CN102992397A - Preparation method for rare earth element-doped titanium dioxide nano material - Google Patents
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Abstract
The invention relates to a preparation method for a rare earth element-doped titanium dioxide nano material. The method comprises the steps of dissolving urea and rare earth element nitrate in absolute ethyl alcohol; adding liquid titanium source into the above solution to form a homogeneous solution; adding deionized water with stirring to form a transparent gel; performing hydro-thermal treatment on the above gel; washing, filtering and drying to obtain the rare earth element-doped titanium dioxide nano material. An object of doping titanium dioxide by using the rare earth element is realized through automatic regulation and control of pH value of a reaction system by slow decomposition of urea in the hydrothermal process. The preparation method is simple in process and flow, has wide parameter adjustable range, strong repeatability and low cost, and can be used for preparing different rare earth element-doped titanium dioxide nano materials or a plurality of the rare earth elements co-doped titanium dioxide nano material.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide nano material, particularly relate to a kind of preparation method of rare earth doped titanium dioxide nano material, belong to the inorganic nano material preparing technical field.
Background technology
Titanium dioxide because have that spectrochemical property is stable, catalytic efficiency is high, oxidation capacity is strong, nontoxic, cheap, simple, advantages such as operational condition is controlled easily, non-secondary pollution of technical process in actual applications, it has received the increasingly extensive concern of people as photocatalyst.The developed countries such as America and Europe have all injected capital into and research effort is carried out the research and development of optically catalytic TiO 2 technology, and new high-tech industry based on this also forms.
Titanium dioxide is as a kind of semiconductor functional material, and its photocatalytic activity mainly determines by the crystalline structure of self, but also very responsive to a small amount of impurity.Can improve spectral response range and the catalytic efficiency of photocatalyst by doping vario-property.At present to the research of single doping vario-property of titanium dioxide comparative maturity, by the doping of some metallic elements and non-metallic element, the photocatalysis performance of titanium dioxide significantly improves.A small amount of metal ion mixes in titanium dioxide, can make it become the right shallow gesture in light induced electron-hole and catch trap, prolong the recombination time in electronics and hole, improve the photocatalysis performance of titanium dioxide, and, some doping can also reduce the energy gap of titanium dioxide, enlarge its light abstraction width, improve the utilization ratio to sunlight.
Rare earth is one of grand strategy resource of China, and its reserves, output and export volume be row the first in the world all.Rare earth element has complicated level structure and spectral response curve, and nano titanium oxide is carried out doping vario-property, but its photocatalysis efficiency of Effective Raise is that tool is wished one of technology that solves the visible light utilization ratio., some preparation method's rare earth elements doping utilization ratio in the past is not high, and the rare earth atom ratio that can successfully replace the lattice sites in the titanium dioxide is lower, so photocatalytic activity improves not obvious.And, adopt the preparation method of two kinds of rare earth element co-doped titanium dioxide, report at present less; Adopt that the preparation method of rare earth element co-doped titanium dioxide there is no report more than three kinds.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method of rare earth doped titanium dioxide nano material.
A kind of preparation method of rare earth doped titanium dioxide nano material is characterized in that, comprises the steps:
(1) in dehydrated alcohol, adds urea, rare earth element nitrate, add the liquid phase titanium source after the stirring and dissolving, stir and form homogeneous phase solution; Then in above-mentioned system, drip while stirring deionized water, until form clear gel;
(2) above-mentioned gel is put into the stainless steel autoclave of teflon lined, 120～200 ℃ of lower hydro-thermal reactions 12～48 hours; With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain rare earth doped titanium dioxide nano material.
The urea quality that adds described in the step (1) is/100 milliliters of 0.1 gram/100 milliliters～3 grams with reaction soln cumulative volume ratio.
Rare earth element nitrate described in the step (1) is a kind of or its combination in the cerous nitrate, lanthanum nitrate, neodymium nitrate, Yttrium trinitrate, Gadolinium trinitrate, europium nitrate, Terbium trinitrate, samaric nitrate, thulium nitrate, Erbium trinitrate, ytterbium nitrate of hydration or non-hydrated.
The rare earth element nitrate quality that adds described in the step (1) is/10 milliliters of 0.001 gram/10 milliliters～0.5 grams with adding liquid phase titanium volume source ratio.
Liquid phase titanium source described in the step (1) is a kind of or its combination in positive four butyl esters of metatitanic acid, isopropyl titanate, the tetraethyl titanate.
Liquid phase titanium source described in the step (1) adds volume and is 5:100～30:100 with reaction soln cumulative volume ratio.
The deionized water volume that adds described in the step (1) is 2:100～20:100 with reaction soln cumulative volume ratio.
In the present invention, the liquid phase titanium source slowly is hydrolyzed and forms the hydrous titanium oxide gel, and rare earth ion is evenly dispersed in the hydrous titanium oxide gel; By the slow decomposition of urea in water-heat process, the acid-basicity of system moves to the weakly alkaline direction gradually, has realized in-situ doped in the titanium oxide lattice of thulium.This preparation method's technique and simple flow, the parameter variable range is wide, and repeatable strong, cost is low, can prepare different rare earth doped and multiple rare earth element codoping titanium dioxide nano materials.Rare earth doped titanium dioxide nano material by above-mentioned preparation method obtains is the nanocrystal of polymolecularity, and grain size is in 10 nanometers, and the size homogeneous has higher photocatalysis Decomposition organic contamination physical performance.
Description of drawings
Fig. 1: the X-ray powder diffraction collection of illustrative plates of the rare earth doping titanium dioxide nano material that is made by embodiment 2.
Fig. 2: the high-resolution-ration transmission electric-lens photo of the rare earth doping titanium dioxide nano material that is made by embodiment 2.
Embodiment
The present invention is further elaborated below by embodiment, and its purpose only is better to understand content of the present invention.Therefore, the cited case does not limit protection scope of the present invention.
Embodiment 1:
In 80 milliliters of dehydrated alcohols, add successively 1 gram urea, 0.5 gram lanthanum nitrate hexahydrate.Add 12 milliliters of isopropyl titanates after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 7 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 170 degrees centigrade of lower hydro-thermal reactions 48 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 8～10 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 40 minutes under 300 watts UV-light.
Embodiment 2:
In 50 milliliters of dehydrated alcohols, add successively 0.5 gram urea, 0.3 gram lanthanum nitrate hexahydrate, 0.02 gram, six nitric hydrate ceriums.Add 8 milliliters of positive four butyl esters of metatitanic acid after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 4 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 150 degrees centigrade of lower hydro-thermal reactions 24 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 5～7 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 30 minutes under 300 watts UV-light.
Embodiment 3:
In 100 milliliters of dehydrated alcohols, add successively 1.2 gram urea, 0.1 gram gadolinium nitrate hexahydrate, 0.05 gram, six nitric hydrate neodymiums.Add 15 milliliters of tetraethyl titanates after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 8 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 200 degrees centigrade of lower hydro-thermal reactions 16 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 7～9 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 50 minutes under 300 watts UV-light.
Embodiment 4:
In 30 milliliters of dehydrated alcohols, add successively 0.3 gram urea, 0.08 gram, six nitric hydrate yttriums, 0.06 gram, six nitric hydrate samariums.Add 5 milliliters of positive four butyl esters of metatitanic acid after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 2 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 160 degrees centigrade of lower hydro-thermal reactions 36 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 6～9 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 40 minutes under 300 watts UV-light.
Embodiment 5:
In 60 milliliters of dehydrated alcohols, add successively 0.8 gram urea, 0.15 gram, six nitric hydrate europiums, 0.09 gram, six nitric hydrate erbiums.Add 9 milliliters of isopropyl titanates after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 6 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 120 degrees centigrade of lower hydro-thermal reactions 40 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 4～6 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 50 minutes under 300 watts UV-light.
Embodiment 6:
In 70 milliliters of dehydrated alcohols, add successively 1.5 gram urea, 0.06 gram, six nitric hydrate terbiums, 0.05 gram ytterbium nitrate, 0.02 gram, six nitric hydrate thuliums.Add 10 milliliters of positive four butyl esters of metatitanic acid after the stirring and dissolving, stir.Then in above-mentioned system, drip while stirring 7 ml deionized water, until form clear gel.Above-mentioned gel is put into the stainless steel autoclave of teflon lined, 150 degrees centigrade of lower hydro-thermal reactions 30 hours.With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain the rare earth doped titanium dioxide nano material of target compound.
Gained rare earth doping titanium dioxide nano material is the nanocrystal of polymolecularity, and particle diameter is approximately 5～8 nanometers, the size homogeneous.0.1 restraining above-mentioned product reaches more than 99% the degradation rate of 20 mg/litre methyl orange solutions in 30 minutes under 300 watts UV-light.
Claims (7)
1. the preparation method of a rare earth doped titanium dioxide nano material is characterized in that, comprises the steps:
(1) in dehydrated alcohol, adds urea, rare earth element nitrate, add the liquid phase titanium source after the stirring and dissolving, stir and form homogeneous phase solution; Then in above-mentioned system, drip while stirring deionized water, until form clear gel;
(2) above-mentioned gel is put into the stainless steel autoclave of teflon lined, 120～200 ℃ of lower hydro-thermal reactions 12～48 hours; With the precipitated product deionized water wash, until the pH of washings is neutral, then carry out drying treatment after reaction finishes, obtain rare earth doped titanium dioxide nano material.
2. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1 is characterized in that, the urea quality that adds described in the step (1) is/100 milliliters of 0.1 gram/100 milliliters～3 grams with reaction soln cumulative volume ratio.
3. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1, it is characterized in that the rare earth element nitrate described in the step (1) is a kind of or its combination in the cerous nitrate, lanthanum nitrate, neodymium nitrate, Yttrium trinitrate, Gadolinium trinitrate, europium nitrate, Terbium trinitrate, samaric nitrate, thulium nitrate, Erbium trinitrate, ytterbium nitrate of hydration or non-hydrated.
4. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1, it is characterized in that the rare earth element nitrate quality that adds described in the step (1) is/10 milliliters of 0.001 gram/10 milliliters～0.5 grams with adding liquid phase titanium volume source ratio.
5. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1 is characterized in that the liquid phase titanium source described in the step (1) is a kind of or its combination in positive four butyl esters of metatitanic acid, isopropyl titanate, the tetraethyl titanate.
6. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1 is characterized in that, the liquid phase titanium source described in the step (1) adds volume and reaction soln cumulative volume than being 5:100～30:100.
7. the preparation method of described a kind of rare earth doped titanium dioxide nano material according to claim 1 is characterized in that, the deionized water volume that adds described in the step (1) and reaction soln cumulative volume are than being 2:100～20:100.
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| CN115337953B (en) * | 2022-09-22 | 2024-02-02 | 浙江工业大学 | Mn and N co-doped TiO is prepared by a one-step hydrothermal method 2 Process for photocatalytic material, product and use in air purification |
| CN117101641A (en) * | 2023-09-25 | 2023-11-24 | 中国人民解放军火箭军工程大学 | Neodymium-doped mesoporous titanium dioxide nano photocatalyst and preparation method and application thereof |
| CN117101641B (en) * | 2023-09-25 | 2024-04-30 | 中国人民解放军火箭军工程大学 | Neodymium-doped mesoporous titanium dioxide nano photocatalyst and preparation method and application thereof |
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