CN113617359A - 一种铁酸铋纤维状热释电催化剂的制备方法及应用 - Google Patents
一种铁酸铋纤维状热释电催化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明公开一种铁酸铋纤维状热释电催化剂的制备方法及应用,利用五水硝酸铋、九水硝酸铁为主要原料,溶解于有机溶剂中,并将PVP溶解于乙醇和DMF的混合溶液中,形成铁酸铋纤维的纺前溶液,将溶液置于注射器中,放至静电纺丝机上,由注射器喷出,锡纸收集、高温煅烧后得到铁酸铋纤维。在制备过程中控制纺前液配料比、静电纺丝电压、煅烧温度等工艺参数,制得铁酸铋纤维状热释电催化剂。本发明工艺流程简单,易操作,可重复性强,成本低,产物重复利用率高,是一种具有商业前景的制备方法。所制备的铁酸铋纤维在热释电催化杀菌和降解有机污染物及增强光催化等方面有重要的应用价值,在应用时可借助昼夜温差激发热释电效应,实现热释电催化,易于操作。
Description
技术领域
本发明属于新型功能材料技术领域,具体涉及一种铁酸铋纤维状热释电催化剂的制备方法及应用。
背景技术
目前,工业的快速发展和化石燃料的消耗加速了环境污染和能源困境。为了缓解上述两个严重问题,一些研究人员致力于寻找环境污废水的处理方法和产品,如光催化、热催化、压电催化产品等。
与上述技术不同,热释电催化可通过温度波动触发,产生氧化还原反应的热生正负电荷。温度变化会引起晶体结构中原子的轻微空间运动,导致热释电体内部的极化和热释电材料表面上的感生热释电电荷发生变化。而钙钛矿类物质,则是热释电催化的一类代表,它的通式为ABX3,B位上较小的过渡金属离子位于X阴离子的共角八面体中,较大的A位阳离子与X一样,是具有12倍的配位的一类物质。CaTiO3是在这个结构家族中被发现的第一种矿物。钙钛矿结构其空间点群为Pm3m,由于钙钛矿氧化物族的柔性电子结构,它们在不同情况中表现出不同的物理和化学性质,包括铁电性巨磁电阻,质子的离子导电性等。作为钙钛矿结构中的一种,BiFeO3不但拥有菱方钙钛矿的结构,而且是一种多铁性的物质。BiFeO3的能带隙约为2.013eV,属于一种窄带隙的半导体,并且具有反铁磁性能。BiFeO3因其优越的性能,如良好的可见光吸收效率、可以自发极化、低成本和无毒性,而备受关注,常用于水分解和降解有机污染物,但传统的BiFeO3制备方式以粉体形式制备,存在着尺寸大,比表面积小的问题,并且废水处理时容易团聚,严重影响了废水处理效果。
发明内容
本发明的目的是提供一种利用五水硝酸铋、九水硝酸铁作为主要原材料,提供一种铁酸铋纤维状热释电催化剂的制备方法及应用。
本发明所采用的技术方案为:
一种铁酸铋纤维状热释电催化剂,其是以静电纺丝和高温煅烧法制备,化学组成为BiFeO3。
a.纺前溶液的制备:将五水硝酸铋(Bi(NO)3·5H2O)和九水硝酸铁(Fe(NO)3·9H2O)溶于2-甲氧基乙二醇溶液中,向溶液中滴加乙二醇胺调节pH,再加入冰醋酸控制溶液粘度,然后将其放在室温环境下机械搅拌2小时,记为溶液A;将聚乙烯吡咯烷酮(PVP)加入到N-N二甲基甲酰胺(DMF)和乙醇的混合溶液中,搅拌1小时,记为溶液B;待两份溶液都混合均匀后,将溶液A缓慢加入到到溶液B中,待混合均匀后,形成BiFeO3的纺前溶液;
b.铁酸铋纤维的制备,将步骤a中制备得到的BiFeO3的纺前溶液移至注射器中,通过静电纺丝的方法,得到BiFeO3的初生纤维;将所得到的BiFeO3初生纤维放置在烘箱中干燥,再经马弗炉煅烧,煅烧后令其自然冷却到室温,最终得到BiFeO3纤维。
步骤a中所述五水硝酸铋、九水硝酸铁中阴离子反应后可除去,不掺杂在铁酸铋中。
步骤a中所述五水硝酸铋、九水硝酸铁的化学计量比为1.05~1.1:1,纺丝前驱体溶液的质量分数为13~15%。
步骤a中所述添加乙二醇胺调节溶液pH为3~4。
步骤b中所述静电纺丝参数为:纺丝距离为10~15cm,工作电压为12~17V,推进速度为0.3~0.5mL/h。
步骤b中所述煅烧工艺参数为:煅烧温度为550~750℃,时间为1.5~2.5h,气氛为空气。
所述铁酸铋纤维状热释电催化剂的铁酸铋纤维之间紧密排列在一起,纤维表面光滑笔直而且没有发生断裂;纤维束径很小。
所述铁酸铋纤维状热释电催化剂在衍射角2θ=22.44°、31.80°、39.02°、45.79°、51.38°、56.47°、66.44°处分别与BiFeO3的(010)、(110)、(111)、(020)、(120)、(121)和(220)晶面特征峰相吻合。
所述BiFeO3纤维状催化剂应用于热释电催化杀菌和降解染料废水中的有机染料及增强光催化。
所述处理过程在一定温差条件下进行,所述温差为20~40℃。优选的,在昼夜自然温差条件下即可完成。
本发明与现有技术相比,具有以下优点和有益效果:
(1)本发明针对现有BiFeO3粉体形式尺寸大,比表面积小,易团聚的问题,采用静电纺丝及高温煅烧的工艺制备BiFeO3纤维状热释电催化剂,形成的纤维状产品提高了比表面积且不会团聚,显著提高了废水处理效果。
(2)本发明的制备方法探索出了优化合理的制备参数,BiFeO3纤维状热释电催化剂,纯度高,纤维表面光滑笔直,不会团聚,同时高温煅烧使纤维表面的有机物挥发散去,通过XRD看出得到的产品没有其他任何杂质峰出现,纯度非常好。在热释电催化杀菌和降解有机污染物及增强光催化方面效果显著,在工业应用时,仅靠昼夜温差即可激发热释电效应,实现热释电催化,易于操作。
(3)本发明采用五水硝酸铋、九水硝酸铁为主要原料,原料简单,价格低廉,整体工艺和流程简单,反应易控制,可重复性强。
附图说明
图1本发明制备的BiFeO3纤维状热释电催化剂的XRD图。
图2本发明制备的BiFeO3纤维状热释电催化剂的SEM图。
图3本发明制备的BiFeO3纤维状热释电催化剂对罗丹明B水溶液的降解图。
具体实施方式
本发明的目的是提供一种铁酸铋纤维状热释电催化剂的制备方法及应用。
本发明通过静电纺丝和高温煅烧法制备铁酸铋纤维状热释电催化剂,通过热释电催化反应,产生温度差,促进所需要的电化学氧化还原反应和热释电效应的耦合,由于ΔQ=c·m·Δt,随着温度差的增加,使热能ΔQ的值增加,有助于有机染料的降解。同时,由于BiFeO3纤维状热释电催化剂表面光滑,不易发生团聚,有良好的重复使用性能;而热释电催化在工业上可借助昼夜温差实现。本方法制备工艺简单,原料低廉,在处理有机污染物方面展现出良好的应用前景。
实施例1:
静电纺丝法制备BiFeO3纺纤前溶液:
将2.43g Bi(NO)3·5H2O和2.02g Fe(NO)3·9H2O溶于10mL 2-甲氧基乙二醇溶液中,向溶液中滴加乙二醇胺将溶液的pH调至3.5,再加入5mL冰醋酸控制溶液粘度,然后将其放在室温环境下机械搅拌,时间约为2小时,记为溶液A;将2g的聚乙烯吡咯烷酮加入到11gN-N二甲基甲酰胺和乙醇的混合溶液中,搅拌1小时,记为溶液B;待两份溶液都混合均匀后,将溶液A缓慢加入到到溶液B中,待混合均匀后,形成BiFeO3的纺前溶液。
实施例2:
高温煅烧法制备BiFeO3纤维状热释电催化剂:
将实施例1中制备得到的BiFeO3的纺前溶液移至注射器中,设置注射器针头与锡纸收集板之间距离为10cm,静电纺丝电压为12V,注射器推进速度为0.4mL/h,保持纺丝过程中环境温湿度恒定,得到BiFeO3的初生纤维;将所得到的BiFeO3初生纤维放置在60℃的烘箱中干燥,烘干后的纤维放入马弗炉中煅烧,将马弗炉的煅烧温度设置为600℃,保温时间为2h,充分去除初生纤维中含有的有机物质,提高BiFeO3纤维的纯度,煅烧后令其自然冷却到室温,最终得到BiFeO3纤维状热释电催化剂。
图1为BiFeO3纤维状热释电催化剂的XRD图,由图1可知,根据各衍射峰位置与PDF#72-2035标准卡片比对后发现,在衍射角2θ=22.44°、31.80°、39.02°、45.79°、51.38°、56.47°、66.44°处分别与BiFeO3的(010)、(110)、(111)、(020)、(120)、(121)和(220)晶面特征峰相吻合。可以确定BiFeO3纤维状热释电催化剂的XRD图谱没有其他任何杂质峰出现,纯度较好。
图2为高温煅烧后得到的BiFeO3纤维状热释电催化剂的SEM图,从图中可以发现,BiFeO3纤维之间紧密排列在一起,纤维表面光滑笔直而且没有发生断裂;纤维束径很小,纤维直径在220nm左右,这是因为在高温煅烧后,纤维表面的有机物挥发散去所导致。
应用例1:
上述所得BiFeO3纤维状热释电催化剂应用于处理废水中有机污染物,对罗丹明(RhB)水溶液降解。
取50mL的5mg/L的罗丹明B溶液,向其中加入0.05g BiFeO3纤维状热释电催化剂,将溶液循环放置于20℃冷水和60℃热水环境中,每10min循环一次,全程保持溶液避光。每1h取一次溶液上清液,将上清液以8000r/min离心3min后,通过紫外光谱仪在554nm处测量吸光度。
对比应用例1:
上述所得BiFeO3纤维状热释电催化剂应用于处理废水中有机污染物,对罗丹明(RhB)水溶液降解。
取50mL的5mg/L的罗丹明B溶液,向其中加入0.05g BiFeO3纤维状热电催化剂,将溶液置于黑暗处搅拌。每1h取一次溶液上清液,将上清液以8000r/min离心3min后,通过紫外光谱仪在554nm处测量吸光度。
图3为BiFeO3纤维状热释电催化剂降解罗丹明B水溶液的曲线图。由图3可以看出,在热释电催化的条件下,BiFeO3纤维状热电催化剂对罗丹明B水溶液的降解明显高于对比应用1中黑暗搅拌条件,当热释电催化7h后,BiFeO3纤维状热释电催化剂对罗丹明B水溶液的降解率可达到85.6%。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化,均仍属于本发明技术方案的保护范围内。
Claims (6)
1.一种铁酸铋纤维状热释电催化剂的制备方法,其特征在于,包括如下步骤
a.纺前溶液的制备:将五水硝酸铋(Bi(NO)3·5H2O)和九水硝酸铁(Fe(NO)3·9H2O)溶于2-甲氧基乙二醇溶液中,所述的五水硝酸铋与九水硝酸铁的化学计量比为1.05~1.1:1,向溶液中滴加乙二醇胺调节pH为3~5,再加入冰醋酸控制溶液粘度,然后将其放在室温环境下机械搅拌2小时,记为溶液A;将聚乙烯吡咯烷酮(PVP)加入到N-N二甲基甲酰胺(DMF)和乙醇的混合溶液中,搅拌1小时,记为溶液B;待两份溶液都混合均匀后,将溶液A缓慢加入到到溶液B中,待混合均匀后,形成BiFeO3的纺前溶液;所述纺丝前驱体溶液的质量分数为13~15%。
b.铁酸铋纤维的制备,将步骤a中制备得到的BiFeO3的纺前溶液移至注射器中,通过静电纺丝的方法,得到BiFeO3的初生纤维;所述静电纺丝参数为:纺丝距离为10~15cm,工作电压为12~17V,推进速度为0.3~0.5mL/h。将所得到的BiFeO3初生纤维放置在烘箱中干燥,再经马弗炉煅烧,所述煅烧工艺参数为;煅烧温度为550~750℃,保温时间为1.5~2.5h,气氛为空气。煅烧后令其自然冷却到室温,最终得到BiFeO3纤维。
2.根据权利要求2所述的一种铁酸铋纤维状热释电催化剂的制备方法,其特征在于,步骤a中所述的五水硝酸铋、九水硝酸铁为可溶于水的盐,且其中的阴离子经反应后不掺杂在铁酸铋纤维中。
3.根据权利要求1~2任所述的方法制备的铁酸铋纤维状热释电催化剂,其特征在于,所述铁酸铋纤维状热释电催化剂的铁酸铋纤维之间紧密排列在一起,纤维表面光滑笔直且无断裂;纤维直径为100~400nm左右;
所述铁酸铋纤维状热释电催化剂在衍射角2θ=22.44°、31.80°、39.02°、45.79°、51.38°、56.47°、66.44°处分别与BiFeO3的(010)、(110)、(111)、(020)、(120)、(121)和(220)晶面特征峰相吻合。
4.一种权利要求3所述的铁酸铋纤维状热电催化剂的应用,其特征在于,所述BiFeO3纤维状催化剂应用于热释电催化杀菌和降解染料废水中的有机染料及增强光催化。
5.一种权利要求4所述的铁酸铋纤维状热电催化剂的应用,其特征在于,所述BiFeO3纤维状催化剂用于处理含有罗丹明(RhB)的废水,所述处理过程在一定温差条件下进行,所述温差为20~40℃。
6.一种权利要求4所述的铁酸铋纤维状热电催化剂的应用,其特征在于,所述处理在昼夜自然温差条件下即可完成。
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