CN102583520A - Method for preparing CaTi2O4(OH)2 nanolayer - Google Patents

Method for preparing CaTi2O4(OH)2 nanolayer Download PDF

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Publication number
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
water
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CN2012100753859A
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赵高凌
董伟霞
韩高荣
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Zhejiang University ZJU
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Zhejiang University ZJU
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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

A kind of preparation CaTi 2O 4(OH) 2The method of nanometer layer
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.
Embodiment 2
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.
CN2012100753859A 2012-03-21 2012-03-21 Method for preparing CaTi2O4(OH)2 nanolayer Pending CN102583520A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
YI-JEN HUANG ET AL: "Artificial Synthesis of Platelet-Like Kassite and Its Transformation to CaTiO3", 《CRYSTAL GROWTH AND DESIGN》 *

Cited By (6)

* Cited by examiner, † Cited by third party
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