CN101113010A - Microwave Assisted Preparation of Cerium Oxide Nanoparticles - Google Patents
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- CN101113010A CN101113010A CNA2007101182685A CN200710118268A CN101113010A CN 101113010 A CN101113010 A CN 101113010A CN A2007101182685 A CNA2007101182685 A CN A2007101182685A CN 200710118268 A CN200710118268 A CN 200710118268A CN 101113010 A CN101113010 A CN 101113010A
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 3
- -1 cerium ion Chemical class 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 150000000703 Cerium Chemical class 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 5
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
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Abstract
一种微波辅助制备氧化铈纳米粒子的方法，属于氧化铈纳米粒子的制备技术领域。首先将铈离子溶液与碱液混合，然后放入微波高压反应罐中，经微波辅助反应得到氧化铈纳米粒子，其化学式为CeO2。本发明的优点在于，制备工艺简单，反应时间短，节省能源，所得氧化铈纳米粒子粒径小，分散性好，形貌规整。
The invention discloses a microwave-assisted method for preparing cerium oxide nanoparticles, which belongs to the technical field of preparation of cerium oxide nanoparticles. First, the cerium ion solution is mixed with the lye, and then put into a microwave high-pressure reaction tank, and the cerium oxide nanoparticle is obtained through microwave-assisted reaction, and its chemical formula is CeO 2 . The invention has the advantages of simple preparation process, short reaction time and energy saving, and the obtained cerium oxide nanoparticles have small particle size, good dispersibility and regular appearance.
Description
技术领域technical field
本发明属于氧化铈纳米粒子的制备技术领域，特别是提供了一种微波辅助制备氧化铈纳米粒子的方法。The invention belongs to the technical field of preparation of cerium oxide nanoparticles, and in particular provides a microwave-assisted method for preparing cerium oxide nanoparticles.
背景技术Background technique
纳米CeO2是一种廉价且用途极广的工业材料，它可以作为固体氧化物燃料电池(SOFC)的氧离子导体的主要基体材料，可以用作发光材料、电子陶瓷、玻璃的抛光剂及玻璃脱色澄清剂，在汽车尾气净化面可用作三元催化助剂，也是超导体、陶瓷、石油裂解催化剂和均相催化剂的重要组成成分，因而，氧化铈纳米粒子新制备技术的探索已成为近年热点研究课题。水热法是一种制备纳米材料的化学方法，该方法为各种前驱物的反应和结晶提供了一个在常压条件下无法得到的物理和化学环境，由于制备过程中不需要高温灼烧处理，避免可能形成的粉硬团聚，制得的粉体纯度高，分散性好，并且污染小，因此，近年来受到人们的广泛重视。传统的水热法中，采用普通加热方式，例如：在Mater Chem andPhys，2000，64：229-240中，J.H Chem Lin等人用Ce(III)的硝酸盐、Ce(IV)的硫酸盐和硫酸铵盐在180℃制备了CeO2纳米粒子。但此方法反应时间长，加热不均匀，升温速度慢，得到的粒子晶形不是很规整。鉴于上述制备过程中存在的问题，探索制备工艺简单易行，能耗少，制备晶形、粒度和分布好的氧化铈纳米粒子方法是十分必要的。Nano- CeO2 is a cheap and widely used industrial material. It can be used as the main matrix material of the oxygen ion conductor of the solid oxide fuel cell (SOFC), and can be used as a luminescent material, electronic ceramics, glass polishing agent and glass The decolorizing clarifier can be used as a three-way catalytic aid in the purification of automobile exhaust, and is also an important component of superconductors, ceramics, petroleum cracking catalysts and homogeneous catalysts. Therefore, the exploration of new preparation technologies for cerium oxide nanoparticles has become a hot topic in recent years research topic. The hydrothermal method is a chemical method for preparing nanomaterials. This method provides a physical and chemical environment that cannot be obtained under normal pressure conditions for the reaction and crystallization of various precursors. Since the preparation process does not require high-temperature burning treatment , to avoid the possible formation of powder hard agglomeration, the prepared powder has high purity, good dispersibility, and less pollution, so it has received extensive attention in recent years. In the traditional hydrothermal method, common heating methods are adopted, for example: in Mater Chem and Phys, 2000, 64: 229-240, JH Chem Lin et al. use Ce(III) nitrate, Ce(IV) sulfate and Ammonium sulfate salt prepared CeO2 nanoparticles at 180 °C. But this method takes a long time to react, the heating is uneven, the heating rate is slow, and the crystal shape of the obtained particles is not very regular. In view of the problems in the above-mentioned preparation process, it is necessary to explore a method for preparing cerium oxide nanoparticles with a simple and easy preparation process, less energy consumption, and good crystal shape, particle size and distribution.
发明内容Contents of the invention
本发明的目的在于提供一种微波辅助制备氧化铈纳米粒子的方法，解决了用传统的水热法制备氧化铈纳米粒子反应时间长，能耗高，粒子晶形不规整等问题。The object of the present invention is to provide a microwave-assisted method for preparing cerium oxide nanoparticles, which solves the problems of long reaction time, high energy consumption, and irregular crystal shape of cerium oxide nanoparticles prepared by traditional hydrothermal method.
本发明的技术方案是首先将铈离子溶液与碱液混合，然后放入微波高压反应罐中，经微波辅助反应得到氧化铈纳米粒子，其化学式为CeO2，其工艺步骤如下：The technical solution of the present invention is to first mix the cerium ion solution with the lye, then put it into a microwave high-pressure reaction tank, and obtain cerium oxide nanoparticles through microwave-assisted reaction, whose chemical formula is CeO 2 , and the process steps are as follows:
1、制备反应混合液1. Preparation of reaction mixture
配制0.1-1mol/L的铈盐溶液和0.1-1mol/L浓度的碱液，取2mL-20mL配制好的铈盐溶液放入烧杯中，加入模板剂，搅拌，再滴加2mL-20mL的碱液混合搅拌，制备得到反应混合液；Prepare 0.1-1mol/L cerium salt solution and 0.1-1mol/L lye solution, take 2mL-20mL prepared cerium salt solution into a beaker, add template agent, stir, then dropwise add 2mL-20mL alkali The liquid is mixed and stirred to prepare a reaction mixture;
2、微波辅助反应2. Microwave-assisted reaction
将步骤1制备的反应混合液放入微波高压反应罐中，在80-200℃下，以200W-1000W的功率用微波辅助进行高温高压反应2min-10h，之后采用炉内冷却至室温，得到含有产物CeO2的溶液；Put the reaction mixture prepared in step 1 into a microwave high-pressure reaction tank, and conduct a high-temperature and high-pressure reaction with microwave assistance at a power of 200W-1000W at 80-200°C for 2min-10h, and then cool it to room temperature in a furnace to obtain A solution of the product CeO2 ;
3、后处理3. Post-processing
将步骤2制备的溶液取出，分别用去离子水、无水乙醇洗涤产品1-5次，离心分离，在40-80℃下6h-24h干燥，研磨，得到粒径在纳米级，分散性好、形貌规整的立方萤石结构CeO2粉末。Take out the solution prepared in step 2, wash the product with deionized water and absolute ethanol for 1-5 times, centrifuge, dry at 40-80°C for 6h-24h, and grind to obtain a particle size in the nanometer scale with good dispersibility , CeO 2 powder with regular cubic fluorite structure.
本发明所述的铈盐溶液为Ce(NO3)3、Ce(Ac)3、Ce(SO4)2中的任何一种；所述的碱液为NaOH、NaAc、(NH2)2CO、NH3·H2O中的任何一种或其任意2-3种的混合物；所述的模板剂为SDS、CTAB、PEG、TEA、TX-100中的任何一种或其任意2-3种的混合物。The cerium salt solution of the present invention is any one of Ce(NO 3 ) 3 , Ce(Ac) 3 , Ce(SO 4 ) 2 ; the lye is NaOH, NaAc, (NH 2 ) 2 CO , NH 3 ·H 2 O, or any mixture of 2-3 of them; the template agent is any of SDS, CTAB, PEG, TEA, TX-100, or any 2-3 of them mixture of species.
与现有技术相比，本发明的优点在于：Compared with the prior art, the present invention has the advantages of:
由于采用微波加热方式，加热速度快，缩短了反应的时间，降低了能耗；另外，微波加热具有从内到外、选择性好、加热均匀、升温速度快等优点，因此所制得的产物有更好的晶形、粒度和分布；本方法制备工艺简单、反应条件容易控制，产品纯度高。Due to the microwave heating method, the heating speed is fast, the reaction time is shortened, and the energy consumption is reduced; in addition, microwave heating has the advantages of good selectivity, uniform heating, and fast heating speed from the inside to the outside, so the obtained product The method has better crystal form, particle size and distribution; the method has simple preparation process, easy control of reaction conditions and high product purity.
附图说明Description of drawings
图1为本发明微波辅助制备纳米氧化铈的制备流程示意图。Fig. 1 is a schematic diagram of the preparation process of microwave-assisted preparation of nano-cerium oxide in the present invention.
图2为本发明实施例1中产物CeO2粉体的XRD谱图。Fig. 2 is the XRD spectrum of the product CeO 2 powder in Example 1 of the present invention.
图3为本发明实施例1中产物CeO2粉体的TEM(100K)相片。Fig. 3 is the TEM (100K) photo of the product CeO 2 powder in Example 1 of the present invention.
图4为本发明实施例1中产物CeO2粉体的TEM(200K)相片Fig. 4 is product CeO in the embodiment of the present invention 1 TEM (200K) photo of powder
具体实施方式Detailed ways
实施例1Example 1
配制0.1mol/L的Ce(NO3)3溶液和0.4mol/L的NaAc溶液，取10ml的0.1mol/LCe(NO3)3溶液放入烧杯中，加入2.73gCTAB搅拌，再加入10ml的0.4mol/L NaAc溶液，混合搅拌。之后将混合液放入微波高压反应釜中进行反应，在180℃下反应6h，炉内冷却至室温。取出反应后的溶液，分别用去离子水、无水乙醇洗涤3次，离心分离，干燥，研磨，得到氧化铈纳米粉体。Prepare 0.1mol/L Ce(NO 3 ) 3 solution and 0.4mol/L NaAc solution, take 10ml of 0.1mol/LCe(NO 3 ) 3 solution into a beaker, add 2.73g CTAB and stir, then add 10ml of 0.4 mol/L NaAc solution, mix and stir. Afterwards, the mixture was put into a microwave autoclave for reaction at 180° C. for 6 h, and cooled to room temperature in the furnace. The reacted solution was taken out, washed three times with deionized water and absolute ethanol respectively, centrifuged, dried, and ground to obtain cerium oxide nanopowder.
对所得粉体进行X-射线衍射分析，结果如图2所示，图中出现的衍射峰均为CeO2的特征衍射峰，确认得到的产物是CeO2，并且产物中无任何杂质。X-ray diffraction analysis was performed on the obtained powder, and the results are shown in Figure 2. The diffraction peaks appearing in the figure are all characteristic diffraction peaks of CeO 2 , confirming that the obtained product is CeO 2 , and there is no impurity in the product.
产物的TEM透射电镜照片如图3、图4所示，从图中可以看出，此方法制得的CeO2为纳米粒子，粒径在10-20nm，晶形为立方萤石结构，并且分散性好、形貌规整。The TEM transmission electron microscope photos of the product are shown in Figure 3 and Figure 4. It can be seen from the figure that the CeO2 prepared by this method is a nano-particle with a particle size of 10-20nm. The crystal form is a cubic fluorite structure, and the dispersion Good, regular appearance.
实施例2Example 2
以Ce(Ac)3和H2O为反应物，采用与实施例1相同的条件和方法，同样可制备得到粒径在纳米级、均匀的CeO2粉体。Using Ce(Ac) 3 and H 2 O as reactants, using the same conditions and methods as in Example 1, a homogeneous CeO 2 powder with a particle size of nanometer can also be prepared.
实施例3Example 3
以Ce(NO3)3和NaOH为反应物，采用与实施例1相同的条件和方法，同样可制备得到粒径在纳米级、均匀的CeO2粉体。Using Ce(NO 3 ) 3 and NaOH as reactants, using the same conditions and methods as in Example 1, a homogeneous CeO 2 powder with a particle size of nanometer can also be prepared.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN102942206A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer hollow spheres |
| CN102951940A (en) * | 2012-11-05 | 2013-03-06 | 昆明理工大学 | Mesoporous cerium dioxide material preparation method |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| RU2487753C2 (en) * | 2008-12-17 | 2013-07-20 | Серион Текнолоджи, Инк. | Fuel additive containing cerium dioxide nanoparticles with altered structure |
| US9221032B2 (en) | 2006-09-05 | 2015-12-29 | Cerion, Llc | Process for making cerium dioxide nanoparticles |
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| US9221032B2 (en) | 2006-09-05 | 2015-12-29 | Cerion, Llc | Process for making cerium dioxide nanoparticles |
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| US9340738B2 (en) | 2006-09-05 | 2016-05-17 | Cerion, Llc | Method of making cerium oxide nanoparticles |
| US9993803B2 (en) | 2006-09-05 | 2018-06-12 | Cerion, Llc | Method of preparing cerium dioxide nanoparticles |
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| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
| CN102951940A (en) * | 2012-11-05 | 2013-03-06 | 昆明理工大学 | Mesoporous cerium dioxide material preparation method |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN102942206A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer hollow spheres |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| US10500228B1 (en) * | 2016-04-26 | 2019-12-10 | Battelle Memorial Institute | Nanoparticles, methods for producing nanoparticles and nanoparticle generators |
| CN109399689A (en) * | 2018-12-17 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A method of rare earth oxide is prepared using microwave technology |
| CN112340766A (en) * | 2020-11-27 | 2021-02-09 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112340766B (en) * | 2020-11-27 | 2022-02-01 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | A kind of preparation method of fluorinated ceria polishing powder under microwave condition |
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