CN111036255A - 一种芦苇基SiC/C光催化产氢催化材料的制备方法及其应用 - Google Patents
一种芦苇基SiC/C光催化产氢催化材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明提供一种芦苇基SiC/C光催化产氢催化材料的制备方法及其应用，所述的制备方法包括以下步骤：将芦苇粉在空气氛围下预烧1~3h，放至室温，研磨，之后在氩气气氛保护下，于1300~1500℃煅烧1~2h，即得到芦苇基SiC/C光催化产氢催化材料。本发明充分利用芦苇中的碳和硅合成出了芦苇基SiC/C，可大幅度促进废弃芦苇的资源化利用。本发明的芦苇基光催化产氢材料包括洋葱状纳米碳和纤维状纳米碳化硅，其催化产氢效率高，且制备方法简单、无污染，原料价格低廉，生产成本低，便于推广应用。
Description
技术领域
本发明涉及一种光催化产氢催化剂的制备方法，具体涉及一种芦苇基SiC/C光催化产氢催化材料的制备方法及其应用。
背景技术
化石燃料的过度消费带来了严重能源危机和环境污染，寻找可再生能源替代化石燃料成为当今能源研究的主题。氢能作为一种高效清洁能源受到了越来越多国内外科研工作者的关注。利用太阳能进行光催化分解水制氢不仅原料丰富、环境友好无污染，而且过程中不会使用和产生有害物质，符合可持续发展的需求。
雄安新区的建立和未来高科技的建设为河北省绿色能源行业的发展带来了商机和挑战，为维护雄安新区白洋淀生态平衡，芦苇收割后作为农业废弃物的再利用及其高附加值产品开发引起了广泛的关注。芦苇是在水生或湿地，甚至在盐碱地和沙漠中生长的草类植物，在调节生态环境中起着重要作用。它可以从根部吸收土壤中的可溶性二氧化硅，并在纤维素微隔室内形成纳米结构的二氧化硅。与其他草类植物相比，芦苇的硅含量更高，并且具有纳米级排列的二氧化硅。
碳化硅（SiC）是有吸引力的第三代半导体材料，具有优异的热稳定性、生物相容性、较高的机械强度、优异的可见光吸收带隙，已被广泛应用于光分解水产氢等光催化应用中。但是，由于碳化硅高的光生载流子复合率及表面逆反应等因素造成其低的量子效率，所以目前碳化硅催化制氢的效率仍然不高。而且，目前大多数SiC的合成是通过碳粉与SiO2的反应获得的，生产成本较高、价格昂贵。因此，开发一种催化制氢效率高，且生产成本较低的碳化硅光催化材料十分重要。
发明内容
本发明的目的就是提供一种芦苇基SiC/C光催化产氢催化材料的制备方法，以解决现有碳化硅催化材料催化制氢效率低，生产成本高的问题。
一种芦苇基SiC/C光催化产氢催化材料的制备方法，包括以下步骤制备：将芦苇粉在空气氛围下预烧1~3h，放至室温，研磨，之后在氩气气氛保护下，于1300~1500℃煅烧1~2h，即得到芦苇基SiC/C光催化产氢催化材料。
所述预烧温度为400~600℃，预烧在马弗炉中进行。
所述煅烧是在管式炉中进行，优选的煅烧温度为1400℃。
所述芦苇基SiC/C光催化产氢催化材料在光催化水产氢中的应用，包括如下步骤：将所述芦苇基SiC/C光催化产氢催化材料置于光反应器中，加入光敏剂、牺牲剂和去离子水，氙灯光照即可。
本发明充分利用芦苇中的碳和硅合成出了芦苇基SiC/C，可大幅度促进废弃芦苇的资源化利用。本发明的芦苇基SiC/C光催化产氢催化材料包括洋葱状纳米碳和纤维状纳米碳化硅，其制备原料单一、催化产氢效率高，且制备方法简单、无污染，生产成本低，便于推广应用，实现了对芦苇的资源化利用和芦苇基高附加值产品的开发。
附图说明
图1为实施例1所得芦苇基SiC/C光催化产氢催化材料的SEM图。
图2为实施例1所得芦苇基SiC/C光催化产氢催化材料的XRD图。
图3为实施例1所得芦苇基SiC/C光催化产氢催化材料中洋葱状纳米碳的HRTEM图。
图4为实施例1所得芦苇基SiC/C光催化产氢催化材料的EDS图。
图5为实施例1所得芦苇基SiC/C光催化产氢催化材料的Mapping图。
图6为时间-光催化析氢量折线图，图中：500℃ AC表示500℃预烧后得到的芦苇基活性炭，1300℃ SiC/C表示1300℃煅烧得到的 SiC/C材料（实施例2），1350℃ SiC/C表示1350℃煅烧得到的 SiC/C材料（实施例3），1400℃ SiC/C表示1400℃煅烧得到的 SiC/C材料（实施例1），1450℃ SiC/C表示1450℃煅烧得到的 SiC/C材料（实施例4），1500℃ SiC/C表示1500℃煅烧得到的 SiC/C材料（实施例5），C表示对比例1制得的芦苇基C，SiC表示对比例2制得的芦苇基SiC。
具体实施方式
下面结合实施例对本发明做进一步的阐述，在下述实施例中未详细描述的过程和方法是本领域公知的常规方法，实施例中所用原料或试剂除另有说明外均为市售品，可通过商业渠道购得。
实施例1：芦苇基SiC/C光催化产氢催化材料的制备
将10g芦苇粉（芦苇整棵粉碎，无所谓颗粒大小）在空气氛围下在马弗炉中于400℃预烧1~3h，得到芦苇基活性炭（AC），取出放至室温，研磨均匀，之后将其置于管式炉中在氩气气氛保护下，于1400℃煅烧1~2h，得到2g芦苇基SiC/C光催化产氢催化材料。
对所得光催化材料进行结构表征，结果见图1~5。从图1中可以看出，纤维状结构为纳米SiC，其余结构为C。图2可以看到所得材料具有SiC的（111）、（200）、（220）和（311）晶面以及前面石墨化的碳峰，说明了成功制备SiC/C。从图3中的HRTEM图中可以看出，形成了洋葱状纳米碳。从图4、5中的EDS（能谱图）与Mapping（元素分布图）中可以看出，得到的产物是由C、O、Si元素组成，说明成功制备了SiC/C，表面有少量的O元素。
实施例2：
预烧温度为500℃，煅烧温度为1300℃，其它条件同实施例1。
实施例3：
预烧温度为600℃，煅烧温度为1350℃，其它条件同实施例1。
实施例4：
预烧温度为600℃，煅烧温度为1450℃，其它条件同实施例1。
实施例5：
预烧温度为600℃，煅烧温度为1500℃，其它条件同实施例1。
对比例1：芦苇基C的制备
将10g芦苇粉在空气氛围下在马弗炉中于400℃预烧1~3h，将预烧后的产物用HF浸泡24h，除去SiO2，再在1400℃下高温煅烧2h，得到1.5g芦苇基C。
对比例2：芦苇基SiC的制备
将实施例1得到的芦苇基SiC/C光催化产氢催化材料在空气氛围下于700℃煅烧6h，得到0.2g芦苇基SiC。
光催化水产氢实验：
分别称取40mg实施例1-5和对比例1-2所制备的产物，分别置于光反应器中，并分别向光反应器中加入光敏剂（酸性红）10-20 mg，牺牲剂（三乙醇胺）5-10mL，去离子水70-75mL，氙灯(带滤光片，模拟可见光)光照一定时间，再利用气相分析仪进行气体分析。结果如图6所示。
由图6可知，随着光照时间的增加，氢气产生量不断增多，且在1400℃煅烧得到的SiC/C材料下产生的氢气量高于其他煅烧温度所得SiC/C材料的产氢量，1400℃煅烧得到的SiC/C的最大析氢速率为22.54μmol/h，相较于其他温度，在1400℃下可以产生洋葱状纳米碳（如图3所示）和纤维状纳米SiC，使其具有更多的缺陷位点，因此具有更好的产氢效果。1300℃煅烧温度产生的C还未成为洋葱状纳米碳（见图2, 2θ= 26°为洋葱状纳米碳特征峰）；而1500℃煅烧温度产生的纤维状纳米SiC减少。
通过对比1400℃煅烧得到的C、SiC/C与SiC的光催化析氢量， SiC/C作为光催化剂的产氢量最高，是洋葱状纳米碳和纤维状纳米SiC协同效应的结果。可见，在1400℃高温下煅烧得到的芦苇基SiC/C材料作为光催化产氢的催化剂，具有优秀的催化效率，且其来源于农业废弃物，原料价格低廉，操作简单，便于实用推广。
Claims (6)
1.一种芦苇基SiC/C光催化产氢催化材料的制备方法，其特征在于，包括如下步骤：先将芦苇粉在空气氛围下预烧，放至室温、研磨，之后在氩气气氛保护下，于1300~1500℃煅烧，即得到芦苇基SiC/C光催化产氢催化材料。
2.根据权利要求1所述的芦苇基SiC/C光催化产氢催化材料的制备方法，其特征在于，所述预烧温度为400~600℃，预烧时间为1~3h。
3.根据权利要求1所述芦苇基SiC/C光催化产氢催化材料的制备方法，其特征在于，所述煅烧是在管式炉中进行，煅烧时间为1~2h。
4.根据权利要求1所述芦苇基SiC/C光催化产氢催化材料的制备方法，其特征在于，所述煅烧温度为1400℃。
5.一种由权利要求1~4中任一项所述制备方法制备得到的芦苇基SiC/C光催化产氢催化材料。
6.一种由权利要求1~4中任一项所述制备方法制备得到的芦苇基SiC/C光催化产氢催化材料在光催化水产氢中的应用。
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