CN103521163A - Method for preparing nanometer composite with chrysanthemum structure - Google Patents
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Abstract
The invention relates to a nanometer composite, and particularly relates to a method for preparing a nanometer composite with a chrysanthemum structure. The method comprises the steps of adding titanium dioxide nanosheets into deionized water, carrying out ultrasonic dispersion, and obtaining a titanium dioxide dispersing liquid; under the condition of magnetic stirring, adding sodium molybdate and thioacetamide into the titanium dioxide dispersing liquid, and obtaining a mixed solution A; after finishing adding, stirring the mixed solution continuously, then transferring the mixed solution into a Teflon inner container, sealing the inner container in a stainless steel hydrothermal reaction kettle for hydrothermal reaction, after finishing the hydrothermal reaction, naturally cooling the reaction kettle to room temperature, centrifuging the obtained product, washing, vacuum drying and obtaining the composite. The method has the advantages that the source of raw materials is wide, and the method is simple and practicable and has low cost. The prepared titanium dioxide or molybdenum disulfide nanometer composite not only has good capacity in absorbing organic contaminants, but also has a good visible light photocatalytic degradation effect to organic contaminants.
Description
Technical field
The present invention relates to nano composite material, refer in particular to a kind of preparation method of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, refer to that in particular a kind of hydro-thermal legal system of using, for the method for adsorption-photocatalytic degradation type chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, belongs to composite, photocatalysis technology and water pollution control field.
Background technology
Environmental problem is day by day serious, and the enforcement that water resource pollution has had a strong impact on quality of life ，Dui China strategy of sustainable development of people has also caused larger impact; In recent years, utilizing photocatalysis technology elimination and degradation of contaminant is one of most active research field in current water environment treatment; Increasing catalysis material is applied to the fields such as environmental protection, water treatment, organic matter degradation, disinfecting, antimicrobial, makes visible-light photocatalysis material obtain increasing concern.
Titanium dioxide has obtained widely and has paid close attention to as conductor photocatalysis material, but, titanium dioxide light abstraction width narrower (only limiting to ultraviolet region), quantum efficiency are lower, particularly low its photocatalytic activity under radiation of visible light that causes of its visible light-responded degree is limited, thereby has limited the practical application of titanium dioxide; In order to improve the photocatalysis performance of titanium dioxide and to expand its range of application, titanium dioxide and other semi-conducting material can be carried out compound, thereby overcome the deficiency of single use titanium dioxide.
Molybdenum bisuphide is a kind of typical lamellar compound, has excellent catalytic performance, is commonly used for the active material of Hydrobon catalyst; Nanoscale molybdenum bisuphide there is the photocatalysis performance more more excellent than micro-meter scale molybdenum bisuphide, thereby chemical synthesis nano molybdenum disulfide is subject to researcher's attention; The research of nano molybdenum disulfide is found to, when the size of molybdenum bisuphide is reduced to enough hour, at visible region, have strong absorption, thereby show excellent photocatalysis performance; Researcher is by molybdenum bisuphide and the compound molybdenum bisuphide/titanium dioxide heterogeneous structure that obtains of titanium dioxide, and this heterojunction structure has the ability of good absorption organic dyestuff, and this depends primarily on sheet and the layer structure of molybdenum bisuphide; Meanwhile, thus because the coupling of being with between molybdenum sulfide and titanium dioxide has suppressed the compound efficiency that improves photocatalysis to degrade organic matter in light induced electron hole; In addition, molybdenum disulfide nano cluster also can be used to sensitization titanium dioxide, thereby makes titanium dioxide show excellent visible light catalytic performance; At present, take plate-like titanium dioxide, sodium molybdate and thioacetamide as raw material, by hydro-thermal method, prepare chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, and be applied to photocatalysis degradation organic contaminant and have no report.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, preparation method and application thereof of preparing simple adsorption-photocatalytic degradation type titanium dioxide/molybdenum disulfide nano composite, overcome the defect that existing capability material cost is high, photocatalysis effect is poor, for technical foundation is established in development and application low-cost, high performance surrounding purifying material.
Realizing the technical solution adopted in the present invention is: a kind of chrysanthemum structure nanometer composite material, by hydro-thermal method, make, and it is characterized in that, preparation process is as follows:
(1) titanium dioxide nanoplate is added in deionized water, ultrasonic dispersion, obtains titanium oxide dispersion, and wherein the concentration of titanium dioxide is 0.08-0.5 g/L;
(2) under stirring condition, sodium molybdate and thioacetamide are added in the prepared titanium oxide dispersion of step (1), obtain mixed solution A, in mixed solution A, the concentration of sodium molybdate is 1.5 g/L, the concentration of thioacetamide is 3 g/L;
(3) after mixed solution A being continued to be stirred to evenly, transfer in polytetrafluoroethylliner liner, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 160-200 ° of C condition, react 20-30 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Described titanium dioxide nanoplate preparation process is as follows:
(1) hydrofluoric acid is added in deionized water, obtain hydrofluoric acid solution, in solution, the mass ratio of hydrofluoric acid is 50%;
(2) under magnetic agitation condition, butyl titanate is dropwise slowly added in the prepared hydrofluoric acid solution of step (1), in reaction system, there is white opacity, the volume ratio of butyl titanate and hydrofluoric acid solution is 5:8;
(3) dropwise after rear mixed solution continues to stir and transfer in polytetrafluoroethylliner liner, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 180 ° of C conditions, react 24 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
The present invention has the following advantages compared with prior art:
A), by the controlled chrysanthemum shape titanium dioxide/molybdenum bisuphide heterojunction structure of preparation structure, can obtain and there is nano composite material strong to Adsorption of Organic ability and that Photocatalytic activity strengthens;
B) preparation is simple for prepared chrysanthemum shape structure nanometer composite material, few to energy resource consumption, green economy;
C) nano composite material all can effectively be removed environmental contaminants under different condition, has round-the-clock adaptive functions;
D) titanium dioxide nanoplate has better visible absorption effect than titanium dioxide granule, for composite, can improve the response of composite to visible ray, thereby the visible light photocatalysis effect of composite is improved.
Accompanying drawing explanation
Fig. 1 is the surface sweeping Electronic Speculum figure of prepared titanium dioxide nanoplate material, visible a large amount of thin plate-like titanium dioxide materials in figure; The size of resulting titanium dioxide nanoplate is between 50-70 nm;
In Fig. 2, the high-resolution-ration transmission electric-lens figure of titanium dioxide nanoplate material shows, the thickness of resulting titanium dioxide nanoplate is between 4-5 nm;
Fig. 3 is the scanning electron microscope diagram of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite;
Fig. 4 is the transmission electron microscope figure of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite;
Fig. 5 is the high resolution transmission electron microscopy figure of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite;
Fig. 6 is the X-ray diffractogram of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite;
Fig. 7 is the adsorption-photocatalytic degradation curve map of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite to rhodamine B.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate content of the present invention, but these embodiment do not limit the scope of the invention.
Embodiment 1
15 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 200 ° of C conditions, react 20 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
10 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 200 ° of C conditions, react 20 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 3
15 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion.Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A.Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 180 ° of C conditions, react 24 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 4
20 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 180 ° of C conditions, react 24 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 5
25 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 160 ° of C conditions, react 30h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 6
30 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 160 ° of C conditions, react 30h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 7
15 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; Under magnetic agitation condition, 90 mg sodium molybdates and 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A; Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 200 ° of C conditions, react 20 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Embodiment 8
15 mg titanium dioxide nanoplates are added in 60 ml deionized waters, and ultrasonic dispersion, obtains titanium oxide dispersion; 90 mg sodium molybdates and the mixing of 180 mg thioacetamides are added in above-mentioned titanium oxide dispersion, obtain mixed solution A.Dropwising rear mixed solution continuation stirring transferred in polytetrafluoroethylliner liner after 30 minutes, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 200 ° of C conditions, react 20 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
Fig. 3 is the scanning electron microscope (SEM) photograph of prepared chrysanthemum shape titanium dioxide/molybdenum disulfide nano composite, from figure, we can see the molybdenum sulfide structure of a large amount of chrysanthemum shapes, and a small amount of titania nanoparticles is deposited on chrysanthemum shape body structure surface or is wrapped up by chrysanthemum shape molybdenum bisuphide; Fig. 4 is the transmission electron microscope figure of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, from figure, can clearly see titanium dioxide/molybdenum disulfide nano composite construction, and titanium dioxide granule is wrapped up by molybdenum bisuphide petal; Fig. 5 is the high-resolution-ration transmission electric-lens figure of prepared chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, further confirmed that in titanium dioxide/molybdenum disulfide nano composite, both are effectively compound, the clear crystal structure of seeing titanium dioxide and molybdenum bisuphide bi-material of energy in figure; Fig. 6 is the X-ray diffractogram of chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite, and in diffraction pattern, all diffraction maximum is well corresponding to the phase of titanium dioxide and molybdenum bisuphide.
In addition, the prepared chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano nano composite material of the present invention is used to absorption and the Photocatalytic Activity for Degradation experiment of organic dyestuff rhodamine B simultaneously, and detailed process and step are as follows:
After the prepared chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano compound material ultrasound of 20 mg being scattered in the rhodamine B solution of 100 milliliter of 10 mg/L ultrasonic 10 minutes, the dispersion liquid mixing is transferred in the quartzy bottle in xenon lamp catalytic reactor, after stirring makes it reach adsorption equilibrium under dark condition, open xenon source, every 10 minutes, with syringe, extracting the postradiation mixed dispersion liquid of 4 mL transfers in the centrifuge tube of mark, after irradiating half an hour, close light source, by the sample centrifugation in all centrifuge tubes, centrifugal rear resulting supernatant liquor is further transferred to and in quartz colorimetric utensil, on ultraviolet-visible spectrophotometer, is measured the absorbance under the different photocatalysis time, thereby obtain titanium dioxide/molybdenum disulfide nano composite photocatalyst material adsorption-photocatalytic degradation curve map to rhodamine B under the radiation of visible light of 400-800 nm under each time period.
Fig. 7 is prepared chrysanthemum flower-like structure titanium dioxide/molybdenum disulfide nano composite adsorption-photocatalytic degradation curve map to rhodamine B, as can be seen from the figure, this nano composite material surpasses 80% to the adsorption rate of rhodamine B under dark condition, radiation of visible light after 60 minutes rhodamine B degraded completely, photocatalytic degradation curve map shows that this chrysanthemum shape titanium dioxide/molybdenum disulfide nano composite has efficient absorption-Photocatalytic Activity for Degradation effect to organic dyestuff rhodamine B.
Claims (4)
1. a preparation method for chrysanthemum structure nanometer composite material, is characterized in that preparation process is as follows:
(1) titanium dioxide nanoplate is added in deionized water, ultrasonic dispersion, obtains titanium oxide dispersion, and wherein the concentration of titanium dioxide is 0.08-0.5 g/L;
(2) under stirring condition, sodium molybdate and thioacetamide are added in the prepared titanium oxide dispersion of step (1), obtain mixed solution A, in mixed solution A, the concentration of sodium molybdate is 1.5 g/L, the concentration of thioacetamide is 3 g/L;
(3) after mixed solution A being continued to be stirred to evenly, transfer in polytetrafluoroethylliner liner, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 160-200 ° of C condition, react 20-30 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
2. the preparation method of a kind of chrysanthemum structure nanometer composite material as claimed in claim 1, is characterized in that described titanium dioxide nanoplate preparation process is as follows:
(1) hydrofluoric acid is added in deionized water, obtain hydrofluoric acid solution, in solution, the mass ratio of hydrofluoric acid is 50%;
(2) under magnetic agitation condition, butyl titanate is dropwise slowly added in the prepared hydrofluoric acid solution of step (1), in reaction system, there is white opacity, the volume ratio of butyl titanate and hydrofluoric acid solution is 5:8;
(3) dropwise after rear mixed solution continues to stir and transfer in polytetrafluoroethylliner liner, and inner bag is sealed in stainless steel hydrothermal reaction kettle, under 180 ° of C conditions, react 24 h, reaction finishes rear reactor and naturally cools to room temperature, washs respectively final vacuum dry after resulting product centrifugation with deionized water and absolute ethyl alcohol.
3. the preparation method of a kind of chrysanthemum structure nanometer composite material as claimed in claim 2, is characterized in that: the size of described titanium dioxide nanoplate is between 50-70 nm; Thickness is between 4-5 nm.
4. the preparation method of a kind of chrysanthemum structure nanometer composite material as claimed in claim 1, it is characterized in that: described chrysanthemum structure nanometer composite material is for the rhodamine B solution of 10 mg/L, under dark condition, the adsorption rate of rhodamine B is surpassed to 80%, under the radiation of visible light of 400-800 nm, after 60 minutes, rhodamine B degraded is complete.
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| CN104140124A (en) * | 2014-07-31 | 2014-11-12 | 中国科学技术大学 | Preparation method of TiO2 nanowire and preparation method of TiO2/MoS2 compound |
| CN104174414A (en) * | 2014-07-28 | 2014-12-03 | 合肥学院 | Molybdenum disulfide/titanium dioxide compound and preparation method thereof |
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