CN115608387B - P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用 - Google Patents
P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用 Download PDFInfo
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Abstract
本发明涉及P‑MoO3/P‑MoO2/P‑Fe3O4异质结构纳米带的制备方法及其光催化应用，具体的说是将α‑MoO3粉末溶解在H2O2溶液中，采用水热合成法得到α‑MoO3纳米带；然后将α‑MoO3纳米带和FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在N2氛围中加热，得到P‑MoO3/P‑MoO2/P‑Fe3O4异质结构纳米带；该P‑MoO3/P‑MoO2/P‑Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝中的应用。
Description
技术领域
本发明涉及P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用，属于材料的制备及其应用领域。
背景技术
研究表明钼基氧化物具有较好的光、电、磁、催化等性能，引起了人们广泛的研究兴趣。目前，形貌可控合成、调变钼基氧化物，使其具有优异的性能，主要集中在MoO3。对MoO2的形貌、尺寸、组成调变，研究其光催化性能较少。因此调控MoO2表面结构，使其光催化降解有机染料，具有重要的理论和现实意义。
利用化学合成方法实现氧化物的可控合成、表面结构调控，是目前调控氧化物电子结构、增加活性位的有效方法。例如：Hu等利用(NH4)6Mo7O24·4H2O、C6H8O7·4H2O、Na2CO3、HCl在200℃水热16h，得到直径为1.5-3.5μm的MoO2微米球，能有效光催化降解10mg/L罗丹明B(Chinese Journal of Inorganic Chemistry,2014,30,398-404)。Li等利用(NH4)6Mo7O24·4H2O、C4H6O6、HNO3、TiO2等在160℃水热5h得到MoO2/TiO2纳米纤维，能有效光催化降解10mg/L罗丹明B(ACS Applied Materials&Interfaces,2014,6,9004-9012)。Li等利用MoO2、C3N4、(CH2OH)2在180℃水热12h，得到MoO2/C3N4微米球，能有效光催化降解10mg/L罗丹明B(Applied Surface Science,2018,457,1142-1150)。因此，实现MoO2晶相、结构的可控合成，使其高活性催化反应具有重要的现实意义。
工业上使用的有机染料排放到水中，严重影响人类健康，其中废水中包含亚甲基蓝。常用的光催化剂是TiO2，关于MoO2基材料光催化降解亚甲基蓝的研究较少。因此调变MoO2基材料，调变电子结构，使其高效催化染料废水中的亚甲基蓝具有重要现实意义。
发明内容：
本发明旨在提供P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用。
基于上述目的，本发明所涉及的技术方案如下：
(1)P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法：将商品化α-MoO3粉末溶解在H2O2中，采用水热合成法在160-210℃下反应8-14h得到α-MoO3纳米带；然后将α-MoO3纳米带和FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在N2氛围中加热，得到P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带。
上述的制备方法，所述α-MoO3粉末质量为1-1.5g，H2O2溶液体积为10-15mL。
上述的制备方法，所述α-MoO3纳米带的宽度为110-360nm、长度为420-6200nm。
上述的制备方法，所述α-MoO3纳米带的质量为15-25mg，FeCl3·6H2O的质量为100-140mg，NaH2PO2·H2O的质量为1-1.5g。
上述的制备方法，所述然后将α-MoO3纳米带和FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在20-30mL/min N2氛围中加热，加热温度为300-350℃，加热时间为1-2小时。
上述的制备方法，所述P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带宽度为100-320nm、长度为300-6000nm。
上述的制备方法，所述P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带中P掺杂MoO3、P掺杂MoO2、P掺杂Fe3O4形成异质结构，MoO3晶相归属于标准卡片JCPDS#05-0508，MoO2晶相归属于标准卡片JCPDS#32-0671，Fe3O4晶相归属于标准卡片JCPDS#19-0629。
(2)一种上述的制备方法制备得到的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝中的应用；在亚甲基蓝浓度为0.1-1mg/L时反应2-6h，脱除率为100％。
本发明具有如下优点：
1)利用α-MoO3、FeCl3·6H2O为前驱体，采用磷化的工艺制备了P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带，开发了P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的新合成路径。
2)P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝反应中具有较好的性能。
3)本发明具有方法简单易操作的优点。
附图说明：
图1是P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的XRD表征结果。
具体实施方式
下列实施例用来进一步说明本发明，但不因此而限制本发明。
实施例1
P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用：将1gα-MoO3粉末溶解在10mL H2O2溶液中，采用水热合成法在180℃下反应12h，将反应得到的产物离心，干燥得到宽度为110-360nm、长度为420-6200nm的α-MoO3纳米带；然后将15mgα-MoO3纳米带和140mg FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取1g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在20mL/min流速的N2氛围中300℃加热1h，得到100-320nm、长度为300-6000nm的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带；将P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝浓度为0.1mg/L时反应2h，脱除率为100％。
实施例2
P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用：将1.5gα-MoO3粉末溶解在15mL H2O2溶液中，采用水热合成法在210℃下反应14h，将反应得到的产物离心，干燥得到宽度为120-360nm、长度为430-6200nm的α-MoO3纳米带；然后将25mgα-MoO3纳米带和140mg FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取1.5g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在30mL/min流速的N2氛围中350℃加热2h，得到120-320nm、长度为350-6000nm的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带；将P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝浓度为1mg/L时反应6h，脱除率为100％。
实施例3
P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用：将1gα-MoO3粉末溶解在12mL H2O2溶液中，采用水热合成法在160℃下反应8h，将反应得到的产物离心，干燥得到宽度为130-360nm、长度为450-6200nm的α-MoO3纳米带；然后将20mgα-MoO3纳米带和100mg FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取1g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在30mL/min流速的N2氛围中300℃加热1h，得到140-320nm、长度为330-6000nm的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带；将P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝浓度为0.1mg/L时反应6h，脱除率为100％。
Claims (6)
1.一种P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法，其特征在于，包括以下步骤：
将商品化α-MoO3粉末溶解在H2O2中，采用水热合成法在160-210℃下反应8-14 h得到α-MoO3纳米带；然后将15-25 mg α-MoO3纳米带和100-140 mg FeCl3·6H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在N2氛围中加热，得到P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带。
2. 如权利要求1所述的制备方法，其特征在于，所述α-MoO3粉末质量为1-1.5 g，H2O2溶液体积为10-15 mL。
3. 如权利要求1所述的制备方法，其特征在于，所述α-MoO3纳米带的宽度为110-360nm、长度为420-6200 nm。
4. 如权利要求1所述的制备方法，其特征在于，所述α-MoO3纳米带的质量为15-25 mg，FeCl3·6H2O的质量为100-140 mg，NaH2PO2·H2O的质量为1-1.5 g，N2流速为20-30 mL/min，N2氛围中加热温度300-350℃，加热1-2小时。
5. 一种由权利要求1-4任一项所述的制备方法制备得到的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带，其特征在于，所述P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带宽度为100-320 nm、长度为300-6000 nm，所述P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带中P掺杂MoO3、P掺杂MoO2、P掺杂Fe3O4形成异质结构，MoO3晶相归属于标准卡片JCPDS#05-0508，MoO2晶相归属于标准卡片 JCPDS#32-0671，Fe3O4晶相归属于标准卡片JCPDS#19-0629。
6. 一种由权利要求1-4任一项所述的制备方法制备得到的P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带在光催化降解废水染料中亚甲基蓝中的应用，在亚甲基蓝浓度为0.1-1 mg/L时反应2-6 h，脱除率为100％。
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