CN105289659A - SiO2-MoS2 mesoporous composite nano material and preparation method and application thereof - Google Patents
SiO2-MoS2 mesoporous composite nano material and preparation method and application thereof Download PDFInfo
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- CN105289659A CN105289659A CN201510633097.4A CN201510633097A CN105289659A CN 105289659 A CN105289659 A CN 105289659A CN 201510633097 A CN201510633097 A CN 201510633097A CN 105289659 A CN105289659 A CN 105289659A
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Abstract
The invention discloses a SiO2-MoS2 mesoporous composite nano material and a preparation method and application thereof, and relates to the technical field of mesoporous composite nano materials. Flower-like MoS2 nano particles grow on a mesoporous SiO2 base body; the aperture of the mesoporous SiO2 base body is 5 to 8nm; the specific surface area (BET) of the composite nano material is 521m<2>/g. The preparation method comprises the steps of dissolving soluble molybdate into an acetic acid-distilled water system, stirring under room temperature, thus obtaining a colorless solution a, slowly adding ethyl orthosilicate into the solution a, continuously stirring, thus obtaining a yellow solution b, performing thermal treatment on the solution b, thus obtaining a solid-state gel block body c, grinding the gel block body c into fine powder, putting the fine powder into a reaction container with an excessive thiourea aqueous solution for sulfidizing. The SiO2-MoS2 mesoporous composite nano material is higher in dispersion property, good in flowability and adsorbency and excellent in photocatalysis and acid resistance performance, can be applied to the aspects such as mechanical lubrication and photocatalytic pollutant degrading, and has a wider application prospect.
Description
Technical field
The present invention relates to composite mesoporous technical field of nano material, specifically relate to a kind of SiO
2-MoS
2composite mesoporous nano material and its preparation method and application.
Background technology
Mesoporous silicon oxide (SiO
2) because of Stability Analysis of Structures, with low cost and higher specific area, can be used as adsorbent and catalyst, there is important using value at catalysis, medicine and biological field.At present, hydro-thermal method and sol-gel process are current synthesising mesoporous SiO
2main method.The product thermal stability that hydro-thermal method prepares is good, and degree of crystallinity is high, and operation is convenient, but the hydrothermal crystallizing time is longer.And although sol-gel process synthesis temperature is not high, need the aftertreatment technologys such as calcining, and obtained product purity is lower.
Molybdenum bisuphide (MoS
2) as transition-metal sulphides, there are good optical, electrical, the performance such as catalysis and lubrication.Report a lot about MoS both at home and abroad
2preparation method, mainly comprise hydro-thermal method and solid phase reduction method.Hydro-thermal method can control MoS very well
2form and purity etc., decrease the adverse effect brought in the required process of lapping of solid phase reduction method synthesis.TingYang etc., with Na
2moO
42H
2o and NH
2cSNH
2for raw material, simple hydro-thermal method is adopted to prepare MoS
2nanosphere.First reducing process prepares amorphous state MoS
3, then use the reducing agents such as hydrogen, hydrazine and azanol by MoS
3be reduced to MoS
2.
For SiO
2-MoS
2the performance of composite mesoporous nano material with and preparation method thereof, have not yet to see pertinent literature report.
Summary of the invention
In order to overcome the above-mentioned defect existed in prior art, an object of the present invention there are provided a kind of SiO
2-MoS
2composite mesoporous nano material, it has higher specific area and good photocatalysis performance, can realize to the methylene blue in acidic aqueous solution and rhodamine B degradable, and can be used as a kind of lubricant of low cost.
For realizing this object, present invention employs following technical scheme: a kind of SiO
2-MoS
2composite mesoporous nano material, by SiO
2and MoS
2composition, in flower-shaped MoS
2nanoparticle growth is at mesoporous SiO
2on matrix, mesoporous SiO
2the aperture of matrix is 5 ~ 8nm, and the specific area (BET) of composite nano materials is 521m
2/ g.
Another object of the present invention is to provide a kind of SiO
2-MoS
2the preparation method of composite mesoporous nano material, adopt sol-gel process, step is as follows:
Step 1, is dissolved in acetic acid-distilled water system by soluble molybdenum hydrochlorate, stirred at ambient temperature makes it fully to dissolve the solution a obtained in colourless;
Step 2, slowly joins in solution a by ethyl orthosilicate (TEOS), continues to stir the solution b obtained in yellow, and hierarchy of control pH value is 1 ~ 6, and the mol ratio of soluble molybdenum hydrochlorate and ethyl orthosilicate (TEOS) is 0.1 ~ 1: 10;
Step 3, obtains in solid-state gel mass c by solution b through heat treatment;
Step 4, grinds to form fine powder (color of fine powder is in white), then loads and fill in the reaction vessel of excessive thiourea solution, vulcanizing treatment 6 ~ 48 hours at 140 ~ 200 DEG C, obtained SiO by gel mass c
2-MoS
2composite mesoporous nano material.
As SiO of the present invention
2-MoS
2the further improvement of the preparation method of composite mesoporous nano material,
In step 1, the mol ratio of acetic acid and distilled water is 0.1 ~ 0.5: 5 ~ 25, and the volume ratio preparing the distilled water added in the ethyl orthosilicate (TEOS) and step 1 used described in solution b in step 2 is 1: 10.In step 1, in the dissolving of soluble molybdenum hydrochlorate and step 2, ethyl orthosilicate (TEOS) is added and all to be mixed by magnetic stirring apparatus afterwards, and mixing time is 1 ~ 3 minute.Heat treatment in step 3 puts solution b into air dry oven, through 60 ~ 100 DEG C of heat treatments 6 ~ 48 hours.In step 4, the granularity of gel fine powder is 0.5 ~ 10 μm.Step 4 vulcanizing treatment products therefrom is carried out cleaning and drying and processing, obtains grizzly SiO
2-MoS
2composite mesoporous nano material.
The present invention is on the basis of sol-gel and Synthesized by Hydrothermal Method material, first employing sol-gel process prepares the xerogel powdery precursor containing Mo (VI) and Si (IV), finally by hydro-thermal vulcanizing treatment technology, prepare SiO
2-MoS
2composite mesoporous nano material.
The present invention have studied SiO
2-MoS
2the catalytic elimination organic pollution of composite mesoporous nano material and lubrication property, show by a series of research and characterization result the SiO that the present invention obtains
2-MoS
2composite mesoporous nano material has higher specific area and has good photocatalysis performance, at a certain amount of H
2o
2in system, can realize to the methylene blue in acidic aqueous solution and rhodamine B degradable.Therefore, this acid proof SiO
2-MoS
2what composite mesoporous nano material was expected to be used as organic pollution in acid waste water removes material.In addition, in mechanical lubrication and anti-attrition, also there is potential application prospect, can be used as a kind of lubricant of low cost.
Compared with prior art, beneficial effect of the present invention shows:
1, present invention achieves by compound precursor liquid solution PhastGel technology, SiO can be obtained by Fast back-projection algorithm
2-MoS
2composite mesoporous nano material, for the synthesis of low cost catalyst and lubricant provides a kind of new approach.
2, present invention process is simple, and whole preparation system easily builds, easy and simple to handle, condition is easily controlled, with low cost, product composition is easily controlled, product is dispersed and mobility is high, be suitable for large-scale production and application.
3, the present invention adopts conventional soluble molybdate and positive silicic acid ethanol as reactant, and the accessory substance produced in preparation process is few, and environmental pollution is less, is a kind of environment-friendly type preparation technology.
4, the product that prepared by the present invention has good dispersiveness, good mobility and adsorptivity, excellent photocatalysis and acid resistance, and can be applied in the aspect such as mechanical lubrication and photocatalytic pollutant degradation has comparatively wide application prospect.
Accompanying drawing explanation
Fig. 1 is the optical photograph figure of embodiment 1 gained colloidal solution b.
Fig. 2 is the optical photograph figure of embodiment 1 gained gel fine powder.
Fig. 3 is the optical photograph figure of embodiment 1 products therefrom.
Fig. 4 is SEM and the EDS figure of embodiment 1 products therefrom.
Fig. 5 is the N of embodiment 1 products therefrom
2adsorption desorption isothermal curve.
Fig. 6 is photocatalytic degradation RhB kinetic curve and the Linear Fit Chart of embodiment 1 products therefrom.
Fig. 7 is the greasy property comparison diagram of embodiment 1 products therefrom.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.The structure of products therefrom, pattern, composition and performance etc. are characterized, selects instrument or the equipment such as X-ray powder diffraction (XRD), field emission scanning electron microscope (FE-SEM) and ultraviolet-visible spectrophotometer (UV-Vis) respectively.
Preparation embodiment 1: preparation SiO
2-MoS
2composite mesoporous nano material
(1) be dissolved in by soluble molybdenum hydrochlorate in acetic acid-distilled water system, room temperature lower magnetic force stirs and within 2 minutes, makes it fully to dissolve the solution a obtained in colourless, and the mol ratio of acetic acid and distilled water is 0.25: 15.Fig. 1 is the reaction precursor liquid solution optical photograph figure prepared under room temperature, and this solution known is yellow, has Tyndall effect, illustrates that the solution a obtained is colloidal solution.
(2) ethyl orthosilicate (TEOS) is slowly joined in solution a, continue magnetic agitation and within 2 minutes, obtain in yellow solution b.Hierarchy of control pH value is 3, and the mol ratio of soluble molybdenum hydrochlorate and ethyl orthosilicate (TEOS) is 0.5: 10, and the volume ratio of the distilled water that ethyl orthosilicate (TEOS) and upper step add is 1: 10.
(3) solution b is put into air dry oven, through 80 DEG C of heat treatments 15 hours.
(4) first, gel mass c is ground to form fine powder (granularity of fine powder is 0.5 ~ 10 μm).Fig. 2 is the optical photograph figure of xerogel fine powder, and as known in the figure, present white states after yellow colloidal solution becomes xerogel fine powder, xerogel fine powder is irregular particle, and particle diameter is comparatively large, better dispersed.
Then, gel fine powder is loaded and fills in the reaction vessel of excessive thiourea solution, vulcanizing treatment 15 hours at 180 DEG C.
(5) vulcanizing treatment products therefrom is carried out cleaning and drying and processing.Fig. 3 is the target product SiO obtained
2-MoS
2optical photograph figure, as seen from the figure, the color of products therefrom is grey.
Fig. 4 is the target product SiO that embodiment 1 obtains
2-MoS
2sEM and EDS figure, as can be seen from Fig. 4 a, flower-shaped MoS
2nanoparticle growth is at SiO
2on mesoporous substrate, define SiO
2-MoS
2composite mesoporous nano material.Fig. 4 b is its energy spectrogram, can confirm both growth characteristic and composition distribution situation further.
Fig. 5 is SiO
2-MoS
2the N of composite nano materials
2adsorption desorption isothermal curve, as can be seen from Figure, the SiO that embodiment 1 obtains
2-MoS
2for mesoporous material.As can be seen from lower right corner illustration SEM further, flower-shaped MoS
2nano particle is that growth is at mesoporous SiO
2on matrix.Mesoporous SiO
2aperture be about 5 ~ 8nm (see upper left corner illustration).The specific area (BET) of composite is about 521m
2/ g.
Preparation embodiment 2: preparation SiO
2-MoS
2composite mesoporous nano material
(1) be dissolved in by soluble molybdenum hydrochlorate in acetic acid-distilled water system, room temperature lower magnetic force stirs and within 1 minute, makes it fully to dissolve the solution a obtained in colourless, and the mol ratio of acetic acid and distilled water is 0.1: 5.
(2) ethyl orthosilicate (TEOS) is slowly joined in solution a, continue magnetic agitation and within 1 minute, obtain in yellow solution b.Hierarchy of control pH value is 4, and the mol ratio of soluble molybdenum hydrochlorate and ethyl orthosilicate (TEOS) is 0.1: 10, and the volume ratio of the distilled water that ethyl orthosilicate (TEOS) and upper step add is 1: 10.
(3) solution b is put into air dry oven, through 60 DEG C of heat treatments 30 hours.
(4) first gel mass c is ground to form fine powder (granularity of fine powder is 0.5 ~ 10 μm).Then being loaded by gel fine powder fills in the reaction vessel of excessive thiourea solution, vulcanizing treatment 20 hours at 160 DEG C.
(5) vulcanizing treatment products therefrom is carried out cleaning and drying and processing, obtain grizzly SiO
2-MoS
2composite mesoporous nano material.
Preparation embodiment 3: preparation SiO
2-MoS
2composite mesoporous nano material
(1) be dissolved in by soluble molybdenum hydrochlorate in acetic acid-distilled water system, room temperature lower magnetic force stirs and within 3 minutes, makes it fully to dissolve the solution a obtained in colourless, and the mol ratio of acetic acid and distilled water is 0.5: 25.
(2) ethyl orthosilicate (TEOS) is slowly joined in solution a, continue magnetic agitation and within 3 minutes, obtain in yellow solution b.Hierarchy of control pH value is 5.5, and the mol ratio of soluble molybdenum hydrochlorate and ethyl orthosilicate (TEOS) is 1: 10, and the volume ratio of the distilled water that ethyl orthosilicate (TEOS) and upper step add is 1: 10.
(3) solution b is put into air dry oven, through 100 DEG C of heat treatments 6 hours.
(4) first gel mass c is ground to form fine powder (granularity of fine powder is 0.5 ~ 10 μm).Then being loaded by gel fine powder fills in the reaction vessel of excessive thiourea solution, vulcanizing treatment 30 hours at 140 DEG C.
(5) vulcanizing treatment products therefrom is carried out cleaning and drying and processing, obtain grizzly SiO
2-MoS
2composite mesoporous nano material.
Application Example 1: the rhodamine B (RhB) in photocatalytic degradation acid solution
(1) take rhodamine B as target contaminant, in the 100mL rhodamine B initial concentration solution (pH is about 1-6) that is 20mg/L, add the SiO prepared by 0.02g embodiment 1
2-MoS
2with the H of 1mL
2o
2, obtain mixed liquor a after Quick uniform mixing, then, put and carry out photocatalysis experiment under visible light.
(2) t
1after minute, from a solution, take out 10mL proceed in the test tube of 20mL dried and clean, after centrifugation, from test tube, get part not containing the liquid b of catalyst.
(3) absorbance A of the solution b obtained after Magneto separate is tested with ultraviolet-visible spectrometer
1, after being completed, refunding test tube and back in solution a after shaking up together with remaining solution and adsorbent.
(4) t
2minute, t
3minute and t
4minute, t
5minute and t
6sampling after minute is identical with (3) two steps with (2) with test process, and the serial absorbance recorded is labeled as A respectively
2, A
3, A
4, A
5and A
6.
(5) time t is made
iand absorbance A
1(i=0,1,2,3,4,5,6) curve.Adsorption time t and concentration C is calculated again according to absorbance A and concentration C relation (langbobier law)
trelation curve.
Fig. 6 a is SiO
2-MoS
2to rhodamine B Photocatalytic Kinetics curve, with accurate second order order reaction kinetic model
(wherein, C
torganic concentration in solution after catalytic action t, C
0be the initial concentration of reaction solution, K is speed constant.) matching is carried out to experimental data, the coefficient R that matching obtains
2be about 0.991 (see Fig. 6 b).SiO is described
2-MoS
2composite mesoporous nano material has excellent photocatalytic activity.
Application Example 2: lubrication Wear vesistance
(1) by the SiO of certain mass
2-MoS
2composite granule is distributed in machinery oil, is mixed with SiO
2-MoS
2solid content is about the machine oil of 2%.
(2) on MQ-800 type end side friction wear testing machine, the above-mentioned machinery oil prepared is studied to the lubrication of No. 45 steel and Wear vesistance.
(3) carry out surface topography with SEM to polishing scratch to observe and comparative analysis.
(Fig. 7 a) and use the abrasion modality on lubricating oil (Fig. 7 b) both lower No. 45 steel surfaces of situation in order not use lubricating oil for Fig. 7.Can find out, under the effect of identical frictional force, it is little more than what do not make with lubricator to use the degree of wear on No. 45 steel surfaces after lubricating fluid.In sum, SiO
2-MoS
2composite mesoporous nano material has good photocatalysis performance and lubrication Wear vesistance concurrently.
Claims (9)
1. a SiO
2-MoS
2composite mesoporous nano material, by SiO
2and MoS
2composition, is characterized in that: in flower-shaped MoS
2nanoparticle growth is at mesoporous SiO
2on matrix, mesoporous SiO
2the aperture of matrix is 5 ~ 8nm, and the specific area (BET) of composite nano materials is 521m
2/ g.
2. prepare SiO as claimed in claim 1 for one kind
2-MoS
2the method of composite mesoporous nano material, adopts sol-gel process, it is characterized in that step is as follows:
Step 1, is dissolved in acetic acid-distilled water system by soluble molybdenum hydrochlorate, stirred at ambient temperature makes it fully to dissolve the solution a obtained in colourless;
Step 2, slowly joins in solution a by ethyl orthosilicate (TEOS), continues to stir the solution b obtained in yellow, and hierarchy of control pH value is 1 ~ 6, and the mol ratio of soluble molybdenum hydrochlorate and ethyl orthosilicate (TEOS) is 0.1 ~ 1: 10;
Step 3, obtains in solid-state gel mass c by solution b through heat treatment;
Step 4, grinds to form fine powder by gel mass c, then loads and fills in the reaction vessel of excessive thiourea solution, vulcanizing treatment 6 ~ 48 hours at 140 ~ 200 DEG C, obtained SiO
2-MoS
2composite mesoporous nano material.
3. preparation method as claimed in claim 2, it is characterized in that: in step 1, the mol ratio of acetic acid and distilled water is 0.1 ~ 0.5: 5 ~ 25, the volume ratio preparing the distilled water added in the ethyl orthosilicate (TEOS) and step 1 used described in solution b in step 2 is 1: 10.
4. preparation method as claimed in claim 2, is characterized in that: in step 1, in the dissolving of soluble molybdenum hydrochlorate and step 2, ethyl orthosilicate (TEOS) is added and all to be mixed by magnetic stirring apparatus afterwards, and mixing time is 1 ~ 3 minute.
5. preparation method as claimed in claim 2, is characterized in that: the heat treatment in step 3 puts solution b into air dry oven, through 60 ~ 100 DEG C of heat treatments 6 ~ 48 hours.
6. preparation method as claimed in claim 2, is characterized in that: in step 4, the granularity of gel fine powder is 0.5 ~ 10 μm.
7. preparation method as claimed in claim 2, is characterized in that: carried out cleaning and drying and processing by step 4 vulcanizing treatment products therefrom.
8. a SiO as claimed in claim 1
2-MoS
2the application of composite mesoporous nano material in catalyze and degrade organic pollutants.
9. a SiO as claimed in claim 1
2-MoS
2the application in the lubricant of composite mesoporous nano material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149230A (en) * | 2017-12-29 | 2018-06-12 | 西安交通大学 | The preparation method of high temperature low friction nanometer γ-Fe2O3/SiO2 composite coatings in steel matrix |
| CN108219914A (en) * | 2018-01-23 | 2018-06-29 | 宿州市微腾知识产权运营有限公司 | A kind of preparation method of colloidal sol antifriction lubrication oil |
| CN109019616A (en) * | 2018-09-30 | 2018-12-18 | 江南大学 | A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material |
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| US20100172823A1 (en) * | 2005-04-07 | 2010-07-08 | Yeda Research & Development Company Ltd. | Process and apparatus for producing inorganic fullerene-like nanoparticles |
| CN104694208A (en) * | 2015-02-15 | 2015-06-10 | 青岛科技大学 | SiO2/MoS2 core-shell-structure microspheres and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149230A (en) * | 2017-12-29 | 2018-06-12 | 西安交通大学 | The preparation method of high temperature low friction nanometer γ-Fe2O3/SiO2 composite coatings in steel matrix |
| CN108149230B (en) * | 2017-12-29 | 2019-10-25 | 西安交通大学 | High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating |
| CN108219914A (en) * | 2018-01-23 | 2018-06-29 | 宿州市微腾知识产权运营有限公司 | A kind of preparation method of colloidal sol antifriction lubrication oil |
| CN109019616A (en) * | 2018-09-30 | 2018-12-18 | 江南大学 | A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material |
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