CN106238071A - A kind of method using absorption calcination method to prepare ZnS@C composite - Google Patents
A kind of method using absorption calcination method to prepare ZnS@C composite Download PDFInfo
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- CN106238071A CN106238071A CN201610541959.5A CN201610541959A CN106238071A CN 106238071 A CN106238071 A CN 106238071A CN 201610541959 A CN201610541959 A CN 201610541959A CN 106238071 A CN106238071 A CN 106238071A
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000001354 calcination Methods 0.000 title claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 title description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 57
- 239000004005 microsphere Substances 0.000 claims abstract description 21
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 17
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 5
- 239000011593 sulfur Substances 0.000 claims abstract description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000007767 bonding agent Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
-
- 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
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of employing and adsorbs the method that calcination method prepares ZnS@C composite: 1) by Zn (NO3)2·6H2O and sulfur source add in deionized water, add and utilize homogeneous hydrothermograph to react 3～5h at 150～180 DEG C in hydrothermal reaction kettle after stirring, and product washing final vacuum is dried to obtain ZnS microsphere；2) citric acid be dissolved in deionized water prepare precursor aqueous solution, take step 1) the zinc sulfide microsphere prepared adds in precursor aqueous solution, ultrasonic after stirring obtain ZnS citric acid presoma；3) by ZnS citric acid presoma in vacuum drying, afterwards at tube furnace N2Under atmosphere, 350～550 DEG C of annealing obtains the ZnS@C product of grey black.Present invention process equipment requirements is simple, and cost is relatively low, and product morphology size and carbon layers having thicknesses are prone to regulation and control, thus very economical, practical, there is good industrial prospect；It has more preferable photocatalytic Activity and stabill relative to ZnS.
Description
Technical field
The present invention relates to Nano semiconductor field of compound material, particularly to a kind of method preparing ZnS@C composite.
Background technology
Nano-zinc sulfide is a kind of important Illuminant nanometer material, and is a kind of semiconductor material with wide forbidden band, and ZnS has
The characteristics such as infrared transparent, fluorescence, phosphorescent.Important work is had in the numerous areas such as electronics industry, chemical industry, national defense industry
With, therefore suffer from extensive concern and the research of scientific research personnel.But in the middle of its actual application, people gradually find pure ZnS
Nano material itself has some limitation and defect, thus hinders our the further applied research to it.Pure
Stability when ZnS nano material can only be excited and be in excited state by the ultraviolet light wave that wavelength is shorter is not the highest.
Summary of the invention
It is an object of the invention to provide a kind of method using absorption-calcination method to prepare ZnS@C composite, to solve
Above-mentioned technical problem.The inventive method is undertaken in two steps product crystallinity and size is easily controllable, and carbon layers having thicknesses distribution is the most more held
Easy-regulating.
In order to achieve the above object, the preparation method that the present invention uses is as follows:
A kind of method using absorption-calcination method to prepare ZnS@C composite, comprises the following steps:
1) by Zn (NO3)2·6H2O and sulfur source add in deionized water, add in hydrothermal reaction kettle and utilize homogeneously after stirring
Hydrothermograph reacts 3～5h at 150～180 DEG C, and product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid be dissolved in deionized water preparing precursor aqueous solution, take step 1) the zinc sulfide microsphere prepared adds forerunner
In solution, ultrasonic rear stirring obtains ZnS-citric acid presoma；
3) by ZnS-citric acid presoma in vacuum drying, afterwards at tube furnace N2Under atmosphere, 350～550 DEG C of annealing obtain
The ZnS@C product of grey black.
3) by ZnS-citric acid presoma 60 DEG C dry 6～12h in vacuum drying oven, afterwards at tube furnace N2Under atmosphere
350～550 DEG C of annealing 2h obtain the ZnS@C product of grey black.
Further, step 1) in use thiourea be sulfur source.
Further, step 1) in Zn (NO3)2·6H2The mol ratio of O and thiourea is (1～2): (30～40)；Step 2)
Precursor aqueous solution in every Aml deionized water adds the citric acid of Bg；The quality of the zinc sulfide microsphere added in precursor aqueous solution is
Cg；A:B:C=(5～10): (0.1～0.2): (0.2～1).
Further, step 2) in be stirred for 6～12h after ultrasonic 30min and obtain ZnS-citric acid presoma.
Further, step 2) in citric acid as bonding agent.
Further, step 3) in by ZnS-citric acid presoma in vacuum drying oven 60 DEG C be dried 6～12h.
Further, step 3) in annealing time be 2h.
Relative to prior art, the method have the advantages that
The present invention prepares ZnS@C composite with absorption-calcination method in situ, utilizes the combination on citric acid nanometer ZnS surface,
Form the citric acid cladding to ZnS, and pass through N2Under atmosphere, calcination processing obtains ZnS@C composite, and its carbon layers having thicknesses is prone to
Regulation, appearance and size is controlled and good dispersion.Reaction raw materials of the present invention is easy to get, and Processes and apparatus requires simple, and required cost is relatively
Low beneficially industrialized production.Material with carbon element has preferable electric conductivity, to the good adsorption of organic pollution and certain because of it
Visible absorption and be widely studied and be applied to the modification to photocatalyst, it is combined closely can promote with zinc sulfide microsphere
Its photocatalytic Activity and stabill have bigger lifting.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the carbon cladding zinc sulfide microsphere prepared by the embodiment of the present invention 2.
Fig. 2 is the SEM figure of the carbon cladding zinc sulfide microsphere prepared by the embodiment of the present invention 2.
Fig. 3 is the photocatalytic degradation figure of the carbon cladding zinc sulfide microsphere prepared by the embodiment of the present invention 2.
Detailed description of the invention
Embodiment 1:
1) by the Zn (NO of 1mmol3)2·6H2The thiourea of O and 40mmol adds in 40ml deionized water, adds after stirring 1h
Utilizing homogeneous hydrothermograph to react 3h at 150 DEG C in hydrothermal reaction kettle, product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid of 0.1g is dissolved in 5ml deionized water prepared precursor aqueous solution, subsequently by above-mentioned for 1g zinc sulfide microsphere
Add in precursor aqueous solution, be stirred for 6h after ultrasonic 30min and obtain ZnS-citric acid presoma；
3) by ZnS-citric acid presoma 60 DEG C of dry 12h in vacuum drying oven, afterwards at tube furnace N2Under atmosphere 350
DEG C annealing 2h obtains the ZnS@C product of grey black.
Embodiment 2:
1) by the Zn (NO of 2mmol3)2·6H2The thiourea of O and 30mmol adds in 40ml deionized water, adds after stirring 1h
Utilizing homogeneous hydrothermograph to react 5h at 180 DEG C in hydrothermal reaction kettle, product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid of 0.2g is dissolved in 10ml deionized water prepared precursor aqueous solution, subsequently by micro-for above-mentioned for 0.5g zinc sulfide
Ball adds in precursor aqueous solution, is stirred for 12h and obtains ZnS-citric acid presoma after ultrasonic 30min；
3) by ZnS-citric acid presoma 60 DEG C of dry 8h in vacuum drying oven, afterwards at tube furnace N2Under atmosphere 450
DEG C annealing 2h obtains the ZnS@C product of grey black.
Fig. 1 is the XRD figure of the carbon cladding zinc sulfide microsphere prepared by the embodiment of the present invention 2, as can be seen from the figure product
Purity high, crystallinity is strong.
Fig. 2 is the SEM figure of the carbon cladding zinc sulfide microsphere prepared by this embodiment of the present invention 2, it can be seen that carbon
Cladding zinc sulfide microsphere is about the micron ball of 200nm.
Fig. 3 is the carbon cladding zinc sulfide microsphere photocatalytic degradation figure to rhodamine B prepared by the embodiment of the present invention 2, from
It can be seen that the photocatalytic activity of ZnS@C composite photo-catalyst after carbon coated is substantially better than simple ZnS in figure.
Embodiment 3:
1) by the Zn (NO of 1.5mmol3)2·6H2The thiourea of O and 30mmol adds in 40ml deionized water, adds after stirring 1h
Entering to utilize in hydrothermal reaction kettle homogeneous hydrothermograph to react 3h at 180 DEG C, product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid of 0.1g is dissolved in 10ml deionized water prepared precursor aqueous solution, subsequently by micro-for above-mentioned for 0.2g zinc sulfide
Ball adds in precursor aqueous solution, is stirred for 8h and obtains ZnS-citric acid presoma after ultrasonic 30min；
3) by ZnS-citric acid presoma 60 DEG C of dry 6h in vacuum drying oven, afterwards at tube furnace N2Under atmosphere 550
DEG C annealing 2h obtains the ZnS@C product of grey black.
Embodiment 4:
1) by the Zn (NO of 2mmol3)2·6H2The thiourea of O and 40mmol adds in 40ml deionized water, adds after stirring 1h
Utilizing homogeneous hydrothermograph to react 5h at 160 DEG C in hydrothermal reaction kettle, product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid of 0.15g is dissolved in 8ml deionized water prepared precursor aqueous solution, subsequently by micro-for above-mentioned for 0.6g zinc sulfide
Ball adds in precursor aqueous solution, is stirred for 10h and obtains ZnS-citric acid presoma after ultrasonic 30min；
3) by ZnS-citric acid presoma 60 DEG C of dry 10h in vacuum drying oven, afterwards at tube furnace N2Under atmosphere 550
DEG C annealing 2h obtains the ZnS@C product of grey black.
Claims (7)
1. one kind uses the method that absorption-calcination method prepares ZnS C composite, it is characterised in that comprise the following steps:
1) by Zn (NO3)2·6H2O and sulfur source add in deionized water, add in hydrothermal reaction kettle and utilize homogeneous hydro-thermal after stirring
Instrument reacts 3～5h at 150～180 DEG C, and product washing final vacuum is dried to obtain ZnS microsphere；
2) citric acid be dissolved in deionized water preparing precursor aqueous solution, take step 1) the zinc sulfide microsphere prepared adds precursor aqueous solution
In, ultrasonic rear stirring obtains ZnS-citric acid presoma；
3) by ZnS-citric acid presoma in vacuum drying, afterwards at tube furnace N2Under atmosphere, 350～550 DEG C of annealing obtain greyish black
The ZnS@C product of color.
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 1, its feature exists
In, step 1) in use thiourea be sulfur source.
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 2, its feature exists
In, step 1) in Zn (NO3)2·6H2The mol ratio of O and thiourea is (1～2): (30～40)；Step 2) precursor aqueous solution in every
Aml deionized water adds the citric acid of Bg；The quality of the zinc sulfide microsphere added in precursor aqueous solution is Cg；A:B:C=(5～
10): (0.1～0.2): (0.2～1).
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 1, its feature exists
In, step 2) in be stirred for 6～12h after ultrasonic 30min and obtain ZnS-citric acid presoma.
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 1, its feature exists
In, step 2) in citric acid as bonding agent.
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 1, its feature exists
In, step 3) in by ZnS-citric acid presoma in vacuum drying oven 60 DEG C be dried 6～12h.
A kind of method using absorption-calcination method to prepare ZnS@C composite the most according to claim 1, its feature exists
In, step 3) in annealing time be 2h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106953092A (en) * | 2017-04-14 | 2017-07-14 | 哈尔滨工业大学 | A kind of preparation method of positive material for lithium-sulfur battery |
| CN107265495A (en) * | 2017-07-20 | 2017-10-20 | 济南大学 | Non-template method prepares zinc sulphide microballoon |
| CN108832094A (en) * | 2018-06-12 | 2018-11-16 | 陕西科技大学 | A kind of one-step method prepares spherical artificial gold/stannous sulfide lithium ion battery negative material method |
| CN109225272A (en) * | 2018-10-19 | 2019-01-18 | 郴州高鑫铂业有限公司 | A kind of Pt-ZnS/C catalyst and its preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106953092A (en) * | 2017-04-14 | 2017-07-14 | 哈尔滨工业大学 | A kind of preparation method of positive material for lithium-sulfur battery |
| CN107265495A (en) * | 2017-07-20 | 2017-10-20 | 济南大学 | Non-template method prepares zinc sulphide microballoon |
| CN108832094A (en) * | 2018-06-12 | 2018-11-16 | 陕西科技大学 | A kind of one-step method prepares spherical artificial gold/stannous sulfide lithium ion battery negative material method |
| CN109225272A (en) * | 2018-10-19 | 2019-01-18 | 郴州高鑫铂业有限公司 | A kind of Pt-ZnS/C catalyst and its preparation method and application |
| CN109225272B (en) * | 2018-10-19 | 2021-09-07 | 湖南高鑫铂业有限公司 | Pt-ZnS/C catalyst and preparation method and application thereof |
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