CN111054349A - 一种黑色多孔氧化锌光催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:将硝酸钴和2‑甲基咪唑分别溶于有机溶剂中,再混合搅拌后加入水热反应釜中,并置于烘箱中保温处理后,经洗涤、干燥后制得ZIF‑8前驱体;将ZIF‑8前驱体置于高温炉中,保温得到白色多孔ZnO粉末;将白色多孔ZnO粉末在还原气氛条件下,经退火处理后制得黑色多孔氧化锌光催化剂。本发明以金属有机骨架化合物为前驱体,制备出具有高可见光响应的黑色多孔ZnO用于光催化污染物降解,本发明在制备过程中不涉及有毒有害试剂,原料成本低,能够满足工业批量生产的要求。
Description
技术领域
本发明涉及光催化剂制备技术领域,尤其涉及一种黑色多孔氧化锌光催化剂的制备方法。
背景技术
20世纪以来,科学技术的快速发展给人们生活带来舒适和便利的同时,也导致能源短缺和环境恶化。从上世纪震惊世界的“八大危害”到近年来发现的全球变暖、臭氧层破坏和生物多样性丧失,环境污染的潜在影响远远大于此,这严重威胁着人类的继续繁衍和生存。因此,控制污染,保护环境,实现可持续发展,是全人类的共同愿望。光催化降解水中污染物是一种新型水处理技术,是从20世纪70年代在治理环境污染这一背景下逐步发展起来的一种新型环保技术。光催化技术利用半导体光催化材料在光照下被激活的表面特性,去除有毒有害物分子;同时具有工艺简单、催化活性高、可在室温下发生反应,为解决环境污染问题提供了一条有效途径,在能源和环境领域有着重要应用前景。
ZnO作为重要的半导体光催化剂,具有无毒性、高效性和价格低廉等优点得到广泛研究。但是ZnO禁带宽度较宽,为3.3eV,因此仅能吸收利用太阳光中波长小于400nm的紫外光部分,而且光生电子和空穴较容易复合,表现出较低的光催化活性,不能满足实际应用要求。对ZnO进行改性能够提高其对可见光的利用率及光催化活性,包括贵金属(Au、Ag、Pt等)负载,金属或非金属掺杂以及形貌控制,都被证明能有效提高氧化锌的光催化效率和活性。因此,研究纳米氧化锌光催化剂的晶格结构以及形态的可控合成对开发新型高效光催化体系具有重要意义。
目前,虽然纳米氧化锌光催化剂的制备方法很多,但是能够在可见光下的工作很少。因此,开发一种廉价、环保、高效、可见光驱动的ZnO光催化剂迫在眉睫。经调研国内外有关ZnO光催化材料的相关文献报道和专利发现,目前还没有关于黑色多孔ZnO纳米材料的制备方法及在光催化领域的应用报道。
发明内容
基于背景技术存在的问题,本发明提出一种黑色多孔氧化锌光催化剂的制备方法。以金属有机骨架化合物为前驱体,制备出具有高可见光响应的黑色多孔ZnO用于光催化污染物降解,本发明在制备过程中不涉及有毒有害试剂,原料成本低,能满足工业批量生产的要求。
本发明提出一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:
S1、将硝酸钴和2-甲基咪唑分别溶于有机溶剂中,再混合搅拌后加入水热反应釜中,置于100-120℃烘箱中保温10-14h,经洗涤、干燥后制得ZIF-8前驱体;
S2、将ZIF-8前驱体置于高温炉中,控制升温的速度,加热至600℃-650℃,保温2-4小时,得到白色多孔ZnO粉末;
S3、将白色多孔ZnO粉末装入刚玉方舟中后,再置于高温炉中,在还原气氛条件下,经退火处理后,制得黑色多孔氧化锌光催化剂。
优选地,S1中硝酸钴和2-甲基咪唑的摩尔比为1:4。
优选地,S1中搅拌时间为10-15min。
优选地,S1中有机溶剂为有机醇类,优选为甲醇。
优选地,S2中升温的速度为5-15℃/min。
优选地,S3中保护气氛为H2和Ar的共混气体,其中H2的含量不低于10%。
优选地,S3中退火处理温度为350-450℃。
优选地,S3中退火处理时间度为2-3h。
本发明提出一种具有高光催化降解活性的黑色多孔氧化锌光催化剂的简单制备方法,以金属有机骨架化合物ZIF-8为前驱体,先在空气中高温煅烧制备白色多孔氧化锌,然后在还原气氛下,通过热处理制备黑色多孔氧化锌光催化剂。在氧化锌晶格中引入氧缺陷,使氧化锌的带隙宽度变窄,同时多孔结构有利于光在孔内散射,从而增强其对可见光的吸收。催化剂在可见光辐照下产生大量的活性自由基,使得黑色多孔氧化锌可以高效地去除水体有机污染物。本发明所得氧化锌产品为深黑色,产物粒径均匀,在紫外-可见-近红外光区间内有很强的吸收,同时制备工艺简单,可大规模工业化生产。
本发明有益效果:
1、制备过程中使用的原料具有较低的生物毒性和环境毒性;
2、合成工艺简单,可由工业设备大量制备;
3、所得的多孔结构有利于光线在空隙内部的多重散射,提高了催化剂的吸光度;
4、黑色氧化锌对可见光有很强的吸收,能够有效的利用可见光进行催化反应。
附图说明
图1为实施例1所制备的金属有机骨架化合物ZIF-8前驱体的SEM照片;
图2为实施例1所制备的黑色多孔ZnO的SEM照片;
图3为实施例1所制备的白色多孔ZnO和黑色多孔ZnO的样品照片;
图4为实施例1所制备的黑色多孔ZnO粉末的吸光谱;
图5为实施例1所制备的黑色多孔ZnO的电子顺磁共振谱;
图6为实施例1所制备的黑色多孔ZnO的在可见光照射下对水体中甲基橙染料的降解效率测试。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:
S1、将0.89克的硝酸钴溶于30mL甲醇中,0.98克2-甲基咪唑溶于10mL 甲醇中,再混合搅拌10min后,加入水热反应釜中,置于100℃烘箱中保温12h,经用水和乙醇各洗涤3次后,在60℃真空干燥后制得ZIF-8前驱体;
S2、将0.1克ZIF-8前驱体置于马弗炉中,以10℃/min的升温速度加热至 600℃,保温3小时后停止加热,待炉内温度降低至室温时,得到白色多孔ZnO 粉末;
S3、将0.1克白色多孔ZnO粉末装入刚玉方舟中后,再置于高温管式炉中,在H2/Ar(10%/90%)气氛条件下,在温度400℃退火处理2h后,待炉内温度降低至室温制得黑色多孔氧化锌光催化剂。
实施例2
一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:
S1、将1.78克的硝酸钴溶于30mL甲醇中,1.96克2-甲基咪唑溶于10mL 甲醇中,再混合搅拌15min后,加入水热反应釜中,置于120℃烘箱中保温12h,经用水和乙醇各洗涤3次后,在60℃真空干燥后制得ZIF-8前驱体;
S2、将0.1克ZIF-8前驱体置于马弗炉中,以8℃/min的升温速度加热至 600℃,保温4小时后停止加热,待炉内温度降低至室温时,得到白色多孔ZnO 粉末;
S3、将0.1克白色多孔ZnO粉末装入刚玉方舟中后,再置于高温管式炉中,在H2/Ar(20%/80%)气氛条件下,在温度400℃退火处理3h后,待炉内温度降低至室温制得黑色多孔氧化锌光催化剂。
实施例3
一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:
S1、将5.9克的硝酸钴溶于100mL甲醇中,7.8克2-甲基咪唑溶于50mL甲醇中,再混合搅拌15min后,加入水热反应釜中,置于120℃烘箱中保温10h,经用水和乙醇各洗涤3次后,在60℃真空干燥后制得ZIF-8前驱体;
S2、将ZIF-8前驱体置于马弗炉中,以5℃/min的升温速度加热至620℃,保温2-4小时,得到白色多孔ZnO粉末;
S3、将白色多孔ZnO粉末装入刚玉方舟中后,再置于高温管式炉中,在H2/Ar(25%/75%)下,在温度350℃退火处理2.5h后,待炉内温度降低至室温制得黑色多孔氧化锌光催化剂。
实施例4
一种黑色多孔氧化锌光催化剂的制备方法,包括如下步骤:
S1、将53.4克的硝酸钴溶于500mL甲醇中,58.8克2-甲基咪唑溶于200mL 甲醇中,再混合搅拌15min后,加入水热反应釜中,置于110℃烘箱中保温14h,经用水和乙醇各洗涤3次后,在60℃真空干燥后制得ZIF-8前驱体;
S2、将ZIF-8前驱体置于马弗炉中,以15℃/min的升温速度加热至630℃,保温2.5小时,得到白色多孔ZnO粉末;
S3、将白色多孔ZnO粉末装入刚玉方舟中后,再置于高温管式炉中,在H2/Ar(30%/70%)下,在温度450℃退火处理3h后,待炉内温度降低至室温制得黑色多孔氧化锌光催化剂。
图1为前驱体ZIF-8的扫描电镜图,证明了其正12面体的微观形貌,表面整洁无孔隙。图2为黑色多孔ZnO样品的扫描电镜图,证明了其正12面体的微观形貌在煅烧以及还原处理后依然保存完好,同时其表面布满了微小孔洞。图3 为制备得到的白色多孔ZnO以及黑色多孔ZnO样品的实物照片,在H2煅烧过程中引入氧空位之后,样品颜色变为黑色。图4为制备得到的黑色多孔ZnO样品的吸光谱,证实了其对紫外光,可见光以及红外光的强吸收。图5为制备得到的黑色多孔ZnO样品的顺磁波谱,证明其表面含有大量的氧空位。图6为制备得到的黑色多孔ZnO样品在可见光的照射下,处理模拟废水,水体中含有浓度为10ppm的甲基橙染料,1小时内脱除率为95.4%。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种黑色多孔氧化锌光催化剂的制备方法,其特征在于,包括如下步骤:
S1、将硝酸钴和2-甲基咪唑分别溶于有机溶剂中,再混合搅拌后加入水热反应釜中,置于100-120℃烘箱中保温10-14h,经洗涤、干燥后制得ZIF-8前驱体;
S2、将ZIF-8前驱体置于高温炉中,控制升温的速度,加热至600℃-650℃,保温2-4小时,得到白色多孔ZnO粉末;
S3、将白色多孔ZnO粉末装入刚玉方舟中后,再置于高温炉中,在还原气氛条件下,经退火处理后,制得黑色多孔氧化锌光催化剂。
2.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S1中硝酸钴和2-甲基咪唑的摩尔比为1:4。
3.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S1中搅拌时间为10-15min。
4.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S1中有机溶剂为有机醇类,优选为甲醇。
5.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S2中升温的速度为5-15℃/min。
6.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S3中保护气氛为H2和Ar的共混气体,其中H2的含量不低于10%。
7.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S3中退火处理温度为350-450℃。
8.根据权利要求1所述黑色多孔氧化锌光催化剂的制备方法,其特征在于,S3中退火处理时间度为2-3h。
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