CN106865497B - 一种原位生长纳米氢化镁负载高比表面材料的制备方法 - Google Patents
一种原位生长纳米氢化镁负载高比表面材料的制备方法 Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 claims abstract description 37
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 35
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Abstract
一种原位生长纳米氢化镁负载高比表面材料的制备方法，利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成。本发明的技术效果是：本发明通过置换反应在支撑材料表面原位生成氢化镁，在温和条件下制备了具有较低操作温度、较快吸放氢速率的纳米复合储氢材料，解决了以往制备纳米氢化镁材料制备条件苛刻、产品粒径大等问题，提高氢化镁储氢材料的热力学、动力学性能。
Description
技术领域
本发明涉及一种原位生长纳米氢化镁(MgH2)负载高比表面材料的制备方法，属于储氢材料技术领域。
背景技术
氢能源具有资源丰富、热值高、绿色环保等优点，被认为是化石能源在未来的最佳替代物。然而，氢气是一种易燃易爆的气体，实现安全、高质量、体积密度的储氢是氢能源储存技术发展的当务之急。近年来，固态储氢的方法受到研究者们的广泛关注。镁基轻质储氢材料，具有密度小、储氢量大、产量丰富、价格低廉等优点。然而镁基材料操作温度高，吸放氢速度慢等缺点限制了其大规模应用。
将储氢材料纳米化，可以有效的降低操作温度，提升吸放氢速率。利用高比表面积的化工产品或工业废料搭载纳米储氢材料，可以稳定材料形貌，控制材料粒径分布。目前制备纳米氢化镁的方法主要为原位还原法和浸渍法，原位还原法获得的纳米颗粒粒径在30nm左右，对储氢性能并没有太大的改善。浸渍法获得的纳米颗粒粒径在3-5nm，但是需要较高的氢压和反应温度，生产存在一定的安全隐患。因此，研究开发在较为温和的条件下制备小粒径的纳米氢化镁复合材料具有很大的意义。
发明内容
本发明的目的在于针对上述存在问题，提供一种温和条件下原位生长纳米氢化镁负载高比表面材料的制备方法，该制备方法可以提高氢化镁储氢材料的热力学、动力学性能，从而降低操作温度，提高吸放氢速率。
本发明技术方案：
一种原位生长纳米氢化镁负载高比表面材料的制备方法，利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成，具体步骤如下：
1)在氩气或氮气气氛下，将氯化镁与氢化锂以1:1-3的摩尔比混合，得到混合物放入球磨罐中，然后加入支撑材料，支撑材料的加入量为混合物质量的5-25％，混合均匀；
2)在0.5MPa氢压下，以200-600rpm的转速下球磨10-60h；
3)在氩气或氮气气氛下，用乙醚或四氢呋喃洗涤3次，离心或过滤分离，对不溶物在50Pa以下真空干燥或40-80℃温度下干燥至质量不再下降，得到目标产物，原位生长的氢化镁为球型或椭球型，粒径为2-8nm。
所述支撑材料为石墨烯、椰壳炭或粉煤灰高比表面积的化工产品或工业废料。
本发明的技术效果是：
本发明通过置换反应在支撑材料表面原位生成氢化镁，在温和条件下制备了具有较低操作温度、较快吸放氢速率的纳米复合储氢材料，解决了以往制备纳米氢化镁材料制备条件苛刻、产品粒径大等问题，提高氢化镁储氢材料的热力学、动力学性能。
附图说明
图1为实施例1和实施例2制备的石墨烯搭载氢化镁和椰壳炭搭载氢化镁纳米材料的XRD图谱。
图2为实施例1制备的石墨烯搭载氢化镁纳米材料的SEM图和TEM图。
图3为实施例1制备的石墨烯搭载氢化镁纳米材料的等温放氢曲线和等温吸氢曲线。
图4为实施例2制备的椰壳炭搭载氢化镁纳米材料的程序升温放氢曲线。
具体实施方式
下面结合实施例对本发明做进一步描述。
实施例1：
一种原位生长纳米氢化镁负载高比表面材料的制备方法，利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成，具体步骤如下：
将0.4g的LiH、2.0g的MgCl2和0.07g还原石墨烯放入球磨罐中，混合均匀；在0.5MPa的氢压下450rpm的转速下球磨30个小时；将得到的混合物用40mL四氢呋喃作溶剂洗涤3次，离心分离，除去溶剂，50Pa以下真空干燥14个小时，得到目标产物。
制备的石墨烯搭载氢化镁和椰壳炭搭载氢化镁纳米材料的XRD图谱如图1所示，图中表明：所得产物为四方晶系MgH2，且无其他杂质。
图2为制备的石墨烯搭载氢化镁纳米材料的SEM图和TEM图，图中表明：MgH2纳米颗粒均匀分布在石墨烯纳米片上。
图3为制备的石墨烯搭载氢化镁纳米材料的等温放氢曲线和等温吸氢曲线，图中表明：石墨烯搭载氢化镁纳米材料的吸放氢动力学性能较优。该材料在325℃下20min内可释放出5.1wt％的氢气，在250℃下5min内吸收4.8wt％的氢气。
实施例2：
一种原位生长纳米氢化镁负载高比表面材料的制备方法，利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成，具体步骤如下：
将0.4g的LiH、2.0g的MgCl2和0.10g椰壳炭放入球磨罐中，混合均匀。在0.5MPa的氢压下450rpm的转速下球磨30个小时；将得到的混合物用40mL四氢呋喃作溶剂洗涤3次，离心分离，除去溶剂；50Pa以下真空干燥14个小时，得到目标产物。
制备的石墨烯搭载氢化镁和椰壳炭搭载氢化镁纳米材料的XRD图谱如图1所示，图中表明：所得产物为四方晶系MgH2，且无其他杂质。
图4为实施例2制备的椰壳炭搭载氢化镁纳米材料的程序升温放氢曲线图中表明：椰壳炭搭载氢化镁纳米材料具有较低的起始放氢温度(245℃)和较高的储氢容量(6.3wt％)。
实施例3：
一种原位生长纳米氢化镁负载高比表面材料的制备方法，利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成，具体步骤如下：
将0.4g的LiH、2.0g的MgCl2和0.10g粉煤灰放入球磨罐中，混合均匀；在0.5MPa的氢压下500rpm的转速下球磨40个小时；将得到的混合物用60mL四氢呋喃作溶剂洗涤3次，离心分离，除去溶剂；50Pa以下真空干燥14个小时，得到目标产物。
Claims (2)
1.一种原位生长纳米氢化镁负载高比表面材料的制备方法，其特征在于利用碱金属氢化物、卤化镁和支撑材料在球磨的条件下原位合成，具体步骤如下：
1)在氩气或氮气气氛下，将氯化镁与氢化锂以1:1-3的摩尔比混合，得到混合物放入球磨罐中，然后加入支撑材料，支撑材料的加入量为混合物质量的5-25％，混合均匀；
2)在0.5MPa氢压下，以200-600rpm的转速下球磨10-60h；
3)在氩气或氮气气氛下，用乙醚或四氢呋喃洗涤3次，离心或过滤分离，对不溶物在50Pa以下真空干燥或40-80℃温度下干燥至质量不再下降，得到目标产物，原位生长的氢化镁为球型或椭球型，粒径为2-8nm。
2.根据权利要求1所述原位生长纳米氢化镁负载高比表面材料的制备方法，其特征在于：所述支撑材料为石墨烯、椰壳炭或工业废料粉煤灰。
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| CN109319732B (zh) * | 2018-10-15 | 2020-09-01 | 浙江大学 | 一种二维负载型纳米镁氢化物储氢材料的制备方法 |
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|---|---|---|---|---|
| GB879230A (en) * | 1958-08-21 | 1961-10-11 | Olin Mathieson | Improvements in or relating to the production of magnesium hydride |
| CN1417878A (zh) * | 2002-12-20 | 2003-05-14 | 南开大学 | 含锂复合储氢合金电极材料及制备方法 |
| JP2008018420A (ja) * | 2006-06-13 | 2008-01-31 | Taiheiyo Cement Corp | 水素貯蔵材料およびその製造方法 |
| CN101970343A (zh) * | 2007-12-10 | 2011-02-09 | 科学研究国家中心 | 氢化镁系储氢材料 |
| CN106006552A (zh) * | 2016-05-17 | 2016-10-12 | 武汉凯迪工程技术研究总院有限公司 | 氢化镁复合物粉末及其制备方法与其制氢储氢一体化装置 |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB879230A (en) * | 1958-08-21 | 1961-10-11 | Olin Mathieson | Improvements in or relating to the production of magnesium hydride |
| CN1417878A (zh) * | 2002-12-20 | 2003-05-14 | 南开大学 | 含锂复合储氢合金电极材料及制备方法 |
| JP2008018420A (ja) * | 2006-06-13 | 2008-01-31 | Taiheiyo Cement Corp | 水素貯蔵材料およびその製造方法 |
| CN101970343A (zh) * | 2007-12-10 | 2011-02-09 | 科学研究国家中心 | 氢化镁系储氢材料 |
| CN106006552A (zh) * | 2016-05-17 | 2016-10-12 | 武汉凯迪工程技术研究总院有限公司 | 氢化镁复合物粉末及其制备方法与其制氢储氢一体化装置 |
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