CN107032391A - A kind of nanocrystalline pattern of stannic disulfide and the method for size regulation and control - Google Patents
A kind of nanocrystalline pattern of stannic disulfide and the method for size regulation and control Download PDFInfo
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- CN107032391A CN107032391A CN201611101942.4A CN201611101942A CN107032391A CN 107032391 A CN107032391 A CN 107032391A CN 201611101942 A CN201611101942 A CN 201611101942A CN 107032391 A CN107032391 A CN 107032391A
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- stannic disulfide
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- stannic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
A kind of nanocrystalline pattern of stannic disulfide and the method for size regulation and control, are related to field of functional materials.The nanocrystalline pattern of stannic disulfide and the method for size regulation and control, comprise the following steps：1) by adjusting control agent ultrasonic disperse in water, Tin tetrachloride pentahydrate and thioacetamide are sequentially added, after dissolving, continues ultrasound, obtains suspension；2) by step 1) obtained suspension moved into water heating kettle, oil bath heating is reacted while stirring, it is cooled to after end and pattern and the regulated stannic disulfide nano flake of size is dried to obtain after room temperature, washing, gained stannic disulfide nano flake can grinds to form fine powder.The regulated stannic disulfide nano flake of prepared pattern and size can be applied in the degraded of organic dyestuff, the reduction of heavy metal ion and lithium battery or electrode of solar battery material.Stannic disulfide pattern and size are with the change of additive addition in regular change.Have a very significant increase in the performance of photocatalytic degradation of dye.
Description
Technical field
The present invention relates to field of functional materials, the side of a kind of nanocrystalline pattern of stannic disulfide and size regulation and control is specifically related to
Method.
Background technology
Stannic disulfide has good chemical stability, especially under acidic or neutral conditions, with excellent physico
Learn and photoelectric properties, and by numerous studies and applied to photoelectric conversion material, holographic recording system, power conversion system and photocatalysis
Material.But the performance of stannic disulfide is largely influenceed by preparation method and condition, prior art hydro-thermal method, solvent
It is variously-shaped that the methods such as hot method and chemical vapor deposition prepare nanometer sheet, nano-plates, nano particle and nano flower etc., size model
Enclose also by several nanometers of generous quantum dots to a few micrometers of size, the specific surface area of material also with pattern and size difference and
Change.For example, document " Size-tunable hydrothermal synthesis of SnS2nanocrystals with
high performance in visible light-driven photocatalytic reductionof aqueous
Cr (VI), Yongcai Zhang et al. " are reached using monohydrate potassium as complexing agent by changing hydrothermal temperature and time
Change the size and the effect of specific surface area of the stannic disulfide prepared.
The content of the invention
In the prior art, find no so far by adding carbonitride, especially nano-pore carbonitride, two sulphur are prepared in hydro-thermal
During changing tin nanometer sheet, the method that original position regulates and controls its pattern and size, it is an object of the invention to provide a kind of curing
Sijna rice crystalline form looks and the method for size regulation and control.
Having another object of the present invention is to the regulated stannic disulfide nano flake of the pattern and size for providing preparation
Application in the degraded of engine dyeing material, the reduction of heavy metal ion and lithium battery or electrode of solar battery material.
The nanocrystalline pattern of stannic disulfide and the method for size regulation and control, comprise the following steps：
1) by adjusting control agent ultrasonic disperse in water, Tin tetrachloride pentahydrate and thioacetamide are sequentially added, after dissolving, after
Continuous ultrasound, obtains suspension；
In step 1) in, the adjusting control agent can use carbonitride or nano-pore carbonitride, and the carbonitride can be with melamine
Amine is that raw material semitight is sintered into carbonitride；The nano-pore carbonitride can use document (A template induced
method to synthesize nanoporous graphitic carbon nitride with enhanced
Photocatalytic activity under visible light, Qianjing Fan, et al.) method prepare；Institute
Stating adjusting control agent can be using big azotized carbon nano pieces of specific surface area such as nano-pore carbonitrides；The water can use deionized water；Institute
It is (0.05~0.5) g ︰ (1.5~2) g ︰ to state adjusting control agent, Tin tetrachloride pentahydrate, thioacetamide, the mass volume ratio example of water
(0.5~1) g ︰ (20~40) mL.
2) by step 1) obtained suspension moved into water heating kettle, and oil bath heating is reacted while stirring, is cooled to after terminating
Pattern and the regulated stannic disulfide nano flake of size, gained stannic disulfide nano flake feasibility study are dried to obtain after room temperature, washing
Wear into fine powder.
In step 2) in, the temperature of the heating response can be 100~200 DEG C, and the heating response time is 1~24h；It is described
Washing can carry out washing 3 times successively and alcohol is washed 1 time；The drying can dry 1~24h in 40~95 DEG C of baking ovens.
The regulated stannic disulfide nano flake of prepared pattern and size can the degraded of organic dyestuff, heavy metal from
Applied in the reduction of son and lithium battery or electrode of solar battery material.
Compared with prior art, the present invention has the special feature that as follows with advantage：
1) a kind of method that the present invention provides new regulation and control stannic disulfide pattern and size.
2) addition of adjusting control agent carbonitride or nano-pore carbonitride of the present invention can seldom realize stannic disulphide nano slice
The notable regulation and control of pattern and size.
3) adjusting control agent of the invention is dissolved or decomposed in water-heat process, only needs after the completion of reaction, centrifugation washing
Washed with alcohol and can obtain pure regulated stannic disulfide.
4) in the present invention, stannic disulfide pattern and size change with the change of additive addition in regular.
5) stannic disulfide prepared by currently preferred adjusting control agent addition under the same terms compared to being not added with adjusting control agent system
Standby stannic disulfide has a very significant increase in the performance of photocatalytic degradation of dye.
Brief description of the drawings
Fig. 1 is to be not added with stannic disulphide nano slice prepared by 150 DEG C of hydro-thermals of adjusting control agent.
Fig. 2 is that nano-pore carbonitride addition is 0.1g/1.75g SnCl4·5H2O, prepared by 150 DEG C of hydro-thermal reaction 12h
Stannic disulphide nano slice.
Fig. 3 is that nano-pore carbonitride addition is 0.23g/1.75g SnCl4·5H2It is prepared by O, 150 DEG C of hydro-thermal reaction 12h
Stannic disulphide nano slice.
Fig. 4 is that nano-pore carbonitride addition is 0.1g/1.75g SnCl4·5H2O, prepared by 160 DEG C of hydro-thermal reaction 12h
Stannic disulphide nano slice.
In Fig. 1~4, scale is 100nm.
Embodiment
It is for a more detailed description to the present invention with reference to embodiment, but the implementation of the present invention is not limited to this.
Embodiment 1
Regulation and control of the carbonitride to the nanocrystalline pattern of stannic disulfide and size are realized according to the following steps：
1) using melamine as raw material, 500 DEG C, insulation calcining 2h, then with same are warming up to by 2 DEG C/min heating rate
The heating rate of sample is warming up to 600 DEG C, and insulation calcining 2h takes out after cooling, grinds to form fine powder, that is, graphite type carbon nitride is made and receives
Rice piece；
2) in the deionization of 38 volume units, add after the carbonitride of 0.1 mass unit, ultrasonic 40min, in stirring
In the case of sequentially add the stannic chloride pentahydrate of 1.75 mass units and the thioacetamide of 0.75 mass unit, stirring and dissolving,
Then proceed to move into water heating kettle after ultrasonic 20min, 160 DEG C of reaction 12h.After cooling, centrifugation washing three times, alcohol is washed once, then
5h is dried in 65 DEG C of baking ovens, fine powder is ground to form with agate mortar, the stannic disulphide nano slice of pattern as shown in Figure 1 is obtained.
As follows measurement the present embodiment obtain it is regulated after stannic disulfide photocatalytic activity：
Take 0.1g catalyst to be added in 100mL, 10mg/L methyl orange solution, 20min is stirred in the dark and reaches that suction is de-
Attached balance, its absorbance is measured with ultraviolet specrophotometer, is converted into concentration with methyl orange standard curve, is designated as initial concentration
C0, 20min then is irradiated with the xenon lamp of 400nm optical filters, its absorbance is surveyed, is converted into concentration, C, the meter of degradation rate is designated as
Calculating formula is：(C0-C)/C0× 100%.
Photocatalysis performance test is carried out to the present embodiment, the degradation rate for obtaining methyl orange is 84.4%.
Embodiment 2
Regulation and control of the nano-pore carbonitride to the nanocrystalline pattern of stannic disulfide and size are realized according to the following steps：
1) using melamine as raw material, by diplomatic method with 2 DEG C/min, 500 DEG C of calcining 2h is warming up to, continue to heat up
To 600 DEG C of calcining 2h heating schedule, nano-pore carbonitride is prepared；
2) in the deionization of 38 volume units, add after the nano-pore carbonitride of 0.1 mass unit, ultrasonic 40min,
The stannic chloride pentahydrate of 1.75 mass units and the thioacetamide of 0.75 mass unit are sequentially added in the case of stirring, is stirred
Dissolving, then proceedes to move into water heating kettle after ultrasonic 20min, 160 DEG C of reaction 12h.After cooling, centrifugation washing three times, alcohol is washed once,
5h is dried in 65 DEG C of baking ovens again, fine powder is ground to form with agate mortar, the stannic disulphide nano slice of pattern as shown in Figure 2 is obtained.
By embodiment 1) method measure that the present embodiment obtains it is regulated after stannic disulfide photocatalytic activity, obtain first
Base orange degradation rate be：95.0%.
Embodiment 3
Regulation and control of the nano-pore carbonitride to the nanocrystalline pattern of stannic disulfide and size are realized according to the following steps：
1) using melamine as raw material, by diplomatic method with 2 DEG C/min, 500 DEG C of calcining 2h is warming up to, continue to heat up
To 600 DEG C of calcining 2h heating schedule, nano-pore carbonitride is prepared；
2) in the deionization of 38 volume units, add after the nano-pore carbonitride of 0.16 mass unit, ultrasonic 40min,
The stannic chloride pentahydrate of 1.75 mass units and the thioacetamide of 0.75 mass unit are sequentially added in the case of stirring, is stirred
Dissolving is mixed, then proceedes to move into water heating kettle after ultrasonic 20min, 160 DEG C of reaction 12h.After cooling, centrifugation washing three times, alcohol washes one
It is secondary, then 5h is dried in 65 DEG C of baking ovens, fine powder is ground to form with agate mortar, the stannic disulphide nano slice of pattern as shown in Figure 3 is obtained.
By embodiment 1) method measure that the present embodiment obtains it is regulated after stannic disulfide photocatalytic activity, obtain first
Base orange degradation rate be：81.8%.
Embodiment 4
Regulation and control of the nano-pore carbonitride to the nanocrystalline pattern of stannic disulfide and size are realized according to the following steps：
1) using melamine as raw material, by diplomatic method with 2 DEG C/min, 500 DEG C of calcining 2h is warming up to, continue to heat up
To 600 DEG C of calcining 2h heating schedule, nano-pore carbonitride is prepared；
2) in the deionization of 38 volume units, add after the nano-pore carbonitride of 0.10 mass unit, ultrasonic 40min,
The stannic chloride pentahydrate of 1.75 mass units and the thioacetamide of 0.75 mass unit are sequentially added in the case of stirring, is stirred
Dissolving is mixed, then proceedes to move into water heating kettle after ultrasonic 20min, 150 DEG C of reaction 12h.After cooling, centrifugation washing three times, alcohol washes one
It is secondary, then 5h is dried in 65 DEG C of baking ovens, fine powder is ground to form with agate mortar, the stannic disulphide nano slice of pattern as shown in Figure 4 is obtained.
By embodiment 1) method measure that the present embodiment obtains it is regulated after stannic disulfide photocatalytic activity, obtain first
Base orange degradation rate be：96.5%.
Present invention carbonitride or nano-pore carbonitride prepare the square piece of stannic disulfide six nanometer as adjusting control agent in hydro-thermal method
Regulate and control its pattern and size in brilliant process.Experiment find, it is regulated after stannic disulphide nano slice for organic dyestuff
During photocatalytic degradation, performance improves a lot than the stannic disulphide nano slice that not regulated Direct Hydrothermal is prepared.
Claims (10)
1. a kind of nanocrystalline pattern of stannic disulfide and the method for size regulation and control, it is characterised in that comprise the following steps：
1) by adjusting control agent ultrasonic disperse in water, Tin tetrachloride pentahydrate and thioacetamide are sequentially added, after dissolving, continues super
Sound, obtains suspension；
2) by step 1) obtained suspension moved into water heating kettle, and oil bath heating is reacted while stirring, and room temperature is cooled to after terminating,
Pattern and the regulated stannic disulfide nano flake of size are dried to obtain after washing, gained stannic disulfide nano flake can be ground to form carefully
Powder.
2. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
1) in, the adjusting control agent uses carbonitride or nano-pore carbonitride.
3. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 2 and the method for size regulation and control, it is characterised in that the nitrogen
Change carbon and be sintered into carbonitride by raw material semitight of melamine.
4. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
1) in, the adjusting control agent is using big azotized carbon nano pieces of specific surface area such as nano-pore carbonitrides.
5. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
1) in, the water uses deionized water.
6. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
1) in, the adjusting control agent, Tin tetrachloride pentahydrate, thioacetamide, the mass volume ratio example of water are (0.05~0.5) g ︰ (1.5
~2) g ︰ (0.5~1) g ︰ (20~40) mL.
7. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
2) in, the temperature of the heating response is 100~200 DEG C, and the heating response time is 1~24h.
8. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
2) in, the washing is that progress washing 3 times and alcohol are washed 1 time successively.
9. a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control, it is characterised in that in step
2) in, the drying is 1~24h of drying in 40~95 DEG C of baking ovens.
10. pattern and size prepared by a kind of nanocrystalline pattern of stannic disulfide as claimed in claim 1 and the method for size regulation and control
Regulated stannic disulfide nano flake is in the degraded of organic dyestuff, the reduction of heavy metal ion and lithium battery or solar cell
Applied in electrode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109192542A (en) * | 2018-09-29 | 2019-01-11 | 上海师范大学 | Supercapacitor stannic disulfide/graphite phase carbon nitride composite material and preparation method |
| CN109999841A (en) * | 2019-04-29 | 2019-07-12 | 陕西科技大学 | A kind of SnS2/1T-MoS2QDS composite photo-catalyst, preparation method and application |
| CN111285397A (en) * | 2020-03-09 | 2020-06-16 | 西安工业大学 | Method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets |
| CN113753942A (en) * | 2021-08-25 | 2021-12-07 | 天津大学 | Transition metal doped stannic disulfide nanoflower and preparation method thereof |
-
2016
- 2016-12-05 CN CN201611101942.4A patent/CN107032391B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| YONG CAI ZHANG ET AL.: ""Size-Tunable Hydrothermal Synthesis of SnS2 Nanocrystals with High Performance in Visible Light-Driven Photocatalytic Reduction of Aqueous Cr(VI)"", 《ENVIRON. SCI. TECHNOL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109192542A (en) * | 2018-09-29 | 2019-01-11 | 上海师范大学 | Supercapacitor stannic disulfide/graphite phase carbon nitride composite material and preparation method |
| CN109999841A (en) * | 2019-04-29 | 2019-07-12 | 陕西科技大学 | A kind of SnS2/1T-MoS2QDS composite photo-catalyst, preparation method and application |
| CN111285397A (en) * | 2020-03-09 | 2020-06-16 | 西安工业大学 | Method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets |
| CN113753942A (en) * | 2021-08-25 | 2021-12-07 | 天津大学 | Transition metal doped stannic disulfide nanoflower and preparation method thereof |
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| CN107032391B (en) | 2018-12-25 |
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