CN108940364A - 一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法 - Google Patents
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Abstract
本发明公开了一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，以硝酸为活化剂，用化学活化法对活性炭进行活化，将活性炭与一定量的硝酸混合，搅拌反应一段时间后过滤，用水反复洗涤至中性后干燥；采用浸渍‑化学还原法制备催化剂：称取经硝酸活化预处理的活性炭，加入到磷钨酸溶液中，水浴搅拌后过滤洗涤，干燥，备用；硼氢化钠催化水解制氢反应；以海水为反应液，加入硼氢化钠和催化剂，在强烈搅拌的条件下，加入反应液时即开始计时，生成的氢气用排水法收集。本发明的有益效果是方法简单，制氢效率高，污染小。
Description
技术领域
本发明属于能源技术领域，涉及一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法。
背景技术
随着化石能源的缺乏以及人们日益重视环境保护，可持续清洁能源越来越受到世界各国的高度重视。氢能因其来源多样性、清洁、可储存及可再生等优点，被认为是化石燃料的重要替代能源。金属氢化物在储氢容量上具有其他材料无法比拟的优势,且通过简单的水解反应即可放出氢气。正因如此,金属氢化物水解作为一种新型供氢技术,近年来受到了极大关注。长期以来,贵金属催化剂由于其稳定的化学性质,良好的催化活性,一直是催化剂研究的热点。贵金属催化剂虽然具有较高的活性，但其价格昂贵、储量有限，限制了其广泛的工业应用。因此，许多研究以制备低成本高活性的非贵金属催化剂为重点。
由于沿海城市海水资源极其丰富，以海水为反应溶剂以及将活性炭负载的杂多酸催化剂应用于硼氢化钠水解制氢反应国内尚未见报道。
发明内容
本发明的目的在于提供一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，本发明的有益效果是方法简单，制氢效率高，污染小。
本发明所采用的技术方案是按照以下步骤进行：
步骤1：以硝酸为活化剂，用化学活化法对活性炭进行活化，将活性炭与一定量的硝酸混合，搅拌反应一段时间后过滤，用水反复洗涤至中性后干燥；
步骤2：采用浸渍-化学还原法制备催化剂：称取经硝酸活化预处理的活性炭，加入到磷钨酸(TPA)溶液中，水浴搅拌后过滤洗涤，干燥，备用；
步骤3：硼氢化钠催化水解制氢反应；以海水为反应液，加入硼氢化钠和催化剂，在强烈搅拌的条件下，加入反应液时即开始计时，生成的氢气用排水法收集。
进一步，步骤1中于80℃下搅拌反应4h后过滤，用水反复洗涤至中性后于110℃下干燥。
进一步，步骤2中称取经硝酸活化预处理的活性炭加入到磷钨酸溶液中，于50℃下水浴搅拌6小时后过滤洗涤，于70℃干燥10h。
进一步，步骤3中反应温度为40℃。
进一步，步骤3中反应物硼氢化钠质量分数为5％，催化剂/反应物质量比为0.1。
附图说明
图1是不同负载量催化剂催化硼氢化钠水解制氢示意图；
图2是不同负载量催化剂催化硼氢化钠水解制氢产率图示意图；
图3是不同负载量催化剂催化硼氢化钠水解制氢速率图示意图。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
原料准备：硼氢化钠(分析纯)，成都市科龙化工试剂厂提供；磷钨酸(分析纯)，天津市科密欧化学试剂有限公司提供；活性炭(分析纯)，天津市福晨化学试剂厂提供；硝酸(分析纯)，莱阳经济技术开发区精细化工厂提供；取自胶州湾的海水。
催化剂的制备：以硝酸为活化剂，用化学活化法对活性炭进行活化。将活性炭与一定量的硝酸混合，于80℃下搅拌反应4h后过滤，用水反复洗涤至中性，后于110℃下干燥。
采用浸渍-化学还原法制备Co-B/C催化剂：称取一定量经硝酸活化预处理的活性炭，加入到磷钨酸溶液中，后于50℃下水浴搅拌6小时后过滤洗涤，于70℃干燥10h,备用。
硼氢化钠催化水解制氢反应：采用在反应温度为40℃,以海水为反应液，其中反应物硼氢化钠质量分数为5％，m(催化剂)/m(反应物)约为0.1，在强烈搅拌的条件下，加入反应液时即开始计时，生成的氢气用排水法收集，测试不同负载量的磷钨酸/C催化剂对氢产率及反应速率的影响。
对本发明进行实验验证：
物性表征：X－射线衍射光谱(XRD)；
试验中XRD分析采用日本RIGAKU公司生产的Utima IV型X射线衍射仪，将试样均匀地覆盖在玻璃板上，电流60mA，电压40kV，记录速度10mm·min-1，角度2°·min-1。管电压50kV，管电流50mA，扫描速度8°·min-1，Cu靶辐射，扫描范围为10°～90°，将2θ角下的衍射强度连续地记录在记录纸上，由计算机标定的各衍射峰的2θ值及相应的面间距(d值)，再查J.C.P.D.S卡，确定出复合材料中的物相及晶面参数。
比表面积和孔特征(BET)：测定活性炭载体和负载样品的比表面积、平均孔径及总孔容值，载气为He，吸附气体为N2，测定温度为液氮温度，根据低温吸附原理对固体的比表面积及孔径分布进行测定。
结果：不同负载量催化剂的催化活性
由表1及图1，2知，在已确定的适宜m(NaBH4)∶m(H2O)＝1:20,m(催化剂)/m(反应物)约为0.1,在适宜温度40℃进行实验,其结果见表1。由表1及图1可知，随着TPA负载量的增加，反应速率逐渐减小，产率先增大后减小，在负载量为2.5％时产率达到最大，而未负载的纯TPA的催化活性最低。
表1.TPA与负载型TPA催化剂的催化效果比较
催化剂表征：
比表面积及孔特征
表2是活性炭载体及不同负载量催化剂的比表面积和孔容值。负载量用每100克活性炭负载的TPA质量表示,单位为g/100g，简写为百分数％。
表2的结果显示：①与体相TPA相比，负载TPA的比表面积明显增加，对催化反应是有利的，有效克服了体相TPA在作为催化剂时，比表面积过小的不足。②对于活性炭负载的TPA催化剂，比表面积和孔容值随负载量的增大而迅速减小。平均孔径也随负载量的增大而减小，这是由于TPA在吸附扩散的过程中，填充了活性炭的微孔和部分中孔，导致比表面积和总孔容减小。
表2.活性炭载体及不同负载量催化剂的比表面积,孔径和孔容值
以上所述仅是对本发明的较佳实施方式而已，并非对本发明作任何形式上的限制，凡是依据本发明的技术实质对以上实施方式所做的任何简单修改，等同变化与修饰，均属于本发明技术方案的范围内。
Claims (5)
1.一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，其特征在于按照以下步骤进行：
步骤1：以硝酸为活化剂，用化学活化法对活性炭进行活化，将活性炭与一定量的硝酸混合，搅拌反应一段时间后过滤，用水反复洗涤至中性后干燥；
步骤2：采用浸渍-化学还原法制备催化剂：称取经硝酸活化预处理的活性炭，加入到磷钨酸溶液中，水浴搅拌后过滤洗涤，干燥，备用；
步骤3：硼氢化钠催化水解制氢反应；以海水为反应液，加入硼氢化钠和催化剂，
在强烈搅拌的条件下，加入反应液时即开始计时，生成的氢气用排水法收集。
2.按照权利要求1所述一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，其特征在于：所述步骤1中于80℃下搅拌反应4h后过滤，用水反复洗涤至中性后于110℃下干燥。
3.按照权利要求1所述一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，其特征在于：所述步骤2中称取经硝酸活化预处理的活性炭加入到磷钨酸溶液中，于50℃下水浴搅拌6小时后过滤洗涤，于70℃干燥10h。
4.按照权利要求1所述一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，其特征在于：所述步骤3中反应温度为40℃。
5.按照权利要求1所述一种活性炭负载杂多酸催化硼氢化钠水解制氢的方法，其特征在于：所述步骤3中反应物硼氢化钠质量分数为5％，催化剂/反应物质量比为0.1。
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| CN114100614A (zh) * | 2021-12-06 | 2022-03-01 | 桂林电子科技大学 | 一种中空碳材料负载Co-Cu-B纳米粒子的复合材料及其制备方法和应用 |
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