CN104645965A - 一种用于光催化的铋-氧化钛纳米线材料及制备方法 - Google Patents

一种用于光催化的铋-氧化钛纳米线材料及制备方法 Download PDF

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CN104645965A
CN104645965A CN201510121107.6A CN201510121107A CN104645965A CN 104645965 A CN104645965 A CN 104645965A CN 201510121107 A CN201510121107 A CN 201510121107A CN 104645965 A CN104645965 A CN 104645965A
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bismuth
titanium oxide
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陈俊芳
陈源
卢秋菊
张敏
陈冬玲
潘远均
徐斌
刘碧桃
刘代军
涂铭旌
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Chongqing University of Arts and Sciences
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Abstract

本发明涉及一种用于光催化的铋-氧化钛纳复合米线及制备方法，属于无机纳米材料领域。铋-氧化钛纳复合米线的制备为：将聚乙烯吡咯烷酮(PVP)、硝酸铋加入到N-N二甲基酰胺（DMF）中，磁力搅拌一段时间后加入钛酸四丁酯和乙酰丙酮，再持续搅拌6小时以上，得到透明稳定的溶液。将溶液在静电纺丝发生装置中于一定条件下进行电纺，得到的电纺前驱纳米纤维首先在马弗炉中进行空烧以除去有机物。冷却至室温后，再放入管式炉中于氢气气氛下还原烧结。本方法节能环保，条件易于控制，成本低廉，容易大规模工业化生产。得到的铋-氧化钛纳米线在光照下对甲基橙表现出良好的降解活性，反应20 min时甲基橙降解率达到95%以上，在污水处理方面具有广阔的应用前景。

Description

一种用于光催化的铋-氧化钛纳米线材料及制备方法
技术领域
本发明属于无机纳米材料和环境污染治理技术领域，具体涉及一种可用于降解污染物（染料）的具有高效光催化活性的铋-氧化钛纳米线材料及制备方法。
背景技术
随着人口的急剧膨胀和工业的快速发展，环境污染问题已经成为影响人类生产、生活的首要问题。各国政府都将环境污染治理列为现阶段以及未来几年的头等大事。特别是印染行业中甲基橙等大量水溶性偶氮染料的大量排放，使人类赖以生存的水质日益恶化。这些污染物质多难生物降解，一旦进入水体，由于其在水体中自然降解过程缓慢，其危害性延滞较长。光催化反应可以将污染物在光照条件下完全矿化为各种无机离子，因此在环境治理方面得到了广泛关注，关于光催化剂的研发，成为目前国内外的研究热点。
纳米氧化钛由于具有尺寸小、比表面积大、表面原子配位不全等特点，从而导致其表面的活性位较多，形成了凸凹不平的原子台阶，在作为催化剂使用时可以增大与反应物的接触面积，因此，和传统催化剂相比，具有更高的催化活性。在光催化领域，纳米氧化钛作为催化剂时能使水中的有害有机物质最终分解，避免其对环境的污染。研究表明，纳米氧化钛的反应速度是大块氧化钛材料的100~1000倍，而且与普通粒子相比，纳米氧化钛几乎不会引起光的散射，因此是极具应用前景的光催化剂之一。
到目前为止，人们已经通过制备多种多样的氧化钛纳米复合材料对氧化钛进行性能良，如氧化锡-氧化钛复合材料，氧化锌-氧化钛复合材料等。虽然方法很多，但仍都存在一些不足，目前得到的氧化钛复合材料对污染物的降解效率仍待提高。寻求价廉、环境友好并具有高催化活性的光催化材料是光催化技术发展的关键。
发明内容
本发明的目的在于克服现有技术的不足，提供一种可用于降解污染物（染料）的具有高效光催化活性的铋-氧化钛纳米线材料及制备方法。
本发明提供的铋-氧化钛纳米线的制备方法，其特征在于采用一种静电纺丝发生装置进行制备，该方法节能环保，条件易于控制，原材料广泛，成本低廉，容易大规模工业化生产。所得铋-氧化钛纳米线在污染物治理方面具有很好的应用前景。具体包括以下步骤：
(1)   首先，将聚乙烯吡咯烷酮(PVP)、硝酸铋加入到N-N二甲基酰胺（DMF）中，磁力搅拌一段时间后加入钛酸四丁酯和乙酰丙酮，再持续搅拌6小时以上，得到透明稳定的溶胶。
(2)   将步骤（1）所述溶胶溶液在静电纺丝发生装置中于一定条件下进行电纺。
(3)将步骤(2)得到的电纺前驱纳米纤维首先在马弗炉中以5℃/min的升温速率进行空烧以除去有机物。
(4)冷却至室温后，放入管式炉中于氢气气氛下还原烧结。
本发明中，步骤（1）中所述透明稳定溶液指经过6h磁力搅拌后溶液中无肉眼可见的不容物质；.步骤（2）中电纺过程必须在一定条件下进行，其中包括：环境温度大于20℃，湿度小于85%RH，纺丝电压8~25 KV,针头直径0.6~1.2 mm，针头与接收器距离15~25 cm；步骤（3）中在马弗炉中焙烧过程采用阶段程序升温，先以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温；步骤（4）中在管式中焙烧过程采用氢气气氛焙烧，先以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温。
与现有技术相比，本发明具有如下有益效果：
本发明方法采用静电纺丝法为制备工艺，原料简单易得，通过氢气还原过程获得了复合材料，整个实验过程过程简单，操作方便，很容易实现产物的大规模生产，所得铋-氧化钛氧化锌纳米线均匀、连续，具有较大的长径比，对染料甲基橙的降解具有很好的催化效果。
附图说明
图1 是制备的铋-氧化钛纳米线的XRD图。
图2 是制备的铋-氧化钛纳米线的SEM图。
图3 是制备的铋-氧化钛纳米线的TEM图。
图4是制备的铋-氧化钛纳米线对甲基橙降解反应的光催化效果图。
具体实施方式
下面结合实施例对本发明进行进一步说明。本发明的生产技术对本专业的人来说是容易实施的。本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和过程，但本发明的保护范围不限于下述的实施例。下列实施例中未注明具体条件的实验方法，通常按照常规条件，或按照制造厂商所建议的条件。
实施例
用电子天平分别称取0.6g聚乙烯吡咯烷酮(PVP)、4g硝酸铋加入到装有8g N-N二甲基酰胺（DMF）的烧杯中，磁力搅拌30min, 然后后加入4钛酸四丁酯和0.4g乙酰丙酮，再持续搅拌6小时，得到透明稳定的溶胶。
将上述溶液移入静电纺丝发生装置中进行电纺，在电放过程中，控制环境温度35℃，湿度80%RH，电压15KV, 针头直径0.9mm，接收距离15cm。电纺过程结束后，得到电纺前驱纳米纤维。
将得到的纳米纤维用镊子收集到坩埚中，放入马弗炉，以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温。
将上述烧结后的纳米线放入管式炉中，通入氢气，以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温。
材料的光催化性能测试
准确称量0.2 g 的铋-氧化钛纳米材料加入500 ml 甲基橙（MO）溶液（40 mg/L）中，超声分散；所得悬浮液避光搅拌1 h 使材料达到吸附平衡；平衡后取出3 ml 悬浮液，将剩余悬浮液倒入500 ml 石英管中，然后放入光催化反应仪中；开启500 W 高压汞灯照射，每隔5 min取3 ml 悬浮液于离心管中，总反应时间55 min ；反应结束，取出的各个样品经离心分离后，取上清液用紫外-可见分光光度计测其在465 nm 左右的吸光度，从而反映各个降解时间段后剩余甲基橙的浓度，以此来反映本方法制得铋-氧化钛光催化剂降解甲基橙的效果。

Claims (7)

1.一种用于光催化的铋-氧化钛复合纳米线材料，其特征在于该材料微观结构为直径约200 nm的线状结构，成分为JCPDS 编号44-1246的铋金属和编号为21-1272的金红石结构的氧化钛。
2.如权利要求1所述的氧化锌纳米片材料的制备方法，其特征在于具体合成步骤如下
(1) 首先，将聚乙烯吡咯烷酮(PVP)、硝酸铋加入到N-N二甲基酰胺（DMF）中，磁力搅拌一段时间后加入钛酸四丁酯和乙酰丙酮，再持续搅拌6小时以上，得到透明稳定的溶胶；
(2) 将步骤（1）所述溶胶溶液在静电纺丝发生装置中于一定条件下进行电纺；
(3)将步骤(2)得到的电纺前驱纳米纤维首先在马弗炉中以5℃/min的升温速率进行空烧以除去有机物；
(4)冷却至室温后，放入管式炉中于氢气气氛下还原烧结。
3.如权利要求2所述的铋-氧化钛纳米线的制备方法，其特征在于采用一种静电纺丝发生装置进行制备，该方法节能环保，条件易于控制，成本低廉，容易大规模工业化生产。
4.如权利要求2所述的铋-氧化钛纳米线材料的制备方法，其特征在于步骤（1）中溶液必须持续搅拌至透明稳定。
5.如权利要求2所述的铋-氧化钛纳米线材料的制备方法，其特征在于步骤（2）中电纺过程必须在一定条件下进行，其中包括：环境温度大于20℃，湿度小于85，纺丝电压8~25KV,针头直径0.6~1.2mm，针头与接收器距离15~25cm。
6.如权利要求2所述的铋-氧化钛纳米线材料的制备方法，其特征在于步骤（3）中在马弗炉中焙烧过程采用阶段程序升温，先以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温。
7.如权利要求2所述的铋-氧化钛纳米线材料的制备方法，其特征在于步骤（4）中在管式中焙烧过程采用氢气气氛焙烧，以5℃/min的加热速率从室温加热至200℃，然后继续以10℃/min的加热速率升温至600℃焙烧2h，最后自然冷却到室温。
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