CN106495203A - 氧化铈空心微球的制备方法 - Google Patents
氧化铈空心微球的制备方法 Download PDFInfo
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 21
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004005 microsphere Substances 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910017920 NH3OH Inorganic materials 0.000 claims abstract description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical class [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000178 monomer Substances 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
本发明涉及一种氧化铈空心微球的制备方法。氧化铈空心微球的制备方法，包括如下步骤：称取10 g苯乙烯单体，100 g水，加入250 mL三口烧瓶中，室温通入氮气30 min，搅拌，升温到70℃，加入0.1g过硫酸钾，保持温度，共计10 h，之后冷却;离心分离，超声分散于水中，制得PS微球模板;称取PS微球模板溶液，25 mL水，加人三口烧瓶中，超声10 min，然后搅拌，升温到60℃，加入0.434 g Ce(N03)3·6H2 O，反应2 h，加入0.25 g NH3·OH，反应2 h后，自然冷却；产物离心，分别用水和乙醇洗涤2次；产物放置在恒温干燥箱中干燥6 h，最后将样品在马弗炉中500℃下煅烧2 h，得氧化铈空心微球。本发明制备CeO2空心微球的球径约220 nm，壳层厚度约20 nm。氧化铈空心微球粒径均匀，单分散。
Description
技术领域
本发明涉及一种氧化铈空心微球的制备方法。
背景技术
光催化氧化技术是近年发展起来的一种节能、环保的绿色环保技术。TiO2是应用最为广泛的光催化剂，具有廉价、无毒、稳定性好等特点，但是TiO2本身存在的问题比如能带较高、量子效率低的缺点阻碍了其进一步应用，因此，开发新型光催化剂成为拓展光催化应用的有效途径之一。
无机空心微球具有形态可控、尺寸均匀、比表面积大等特点。与其它形貌材料相比，反应物分子更容易地转移到多孔壳壁的活性位置而提高催化效率。并且，这种空心结构光在内部孔洞中多次反射而提高光源的利用率。在当前环境污染严重的形势之下，无机空心球的光催化特性已成为解决环境问题的途径之一。CeO2空心微球可以通过模板法制备。以碳球为模板，利用碳球表面的羟基与Ce3+作用，制备粒径为150nm的CeO2空球。以油菜花粉为模板，制备了粒径为10nm的CeO2空心球，在可见光照射下对品红溶液降解。目前，使用模板法制备CeO2空心微球的方法要么表面改性较为复杂，要么受制于天然原料难于规模化。CeO2空心微球简便的制备方法鲜有报道。
发明内容
本发明旨在针对上述问题，提出一种CeO2空心微球简便的制备方法。
本发明的技术方案在于：
氧化铈空心微球的制备方法，包括如下步骤：
（1）PS模板的制备：
称取10 g苯乙烯单体，100 g水，加入250 mL三口烧瓶中，室温通入氮气30 min，搅拌，升温到70℃，加入0.1 g过硫酸钾，保持温度，共计10 h，之后冷却;制备胶体溶液离心分离，超声分散于水中，制得5％的PS微球模板;
（2）氧化铈空心微球的制备：
称取40 g PS微球模板溶液，25 mL水，加人三口烧瓶中，超声10 min，然后搅拌，升温到60℃，加入0.434 g Ce(N03)3·6H2 O，反应2 h，加入0.25 g NH3·OH，反应2 h后，自然冷却；
产物离心，分别用水和乙醇洗涤2次；产物放置在恒温干燥箱中干燥6 h，最后将样品在马弗炉中500℃下煅烧2 h，制得氧化铈空心微球。
所述的过硫酸钾提前溶解于10 mL水。
所述的NH3·OH提前溶解于20 mL水中。
本发明的技术效果在于：
本发明通过聚合物模板法制备了氧化铈空心微球，实验结果表明，制备的CeO2空心微球的球径约为220 nm，壳层厚度约为20 nm。氧化铈空心微球粒径均匀，单分散。可见光条件下，光催化降解RhB的实验表明氧化铈空心微球具有优异的光催化性能。
具体实施方式
氧化铈空心微球的制备方法，包括如下步骤：
（1）PS模板的制备：
称取10 g苯乙烯单体，100 g水，加入250 mL三口烧瓶中，室温通入氮气30 min，搅拌，升温到70℃，加入0.1 g过硫酸钾，保持温度，共计10 h，之后冷却;制备胶体溶液离心分离，超声分散于水中，制得5％的PS微球模板;
（2）氧化铈空心微球的制备：
称取40 g PS微球模板溶液，25 mL水，加人三口烧瓶中，超声10 min，然后搅拌，升温到60℃，加入0.434 g Ce(N03)3·6H2 O，反应2 h，加入0.25 g NH3·OH，反应2 h后，自然冷却；
产物离心，分别用水和乙醇洗涤2次；产物放置在恒温干燥箱中干燥6 h，最后将样品在马弗炉中500℃下煅烧2 h，制得氧化铈空心微球。
所述的过硫酸钾提前溶解于10 mL水。
所述的NH3·OH提前溶解于20 mL水中。
Claims (3)
1.氧化铈空心微球的制备方法，其特征在于：包括如下步骤：
（1）PS模板的制备：
称取10 g苯乙烯单体，100 g水，加入250 mL三口烧瓶中，室温通入氮气30 min，搅拌，升温到70℃，加入0.1 g过硫酸钾，保持温度，共计10 h，之后冷却;制备胶体溶液离心分离，超声分散于水中，制得5％的PS微球模板;
（2）氧化铈空心微球的制备：
称取40 g PS微球模板溶液，25 mL水，加人三口烧瓶中，超声10 min，然后搅拌，升温到60℃，加入0.434 g Ce(N03)3·6H2 O，反应2 h，加入0.25 g NH3·OH，反应2 h后，自然冷却；
产物离心，分别用水和乙醇洗涤2次；产物放置在恒温干燥箱中干燥6 h，最后将样品在马弗炉中500℃下煅烧2 h，制得氧化铈空心微球。
2.根据权利要求1所述的氧化铈空心微球的制备方法，其特征在于：所述的过硫酸钾提前溶解于10 mL水。
3.根据权利要求1所述的氧化铈空心微球的制备方法，其特征在于：所述的NH3·OH提前溶解于20 mL水中。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108722391A (zh) * | 2018-06-04 | 2018-11-02 | 中国科学院海洋研究所 | 一种3D C/CeO2空心纳米结构框架材料及其制备方法与应用 |
| CN111662714A (zh) * | 2020-06-08 | 2020-09-15 | 苏州麦茂思传感技术有限公司 | 一种颗粒均一的红色荧光粉及其制备方法 |
| CN112371127A (zh) * | 2020-11-17 | 2021-02-19 | 惠州学院 | 一种具有摇铃结构钴酸盐纳米复合材料的制备方法及其在催化氨硼烷水解产氢上的应用 |
| CN112919522A (zh) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | 一种氧化铈材料及其制备方法与应用 |
-
2016
- 2016-11-18 CN CN201611015044.7A patent/CN106495203A/zh active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108722391A (zh) * | 2018-06-04 | 2018-11-02 | 中国科学院海洋研究所 | 一种3D C/CeO2空心纳米结构框架材料及其制备方法与应用 |
| CN112919522A (zh) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | 一种氧化铈材料及其制备方法与应用 |
| CN111662714A (zh) * | 2020-06-08 | 2020-09-15 | 苏州麦茂思传感技术有限公司 | 一种颗粒均一的红色荧光粉及其制备方法 |
| CN112371127A (zh) * | 2020-11-17 | 2021-02-19 | 惠州学院 | 一种具有摇铃结构钴酸盐纳米复合材料的制备方法及其在催化氨硼烷水解产氢上的应用 |
| CN112371127B (zh) * | 2020-11-17 | 2023-07-14 | 惠州学院 | 一种具有摇铃结构钴酸盐纳米复合材料的制备方法及其在催化氨硼烷水解产氢上的应用 |
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