CN108525665A - 一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法 - Google Patents
一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法 Download PDFInfo
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Abstract
一种介孔γ‑Fe2O3/TiO2磁/催化双功能复合微球的制备方法,涉及适用于环境污水修复方面复合材料制备技术领域。将氨基酸、钛酸四丁酯和二茂铁溶解于乙醇和水混合溶液中,搅拌混合均匀;然后将搅拌混合液转入反应釜中,将反应釜盖好并放到恒温鼓风烘箱中进行反应,反应完全后经后处理得到灰白色的介孔γ‑Fe2O3/TiO2磁/催化双功能复合微球。本发明通过氨基酸辅助溶剂热法成功地获得了一种介孔γ‑Fe2O3/TiO2磁/催化双功能复合微球。通过系列实验结果表明其具有粒度分布较窄、形貌分布均一和粒径可控等特点。
Description
技术领域
本发明涉及适用于环境污水修复方面复合材料制备技术领域,具体是涉及一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法。
背景技术
目前,TiO2由于其强氧化性、化学稳定性好、无毒和廉价等优点在环境和能源相关的领域有着重要的应用前景。特别是在光催化、太阳能电池、传感器等方面。
TiO2晶体结构主要有锐钛矿、金红石和板钛矿,其中锐铁矿和金红石相,其中,锐钛矿和金红石相的TiO2禁带宽度(Eg)分别为3.2eV和3.0eV,能隙大吸收紫外光能力强,其光生电子的还原性和空穴的氧化性强,能够实现分解水产氨产氧,广泛应用于水纯化,废水处理,有毒污水控制,空气净化和杀菌消毒等领域。为了提高TiO2的可见光催化活性,通过对TiO2进行改性来提高其电子-空穴转移速率及拓宽其可见光光响应范围,增加对可见光的利用率。
纳米γ-Fe2O3具有无毒、廉价、无污染、强磁性等优点,在吸附、催化、生物医疗、磁制冷、磁记录等领域有着广泛的应用。
介孔TiO2粉体因其具有高比表面积、孔径可调和易于改性等特点,在水处理、空气净化、太阳能电池和生物材料等方面表现出广阔潜在的应用前景。将介孔TiO2粉体和磁性γ-Fe2O3结合起来能够有效的解决此类催化剂的回收问题。但是关于通过一步法技术合成介孔γ-Fe2O3/TiO2磁/催化双功能材料的报道较少。
发明内容
本发明要解决的技术问题为提供一种工艺简单、成本低、适合工业化规模生产的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法。
为了实现上述目的,本发明所采用的技术方案为:一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法,采用溶剂热法,具体是将氨基酸、钛酸四丁酯和二茂铁溶解于乙醇和水混合溶液中,搅拌混合均匀;然后将搅拌混合液转入反应釜中,将反应釜盖好并放到恒温鼓风烘箱中进行反应,反应完全后经后处理得到灰白色的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球。
作为本发明的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法的优选技术方案,制备方法中,氨基酸选自甘氨酸或L-天冬氨酸。氨基酸、钛酸四丁酯和二茂铁之间的摩尔比为5~15:8~9.5:2~0.5。溶剂热法反应温度为140~180℃,反应时间为12~48h。后处理是将反应产物固液分离后分别使用无水乙醇及去离子水交替洗涤,然后置于恒温干燥箱中进行干燥,恒温干燥箱中干燥温度为20~60℃,干燥时间为4~12h。
本发明通过氨基酸辅助溶剂热法成功地获得了一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球。通过系列实验结果表明其具有粒度分布较窄、形貌分布均一和粒径可控等特点。与现有技术相比,本发明具有以下优点:
1)、本发明工艺简单,整个制备体系容易构建、操作简便、条件易控、成本低廉、产物组成易控、产物分布均匀、不易团聚、适合于大规模工业生产。
2)、本发明是采用常规可溶性钛酸四丁酯作为反应物,在制备过程中不添加其它的辅助物质,产生的副产物少,对环境污染较小,是一种环保型合成工艺。
3)、本发明制备的产物具有良好的催化活性,能用在环境污染修复和新能源材料等方面。
附图说明
以下结合实施例和附图对本发明的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的简易合成方法作出进一步的详述。
图1是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像)。
图2是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的XRD图。
图3是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的BET图。
图4是实施例2制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的场发射扫描电镜(FE-SEM)图。
图5是实施例3制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的场发射扫描电镜(FE-SEM)图。
具体实施方式
实施例1
介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备
(1)首先量取3.060g的钛酸四丁酯滴入50mL烧杯中,然后量取10mL乙醇倒入该烧杯中,将此烧杯放入到超声波清洗器中超声5min,形成溶液A;接着称取0.187g的二茂铁、0.751g的甘氨酸倒入此烧杯中,加入5mL水,形成溶液B;最后把溶液B放在磁力搅拌器进行搅拌,搅拌1h形成混合液C。
(2)将混合液C转入事先洗好的25mL反应釜中,然后将反应釜盖好放到恒温鼓风干燥箱中,设置温度为180℃,设置反应时间36h;待反应结束后,取出反应釜,将反应后生成的产物用离心机离心,并分别用无水乙醇和去离子水交替洗涤数次,将洗涤后的产物放到恒温干燥箱中,设置温度为40℃,干燥6h得到粉末。
图1是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像)。在低倍镜下,由图1a可知,产物形貌较好,是由类似于球状的颗粒组成,分散性较好,且大小不一样,平均粒径为200-500nm左右,这些颗粒分布不是很均匀,一部分可能是TiO2纳米粒子,另外一部分可能是生成的磁载体粒子γ-Fe2O3;由图1b可知,在高倍镜下,颗粒呈很规则的球状结构,且表面比较粗糙。
图2是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的XRD图。与标准PDF卡片JCPDS(PDF39-1346)和JCPDS(PDF65-2448)对比可知,该产品是由TiO2和γ-Fe2O3组成。在2θ为14.958°、18.834°、23.771°、35.630°出现的是γ-Fe2O3的峰,对应的晶面指数是(110)、(111)、(210)、(311);其他的则归属于TiO2的衍射峰。
图3是实施例1制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的BET图。由图3可知,当相对压力P/P0从0增长到0.6时,吸附量增加缓慢;相对压力P/P0从0.6增长到0.8时,吸附量增加速度变大;相对压力P/P0从0.8增长到1时,吸附量增加速度又变小。该复合粉体的比表面积为222.906m2/g,非常大,因此吸附量非常大,由上面的吸附脱附等温曲线也可以知道,根据BJH吸附可知,孔体积为0.416cc/g,孔半径为38.932nm,根据该吸附等温曲线的特点可判断它为IV型吸附等温线,该产物属于介孔材料。
实施例2
介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备
(1)首先量取6.460g的钛酸四丁酯滴入50mL烧杯中,然后量取10mL乙醇倒入该烧杯中,将此烧杯放入到超声波清洗器中超声5min,形成溶液A;接着称取0.748g的二茂铁、0.751g的甘氨酸倒入此烧杯中,加入5mL水,形成溶液B;最后把溶液B放在磁力搅拌器进行搅拌,搅拌1h形成混合液C。
(2)将混合液C转入事先洗好的25mL反应釜中,然后将反应釜盖好放到恒温鼓风干燥箱中,设置温度为160℃,设置反应时间12h;待反应结束后,取出反应釜,将反应后生成的产物用离心机离心,并分别用无水乙醇和去离子水交替洗涤数次,将洗涤后的产物放到恒温干燥箱中,设置温度为20℃,干燥12h得到粉末。
图4是实施例2制备的介孔γ-Fe2O3/TiO2复合球状粉体的场发射扫描电镜(FE-SEM)图。由图可知,产物形貌较好,是由类似于球状的颗粒组成,分散性较好,且大小不一样,平均粒径为1-2μm。
实施例3
介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备
(1)首先量取1.700g的钛酸四丁酯滴入50mL烧杯中,然后量取10mL乙醇倒入该烧杯中,将此烧杯放入到超声波清洗器中超声5min,形成溶液A;接着称取0.561g的二茂铁、1.330g的L-天冬氨酸倒入此烧杯中,加入5mL水,形成溶液B;最后把溶液B放在磁力搅拌器进行搅拌,搅拌1h形成混合液C。
(2)将混合液C转入事先洗好的25mL反应釜中,然后将反应釜盖好放到恒温鼓风干燥箱中,设置温度为140℃,设置反应时间48h;待反应结束后,取出反应釜,将反应后生成的产物用离心机离心,并分别用无水乙醇和去离子水交替洗涤数次,将洗涤后的产物放到恒温干燥箱中,设置温度为60℃,干燥4h得到粉末。
图5是实施例3制备的介孔γ-Fe2O3/TiO2复合球状粉体的场发射扫描电镜(FE-SEM)图。由图可知,产物形貌较好,是由类似于球状的颗粒组成,分散性较好,且大小不一样,平均粒径为0.5-1μm。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (6)
1.一种介孔γ-Fe2O3/TiO2磁/催化双功能复合微球的制备方法,采用溶剂热法,其特征在于,将氨基酸、钛酸四丁酯和二茂铁溶解于乙醇和水混合溶液中,搅拌混合均匀;然后将搅拌混合液转入反应釜中,将反应釜盖好并放到恒温鼓风烘箱中进行反应,反应完全后经后处理得到灰白色的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球。
2.如权利要求1所述的制备方法,其特征在于,氨基酸选自甘氨酸或L-天冬氨酸。
3.如权利要求1或2所述的制备方法,其特征在于,氨基酸、钛酸四丁酯和二茂铁之间的摩尔比为5~15:8~9.5:2~0.5。
4.如权利要求1所述的制备方法,其特征在于,溶剂热法反应温度为140~180℃,反应时间为12~48h。
5.如权利要求1所述的制备方法,其特征在于,后处理是将反应产物固液分离后分别使用无水乙醇及去离子水交替洗涤,然后置于恒温干燥箱中进行干燥,恒温干燥箱中干燥温度为20~60℃,干燥时间为4~12h。
6.一种如权利要求1~5任一项所述方法制备的介孔γ-Fe2O3/TiO2磁/催化双功能复合微球,其特征在于,复合微球的平均粒径为200-2000nm,比表面积为222.906m2/g,孔体积为0.416cc/g,孔半径为38.932nm。
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