CN114210322B - 高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料及制备方法和应用 - Google Patents
高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料及制备方法和应用 Download PDFInfo
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Abstract
本发明涉及高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料及制备方法和应用。本发明通过简单的溶剂热法制备了具有特定{010}暴露面的二维Bi2MoO6纳米片，进一步水热在其侧面边缘定向原位生长零价态半金属Bi0，即可得到Bi0/Bi2MoO6{010}吸波材料。该材料在微波驱动下对抗生素类有机污染物土霉素(OTC)展现了超高的催化活性，在环境水体净化方面具有潜在的应用前景。
Description
技术领域
本发明属于吸波材料制备领域，具体的涉及一种高暴露{010}晶面的Bi0/Bi2MoO6吸波材料及其制备方法和应用。
背景技术
抗生素自问世以来，在人类对抗疾病的历程中起到了不可或缺的作用。然而，使用过程中部分抗生素不可避免地进入自然环境，会影响植物的正常生长，甚至导致细菌耐药性的增加。此外，抗生素类有机污染物土霉素(OTC)作为一种非常稳定的有机大分子，很难自然降解，伴随食物链进入人体后，严重威胁着人类的生命健康。因此，高效去除水体中抗生素污染物，创建清洁的水环境迫在眉睫，这也是关乎未来可持续发展的关键因素。
相比于传统的加热手段，微波加热速度更快，物料内外受热更加均匀，已被广泛应用于处理各类环境污染问题。微波与吸波材料相结合的催化技术，被用于高效诱导有机污染物的降解。
Bi2MoO6是一种层状结构的双金属氧化物，具有良好的吸波性能，近年来受到了广泛关注。Bi2MoO6微波催化活性与其形貌、组成、尺寸、暴露晶面等有关。文献报道表明，合适的暴露晶面可明显增强其催化活性。
发明内容
为了解决上述技术问题，本发明的目的之一是提供一种采用简单的溶剂热法制备高暴露{010}晶面诱导定向生长Bi0的Bi0/Bi2MoO6{010}吸波材料。
本发明的目的之二是提供Bi0/Bi2MoO6{010}吸波材料协同微波高效催化降解抗生素中的应用。
本发明采用的技术方案是：一种高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，按质量百分比，Bi0占Bi2MoO6质量的5-20％。
一种高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料的制备方法，包括如下步骤：
1)Bi2MoO6{010}纳米片的制备：将铋盐、钼盐和CTAB(十六烷基三甲基溴化铵)溶解在去离子水中，剧烈搅拌30min后，用氨水调节pH＝10，将所得混合物转移到反应釜中，水热反应后，用去离子水和乙醇清洗至中性，60℃干燥，得到Bi2MoO6{010}纳米片；
2)Bi0/Bi2MoO6{010}的制备：将铋盐溶解在乙二醇中，加入Bi2MoO6{010}纳米片，超声分散1h后，转移到反应釜中，水热反应后，洗涤，干燥，得到Bi0/Bi2MoO6{010}吸波材料。
进一步的，上述的制备方法，所述铋盐为Bi(NO3)3·5H2O。
进一步的，上述的制备方法，所述钼盐为Na2MoO4·2H2O。
进一步的，上述的制备方法，步骤1)中，所述水热反应为，140℃下反应24h。
进一步的，上述的制备方法，步骤2)中，铋盐中Bi和Bi2MoO6{010}纳米片的质量比为5-20％。
进一步的，上述的制备方法，步骤2)中，所述水热反应为，160℃反应12h。
本发明提供的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料在降解废水中抗生素中的应用。
进一步的，方法如下：于含有抗生素的废水中加入Bi0/Bi2MoO6{010}吸波材料，控制微波功率为700W，催化降解。
本发明的有益效果是：本发明通过简单的溶剂热法制备了具有特定{010}暴露面的二维Bi2MoO6纳米片，零价态半金属Bi0高度定向生长在二维Bi2MoO6{010}纳米片边缘；MW驱动Bi0/Bi2MoO6{010}催化下，仅需5min，对OTC就展现了超高的催化去除效率。本发明Bi0/Bi2MoO6{010}吸波材料在微波驱动下对抗生素类有机污染物土霉素(OTC)展现了超高的催化活性，并在环境水体净化方面具有潜在的应用前景。
附图说明
图1是Bi2MoO6，Bi2MoO6{010}，Bi0/Bi2MoO6{010}的XRD图谱。
图2是Bi2MoO6{010}的SEM图。
图3是Bi0/Bi2MoO6{010}的SEM图像(a)和TEM(b)图像。
图4是MW，Bi2MoO6{010}，Bi0/Bi2MoO6{010}和Bi0/Bi2MoO6的微波催化氧化OTC性能对比。
图5是Bi2MoO6{010}，Bi0/Bi2MoO6{010}和Bi0/Bi2MoO6的微波催化氧化OTC动力学。
具体实施方式
实施例1高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料(一)Bi0/Bi2MoO6{010}吸波材料，制备方法如下：
1、Bi2MoO6{010}纳米片的制备：
将Bi(NO3)3·5H2O(970mg，2mmol)、Na2MoO4·2H2O(242mg，1mmol)和CTAB(50mg，0.1mmol)溶解在40mL去离子水中，剧烈磁搅拌30min，形成非晶态白色沉淀，用氨水调节pH＝10，将所得混合物转移到100mL的反应釜中，140℃下水热反应24h后，产物用去离子水和乙醇清洗至中性，60℃干燥12小时，得到Bi2MoO6{010}纳米片。
2、Bi0/Bi2MoO6{010}吸波材料的制备：
将Bi(NO3)3·5H2O(145.5mg，0.3mmol)溶解在40mL的乙二醇中，再加入Bi2MoO6{010}纳米片(418mg，0.7mmol)，超声分散1h后，转移到100mL反应釜中，160℃水热反应12h后，所得产物洗涤，干燥，得到Bi0/Bi2MoO6{010}吸波材料。
(二)对比例——Bi2MoO6、Bi0/Bi2MoO6的制备：
将Bi(NO3)3·5H2O(970mg，2mmol)、Na2MoO4·2H2O(242mg，1mmol)和CTAB(50mg，0.1mmol)溶解在40mL去离子水中，剧烈磁搅拌30min，形成非晶态白色沉淀，将所得混合物转移到100mL的反应釜中，140℃下水热反应24h后，产物用去离子水和乙醇清洗至中性，60℃干燥12小时，得到Bi2MoO6材料。
将Bi(NO3)3·5H2O(145.5mg，0.3mmol)溶解在40mL的乙二醇中，再加入Bi2MoO6材料(418mg，0.7mmol)，超声分散1h后，转移到100mL反应釜中，160℃水热反应12h后，所得产物洗涤，干燥，得到Bi0/Bi2MoO6材料。
(三)Bi0/Bi2MoO6{010}的表征
图1是Bi2MoO6，Bi2MoO6{010}，Bi0/Bi2MoO6{010}的XRD图谱。由图1可知，通过水热直接合成的Bi2MoO6(未调pH)和本发明合成的Bi2MoO6{010}样品的XRD衍射峰均与PDFNo.21-0102标准图谱相匹配。其中，本发明合成的Bi2MoO6{010}样品结晶程度更高，并且，Bi2MoO6{010}样品的(060)晶面与(200)/(002)晶面的峰高比值显著提高，说明Bi2MoO6{010}样品高度暴露{010}晶面。在进一步水热得到的材料Bi0/Bi2MoO6{010}的XRD图谱中，可清晰地观察到Bi0(PDF No.44-1246)的衍射峰，说明零价态半金属Bi0被成功地沉积在了Bi2MoO6{010}纳米片上，并且暴露晶面没有明显变化。
图2是Bi2MoO6{010}的SEM图。由图2可见，Bi2MoO6{010}呈现2D纳米片结构，且表面及边缘均光滑。
图3为Bi0/Bi2MoO6{010}的SEM和TEM图。由图3中(a)Bi0/Bi2MoO6{010}的SEM图可见，纳米片的表面仍旧光滑，无明显沉积物，而其侧面边缘生长出极小的纳米粒子。由图3中(b)Bi0/Bi2MoO6{010}的TEM图也证明了这一点，说明在Bi0/Bi2MoO6{010}合成过程中Bi0的生长位置具有高选择性。
实施例2高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料在降解废水中抗生素中的应用
方法如下：
采用微波仪进行催化降解实验，其温度、功率、反应时间可控，并配有冷凝回流装置。
移取50mL 10mg·L-1土霉素(OTC)溶液于250mL的三口圆底烧瓶中，加入10mg的吸波材料，开启微波辐射(700W)。一定时间间隔取样后，溶液中OTC的含量采用紫外可见分光光度计进行监测。
1、不同降解方法对降解率的影响
方法如下：
移取50mL 10mg·L-1OTC溶液于250mL的三口圆底烧瓶中，如表1采用不同的降解方法：①加入10mg的Bi0/Bi2MoO6{010}吸波材料，吸附10min；②不加入吸波材料，开启微波辐射(700W)，单独微波辐射5min；③加入10mg的Bi2MoO6{010}单体协同微波辐射(700W)5min；④加入10mg的Bi0/Bi2MoO6{010}单体协同微波辐射(700W)5min。结果如图4和表1。
表1不同方法对OTC降解效果对比
表1表明，Bi0/Bi2MoO6{010}对OTC单独吸附10min去除率仅为5.7％；单独微波辐射对OTC的降解作用几乎可以忽略。
图4表明，Bi2MoO6{010}单体在微波驱动下，5min内对OTC的氧化降解为37.0％；相同条件下，Bi0/Bi2MoO6{010}吸波材料对OTC的氧化降解效率可达93.4％，Bi0/Bi2MoO6对OTC降解效果为70.1％，说明在微波协同作用下，Bi0/Bi2MoO6{010}吸波材料展现了更高的催化活性。
由图5可见，本发明的催化过程符合准一级动力学模型，Bi2MoO6{010}与Bi0/Bi2MoO6{010}的反应速率常数k分别为0.096min-1和0.496min-1，Bi0/Bi2MoO6{010}吸波材料较Bi2MoO6{010}单体的反应速率提高了4.2倍。
2、Bi0/Bi2MoO6{010}用量对抗生素降解率的影响
方法：移取50mL 10mg·L-1OTC溶液于250mL的三口圆底烧瓶中，分别加入1mg，3mg，5mg，7mg，10mg和15mg的Bi0/Bi2MoO6{010}，微波功率700W，辐射5min。结果如表2。
表2催化剂用量对OTC降解效果的影响
由表2可见，随着催化剂用量的增加，降解效率也随之增大。催化剂用量为10mg时，降解率可达到93.4％，进一步增加用量催化效率没有明显提升。
3、Bi0负载量对抗生素降解率的影响
将Bi(NO3)3·5H2O(970mg，2mmol)、Na2MoO4·2H2O(242mg，1mmol)和CTAB(50mg，0.1mmol)溶解在40mL去离子水中，剧烈磁搅拌30min，形成非晶态白色沉淀，用氨水调节pH＝10，将所得混合物转移到100mL的反应釜中，140℃下水热反应24h后，产物用去离子水和乙醇清洗至中性，60℃干燥12小时，得到Bi2MoO6{010}纳米片。
分别取48.5mg，97mg，145.5mg，194mg Bi(NO3)3·5H2O溶解在40mL的乙二醇中，再加入418mg Bi2MoO6{010}纳米片，超声分散1h后，转移到100mL反应釜中，160℃水热反应12h后，所得产物洗涤，干燥，得到Bi0负载量分别为5％，10％，15％和20％的Bi0/Bi2MoO6{010}吸波材料。
移取50mL 10mg L-1OTC溶液于250mL的三口圆底烧瓶中，随后加入10mg不同Bi0负载量的Bi0/Bi2MoO6{010}吸波材料，并开启微波辐射(700W)辐射5min，结果如表3。
表3不同Bi0负载量对OTC降解效率的影响
由表3可见，微波辐射下，Bi0/Bi2MoO6{010}对OTC的催化氧化效果随着Bi0负载量的增加呈现先升高后降低的趋势，Bi0负载量为15％的催化剂在5min内对OTC的降解效率最佳。
Claims (7)
1.一种高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，其特征在于，所述高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，按质量百分比，Bi0占Bi2MoO6质量的5-20%；
所述高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料的制备方法，包括如下步骤：
1）Bi2MoO6{010}纳米片的制备：将铋盐、钼盐和CTAB溶解在去离子水中，剧烈搅拌30min后，用氨水调节pH=10，将所得混合物转移到反应釜中，水热反应后，用去离子水和乙醇清洗至中性，60℃干燥，得到Bi2MoO6{010}纳米片；
2）Bi0/Bi2MoO6{010}的制备：将铋盐溶解在乙二醇中，加入Bi2MoO6{010}纳米片，超声分散1h后，转移到反应釜中，水热反应后，洗涤，干燥，得到Bi0/Bi2MoO6{010}吸波材料。
2.根据权利要求1所述的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，其特征在于，所述铋盐为Bi(NO3)3·5H2O。
3.根据权利要求1所述的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，其特征在于，所述钼盐为Na2MoO4·2H2O。
4.根据权利要求1所述的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，其特征在于，步骤1）中，所述水热反应为，140℃下反应24h。
5.根据权利要求1所述的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料，其特征在于，步骤2）中，所述水热反应为，160℃反应12h。
6.权利要求1所述的高暴露{010}晶面的Bi0/Bi2MoO6{010}吸波材料在降解废水中抗生素中的应用。
7.根据权利要求6所述的应用，其特征在于，方法如下：于含有抗生素的废水中加入Bi0/Bi2MoO6{010}吸波材料，控制微波功率为700W，催化降解。
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