CN104096530A - SnS2 nanosheet as well as preparation method and application thereof - Google Patents

SnS2 nanosheet as well as preparation method and application thereof Download PDF

Info

Publication number
CN104096530A
CN104096530A CN201410347496.XA CN201410347496A CN104096530A CN 104096530 A CN104096530 A CN 104096530A CN 201410347496 A CN201410347496 A CN 201410347496A CN 104096530 A CN104096530 A CN 104096530A
Authority
CN
China
Prior art keywords
preparation
sns
solution
nanometer sheet
visible light
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.)
Granted
Application number
CN201410347496.XA
Other languages
Chinese (zh)
Other versions
CN104096530B (en
Inventor
吴正翠
薛业静
李保贰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Normal University
Original Assignee
Anhui Normal University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Anhui Normal University filed Critical Anhui Normal University
Priority to CN201410347496.XA priority Critical patent/CN104096530B/en
Publication of CN104096530A publication Critical patent/CN104096530A/en
Application granted granted Critical
Publication of CN104096530B publication Critical patent/CN104096530B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Landscapes

  • Catalysts (AREA)

Abstract

The invention provides an SnS2 nanosheet as well as a preparation method and an application thereof. The SnS2 nanosheet with both high adsorption and a high visible light catalysis degradation property is prepared with simple chemical liquid phase synthesis method. The preparation technology is simple and low in cost. The SnS2 nanosheet which can be applied to both adsorption and visible light degradation has the advantages of high adsorption, short adsorption equilibrium time, high visible light catalysis degradation efficiency, high degradation rate, environment-friendliness and the like.

Description

A kind of SnS 2nanometer sheet, preparation method and application thereof
Technical field
The invention belongs to preparation method of nano material and Environmental Chemistry cross-application field, be specifically related to possess the SnS of strong absorption and strong visible light photocatalytic degradation organic dyestuff performance simultaneously 2nanometer sheet, preparation method and application thereof.
Background technology
Along with the enhancing of people to environmental protection consciousness, the pollutant processing that industrialization brings has obtained extremely paying attention to, and wherein utilizes the application of absorption and photocatalytic degradation trade effluent more extensive.Aspect absorption, most widely used, maximum in current industrial sewage disposal is acticarbon, but the demand of factor can not meet the modernization development such as the bad mechanical strength of active carbon self, regeneration difficulty, recycling rate of waterused be low.Therefore, need the adsorbent of the more practicality of exploitation.Along with the further investigation of nano material, it is found that nano material has very large specific area, special skin effect, make material have very high surface-active and surface can, there are huge potentiality preparing aspect high-performance adsorbent.Aspect photocatalytic degradation, people have carried out research for a long time to titanium dioxide, but due to the wider (anatase: 3.2eV of its band gap; Rutile: 3.0eV), can only absorb and account for the seldom ultraviolet light of part of sunshine, limit its practical application.Therefore,, based on application and economic object, need to find the visible light catalyst that can effectively utilize solar energy.The metal sulfide with narrow band gap is good selection, in sulfide CdS research more, but cadmium compound has carcinogenic risk, has limited its practical application.By contrast, SnS 2hypotoxicity and the visible light catalysis activity of Geng Gao, have more practical application potentiality.
As a kind of N-shaped semi-conducting material, SnS 2there are stratiform six side CdI 2the crystal structure of type, band gap is about 2.35eV, has stronger anisotropic optical property, makes to have in its layer structure a large amount of unsaturated electronics, can more effectively utilize sunshine and promote light to produce the separation of electron-hole pair, show very strong photocatalytic degradation ability.
At present aspect sewage disposal, people are absorption and the photocatalysis performance of research material mostly separately, and has ignored the collaborative of multiple performance that material may have.The photochemical catalyst that simultaneously possesses strong absorption and strong Visible Light Induced Photocatalytic if can develop, will have higher practical value.Preparation has the SnS of special two-dimensional structure 2nanometer sheet possesses the superior function of strong absorption and strong visible light photocatalytic degradation simultaneously, still there is no at present correlative study.
Summary of the invention
The object of the present invention is to provide a kind of SnS 2nanometer sheet and preparation method thereof, utilizes low temperature liquid phase synthetic method, has technique feature simple, with low cost.
A further object of the invention, provides a kind of SnS 2nanometer sheet is as the application of strong absorption and strong visible light photocatalytic degradation organic dyestuff.
A kind of SnS provided by the invention 2nanometer sheet, is round sheet, and diameter is at 220～280nm, and thickness is at 10～20nm.
A kind of SnS provided by the invention 2the preparation method of nanometer sheet, comprises the following steps:
(1) DDTC three hydration sodium diethyldithiocarbamates are dissolved in the solution that ethylene glycol mixes with glacial acetic acid, add subsequently SnCl 45H 2o, continues to stir 10min, obtains colourless solution;
(2) solution that then prepared by step (1) is transferred in 50mL teflon-lined stainless steel cauldron and is sealed, add thermal response, after finishing, reaction naturally cools to room temperature, the yellow centrifugal collection of sediment is also respectively washed 3-5 time with deionized water and absolute ethyl alcohol, is placed in 60 DEG C of vacuum drying chambers and is dried 12h.
The solution that described in step (1), ethylene glycol mixes with glacial acetic acid, volume ratio is 2～10:1;
Adding the solution concentration that three hydration sodium diethyldithiocarbamates mix with glacial acetic acid at ethylene glycol in step (1) is 0.03～0.2mol/L;
In step (1), add SnCl 45H 2o is 1:1.7～3 with the ratio of the amount of substance of three hydration sodium diethyldithiocarbamates;
Step adds thermal response described in (2), 140～180 DEG C of temperature, reaction time 8～24h.
The present invention also provides a kind of SnS 2nanometer sheet possesses the application of strong absorption and strong visible light photocatalytic degradation organic dyestuff simultaneously.
SnS prepared by the present invention 2nanometer sheet visible light photocatalytic degradation organic dyestuff, taking methylene blue as example.
Absorption method of testing: 10mg SnS prepared by the present invention 2nanometer sheet joins in 150mL0.025mmol/L methylene blue solution, is placed in dark place, after ultrasonic 1-2 minute, stirs with magnetic stirring apparatus always, makes it to keep being dispersed in solution.After 20min, reach the attached balance of absorption-desorption, get 5ml sample, after centrifugal (10000rpm, 2min), get supernatant, use ultraviolet-visible spectrophotometer to measure the absorption spectrum of solution.Determine the concentration of methylene blue by the characteristic absorption peak at 662nm place.
Light degradation method of testing: by the above-mentioned methylene blue solution reaching after the attached balance of absorption-desorption, use 300W xenon lamp (λ >420nm) as radiation of visible light.Get 5mL sample every 10min, after centrifugal (10000rpm, 2min), get supernatant, use ultraviolet-visible spectrophotometer to measure the absorption spectrum of solution.Determine the concentration of methylene blue by the characteristic absorption peak at 662nm place.
The present invention adopts chemical liquid phase synthetic method, and DDTC not only provides sulphur source also to play coordination, and glacial acetic acid provides weak acid environment to make the SnS forming 2there are a large amount of unsaturated electric charges in nanometer sheet surface, has also greatly promoted photocatalytic degradation efficiency when having strengthened adsorption capacity.Prepared by technique simple, with low cost.Provided by the present invention possess absorption and the application of visible light photocatalytic degradation simultaneously, have that adsorptivity is strong, time of equilibrium adsorption is short and visible light photocatalytic degradation efficiency is high, degradation rate soon, advantages of environment protection.
Brief description of the drawings
Fig. 1 is SnS prepared by embodiment 1 2x-ray powder diffraction (XRD) figure of nanometer sheet.
Fig. 2 is SnS prepared by embodiment 1 2sEM (SEM) figure of nanometer sheet.
Fig. 3 is SnS prepared by embodiment 1 2transmission electron microscope (TEM) figure of nanometer sheet.
Fig. 4 is SnS prepared by embodiment 1 2high resolution transmission electron microscopy (HRTEM) figure of nanometer sheet.
Fig. 5 is SnS prepared by embodiment 1 2solid UV Diffuse Reflectance Spectroscopy (UV-vis DRS) figure of nanometer sheet.
Fig. 6 is embodiment 2SnS 2ultra-violet absorption spectrum (UV) figure of nanometer sheet absorption and Visible Light Induced Photocatalytic methylene blue organic dyestuff.
Fig. 7 is embodiment 2SnS 2the concentration changes with time figure of nanometer sheet absorption and visible light photocatalytic degradation methylene blue organic dyestuff.
Detailed description of the invention
Embodiment 1
A kind of SnS 2the preparation method of nanometer sheet, comprises the following steps:
(1) get 2mmol tri-hydration sodium diethyldithiocarbamates (DDTC) and be dissolved in the acid solution that 25mL ethylene glycol mixes with 5mL glacial acetic acid, add subsequently 1mmol SnCl 45H 2o, continues to stir 10min to colourless solution.
(2) then liquid rotating is moved on in 50mL teflon-lined stainless steel cauldron, sealing is also heated 12h at 160 DEG C, naturally cools to room temperature.The yellow centrifugal collection of sediment is also respectively washed for several times with deionized water and absolute ethyl alcohol, is finally placed in 60 DEG C of vacuum drying chambers and is dried 12h.
The structure of product and morphology characterization
Embodiment 1 products therefrom (Cu target) is carried out to the thing identification of phases with Rigaku TTRIII X-ray powder diffraction instrument, as shown in Figure 1.Contrast JCPDS standard card (83-1705), all diffraction maximums and six side's phase SnS 2fit like a glove, occur without other impurity peaks, show that the product making is the SnS of six side's phases 2.Product is carried out to morphology analysis with ESEM, result as shown in Figure 2.Show prepared SnS 2for nanometer sheet structure, average diameter 200nm.Product is carried out to morphology analysis with transmission electron microscope, result as shown in Figure 3.Further show that product is the nanometer sheet structure of diameter 200nm.Product is carried out to structural analysis with high-resolution-ration transmission electric-lens, result as shown in Figure 4.The interplanar distance of its 0.32nm can index be six side's phase SnS 2(100) crystal face.With ultraviolet-uisible spectrophotometer to SnS 2the solid UV Diffuse Reflectance Spectroscopy of nanometer sheet is analyzed, and result as shown in Figure 5.Show prepared SnS 2nanometer sheet has obvious absorption at visible region.
Embodiment 2
A kind of SnS 2the application of nanometer sheet absorption and visible light photocatalytic degradation organic dyestuff, taking methylene blue organic dyestuff as example.
Absorption method of testing: 10mg SnS prepared by embodiment 1 2nanometer sheet joins in 150mL0.025mmol/L methylene blue solution, is placed in dark place, after ultrasonic 1-2 minute, stirs with magnetic stirring apparatus always, makes it to keep being dispersed in solution.After 20min, reach the attached balance of absorption-desorption, get 5mL sample, after centrifugal (10000rpm, 2min), get supernatant.By measuring the spectrogram of UV absorption, calculate adsorbance, be 66.6%, result is as shown in Figure 6,7.
Light degradation method of testing: by the solution reaching after the attached balance of absorption-desorption, use 300W xenon lamp (λ >420nm) as radiation of visible light.Get 5mL solution every 10min, after centrifugal (10000rpm, 2min), get supernatant.By measuring the spectrogram of UV absorption, calculate photocatalytic degradation amount, concentration excess dye concentration 5.1% after photocatalytic degradation 1h, result is as shown in Figure 6,7.
Embodiment 3
A kind of SnS 2the preparation method of nanometer sheet, comprises the following steps:
(1) get 2mmol tri-hydration sodium diethyldithiocarbamates (DDTC) and be dissolved in the acid solution that 15mL ethylene glycol mixes with 5mL glacial acetic acid, add subsequently 1.9mmol SnCl 45H 2o, continues to stir 10min to colourless solution.
(2) then liquid rotating is moved on in 50mL teflon-lined stainless steel cauldron, sealing is also heated 15h at 140 DEG C, naturally cools to room temperature.The yellow centrifugal collection of sediment is also respectively washed for several times with deionized water and absolute ethyl alcohol, is finally placed in 60 DEG C of vacuum drying chambers and is dried 12h.
Embodiment 4
A kind of SnS 2the preparation method of nanometer sheet, comprises the following steps:
(1) get 5.4mmol tri-hydration sodium diethyldithiocarbamates (DDTC) and be dissolved in the acid solution that 32mL ethylene glycol mixes with 4mL glacial acetic acid, add subsequently 1.8mmol SnCl 45H 2o, continues to stir 10min to colourless solution.
(2) then liquid rotating is moved on in 50mL teflon-lined stainless steel cauldron, sealing is also heated 20h at 180 DEG C, naturally cools to room temperature.The yellow centrifugal collection of sediment is also respectively washed for several times with deionized water and absolute ethyl alcohol, is finally placed in 60 DEG C of vacuum drying chambers and is dried 12h.

Claims (7)

1. a SnS 2nanometer sheet, is characterized in that, is round sheet, and diameter is 220～280nm, and thickness is 10～20nm.
2. a SnS 2the preparation method of nanometer sheet, is characterized in that, described preparation method comprises the following steps:
(1) DDTC three hydration sodium diethyldithiocarbamates are dissolved in the solution that ethylene glycol mixes with glacial acetic acid, add subsequently SnCl 45H 2o, continues to stir 10min, obtains colourless solution;
(2) solution that then prepared by step (1) is transferred in 50mL teflon-lined stainless steel cauldron and is sealed, add thermal response, after finishing, reaction naturally cools to room temperature, the yellow centrifugal collection of sediment is also respectively washed 3-5 time with deionized water and absolute ethyl alcohol, is placed in 60 DEG C of vacuum drying chambers and is dried 12h.
3. preparation method according to claim 2, is characterized in that, the solution that described in step (1), ethylene glycol mixes with glacial acetic acid, and volume ratio is 2～10:1.
4. preparation method according to claim 2, is characterized in that, adding the solution concentration that three hydration sodium diethyldithiocarbamates mix with glacial acetic acid at ethylene glycol in step (1) is 0.03～0.2mol/L.
5. preparation method according to claim 2, is characterized in that, adds SnCl in step (1) 45H 2o is 1:1.7～3 with the ratio of the amount of substance of three hydration sodium diethyldithiocarbamates.
6. preparation method according to claim 2, is characterized in that, step adds thermal response described in (2), 140～180 DEG C of temperature, reaction time 8～24h.
7. a SnS claimed in claim 1 2nanometer sheet is as the application of absorption and visible light photocatalytic degradation organic dyestuff.
CN201410347496.XA 2014-07-21 2014-07-21 A kind of SnS2Nanometer sheet, preparation method and application thereof Expired - Fee Related CN104096530B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410347496.XA CN104096530B (en) 2014-07-21 2014-07-21 A kind of SnS2Nanometer sheet, preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410347496.XA CN104096530B (en) 2014-07-21 2014-07-21 A kind of SnS2Nanometer sheet, preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN104096530A true CN104096530A (en) 2014-10-15
CN104096530B CN104096530B (en) 2016-07-06

Family

ID=51665304

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410347496.XA Expired - Fee Related CN104096530B (en) 2014-07-21 2014-07-21 A kind of SnS2Nanometer sheet, preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN104096530B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106711446A (en) * 2016-12-07 2017-05-24 陕西科技大学 Preparation method of nanosheet assembled walnut-shaped SnS2 sodium-ion battery anode material
CN106753695A (en) * 2016-12-14 2017-05-31 刘兴旺 A kind of lube oil additive
CN107224984A (en) * 2017-05-23 2017-10-03 国家纳米科学中心 Artificial gold cerium sulphide cerium oxide ternary heterojunction, preparation method and the usage
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
CN111346595A (en) * 2020-03-09 2020-06-30 浙江理工大学 SnS2@SnO2Heterojunction and preparation method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102476825A (en) * 2010-11-24 2012-05-30 扬州大学 Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102476825A (en) * 2010-11-24 2012-05-30 扬州大学 Method for preparing high-quality stannic sulfide nanosheet by use of single-source molecular precursor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YEJUN ZHANG ET AL: "Ultralarge single crystal SnS rectangular nanosheets", 《CHEM. COMMUN.》 *
范英华等: "SnS2纳米材料的水热合成及光催化性质", 《无机化学学报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106711446A (en) * 2016-12-07 2017-05-24 陕西科技大学 Preparation method of nanosheet assembled walnut-shaped SnS2 sodium-ion battery anode material
CN106753695A (en) * 2016-12-14 2017-05-31 刘兴旺 A kind of lube oil additive
CN107224984A (en) * 2017-05-23 2017-10-03 国家纳米科学中心 Artificial gold cerium sulphide cerium oxide ternary heterojunction, preparation method and the usage
CN107224984B (en) * 2017-05-23 2020-03-03 国家纳米科学中心 Tin sulfide-cerium oxide ternary heterojunction and preparation method and application thereof
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
CN111346595A (en) * 2020-03-09 2020-06-30 浙江理工大学 SnS2@SnO2Heterojunction and preparation method

Also Published As

Publication number Publication date
CN104096530B (en) 2016-07-06

Similar Documents

Publication Publication Date Title
Fang et al. Direct Z-scheme CdFe2O4/g-C3N4 hybrid photocatalysts for highly efficient ceftiofur sodium photodegradation
Zhang et al. Self-assembled perylene diimide based supramolecular heterojunction with Bi2WO6 for efficient visible-light-driven photocatalysis
Zhou et al. Highly porous carbon nitride by supramolecular preassembly of monomers for photocatalytic removal of sulfamethazine under visible light driven
Chen et al. Preparation of CdS/g-C3N4/MOF composite with enhanced visible-light photocatalytic activity for dye degradation
Soltani et al. Sono-synthesis of bismuth ferrite nanoparticles with high photocatalytic activity in degradation of Rhodamine B under solar light irradiation
Zhu et al. Insight into the role of Ti3+ in photocatalytic performance of shuriken-shaped BiVO4/TiO2− x heterojunction
Zhang et al. Microwave hydrothermal synthesis of AgInS2 with visible light photocatalytic activity
Hunge Sunlight assisted photoelectrocatalytic degradation of benzoic acid using stratified WO3/TiO2 thin films
Zhao et al. Atomic single layer graphitic-C 3 N 4: fabrication and its high photocatalytic performance under visible light irradiation
Chen et al. Kinetic comparison of photocatalysis with H2O2-free photo-Fenton process on BiVO4 and the effective antibiotic degradation
She et al. Controllable synthesis of CeO 2/gC 3 N 4 composites and their applications in the environment
Zhang et al. Near-infrared light photocatalysis with metallic/semiconducting HxWO3/WO3 nanoheterostructure in situ formed in mesoporous template
Kumar et al. Synthesis of novel and stable gC 3 N 4/N-doped SrTiO 3 hybrid nanocomposites with improved photocurrent and photocatalytic activity under visible light irradiation
Hou et al. In situ synthesis of α–β phase heterojunction on Bi2O3 nanowires with exceptional visible-light photocatalytic performance
Zhang et al. One-step in situ solvothermal synthesis of SnS2/TiO2 nanocomposites with high performance in visible light-driven photocatalytic reduction of aqueous Cr (VI)
CN104096530A (en) SnS2 nanosheet as well as preparation method and application thereof
Han et al. In-situ polymerization for PPy/g-C3N4 composites with enhanced visible light photocatalytic performance
Chang et al. Synthesis and significantly enhanced visible light photocatalytic activity of BiOCl/AgBr heterostructured composites
CN103934012B (en) SnS 2/ g-C 3n 4composite nano plate photochemical catalyst and preparation method
Wang et al. Facile fabrication of CdS/UiO-66-NH2 heterojunction photocatalysts for efficient and stable photodegradation of pollution
Hariz et al. A novel MgCr2O4/WO3 hetero-junction photocatalyst for solar photo reduction of hexavalent chromium Cr (VI)
Ahmed et al. Surfactant-free synthesis of m-BiVO4 nanoribbons and enhanced visible-light photocatalytic properties
Su et al. Direct hydrolysis synthesis of BiOI flowerlike hierarchical structures and it's photocatalytic activity under simulated sunlight irradiation
Hussain et al. The synthesis of a BiOCl x Br 1− x nanostructure photocatalyst with high surface area for the enhanced visible-light photocatalytic reduction of Cr (vi)
Yuan et al. Synthesis and photocatalytic properties of core–shell TiO2@ ZnIn2S4 photocatalyst

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160706

Termination date: 20180721