CN106475123B - 一种高比表面积低能隙碳掺杂二氧化钛粉体及其制备方法 - Google Patents
一种高比表面积低能隙碳掺杂二氧化钛粉体及其制备方法 Download PDFInfo
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Abstract
本发明属于可见光催化材料领域,具体涉及一种高比表面积、低能隙碳掺杂TiO2及其制备方法。本专利利用溶剂热法,用葡萄糖作为碳源和催化剂,制备出高比表面积低能隙碳掺杂TiO2,比表面积为241.908m2/g,孔容积0.1468cm3/g,孔径15.261nm,带隙能为1.55eV,光谱吸收范围包括200‑800nm,可见光下快速降解目标污染物罗丹明B。
Description
技术领域
本发明涉及一种高比表面积、低能隙碳掺杂TiO2粉体及其制备方法,特别是指一种溶剂热法制备高比表面积、低能隙碳掺杂的TiO2粉体,及其在可见光下降解水中污染物的应用。此材料具有良好的吸附性能,可见光催化降解性能,制备工艺操作简单、安全简便。
背景技术
随着全球经济的快速发展,地球上人口激增,环境和能源面临严重的挑战,成为亟待解决的问题。太阳能是一种清洁可持续的能源。开发新型、具有良好光学性能的新型环保材料具有非常重要的意义。
TiO2属于无机半导体材料,带隙能为3.2eV,对紫外光有良好的吸收,化学性质无毒稳定,应用范围包括光催化、染料敏化光伏电池及光催化裂解水制氢等领域。
然而TiO2在实际应用中还存在很多问题。由于TiO2带隙能高(3.2eV)导致了其只能吸收紫外光,而紫外光只占太阳能的不到5%,太阳能利用率低。此外一般TiO2粉体比表面积低,光催化中较少的表面提供较少的活性点,降低了催化效率。碳掺杂能够有效的降低纳米TiO2带隙能,改善可见光吸收性能,提高太阳能利用率。然而,以往的掺杂方法主要用到氢气、甲烷等可燃气体,高温(400-600℃)高压下加热将碳掺杂进TiO2,这种方法不仅危险,碳掺杂量低,可见光吸收性能改善效果有限。
因此如何设计一种制备方法,一方面能够安全简便,避免需要高温高压条件和使用可燃气体;另一方面制备出的TiO2带隙能够低,比表面积高,化学性质稳定有着重要的意义。
发明内容
本发明在于提供一种制备高比表面积、低能隙碳掺杂TiO2的制备方法及其在光催化污水处理中的应用。
为实现上述目的现采用如下技术方案:
利用TiCl3溶液在异丙醇中稳定存在,搅拌时在空气中缓慢氧化,转移到反应釜加热后,在溶剂热条件下与葡萄糖发生反应,反应过程中碳掺杂进TiO2中并发生部分还原形成氧空缺,从而导致了TiO2的带隙能降低,可见光吸收性能改善同时得到的TiO2的比表面积较高。
一种制备高比表面积低能隙碳掺杂TiO2的制备,其特征在于采用以下步骤:
(1)在异丙醇中加入葡萄糖搅拌均匀得到溶液1。
(2)往溶液1中加入TiCl3溶液,敞口搅拌直至溶液1成无色。
(3)将搅拌好的无色溶液加入到反应釜中加热。
(4)将反应好的样品离心洗涤,干燥研磨即可得到样品。
步骤(1)中,每升异丙醇中加入9g葡萄糖。
步骤(2)中的TiCl3溶液和步骤(1)中异丙醇的体积比为1:30;TiCl3溶液的质量浓度为15%。
步骤(3)中的加热温度为180℃,时间为6h。
步骤(4)中的离心清洗过程为先用乙醇清洗2次,再用去离子水清洗2次,离心速率10000rpm,时间10min。
所述碳掺杂TiO2粉体用于水中目标污染物的可见光催化降解。
目标污染物为罗丹明B。
本发明具有如下优点:本发明制备方法采用的是溶剂热法,一方面实验条件安全,避免使用危险气体和高温高压条件;另一方实验步骤简单,一步完成,避免了反复多次操作减少出现误差的可能性。本发明制备的一种高比表面积低能隙碳掺杂TiO2粉体,经过氮气吸附实验计算发现比表面积大(241.908m2/g),孔容积大(0.1468cm3/g),孔径大(15.261nm),见图1。碳掺杂后TiO2的可见光吸收性能明显改善(图2),对可见光吸收相对于纯TiO2的0%提升到60%以上,带隙能降低为1.55eV(图3);碳元素含量为39.5%(图4)。
附图说明
图1为实施例1氮气吸附脱附等温曲线。
图2为实施例1制备TiO2粉体的固体紫外可见光光谱。
图3为根据Kubelka-Munk公式计算出实施例1制备TiO2粉体的带隙能图。
图4为实施例1制备出TiO2粉体元素含量分布图。
图5为实施例2方法得到的光催化曲线。
具体实施方式
一种高比表面积、低能隙碳掺杂TiO2,其特征在于采用以下步骤:
(1)在异丙醇中加入葡萄糖搅拌均匀。
(2)往葡萄糖异丙醇溶液中加入TiCl3溶液,敞口搅拌直至溶液成无色。
(3)将搅拌好的无色溶液加入到反应釜中加热。
(4)将反应好的样品离心洗涤,干燥研磨即可得到样品。
步骤(1)中的葡萄糖浓度为9.00g/L。
步骤(2)中的TiCl3溶液和步骤(1)中异丙醇的体积比例为1:30。
步骤(3)中的加热温度为180℃,时间为6h。
步骤(4)中的离心清洗过程为先用乙醇清洗2次,在用去离子水清洗2次,离心速率10000rpm,时间10min。
将上述制备方法制得的碳掺杂TiO2粉体用于水中罗丹明B的紫外光光催化降解。
下面例举实施例子制备碳掺杂TiO2粉体。
实施例1:高比表面积、低能隙碳掺杂TiO2
烧杯中量取异丙醇30毫升,称量葡萄糖粉末0.27g,磁力搅拌。用移液管移取TiCl3溶液1mL,加入到上述溶液中磁力搅拌,直至溶液由紫色变为无色,时间为30min,再将溶液倒入反应釜中,然后加热,加热温度为180℃,时间为6h。反应完成后,离心洗涤,先用乙醇清洗2次,在用水洗2次,离心速度为10000rpm,时间为10min。最后烘箱中60℃干燥,研磨即得到样品。
按实施例1制备的样品,经氮气吸附脱附检测后测得其比表面积、孔容积和孔径分别为241.908m2/g,0.1468cm3/g和15.261nm,见图1。同时固体紫外可见光谱显示施例1制备的样品吸收范围为200-800nm,根据Kubelka-Munk公式计算出实施例1制备样品的带隙能为1.55eV,见图2和图3。碳元素含量为39.5%(图4)。
实施例2:碳掺杂TiO2粉体在可见光下降解罗丹明B
按实施例1方法制备的碳掺杂TiO2粉体进行降解罗丹明B的实验,罗丹明B溶液的浓度是1×10-5mol L-1;取碳掺杂TiO2粉体50mg,置于100mL上述罗丹明B溶液中,在暗室中搅拌30分钟,然后将溶液置于紫外光被过滤掉的可见光源中,每10分钟取4mL罗丹明B溶液,用紫外-可见分光光度计测出溶液中罗丹明B的特征峰值。
按实施例2得到碳掺杂TiO2粉体紫外光降解罗丹明B的降解曲线,图5为施例1制备得到碳掺杂TiO2粉体的可见光催化曲线,图5可以看出施例1制备的碳掺杂TiO2粉体在可见光照60min后催化降解达到90%以上。
Claims (2)
1.一种高比表面积低能隙碳掺杂二氧化钛粉体的制备方法,所述二氧化钛粉体比表面积为241.908m2/g,孔容积为0.1468cm3/g,孔径为15.261nm,光谱吸收范围包括200-800nm,带隙能大小为1.55eV,对可见光吸收相对于纯TiO2的0%提升到60%以上;在可见光下降解罗丹明B,60min后催化降解达到90%以上,碳元素含量为39.5%;其特征在于具体步骤如下:
(1)在异丙醇中加入葡萄糖搅拌均匀得到溶液1;
(2)往溶液1中加入TiCl3溶液,敞口搅拌直至溶液1成无色;
(3)将搅拌好的无色溶液加入到反应釜中加热;
(4)将反应好的样品离心洗涤,干燥研磨即可得到样品;
步骤(1)中,每升异丙醇中加入9g葡萄糖;
步骤(2)中的TiCl3溶液和步骤(1)中异丙醇的体积比为1:30;TiCl3溶液的质量浓度为15%;
步骤(3)中的加热温度为180℃,时间为6h。
2.如权利要求1所述的一种高比表面积低能隙碳掺杂二氧化钛粉体的制备方法,其特征在于,步骤(4)中的离心清洗过程为先用乙醇清洗2次,再用去离子水清洗2次,离心速率10000rpm,时间10min。
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