CN103318954B - Method for preparing sodium trititanate nanorods through solid-phase chemical reaction - Google Patents
Method for preparing sodium trititanate nanorods through solid-phase chemical reaction Download PDFInfo
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- CN103318954B CN103318954B CN201310292883.3A CN201310292883A CN103318954B CN 103318954 B CN103318954 B CN 103318954B CN 201310292883 A CN201310292883 A CN 201310292883A CN 103318954 B CN103318954 B CN 103318954B
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Abstract
The invention aims to provide a preparation method of sodium trititanate nanorods. The method is characterized in that the sodium trititanate nanorods are synthesized through a solid-phase chemical reaction of cheap raw materials by adopting a simple operation process. The method concretely comprises the following steps: grinding titanium oxysulfate and sodium hydroxide or a sodium salt as reactants at room temperature to synthesize a precursor, carrying out heat treatment, and washing and drying the obtained product to obtain the sodium trititanate nanorods. The sodium trititanate nanorods are prepared only through adopting the cheap raw materials, simply grinding, carrying out proper heat treatment, washing and drying on the basis of the solid-phase chemical reaction. The sodium trititanate nanorods have the characteristics of simple preparation method, high yield, environmental protection, easy realization of the large batch production, and the like, so the method has an extremely wide application prospect.
Description
Technical field
The present invention relates to a kind of method being prepared sodium trititanate nanometer rod by solid state reaction.
Background technology
Sodium trititanate belongs to oblique system.In sodium trititanate, (Ti
3o
7)
2-layer is by alkalimetal ion Na
+combine, for laminate structure, this laminate structure makes it have very strong cationic exchange and absorption property, especially the exchange of heavy metal ion and absorption, show the performance of its uniqueness, at present for for the separation of trace heavy metal ion and enrichment.The crystalline structure of sodium trititanate is tunnel-like structures, and sodium ion is covered by the middle of tunnel, has high chemical stability.
Sodium trititanate has special structures and characteristics, and at microelectronics, electroluminescent, battery terminal, absorption, ion-exchange, matrix material, coating and pigment, and catalytic field has extensive use.Sodium trititanate can be used for the oxygen electrode etc. of the travelling belt of the dielectric resonator of ion-exchange, ceramic condenser, microwave oscillator etc., plastics toughener, insulating material, potentiometer transducer.Sodium trititanate is n-type semiconductor, shows fabulous photocatalytic activity.Sodium trititanate is often used as the inductor of titania-based material, to improve ion exchange reaction speed or to dope the material of the unique properties after transition metal wherein.Synthesized higher than sedimentation by the chemical stability of the sodium trititanate of Melting Synthesis and thermostability, and more convenient for nuclear technology field, directly can use the process in nuke rubbish field.Some documents have relevant report: Journal of Materials Chemistry A. 1 (2013) .2653-2662 reports water heat transfer sodium trititanate as sodium ion battery electrode material; Materials Research Bulletin. 47 (2012) .3770-3773 reports research of synthesis sodium trititanate and optical property thereof etc.
At present, the main method of synthesis sodium titanate nano material has at present: VLS growth mechanism and vapor-solid process; Water (solvent) hot method; Solution-liquid-solid growth method; Template synthesis method; Self-assembly method, hydrothermal method etc.These method building-up processes are complicated, and cost is high, material poor heat stability.Therefore, select a kind of simple preparation method, prepare sodium trititanate tool and be of great significance.Solid-state chemical reaction method method does not use solvent, has highly selective, high yield, simple technological process and other advantages, has become a kind of important method of nano materials.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of sodium trititanate nanometer rod, the method, by using cheap raw material, adopts simple operation method, can synthesize sodium trititanate nanometer rod through solid state reaction.
Technical scheme of the present invention is as follows:
Solid state reaction prepares a method for sodium titanate nanometer rod, and it comprises the following steps: the ratio of titanyl sulfate and sodium hydroxide or sodium salt is 1:1.2 ~ 5; The time of griding reaction is 20 ~ 60 minutes; Presoma in air atmosphere with per minute 5 ~ 10 DEG C of min
-1speed rises to 900 ~ 1000 DEG C, heat-treats 2 hours; Drying at room temperature after product distilled water wash, obtains sodium trititanate nanometer rod.
Sodium salt of the present invention is one or more in sodium oxalate, sodium carbonate, sodium bicarbonate.
Compared with prior art, the present invention has the following advantages: based on solid state reaction, adopts raw material cheap and easy to get, by simple grinding, then passes through suitable thermal treatment, can obtain sodium trititanate nanometer rod after washing drying.Preparation method is simple, and product yield is high, environmental friendliness, is easy to realize the features such as production in enormous quantities and all makes the present invention have very wide application prospect.
Accompanying drawing explanation
Fig. 1 is the powder diagram of prepared sodium trititanate nanometer rod.
Fig. 2 is the projection Electronic Speculum figure of prepared sodium trititanate nanometer rod.
Fig. 3 is the scanning electron microscope (SEM) photograph of prepared sodium trititanate nanometer rod.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiments are interpreted as only being not used in for illustration of the present invention limiting the scope of the invention.After having read the content that the present invention records, the various change made the present invention based on principle of the present invention or amendment have fallen into claims of the present invention limited range equally.
Embodiment one:
Precise 0.01 mol titanyl sulfate and 0.015 mol sodium hydroxide are in different mortar, porphyrize mixing respectively, grinding fast after mixing, along with the carrying out of grinding, mixture becomes the powder of the thin shape of white, continues grinding 30 min and guarantees fully carrying out of reaction.Presoma is placed in retort furnace, rises to 900 DEG C with the temperature rise rate of 5 DEG C/min, at this temperature calcination 2h, drying at room temperature after product distilled water wash, can obtain sodium trititanate nanometer rod.
Embodiment two:
Precise 0.01 mol titanyl sulfate and 0.02 mol sodium oxalate are in different mortar, porphyrize mixing respectively, grinding fast after mixing, along with the carrying out of grinding, mixture becomes the powder of the thin shape of white, continues grinding 30 min and guarantees fully carrying out of reaction.Presoma is placed in retort furnace, rises to 900 DEG C with the temperature rise rate of 8 DEG C/min, at this temperature calcination 2h, drying at room temperature after product distilled water wash, can obtain sodium trititanate nanometer rod.
Embodiment three:
Precise 0.01 mol titanyl sulfate and 0.03 mol sodium carbonate are in different mortar, porphyrize mixing respectively, grinding fast after mixing, along with the carrying out of grinding, mixture becomes the powder of the thin shape of white, continues grinding 30 min and guarantees fully carrying out of reaction.Presoma is placed in retort furnace, rises to 1000 DEG C with the temperature rise rate of 10 DEG C/min, at this temperature calcination 2h, drying at room temperature after product distilled water wash, can obtain sodium trititanate nanometer rod.
Claims (2)
1. solid state reaction prepares a method for sodium trititanate nanometer rod, and it comprises the following steps: mixed with sodium hydroxide or sodium salt by titanyl sulfate, carries out griding reaction and obtains presoma, and presoma after heat treatment obtains final sodium trititanate nanometer rod; The mol ratio of titanyl sulfate and sodium hydroxide or sodium salt is 1:1.2 ~ 5; The time of griding reaction is 20 ~ 60 minutes; Presoma in air atmosphere with per minute 5 ~ 10 DEG C of min
-1speed rises to 900 ~ 1000 DEG C, heat-treats 2 hours.
2. prepare the method for sodium trititanate nanometer rod according to a kind of solid state reaction described in claim 1, it is characterized in that: the sodium salt used is sodium oxalate, sodium carbonate, sodium bicarbonate one or more.
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CN104058449B (en) * | 2014-06-03 | 2016-06-01 | 北京理工大学 | The preparation method of a kind of hollow structure sodium titanate negative material |
CN106315668B (en) * | 2016-08-26 | 2017-10-20 | 浙江工业大学 | A kind of sodium titanate raw powder's production technology |
CN112357955B (en) * | 2020-10-16 | 2022-07-26 | 安徽景成新材料有限公司 | Method for preparing titanium dioxide powder with different morphologies by solid phase method |
CN113789570B (en) * | 2021-09-17 | 2022-06-14 | 南通奥新电子科技有限公司 | Ball-milling heating equipment of sodium titanate whisker |
CN115472800A (en) * | 2022-10-08 | 2022-12-13 | 青岛大学 | Potassium-doped sodium titanate electrode material and preparation method and application thereof |
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CN101117729A (en) * | 2006-08-04 | 2008-02-06 | 上海秀普复合材料有限公司 | Method for treating water solution heavy metallic ion by using trititanic acid sodium whisker |
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CN101117729A (en) * | 2006-08-04 | 2008-02-06 | 上海秀普复合材料有限公司 | Method for treating water solution heavy metallic ion by using trititanic acid sodium whisker |
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