CN105645469A - Nano rodlike lanthanum titanate powder and preparation method thereof - Google Patents
Nano rodlike lanthanum titanate powder and preparation method thereof Download PDFInfo
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- CN105645469A CN105645469A CN201610134473.XA CN201610134473A CN105645469A CN 105645469 A CN105645469 A CN 105645469A CN 201610134473 A CN201610134473 A CN 201610134473A CN 105645469 A CN105645469 A CN 105645469A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses nano rodlike lanthanum titanate powder and a preparation method thereof. The technical scheme includes: mixing lanthanum trioxide of 9-33wt%, titanium dioxide of 4-17wt% and chloride powder of 50-87wt% well to obtain a mixture; placing the mixture in a muffle furnace, heating to 600-1000 DEG C at a heating rate of 2-10 DEG C/min, holding the temperature for 1-5 h, and cooling with the furnace to room temperature; using deionized water to wash a product, and drying at 80-100 DEG C for 10-14 h to obtain the nano rodlike lanthanum titanate. The preparation method has the advantages of low reaction temperature, low cost, simple synthesis process, controllability in morphology, high yield and suitability for industrialized production, and the nano rodlike lanthanum titanate powder prepared by the method is small in grain diameter, high in purity, stable in performance and high in photocatalysis activity.
Description
Technical field
The invention belongs to lanthanium titanate powder technology field. It is specifically related to a kind of nano bar-shape lanthanium titanate powder body and preparation method thereof.
Background technology
Since titanium dioxide in 1972 is found to photocatalytic degradation water, the application of Photocatalitic Technique of Semiconductor is paid close attention to widely, the features such as it has that technique is simple, with low cost, non-secondary pollution, nonirritant and safety non-toxic, and can long term beneficial in ecological natural environment, be most one of green environmental protection technique with DEVELOPMENT PROSPECT.
Lanthanium titanate has the laminated perovskite structure along (110) crystal face, when without any additive, can be used for photolysis water hydrogen and degradable organic pollutant through ultraviolet radiation. The broader forbidden band of lanthanium titanate and special layer structure, compared to titanium dioxide, it has more excellent photocatalytic activity, thus has application prospect uniqueness, efficient and wide. At present, the technology of preparing means of lanthanium titanate are mainly solid phase method, hydro-thermal method, sol-gal process and coprecipitation etc. Although these methods are respectively arranged with advantage, but all there is certain deficiency: the shortcoming of solid reaction process is that temperature required height, response time length, diameter of particle be big and skewness etc.; The form of powder body obtained by hydro-thermal method is uncontrollable, crystallization is bad, thus needs further heat treatment, and productivity is low, is unsuitable for producing in enormous quantities; The preparation technology of sol-gal process and coprecipitation is complex, and cost of material is also of a relatively high.
Therefore, the deficiency that the technology of preparing of current powder body exists is: synthesis temperature height, cost height, complex process, powder granularity are relatively slightly, pattern is uncontrollable, cycle length and be not suitable for commercial production etc.
Summary of the invention
It is contemplated that overcome the deficiency that prior art exists, it is therefore an objective to provide that a kind of reaction temperature is low, cost is low, synthesis technique is simple, morphology controllable, productivity are high and are suitable to the nano bar-shape lanthanium titanate raw powder's production technology that industrialization produces; The particle diameter of the nano bar-shape lanthanium titanate powder body prepared by the method is little, purity is high, stable performance and photocatalytic activity high.
For achieving the above object, the technical solution used in the present invention is: by the chloride powder body mix homogeneously of the lanthanum sesquioxide of 9��33wt%, the titanium dioxide of 4��17wt% and 50��87wt%, prepares mixture.Again mixture is inserted Muffle furnace, be warming up to 600��1000 DEG C with the heating rate of 2��10 DEG C/min, be incubated 1��5 hour, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Described lanthanum sesquioxide is technical pure or is analytical pure, particle diameter��10 ��m.
Described titanium dioxide is technical pure or is analytical pure, particle diameter��10 ��m.
Described chloride is that more than one in potassium chloride and lithium chloride, potassium chloride and lithium chloride are technical pure or analytical pure, particle diameter all��100 ��m.
Owing to adopting technique scheme, the present invention compared with prior art has following good effect and outstanding feature:
1, the raw material sources of the present invention are extensive and cheap, and production cost is low, and technological process is simple, thus have very big industrialization prospect of production.
2, the present invention realizes the Homogeneous phase mixing of reactant atomic scale in fused-salt medium so that the diffusion rate between reactant significantly improves, thus can greatly reduce reaction temperature and shorten the response time.
3, the present invention can more easily control the shape and size of powder body by molten-salt growth method, and prepared product purity is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 30��50nm, and axial dimension is 300��500nm. Thus its specific surface area is big, it is remarkably improved the contact probability of nano bar-shape lanthanium titanate powder body and organic dyestuff, is conducive to improving photocatalysis efficiency.
4, the nano bar-shape lanthanium titanate powder body present invention prepared is placed in rhodamine B solution, carries out photocatalysis performance test: degradation rate is 15��35%/hour.
5, the present invention is in course of reaction and cleaning process subsequently, is conducive to the removing of impurity, has prepared high-purity nano bar-shape lanthanium titanate powder body.
Therefore, the present invention has the advantages that reaction temperature is low, cost is low, synthesis technique is simple, morphology controllable, productivity high and is suitable to industrialization production. The particle diameter of prepared nano bar-shape lanthanium titanate powder body is little, purity is high, stable performance and photocatalytic activity high.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of a kind of nano bar-shape lanthanium titanate powder body prepared by the present invention;
Fig. 2 is the SEM figure of the nano bar-shape lanthanium titanate powder body shown in Fig. 1.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention will be further described, not the restriction to its protection domain.
For avoiding repeating, first by as follows for the raw material Unify legislation involved by this detailed description of the invention, embodiment repeats no more:
Described lanthanum sesquioxide is technical pure or is analytical pure, particle diameter��10 ��m.
Described titanium dioxide is technical pure or is analytical pure, particle diameter��10 ��m.
Described potassium chloride and lithium chloride are technical pure or analytical pure, particle diameter all��100 ��m.
Embodiment 1
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 9��15wt%, the titanium dioxide of 4��7wt% and 80��87wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 600��800 DEG C with the heating rate of 4��8 DEG C/min, be incubated 3��5 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 40��60wt% potassium chloride and the mixture of 40��60wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape radial dimension is 50��80nm, and axial dimension is 500��800nm.
The method of testing of the photocatalysis performance of the present embodiment: 1) take the nano bar-shape lanthanium titanate powder body prepared by the rhodamine B solution (concentration is 30mg/L) of 50mL and 50mg the present embodiment respectively and put in test tube; 2) this test tube is placed in photochemical reaction instrument (model XPA-4, Xujiang Electromechanical Plant, Nanjing, China), dark lower magnetic agitation 2h; 3) open xenon lamp (power 500W) illumination 30min, close xenon lamp; 4) rhodamine B solution carry out centrifugal treating after taking the light degradation of 3mL, takes the supernatant and measures its absorption spectrum with ultraviolet-visual spectrometer (model UV2550, Shimadzu (China) company limited); 5) repetitive process 3) and 4) until rhodamine B solution is degradable. Its test result is: light degradation speed is 22��28%/hour.
Embodiment 2
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 13��24wt%, the titanium dioxide of 5��13wt% and 63��82wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 600��800 DEG C with the heating rate of 4��8 DEG C/min, be incubated 3��5 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 40��60wt% potassium chloride and the mixture of 40��60wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 30��50nm, and axial dimension is 300��500nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 30��35%/hour.
Embodiment 3
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 22��33wt%, the titanium dioxide of 11��17wt% and 50��65wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 600��800 DEG C with the heating rate of 4��8 DEG C/min, be incubated 3��5 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 40��60wt% potassium chloride and the mixture of 40��60wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 40��60nm, and axial dimension is 400��600nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 24��31%/hour.
Embodiment 4
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 9��15wt%, the titanium dioxide of 4��7wt% and 80��87wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 700��900 DEG C with the heating rate of 6��10 DEG C/min, be incubated 2��4 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 30��50wt% potassium chloride and the mixture of 50��70wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 40��60nm, and axial dimension is 200��500nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 28��35%/hour.
Embodiment 5
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 13��24wt%, the titanium dioxide of 5��13wt% and 63��82wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 700��900 DEG C with the heating rate of 4��8 DEG C/min, be incubated 1��3 hour, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 50��60wt% potassium chloride and the mixture of 40��50wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 20��40nm, and axial dimension is 200��400nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 26��32%/hour.
Embodiment 6
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 22��33wt%, the titanium dioxide of 11��17wt% and 50��65wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 800��1000 DEG C with the heating rate of 6��10 DEG C/min, be incubated 1��3 hour, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 50��60wt% potassium chloride and the mixture of 40��50wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 35��60nm, and axial dimension is 400��800nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 27��33%/hour.
Embodiment 7
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 9��15wt%, the titanium dioxide of 4��7wt% and 80��87wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 700��900 DEG C with the heating rate of 6��10 DEG C/min, be incubated 2��4 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is 30��50wt% potassium chloride and the mixture of 50��70wt% lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 30��50nm, and axial dimension is 200��500nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 29��35%/hour.
Embodiment 8
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 13��24wt%, the titanium dioxide of 5��13wt% and 63��82wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 800��1000 DEG C with the heating rate of 2��6 DEG C/min, be incubated 3��5 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is potassium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 50��100nm, and axial dimension is 500��800nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 15��21%/hour.
Embodiment 9
A kind of nano bar-shape lanthanium titanate powder body and preparation method thereof. By the chloride powder body mix homogeneously of the lanthanum sesquioxide of 13��24wt%, the titanium dioxide of 5��13wt% and 63��82wt%, prepare mixture. Again mixture is inserted Muffle furnace, be warming up to 800��1000 DEG C with the heating rate of 2��6 DEG C/min, be incubated 3��5 hours, cool to room temperature with the furnace. Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
Chloride in the present embodiment is lithium chloride.
Nano bar-shape lanthanium titanate powder purity prepared by the present embodiment is high, and granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 50��80nm, and axial dimension is 300��600nm.
The photocatalysis performance method of testing of nano bar-shape lanthanium titanate powder body prepared by the present embodiment is with embodiment 1, and its test result is: light degradation speed is 18��24%/hour.
This detailed description of the invention compared with prior art has following good effect and outstanding feature:
1, the raw material sources of this detailed description of the invention are extensive and cheap, and production cost is low, and technological process is simple, thus have very big industrialization prospect of production.
2, this detailed description of the invention realizes the Homogeneous phase mixing of reactant atomic scale in fused-salt medium so that the diffusion rate between reactant significantly improves, thus can greatly reduce reaction temperature and shorten the response time.
3, this detailed description of the invention can more easily control the shape and size of powder body by molten-salt growth method, and as shown in drawings, Fig. 1 is the XRD figure spectrum of a kind of nano bar-shape lanthanium titanate powder body of embodiment 2 preparation to prepared nano bar-shape lanthanium titanate powder body; Fig. 2 is the SEM figure of the nano bar-shape lanthanium titanate powder body shown in Fig. 1. From Fig. 1 and Fig. 2 it can be seen that prepared product purity is high, granule soilless sticking, crystal morphology is nano bar-shape, and radial dimension is 30��50nm, and axial dimension is 300��500nm. Thus its specific surface area is big, it is remarkably improved the contact probability of nano bar-shape lanthanium titanate powder body and organic dyestuff, is conducive to improving photocatalysis efficiency.
4, the nano bar-shape lanthanium titanate powder body this detailed description of the invention prepared is placed in rhodamine B solution, carries out photocatalysis performance test: degradation rate is 15��35%/hour.
5, this detailed description of the invention is in course of reaction and cleaning process subsequently, is conducive to the removing of impurity, has prepared high-purity nano bar-shape lanthanium titanate powder body.
Therefore, this detailed description of the invention has the advantages that reaction temperature is low, cost is low, synthesis technique is simple, morphology controllable, productivity high and is suitable to industrialization production.The particle diameter of prepared nano bar-shape lanthanium titanate powder body is little, purity is high, stable performance and photocatalytic activity high.
Claims (5)
1. a nano bar-shape lanthanium titanate raw powder's production technology, it is characterised in that by the chloride powder body mix homogeneously of the lanthanum sesquioxide of 9��33wt%, the titanium dioxide of 4��17wt% and 50��87wt%, prepares mixture; Again mixture is inserted Muffle furnace, be warming up to 600��1000 DEG C with the heating rate of 2��10 DEG C/min, be incubated 1��5 hour, cool to room temperature with the furnace; Then products therefrom deionized water is cleaned, dry 10��14 hours under 80��100 DEG C of conditions, prepare nano bar-shape lanthanium titanate powder body.
2. according to claim 1 nano bar-shape lanthanium titanate raw powder's production technology, it is characterised in that described lanthanum sesquioxide is technical pure or is analytical pure, particle diameter��10 ��m.
3. according to claim 1 nano bar-shape lanthanium titanate raw powder's production technology, it is characterised in that described titanium dioxide is technical pure or is analytical pure, particle diameter��10 ��m.
4. according to claim 1 nano bar-shape lanthanium titanate raw powder's production technology, it is characterised in that described chloride is that more than one in potassium chloride and lithium chloride, potassium chloride and lithium chloride are technical pure or analytical pure, particle diameter all��100 ��m.
5. a nano bar-shape lanthanium titanate powder body, it is characterised in that described nano bar-shape lanthanium titanate powder body is the nano bar-shape lanthanium titanate powder body prepared by nano bar-shape lanthanium titanate raw powder's production technology according to any one of Claims 1 to 4 item.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106365194A (en) * | 2016-11-10 | 2017-02-01 | 渤海大学 | Preparation method of lanthanum titanate nanometer material |
| CN108246278A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of preparation method of environmental purification function type expanded vermiculite particle |
| CN109336174A (en) * | 2018-12-06 | 2019-02-15 | 洛阳理工学院 | A kind of method that molten-salt growth method prepares bismuth titanates nanometer rods |
| CN109437296A (en) * | 2018-12-06 | 2019-03-08 | 洛阳理工学院 | A kind of method that molten-salt growth method prepares tetragonal phase zirconia nanorod |
| CN109593611A (en) * | 2018-10-26 | 2019-04-09 | 安徽财经大学 | A kind of preparation and application of paintbrush brush detergent and detergent |
| CN109879308A (en) * | 2019-02-25 | 2019-06-14 | 江西师范大学 | A method of preparing lanthanium titanate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365194A (en) * | 2016-11-10 | 2017-02-01 | 渤海大学 | Preparation method of lanthanum titanate nanometer material |
| CN106365194B (en) * | 2016-11-10 | 2018-05-15 | 渤海大学 | A kind of preparation method of lanthanium titanate nano material |
| CN108246278A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of preparation method of environmental purification function type expanded vermiculite particle |
| CN108246278B (en) * | 2018-01-08 | 2020-11-17 | 沈阳理工大学 | Preparation method of environment purification functional expanded vermiculite particles |
| CN109593611A (en) * | 2018-10-26 | 2019-04-09 | 安徽财经大学 | A kind of preparation and application of paintbrush brush detergent and detergent |
| CN109336174A (en) * | 2018-12-06 | 2019-02-15 | 洛阳理工学院 | A kind of method that molten-salt growth method prepares bismuth titanates nanometer rods |
| CN109437296A (en) * | 2018-12-06 | 2019-03-08 | 洛阳理工学院 | A kind of method that molten-salt growth method prepares tetragonal phase zirconia nanorod |
| CN109437296B (en) * | 2018-12-06 | 2021-03-30 | 洛阳理工学院 | Method for preparing tetragonal-phase zirconia nanorod by molten salt growth method |
| CN109336174B (en) * | 2018-12-06 | 2021-04-20 | 洛阳理工学院 | Method for preparing bismuth titanate nano-rod by molten salt method |
| CN109879308A (en) * | 2019-02-25 | 2019-06-14 | 江西师范大学 | A method of preparing lanthanium titanate |
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Application publication date: 20160608 |