CN113289628B - 一种磁性钙钛矿催化剂及其制备方法和应用 - Google Patents
一种磁性钙钛矿催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种磁性钙钛矿催化剂,其制备工艺包括:(1)称取可溶性钴盐、可溶性锶盐、可溶性铁盐共同溶于水中,形成均质溶液,Co、Sr、Fe的摩尔比1:1‑2:1;(2)按照总的金属离子和碳酸钠(Na2CO3)的摩尔比为12:20的比例,向均质溶液逐滴添加Na2CO3溶液,滴加结束后,继续搅拌30 min,然后静置1 h;(3)将上述溶液过滤,用洗涤滤渣直至滤液pH=7,然后将洗涤后的滤渣在80℃下干燥12h,将干燥后滤渣研磨成粉末,得到前驱体;(4)将前驱体在725℃~1025℃下焙烧6h,得到产品磁性钙钛矿催化剂。该催化剂结构稳定,能够激活过一硫酸氢盐,降解抗生素,催化效率高,无残留。
Description
技术领域
本发明涉及催化剂领域,尤其是涉及一种磁性钙钛矿催化剂及其制备方法和应用。
背景技术
抗生素具有抑制或杀灭各种病原体和有害微生物的功效,可用于治疗疾病和抵御细菌,因此在畜牧、水产养殖以及农业生产等领域应用非常广泛,目前可大规模生产的抗生素有几千种,抗生素使用量很大,而且也存在抗生素的滥用情况,其进入生物体之后,难以被吸收,大部分从生物体排出最终进入环境比如土壤、地表水体、城市污水以及地下水中,造成环境抗生素污染,不仅容易滋生大量的抗药性细菌或病毒,还有可能进化成超级细菌或超级病毒,从而引起全球瘟疫,进而严重威胁人类的健康安全。因此,寻找一种高效、低成本的方法消除水环境中抗生素的不当排放具有重要意义。
现有技术中对于抗生素降解也进行了大量的研究。中国专利文献(申请号2020102204795)公开一种用于催化降解抗生素的改性钙钦矿中空多孔微球及其制备方法和应用,涉及用于催化降解抗生素的改性钙钛矿中空多孔微球及其制备方法和应用,所述中空多孔微球制备方法包括以下步骤:1)制备硝酸盐溶液;(2)制备钛酸四正丁酯溶液;(3)将碳酸氢氨搅拌溶解于水中制得饱和碳酸氢氨水溶液;(4)混合;(5)加热反应;(6)锻烧。该发明具有较好的孔状结构,极大的比表面积,且吸附性极佳,再配合多孔微球材料表面金属的光催化性,使废水中的抗生素吸附在表面上,在可见光的作用下催化降解,达到高效去除抗生素的目的,而且处理能耗低、成本低、管理简单,易于分离、回收,可循环使用,降低了抗生素废水的处理成本,且不会对环境造成二次污染。但是其制备工艺比较复杂,而且催化反应效率低,反应后回收程序复杂,成本高。
另外现有技术中的一些复合催化剂,其催化剂结构不够稳定,也面临催化剂中金属离子浸出浓度大,容易引起二次污染的问题。
发明内容
有鉴于此,本发明的目的是针对现有技术的不足,提供一种磁性钙钛矿催化剂,其结构稳定,能够激活过一硫酸氢盐,降解抗生素,催化效率高,无残留。
为达到上述目的,本发明采用以下技术方案:
一种磁性钙钛矿催化剂,其结构式为 SrCo1-δFeδO2.78,其中δ=0.19。
一种磁性钙钛矿催化剂的制备方法,包括以下步骤:
(1)称取可溶性钴盐、可溶性锶盐、可溶性铁盐共同溶于水中,形成均质溶液,Co、Sr、Fe的摩尔比1:1-2:1;
(2)按照总的金属离子和碳酸钠(Na2CO3)的摩尔比为12:20的比例,向均质溶液逐滴添加Na2CO3溶液,滴加结束后,继续搅拌30 min, 然后静置1 h;
(3)将上述溶液过滤,用洗涤滤渣直至滤液pH=7,然后将洗涤后的滤渣在80 ℃下干燥12h,将干燥后滤渣研磨成粉末,得到前驱体;
(4)将前驱体在725℃~1025 ℃温度下焙烧6h,得到产品磁性钙钛矿催化剂。
进一步的,所述可溶性钴盐为六水硝酸钴,可溶性锶盐为硝酸锶,可溶性铁盐为硝酸铁。
进一步的,所述焙烧时升温速率为10℃/min。
一种磁性钙钛矿催化剂在催化降解抗生素中的应用。
本发明的有益效果是:
1、本发明采用硝酸钴、硝酸锶和硝酸铁制备磁性钙钛矿催化剂,制备工艺简单,制备的催化剂具有磁性,便于反应后回收。
2、制备的钙钛矿具有稳定的晶体结构,降低金属离子浸出,避免二次污染。
3、将其用于激活过一硫酸氢盐,产生硫酸根自由基,单态氧,超氧自由基和羟基自由基等多活性物种体系,降解抗生素,在27min内实现全降解,效率高,无残留。
附图说明
图1为本发明实施例1-4制备的钙钛矿的XRD图;
图2为本发明实施例1-4制备的钙钛矿的SEM图,其中(a) 725 ℃, (b) 825 ℃,(c) 925 ℃, (d) 1025 ℃;
图3为本发明实施例4的磁滞回线;
图4为氟苯尼考的降解率曲线。
具体实施方式
下面结合具体实施例对本发明作进一步的描述。
实施例1
一种磁性钙钛矿催化剂,其结构式为SrCo0.81Fe0.19O2.78,其制备方法具体包括以下步骤:
(1)称取1 mol六水硝酸钴 (Co(NO3)2 ·6H2O), 2.0 mol硝酸锶 (Sr(NO3)2), 1 mol硝酸铁 (Fe(NO3)3 ·9H2O) 共同溶于50 mL 水中,形成均质溶液;
(2)按照总的金属离子和碳酸钠(Na2CO3)的摩尔比为12:20的比例,向均质溶液逐滴添加Na2CO3溶液。滴加结束后,继续搅拌30 min,然后静置1 h;
(3)将上述溶液过滤,用洗涤滤渣直至滤液pH=7 为止,然后将洗涤后的滤渣收集至坩埚中,坩埚置于鼓风干燥箱中,在80 ℃下干燥 12h,将干燥后滤渣研磨成粉末,得到前驱体;
(4)将前驱体置于刚玉坩埚中,放置于马弗炉中,升温速率为10℃/min,在725℃温度下焙烧6h,得到产品磁性钙钛矿催化剂SrCo0.81Fe0.19O2.78。
实施例2-4
实施例2-4与实施例1不同之处在于,焙烧温度分别为825℃、925℃、1025℃。
性能表征以及检测
1、性能表征
图1为不同温度下(725℃、825℃、925℃、1025℃)焙烧样品的XRD图谱,由图谱上可以明显看出,当焙烧温度为725℃时,样品中含有大量的碳酸锶杂质,当焙烧温度上升至为825℃时,碳酸锶杂质消失,并形成完整磁性钙钛矿催化剂SrCo0.81Fe0.19O2.78,与标准卡片JCPDS 82-2445完全吻合。此外,从XRD图上能看出,在焙烧温度在825℃、925℃、1025℃均能制备出纯SrCo0.81Fe0.19O2.78。考虑到能耗问题,我们选择了焙烧温度在825℃时制备的催化剂。
图2为不同温度下焙烧样品的扫描电镜图,由图可以看出,当焙烧温度为725℃时,没有观察到钙钛矿的结构,XRD测试结果也显示该温度下制备的样品中存在大量的碳酸锶。但焙烧温度为825℃时,钙钛矿结构已经形成,随着焙烧温度的升高,钙钛矿结构形成越完整。同样地,虑到能耗问题,后续试验检测采用实施例2样品(焙烧温度825℃)。
图3为实施例2制备的样品的磁性回线,结果表明制备的样品显示出明显的滞回特性,饱和磁化强度0.71 emu/g,能够满足催化剂反应的简单分离回收。
2、催化降解抗生素检测试验
试验条件:氟苯尼考的浓度20 mg·L-1,催化剂的用量 0.2 g·L-1,过一硫酸氢盐的浓度0.4 g·L-1, 初始溶液 pH = 7.4,温度为 20 ℃。
其中催化剂分别采用实施例2样品、SrO、Fe3O4、Co3O4、CoFe2O4、SrO/Fe3O4/Co3O4等重量混合物,分别检测1min、5min、9min、15min、21min、27min的氟苯尼考的浓度,具体降解曲线参见图4。
由图4可以看出,通过对氟苯尼考在不同催化剂作用下降解效果比较发现,SrCo0.81Fe0.19O2.78对氟苯尼考的降解效果最优,前期反应速度很快,而且在27min内实现了全降解。
最后说明的是,以上实例仅用以说明本发明的技术方案而非限制,本领域普通技术人员对本发明的技术方案所做的其他修改或者等同替换,只要不脱离本发明技术方案的精神和范围,均应涵盖在本发明的权利要求范围当中。
Claims (4)
1.一种磁性钙钛矿催化剂的制备方法,其特征在于:所述磁性钙钛矿催化剂结构式为SrCo1-δFeδO2.78,其中δ=0.19;
所述磁性钙钛矿催化剂的制备方法,包括以下步骤:
(1)称取可溶性钴盐、可溶性锶盐、可溶性铁盐共同溶于水中,形成均质溶液,Co、Sr、Fe的摩尔比1:2:1;
(2)按照总的金属离子和碳酸钠的摩尔比为12:20的比例,向均质溶液逐滴添加Na2CO3溶液,滴加结束后,继续搅拌30 min,然后静置1 h;
(3)将上述溶液过滤,洗涤滤渣直至滤液pH=7,然后将洗涤后的滤渣在80 ℃下干燥12h,将干燥后滤渣研磨成粉末,得到前驱体;
(4)将前驱体在825℃~1025 ℃温度下焙烧6h,得到产品磁性钙钛矿催化剂。
2.根据权利要求1所述的磁性钙钛矿催化剂的制备方法,其特征在于:所述可溶性钴盐为六水硝酸钴,可溶性锶盐为硝酸锶,可溶性铁盐为硝酸铁。
3.根据权利要求1所述的磁性钙钛矿催化剂的制备方法,其特征在于:所述焙烧时升温速率为10℃/min。
4.一种如权利要求1所述的制备方法制备的磁性钙钛矿催化剂在催化降解抗生素中的应用。
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