CN102583520A - Method for preparing CaTi2O4(OH)2 nanolayer - Google Patents
Method for preparing CaTi2O4(OH)2 nanolayer Download PDFInfo
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- CN102583520A CN102583520A CN2012100753859A CN201210075385A CN102583520A CN 102583520 A CN102583520 A CN 102583520A CN 2012100753859 A CN2012100753859 A CN 2012100753859A CN 201210075385 A CN201210075385 A CN 201210075385A CN 102583520 A CN102583520 A CN 102583520A
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- cati
- liquid
- cati2o4
- nanolayer
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Abstract
The invention discloses a method for preparing a CaTi2O4(OH)2 nanolayer. A hydrothermal method is adopted, and the method comprises the following steps of: dissolving a titanium compound in an ethanol solvent to obtain a solution A; mixing calcium chloride dihydrate, distilled water and the ethanol solvent to obtain a solution B; and slowly dripping the solution A into the solution B, regulating the pH value to be 8-12, stirring and mixing, putting into a hydrothermal kettle, and keeping the temperature of between 180 and 260DEG C for 1 to 36 hours to obtain the CaTi2O4(OH)2 nanolayer. The pure CaTi2O4(OH)2 nanolayer is prepared from cheap raw materials, namely the calcium chloride dehydrate and butyl titanate by taking water-ethanol as a solvent through one-step hydrothermal method, the process route is simple, and the prepared CaTi2O4(OH)2 nanolayer is high in yield and high in controllability.
Description
Technical field
The present invention relates to prepare CaTi
2O
4(OH)
2The method of nanometer layer.
Background technology
CaTi
2O
4(OH)
2And CaTiO
3All form by calcium, titanium oxide.But at occurring in nature, it is but very big that their distributed quantities differ.Recently, there has been report to prepare CaTiO through hydrothermal method and solid phase method
3Phase.But relevant preparation CaTi
2O
4(OH)
2Report does not almost have.CaTi
2O
4(OH)
2Nanometer layer and CaTiO
3Orthohormbic structure is different, and it is a kind of Kassite laminate structure, is similar to hydrotalcite, is main body laminate and interlayer OH by calcium oxygen octahedra and titanyl octahedral body
-The compound that interaction through non covalent bond assembles.
At present, CaTi
2O
4(OH)
2The preparation of laminate structure and performance study are almost blank.Concerning laminate structure, but because the chemical constitution modulation of its main body laminate; Characteristics such as the grain size of the anionic kind of interlayer object and adjustable number change and intercalation assembly and distribution are adjustable; Be widely used in ion-exchanger, absorption unit, photocatalyst; Industrial circle such as electroactive material and light active material, and Kassite structure [CaTi
2O
4(OH)
2] also belong to layered metal oxide, this means that it also has the industrial circle that is similar to the layered metal oxide hydrotalcite material.According to theoretical basis, CaTi
2O
4(OH)
2In the process that chemical reaction takes place, have electron exchange, thereby CaTi
2O
4(OH)
2Stratiform might have broad application prospects in electrochemical field.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare CaTi with one step hydro thermal method
2O
4(OH)
2The method of nanometer layer.
The present invention prepares CaTi
2O
4(OH)
2The method of nanometer layer, employing be hydrothermal method, step is following:
1) butyl(tetra)titanate is dissolved in the alcohol solvent, butyl(tetra)titanate and alcoholic acid mol ratio are 1:1 ~ 5, are stirred to and evenly obtain A liquid;
2) Calcium dichloride dihydrate is dissolved in the zero(ppm) water, adds ethanol then, be stirred to and evenly obtain B liquid, Calcium dichloride dihydrate: water: the alcoholic acid mol ratio is 1:1 ~ 600:1 ~ 10;
3) stir down, A liquid is dropwise splashed in the B liquid, regulate pH value to 8 ~ 12, be placed in the water heating kettle, be incubated 1 ~ 36h down, use distilled water wash, obtain CaTi at 180 ~ 200 ℃
2O
4(OH)
2Nanometer layer.
Beneficial effect of the present invention is:
The present invention adopts cheap raw material Calcium dichloride dihydrate and butyl(tetra)titanate under the low temperature non-equilibrium condition, prepared CaTi as solvent through one step hydro thermal method with water-ethanol
2O
4(OH)
2Nanometer layer.Operational path of the present invention is simple, can control CaTi easily through regulating processing parameter
2O
4(OH)
2Nanometer layer.
Description of drawings
Fig. 1 is the CaTi of instance 1
2O
4(OH)
2The X ray diffracting spectrum of nanometer layer.
Fig. 2 is CaTi
2O
4(OH)
2The stereoscan photograph of nanometer layer.
Fig. 3 is CaTi
2O
4(OH)
2The transmission electron microscope photo of nanometer layer.
Fig. 4 is CaTi
2O
4(OH)
2The optical property collection of illustrative plates of nanometer layer.
Fig. 5 is CaTi
2O
4(OH)
2The photocatalytic activity of nanometer layer decomposition of methyl orange solution, C/C among the figure
0Be degradation rate, C
0Being respectively light application time with C is 0 the concentration of tropeolin-D when the t.
Embodiment
Embodiment 1
1) butyl(tetra)titanate is dissolved in the ethanol, butyl(tetra)titanate and alcoholic acid mol ratio are 1:5, are stirred to and evenly obtain A liquid;
2) Calcium dichloride dihydrate is dissolved in the zero(ppm) water, and mixes with ethanol to stir and obtain B liquid, Calcium dichloride dihydrate: water: the alcoholic acid mol ratio is 1:400:10;
3) A liquid is dropwise splashed in the B liquid, stir 10min, then drip NaOH solution gradually, regulate pH value to 8, continue to stir and be placed in the water heating kettle after 15min mixes, at 180 ℃ of hydrothermal temperatures insulation 36h down, with distilled water wash 6 times, acquisition CaTi
2O
4(OH)
2Nanometer layer.Its X ray diffracting spectrum is as shown in Figure 1, its diffraction peak and CaTi
2O
4(OH)
2The standard diagram of phase is consistent, explains that products obtained therefrom is CaTi
2O
4(OH)
2Phase.
1) butyl(tetra)titanate is dissolved in the ethanol, butyl(tetra)titanate and alcoholic acid mol ratio are 1:5, are stirred to and evenly obtain A liquid;
2) Calcium dichloride dihydrate is dissolved in the zero(ppm) water, and mixes with ethanol to stir and obtain B liquid, Calcium dichloride dihydrate: water: the alcoholic acid mol ratio is 1:50:5;
3) A liquid is dropwise splashed in the B liquid, stir 5min, then dropping ammonia solution is gradually regulated pH value to 12, continues to stir to be placed in the water heating kettle after 15min mixes, and is incubated 24h down for 200 ℃ at hydrothermal temperature.Obtain CaTi 3 times with distilled water wash
2O
4(OH)
2Its stereoscan photograph and transmission electron microscope photo are seen Fig. 2 and Fig. 3, can be clearly seen that by Fig. 2 and Fig. 3: this sample topography in the form of sheets, and is different with traditional cubes pattern.
Embodiment 3
1) butyl(tetra)titanate is dissolved in the ethanol, butyl(tetra)titanate and alcoholic acid mol ratio are 1:1, are stirred to and evenly obtain A liquid;
2) Calcium dichloride dihydrate is soluble in water, and mix with ethanol to stir and obtain B liquid, two water
Calcium chloride: water: the alcoholic acid mol ratio is 1:400:5;
3) A liquid is dropwise splashed in the B liquid, stir 8min, then drip KOH solution gradually, regulate pH value to 8, continue to stir and be placed in the water heating kettle after 15min mixes, at 200 ℃ of hydrothermal temperatures insulation 18h down, with distilled water wash 6 times, acquisition CaTi
2O
4(OH)
2Phase.It is as shown in Figure 4 that sample has been carried out optical performance test, and test result shows the CaTi that the present invention prepares
2O
4(OH)
2Nanometer layer does not almost absorb at visible region, only at ultraviolet region absorption is arranged, and the ABSORPTION EDGE of this sample is 358nm.According to being with calculation formula E
g=1240/ λ can know that this can be with and be 3.46ev.It is as shown in Figure 5 simultaneously sample have been carried out the photocatalysis performance test.Test result shows the CaTi that the present invention prepares
2O
4(OH)
2Nanometer layer has certain photocatalysis performance.
Embodiment 4
1) butyl(tetra)titanate is dissolved in the ethanol, is stirred to and evenly obtains A liquid, butyl(tetra)titanate and alcoholic acid mol ratio are 1:3;
2) Calcium dichloride dihydrate is soluble in water, and mix with ethanol to stir and obtain B liquid, Calcium dichloride dihydrate: water: the alcoholic acid mol ratio is 1:50:8;
3) A liquid is dropwise splashed in the B liquid, stir 8min, then drip NaOH solution gradually, regulate pH value to 8, continue to stir and be placed in the water heating kettle after 15min mixes, at 200 ℃ of hydrothermal temperatures insulation 18h down, with distilled water wash 6 times, acquisition CaTi
2O
4(OH)
2Phase.
Claims (1)
1. one kind prepares CaTi
2O
4(OH)
2The method of nanometer layer is characterized in that may further comprise the steps:
1) butyl(tetra)titanate is dissolved in the alcohol solvent, butyl(tetra)titanate and alcoholic acid mol ratio are 1:1 ~ 5, are stirred to and evenly obtain A liquid;
2) Calcium dichloride dihydrate is dissolved in the zero(ppm) water, adds ethanol then, be stirred to and evenly obtain B liquid, Calcium dichloride dihydrate: water: the alcoholic acid mol ratio is 1:1 ~ 600:1 ~ 10;
3) stir down, A liquid is dropwise splashed in the B liquid, regulate pH value to 8 ~ 12, be placed in the water heating kettle, be incubated 1 ~ 36h down, use distilled water wash, obtain CaTi at 180 ~ 200 ℃
2O
4(OH)
2Nanometer layer.
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Family
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104528814A (en) * | 2014-12-19 | 2015-04-22 | 浙江大学 | Preparation method and product of CaTi2O4(OH)4 diamond nanosheet with lamellar structure |
CN104888744A (en) * | 2015-05-26 | 2015-09-09 | 景德镇陶瓷学院 | CaFexTi(2-x)O4(OH)2 photocatalyst material and preparation method thereof |
CN104941623A (en) * | 2015-05-26 | 2015-09-30 | 景德镇陶瓷学院 | CaTi2O5/CaTi2O4(OH)2 composite micro-nano structure material and preparation method thereof |
CN106373786A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing CaTi<2-x>M<x>O<4>(OH)<2> (M=Co, Ni, Fe) nanosheet by adopting solvothermal method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5082648A (en) * | 1989-01-26 | 1992-01-21 | Pfizer Inc. | Process for the preparation of high purity calcium titanate hydrates and product produced thereby |
CN102242400A (en) * | 2011-06-29 | 2011-11-16 | 浙江大学 | Method for preparing monocrystalline CaTiO3 dendrite |
-
2012
- 2012-03-21 CN CN2012100753859A patent/CN102583520A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5082648A (en) * | 1989-01-26 | 1992-01-21 | Pfizer Inc. | Process for the preparation of high purity calcium titanate hydrates and product produced thereby |
CN102242400A (en) * | 2011-06-29 | 2011-11-16 | 浙江大学 | Method for preparing monocrystalline CaTiO3 dendrite |
Non-Patent Citations (1)
Title |
---|
YI-JEN HUANG ET AL: "Artificial Synthesis of Platelet-Like Kassite and Its Transformation to CaTiO3", 《CRYSTAL GROWTH AND DESIGN》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104528814A (en) * | 2014-12-19 | 2015-04-22 | 浙江大学 | Preparation method and product of CaTi2O4(OH)4 diamond nanosheet with lamellar structure |
CN104888744A (en) * | 2015-05-26 | 2015-09-09 | 景德镇陶瓷学院 | CaFexTi(2-x)O4(OH)2 photocatalyst material and preparation method thereof |
CN104941623A (en) * | 2015-05-26 | 2015-09-30 | 景德镇陶瓷学院 | CaTi2O5/CaTi2O4(OH)2 composite micro-nano structure material and preparation method thereof |
CN104888744B (en) * | 2015-05-26 | 2017-04-05 | 景德镇陶瓷学院 | A kind of CaFexTi2‑xO4(OH)2Photocatalyst material and preparation method thereof |
CN106373786A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing CaTi<2-x>M<x>O<4>(OH)<2> (M=Co, Ni, Fe) nanosheet by adopting solvothermal method |
CN106373786B (en) * | 2016-09-06 | 2018-09-14 | 景德镇陶瓷大学 | It is a kind of that CaTi is prepared using solvent-thermal method2-xMxO4(OH)2The method of (M=Co, Ni, Fe) nanometer sheet |
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Application publication date: 20120718 |