CN105289659B - A kind of SiO2‑MoS2Composite mesoporous nano material and its preparation method and application - Google Patents

A kind of SiO2‑MoS2Composite mesoporous nano material and its preparation method and application Download PDF

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CN105289659B
CN105289659B CN201510633097.4A CN201510633097A CN105289659B CN 105289659 B CN105289659 B CN 105289659B CN 201510633097 A CN201510633097 A CN 201510633097A CN 105289659 B CN105289659 B CN 105289659B
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CN105289659A (en
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韩成良
沈寿国
张凌云
姚李
胡坤宏
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Hefei College
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Abstract

A kind of SiO2‑MoS2Composite mesoporous nano material and its preparation method and application, it is related to composite mesoporous technical field of nano material.In flower-shaped MoS2Nanoparticle growth is in mesoporous SiO2On matrix, mesoporous SiO2The aperture of matrix is 5~8nm, and the specific surface area (BET) of composite nano materials is 521m2/g.Soluble molybdenum hydrochlorate is dissolved in acetic acid distillation aqueous systems, stirring obtains being in colourless solution a at room temperature, tetraethyl orthosilicate is slowly added into solution a, continue stirring and obtain the solution b in yellow, by the thermally treated gel mass c obtained in solid-state of solution b, gel mass c is ground into fine powder, is fitted into vulcanizing treatment in the reaction vessel for filling excessive thiourea solution.With preferable dispersed, good mobility and adsorptivity, excellent photocatalysis and acid resistance, can apply has more wide application prospect in mechanical lubrication and photocatalytic pollutant degradation etc..

Description

A kind of SiO2-MoS2Composite mesoporous nano material and its preparation method and application
Technical field
The present invention relates to composite mesoporous technical field of nano material, is specifically related to a kind of SiO2-MoS2Composite mesoporous nanometer Material and its preparation method and application.
Background technology
Mesoporous silicon oxide (SiO2) because of the cheap and higher specific surface area of Stability Analysis of Structures, cost, can be used as adsorbent and Catalyst, there is important application value in catalysis, medicine and biological field.At present, hydro-thermal method and sol-gel process are current Synthesising mesoporous SiO2Main method.The product thermal stability that hydro-thermal method prepares is good, and crystallinity is high, operation facility, but The hydrothermal crystallizing time is longer.Although and sol-gel process synthesis temperature is not high, the aftertreatment technologys such as calcining are needed, and be made Product purity it is relatively low.
Molybdenum disulfide (MoS2) transition-metal sulphides are used as, there are the performances such as good light, electricity, catalysis and lubrication. Both at home and abroad it has been reported that much on MoS2Preparation method, mainly include hydro-thermal method and solid phase reduction method.Hydro-thermal method can be very Control MoS well2Form and purity etc., reduce the adverse effect brought in process of lapping needed for the synthesis of solid phase reduction method. Ting Yang etc., with Na2MoO4·2H2O and NH2CSNH2For raw material, MoS can be prepared using simple hydro-thermal method2Nanometer Ball.Reducing process prepares amorphous state MoS first3, then using reducing agents such as hydrogen, hydrazine and azanols by MoS3It is reduced to MoS2。
For SiO2-MoS2The performance of composite mesoporous nano material with and preparation method thereof, have not yet to see pertinent literature report Road.
The content of the invention
In order to overcome drawbacks described above present in prior art, an object of the present invention is the provision of a kind of SiO2- MoS2Composite mesoporous nano material, it has higher specific surface area and preferable photocatalysis performance, can realized to acidity Methylene blue and rhodamine B in the aqueous solution is degradable, and can be as a kind of inexpensive lubricant.
To realize the purpose, present invention employs following technical scheme：A kind of SiO2-MoS2Composite mesoporous nano material, by SiO2And MoS2Composition, in flower-shaped MoS2Nanoparticle growth is in mesoporous SiO2On matrix, mesoporous SiO2The aperture of matrix is 5~8nm, the specific surface area (BET) of composite nano materials is 521m2/g。
Another object of the present invention is to provide a kind of SiO2-MoS2The preparation method of composite mesoporous nano material, use Colloidal sol-gel method, step are as follows：
Step 1, soluble molybdenum hydrochlorate is dissolved in acetic acid-distillation aqueous systems, stirring at room temperature is allowed to fully dissolve To in colourless solution a；
Step 2, tetraethyl orthosilicate (TEOS) is slowly added into solution a, continues stirring and obtain the solution b in yellow, Control system pH value is 1~6, and the mol ratio of soluble molybdenum hydrochlorate and tetraethyl orthosilicate (TEOS) is 0.1~1: 10；
Step 3, by the thermally treated gel mass c obtained in solid-state of solution b；
Step 4, gel mass c is ground into fine powder (color of fine powder is white), is then charged into and fills excessive thiocarbamide In the reaction vessel of the aqueous solution, vulcanizing treatment 6~48 hours at 140~200 DEG C, SiO is made2-MoS2Composite mesoporous nanometer material Material.
SiO as the present invention2-MoS2The further improvement of the preparation method of composite mesoporous nano material,
The mol ratio of acetic acid and distilled water is 0.1~0.5: 5~25 in step 1, and use described in solution b is prepared in step 2 Tetraethyl orthosilicate (TEOS) and step 1 in the volume ratio of distilled water that adds be 1: 10.Soluble molybdenum hydrochlorate is molten in step 1 Tetraethyl orthosilicate (TEOS) is mixed after adding by magnetic stirring apparatus in solution and step 2, and mixing time is 1~3 point Clock.Heat treatment in step 3 is to put solution b into air dry ovens, is heat-treated 6~48 hours through 60~100 DEG C.Step 4 The granularity of middle gel fine powder is 0.5~10 μm.Step 4 vulcanizing treatment products therefrom is cleaned and drying and processing, is in The SiO of grey2-MoS2Composite mesoporous nano material.
The present invention is prepared using sol-gel process first on the basis of sol-gel and Synthesized by Hydrothermal Method material Go out to contain Mo (VI) and Si (IV) xerogel powdery precursor, finally by hydro-thermal vulcanizing treatment technology, prepared SiO2- MoS2Composite mesoporous nano material.
The present invention have studied SiO2-MoS2The catalytic elimination organic pollution and lubrication property of composite mesoporous nano material, lead to Cross a series of research and characterization result shows the SiO that the present invention is obtained2-MoS2Composite mesoporous nano material has higher Specific surface area and there is preferable photocatalysis performance, in a certain amount of H2O2In system, it can realize to the Asia in acidic aqueous solution Methyl blue and rhodamine B are degradable.Therefore, this acid proof SiO2-MoS2Composite mesoporous nano material is expected to be used as acid The removing material of property Organic Pollutants in Wastewater.In addition, also there is potential application prospect in terms of mechanical lubrication and anti-attrition, can make For a kind of inexpensive lubricant.
Compared with prior art, beneficial effects of the present invention are shown：
1st, the present invention is realized by compound precursor liquid solution PhastGel technology, can Fast back-projection algorithm obtain SiO2-MoS2It is situated between Hole composite nano materials, the synthesis for inexpensive catalyst and lubricant provide a kind of new approach.
2nd, present invention process is simple, and whole preparation system easily builds, be easy to operate, condition is easily-controllable, cost is cheap, product Form that easily-controllable, product is dispersed and mobility is high, is suitable for large-scale production and application.
3rd, the present invention is produced using conventional soluble molybdate and tetraethyl orthosilicate as reactant in preparation process Accessory substance it is few, environmental pollution is smaller, is a kind of environment-friendly type preparation technology.
4th, product prepared by the present invention has preferably dispersed, good mobility and adsorptivity, excellent photocatalysis And acid resistance, it can apply before having more wide application in mechanical lubrication and photocatalytic pollutant degradation etc. Scape.
Brief description of the drawings
Fig. 1 is the gained colloidal solution b of embodiment 1 optical photograph figure.
Fig. 2 is the optical photograph figure of the gained gel fine powder of embodiment 1.
Fig. 3 is the optical photograph figure of the products therefrom of embodiment 1.
Fig. 4 is that the SEM and EDS of the products therefrom of embodiment 1 scheme.
Fig. 5 is the N of the products therefrom of embodiment 12Adsorption desorption isothermal curve.
Fig. 6 is the photocatalytic degradation RhB kinetic curves and Linear Fit Chart of the products therefrom of embodiment 1.
Fig. 7 is the greasy property comparison diagram of the products therefrom of embodiment 1.
Embodiment
The present invention is described in further detail with reference to embodiments.To the structure of products therefrom, pattern, composition and property Can etc. characterized, respectively from X-ray powder diffraction (XRD), field emission scanning electron microscope (FE-SEM) and ultraviolet-can See instrument or the equipment such as light spectrophotometer (UV-Vis).
Prepare embodiment 1：Prepare SiO2-MoS2Composite mesoporous nano material
(1) soluble molybdenum hydrochlorate is dissolved in acetic acid-distillation aqueous systems, magnetic agitation is allowed to abundant in 2 minutes at room temperature Dissolving obtains be in colourless solution a, and the mol ratio of acetic acid and distilled water is 0.25: 15.Fig. 1 is the reaction precursor prepared at room temperature Liquid solution optical photograph figure, it is known that the solution is yellow, has Tyndall effect, and the solution a for illustrating to obtain is colloidal solution.
(2) tetraethyl orthosilicate (TEOS) is slowly added into solution a, continues magnetic agitation and obtain within 2 minutes in yellow Solution b.Control system pH value is 3, and the mol ratio of soluble molybdenum hydrochlorate and tetraethyl orthosilicate (TEOS) is 0.5: 10, positive silicic acid second The volume ratio for the distilled water that ester (TEOS) adds with upper step is 1: 10.
(3) put solution b into air dry ovens, be heat-treated 15 hours through 80 DEG C.
(4) first, gel mass c is ground into fine powder (granularity of fine powder is 0.5~10 μm).Fig. 2 is xerogel fine powder Optical photograph figure, it can be seen that white states, xerogel fine powder is presented after becoming xerogel fine powder in the colloidal solution of yellow For irregular particle, particle diameter is larger, and dispersiveness is preferably.
Then, gel fine powder is fitted into the reaction vessel for filling excessive thiourea solution, the vulcanizing treatment at 180 DEG C 15 hours.
(5) vulcanizing treatment products therefrom is cleaned and drying and processing.Fig. 3 is the target product SiO obtained2-MoS2's Optical photograph figure, as seen from the figure, the color of products therefrom is grey.
Fig. 4 is the target product SiO that embodiment 1 obtains2-MoS2SEM and EDS figure, it is flower-shaped it can be seen from Fig. 4 a MoS2Nanoparticle growth is in SiO2On mesoporous substrate, SiO is formd2-MoS2Composite mesoporous nano material.Fig. 4 b are its power spectrum Figure, both growth characteristics and composition distribution situation can be further confirmed that.
Fig. 5 is SiO2-MoS2The N of composite nano materials2Adsorption desorption isothermal curve, as can be seen from Figure, embodiment 1 are obtained SiO2-MoS2For mesoporous material.By the SEM of lower right corner illustration it can further be seen that flower-shaped MoS2Nano particle is raw Grow in mesoporous SiO2On matrix.Mesoporous SiO2Aperture be about 5~8nm (see upper left corner illustration).The specific surface area of composite (BET) it is about 521m2/g。
Prepare embodiment 2：Prepare SiO2-MoS2Composite mesoporous nano material
(1) soluble molybdenum hydrochlorate is dissolved in acetic acid-distillation aqueous systems, magnetic agitation is allowed to abundant in 1 minute at room temperature Dissolving obtains be in colourless solution a, and the mol ratio of acetic acid and distilled water is 0.1: 5.
(2) tetraethyl orthosilicate (TEOS) is slowly added into solution a, continues magnetic agitation and obtain within 1 minute in yellow Solution b.Control system pH value is 4, and the mol ratio of soluble molybdenum hydrochlorate and tetraethyl orthosilicate (TEOS) is 0.1: 10, positive silicic acid second The volume ratio for the distilled water that ester (TEOS) adds with upper step is 1: 10.
(3) put solution b into air dry ovens, be heat-treated 30 hours through 60 DEG C.
(4) gel mass c is ground into fine powder first (granularity of fine powder is 0.5~10 μm).Then gel fine powder is filled Enter in the reaction vessel for filling excessive thiourea solution, vulcanizing treatment 20 hours at 160 DEG C.
(5) vulcanizing treatment products therefrom is cleaned and drying and processing, obtains the SiO of gray2-MoS2It is composite mesoporous Nano material.
Prepare embodiment 3：Prepare SiO2-MoS2Composite mesoporous nano material
(1) soluble molybdenum hydrochlorate is dissolved in acetic acid-distillation aqueous systems, magnetic agitation is allowed to abundant in 3 minutes at room temperature Dissolving obtains be in colourless solution a, and the mol ratio of acetic acid and distilled water is 0.5: 25.
(2) tetraethyl orthosilicate (TEOS) is slowly added into solution a, continues magnetic agitation and obtain within 3 minutes in yellow Solution b.Control system pH value is 5.5, and the mol ratio of soluble molybdenum hydrochlorate and tetraethyl orthosilicate (TEOS) is 1: 10, positive silicic acid second The volume ratio for the distilled water that ester (TEOS) adds with upper step is 1: 10.
(3) put solution b into air dry ovens, be heat-treated 6 hours through 100 DEG C.
(4) gel mass c is ground into fine powder first (granularity of fine powder is 0.5~10 μm).Then gel fine powder is filled Enter in the reaction vessel for filling excessive thiourea solution, vulcanizing treatment 30 hours at 140 DEG C.
(5) vulcanizing treatment products therefrom is cleaned and drying and processing, obtains the SiO of gray2-MoS2It is composite mesoporous Nano material.
Application Example 1：Rhodamine B (RhB) in photocatalytic degradation acid solution
(1) using rhodamine B as target contaminant, in the solution that 100mL rhodamine Bs initial concentration is 20mg/L, (pH is about The SiO prepared by 0.02g embodiments 1 is added in 1-6)2-MoS2With 1mL H2O2, mixed liquor a is obtained after Quick uniform mixing, Then, progress photocatalysis experiment under visible light is put.
(2)t1After minute, taking-up 10mL is transferred in the test tube of 20mL dried and cleans from a solution, after being centrifuged, from Part is taken to be free of the liquid b of catalyst in test tube.
(3) the solution b obtained with ultraviolet-visible spectrometer test after Magneto separate absorbance A1, after being completed, fall Return test tube and backed after being shaken up together with remaining solution and adsorbent in solution a.
(4)t2Minute, t3Minute and t4Minute, t5Minute and t6Sampling and test process and (2) and (3) two steps after minute Identical, the serial absorbance measured is respectively labeled as A2、A3、A4、A5And A6。
(5) time t is madeiAnd absorbance A1(i=0,1,2,3,4,5,6) curve.Again according to absorbance A and concentration C relation Adsorption time t and concentration C is calculated in (langbobier law)tRelation curve.
Fig. 6 a are SiO2-MoS2To rhodamine B Photocatalytic Kinetics curve, with quasi- second order order reaction kinetic model(wherein, CtIt is organic concentration, C in solution after catalytic action t0It is the initial concentration of reaction solution, K is speed constant.) experimental data is fitted, it is fitted obtained coefficient R2About 0.991 (see Fig. 6 b).Explanation SiO2-MoS2Composite mesoporous nano material has excellent photocatalytic activity.
Application Example 2：Lubricate Wear vesistance
(1) by the SiO of certain mass2-MoS2Composite granule is distributed in machinery oil, is configured to SiO2-MoS2Solid content is about For 2% machine oil
(2) lubrication of the above-mentioned machinery oil prepared to No. 45 steel is studied on MQ-800 type end side friction wear testing machines And Wear vesistance.
(3) surface topography is carried out to polishing scratch with SEM to be observed and comparative analysis.
Fig. 7 is without using lubricating oil (Fig. 7 a) and the abrasion shape using No. 45 steel surfaces in the case of both lubricating oil (Fig. 7 b) State.As can be seen that in the presence of identical frictional force, using the degree of wear of No. 45 steel surfaces after lubricating fluid than without using profit Lubrication prescription it is small more.In summary, SiO2-MoS2Composite mesoporous nano material has good photocatalysis performance and lubrication anti-attrition concurrently Performance.

Claims (3)

  1. A kind of 1. SiO2-MoS2Composite mesoporous nano material, by SiO2And MoS2Composition, it is characterised in that：In flower-shaped MoS2Receive Rice grain is grown in mesoporous SiO2On matrix, mesoporous SiO2The aperture of matrix is 5~8nm, the specific surface area of composite nano materials (BET) it is 521m2/g；
    Preparation method uses sol-gel process, and step is as follows：
    Step 1, soluble molybdenum hydrochlorate is dissolved in acetic acid-distillation aqueous systems, passes through magnetic stirrer 1~3 at room temperature Minute is allowed to fully dissolving and obtains be in colourless solution a, and the mol ratio of acetic acid and distilled water is 0.1~0.5: 5~25；
    Step 2, tetraethyl orthosilicate (TEOS) is slowly added into solution a, the volume of tetraethyl orthosilicate (TEOS) and distilled water Than for 1: 10, mixing being carried out by magnetic stirring apparatus and obtains within 1~3 minute solution b in yellow, control system pH value is 1~6, The mol ratio of soluble molybdenum hydrochlorate and tetraethyl orthosilicate (TEOS) is 0.1~1: 10；
    Step 3, put solution b into air dry ovens, the gel in solid-state is obtained within 6~48 hours through 60~100 DEG C of heat treatments Block c；
    Step 4, gel mass c is ground into the fine powder that granularity is 0.5~10 μm, is then charged into and fills excessive thiourea solution Reaction vessel in, vulcanizing treatment 6~48 hours at 140~200 DEG C, vulcanizing treatment products therefrom cleaned and drying at Reason, SiO is made2-MoS2Composite mesoporous nano material.
  2. A kind of 2. SiO as claimed in claim 12-MoS2Composite mesoporous nano material answering in catalytic degradation organic pollution With.
  3. A kind of 3. SiO as claimed in claim 12-MoS2The application of composite mesoporous nano material in the lubricant.
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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
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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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