CN104826620B - A kind of MgTi2O5The preparation method of nanocatalyst - Google Patents

A kind of MgTi2O5The preparation method of nanocatalyst Download PDF

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CN104826620B
CN104826620B CN201510201203.1A CN201510201203A CN104826620B CN 104826620 B CN104826620 B CN 104826620B CN 201510201203 A CN201510201203 A CN 201510201203A CN 104826620 B CN104826620 B CN 104826620B
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mgti
nanocatalyst
preparation
temperature
present
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CN104826620A (en
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王国凤
张柠
曲阳
潘凯
潘清江
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Heilongjiang University
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Heilongjiang University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

A kind of MgTi2O5The preparation method of nanocatalyst, the present invention relates to the preparation method of nanocatalyst.The invention solves the problems that existing method is difficult to prepare pure phase MgTi2O5Nanocrystalline technical problem.Method:First, magnesium acetate and butyl titanate are added in ethylene glycol solution, are stirred;2nd, wash, dry;3rd, it is calcined.The inventive method can prepare the MgTi of pure phase2O5, and the MgTi2O5Average particle diameter size is less than 100 nanometers, is a kind of catalytic efficiency nano-photocatalyst very high.The present invention is for preparing MgTi2O5Nanocatalyst.

Description

A kind of MgTi2O5The preparation method of nanocatalyst
Technical field
The present invention relates to the preparation method of nanocatalyst.
Background technology
Photolysis water hydrogen technology starts from 1972, and TiO is found by two professors of Fujishima A and Honda K2Monocrystalline electricity Pole photochemical catalyzing so as to produce hydrogen this phenomenon, so as to disclose using the possibility of the direct hydrogen production by water decomposition of solar energy Property, open using the research road of solar photolysis water hydrogen.The principle of photocatalytic water is:Light radiation on the semiconductor, works as spoke The energy penetrated be more than or equivalent to semiconductor energy gap when, electronics to be stimulated and transit to conduction band from valence band in semiconductor, and Hole then stays in valence band, separates electronics and hole, and water then is reduced into hydrogen in the diverse location of semiconductor respectively Or water oxygen is melted into oxygen.
In this kind of compound of titanate, TiO8Octahedra corner-sharing or common side form electronegative layer structure, positively charged Metal ion filling between the layers, and distort TiO8Octahedron is considered as being risen emphatically in the generation of photocatalytic activity Act on.Particularly magnesium titanate is nanocrystalline with good photocatalytic activity, but pure phase magnesium titanate is difficult synthesis.It is particularly pure Phase MgTi2O5It is nanocrystalline not to be reported also.
In sum, synthesis pure phase MgTi is prepared2O5It is nanocrystalline that a kind of high-performance nano photochemical catalyst can be provided.It is another Aspect, the performance of nano-photocatalyst depends on the synthetic method of nano material.
The content of the invention
The invention solves the problems that existing method is difficult to prepare pure phase MgTi2O5Nanocrystalline technical problem, and provide a kind of MgTi2O5The preparation method of nanocatalyst.
A kind of MgTi2O5The preparation method of nanocatalyst, specifically follows the steps below:
First, magnesium acetate and butyl titanate are added in ethylene glycol solution, it is 20 DEG C to control temperature, and mixing speed is 100r/min, stirs 20min, obtains mixture;
2nd, the mixture obtained using absolute ethanol washing step one, is vacuum dried under the conditions of being then 80 DEG C in temperature 6h, obtains preformed objects;
3rd, the preformed objects that step 2 is obtained are calcined, are obtained MgTi2O5Nanocatalyst.
The beneficial effects of the invention are as follows:The inventive method can prepare the MgTi of pure phase2O5, and the MgTi2O5Average grain Footpath size is less than 100 nanometers, and under ultraviolet light, hydrogen output, per hour up to 400 micromoles, is that a kind of catalytic efficiency is very high Nano-photocatalyst.
The present invention is for preparing MgTi2O5Nanocatalyst.
Brief description of the drawings
Fig. 1 is MgTi prepared by embodiment one2O5The transmission electron microscope photo of nanocatalyst;
Fig. 2 is MgTi prepared by embodiment one2O5The XRD spectra of nanocatalyst;
Fig. 3 is MgTi prepared by embodiment one2O5The photocatalytic water hydrogen output figure of nanocatalyst.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also including each specific embodiment it Between any combination.
Specific embodiment one:A kind of MgTi of present embodiment2O5The preparation method of nanocatalyst, specifically according to What lower step was carried out:
First, magnesium acetate and butyl titanate are added in ethylene glycol solution, it is 20 DEG C to control temperature, and mixing speed is 100r/min, stirs 20min, obtains mixture;
2nd, the mixture obtained using absolute ethanol washing step one, is vacuum dried under the conditions of being then 80 DEG C in temperature 6h, obtains preformed objects;
3rd, the preformed objects that step 2 is obtained are calcined, are obtained MgTi2O5Nanocatalyst.
Specific embodiment two:Present embodiment from unlike specific embodiment one:Magnesium acetate is in step one 0.268g, butyl titanate is 0.425mL, and ethylene glycol solution is 60mL.Other are identical with specific embodiment one.
Specific embodiment three:Present embodiment from unlike specific embodiment one or two:When being calcined in step 3, Programming rate is controlled for 1~20 DEG C/min, it is 400~700 DEG C to be warming up to temperature, and roasting time is 1~8h.Other and specific reality Apply mode one or two identical.
Specific embodiment four:Present embodiment from unlike specific embodiment one or two:When being calcined in step 3, Programming rate is controlled for 10~15 DEG C/min, it is 500~650 DEG C to be warming up to temperature, and roasting time is 2~6h.Other with it is specific Implementation method one or two is identical.
Specific embodiment five:Present embodiment from unlike specific embodiment one or two:When being calcined in step 3, Temperature is warming up to for 600 DEG C.Other are identical with specific embodiment one or two.
Beneficial effects of the present invention are verified using following examples:
Embodiment one:
A kind of MgTi of the present embodiment2O5The preparation method of nanocatalyst, specifically follows the steps below:
First, 0.268g magnesium acetates and 0.425mL butyl titanates are added in 60mL ethylene glycol solutions, control the temperature to be 20 DEG C, mixing speed is 100r/min, stirs 20min, obtains mixture;
2nd, the mixture obtained using absolute ethanol washing step one, is vacuum dried under the conditions of being then 80 DEG C in temperature 6h, obtains preformed objects;
3rd, the preformed objects that step 2 is obtained are calcined, are obtained MgTi2O5Nanocatalyst, during roasting, control heats up Speed is 10 DEG C/min, is warming up to temperature for 600 DEG C, and roasting time is 5h.
MgTi manufactured in the present embodiment2O5The transmission electron microscope photo of nanocatalyst is as shown in figure 1, can from Fig. 1 To find out, MgTi2O5Average particle diameter size is less than 100 nanometers.
MgTi manufactured in the present embodiment2O5The XRD spectra of nanocatalyst is as shown in Fig. 2 as can be seen from the figure MgTi2O5Nanocatalyst is orthorhombic crystal phase.
MgTi manufactured in the present embodiment2O5The photocatalytic water hydrogen output figure of nanocatalyst is as shown in figure 3, can from figure Go out MgTi2O5It is a kind of catalytic efficiency nano-photocatalyst very high.

Claims (4)

1. a kind of MgTi2O5The preparation method of nanocatalyst, it is characterised in that the method is specifically to follow the steps below 's:
First, magnesium acetate and butyl titanate are added in ethylene glycol solution, control temperature for 20 DEG C, mixing speed is 100r/ Min, stirs 20min, obtains mixture;
2nd, the mixture obtained using absolute ethanol washing step one, 6h is vacuum dried under the conditions of being then 80 DEG C in temperature, is obtained To preformed objects;
3rd, the preformed objects that step 2 is obtained are calcined, are obtained MgTi2O5Nanocatalyst;
Magnesium acetate is 0.268g wherein in step one, and butyl titanate is 0.425mL, and ethylene glycol solution is 60mL.
2. a kind of MgTi according to claim 12O5The preparation method of nanocatalyst, it is characterised in that roasted in step 3 During burning, programming rate is controlled for 1~20 DEG C/min, it is 400~700 DEG C to be warming up to temperature, and roasting time is 1~8h.
3. a kind of MgTi according to claim 22O5The preparation method of nanocatalyst, it is characterised in that roasted in step 3 During burning, programming rate is controlled for 10~15 DEG C/min, it is 500~650 DEG C to be warming up to temperature, and roasting time is 2~6h.
4. a kind of MgTi according to claim 32O5The preparation method of nanocatalyst, it is characterised in that roasted in step 3 During burning, temperature is warming up to for 600 DEG C.
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CN110835155B (en) * 2019-11-19 2021-12-07 浙江工业大学 Method for treating water by catalyzing ozone oxidation through magnesium titanate
CN118698563A (en) * 2024-08-29 2024-09-27 中国市政工程西北设计研究院有限公司 Titanium-based perovskite oxide heterojunction catalytic material and preparation method and application thereof

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DD258213A1 (en) * 1987-03-06 1988-07-13 Univ Schiller Jena PROCESS FOR PRODUCING DISPERSER POWDER OF MG LOW2 TIO DEEP4, MGTIO LOW 3 AND MGTI LOW2 O LOW 5
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DD258213A1 (en) * 1987-03-06 1988-07-13 Univ Schiller Jena PROCESS FOR PRODUCING DISPERSER POWDER OF MG LOW2 TIO DEEP4, MGTIO LOW 3 AND MGTI LOW2 O LOW 5
CN102351242A (en) * 2011-08-17 2012-02-15 南京师范大学 Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7
CN103011264A (en) * 2012-12-19 2013-04-03 黑龙江大学 Preparation method of one-dimensional metal titanate nanorods
CN104084184A (en) * 2014-06-12 2014-10-08 陕西师范大学 Preparation method and application of semiconductor photo-catalyst sodium magnesium titanate

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"Heavy metal sorption properties of magnesium titanate mesoporous nanorods";Xueyun Wang et al.;《Journal of Materials Chemistry A》;20150415;第3卷;第11796-11800页 *
"Photocatalytic activity of MTiO3(M=Ca,Ni,and Zn) nanocrystals for water decomposition to hydrogen;Shuai Liu et al.;《Journal of Materials Research》;20140604;第29卷(第11期);第1295-1301页 *

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