CN105833887A - 一种BiOCl/β-FeOOH复合纳米材料及其制备方法 - Google Patents
一种BiOCl/β-FeOOH复合纳米材料及其制备方法 Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910003153 β-FeOOH Inorganic materials 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 10
- 239000008103 glucose Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 9
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
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- 239000010865 sewage Substances 0.000 abstract description 2
- 239000002073 nanorod Substances 0.000 abstract 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 239000002135 nanosheet Substances 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 43
- 239000000243 solution Substances 0.000 description 28
- 239000000047 product Substances 0.000 description 17
- 238000013019 agitation Methods 0.000 description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 239000012028 Fenton's reagent Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition-metal sulphides Chemical class 0.000 description 1
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Abstract
一种BiOCl/β‑FeOOH复合纳米材料及其制备方法,涉及复合纳米材料技术领域。先将FeCl3·6H2O溶解于蒸馏水中,再依次加入Bi(NO3)3·5H2O、葡萄糖后混合均匀,调节pH值至3~6,然后经水热合成反应得到BiOCl/β‑FeOOH复合纳米材料。采用低温水热法合成,通过葡萄糖生物大分子来控制β‑FeOOH纳米棒在BiOCl纳米片上的附着生长,在BiOCl/β‑FeOOH纳米复合材料的结构中,呈纺锤形的β‑FeOOH纳米棒分布在呈片状的BiOCl上,这种纳米复合材料具有较高的比表面积、优异的光催化和类芬顿催化活性等优点,可望用作脱除污水中各类有机污染物的有效催化剂。
Description
技术领域
本发明涉及复合纳米材料技术领域,具体是涉及一种BiOCl/β-FeOOH复合纳米材料及其制备方法。
背景技术
羟基氧化铁(β-FeOOH)是一种性能优良的功能材料,可用作颜料、催化剂、磁记录介质的前驱体、磁性涂料和气体传感器等。具有成本低廉和较高的比表面积,可用作吸附剂和类芬顿试剂,在催化、医药和生物领域有着重要的应用价值。
氯氧化铋(BiOCl)作为过渡族金属硫化物,纳米BiOCl具有比表面积大,可作为光催化剂来去除有机污染物。然而,纳米BiOCl光催化剂对可见光响应范围狭小的,因而,其可见光催化效应不明显。已研究表明,β-FeOOH和BiOCl都为层状结构,这为两者的复合提供可能的依据。目前,关于利用β-FeOOH来调控BiOCl光催化性能方面的研究报道较少。
发明内容
为了克服现有技术中存在的上述缺陷,本发明的目的在于提供了一种BiOCl/β-FeOOH复合纳米材料及其制备方法,获得的复合材料具有优异的可见光和类芬顿双重催化功能。
为实现该目的,本发明采用了以下技术方案:
一种BiOCl/β-FeOOH复合纳米材料,呈纺锤形的β-FeOOH纳米棒分布在呈片状的BiOCl上。
一种BiOCl/β-FeOOH复合纳米材料的制备方法,先将FeCl3·6H2O溶解于蒸馏水中,再依次加入Bi(NO3)3·5H2O、葡萄糖后混合均匀,调节pH值至3~6,然后经水热合成反应得到BiOCl/β-FeOOH复合纳米材料。
作为上述制备方法的进一步改进,反应体系中FeCl3·6H2O、Bi(NO3)3·5H2O和葡萄糖的质量浓度依次为0.27~1.35g/mL、0.485~7.276g/mL、3.5~8.5g/L。水热合成反应的时间为24~48h,反应温度为80~100℃。水热合成反应产物经固液分离、洗涤、烘干得到复合纳米材料,烘干温度为60~80℃,烘干时间为2~6h。
与现有技术相比,本发明的有益效果表现在:
1、本发明采用低温水热法合成,通过葡萄糖生物大分子来控制β-FeOOH纳米棒在BiOCl纳米片上的附着生长,在BiOCl/β-FeOOH纳米复合材料的结构中,呈纺锤形的β-FeOOH纳米棒分布在呈片状的BiOCl上,这种纳米复合材料具有较高的比表面积、优异的光催化和类芬顿催化活性等优点,可望用作脱除污水中各类有机污染物的有效催化剂。另外,在颜料和磁性元件等方面上也有潜在的应用价值。
2、本发明制备方法工艺简单,整个制备体系容易构建、操作简便、条件易控、成本低廉、产物组成可控、适合于大规模工业生产。采用常规可溶性铁盐作为反应物,在制备过程中产生的副产物少,对环境污染较小,是一种环保型合成工艺。
附图说明
图1是实施例1所得产物的XRD谱图
图2a是实施例1所得产物的扫描电镜图像。
图2b是对单个BiOCl/β-FeOOH复合片的面扫描能谱分析图。
图3a是实施例1所得产物的低倍率TEM投射照片。
图3b是BiOCl和β-FeOOH的电子衍射分析结果。
图4是β-FeOOH、BiOCl和β-FeOOH/BiOCl三者的紫外-可见吸收光谱图。
图5是β-FeOOH、BiOCl和β-FeOOH/BiOCl复合材料光催化降解甲基橙的动力学曲线。
具体实施方式
以下结合实施例以及附图对本发明作进一步详细描述。
实施例1
(1)、将27g的FeCl3·6H2O溶解在100mL蒸馏水中,室温下磁力搅拌2分钟使之充分溶解得到溶液a。
(2)、称取48.5g的Bi(NO3)3·5H2O加入到上述溶液a中,继续磁力搅拌1分钟得到溶液b。
(3)、称0.35g的葡萄糖加入到溶液b中,用HCl溶液调节溶液pH为3,得到溶液c。
(4)、将溶液c装入反应釜中进行水热合成反应,反应时间为24h,反应温度为100℃。
(5)、反应结束后取出产物,经过洗涤、离心和干燥,得到目标产物,烘干温度为70℃,烘干时间为4h。
图1为实施例1所得产物的XRD谱图。将产物的XRD所有衍射峰与标准BiOCl(PDF#34-1266)与β-FeOOH(PDF#06-0249)的XRD谱图进行对比分析,可以看出,所得产物中出现了BiOCl和β-FeOOH的特征衍射峰,可以初步确定所得的产物为BiOCl/β-FeOOH复合物,且两者的结晶度较高。
图2a是实施例1所得产物的扫描电镜图像,从图中可以看出在片状的BiOCl上分布着纺锤形的β-FeOOH纳米棒,片状BiOCl的尺寸约为几个微米。图2b是对单个BiOCl/β-FeOOH复合片进行了面扫描能谱分析图,从分析结果中可以看出,Bi和Cl元素的分布均匀,且形状基本一致,而Fe和O元素分布区域基本一致。结合图1的XRD和图2b的能谱分析结果,可初步认为得到的产物为BiOCl/β-FeOOH复合片。
为了进一步确认复合纳米片中的BiOCl和β-FeOOH两者的结合关系,对产物进行了TEM和HRTEM分析,其结果如图3所示。图3a为产物的低倍投射照片,由图3a可以清晰看出,复合纳米片是由片状的BiOCl和纺锤形的β-FeOOH构成。图3b为两者的电子衍射分析结果,从图3b中标注的结果进一步可以证明,复合纳米片中BiOCl和β-FeOOH位向关系,两者依附生长在一起,结晶程度高。
图4是β-FeOOH、BiOCl和β-FeOOH/BiOCl三者的紫外-可见吸收光谱图。从图4中可以看出,纯的BiOCl和β-FeOOH的吸收峰均在360nm左右,说明两者在可见光范围内(>420nm)内吸收不明显。而BiOCl/β-FeOOH复合纳米片最大吸收峰为480nm左右,说明获得的BiOCl/β-FeOOH复合纳米材料具有良好的可见光吸收性能。
实施例2
(1)、将135g的FeCl3·6H2O溶解在100mL蒸馏水中,室温下磁力搅拌3分钟使之充分溶解得到溶液a。
(2)、称取48.5g的Bi(NO3)3·5H2O加入到上述溶液a中,继续磁力搅拌1分钟得到溶液b。
(3)、称0.55g的葡萄糖加入到溶液b中,用HCl溶液调节溶液pH为4,得到溶液c。
(4)、将溶液c装入反应釜中进行水热合成反应,反应时间为48h,反应温度为80℃。
(5)、反应结束后取出产物,经过洗涤、离心和干燥,得到目标产物,烘干温度为80℃,烘干时间为2h。
实施例3
(1)、将27g的FeCl3·6H2O溶解在100mL蒸馏水中,室温下磁力搅拌1分钟使之充分溶解得到溶液a。
(2)、称取727.6g的Bi(NO3)3·5H2O加入到上述溶液a中,继续磁力搅拌3分钟得到溶液b。
(3)、称0.85g的葡萄糖加入到溶液b中,用HCl溶液调节溶液pH为6,得到溶液c。
(4)、将溶液c装入反应釜中进行水热合成反应,反应时间为36h,反应温度为90℃。
(5)、反应结束后取出产物,经过洗涤、离心和干燥,得到目标产物,烘干温度为60℃,烘干时间为6h。
实施例4(BiOCl/β-FeOOH纳米复合材料光催化降解污染物)
(1)、以甲基橙为目标污染物,在100mL甲基橙初始浓度为20mg/L的溶液中加入0.1g所制备的BiOCl/β-FeOOH复合材料,快速均匀分散后得到混合液a,然后放入光催化装置中进行光催化实验。
(2)、光照t1分钟后,从a溶液中取出10mL进行离心分离,得到上清液b。
(3)、用紫外-可见光谱仪测试溶液b的吸光度A1,测试完毕后,倒回试管并连同剩余的溶液和催化剂摇匀后倒回到溶液a中,继续进行光催化实验。
(4)、光照t2分钟、t3分钟和t4分钟、t5分钟和t6分钟后的取样和测试过程与(2)和(3)两步完全相同,测得的系列吸光度分别标记为A2、A3、A4、A5和A6。
(5)、作时间ti和吸光度Ai(i=0,1,2,3,4,5,6)曲线。再依据吸光度A和浓度C关系(朗伯比尔定律)计算得到吸附时间t和浓度Ct的关系曲线。
图5是β-FeOOH、BiOCl和β-FeOOH/BiOCl复合材料光催化降解甲基橙的动力学曲线。对比三者的可见光催化动力学曲线后可以看出,BiOCl和β-FeOOH可见光催化效果不明显,而BiOCl/β-FeOOH复合材料能有效光催化降解甲基橙。
Claims (5)
1.一种BiOCl/β-FeOOH复合纳米材料,其特征在于:呈纺锤形的β-FeOOH纳米棒分布在呈片状的BiOCl上。
2.一种BiOCl/β-FeOOH复合纳米材料的制备方法,其特征在于先将FeCl3·6H2O溶解于蒸馏水中,再依次加入Bi(NO3)3·5H2O、葡萄糖后混合均匀,调节pH值至3~6,然后经水热合成反应得到BiOCl/β-FeOOH复合纳米材料。
3.如权利要求1所述的BiOCl/β-FeOOH复合纳米材料的制备方法,其特征在于反应体系中FeCl3·6H2O、Bi(NO3)3·5H2O和葡萄糖的质量浓度依次为0.27~1.35g/mL、0.485~7.276g/mL、3.5~8.5g/L。
4.如权利要求1所述的BiOCl/β-FeOOH复合纳米材料的制备方法,其特征在于水热合成反应的时间为24~48h,反应温度为80~100℃。
5.如权利要求1所述的BiOCl/β-FeOOH复合纳米材料的制备方法,其特征在于水热合成反应产物经固液分离、洗涤、烘干得到复合纳米材料,烘干温度为60~80℃,烘干时间为2~6h。
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