CN102527318A - Tin bisulfide single-crystal nanosheets selectively absorbing organic dyes, and preparation method thereof - Google Patents
Tin bisulfide single-crystal nanosheets selectively absorbing organic dyes, and preparation method thereof Download PDFInfo
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- CN102527318A CN102527318A CN2011104592777A CN201110459277A CN102527318A CN 102527318 A CN102527318 A CN 102527318A CN 2011104592777 A CN2011104592777 A CN 2011104592777A CN 201110459277 A CN201110459277 A CN 201110459277A CN 102527318 A CN102527318 A CN 102527318A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses tin bisulfide single-crystal nanosheets selectively absorbing organic dyes, and a preparation method thereof. The hydrothermal temperature and the sulfur source are controlled to modulate the size dimension, specific area and other parameters of the tin bisulfide single-crystal nanosheets. The tin bisulfide single-crystal nanosheets prepared by the invention have selectivity on absorption of different types of organic dyes, can be used for absorbing dye molecules and reducing the concentration of dye wastewater, and can be used as an auxiliary for a photocatalyst to cooperate with the photocatalyst to treat high-concentration dye wastewater.
Description
Technical field
The invention belongs to the adsorbent field, be specifically related to a kind of stannic disulfide single crystal nanoplate to the organic dyestuff selective absorption and preparation method thereof.
Background technology
The crystallization stannic disulfide has effulgent golden yellow, is called as pseudo-gold or type bronze, in industry, uses mainly as a kind of colouring agent.Up-to-date research shows; With lepidiod stannic disulfide is raw material; The present widely used bronzing varnish of instead (copper powder) is used for fields such as urban construction, advertisement, printing, decoration, the fine arts, weaving, clothes, is prone to shortcomings such as oxidation, weatherability, resistance to acids and bases and poor heat resistance to overcome bronzing varnish (copper powder).
Because of stannic disulfide has wide band gap (2.18 eV), make it can be used as basic heterogeneous structure material again, potential application is arranged in the solar cell photoelectric switching device; Can also be as the form absorbing material in the solar cell; Can also prepare the quantum structure of trap in theory.
In addition, the weak interlaminar action power of stannic disulfide makes the monocrystalline of this lamellar compound to process base material very easily along smooth surperficial cleavage, comes the stringer organic dyestuff with the molecular beam epitaxial growth method, and then is used to study its optical property.But as the high-efficiency adsorbent of organic dyestuff, unprecedented research report.
Summary of the invention
The objective of the invention is to propose a kind of stannic disulfide single crystal nanoplate to organic dyestuff selective absorption in the water body and preparation method thereof; Prepared stannic disulfide single crystal nanoplate has very strong absorption property to the fluorescein(e) dye molecule that contains the nominal price azanyl, is having a good application prospect aspect the processing of dye wastewater with high concentration.
For this reason, the present invention takes following technical scheme:
Prepare said stannic disulfide single crystal nanoplate according to the following steps:
Under the room temperature, the predecessor of stannic chloride pentahydrate and the sulphur mol ratio according to 1: 2～1: 4 is dissolved in the deionized water, under 110 ℃～200 ℃ hydro-thermals, keeps 20～30h; Naturally cool to room temperature then; Centrifugal, filter washing; Drying promptly gets the hexagon stannic disulfide single crystal nanoplate to the organic dyestuff selective absorption of the present invention.
The mol ratio of stannic chloride pentahydrate and deionized water is 1: 800～1: 1000.
The predecessor of said sulphur is a kind of in thioacetamide and the thiocarbamide.
A preferred embodiment of the present invention is: the predecessor of sulphur is a thioacetamide, and the mol ratio of stannic chloride pentahydrate and thioacetamide is 1: 4, and hydrothermal temperature is 110 ℃.
Prepared as stated above stannic disulfide material has following characteristic: be the hexagonal crystal phase, grain shape is a hexagon, and it is of a size of 20～50nm, and specific area is at 56～151m
2/ g, the aperture is at 3.2～19.2nm.
The present invention adopts hydrothermal method, through control hydrothermal temperature and change sulphur source, realizes the isoparametric modulation of size, specific area, pore structure to the stannic disulfide single crystal nanoplate.In the test of the absorption property of dye molecule, prepared monocrystalline stannic disulphide nano slice has selectivity to the absorption property of dissimilar dye molecules, and its absorption property to the fluorescein(e) dye molecule that contains the nominal price azanyl is very strong.It can be used for adsorpting dye molecule having a good application prospect aspect the processing of dye wastewater with high concentration, reduces waste water from dyestuff concentration, as the assistant of photochemical catalyst, and cooperative photocatalysis agent treatment of high concentration waste water from dyestuff.
Description of drawings
Fig. 1 is the X-ray powder diffraction collection of illustrative plates of the prepared stannic disulphide nano slice of embodiment of the invention 1-5.
Fig. 2 is the field emission scanning electron microscope figure of the embodiment of the invention 1 prepared stannic disulphide nano slice.
Fig. 3 is the field emission scanning electron microscope figure of the embodiment of the invention 2 prepared stannic disulphide nano slices.
Fig. 4 is the field emission scanning electron microscope figure of the embodiment of the invention 3 prepared stannic disulphide nano slices.
Fig. 5 is the field emission scanning electron microscope figure of the embodiment of the invention 4 prepared stannic disulphide nano slices.
Fig. 6 is the field emission scanning electron microscope figure of the embodiment of the invention 5 prepared stannic disulphide nano slices.
Fig. 7～9 are the transmission electron microscope picture of the embodiment of the invention 4 prepared stannic disulphide nano slices.
Figure 10 is the SEAD picture of the embodiment of the invention 4 prepared stannic disulphide nano slices.
Figure 11 is the nitrogen adsorption isothermal curve of the prepared stannic disulphide nano slice of embodiment of the invention 1-5.
Figure 12 tests the molecular structure of employed organic dye molecule for this absorption property.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 40mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 110 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, stannic disulfide sample (SA-110).Its X-ray powder diffraction collection of illustrative plates is as shown in Figure 1, and the result shows that embodiment 1 sample belongs to six side's phase stannic disulfides; Figure is as shown in Figure 2 for its field emission scanning electron microscope, shows that it is the tiny nano particle of size, and size is less than 30nm.
Embodiment 2
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 40mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 160 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, stannic disulfide sample (SA-160).Its X-ray powder diffraction spectrum is as shown in Figure 1, and the result shows that embodiment 2 samples belong to six side's phase stannic disulfides; Figure is as shown in Figure 3 for its field emission scanning electron microscope, and particle has formed hexagonal shape, and size is about 30nm.
Embodiment 3
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 40mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 180 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, stannic disulfide sample (SA-180).Its X-ray powder diffraction spectrum is as shown in Figure 1, and the result shows that embodiment 3 samples belong to six side's phase stannic disulfides; Figure is as shown in Figure 4 for its field emission scanning electron microscope, and particle is hexagon, and size is about 40nm.
Embodiment 4
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 40mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 200 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, stannic disulfide sample (SA-200).Its X-ray powder diffraction spectrum is as shown in Figure 1, and the result shows that embodiment 4 samples belong to six side's phase stannic disulfides; Figure is as shown in Figure 5 for its field emission scanning electron microscope, and particle is hexagon, and size is about 50nm; Its transmission electron microscope picture is shown in Fig. 7～9, and particle is hexagon, and size is about 50nm, and nanometer sheet thickness is 5～10nm, and hexagonal surfaces is (001) crystal face; SEAD figure is shown in figure 10, explains that also this nanometer sheet is a monocrystalline, and hexagonal surfaces is (001) crystal face.
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thiocarbamide are added in the 40mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 160 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter yellow powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, stannic disulfide sample (SI-160).Its X-ray powder diffraction spectrum is as shown in Figure 1, and the result shows that embodiment 5 samples belong to six side's phase stannic disulfides; Figure is as shown in Figure 6 for its field emission scanning electron microscope, and the nanometer sheet of formation is a hexagonal shape, and size is about 500nm.
Embodiment 6
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 45mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 200 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, the stannic disulfide sample.
Embodiment 7
Under the room temperature, 0.87g (2.5mmo1) stannic chloride pentahydrate and 0.38g (5mmol) thioacetamide are added in the 36mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 200 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, the stannic disulfide sample.
Embodiment 8
Under the room temperature, 0.87g (2.5mmol) stannic chloride pentahydrate and 0.76g (10mmol) thioacetamide are added in the 36mL deionized water, be stirred to the solution achromaticity and clarification; Then solution is transferred in the 50mL water heating kettle, sealing is positioned over 200 ℃ of constant temperature maintenance 24h in the baking oven; Naturally cool to room temperature, centrifugal, cross and filter brown powder; The gained powder is used deionized water and absolute ethanol washing respectively 3 times, 80 ℃ of oven dry, the stannic disulfide sample.
Shown in Figure 11 is the nitrogen adsorption isothermal curve of embodiment 1～5 prepared stannic disulphide nano slice; Prepared stannic disulphide nano slice all has pore passage structure; Calculate to such an extent that the aperture and the specific area of stannic disulphide nano slice of embodiment 1～5 is respectively: 3.20nm, 151m
2/ g; 7.28nm, 107m
2/ g; 11.0nm, 88m
2/ g; 19.2nm, 56m
2/ g; 3.60nm, 89m
2/ g.
The absorption property test
Adsorption activity experiment concrete operations are following: the rhodamine B dye solution of 0.06mmol/L of getting stannic disulfide sorbing material that above-mentioned each embodiment of 0.050g makes and 100mL respectively is as adsorbate solution; Absorption 4h gets 4mL solution, high speed centrifugation in advance; Get supernatant liquor; Record absorbance with UV 7504/PC type ultraviolet-visible spectrophotometer at dyestuff characteristic absorption wavelength place separately, and calculate the adsorption rate of dyestuff thus, reflect the absorption property of prepared adsorbent with this.More than the equal triplicate of each absorption test, with interior (＜5%), the structural parameters and the absorption result of each sorbing material are as shown in table 1 in the error range that allows for repeated experiments result.
The structural parameters of table 1 stannic disulphide nano slice and absorption property
Can find out that by table 1 embodiment 1 prepared sample has higher adsorption efficiency.
The various dye solutions of sample 0.050g that makes with embodiment 4 and the 0.06mmol/L of 100mL repeat above-mentioned adsorption activity test as adsorbate solution, and the result is as shown in table 2.
Table 2 stannic disulfide single crystal nanoplate (SA-200) is to the absorption property of different organic dyestuff
| Dyestuff | Methyl orange | Orange II | Congo red | Rhodamine B | Methylene blue | Malachite green |
| Adsorption rate (%) | 7 | 5 | 11 | 55 | 99 | 48 |
The structural formula of the listed organic dyestuff of table 2 is shown in figure 12, can find out that by table 2 the prepared sorbing material of the present invention has the selection adsorptivity, and especially the absorption property to the fluorescein(e) dye molecule that contains the nominal price azanyl is very strong.
The foregoing description is interpreted as only being used to the present invention is described and is not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can do various changes or modification to the present invention, and these equivalences change and modify and fall into claim of the present invention institute restricted portion equally.
Claims (5)
1. the preparation method to the stannic disulfide single crystal nanoplate of organic dyestuff selective absorption is characterized in that, may further comprise the steps: under the room temperature; The predecessor of stannic chloride pentahydrate and the sulphur mol ratio according to 1: 2～1: 4 is dissolved in the deionized water, under 110 ℃～200 ℃ hydro-thermals, keeps 20～30h, naturally cool to room temperature then; Centrifugal; Filter washing, drying.
2. the preparation method of the said stannic disulfide single crystal nanoplate to the organic dyestuff selective absorption of claim 1 is characterized in that the mol ratio of stannic chloride pentahydrate and deionized water is 1: 800～1: 1000.
3. the preparation method of claim 1 or 2 said stannic disulfide single crystal nanoplates to the organic dyestuff selective absorption is characterized in that, the predecessor of said sulphur is a kind of in thioacetamide and the thiocarbamide.
4. the said stannic disulfide nanometer monocrystalline piece preparation method to the organic dyestuff selective absorption of claim 3 is characterized in that the predecessor of sulphur is a thioacetamide, and the mol ratio of stannic chloride pentahydrate and thioacetamide is 1: 4, and hydrothermal temperature is 110 ℃.
5. the stannic disulfide single crystal nanoplate to the organic dyestuff selective absorption is characterized in that, and is prepared according to any described method of claim 1～4; Be the hexagonal crystal phase; Grain shape is a hexagon, and it is of a size of 20～50nm, and specific area is at 56～151m
2/ g, the aperture is at 3.2～19.2nm.
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Cited By (9)
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| CN102774878A (en) * | 2012-07-23 | 2012-11-14 | 彩虹集团公司 | Preparation method for tin-based cathode material of high-capacity lithium ion battery |
| CN104888753A (en) * | 2015-05-28 | 2015-09-09 | 陕西科技大学 | Tin disulfide/titanium dioxide compound photocatalyst and preparation method thereof |
| CN106564934A (en) * | 2016-11-02 | 2017-04-19 | 陕西科技大学 | Method for preparing granular assembly spherical SnS<2> sodium ion battery anode material |
| 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 |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
| 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 |
| CN110526281A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of synthesis stannic disulfide |
| CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
| CN113101950A (en) * | 2021-04-13 | 2021-07-13 | 西南科技大学 | Preparation method of surface oxidized tin disulfide nanosheet-coated tellurium nanowire for treating radioactive wastewater |
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| CN102774878A (en) * | 2012-07-23 | 2012-11-14 | 彩虹集团公司 | Preparation method for tin-based cathode material of high-capacity lithium ion battery |
| CN104888753A (en) * | 2015-05-28 | 2015-09-09 | 陕西科技大学 | Tin disulfide/titanium dioxide compound photocatalyst and preparation method thereof |
| CN106564934A (en) * | 2016-11-02 | 2017-04-19 | 陕西科技大学 | Method for preparing granular assembly spherical SnS<2> sodium ion battery anode material |
| CN106564934B (en) * | 2016-11-02 | 2018-03-27 | 陕西科技大学 | A kind of particle assembles spherical SnS2The preparation method of anode material of lithium-ion battery |
| 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 |
| 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 |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
| 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 |
| CN110526281A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of synthesis stannic disulfide |
| CN110526281B (en) * | 2019-08-26 | 2021-08-24 | 浙江工业大学 | Method for synthesizing tin disulfide |
| CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
| CN111871431B (en) * | 2020-08-27 | 2022-09-20 | 东北师范大学 | Tin disulfide/gold composite catalyst, and preparation method and application thereof |
| CN113101950A (en) * | 2021-04-13 | 2021-07-13 | 西南科技大学 | Preparation method of surface oxidized tin disulfide nanosheet-coated tellurium nanowire for treating radioactive wastewater |
| CN113101950B (en) * | 2021-04-13 | 2021-11-26 | 西南科技大学 | Preparation method of surface oxidized tin disulfide nanosheet-coated tellurium nanowire for treating radioactive wastewater |
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Application publication date: 20120704 |