CN111036211A - 一种球形α-Fe2O3光催化剂及其制备和应用方法 - Google Patents
一种球形α-Fe2O3光催化剂及其制备和应用方法 Download PDFInfo
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Abstract
一种球形α‑Fe2O3光催化剂及其制备和应用方法,属于光催化剂技术领域,其中,所述球形α‑Fe2O3光催化剂颗粒尺寸为10~80nm,并且α‑Fe2O3的窄带宽度为1.7~2.2eV,具有很强的可见光吸收性能。采用化学中和沉淀—煅烧法制备α‑Fe2O3光催化剂,工艺简单,环境友好;经对该球形α‑Fe2O3光催化剂进行有机染料的降解应用,结果表面,本发明方法制备的球形α‑Fe2O3光催化剂对甲基橙有机染料的降解率为≥90%,对亚甲基蓝有机染料的降解率为≥90%。
Description
技术领域
本发明属于光催化剂技术领域,具体涉及一种球形α-Fe2O3光催化剂及其制备方法、应用方法。
背景技术
随着现代工业的不断发展,由有机染料分子引起的水污染已成为严重的环境问题之一。染料废水作为难处理的主要工业废水,具有色度高、有机物浓度高且成分复杂、含盐量高、水质水量变化大、毒性大等特点,排入天然水体的染料废水中含有大量未反应的原料中间体、副产物和残余染料,不仅会消耗水中的溶解氧,使水生生物大量死亡,一些苯胺、偶氮类的染料还具有强致癌性,严重危害人类健康。
光催化技术作为一种绿色高级氧化技术,与传统的难降解有机污染物处理技术相比,更加经济(无毒、成本低、能耗低)、高效(反应时间快、无二次污染、几乎可以去除所有难降解有机物),在环境污染治理和能源转化方面具有广阔的应用前景。目前,半导体氧化物的光催化降解已成为去除合成染料的有效方法。在可见光或紫外线的驱动下,催化剂表面会形成空穴和电子,并产生强氧化剂·OH,从而有效地将染料分解为无毒的二氧化碳和其他小分子。
自1972年Fujishima和Honda将二氧化钛用于光解水生成氢气以来,TiO2一直是光催化剂研究的热点,在其制备及其光催化性能的改善已经投入了大量的研究工作。然而由于TiO2的带隙相对较大(3.2eV),只能使用波长小于385nm的紫外光源,这样的能量仅占太阳光谱总能量的5%左右。因此,开发能够有效利用可见光能的带隙较小的光催化剂已成为一个重要的研究课题。
在众多半导体材料中,α-Fe2O3作为重要的n型金属氧化物半导体材料,具有性能稳定、天然丰度高、低成本合成、无二次污染等优良特性,在光解水、催化剂、气体传感、锂离子电池及生物医疗等方面具有广阔的发展应用前景。特别是其窄带宽度(1.7~2.2eV)能够充分的利用太阳光中的可见光部分,因此被认为是潜在的光催化材料。
然而,α-Fe2O3用作光催化剂时具有复合率高和空穴扩散长度(2~4nm)低的缺点,这限制了它的光催化活性。研究学者们通过合成具有不同形状和尺寸的α-Fe2O3纳米结构,掺杂不同的元素,利用贵金属负载和半导体复合,制备异质结构等方式,改善α-Fe2O3的光催化性能。
实际上,通过设计适当的方法并控制相应的过程以获得具有特定形貌和粒径的产物,提高单相α-Fe2O3的光催化性能不仅是一种经济有效的途径,还可以避免复杂的反应条件或使用昂贵的材料。
发明内容
针对现有技术不足,本发明通过设计适当的制备方法获得具有特定形貌和粒径的单相球形α-Fe2O3光催化剂,同时提供球形α-Fe2O3光催化剂在降解甲基橙或亚甲基蓝有机染料的应用及应用方法。
本发明的一种球形α-Fe2O3光催化剂,该球形α-Fe2O3光催化剂的颗粒尺寸为10~80nm;所述球形α-Fe2O3光催化剂的禁带宽度为1.7~2.2eV,具有强烈的可见光吸收性;所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料中应用。
上述球形α-Fe2O3光催化剂的制备方法,按照以下步骤进行:
(1)将水合氯化铁或硫酸铁的无机铁盐溶解于一定量的水中,形成铁离子浓度为0.05~0.2mol/L的溶液,在搅拌速度为100~500r/min的条件下升温加热至40~95℃;
(2)以1~5ml/min的速度向溶液中滴加浓度为0.5~4mol/L的氨水溶液,调节溶液的pH值为4.0~9.0后,继续搅拌0.5~3h;
(3)进行离心分离、洗涤、干燥,得到含铁的前驱体;
(4)将含铁的前驱体在300~600℃的温度下焙烧0.5~4h,得到球形,颗粒尺寸为10~80nm,禁带宽度为1.7~2.2eV的α-Fe2O3光催化剂。
上述球形α-Fe2O3光催化剂在降解甲基橙或亚甲基蓝有机染料的应用方法,按照以下步骤进行:
(1)将0.015~0.3g的球形α-Fe2O3光催化剂,在25℃下加入到一定量的甲基橙(MO)或亚甲基蓝(MB)的有机染料水溶液中,在搅拌速度为100~500r/min条件下搅拌10~120min,使有机染料与α-Fe2O3光催化剂达到吸附-解吸平衡;其中,甲基橙(MO)有机染料水溶液浓度为5~100mg/L,亚甲基蓝(MB)有机染料水溶液浓度为1~50mg/L;球形α-Fe2O3光催化剂与甲基橙或与亚甲基蓝的质量比为(20~267):1;
(2)向达到吸附-解吸平衡的甲基橙或亚甲基蓝溶液中加入0.05~5mL的30%过氧化氢(H2O2),并在紫外可见光照射下以100~500r/min的搅拌速度继续搅拌10~240min。
具体降解率计算方法为,在504nm或664nm处采用紫外分光光度计测定甲基橙或亚甲基蓝有机染料水溶液的浓度,根据式(1)计算光催化降解甲基橙有机染料或亚甲基蓝有机染料的降解率。
降解率=(1-Ct/C0)×100% (1)
其中,C0和Ct分别是溶液中甲基橙或亚甲基蓝有机染料的初始浓度和t时刻时的浓度。
本发明的优点及有益效果在于:
(1)α-Fe2O3是一种n型半导体材料,性能稳定,天然丰度高;
(2)采用化学中和沉淀—煅烧法制备α-Fe2O3光催化剂,工艺简单,环境友好;
(3)α-Fe2O3的窄带宽度为1.7~2.2eV,具有很强的可见光吸收性能,可有效降解甲基橙和亚甲基蓝有机染料;
(4)本发明方法制备的球形α-Fe2O3光催化剂在光催化下对甲基橙有机染料的降解率为≥90%,对亚甲基蓝有机染料的降解率为≥90%。
附图说明
图1本发明实施例1中制备的球形α-Fe2O3光催化剂的XRD分析谱图。
图2本发明实施例1中制备的球形α-Fe2O3光催化剂的SEM分析图。
具体实施方式
下面结合实施例对本发明作进一步的详细说明。
本发明实施例1~3中的球形α-Fe2O3光催化剂是通过采用X射线衍射分析仪(XRD,Rigaku-Smartlab,Japan with Cu Ka radiation)测定其物相结构;采用扫描电子显微镜(SEM,ZEISS-Sigma,Germany)观察其形貌,颗粒尺寸;在504nm或664nm处采用紫外分光光度计测定甲基橙或亚甲基蓝有机染料水溶液的浓度,根据本发明中公式(1)计算光催化降解甲基橙或亚甲基蓝有机染料的降解率。
实施例1
一种球形α-Fe2O3光催化剂,该球形α-Fe2O3光催化剂的颗粒尺寸为30~40nm,禁带宽度为1.93eV;所述的球形α-Fe2O3光催化剂,在可见光区具有强烈的光吸收;所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料中应用。
上述球形α-Fe2O3光催化剂的制备方法,具体操作步骤:
(1)将水合氯化铁溶解于一定量的水中,形成铁离子浓度为0.1mol/L的溶液。取150mL的溶液在搅拌速度为150r/min的条件下升温加热至65℃;
(2)以1ml/min的速度向溶液中滴加浓度为0.5mol/L的氨水溶液,调节溶液的pH值为9.0后,继续以150r/min搅拌速度搅拌1h;
(3)将溶液进行离心分离、洗涤、干燥,得到含铁的前驱体;
(4)将含铁的前驱体在400℃的马弗炉中焙烧2h,得到球形、颗粒尺寸为30~40nm,禁带宽度为1.93eV的α-Fe2O3光催化剂。
对所制备得到的球形α-Fe2O3光催化剂进行XRD物相结构的表征,结果如图1所示;另外SEM微观形貌的观察结果及颗粒尺寸测量结果如图2所示。
上述球形α-Fe2O3光催化剂在降解甲基橙或亚甲基蓝有机染料的应用方法,具体步骤如下:
(1)在25℃下向150mL浓度为20mg/L的甲基橙有机染料水溶液和150mL浓度为5mg/L的亚甲基蓝有机染料水溶液中各加入0.2g球形α-Fe2O3光催化剂,在搅拌速度为150r/min条件下使球形α-Fe2O3光催化剂吸附有机染料溶液20min,达到吸附-解吸平衡;
(2)向达到吸附-解吸平衡的甲基橙和亚甲基蓝有机染料水溶液中各加入1mL的30%过氧化氢(H2O2),在紫外可见光照射下以150r/min的搅拌速度继续搅拌180min。
对实施例1中的甲基橙和亚甲基蓝有机染料水溶液进行浓度测定,根据本发明中公式(1)计算球形α-Fe2O3光催化剂降解甲基橙和亚甲基蓝有机染料的降解率。计算结果为,本实施例1制备得到的球形α-Fe2O3光催化剂对甲基橙有机染料的降解率为99%,对亚甲基蓝有机染料的降解率为97%。
实施例2
一种球形α-Fe2O3光催化剂,该球形α-Fe2O3光催化剂的颗粒尺寸为30~40nm,禁带宽度为2.06eV;所述的球形α-Fe2O3光催化剂,在可见光区具有强烈的光吸收;所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料中应用。
上述球形α-Fe2O3光催化剂的制备方法,具体操作步骤:
(1)将硫酸铁溶解于一定量的水中,形成铁离子浓度为0.2mol/L的溶液。取150mL的溶液在搅拌速度为350r/min的条件下升温加热至40℃;
(2)以2ml/min的速度向溶液中滴加浓度为1.5mol/L的氨水溶液,调节溶液的pH值为8后,以350r/min搅拌速度继续搅拌1.5h;
(3)进行离心分离、洗涤、干燥后,得到含铁的前驱体;
(4)将含铁的前驱体在500℃的马弗炉中焙烧2.5h,得到球形、颗粒尺寸为30~40nm,禁带宽度为2.06eV的α-Fe2O3光催化剂。
上述球形α-Fe2O3光催化剂在降解甲基橙或亚甲基蓝有机染料的应用方法,具体步骤如下:
(1)在25℃下向200mL浓度为30mg/L的甲基橙有机染料水溶液和200mL浓度为18mg/L的亚甲基蓝有机染料水溶液中各加入0.3g球形α-Fe2O3光催化剂,在搅拌速度为250r/min条件下使球形α-Fe2O3光催化剂吸附有机染料溶液80min,达到吸附-解吸平衡;
(2)向达到吸附-解吸平衡的甲基橙和亚甲基蓝有机染料水溶液中各加入1.5mL的30%过氧化氢(H2O2),在紫外可见光照射下以250r/min的搅拌速度继续搅拌150min。
对实施例2中的甲基橙和亚甲基蓝有机染料水溶液进行浓度测定,根据本发明中公式(1)计算球形α-Fe2O3光催化剂降解甲基橙和亚甲基蓝有机染料的降解率。计算结果为,本实施例2制备得到的球形α-Fe2O3光催化剂对甲基橙有机染料的降解率为98%,对亚甲基蓝有机染料的降解率为95%。
实施例3
一种球形α-Fe2O3光催化剂,该球形α-Fe2O3光催化剂的颗粒尺寸为50~60nm,禁带宽度为1.88eV;所述的球形α-Fe2O3光催化剂,在可见光区具有强烈的光吸收;所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料中应用。
上述球形α-Fe2O3光催化剂的制备方法,具体操作步骤:
(1)将水合氯化铁溶解于一定量的水中,形成铁离子浓度为0.05mol/L的溶液。取150mL的溶液在搅拌速度为500r/min的条件下升温加热至95℃;
(2)以5ml/min的速度向溶液中滴加浓度为4mol/L的氨水溶液,调节溶液的pH值为4后,继续以500r/min搅拌速度搅拌3h;
(3)将溶液进行离心分离、洗涤、干燥,得到含铁的前驱体;
(4)将含铁的前驱体在600℃的马弗炉中焙烧0.5h,得到球形、颗粒尺寸为50~60nm,禁带宽度为1.88eV的α-Fe2O3光催化剂。
上述球形α-Fe2O3光催化剂在降解甲基橙或亚甲基蓝有机染料的应用方法,具体步骤如下:
(1)在25℃下向150mL浓度为5mg/L的甲基橙有机染料水溶液和150mL浓度为1mg/L的亚甲基蓝有机染料水溶液中各加入0.015g球形α-Fe2O3光催化剂,在搅拌速度为500r/min条件下使α-Fe2O3光催化剂吸附有机染料溶液100min,达到吸附-解吸平衡;
(2)向达到吸附-解吸平衡的甲基橙和亚甲基蓝有机染料水溶液中各加入5mL的30%过氧化氢(H2O2),在紫外可见光照射下以450r/min的搅拌速度继续搅拌50min。
对实施例3中的甲基橙和亚甲基蓝有机染料水溶液进行浓度测定,根据本发明中公式(1)计算光球形α-Fe2O3光催化剂降解甲基橙和亚甲基蓝有机染料的降解率。计算结果为,本实施例3中制备得到的球形α-Fe2O3光催化剂对甲基橙有机染料的降解率为98%,对亚甲基蓝有机染料的降解率为96%。
Claims (4)
1.一种球形α-Fe2O3光催化剂,其特征在于,所述球形α-Fe2O3光催化剂颗粒尺寸为10~80nm;所述球形α-Fe2O3光催化剂的禁带宽度为1.7~2.2eV,具有强烈的可见光吸收性;所述球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料中应用。
2.权利要求1所述的球形α-Fe2O3光催化剂的制备方法,其特征在于,按照以下步骤进行:
(1)将水合氯化铁或硫酸铁的无机铁盐溶解于一定量的水中,形成铁离子浓度为0.05~0.2mol/L的溶液,在搅拌速度为100~500r/min的条件下升温加热至40~95℃;
(2)以1~5ml/min的速度向溶液中滴加浓度为0.5~4mol/L的氨水溶液,调节溶液的pH值为4.0~9.0后,继续搅拌0.5~3h;
(3)进行离心分离、洗涤、干燥后,得到含铁的前驱体;
(4)将含铁的前驱体在300~600℃的温度下焙烧0.5~4h,得到球形、颗粒尺寸为10~80nm,禁带宽度为1.7~2.2eV的α-Fe2O3光催化剂。
3.权利要求1所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料的应用方法,其特征在于,包括以下步骤:
(1)将0.015~0.3g球形α-Fe2O3光催化剂,在25℃下加入到一定量的甲基橙或亚甲基蓝的有机染料水溶液中,在搅拌速度为100~500r/min条件下搅拌10~120min,使有机染料与α-Fe2O3光催化剂达到吸附-解吸平衡;其中,甲基橙有机染料水溶液浓度为5~100mg/L,亚甲基蓝有机染料水溶液浓度为1~50mg/L,球形α-Fe2O3光催化剂与甲基橙或与亚甲基蓝的质量比为(20~267):1;
(2)向达到吸附-解吸平衡的甲基橙或亚甲基蓝溶液中加入0.05~5mL的30%过氧化氢,并在紫外可见光照射下以100~500r/min的搅拌速度继续搅拌10~240min。
4.如权利要求4所述的球形α-Fe2O3光催化剂在降解甲基橙有机染料或亚甲基蓝有机染料的应用方法,其特征在于,所述球形α-Fe2O3光催化剂对甲基橙有机染料的降解率为≥90%,对亚甲基蓝有机染料的降解率为≥90%。
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