CN106475039B - 一种海胆状三维Fe3O4/SnO2纳米棒阵列及其合成方法与应用 - Google Patents
一种海胆状三维Fe3O4/SnO2纳米棒阵列及其合成方法与应用 Download PDFInfo
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Abstract
本发明涉及一种海胆状三维Fe3O4/SnO2纳米棒阵列及其合成方法与应用,具体为本发明利用常见的四氧化三铁和四氯化锡为前驱体,通过简单的两步生长法,首次合成集吸附和光催化功能为一体的多功能海胆状三维Fe304/SnO2复合材料,并实现了对产品形貌的控制。与现有技术相比,本发明使用材料廉价易得,工艺简单,制备条件通用,产物形貌稳定,纯度高,且产物处理简单,适合中等规模工业生产。
Description
技术领域
本发明属于无机纳米材料技术领域,尤其是涉及一种海胆状三维Fe3O4/SnO2纳米棒阵列及其合成方法与应用。
背景技术
使用吸附剂对有机污染物和重金属离子进行吸附处理以及使用半导体为基的光催化材料对有机污染物进行光催化降解,是目前研究最多的技术。但是在应用于污水处理过程中时,难分离和回收的特性大大制约了它的广泛应用。光催化剂的磁分离技术是一个理想的解决方案。
二氧化锡作为一种宽禁带(Eg=3.6eV)的半导体材料,广泛应用于气敏、锂离子电池、催化、吸附等领域。由于二氧化锡优良的光电特性、化学稳定性和无毒性,它在光催化领域内的应用前景受到较多关注。
四氧化三铁由于其方便回收和分离,而广泛应用于污水处理领域。
目前文献中以四氧化三铁为基,与二氧化锡复合并形成三维海胆状结构鲜有报道,并且目前,将其用作吸附和光催化领域的报道也较少,吸附和光催化活性需要调整温度、pH等条件才能达到最优值。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种海胆状三维Fe3O4/SnO2纳米棒阵列及其合成方法与应用。
本发明的目的可以通过以下技术方案来实现:
技术方案一:海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法包括以下步骤:
(1)将四氧化三铁溶于四氯化锡水溶液中,超声,混合均匀后静置,然后用乙醇冲洗,并干燥;
(2)将(1)所得产品置于由SnCl·5H2O、碱和SDS组成的混合溶液中,超声分散至溶解完全,置于反应釜中水热反应,得到海胆状三维Fe3O4/SnO2纳米棒阵列。
步骤(1)所述的四氧化三铁为空心纳米球结构。
步骤(1)所述的四氧化三铁粒径在400nm以上,这样才能为二氧化锡晶种提供更多附着界面和生长空间。
步骤(1)中,所述的四氧化三铁和四氯化锡的摩尔比为(1~10):1。
步骤(1)中,静置时间在1~24h。
步骤(1)中,干燥温度在60~105℃,干燥时间在0.5~5h。
步骤(2)中,所述的SnCl4·5H2O、碱和SDS的摩尔比为1:(10~50):(1~10)。
步骤(2)所述的四氧化三铁与混合溶液中SDS的摩尔比为1:(1~10)。
步骤(2)所述的碱包括NaOH、KOH或NH4OH。
步骤(2)所述的水热反应温度在150~220℃,水热反应时间在15~36h。
技术方案二:提供上述制备方法得到的海胆状三维Fe3O4/SnO2纳米棒阵列。
技术方案三:提供上述制备方法得到的海胆状三维Fe3O4/SnO2纳米棒阵列用于污水处理中的应用。
所述的海胆状三维Fe3O4/SnO2纳米棒阵列用于对有机污染物吸附去除,或对有机污染物光催化降解。
与现有技术相比,本发明具有以下优点及有益效果:
1、本发明实现了以四氧化三铁空心纳米球为基体,通过晶种负载和外延生长的两步生长法制备了海胆状三维Fe3O4/SnO2纳米棒阵列。其次,将其用作污水处理。在对有机污染物吸附去除的过程中,发现其对210mg/L的高浓度刚果红溶液,吸附容量可达86.6mg/g,循环使用7次之后,吸附容量仍能保持在78mg/g。在对有机污染物光催化降解过程中,发现其对罗丹明B在4h光催化降解率达87%,循环使用7次后,光催化降解率仍能保持在79.8%。
2、本发明的方法对产物的形貌有很高的调控性。
3、本发明采用简单无机盐作为反应物,具有很强的通用性。
4、本发明制备的产物可以作为良好的污水处理材料,有较为广阔的发展前景和应用空间。
5、本发明的工艺简单,制备条件通用,产物形貌稳定、纯度高,且产物处理方便简洁,适合于中等规模工业生产。
6、本发明的方法具有条件温和、加热均匀、节能高效、易于控制等特点。
附图说明
图1为实施例1中在1um的倍数下得到的产物Fe3O4/SnO2的SEM照片。
图2为实施例1中在不同粒径(自上至下依次为 10~20nm,200~250nm,400~500nm)的四氧化三铁为基得到的产物Fe3O4/SnO2的 SEM照片。
图3为实施例1中在50nm的倍数下得到的底物Fe3O4的TEM照片。
图4为实施例1中在100nm的倍数下得到的产物Fe3O4/SnO2的TEM照片。
图5为实施例1中得到的底物Fe3O4和产物Fe3O4/SnO2的XRD图谱。
图6为实施例1所得底物Fe3O4和产物Fe3O4/SnO2的吸附脱附曲线和孔径分布图。
图7为实施例1所得底物Fe3O4和产物Fe3O4/SnO2的荧光谱图。
图8为实施例1所得底物Fe3O4和产物Fe3O4/SnO2的VSM图谱。
图9为实施例1所得产物Fe3O4/SnO2吸附刚果红溶液的紫外-可见光谱图。
图10为实施例1所得产物Fe3O4/SnO2光催化降解罗丹明B溶液的紫外-可见光谱图(图10a)和自制SnO2与Fe3O4/SnO2对于罗丹明B的光催化降解率曲线图 (图10b)。
图11为实施例1所得产物Fe3O4/SnO2循环使用7次吸附刚果红的吸附容量图 (图11a)和循环使用7次降解罗丹明B的降解率图(图11b)。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
实施例1
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由SnCl4·5H2O、NaOH和SDS的摩尔比为 1:20:4组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥 12h。所得产品的SEM如图1所示。用不同粒径的Fe3O4合成的Fe3O4/SnO2,产物如图2所示,本实施例所用底物Fe3O4的TEM和产物Fe3O4/SnO2的TEM如图3 和图4所示。
从图1~图4中可以看到此条件下合成的Fe3O4/SnO2是直径约为0.6~1um的海胆状三维结构的球体。从图5可以看出产物Fe3O4/SnO2确实为二者的复合材料。从图7可以看出,SnO2与Fe3O4复合之后,荧光强度变强,这可能是因为Fe3O4中的Fe3+充当了电子俘获中心,降低了电子-空穴的复合几率,这对于提升其光催化活性有着至关重要的作用。
从图6可以看出该材料的吸附等温线为IV型等温线,滞后环的出现是由于多孔吸附剂的毛细凝聚,H3型滞后环的出现是由于二氧化锡纳米棒的堆积导致在较高相对压力区域没有表现出吸附饱和。从图8可以看出Fe3O4/SnO2仍然具有顺磁性,饱和磁化强度在28emu/g,能够满足磁分离的要求(Ms需要大于1emu/g)。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
图9可以看出Fe3O4/SnO2对于210mg/L的刚果红溶液在前15min,去除率就能达到72%以上,吸附时间在120min,去除率可达81%以上,经计算,平衡吸附容量为86.6mg/g。图10可以看出Fe3O4/SnO2对于罗丹明B的光催化效果较佳。图 11可以看出,在循环使用7次之后,无论是作为吸附剂吸附刚果红,还是作为催化剂催化罗丹明B,Fe3O4/SnO2的循环使用性都较好。
实施例2
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由SnCl4·5H2O、KOH和SDS的摩尔比为1:20: 2组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥 12h。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
实施例3
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由由SnCl4·5H2O、NH4OH和SDS的摩尔比为1:25:1组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥12h。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
实施例4
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由SnCl4·5H2O、NaOH和SDS的摩尔比为 1:20:2组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥 12h。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
实施例5
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由SnCl4·5H2O、NH4OH和SDS的摩尔比为 1:20:2组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥 12h。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
实施例6
一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法如下:
第一步:称取0.2g粒径为500nm的Fe3O4置于50mL烧杯A中,加入 40mL0.005MSnCl·5H2O中,超声30min,混合均匀,静置12h,乙醇冲洗一次,85℃干燥1h。
第二步:将A中产品置于35mL由由SnCl4·5H2O、NaOH和SDS的摩尔比为 1:25:1组成的混合溶液中,超声分散至溶解完全,置于50mL反应釜中200℃反应 20h。
第三步:将上述产品用无水乙醇和去离子水交替洗涤数次,60℃下真空干燥 12h。
上述方法得到的Fe3O4/SnO2材料用于污水处理中。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于上述实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (6)
1.一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法,其特征在于,包括以下步骤:
(1)将四氧化三铁溶于四氯化锡水溶液中,超声,混合均匀后静置,然后用乙醇冲洗,并干燥;
(2)将步骤(1)所得产品置于由SnCl4∙5H2O、碱和SDS组成的混合溶液中,超声分散至溶解完全,置于反应釜中水热反应,得到海胆状三维Fe3O4/SnO2纳米棒阵列;
步骤(1)所述的四氧化三铁为空心纳米球结构,步骤(1)所述的四氧化三铁粒径在400nm以上,步骤(1)中,所述的四氧化三铁和四氯化锡的摩尔比为(1~10):1;
步骤(2)中,所述的SnCl4∙5H2O、碱和SDS的摩尔比为1:(10~50):(1~10)。
2.根据权利要求1所述的一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法,其特征在于,步骤(2)中,四氧化三铁与所述混合溶液中SDS的摩尔比为1:(1~10)。
3.根据权利要求1所述的一种海胆状三维Fe3O4/SnO2纳米棒阵列的合成方法,其特征在于,步骤(2)所述的水热反应中反应温度为150~220℃,步骤(2)所述的水热反应中反应时间为15~36h。
4.采用权利要求1-3任一所述的合成方法制得的海胆状三维Fe3O4/SnO2纳米棒阵列。
5.如权利要求4所述的海胆状三维Fe3O4/SnO2纳米棒阵列用于污水处理中的应用。
6.根据权利要求5所述的海胆状三维Fe3O4/SnO2纳米棒阵列用于污水处理中的应用,其特征在于,所述的海胆状三维Fe3O4/SnO2纳米棒阵列用于对有机污染物吸附去除,或对有机污染物光催化降解。
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