CN103111627B - Method for manufacturing layered metal and metallic oxide material - Google Patents
Method for manufacturing layered metal and metallic oxide material Download PDFInfo
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- CN103111627B CN103111627B CN201310046893.9A CN201310046893A CN103111627B CN 103111627 B CN103111627 B CN 103111627B CN 201310046893 A CN201310046893 A CN 201310046893A CN 103111627 B CN103111627 B CN 103111627B
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Abstract
The invention relates to the technical field of the combination of material chemistry and a nanometer material. The method for manufacturing the layered metal and a metallic oxide material aims to provide a method of the preparation layer shape metal or the metallic oxide material. A layered double hydroxyl mixed metal oxide is a carrier, and metal negative ions are exchanged to an interlayer of the layered double hydroxyl mixed metal oxide through the way of the ion exchanging. The carrier completing the ion exchange is filtered, washed and dried, thus the layered metal or the metal oxide is obtained through reduction or roasting. The method of the preparation layer shaped metal and the metallic oxide material is simple and effective. Features of the metal or the metal oxide material are controlled by taking advantage of the interlayer limiting role of lactate dehydrogenase (LDH), thus the layered metal and the metallic oxide material are developed. The layer thickness is between the 1-20 layers of atoms. Besides, the material is stable due to the fact the LDT is limited. Even if being placed in the air for a long time or roasted under the high temperature, the layered metal and the metallic oxide material do not experience agglomeration.
Description
Technical field
The present invention relates to the technical field of materials chemistry and nano material synthesis, be related specifically to a kind of method of new synthesis laminated metal or metal oxide.
Background technology
In recent years, nano material plays more and more important effect in every field such as catalysis, electrochemistry, Solar use.The synthesis of novel nano-material causes everybody extensive attention.Since Nobel Prize in physics in 2010 has authorized the finder of Graphene, the nano material of stratiform has shown the performance being different from traditional nano particle in all fields.Because compared with traditional nano particle, the nano material of stratiform has the atom of more how low ligancy.But the shortcomings such as general stratified nano materials synthesis difficulty, cost are high, unstable, limit their extensive use.
Therefore, how to prepare the metal nano material of stratiform fast and easily, become a very concrete challenging problem.In this patent, we introduce a kind of very simple, effective, general method, the metal of preparation stratiform or metal oxide materials.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, provides a kind of method preparing laminated metal or metal oxide materials.
For technical solution problem, solution of the present invention is:
A kind of method preparing laminated metal or metal oxide materials is provided, comprises the steps:
With layered di-hydroxyl composite metal oxidate (LDH) for carrier, by the mode of ion-exchange, anionic metal is exchanged to the interlayer (because layered vector has superpower anion exchange capacity, the anionic metal majority (~ 85%) in precursor liquid all can be switched to carrier and get on) of layered di-hydroxyl composite metal oxidate; The carrier completing ion-exchange is filtered, washs and drying, then obtained metal or the metal oxide of stratiform by reduction or roasting; Institute's layered di-hydroxyl composite metal oxidate is hydrotalcite or houghite compound, specifically refers to the one in magnalium hydrotalcite, cobalt aluminum hydrotalcite, nickel aluminum hydrotalcite or zinc-iron hydrotalcite, and the load capacity of its metal or metal oxide is 0.01 ~ 15.0%; Described anionic metal refers to the anion of any one metallic element of Au, Pd, Mn, Pt, Ru or Rh.
In the present invention, described ion-exchange refers to, is added by layered di-hydroxyl composite metal oxidate in the solution containing described anionic metal, at room temperature carries out ion-exchange.
In the present invention, described reduction refers to, will filter, wash and dried support dispersion in solvent, add reducing agent and carry out reduction reaction under room temperature; Described solvent is methyl alcohol, ethanol, water or dimethyl formamide, and described reducing agent is sodium borohydride or potassium borohydride, and the mol ratio of the anionic metal that feeds intake in reducing agent and precursor aqueous solution is 10-100.
In the present invention, described roasting refers to, by the carrier roasting in atmosphere after filtration, after washing and dry process, sintering temperature controls at 400 ~ 800 DEG C.
Beneficial effect of the present invention is:
The present invention is simply effective, utilizes the interlayer restriction of LDH, controls the pattern of metal or metal oxide materials, makes it be grown to serve as stratiform.Layer thickness is between 1-20 layer atom.In addition, owing to there being the restriction of LDH, this material can be highly stable., all can not there is agglomeration in long-time placement or high-temperature roasting in atmosphere.
Detailed description of the invention
Below in conjunction with specific embodiment, realization of the present invention is described in detail.
Embodiment 1:
1g magnalium hydrotalcite is joined in the solution containing 0.22mg gold chloride, after room-temperature ion exchanges, by solid filtering out, after washing drying, be distributed in ethanolic solution, add 0.44mg sodium borohydride, room temperature by dry for solid filtering washing, just can obtain the stratiform Au nano material of magnalium hydrotalcite load after being reduced to solution change brownish red, the load capacity of Au is that the thickness of 0.01%, stratiform Au is at 1-5 layer atom.
Embodiment 2:
1g nickel aluminum hydrotalcite is joined in the solution containing the acid of 10mg chlorine palladium, after room-temperature ion exchanges, by solid filtering out, after washing drying, be distributed in the aqueous solution, add 30mg potassium borohydride, room temperature is reduced to after solution grays, and by dry for solid filtering washing, just can obtain the stratiform Pd nano material of nickel aluminum hydrotalcite load, the load capacity of Pd is that the thickness of 1%, stratiform Pd is at 1-10 layer atom.
Embodiment 3:
1g cobalt aluminum hydrotalcite is joined in the solution containing 30mg chloroplatinic acid, after room-temperature ion exchanges, by solid filtering out, after washing drying, be distributed in dimethyl formamide solution, add 200mg potassium borohydride, room temperature is reduced to after solution grays, and by dry for solid filtering washing, just can obtain the stratiform Pt nano material of cobalt aluminum hydrotalcite load, the load capacity of Pt is that the thickness of 4%, stratiform Pt is at 1-10 layer atom.
Embodiment 4:
1g zinc-iron hydrotalcite is joined in the solution containing 350mg ruthenium hydrochloride, after room-temperature ion exchanges, by solid filtering out, after washing drying, be distributed in methanol solution, add 3.8g sodium borohydride, room temperature is reduced to after solution grays, and by dry for solid filtering washing, just can obtain the stratiform Ru nano material of zinc-iron hydrotalcite load, the load capacity of Ru is that the thickness of 10%, stratiform Ru is at 5-20 layer atom.
Embodiment 5:
1g magnalium hydrotalcite is joined in the solution containing 50mg potassium permanganate, after room-temperature ion exchanges, by solid filtering out, after washing drying, the solid that obtains of 800 DEG C of roastings in atmosphere, just can obtain the stratiform manganese oxide nanometer material of magnalium hydrotalcite load, the load capacity of manganese oxide is 1%, and the thickness of stratiform manganese oxide is at 5-10 layer atom.
Embodiment 6:
1g magnalium hydrotalcite is joined in the solution containing the acid of 160mg chlorine palladium, after room-temperature ion exchanges, by solid filtering out, after washing drying, the solid that obtains of 600 DEG C of roastings in atmosphere, just can obtain the stratiform PdO nano material of magnalium hydrotalcite load, the load capacity of PdO is that the thickness of 15%, stratiform PdO is at 15-20 layer atom.
Embodiment 7:
1g magnalium hydrotalcite is joined in the solution containing the acid of 160mg chlorine palladium, after room-temperature ion exchanges, by solid filtering out, after washing drying, the solid that obtains of 400 DEG C of roastings in atmosphere, just can obtain the stratiform PdO nano material of magnalium hydrotalcite load, the load capacity of PdO is that the thickness of 15%, stratiform PdO is at 10-20 layer atom.
Finally, the thing that also should be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be had.All distortion that those of ordinary skill in the art all can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (3)
1. prepare a method for laminated metal or metal oxide materials, it is characterized in that, comprise the steps:
Take layered di-hydroxyl composite metal oxidate as carrier, by the mode of ion-exchange by the interlayer of the anion exchange of containing metal element to layered di-hydroxyl composite metal oxidate; The carrier completing ion-exchange is filtered, washs and drying, then obtained metal or the metal oxide of stratiform by reduction or roasting;
Layered di-hydroxyl composite metal oxidate specifically refers to the one in magnalium hydrotalcite, cobalt aluminum hydrotalcite, nickel aluminum hydrotalcite or zinc-iron hydrotalcite, and the load capacity of its metal or metal oxide is 0.01 ~ 15.0%; The anion of described containing metal element refers to the anion containing any one metallic element of Au, Pd, Mn, Pt, Ru or Rh;
Described ion-exchange refers to, is added by layered di-hydroxyl composite metal oxidate in the solution of the anion containing described containing metal element, at room temperature carries out ion-exchange.
2. method according to claim 1, is characterized in that, described reduction refers to, will filter, wash and dried support dispersion in solvent, add reducing agent and carry out reduction reaction under room temperature; Described solvent is methyl alcohol, ethanol, water or dimethyl formamide, and described reducing agent is sodium borohydride or potassium borohydride, and the mol ratio of the anion of the containing metal element that feeds intake in reducing agent and precursor aqueous solution is 10-100.
3. method according to claim 1, is characterized in that, described roasting refers to, by the carrier roasting in atmosphere after filtration, after washing and dry process, sintering temperature controls at 400 ~ 800 DEG C.
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| CN105502556B (en) * | 2015-12-03 | 2017-12-01 | 常州大学 | A kind of method for handling organic pollutants |
| GB201703558D0 (en) * | 2017-03-06 | 2017-04-19 | Univ Oxford Innovation Ltd | catalysts |
| CN107419266A (en) * | 2017-05-08 | 2017-12-01 | 西华大学 | A kind of surface in situ growth has magnesium alloy of composite biological coating and preparation method thereof |
| CN109529866B (en) * | 2018-09-28 | 2021-09-07 | 天津大学 | Preparation method and application of potassium permanganate modified layered metal oxide |
| CN109659543B (en) * | 2018-12-24 | 2020-09-08 | 苏州大学 | Bimetallic oxide nano material and preparation and application thereof |
| CN113956883B (en) * | 2021-11-25 | 2022-11-18 | 北京化工大学 | Monoatomic/magnesium-aluminum hydrotalcite material and preparation method and application thereof |
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| CN101402039A (en) * | 2008-11-13 | 2009-04-08 | 北京化工大学 | Method for producing supported metal palladium catalyst |
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| JP4297716B2 (en) * | 2003-03-31 | 2009-07-15 | カウンシル オブ サイエンティフィク アンド インダストリアル リサーチ | Method for forming CC bond |
| TW201132346A (en) * | 2010-03-26 | 2011-10-01 | Univ Nat Taiwan | A method for controlling toxicity of metallic particles and a low-toxic composite of metallic nanoparticles and inorganic clay |
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| CN101391201A (en) * | 2008-10-15 | 2009-03-25 | 东华大学 | Zinc oxide nano-rod/ magnalium laminar double-hydroxide preparation method and use thereof |
| CN101402039A (en) * | 2008-11-13 | 2009-04-08 | 北京化工大学 | Method for producing supported metal palladium catalyst |
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