CN108557869A - 一种基于细菌纤维素骨架的CdS纳米片制备方法 - Google Patents
一种基于细菌纤维素骨架的CdS纳米片制备方法 Download PDFInfo
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Abstract
本发明涉及一种基于细菌纤维素骨架的CdS纳米片制备方法，包括步骤：细菌纤维素的预处理、CdS纳米片的制备。本发明的有益效果是：通过简单的离子交换，采用水热合成的方法制备出了CdS纳米片。如此制备的CdS对于光催化降解具有高活性。
Description
技术领域
本发明属于纳米材料制备及应用技术领域，涉及一种以无机纤维骨架作为支撑位点制备CdS纳米片光催化剂的方法。
背景技术
光催化技术逐渐成为治理环境污染以及能源短缺问题的最关键的技术之一，并引发了国内外科学家的广泛研究。许多研究工作集中在高效光催化剂的搜索和适当设计上，因为直接使用太阳辐射来驱动反应已被证明是一种科学，有效和绿色的方法。
在过去的几十年中，纳米材料的维度和形貌控制变化呈指数级增长。具有不同形貌的纳米材料，例如纳米颗粒、纳米管、纳米线，作为科学研究和工业应用的潜在***变得越来越重要。其中，二维纳米材料如石墨烯和过渡金属氧化物引起广泛兴趣。这些二维纳米材料的特征在于其纳米级的厚度和亚微米至微米级的横向尺寸，从而具有优异的各向异性性质和高比表面积，这对于各种应用是非常重要的。此外，对于具有微孔特征的多层薄膜重新堆积，二维纳米片显示出巨大的潜力，可赋予新的或增强的性质。例如，用于催化的HTiNbO5纳米片和SnO2纳米粒子/石墨烯纳米片可作为锂电池的电极材料。
然而，从科学和技术重要性的角度来看，不具有层状结构的材料(例如ZnO和CdS)制备出二维纳米片仍然是一项挑战。迄今为止一些典型的合成方法包括液-液界面生长、物理/化学气相沉积、超声辅助液相剥离等已经被开发出来。例如，通过ZnS粉末的热蒸发，Ma等人观察到各种ZnS纳米结构包括纳米片，纳米带等纳米结构的形成。通过蒸发和氧化GaN粉末制备Ga2O3纳米片和纳米带。通过热蒸发金属锌粉末制备具有微米横向尺寸的多层ZnO薄片。然而，这些通过气相沉积工艺获得的纳米片通常形状和尺寸不规则；此外，到目前为止还不清楚原子或离子合理组装成二维片状纳米结构而不是其他稳定形式(例如颗粒)的机理。因此使人们能够制备具有可预测形态和维度的纳米材料的合成方法显然是重要的。
细菌纤维素是具有多长度结构层次有组织的物质，其由自组装的生物大分子和无机纳米粒子组装而成。该材料具有支架结构和分级孔隙率，是可用于制备CdS纳米片的生物纳米复合材料。通过模板矿化和双离子交换以及种子生长来实现。本实验在乙醇溶液中，使用氯化镉和硫脲分别作为Cd2+和S2-前体，优化的CdS纳米片显示出良好的降解性能。生物纳米复合材料泡沫具有柔韧性，整体性和层次多孔性，可实现轻松分离催化剂、快速分子运输和高反应表面积，非常适合从催化剂到能源的广泛应用。用生物大分子代替石油衍生聚合物显现了先进纳米复合材料发展方向的可持续性。目前的工作提供了一种多用途和可持续的策略，用于生产具有“脚手架”结构、等级孔隙率、多种组合物的生物复合材料泡沫。因此，研究这种从一维到二维的纳米材料是特别有意义的。
发明内容
本发明要解决的技术问题是：基于上述问题，本发明提供以细菌纤维素作为支撑位点制备CdS纳米片光催化剂的方法，包括以下步骤：
(1)细菌纤维素处理：细菌纤维素水凝胶由桂林奇宏科技有限公司提供，并对其进行再处理。将细菌纤维素水凝胶在NaOH水溶液中纯化，除去膜中的细菌和残余反应物，然后使用去离子水水洗至pH＝7.0。将水洗后的细菌纤维素剪成小块浸没到液氮中，进行冷冻干燥，获得具有分层结构的细菌纤维素气凝胶。
(2)CdS纳米片的制备：100ml的乙醇溶液中加入0.1M柠檬酸钠、一定浓度的CdCl2，放入50mg细菌纤维素。超声10min，使镉盐均匀沉降在纤维素上，然后向溶液中加入0.7ml浓氨水、0.2M硫脲。将溶液在高压釜中密封，并在烘箱中加热，得到的样品用乙醇清洗几次，清除未负载上去的CdS，然后在真空(80℃，12h)下干燥。
进一步地，所述的步骤(1)中NaOH溶液的浓度是1M，温度是90℃。；
进一步地，所述的步骤(1)中冷冻干燥的时间为12h～48h。；
进一步地，所述的步骤(2)中CdCl2浓度分别是0.025M。；
进一步地，所述的步骤(2)中烘箱温度为150℃，时间为48h。
CdS纳米片光催化剂的应用，用于光催化降解亚甲蓝(MB)溶液，按照下述步骤进行：
称取30mg催化剂放入试管中，加入50mL 25mg/L MB溶液，用500W汞灯作为光源，进行光催化降解反应。暗反应时间为40min，光照后，每10min取次样，进行离心，进而测其吸光度。
本发明的有益效果是：该制备方法较为简单，制备条件容易控制，所制备的光催化剂采用了来源丰富的生物质材料，并利用纤维本身的一维结构制备出纳米级二维片状的CdS。该催化剂，具有无污染，催化效率高等优点，具有一定的应用价值。
附图说明
下面结合附图对本发明进一步说明。
图1是本发明实施例1制备得到的细菌纤维素扫描电镜图；
图2是本发明实施例1制备得到的CdS纳米片催化剂的扫描电镜图；
图3是本发明实施例1制备得到的CdS纳米片催化剂的X射线衍射图；
图4是本发明实施例1制备得到的CdS纳米片催化剂的光降解亚甲蓝的浓度随光照时间变化图(1～5分别对应0.0125M、0.025M、0.05M、0.1M、0.2M的CdCl2)。
具体实施方式
现在结合具体实施例对本发明作进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
(1)细菌纤维素处理：细菌纤维素水凝胶由桂林奇宏科技有限公司提供，并对其进行再处理。将细菌纤维素水凝胶在NaOH水溶液中纯化，除去膜中的细菌和残余反应物，然后使用去离子水水洗至pH＝7.0。将水洗后的细菌纤维素剪成小块浸没到液氮中，进行冷冻干燥，获得具有分层结构的细菌纤维素气凝胶。；
(2)CdS纳米片的制备：100ml的乙醇溶液中加入0.1M柠檬酸钠、一定浓度的CdCl2，放入50mg细菌纤维素。超声10min，使镉盐均匀沉降在纤维素上，然后向溶液中加入0.7ml浓氨水、0.2M硫脲。将溶液在高压釜中密封，并在烘箱中加热，得到的样品用乙醇清洗几次，清除未负载上去的CdS，然后在真空(80℃，12h)下干燥。；
如图1、2的扫面电镜图所示，本实施方式制备的CdS纳米片光催化剂的形貌为纤维骨架之间生长出CdS纳米片，且分布较为均匀。
实施例1所制备的CdS纳米片晶相结构由日本理学D/max 2500PC自转X-射线衍射仪分析，其中，X射线为Cu靶电压40kV，电流100mA，步长为0.02°，扫描范围5°～80°。X射线衍射图谱如图3所示，随着CdS量的增大细菌纤维素的特征峰逐渐减弱，CdS的特征峰逐渐增强，因此也可得出降解效果并不是随着负载量的增加而变强。
如图四，经过比例调变以后发现浓度为0.025M的CdCl2降解效果最好。而未经负载的细菌纤维素吸附效果比负载后的更佳，是因为在称取同等质量的催化时，未经负载的样品中细菌纤维素含量最高，裸露的吸附位点最多，所以吸附量更大。但是开灯之后没有降解效果，这也印证了CdS纳米片的负载具有较好的光催化活性。
(3)将实施例1中制备的CdS纳米片作为光催化剂降解亚甲蓝溶液，其中亚甲蓝溶液浓度为25mg/L，取CdS纳米片催化剂30mg，先暗反应40min使溶液达到吸附解吸平衡，再进行紫外光催化反应，采用500W汞灯作为光源，每隔10min用滴管抽取3ml反应液于离心管中，放入高速离心机中离心3min后，后用紫外分光光度计测量光催化效果。
Claims (5)
1.一种基于细菌纤维素骨架的CdS纳米片制备方法，其特征在于，包括以下步骤：
(1)细菌纤维素处理：细菌纤维素水凝胶由桂林奇宏科技有限公司提供，并对其进行再处理。将细菌纤维素水凝胶在NaOH水溶液中纯化，除去膜中的细菌和残余反应物，然后使用去离子水水洗至pH＝7.0。将水洗后的细菌纤维素剪成小块浸没到液氮中，进行冷冻干燥，获得具有分层结构的细菌纤维素气凝胶。；
(2)CdS纳米片的制备：100ml的乙醇溶液中加入0.1M柠檬酸钠、一定浓度的CdCl2，放入50mg细菌纤维素。超声10min，使镉盐均匀沉降在纤维素上，然后向溶液中加入0.7ml浓氨水、0.2M硫脲。将溶液在高压釜中密封，并在烘箱中加热，得到的样品用乙醇清洗几次，清除未负载上去的CdS，然后在真空(80℃，12h)下干燥。
2.根据权利要求1所述的细菌纤维素的合成方法，其特征是：所述的步骤(1)中NaOH溶液的浓度是1M，温度是90℃。
3.根据权利要求1所述的细菌纤维素的合成方法，其特征是：所述的步骤(1)中冷冻干燥的时间为12h～48h。
4.根据权利要求1所述的CdS纳米片光催化剂的制备方法，其特征是：所述的步骤(2)中CdCl2浓度分别是0.025M。
5.根据权利要求1所述的CdS纳米片光催化剂的制备方法，其特征是：所述的步骤(2)中烘箱温度为150℃，时间为48h。
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| CN109999835A (zh) * | 2019-03-27 | 2019-07-12 | 武汉理工大学 | 一种碳化细菌纤维素-硫化镉复合光催化材料及其制备方法和用途 |
| CN110808361A (zh) * | 2019-10-09 | 2020-02-18 | 天津大学 | 一种基于细菌纤维素制备锂硫电池正极材料的方法 |
| CN112768655A (zh) * | 2021-01-11 | 2021-05-07 | 上海应用技术大学 | 一种二氧化锡@氧化细菌纤维素/还原氧化石墨烯电极材料的制备方法 |
| CN113663655A (zh) * | 2021-08-10 | 2021-11-19 | 常州大学 | 一种高弹性pdms/cbc海绵吸附材料的制备方法 |
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| CN109999835A (zh) * | 2019-03-27 | 2019-07-12 | 武汉理工大学 | 一种碳化细菌纤维素-硫化镉复合光催化材料及其制备方法和用途 |
| CN109999835B (zh) * | 2019-03-27 | 2022-05-10 | 武汉理工大学 | 一种碳化细菌纤维素-硫化镉复合光催化材料及其制备方法和用途 |
| CN110808361A (zh) * | 2019-10-09 | 2020-02-18 | 天津大学 | 一种基于细菌纤维素制备锂硫电池正极材料的方法 |
| CN112768655A (zh) * | 2021-01-11 | 2021-05-07 | 上海应用技术大学 | 一种二氧化锡@氧化细菌纤维素/还原氧化石墨烯电极材料的制备方法 |
| CN113663655A (zh) * | 2021-08-10 | 2021-11-19 | 常州大学 | 一种高弹性pdms/cbc海绵吸附材料的制备方法 |
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