediment, obtained sediment is cleaned with ethyl alcohol and deionized water, 60
It is 10 hours dry under conditions of DEG C, finally take out the cuprous sulfide nano material of manufactured similar maple leaf structure.
Embodiment 1
Step 1: measuring 1 mM of stannous chloride first and 10 milliliters of ethylenediamines are sufficiently mixed magnetic agitation 30 minutes, make
Standby first solution.
Step 2: and then 3 mMs of thiocarbamides are added in the first solution, subsequently made solution by magnetic agitation 30 minutes
It is sufficiently mixed uniformly, produces the second solution.
Step 3: the second solution is placed into hydrothermal reaction kettle, is reacted 12 hours at 120 DEG C, and third solution is prepared.
Step 4: filtering third solution obtains sediment, and obtained sediment is washed with ethyl alcohol and deionized water.It connects again
The sediment after washing is dried 10 hours under conditions of 60 DEG C, the cuprous sulfide nanometer material of similar maple leaf structure is made
Material.
The cuprous sulfide nano material of similar maple leaf structure, wide with a thickness of 100~200 nanometers made from above-described embodiment 1
Degree is 10~20 microns.Compared with commercial titanium dioxide nano particle and cuprous sulfide nano particle, the sulphur of similar maple leaf structure
Change cuprous nano material and effectively widened light abstraction width, under visible light to methyl orange photocatalysis efficiency with higher, has
Effect improves the utilization rate to sunlight.
Embodiment 2
Step 1: measuring 1 mM of stannous chloride first and 30 milliliters of ethylenediamines are sufficiently mixed magnetic agitation 30 minutes, make
Standby first solution.
Step 2: and then 3 mMs of thiocarbamides are added in the first solution, subsequently made solution by magnetic agitation 30 minutes
It is sufficiently mixed uniformly, produces the second solution.
Step 3: the second solution is placed into hydrothermal reaction kettle, is reacted 12 hours at 120 DEG C, and third solution is prepared.
Step 4: filtering third solution obtains sediment, and obtained sediment is washed with ethyl alcohol and deionized water.It connects again
The sediment after washing is dried 10 hours under conditions of 60 DEG C, the cuprous sulfide nanometer material of similar maple leaf structure is made
Material.
The cuprous sulfide nano material of similar maple leaf structure, wide with a thickness of 100~200 nanometers made from above-described embodiment 2
Degree is 5~8 microns.Compared with commercial titanium dioxide nano particle and cuprous sulfide nano particle, the vulcanization of similar maple leaf structure
Cuprous nano material has effectively widened light abstraction width, under visible light to methyl orange photocatalysis efficiency with higher, effectively
Improve the utilization rate to sunlight.
Embodiment 3
Step 1: measuring 1 mM of stannous chloride first and 50 milliliters of ethylenediamines are sufficiently mixed magnetic agitation 30 minutes, make
Standby first solution.
Step 2: and then 3 mMs of thiocarbamides are added in the first solution, subsequently made solution by magnetic agitation 30 minutes
It is sufficiently mixed uniformly, produces the second solution.
Step 3: the second solution is placed into hydrothermal reaction kettle, is reacted 12 hours at 120 DEG C, and third solution is prepared.
Step 4: filtering third solution obtains sediment, and obtained sediment is washed with ethyl alcohol and deionized water.It connects again
The sediment after washing is dried 10 hours under conditions of 60 DEG C, the cuprous sulfide nanometer material of similar maple leaf structure is made
Material.
The cuprous sulfide nano material of similar maple leaf structure, wide with a thickness of 100~200 nanometers made from above-described embodiment 3
Degree is 20~30 microns.Compared with commercial titanium dioxide nano particle and cuprous sulfide nano particle, the sulphur of similar maple leaf structure
Change cuprous nano material and effectively widened light abstraction width, under visible light to methyl orange photocatalysis efficiency with higher, has
Effect improves the utilization rate to sunlight.
Embodiment 4
Step 1: measuring 1 mM of stannous chloride first and 30 milliliters of ethylenediamines are sufficiently mixed magnetic agitation 30 minutes, make
Standby first solution.
Step 2: and then 3 mMs of thiocarbamides are added in the first solution, subsequently made solution by magnetic agitation 30 minutes
It is sufficiently mixed uniformly, produces the second solution.
Step 3: the second solution is placed into hydrothermal reaction kettle, is reacted 8 hours at 80 DEG C, and third solution is prepared.
Step 4: filtering third solution obtains sediment, and obtained sediment is washed with ethyl alcohol and deionized water.It connects again
The sediment after washing is dried 10 hours under conditions of 60 DEG C, similar maple leaf structure cuprous sulfide nano material is made.
The cuprous sulfide nano material of similar maple leaf structure, wide with a thickness of 100~200 nanometers made from above-described embodiment 4
Degree is 10~20 microns.Compared with commercial titanium dioxide nano particle and cuprous sulfide nano particle, the sulphur of similar maple leaf structure
Change cuprous nano material and effectively widened light abstraction width, under visible light to methyl orange photocatalysis efficiency with higher, has
Effect improves the utilization rate to sunlight.
Embodiment 5
Step 1: measuring 1 mM of stannous chloride first and 30 milliliters of ethylenediamines are sufficiently mixed magnetic agitation 30 minutes, make
Standby first solution.
Step 2: and then 3 mMs of thiocarbamides are added in the first solution, subsequently made solution by magnetic agitation 30 minutes
It is sufficiently mixed uniformly, produces the second solution.
Step 3: the second solution is placed into hydrothermal reaction kettle, is reacted 24 hours at 200 DEG C, and third solution is prepared.
Step 4: filtering third solution obtains sediment, and obtained sediment is washed with ethyl alcohol and deionized water.It connects again
The sediment after washing is dried 10 hours under conditions of 60 DEG C, similar maple leaf structure cuprous sulfide nano material is made.
The cuprous sulfide nano material of similar maple leaf structure, wide with a thickness of 100~200 nanometers made from above-described embodiment 5
Degree is 20~30 microns.Compared with commercial titanium dioxide nano particle and cuprous sulfide nano particle, the sulphur of similar maple leaf structure
Change cuprous nano material and effectively widened light abstraction width, under visible light to methyl orange photocatalysis efficiency with higher, has
Effect improves the utilization rate to sunlight.
By cuprous sulfide nano material, commercial titanium dioxide nano particle and quotient obtained in Fig. 2 comparing embodiment 1~5
Industry cuprous sulfide nano particle is compared, under visible light illumination can to the variation of the photocatalytic activity of methyl orange solution and time
Know, ethylenediamine additional amount is 30 milliliters, and it is high-efficient that hydro-thermal reaction reacts 12 hours visible light photocatalytic degradations at 120 DEG C.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (9)
1. a kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure, characterized in that take 30 milliliters of ethylenediamines and 1
MM stannous chloride was sufficiently mixed solution uniformly by magnetic agitation 30 minutes, obtained first solution, then to the first solution
The second solution is made in middle addition thiocarbamide, and the second solution is reacted using solvent-thermal method, the material after reaction is purified
It handles up to the cuprous sulfide nano material of similar maple leaf structure；The reaction condition of the solvent-thermal method is reaction temperature 120
DEG C, the reaction time is 12 hours.
2. preparation method as described in claim 1, characterized in that the additional amount of the thiocarbamide is 2.5~3.5 mMs.
3. preparation method as described in claim 1, characterized in that be added after thiocarbamide magnetic agitation 30 minutes.
4. preparation method as described in claim 1, characterized in that the process of the purification process is filtering, cleaning, drying.
5. preparation method as claimed in claim 4, characterized in that the drying condition is that drying temperature is 60 DEG C, when dry
Between be 10 hours.
6. a kind of cuprous sulfide nano material of the similar maple leaf structure of any preparation method preparation of Claims 1 to 5.
7. the cuprous sulfide nano material of similar maple leaf structure as claimed in claim 6, characterized in that the cuprous sulfide is received
Rice material with a thickness of 100~200 nanometers, width is 5~8 microns.
8. the cuprous sulfide nano material of similar maple leaf structure is in visible light photocatalysis described in a kind of claim 6 or 7
Using.
9. a kind of photochemical catalyst, using the cuprous sulfide nano material of similar maple leaf structure described in claim 6 or 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710303765.6A CN107098375B (en) | 2017-05-03 | 2017-05-03 | A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710303765.6A CN107098375B (en) | 2017-05-03 | 2017-05-03 | A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107098375A CN107098375A (en) | 2017-08-29 |
| CN107098375B true CN107098375B (en) | 2019-02-15 |
Family
ID=59657630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710303765.6A Active CN107098375B (en) | 2017-05-03 | 2017-05-03 | A kind of preparation method of the cuprous sulfide nano material of similar maple leaf structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107098375B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102237200A (en) * | 2011-03-04 | 2011-11-09 | 中国科学院物理研究所 | Metal sulfide counter electrode for sensitized solar cell and preparation method thereof |
| CN103739001A (en) * | 2013-12-31 | 2014-04-23 | 华东师范大学 | Cuprous sulfide nano ring structure semiconductor material and preparation method thereof |
-
2017
- 2017-05-03 CN CN201710303765.6A patent/CN107098375B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102237200A (en) * | 2011-03-04 | 2011-11-09 | 中国科学院物理研究所 | Metal sulfide counter electrode for sensitized solar cell and preparation method thereof |
| CN103739001A (en) * | 2013-12-31 | 2014-04-23 | 华东师范大学 | Cuprous sulfide nano ring structure semiconductor material and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| Cu2S纳米材料的制备及应用研究进展;许立信等;《材料导报Ａ：综述篇》;20160331;第30卷(第3期);第40-62页 |
| Cu2S纳米片的溶剂热合成及其光催化性能研究;邱玉章等;《中国陶瓷》;20121031;第48卷(第10期);第14-16页 |
| From Winter Snowflakes to Spring Blossoms: Manipulating the Growth of Copper Sulfide Dendrites;Wen Pei Lim等;《Crystal Growth & Design》;20071231;第7卷(第12期);第2429-2435页 |
| Synthesis of flower-like Cu2S dendrites via solvothermal route;Soma Gorai等;《Materials Letters》;20041202;第59卷;第826-828页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107098375A (en) | 2017-08-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Du et al. | Enhanced photocatalytic activity of Bi2WO6/TiO2 composite coated polyester fabric under visible light irradiation | |
| Shi et al. | Hydrothermal synthesis of InVO4/Graphitic carbon nitride heterojunctions and excellent visible-light-driven photocatalytic performance for rhodamine B | |
| CN106179262B (en) | Composite material and preparation method and purposes with absorption-visible light photocatalytic degradation synergistic effect | |
| Keerthana et al. | Influence of tin (Sn) doping on Co3O4 for enhanced photocatalytic dye degradation | |
| Liao et al. | Enhanced photocatalytic performance through the ferroelectric synergistic effect of pn heterojunction BiFeO3/TiO2 under visible-light irradiation | |
| Ao et al. | Graphene and TiO2 co-modified flower-like Bi2O2CO3: a novel multi-heterojunction photocatalyst with enhanced photocatalytic activity | |
| Wang et al. | Ag 2 O/TiO 2/V 2 O 5 one-dimensional nanoheterostructures for superior solar light photocatalytic activity | |
| Raja et al. | Facile sonochemical synthesis of Zn2SnO4-V2O5 nanocomposite as an effective photocatalyst for degradation of Eosin Yellow | |
| CN106423224B (en) | A kind of BiVO4/ BiOI heterojunction composite photocatalyst and its preparation method and application | |
| Zhang et al. | Preparation of coal-based C-Dots/TiO2 and its visible-light photocatalytic characteristics for degradation of pulping black liquor | |
| CN107486198B (en) | Bi based on peach blossom biomass carbon modification2WO6Preparation method and application of composite photocatalyst | |
| Nahyoon et al. | Synthesis of novel visible light driven MgO@ GO nanocomposite photocatalyst for degradation of Rhodamine 6G | |
| CN103599802A (en) | Preparation method of silver phosphate/graphene nanocomposite | |
| Ge et al. | A durable superhydrophobic BiOBr/PFW cotton fabric for visible light response degradation and oil/water separation performance | |
| Li et al. | Facile preparation of ZnO/Ag2CO3 heterostructured nanorod arrays with improved photocatalytic activity | |
| Liu et al. | Synthesis of BiOBrxI1− x solid solutions with dominant exposed {0 0 1} and {1 1 0} facets and their visible-light-induced photocatalytic properties | |
| Li et al. | P123-assisted preparation of Ag/Ag2O with significantly enhanced photocatalytic performance | |
| Chen et al. | Facile synthesis of MoS2/ZnO quantum dots for enhanced visible-light photocatalytic performance and antibacterial applications | |
| CN108355700A (en) | Polyoxometallate and its compound, preparation method and application | |
| Yu et al. | Interfacial structure and photocatalytic degradation performance of graphene oxide bridged chitin-modified TiO2/carbon fiber composites | |
| Liaqat et al. | Enhancing photocatalytic activity: investigating the synthesis and characterization of BiVO4/Cu2O/graphene ternary nanocomposites | |
| CN109465037A (en) | The magnetic CDs-MoS of micropollutants in a kind of degradation water2-Fe3O4The green synthesis method of catalysis material | |
| CN107244695B (en) | The method of controlledly synthesis diverse microcosmic appearance blue titanium dioxide nano-powder | |
| Haghighizadeh et al. | Green synthesis of ZnO-TiO2 nano-photocatalyst doped with Fe (III) ions using bitter olive extract to treat textile wastewater containing reactive dyes | |
| Mohammed et al. | Enhanced photocatalytic degradation activity of ZIF-8 doped with Ag2WO4 photocatalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |