CN107262104A - 一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用 - Google Patents
一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用 Download PDFInfo
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Abstract
一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用,属于合成材料技术领域。所述方法如下:(1)配制硝酸铁、硝酸铋、硝酸铅和氧化石墨的混合液,超声处理,然后加入氢氧化钠及泡沫镍,继续搅拌待用;(2)在微波炉内进行微波辅助水热合成,反应结束,取出产物,清洗、干燥,得到铅、石墨烯掺杂铁酸铋与泡沫镍复合催化材料,可用于类Fenton和光催化反应体系处理难降解有机物废水,有效降低废水中的TOC含量。本发明在制备过程中采用微波辅助水热法一步、快速合成铁酸铋基复合催化材料,充分利用了微波的非热效应和原位生长能力强的优点,能够更快速高效地完成化学合成反应,制备时间大大缩短,并且操作简单、方便易行。
Description
技术领域
本发明属于合成材料技术领域,具体涉及一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用。
背景技术
铁酸铋(BiFeO3,BFO)是一种多铁性材料,最早成功合成于上世纪五十年代末,因其具有铁电性和反铁磁性,是当前多铁材料研究的热点之一。钙钛矿结构的铁酸铋晶体结构在室温下属于R3c空间群,其结构可以反相八面体倾斜,离子从对称中心分别沿[111]伪立方方向偏移。BFO既具有铁电性,又具有G型反铁磁性,其铁电居里温度为830℃,反铁磁奈尔温度为370℃,而且每一个[111]晶面自旋形成摆线,具有很大的饱和极化强度,饱和极化强度可达100µCcm-2。
石墨烯是目前自然界最薄、强度最高、导电导热性能最强的一种新型纳米材料,因其独特的性能,石墨烯作为"新材料之王"成为材料领域中新的宠儿。随着批量化生产以及大尺寸等难题的逐步突破,石墨烯的产业化应用步伐逐步加快,基于石墨烯复合材料是石墨烯应用领域中的重要研究方向,其在能量储存、液晶器件、电子器件、生物材料、传感材料和催化剂载体等领域展现出了优良性能,具有广阔的应用前景。作为催化剂的载体,石墨烯具有增大比表面积、改变催化剂的禁带宽度以及抑制激发电子-空穴复合等作用。这些作用都大大提高了催化剂的催化性能,并且在实际应用中有不可小觑的作用。
催化材料在实际应用中的研究重点是发展负载型催化材料,以提高反应过程中反应物与催化剂的接触面积,提高催化效率。载体的选择和催化剂的固定成为研发负载型催化剂的关键环节。泡沫镍具有比表面积大、多孔结构、可快速传热、导电的特点,是一种良好的载体选择。而催化材料的另一个限制因素是合成方法的选择,快速、高效的制备催化材料是研究的热点之一。
目前在合成材料中,传统的合成方法包括水热法、浸渍法、共沉淀法和溶胶凝胶法,这些方法都需要较长的合成时间,合成条件较为复杂,并且合成的催化剂效率不稳定,这些因素都限制了催化剂在实际生产中的应用。然而微波因其热效应与非热效应的共同作用可以大大缩短反应时间,简化合成步骤,同时提升合成材料的性能等优点被视为一种在加热过程中起着独一无二作用的新技术,更加难能可贵的是微波是一种绿色、无污染并且不会对环境造成二次污染的新型技术。因此,研发快速合成材料的新方法在实际生产中显得尤为重要。
目前关于泡沫镍的相关发明专利还没有,石墨烯复合材料种类较多,但大多都应用在化学化工、冶金、石油等领域(如:过渡金属硫化物/石墨烯复合材料及其合成方法和应用:201210254567.2;PbSe立方颗粒/石墨烯复合材料及其合成方法和应用:201310105877.2;Bi2Te3薄片/石墨烯复合材料及其合成方法和应用:201210254834.6),但是在环境领域用于处理难降解有机物的相关内容还未见报道。在合成方法上大多是水热合成法或溶胶凝胶法(如:锡基复杂氧化物/石墨烯复合材料及其合成方法和应用专利号:201210254843.5;钴基复杂氧化物/石墨烯复合材料及其合成方法和应用:201310032042.9;PbTe立方颗粒/石墨烯复合材料及其合成方法和应用:201210254645.9),但这些合成催化剂的方法均需要消耗很长时间,给实际应用带来困难。
发明内容
本发明的目的是为了解决现有复合催化材料的合成时间较长、合成效果不佳以及在环境领域应用较少的问题,提供了一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用。该方法可以快速合成性能良好、环境友好型的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料,原料来源广泛、廉价易得,合成方法快速简单、易于实现工业化,而且对环境没有污染。
为实现上述目的,本发明采取的技术方案如下:
一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,所述方法步骤如下:
一、铁酸铋基复合材料的预处理
取4~5 g硝酸铁、4~5 g硝酸铋、0.1~0.3 g硝酸铅、0.5~1.0 g氧化石墨及25~35 mL去离子水或超纯水混合在烧杯中,在25~30℃条件下超声处理15~ 30 min,然后加入3~5 g氢氧化钠继续搅拌20~30 min,随后添加1~2 g泡沫镍,最后将混合物移至聚四氟乙烯反应罐中待合成;
二、预处理铁酸铋基复合材料的微波快速合成
将聚四氟乙烯反应罐放置于微波炉中进行微波辅助水热合成,反应结束后取出聚四氟乙烯反应罐,清洗后将产物置于烘箱内烘干至恒重,得到铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料。
一种上述方法制备的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的应用,所述复合材料应用于类Fenton和光催化反应体系处理难降解有机物废水,有效去除有机污染物以及降低废水中的TOC含量。
本发明相对于现有技术的有益效果是:
1、本发明在合成过程中采用微波辐照技术对复合材料进行一步法快速合成,得到铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料,充分利用了微波的非热效应和热点效应的优点,反应在30 min内即完成合成过程,合成时间大大缩短,并且操作简单、方便易行。
2、本发明选用的氧化石墨由本申请人制备得到,已申请专利(CN106082197A)。
3、本发明合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料具有良好的催化性能,可以在微波强化类Fenton体系中,有效降解全氟辛酸废水。
4、本发明合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料同时还具有一定的光催化活性,在紫外光照射下,可以有效降解全氟辛酸废水。
5、本发明合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料对大肠杆菌也具有一定的抑制作用。
6、本发明合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料因合成方法简单、合成时间短,具有一定的实际应用价值,对处理废水有显著的效果。
7、本发明合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料具有可回收、重复利用等优点,可在实际废水处理中得到广泛应用。
8、本发明使用的原料来源广泛、廉价易得,制得的复合材料易于实现工业化,对环境没有污染。
附图说明
图1为实施例1中铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的SEM图;
图2为实施例1中铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的EDX图;
图3为实施例1中铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的XRD图;
图4为实施例1中铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料去除PFOA和TOC的效果图。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
具体实施方式一:本实施方式记载的是一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,所述方法步骤如下:
一、铁酸铋基复合材料的预处理
取4~5 g硝酸铁、4~5 g硝酸铋、0.1~0.3 g硝酸铅、0.5~1.0 g氧化石墨(粉末状)及25~35 mL去离子水或超纯水混合在烧杯中,在25~30℃条件下超声处理15~ 30 min,然后加入3~5 g氢氧化钠继续搅拌20~30 min,随后添加1~2 g泡沫镍,最后将混合物移至聚四氟乙烯反应罐中待合成;
二、预处理铁酸铋基复合材料的微波快速合成
将聚四氟乙烯反应罐放置于微波炉中进行微波辅助水热合成,反应结束后取出聚四氟乙烯反应罐,清洗后将产物置于烘箱内烘干至恒重,得到铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料。
具体实施方式二:具体实施方式一所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,步骤二中,微波反应温度为180~200oC,反应时间为20~40 min。
具体实施方式三:具体实施方式一所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,步骤二中,烘干温度为70~100℃,烘干时间2 h。
具体实施方式四:具体实施方式一所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,步骤二中,使用无水乙醇和去离子水进行离心清洗,离心转速为3500 rap/min,离心时间为5 min。
具体实施方式五:一种具体实施方式一所述方法制备的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的应用,所述复合材料应用于类Fenton和光催化反应体系处理难降解有机物废水,有效去除有机污染物以及降低废水中的TOC含量。
具体步骤为:在不改变初始溶液pH的条件下,室温下2 g/L的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料,在微波强化Fenton-like体系中降解全氟辛酸废水,反应6 min溶液即可降解90%以上。
实施例1:
本实施例以铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料作为催化剂,选择全氟辛酸作为目标污染物,具体技术方案如下:
一、先将4.84 g硝酸铋、4.04 g硝酸铁、0.2 g硝酸铅和0.07 g氧化石墨放入烧杯中,加入30 mL去离子水超声20 min,然后加入4 g氢氧化钠继续搅拌30 min,随后将1 g泡沫镍加入上述混合液中,然后移至聚四氟乙烯反应罐中待合成;
二、经过步骤一预处理,将聚四氟乙烯反应罐放置于微波炉中,反应在微波炉内进行,调节温度在185~195℃,反应时间控制在25~30 min,取出聚四氟乙烯反应罐,清洗后将产物置于烘箱内烘干至恒重,得到铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料。铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的形貌分析如图1所示、元素分析如图2所示、晶型分析如图3所示。
三、降解步骤:取0.2 g上述方法合成的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料置于500 mL的三口烧瓶中,加入100 mL的全氟辛酸溶液(PFOA,20 mg/L),不改变溶液的pH值,将三口烧瓶转入微波炉中,调整微波功率为150 W,加入1 mL过氧化氢,反应6 min,采用超高效液相色谱对PFOA进行检测分析。采用TOC分析仪对全氟辛酸溶液中的总碳进行检测。反应6 min后PFOA的去除率达到90%以上,TOC去除率达到60%。铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料去除PFOA和TOC的效果如图4所示。
本研究采用微波强化类Fenton工艺,通过对催化剂添加量、微波反应时间、微波反应温度、过氧化氢添加量以及PFOA的初始浓度进行研究,确定最佳工艺参数。同时发现铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料具有很好的吸波效果,以及催化性能。
Claims (5)
1.一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,其特征在于:所述方法步骤如下:
一、铁酸铋基复合材料的预处理
取4~5 g硝酸铁、4~5 g硝酸铋、0.1~0.3 g硝酸铅、0.5~1.0 g氧化石墨及25~35 mL去离子水或超纯水混合在烧杯中,在25~30℃条件下超声处理15~ 30 min,然后加入3~5 g氢氧化钠继续搅拌20~30 min,随后添加1~2 g泡沫镍,最后将混合物移至聚四氟乙烯反应罐中待合成;
二、预处理铁酸铋基复合材料的微波快速合成
将聚四氟乙烯反应罐放置于微波炉中进行微波辅助水热合成,反应结束后取出聚四氟乙烯反应罐,清洗后将产物置于烘箱内烘干至恒重,得到铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料。
2.根据权利要求1所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,其特征在于:步骤二中,微波反应温度为180~200oC,反应时间为20~40 min。
3.根据权利要求1所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,其特征在于:步骤二中,烘干温度为70~100℃,烘干时间2 h。
4.根据权利要求1所述的微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法,其特征在于:步骤二中,使用无水乙醇和去离子水进行离心清洗,离心转速为3500rap/min,离心时间为5 min。
5.一种权利要求1所述方法制备的铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的应用,其特征在于:所述复合材料应用于类Fenton和光催化反应体系处理难降解有机物废水,有效去除有机污染物以及降低废水中的TOC含量。
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