CN109174099A - 一种SiO2-金属复合空心球催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种SiO2‑金属复合空心球催化剂的制备方法，简单可控，适用于制备高性价比的亚纳米级金属催化剂，提升了现有的制备技术，该结构中金属均匀地分布在SiO2球壳上而非传统地包裹在空心球内部，使得其具有较高的催化活性，而且无需使用表面活性剂等其他物质，避免了由表面改性剂带来的毒性风险，绿色环保。
Description
技术领域
本发明涉及一种SiO2-金属复合空心球催化剂的制备方法。
背景技术
金属纳米复合材料广泛地应用在催化、能源、环保等领域。而金属纳米复合材料中金属纳米颗粒可由几百到几十纳米，也可以控制在亚纳米级范围。负载型金属催化剂是一种典型的非均相催化剂，大多数负载型金属催化剂的金属颗粒尺寸为纳米尺度。研究表明，当金属颗粒尺寸减小到亚纳米尺度时，能够大大提高金属利用率。除此之外，由于具有特殊的几何结构和电子性质，亚纳米催化剂还体现出不同于通常纳米催化剂的优异催化性质。近年来，在催化领域亚纳米级催化剂的研发引起了科研人员的广大关注。为了合成亚纳米催化剂材料，研究人员做了大量的尝试。Qiao等人(Nature Chemistry,2011,3(8):634-641.)报道采用共沉淀方法制备的Pt/FeOx催化剂，该催化剂中Pt的负载量仅为0.17wt％；Liu等人(Science,2016,352(6287):797-801.)尝试采用光化学方法将金属负载量提高到1.5wt％；Corma等人(Nature Chemistry,2013,5(9):775-781.)研究的金纳米簇负载在碳纳米管上的金属负载率仅为0.015wt％；Yin等人(Angewandte Chemie,2016,128(36):10958-10963.)利用金属有机框架合成亚纳米级的钴基催化剂，其金属钴载量达到4wt％。Raul Arenal等人(Nature Communications,2018,9(1).)报道了一种新策略直接合成亚纳米级Pt基-MCM-22沸石复合催化剂，Pt的负载量为0.1wt％，甚至更低。
综上所述目前亚纳米级催化剂面临着两个主要的问题：金属载量较低和以贵金属研究为主。
因此，针对上述问题提出一种新的SiO2-金属复合空心球催化剂的制备方法。
发明内容
本发明的目的就在于为了解决上述问题而提供一种SiO2-金属复合空心球催化剂的制备方法。
本发明通过以下技术方案来实现上述目的，
一种SiO2-金属复合空心球催化剂的制备方法，包括以下步骤：
一、将SiO2纳米颗粒分散在去离子水中，超声至少10min后获得白色悬浊液；
二、向步骤一得到的白色悬浊液中加入金属盐，超声10min以上，得到中间溶液；
三、将步骤二得到的中间溶液移至反应釜中，将硼氢化钠加入步骤二得到的中间溶液中进行水热反应，得到第二中间溶液；
四、将步骤三得到的第二中间溶液离心水洗至中性后冷冻干燥，干燥后即得具有金属原子分散的SiO2中空球。
更进一步的，步骤一中SiO2纳米颗粒的直径为50nm-900nm。
更进一步的，步骤一中白色悬浊液中SiO2的浓度为10mg/ml-100mg/ml。
更进一步的，步骤二中金属盐为Fe盐。
更进一步的，步骤二中金属盐为硫酸盐、氯化盐、硝酸盐、醋酸盐、乙醇基盐或葡萄糖基盐。
更进一步的，步骤三的第二中间溶液中硼氢化钠的浓度为0.05g/ml-0.2g/ml。
更进一步的，步骤三中水热反应的温度为65℃-200℃，时间为0.5-48小时。
更进一步的,步骤二的中间溶液中金属盐的浓度为0.002mmol/ml-1mmol/ml。
有益效果：本发明的SiO2-金属复合空心球催化剂的制备方法简单可控，适用于制备高性价比的亚纳米级金属催化剂，提升了现有的制备技术，该结构中金属均匀地分布在SiO2球壳上而非传统地包裹在空心球内部，使得其具有较高的催化活性，而且无需使用表面活性剂等其他物质，避免了由表面改性剂带来的毒性风险，绿色环保。
附图说明
图1为实施例1所得的Fe-SiO2中空球的扫描电子显微图；
图2为实施例1所得的Fe-SiO2中空球的100nm下的透射电子显微图；
图3为实施例1所得的Fe-SiO2中空球的5nm下的透射电子显微图；
图4为实施例1所得的Fe-SiO2中空球的250nm下的透射电子显微图；
图5为实施例1所得的Fe-SiO2中空球的250nm下的透射电子显微图；
图6为实施例1所得的Fe-SiO2中空球的250nm下的透射电子显微图；
图7为实施例1所得的Fe-SiO2中空球的X射线能谱仪图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
步骤1：制备SiO2水溶液。具体包括如下步骤：称量150mg的SiO2实心球纳米颗粒，其尺寸为450nm左右，将其放入烧杯中，向烧杯中加入5mL的去离子水，将得到的溶液超声处理10分钟；
步骤2：制备Fe-SiO2NPs溶液。具体包括如下步骤：步骤1所制得的溶液中加入5mmol的三氯化铁(FeCl3)，将该溶液超声处理10分钟；
步骤3：制备Fe-SiO2中空球前驱体。具体包括如下步骤：将步骤2中制备的Fe-SiO2NPs溶液移入20mL容量的聚四氟乙烯衬里的高压釜中，向其加入0.50gNaBH4，并在80℃下进行反应12小时；
步骤4：将得到的溶液离心水洗至中性后进行冷冻干燥。干燥后的样品为Fe-SiO2中空球。
实施例2
与实施例1类似，区别在于，将实施例1的步骤2中的FeCl3改为氯化亚铁(FeCl2)，其他条件保持一致。
实施例3
与实施例1类似，区别在于，将实施例1的步骤2中的FeCl3改为醋酸铁(C4H7FeO5)，其他条件保持一致。
实施例4
与实施例1类似，区别在于，将实施例1的步骤3的加热温度改为160℃，其他条件保持一致。
实施例5
与实施例1类似，区别在于，将实施例1的步骤3的加热时间改为1小时，其他条件保持一致。
实施1-5得到如图1、图2、图3、图4、图5和图6所示的Fe-SiO2中空球。
表一、实施例1所得的Fe-SiO2中空球的X射线能谱仪数据表
| 元素 | 线类型 | wt％ | wt％Sigma | 原子百分比 | 标准样品标签 | 厂家标准 |
| O | K线系 | 61.43 | 0.85 | 78.61 | SiO2 | 是 |
| Si | K线系 | 19.99 | 0.60 | 14.58 | SiO2 | 是 |
| Fe | K线系 | 18.58 | 0.69 | 6.81 | Fe | 是 |
| 总量: | 100.00 | 100.00 |
图7为本发明实施例1所得的Fe-SiO2中空球的X射线能谱仪结果图。
本发明的优点与得到的效果如下：
1.制备工艺简单可控，绿色环保；
2.金属-SiO2催化剂的金属尺寸为亚纳米级，其载量高达18wt％；
3.该方法适用于制备高性价比的亚纳米级金属催化剂，提升了现有的制备技术；
4.该结构中金属均匀地分布在SiO2球壳上而非传统地包裹在空心球内部，使得其具有较高的催化活性；
5.无需使用表面活性剂等其他物质，避免了由表面改性剂带来的毒性风险。
Claims (8)
1.一种SiO2-金属复合空心球催化剂的制备方法，其特征在于，
包括以下步骤：
一、将SiO2纳米颗粒分散在去离子水中，超声至少10min后获得白色悬浊液；
二、向步骤一得到的白色悬浊液中加入金属盐，超声10min以上，得到中间溶液；
三、将步骤二得到的中间溶液移至反应釜中，将硼氢化钠加入步骤二得到的中间溶液中进行水热反应，得到第二中间溶液；
四、将步骤三得到的第二中间溶液离心水洗至中性后冷冻干燥，干燥后即得具有金属原子分散的SiO2中空球。
2.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤一中SiO2纳米颗粒的直径为50nm-900nm。
3.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤一中白色悬浊液中SiO2的浓度为10mg/ml-100mg/ml。
4.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤二中金属盐为Fe盐。
5.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤二中金属盐为硫酸盐、氯化盐、硝酸盐、醋酸盐、乙醇基盐或葡萄糖基盐。
6.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤三的第二中间溶液中硼氢化钠的浓度为0.05g/ml-0.2g/ml。
7.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤三中水热反应的温度为65℃-200℃，时间为0.5-48小时。
8.根据权利要求1所述的SiO2-金属复合空心球催化剂的制备方法，其特征在于：步骤二的中间溶液中金属盐的浓度为0.002mmol/ml-1mmol/ml。
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