CN114655992A - 一种铁酸铋纳米片材料及其制备方法及用途 - Google Patents
一种铁酸铋纳米片材料及其制备方法及用途 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 title claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims description 5
- 229910000859 α-Fe Inorganic materials 0.000 title description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
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- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 229910002897 Bi2Fe4O9 Inorganic materials 0.000 claims abstract description 23
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229960005404 sulfamethoxazole Drugs 0.000 claims description 7
- JLKIGFTWXXRPMT-UHFFFAOYSA-N sulphamethoxazole Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 JLKIGFTWXXRPMT-UHFFFAOYSA-N 0.000 claims description 7
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- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种制备Bi2Fe4O9纳米片材料的方法,包括如下步骤:(a)将分析纯的铋盐和铁盐以0.7‑1.2:1的摩尔比溶于乙二醇溶液;(b)向步骤(a)中所形成的溶液加入去离子水并搅拌均匀,然后逐滴加入过量的浓氨水至溶液完全沉淀;(c)将步骤(b)中上层清液倒出,加入去离子水到所得沉淀物中,振荡、洗涤,并进行离心;(d)将NaOH溶液加入到步骤(c)中反复洗涤的沉淀物中,搅拌30min,形成溶液并装入反应釜中,反应一段时间;(e)在步骤(d)结束后,将反应釜自然冷却至室温,然后将反应最终产物分别用去离子水和无水乙醇洗涤,并在60℃的烘箱中干燥12h,得到Bi2Fe4O9纳米片材料。
Description
技术领域
本发明属于环境工程领域,涉及压电催化材料的制备及应用,更具体地,涉及Bi2Fe4O9纳米片材料的制备及压电催化有机污染物。
背景技术
环境污染和清洁能源短缺是最紧迫的问题之一,威胁着人类文明的可持续发展。向废水中排放生物难降解有机物造成的水污染是环境污染的主要来源之一。目前为止,研究人员已经专门探索了几种结合高级氧化工艺(AOPs)的处理技术来去除水中的有机污染物,如Fenton氧化、UV光解、臭氧氧化和光催化,然而它们或催化效率低或难以大规模工业化或需要相对苛刻的条件(例如,用Fenton高效处理需要酸性pH值)。另一方面,能源不足迫使人们考虑各种收集、利用满足社会发展需要的自然能源形式。
压电催化作为一种高级氧化技术,可通过收集自然界的振动能来实现染料的分解,近年来得到了广泛的应用与开发。压电材料在风、潮、声、大气压等自然界能量作用下发生机械变形,在其内部产生电子和空穴并发生迁移在材料表面积累,这些载流子可以容易地捕获氧气或水,生成活性氧物种,去除污染物。铁酸铋作为一种智能材料,具有多铁性,主要有BiFeO3和Bi2Fe4O9两种结构,基于BiFeO3压电特性的应用已得到广泛研究,而Bi2Fe4O9的压电特性及应用鲜有报道。Bi2Fe4O9的压电特性,使其可通过收集自然界振动能压电催化净化生物难降解有机废水,这些性质使Bi2Fe4O9在生物降解有机废水的高效节能处理领域具有极大的应用潜力和商业前景。
目前,已有多种制备方法用于制备Bi2Fe4O9材料,例如固相烧结法、磁控溅射法、快速液相烧结法、溶胶凝胶法和微波水热法等。传统制备方法通常需要在600℃预烧,然后加热到750℃到850℃之间得到产物。另外,传统制备方法得到的Bi2Fe4O9颗粒大且难以调节尺寸。虽然有研究表明加入有机助剂可以降低温度,但造价较高不利于工业生产。CN101890354A公开了一种降解水中有机污染物的Bi2Fe4O9制备方法。该方法采用溶剂热法合成Bi2Fe4O9,合成时硝酸铋与硝酸铁的摩尔比为12:1,但该方法合成的催化剂颗粒尺寸大,因此反应比表面积较小。因此,制备一种颗粒均匀、压电催化反应活性高Bi2Fe4O9催化剂仍然面临挑战。
发明内容
本发明的目的旨在提供一种Bi2Fe4O9纳米片材料及其制备方法及用途。主要包括以下方面:本发明提供了一种制备Bi2Fe4O9纳米片材料的方法,包括如下步骤:
(a)将分析纯的铋盐和铁盐以0.7-1.2:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解;(b)向步骤(a)中所形成的溶液加入去离子水并搅拌均匀,然后逐滴加入过量的浓氨水至溶液完全沉淀;(c)将步骤(b)中上层清液倒出,加入去离子水到所得沉淀物中,振荡、洗涤,并进行离心,重复上述操作2-3次;(d)将NaOH溶液加入到步骤(c)中反复洗涤的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在一定温度下保持反应一定的时间;(e)在步骤(d)结束后,将所述高压反应釜自然冷却至室温,然后将反应最终产物分别用去离子水和无水乙醇洗涤3-5次,并在60℃的烘箱中干燥12h,得到Bi2Fe4O9纳米片材料。
根据本发明一个实施例,所述NaOH溶液的浓度为10-14mol/L。
根据本发明一个实施例,所述反应温度为在170-190℃。
根据本发明一个实施例,所述反应时间为72h。
根据本发明一个实施例,所述铋盐和铁盐分别包括Bi(NO3)3·5H2O和FeCl3·6H2O。
本发明提供了一种Bi2Fe4O9纳米片材料,其特征在于:所述纳米片材料的粒径尺寸为2-5μm。
根据本发明一个实施例,所述纳米片材料主相为Bi2Fe4O9与JPCDS卡片25-0090相对应。
本发明提供了一种用机械力提供装置纳米片材料应用到降解有机污染物中用途。
根据本发明一个实施例,所述机械力提供装置包括超声波清洗机或磁力搅拌器。
根据本发明一个实施例,所述有机污染物包括磺胺甲恶唑等抗生素类药物和罗丹明等染料类有机物。
本发明以Bi(NO3)3·5H2O和FeCl3·6H2O为前驱体,NaOH溶液为矿化剂采用溶剂热法通过调节反应物浓度、反应温度及时间制备了颗粒均匀、粒径较小、比较面积大、压电催化活性高的Bi2Fe4O9纳米片材料,解决了现有技术中的颗粒尺寸大、催化活性的问题。
附图说明
图1显示了根据实施例1制备的Bi2Fe4O9XRD图谱;
图2显示了根据实施例1制备的Bi2Fe4O9SEM图像;
图3显示了根据实施例2制备的Bi2Fe4O9XRD图谱;
图4显示了根据实施例2制备的Bi2Fe4O9SEM图像;
图5显示了根据实施例1制备的Bi2Fe4O9压电催化氧化降解磺胺甲恶唑;
图6显示了根据实施例1制备的Bi2Fe4O9压电催化氧化降解罗丹明B。
具体实施例
以下将通过实施例结合附图对本发明进行详细说明。
实施例一
将分析纯的Bi(NO3)3·5H2O和FeCl3·6H2O以1:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解。向上述溶液中加入200mL的去离子水,搅拌,然后逐滴加入过量的浓氨水使溶液完全沉淀。倒出上层清液,将去离子水加入到所得沉淀物中,振荡、洗涤并进行离心,重复上述洗涤操作2-3次。将10mol/L的NaOH加入到洗涤完的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在烘箱中180℃下反应72h。反应结束后,关闭烘箱电源,让高压反应釜在烘箱中自然冷却至室温。反应最终产物分别用去离子水和无水乙醇洗涤3-5次,在烘箱中60℃干燥12h,最后得到粉末样品用于粉末X射线衍射表征,如图1所示,所制备的粉末衍射峰与标准卡片25-0090的一一对应,结果证明所制备的粉末主相为Bi2Fe4O9。此外,峰强较高且半峰宽较小,说明所制备的Bi2Fe4O9纳米片的结晶度较高且粒径尺寸较小为2-5μm(如图2所示)。
实施例二
将分析纯的Bi(NO3)3·5H2O和FeCl3·6H2O以1:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解。向上述溶液中加入200mL的去离子水,搅拌,然后逐滴加入过量的浓氨水使溶液完全沉淀。倒出上层清液,将去离子水加入到所得沉淀物中,振荡、洗涤并进行离心,重复上述洗涤操作2-3次。将14mol/L的NaOH加入到洗涤完的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在烘箱中180℃下反应72h。反应结束后,关闭烘箱电源,让高压反应釜在烘箱中自然冷却至室温。反应最终产物分别用去离子水和无水乙醇洗涤3-5次,在烘箱中60℃干燥12h,最后得到粉末样品用于粉末X射线衍射表征,如图3所示,所制备的粉末衍射峰与标准卡片25-0090的一一对应,结果证明所制备的粉末主相为Bi2Fe4O9。此外,峰强较高且半峰宽较小,说明所制备的Bi2Fe4O9纳米片的结晶度较高且粒径尺寸较小为2-5μm(如图4所示)。
实施例三
将分析纯的Bi(NO3)3·5H2O和FeCl3·6H2O以0.7:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解。向上述溶液中加入200mL的去离子水,搅拌,然后逐滴加入过量的浓氨水使溶液完全沉淀。倒出上层清液,将去离子水加入到所得沉淀物中,振荡、洗涤并进行离心,重复上述洗涤操作2-3次。将10mol/L的NaOH加入到洗涤完的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在烘箱中180℃下反应72h。反应结束后,关闭烘箱电源,让高压反应釜在烘箱中自然冷却至室温。反应最终产物分别用去离子水和无水乙醇洗涤3-5次,在烘箱中60℃干燥12h,最后得到粉末样品用于粉末X射线衍射表征,所制备的粉末衍射峰与标准卡片25-0090的一一对应,结果证明所制备的粉末主相为Bi2Fe4O9。
实施例四
将分析纯的Bi(NO3)3·5H2O和FeCl3·6H2O以0.9:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解。向上述溶液中加入200mL的去离子水,搅拌,然后逐滴加入过量的浓氨水使溶液完全沉淀。倒出上层清液,将去离子水加入到所得沉淀物中,振荡、洗涤并进行离心,重复上述洗涤操作2-3次。将10mol/L的NaOH加入到洗涤完的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在烘箱中180℃下反应72h。反应结束后,关闭烘箱电源,让高压反应釜在烘箱中自然冷却至室温。反应最终产物分别用去离子水和无水乙醇洗涤3-5次,在烘箱中60℃干燥12h,最后得到粉末样品用于粉末X射线衍射表征,所制备的粉末衍射峰与标准卡片25-0090的一一对应,结果证明所制备的粉末主相为Bi2Fe4O9。
实施案例五
将分析纯的Bi(NO3)3·5H2O和FeCl3·6H2O以0.7:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解。向上述溶液中加入200mL的去离子水,搅拌,然后逐滴加入过量的浓氨水使溶液完全沉淀。倒出上层清液,将去离子水加入到所得沉淀物中,振荡、洗涤并进行离心,重复上述洗涤操作2-3次。将14mol/L的NaOH加入到洗涤完的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在烘箱中180℃下反应72h。反应结束后,关闭烘箱电源,让高压反应釜在烘箱中自然冷却至室温。反应最终产物分别用去离子水和无水乙醇洗涤3-5次,在烘箱中60℃干燥12h,最后得到粉末样品用于粉末X射线衍射表征,所制备的粉末衍射峰与标准卡片25-0090的一一对应,结果证明所制备的粉末主相为Bi2Fe4O9。
磺胺甲恶唑降解实验
使用超声波清洗机(US)提供机械力使根据实施例一制备的Bi2Fe4O9变形产生压电效应。50mL棕色试剂瓶作为反应器放置在超声波清洗机中,反应通过打开超声波清洗机提供外力而开始,棕色试剂瓶可以消除外界可见光的干扰。压电催化降解效果如图5所示,超声单独作用下,磺胺甲恶唑去除率为4%,超声辅助下Bi2Fe4O9压电催化氧化去除率为35%,反应条件下为在10ml过磺胺甲恶唑溶(20μmol/L)中加入40㎎Bi2Fe4O9,处理时间1h,取一次样品,经0.22μm滤膜后通过超高效液相色谱仪分析、计算磺胺甲恶唑浓度。
罗丹明B降解实验
将根据实施例一制备的Bi2Fe4O9分散到罗丹明B溶液中,采用磁力搅拌器带动溶液高速旋转产生的强大剪切力作用在Bi2Fe4O9纳米片上,通过压电效应产生电子和空穴,降解模型污染物罗丹明B,不同转速下罗丹明B的降解效果如图6所示,随着转速增大,去除率逐渐增大,当转速为1500rpm时,罗丹明B去除率为56.3%,反应条件为在10ml过罗丹明B溶液(5mg/L)中加入40㎎Bi2Fe4O9,处理时间2h,经0.22μm滤膜后使用紫外可见分光光度法测量、特征吸收峰为554nm。
应当理解,上述实施例仅为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种制备Bi2Fe4O9纳米片材料的方法,包括如下步骤:
(a)将分析纯的铋盐和铁盐以0.7-1.2:1的摩尔比溶于乙二醇溶液,充分搅拌至完全溶解;
(b)向步骤(a)中所形成的溶液加入去离子水并搅拌均匀,然后逐滴加入过量的浓氨水至溶液完全沉淀;
(c)将步骤(b)中上层清液倒出,加入去离子水到所得沉淀物中,振荡、洗涤,并进行离心,重复上述操作;
(d)将NaOH溶液加入到步骤(c)中反复洗涤的沉淀物中,搅拌30min,形成溶液并装入具有聚四氟乙烯内衬的不锈钢高压反应釜中,在一定温度下保持反应一定的时间;
(e)在步骤(d)结束后,将所述高压反应釜自然冷却至室温,然后将反应最终产物分别用去离子水和无水乙醇洗涤,并在60℃的烘箱中干燥12h,得到Bi2Fe4O9纳米片材料。
2.根据权利要求1所述的方法,所述NaOH溶液的浓度为10-14mol/L。
3.根据权利要求1所述的方法,所述反应温度为在170-190℃。
4.根据权利要求1所述的方法,所述反应时间为72h。
5.根据权利要求1所述的方法,所述铋盐和铁盐分别包括Bi(NO3)3·5H2O和FeCl3·6H2O。
6.一种根据权利要求1-5中任一项所述的方法制备的Bi2Fe4O9纳米片材料,其特征在于:所述纳米片材料的粒径尺寸为2-5μm。
7.根据权利要求6所述的纳米片材料,所述纳米片材料主相为Bi2Fe4O9与JPCDS卡片25-0090相对应。
8.一种用机械力提供装置将权利要求6或7中所述的纳米片材料应用到降解有机污染物中用途。
9.根据权利要求8所述的用途,所述机械力提供装置包括超声波清洗机或磁力搅拌器。
10.根据权利要求8所述的用途,所述有机污染物包括磺胺甲恶唑等抗生素类药物和罗丹明等染料类有机物。
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