CN106362750A - 一种Co/ZnO复合材料的制备方法 - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 229910052723 transition metal Inorganic materials 0.000 abstract description 7
- 150000003624 transition metals Chemical class 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 3
- 238000013329 compounding Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000011592 zinc chloride Substances 0.000 abstract 1
- 235000005074 zinc chloride Nutrition 0.000 abstract 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
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- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- 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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Abstract
一种Co/ZnO复合材料的制备方法,将53gZnCl2、2gCoCl2·6H2O和43gNaOH分别溶解于100mL的去离子水中,再将3种溶液于磁力搅拌条件下充分混合,20min后移入高压反应釜中,在105‑115℃下反应8‑10h后,将反应釜内产物用去离子水和无水乙醇各洗涤3次后离心处理,于70‑75℃真空干燥箱中干燥8‑10h,即得。本发明的有益效果是:合成工艺简单,反应条件温和,生产成本较低,可重复性好,过渡金属Co存在于ZnO的间隙、晶格或表面,可导致晶格缺陷,使空穴-电子对的复合几率降低,进而使得ZnO对光的吸收率增强,从而提高其光催化性能。
Description
技术领域
本发明涉及材料合成方法,具体的是一种Co /ZnO复合材料的制备方法。
背景技术
近年来,随着人们生活质量的提高对环境的要求也越来越高,但由于全球工业迅速发展,环境污染已日趋严重,其中水污染已成为威胁人类健康的重要问题 因此 如何有效地治理水污染就成为当今社会迫切需要解决的难题之一 。
纳米ZnO作为一种新型的n型半导体材料(Eg=3.37eV),因其具有较高的光催化活性,且易制备、无污染、价廉易得和独特的电学及光学性能以及特殊的结构等诸多优点而备受人们的青睐,其对废水中有机污染物有较好的光催化降解效果,是一种常用的光催化剂,但由于纯ZnO带隙较宽使得其只有在较短波长385nm的紫外光照条件下才具有较好的光催化活性,因而大大限制了ZnO作为光催化剂的工业应用。
目前可通过改性ZnO如掺杂金属或非金属离子以形成染料敏化或固熔体等方法,进而改变带隙并控制其能带结构,达到提高ZnO光催化活性的目的。李侠等采用金属离子掺杂的方法,分别制备了纳米CeZnO及纳米AgZnO,发现稀土离子Ce及过渡金属离子Ag的掺杂,均可显著提高纳米ZnO对亚甲基蓝的光催化降解效果。Kong等通过掺杂Ta5+进而提高了ZnO对苯的降解能力。余长林等采用水热处理结合焙烧的方法制备了Zr/ZnO,Al/ZnO及Zr-Al/ZnO,发现Zr Al单独掺杂及Zr- Al共掺均可较大程度的提高纳米ZnO对酸性橙的光催化,降解效果。
掺杂过渡金属离子可在ZnO中引入缺陷位,形成中间能带,进而扩大ZnO的光吸收范围,以提高其光催化活性,但对于过渡金属离子掺杂的纳米ZnO却鲜有报道。
发明内容
本发明所要解决的技术问题在于提供一种Co /ZnO复合材料的制备方法,提供一种新的合成方法。
本发明采用的合成方法,包括如下步骤:
将53gZnCl2、2gCoCl2·6H2O和43gNaOH分别溶解于100mL的去离子水中,再将3种溶液于磁力搅拌条件下充分混合,20min后移入高压反应釜中,在105-115℃下反应8-10h后,将反应釜内产物用去离子水和无水乙醇各洗涤3次后离心处理,于70-75℃真空干燥箱中干燥8-10h,即得。
本发明的有益效果是:合成工艺简单,反应条件温和,生产成本较低,可重复性好,过渡金属Co存在于ZnO的间隙、晶格或表面,可导致晶格缺陷,使空穴-电子对的复合几率降低,进而使得ZnO对光的吸收率增强,从而提高其光催化性能。
具体实施方式
以下结合实例进一步说明本发明的内容,由技术常识可知,本发明也可通过其它的不脱离本发明技术特征的方案来描述,因此所有在本发明范围内或等同本发明范围内的改变均被本发明包含。
实施例1:
将53gZnCl2、2gCoCl2·6H2O和43gNaOH分别溶解于100mL的去离子水中,再将3种溶液于磁力搅拌条件下充分混合,20min后移入高压反应釜中,在105℃下反应8h后,将反应釜内产物用去离子水和无水乙醇各洗涤3次后离心处理,于70℃真空干燥箱中干燥8h,即得。
实施例2:
将53gZnCl2、2gCoCl2·6H2O和43gNaOH分别溶解于100mL的去离子水中,再将3种溶液于磁力搅拌条件下充分混合,20min后移入高压反应釜中,在115℃下反应10h后,将反应釜内产物用去离子水和无水乙醇各洗涤3次后离心处理,于75℃真空干燥箱中干燥10h,即得。
通过实验,紫外光照射下纯ZnO可降解亚甲基蓝,当紫外光照射60min时,其降解率最高只能达到74.55%,说明纯ZnO对亚甲基蓝的光催化降解效果一般。当掺杂了过渡金属Co后,Co/ZnO复合材料在紫外光的照射下,随着时间的延长,其对亚甲基蓝的光催化降解效果明显提高,紫外光照射40min时,Co/ZnO复合材料对亚甲基蓝的降解率就达到了95.2%,随着紫外光照射时间的延长,其对亚甲基蓝的最高降解率可达到96.1%。由此证明,掺杂过渡金属Co可显著提高ZnO对亚甲基蓝的光催化降解能力。
掺杂过渡金属Co可有效提高ZnO对亚甲基蓝的光催化降解效果,原因是Zn离子半径(0.060nm)与Co离子半径(0.058nm)相近,过渡金属Co存在于ZnO的间隙、晶格或表面,可导致晶格缺陷,使空穴-电子对的复合几率降低,进而使得ZnO对光的吸收率增强,从而提高其光催化性能。
Claims (1)
1.一种Co/ZnO复合材料的制备方法,包括如下步骤:将53gZnCl2、2gCoCl2·6H2O和43gNaOH分别溶解于100mL的去离子水中,再将3种溶液于磁力搅拌条件下充分混合,20min后移入高压反应釜中,在105-115℃下反应8-10h后,将反应釜内产物用去离子水和无水乙醇各洗涤3次后离心处理,于70-75℃真空干燥箱中干燥8-10h,即得。
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102533261A (zh) * | 2011-11-29 | 2012-07-04 | 天津理工大学 | 一种基于Co掺杂ZnO的红光材料的制备方法及应用 |
CN103977806A (zh) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | 一种光催化降解材料Co掺杂纳米ZnO及其制备方法 |
CN105032434A (zh) * | 2015-06-01 | 2015-11-11 | 东南大学 | 铁磁性ZnO可见光催化剂的制备方法 |
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CN102533261A (zh) * | 2011-11-29 | 2012-07-04 | 天津理工大学 | 一种基于Co掺杂ZnO的红光材料的制备方法及应用 |
CN103977806A (zh) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | 一种光催化降解材料Co掺杂纳米ZnO及其制备方法 |
CN105032434A (zh) * | 2015-06-01 | 2015-11-11 | 东南大学 | 铁磁性ZnO可见光催化剂的制备方法 |
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