CN106082307A - 一种氧化锌纳米软管的制备方法 - Google Patents
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 15
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- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
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- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
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Abstract
本发明涉及一种氧化锌纳米软管的制备方法。其利用水热法可控合成氧化锌纳米软管。其制备的氧化锌纳米软管可作为光催化降解环境污染物的催化剂，在紫外光的照射下，实现了对甲基橙的快速、高效、彻底降解。
Description
技术领域
本发明属于纳米材料技术领域，具体涉及一种氧化锌纳米软管的制备方法。
背景技术
光催化氧化法是近几十年来发展起来的一种先进的氧化技术。它是将特定光源（如紫外光）与催化剂（ZnO、TiO2等）联合作用对有机废水进行降解处理的过程。光催化氧化法与传统水处理技术中以污染物的分离、浓缩以及相转移等为主的物理方法相比，具有明显的节能、快速、高效、污染物降解彻底等优点。
ZnO是典型的直接带隙宽禁带半导体材料，在室温下其禁带宽度约为3.37 eV。与普通的氧化锌相比，氧化锌纳米软管在太阳能电池、表面声波和压电材料、场发射、纳米激光等光电技术领域具有重要的潜在应用价值，其在光催化氧化法中的应用也引起了人们的重视。
目前，氧化锌纳米材料的制备方法多种多样，主要有:射频溅射法、双离子束溅射沉积法、化学气相沉积法、分子束蒸发沉积、脉冲激光沉积、喷雾热分解法以及溶胶一凝胶法等，但是，以上方法都比较繁琐，制备过程较为复杂、纳米形貌不好控制。
发明内容
针对现有技术的不足，本发明提供一种氧化锌纳米软管的制备方法，利用水热法可控合成氧化锌纳米软管，制备的氧化锌纳米软管可作为光催化降解环境污染物的催化剂，在紫外光的照射下，实现对甲基橙的快速、高效、彻底降解。
本发明采用的技术方案是：
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗；超声清洗时间为10-20min，可以达到活化表面、在表面生成氧化锌纳米种子的目的；
b、将无水乙醇、油酸、盐酸混合均匀后加入反应釜中，将处理过的表面洁净的锌片浸入混合液中，将反应釜密闭，在40 oC-80 oC下反应2-8小时，冷却至室温，清洗，室温干燥，即制得氧化锌纳米软管。所述无水乙醇和盐酸的体积比为20-60: 1。；所述盐酸的浓度≥12mol/L。
本发明一种氧化锌纳米软管的制备方法，是在密闭的高温高压反应釜中，采用无水乙醇作为反应溶剂，加入油酸和盐酸混合均匀，通过加热反应体系，产生一个高压环境而进行材料制备的一种有效方法。本发明制备方法产物纯度高、分散性好、晶形好且可控制，生产成本低，重现性好。所制备出的氧化锌纳米软管可作为光催化降解环境污染物的催化剂，在紫外光的照射下，实现对污染物甲基橙的高效、快速、彻底降解。
附图说明
图1为实施例1制备的氧化锌纳米软管的扫描电子显微镜照片（SEM）；
图2为实施例2制备的氧化锌纳米软管的扫描电子显微镜照片（SEM）；
图3为实施例3制备的氧化锌纳米软管的扫描电子显微镜照片（SEM）；
图4为实施例4制备的氧化锌纳米软管的扫描电子显微镜照片（SEM）；
图5为实施例5制备的氧化锌纳米软管的扫描电子显微镜照片（SEM）。
具体实施方式
实施例1
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗15min；
b、将20 mL无水乙醇、2 mL油酸和0. 6 mL 12 mol/L的盐酸混合均匀后加入60 mL反应釜中，将处理过的锌片浸入混合液中，拧紧釜盖，在70 oC下反应5小时，取出反应釜自然冷却至室温，依次用乙醇、二次蒸馏水冲洗干净，室温干燥，即制得氧化锌纳米软管。
制备的氧化锌纳米软管与锌制电极的质量面积比为0.0175g/cm2。
将实施例1制备的氧化锌纳米软管，作为光催化降解环境污染物的催化剂，在紫外光的照射下实现了对污染物甲基橙的快速、高效、彻底降解。
配制浓度50 mg/L 100 mL的甲基橙溶液，加入0.05 g制备的氧化锌纳米软管，磁力搅拌1小时，实现吸附和脱附平衡，在300 W紫外灯的照射下进行反应，光源距离液面10cm,同时进行电磁搅拌。每隔5 min取一次样，先将样品按8000 r/min的转速离心旋转10min，分离出上清液，再将所得的上清液按10000 r/min的转速离心旋转15 min,分离出上清液。
在UV-754型紫外可见分光光度计上，在甲基橙最大吸收波长464nm处测量其在不同时间段的吸光度。通过不同时间段吸光度计算甲基橙的降解率为D=[(A0-As)/A0]×100%，其中：A0为光照分解前甲基橙的吸光度，As为光照分解后甲基橙的吸光度。通过In(C0/Ct)=kt得出一级反应的线性关系。其中：C0为甲基橙的原始浓度，Ct为反应一段时间后甲基橙的浓度。
实施例2
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗15min；
b、将20 mL无水乙醇、2 mL油酸和0. 6 mL 12 mol/L的盐酸混合均匀后加入60 mL反应釜中，将处理过的锌片浸入混合液中，拧紧釜盖，在100 oC下反应5小时，取出反应釜自然冷却至室温，依次用乙醇、二次蒸馏水冲洗干净，室温干燥，即制得氧化锌纳米软管。
实施例3
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗15min；
b、将20 mL无水乙醇、3 mL油酸和0. 8 mL 12 mol/L的盐酸混合均匀后加入60 mL反应釜中，将处理过的锌片浸入混合液中，拧紧釜盖，在80 oC下反应5小时，取出反应釜自然冷却至室温，依次用乙醇、二次蒸馏水冲洗干净，室温干燥，即制得氧化锌纳米软管。
实施例4
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗15min；
b、将20 mL无水乙醇、1 mL油酸和1 mL 12 mol/L的盐酸混合均匀后加入60 mL反应釜中，将处理过的锌片浸入混合液中，拧紧釜盖，在60 oC下反应5小时，取出反应釜自然冷却至室温，依次用乙醇、二次蒸馏水冲洗干净，室温干燥，即制得氧化锌纳米软管。
实施例5
一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗15 min；
b、将20 mL无水乙醇、4 mL油酸和0. 6 mL 13 mol/L的盐酸混合均匀后加入60 mL反应釜中，将处理过的锌片浸入混合液中，拧紧釜盖，在40 oC下反应5小时，取出反应釜自然冷却至室温，依次用乙醇、二次蒸馏水冲洗干净，室温干燥，即制得氧化锌纳米软管。
Claims (4)
1.一种氧化锌纳米软管的制备方法，包括以下步骤：
a、将锌片依次放入乙醇、水中进行超声清洗；
b、将无水乙醇、油酸、盐酸混合均匀后加入反应釜中，将处理过的表面洁净的锌片浸入混合液中，将反应釜密闭，在40 oC-100 oC下反应2-8小时，冷却至室温，清洗，室温干燥，即制得氧化锌纳米软管。
2.如权利要求1所述氧化锌纳米软管的制备方法，其特征在于：所述步骤a中超声清洗时间为10-20 min。
3.如权利要求1所述氧化锌纳米软管的制备方法,其特征在于：所述步骤b中所述无水乙醇和盐酸的体积比为20-60: 1;无水乙醇和油酸的体积比为10-20: 1。
4.如权利要求1所述氧化锌纳米软管的制备方法，其特征在于：所述步骤b中盐酸的浓度≥12 mol/L。
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| CN102161499A (zh) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | 一种量子尺寸氧化锌及其制备方法和应用 |
| CN104828855A (zh) * | 2015-05-05 | 2015-08-12 | 上海交通大学 | 超长层级结构ZnO晶须及其基于水热离子诱导技术制备方法 |
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| JP2008024556A (ja) * | 2006-07-21 | 2008-02-07 | Tokyo Univ Of Science | 金属酸化物粉末の製造方法、及び当該製造方法により得られる金属酸化物粉末 |
| CN101559973A (zh) * | 2009-05-18 | 2009-10-21 | 清华大学 | 以工业硫酸锌为原料制备纳米氧化锌和晶须氧化锌的方法 |
| CN102161499A (zh) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | 一种量子尺寸氧化锌及其制备方法和应用 |
| CN104828855A (zh) * | 2015-05-05 | 2015-08-12 | 上海交通大学 | 超长层级结构ZnO晶须及其基于水热离子诱导技术制备方法 |
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