CN107381616A - A kind of method that active porous nano ceric oxide is prepared based on organic formwork - Google Patents

A kind of method that active porous nano ceric oxide is prepared based on organic formwork Download PDF

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Publication number
CN107381616A
CN107381616A CN201710835530.1A CN201710835530A CN107381616A CN 107381616 A CN107381616 A CN 107381616A CN 201710835530 A CN201710835530 A CN 201710835530A CN 107381616 A CN107381616 A CN 107381616A
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presoma
prepared based
nanoparticle
organic formwork
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CN107381616B (en
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伍久林
郭小斑
孙新玉
纪明宇
张其清
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Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of method that active porous nano ceric oxide is prepared based on organic formwork, and it is using 2 methylimidazoles as mould material, by controlling calcination atmosphere, calcining heat, synthesizes the homogeneous and porous CeO of pattern2Nanoparticle.Gained CeO of the invention2Nanoparticle has the characteristics that size, particle diameter are small, and has good peroxidase activity, and its preparation method is simple, prepares low cost and other advantages, beneficial to large-scale promotion.

Description

A kind of method that active porous nano ceric oxide is prepared based on organic formwork
Technical field
The invention belongs to field of material preparation, and in particular to one kind prepares active porous nanometer titanium dioxide based on organic formwork The method of cerium.
Background technology
The method for preparing cerium dioxide nano grain mainly has the precipitation method, sol-gel process, hydro-thermal method.The precipitation method have make With equipment is simple, technical process is easily controlled, product purity is high, is easy to the advantages that commercialization, but filtering and washing precipitation When it is relatively difficult, and easily there is particle aggregation phenomenon in each stage.Sol-gel process is to prepare under cryogenic The common method of nano-metal-oxide particle, it has the advantages that, and product purity is high, specific surface area is big, good dispersion, still Reaction time is grown, and particle is easily reunited hardened, and cost of material is high.It is high, good dispersion that purity can be obtained using hydro-thermal method Nano-oxide, and this method environmental pollution is small, less energy consumption, but because reaction is carried out under high-temperature and high-pressure conditions, it is right Experimental facilities requires stricter, and investment is big, and operates dangerous, current less use.
Metal organic frame（Metal-organic frameworks, MOFs）It is a kind of Porous coordination polymer, by gold Category ion and organic ligand assemble under certain condition, have the advantages that structure and size, composition and property are controllable. MOFs has the porosity of superelevation and high specific surface area, makes it in the side such as gas storage and separation, air-sensitive and drug delivery Mask is widely used.There is presently no the report that ceria is prepared using metal organic formwork, and prior art system There is size heterogeneity in standby ceria, particle is easily reunited, and the problems such as severe reaction conditions, limit the hair of ceria Exhibition.The present invention is prepared for a kind of nanometer titanium dioxide with loose structure using six nitric hydrate ceriums and 2-methylimidazole as raw material Cerium.
The content of the invention
It is an object of the invention to provide a kind of method that active porous nano ceric oxide is prepared based on organic formwork, its Have the characteristics that size, particle diameter are small using 2-methylimidazole as ceria made from mould material, and there is good peroxidating Thing enzymatic activity, and its preparation method is simple, beneficial to large-scale promotion.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that active porous nano ceric oxide is prepared based on organic formwork, it comprises the following steps：
（1）The synthesis of presoma：By 3 mL, 1.55 mmol Ce (NO3)3•6H2The 2- first of O solution and 20 mL, 67.1mmol Base imidazole solution mixes 6h at room temperature, and gained yellow mercury oxide is washed three times with ethanol after centrifugation, then in 80 DEG C of bakings 24h is dried in case, obtains presoma；
（2）The synthesis of porous silica cerium nanoparticle：Gained presoma is placed in porcelain boat, is put into Muffle furnace, at 300-400 DEG C 3h is calcined in air atmosphere, gained yellow powder is porous silica cerium nanoparticle.
MOFs is a kind of hybrid inorganic-organic materials, and it can be obtained by inorganic unit and the structure of a variety of organic ligands To controllable loose structure, new property can be obtained by the combination of these construction units.The present invention utilizes 2-methylimidazole For template, by controlling calcination atmosphere, calcining heat, synthesize the homogeneous and porous metal oxide CeO of pattern2。
Cerium dioxide nano particle size, particle diameter prepared by the present invention is small, has good peroxidase activity, and it is made Preparation Method is simple, workable, and preparation cost is low, without adding surfactant, beneficial to large-scale promotion.
Brief description of the drawings
Fig. 1 is the XRD diffraction patterns of porous silica cerium nanoparticle obtained by embodiment 1-3 differences calcining heat.
Fig. 2 is the peroxidase activity contrast of porous silica cerium nanoparticle obtained by embodiment 1-3 differences calcining heat Figure.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
（1）The synthesis of presoma：By 3 mL, 1.55 mmol Ce (NO3)3•6H2The 2- first of O solution and 20 mL, 67.1mmol Base imidazole solution mixes 6h at room temperature, and gained yellow mercury oxide is washed three times with ethanol after centrifugation, then in 80 DEG C of bakings 24h is dried in case, obtains presoma；
（2）The synthesis of porous silica cerium nanoparticle：Gained presoma is placed in porcelain boat, is put into Muffle furnace, in 300 DEG C of air 3h is calcined in atmosphere, gained yellow powder is porous silica cerium nanoparticle.
Embodiment 2
（1）The synthesis of presoma：By 3 mL, 1.55 mmol Ce (NO3)3•6H2The 2- first of O solution and 20 mL, 67.1mmol Base imidazole solution mixes 6h at room temperature, and gained yellow mercury oxide is washed three times with ethanol after centrifugation, then in 80 DEG C of bakings 24h is dried in case, obtains presoma；
（2）The synthesis of porous silica cerium nanoparticle：Gained presoma is placed in porcelain boat, is put into Muffle furnace, in 350 DEG C of air 3h is calcined in atmosphere, gained yellow powder is porous silica cerium nanoparticle.
Embodiment 3
（1）The synthesis of presoma：By 3 mL, 1.55 mmol Ce (NO3)3•6H2The 2- first of O solution and 20 mL, 67.1mmol Base imidazole solution mixes 6h at room temperature, and gained yellow mercury oxide is washed three times with ethanol after centrifugation, then in 80 DEG C of bakings 24h is dried in case, obtains presoma；
（2）The synthesis of porous silica cerium nanoparticle：Gained presoma is placed in porcelain boat, is put into Muffle furnace, in 400 DEG C of air 3h is calcined in atmosphere, gained yellow powder is porous silica cerium nanoparticle.
Fig. 1 is the XRD diffraction patterns of cerium dioxide nano grain obtained by embodiment 1-3.
Cerium dioxide nano grain obtained by embodiment 1-3 is dissolved in water respectively, then using UV detector, Kinetic scans are carried out to solution under 652nm wavelength, reaction time 540s, determined under different temperatures every 30s records once The peroxidase activity of obtained porous silica cerium nanoparticle is calcined, as a result as shown in Figure 2.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, it should all belong to the covering scope of the present invention.

Claims (1)

  1. A kind of 1. method that active porous nano ceric oxide is prepared based on organic formwork, it is characterised in that：Comprise the following steps：
    （1）The synthesis of presoma：By 3 mL, 1.55 mmol Ce (NO3)3•6H2The 2- first of O solution and 20 mL, 67.1mmol Base imidazole solution mixes 6h at room temperature, and gained yellow mercury oxide is washed three times with ethanol after centrifugation, then in 80 DEG C of bakings 24h is dried in case, obtains presoma；
    （2）The synthesis of porous silica cerium nanoparticle：Gained presoma is placed in porcelain boat, is put into Muffle furnace, at 300-400 DEG C 3h is calcined in air atmosphere, gained yellow powder is porous silica cerium nanoparticle.
CN201710835530.1A 2017-09-15 2017-09-15 A method of active porous nano ceric oxide is prepared based on organic formwork Active CN107381616B (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN108786825A (en) * 2018-05-31 2018-11-13 西京学院 A kind of ceria base nano electro-catalytic liberation of hydrogen catalyst and preparation method thereof
CN110455874A (en) * 2019-08-22 2019-11-15 有研工程技术研究院有限公司 A kind of CoSn double metal oxide semiconductor material and preparation method thereof
CN112744853A (en) * 2020-12-30 2021-05-04 成都理工大学 Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora
CN112939059A (en) * 2021-03-23 2021-06-11 宁夏京成天宝饲料添加剂有限公司 Preparation method of porous zinc oxide
US20220119270A1 (en) * 2020-10-16 2022-04-21 Research & Business Foundation Sungkyunkwan University Ceria nanoparticles and ceria nanoparticles preparation method
CN115259201A (en) * 2022-07-27 2022-11-01 中国原子能科学研究院 Preparation method of nano thorium dioxide
CN115259096A (en) * 2022-07-27 2022-11-01 中国原子能科学研究院 Preparation method of nano metal oxide

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CN104741088A (en) * 2015-04-09 2015-07-01 云南大学 Method for preparing fluorine-containing wastewater defluorinating agent Fe-Al bimetallic organic framework compound
CN105529472A (en) * 2015-12-09 2016-04-27 武汉理工大学 Co-N double-doped flaky porous two-dimensional carbon material and preparation method thereof
CN107029772A (en) * 2016-02-04 2017-08-11 武汉理工大学 A kind of non-precious metal catalyst and preparation method thereof

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CN104741088A (en) * 2015-04-09 2015-07-01 云南大学 Method for preparing fluorine-containing wastewater defluorinating agent Fe-Al bimetallic organic framework compound
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108786825A (en) * 2018-05-31 2018-11-13 西京学院 A kind of ceria base nano electro-catalytic liberation of hydrogen catalyst and preparation method thereof
CN108786825B (en) * 2018-05-31 2020-12-22 西京学院 Cerium dioxide-based nano electro-catalytic hydrogen evolution catalyst and preparation method thereof
CN110455874A (en) * 2019-08-22 2019-11-15 有研工程技术研究院有限公司 A kind of CoSn double metal oxide semiconductor material and preparation method thereof
US20220119270A1 (en) * 2020-10-16 2022-04-21 Research & Business Foundation Sungkyunkwan University Ceria nanoparticles and ceria nanoparticles preparation method
US12077448B2 (en) * 2020-10-16 2024-09-03 Research & Business Foundation Sungkyunkwan University Ceria nanoparticles and ceria nanoparticles preparation method
CN112744853A (en) * 2020-12-30 2021-05-04 成都理工大学 Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora
CN112939059A (en) * 2021-03-23 2021-06-11 宁夏京成天宝饲料添加剂有限公司 Preparation method of porous zinc oxide
CN115259201A (en) * 2022-07-27 2022-11-01 中国原子能科学研究院 Preparation method of nano thorium dioxide
CN115259096A (en) * 2022-07-27 2022-11-01 中国原子能科学研究院 Preparation method of nano metal oxide
CN115259201B (en) * 2022-07-27 2023-12-12 中国原子能科学研究院 Preparation method of nano thorium dioxide

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