CN113979407A - 一种复合储氢材料NaBH4@NiB-CNC及其制备方法 - Google Patents
一种复合储氢材料NaBH4@NiB-CNC及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种复合储氢材料NaBH4@NiB‑CNC及其制备方法。其方法包括:NiB‑CNC模板材料的制备;NaBH4@NiB‑CNC的制备。其中通过控制化学还原过程中Ni源和NaBH4的加入量控制NiB‑CNC模板材料中催化剂NiB的含量;储氢材料NaBH4的负载量为30~75 wt%,模板材料NiB‑CNC的质量分数为70~25 wt%。通过本发明方法,复合材料中的NaBH4在400℃以下即可实现完全放氢,并且放氢动力学性能明显改善。本发明所制备的材料具有优越的储氢性能。本发明工艺简单易操作,合成方便,易于实现。
Description
技术领域
本发明属于储氢材料技术领域,具体涉及一种复合储氢材料NaBH4@NiB-CNC及其制备方法。
背景技术
氢气的存储是连接氢气的制备和应用的中间环节,氢气的安全高效存储是氢能技术能否实现实际应用的关键,因此开发具有高储氢容量和安全稳定的储氢方式是氢能技术应用的前提。与传统的高压储氢和低温液态储氢相比,固态储氢具有储氢密度高、安全性好,成本相对较低等优点,是最有可能实际应用的储氢方式[1]。
在固态储氢材料中,金属配位氢化物由于具有高的重量储氢密度和体积储氢密度被视为最有潜力的储氢材料之一[2]。NaBH4具有10.8wt%理论储氢容量、空气稳定性高、安全无毒性等优点,因此是一种很有潜力的储氢材料[3]。但是其热力学稳定性高、放氢温度高、放氢动力学性能差、循环吸放氢动力学性能差等缺点阻碍了其作为车载储氢材料的实际应用[4]。因此近些年来,研究者们通过纳米限域,添加过渡金属基的催化剂,以及纳米限域和催化相结合的方法来改善其动力学性能和循环吸放氢性能[5,6]。Humphries等对比了不同过渡金属硼化物对NaBH4储氢性能的影响发现,过渡金属硼化物都可以在一定程度上降低NaBH4的放氢温度,而其中Ni3B具有最好的催化效果,在此基础之上研究了不同含Ni催化剂对NaBH4储氢性能的影响,结果表明在放氢反应过程中,含Ni催化剂均会与NaBH4的分解产物反应生成NixBy型的化合物,促进放氢反应的进行[7]。Ngene等研究发现,将NaBH4限域在纳米多孔的碳模板中,复合材料的初始放氢温度下降了220℃,在325℃和60bar氢压下吸氢后再次放氢,实现43%的可逆容量[8]。在这些研究的基础上,我们结合NiB良好的催化作用和纳米碳笼大的比表面积和孔体积,利用纳米限域和原位催化结合相结合的方法,大幅降低了NaBH4的放氢温度同时改善了放氢反应动力学性能。
[1]Reardon H,Hanlon J M,Hughes R W,Godula-Jopek A,Mandal T K,GregoryD H.Emerging concepts in solid-state hydrogen storage:the role ofnanomaterials design[J].Energy & Environmental Science,2012,5(3):5951-5979.
[2]Ley M B,Jepsen L H,Lee Y-S,Cho Y W,Bellosta Von Colbe J M,DornheimM,Rokni M,Jensen J O,Sloth M,Filinchuk Y,J E,Besenbacher F,Jensen TR.Complex hydrides for hydrogen storage–new perspectives[J].Materials Today,2014,17(3):122-128.
[3]Chong L,Zeng X,Ding W,Liu D-J,Zou J.NaBH4 in“Graphene Wrapper:”Significantly Enhanced Hydrogen Storage Capacity and Regenerability throughNanoencapsulation[J].2015,27(34):5070-5074.
[4]Schüth F,B,Felderhoff M.Light metal hydrides and complexhydrides for hydrogen storage[J].Chemical Communications,2004,(20):2249-2258.
[5]Jubert Tomasso C,Pham AL,Mattox T M,Urban J J.Using Additives toControl the Decomposition Temperature of Sodium Borohydride[J].Journal ofEnergy and Power Technology,2020,2(2):1-20.
[6]Grochala W,Edwards P P.Thermal Decomposition of the Non-Interstitial Hydrides for the Storage and Production of Hydrogen[J].ChemicalReviews,2004,104(3):1283-1316.
[7]Humphries T D,Kalantzopoulos G N,Llamas-Jansa I,Olsen J E,HaubackB C.Reversible Hydrogenation Studies of NaBH4 Milled with Ni-ContainingAdditives[J].The Journal of Physical Chemistry C,2013,117(12):6060-6065.
[8]Ngene P,van den Berg R,Verkuijlen M H W,et al.Reversibility of thehydrogen desorption from NaBH4 by confinement in nanoporous carbon[J].Energy& Environmental Science,2011,4(10):4108-4115。
发明内容
本发明的目的是提供一种储氢容量高、放氢温度降低、循环性能好的复合储氢材料及其制备方法。
本发明提供的复合储氢材料,是一种硼氢化钠(NaBH4)负载于附有NiB催化剂的纳米碳笼而得到的复合材料,记为NaBH4@NiB-CNC。
本发明提出的复合储氢材料NaBH4@NiB-CNC的制备方法,包括化学还原法制备NiB-CNC;将NaBH4溶于有机溶剂,通过溶液负载并除溶剂,得到复合储氢材料NaBH4@NiB-CNC;具体步骤如下:
(1)附有NiB催化剂的纳米碳笼的制备:
以去离子水为溶剂,以Ni盐作为Ni源,以硼氢化钠为还原剂,在持续搅拌状态下将硼氢化钠溶液逐滴滴入Ni盐溶液中,室温下反应25-35分钟;将反应后的产物离心清洗、真空干燥得到附有NiB催化剂的纳米碳笼,记为NiB-CNC;
具体操作:在室温(如25-30℃)下,将Ni盐和硼氢化钠分别溶于去离子水中;在搅拌状态下将硼氢化钠溶液逐滴滴入Ni盐溶液中,待25-35min后,将产物转移到离心管中用去离子水离心清洗三次,将最终产物转移到真空干燥箱中在50-70℃下烘干8-15h,得到的黑色粉末即为NiB-CNC;
(2)溶液法将NaBH4负载到NiCo-NC:
将NaBH4溶于有机溶剂(如乙二醇二甲醚、二乙二醇二甲醚、四氢呋喃等)中,搅拌溶解得到无色澄清溶液;向其中加入NiB-CNC,超声分散均匀;通过抽溶剂的方法去除溶剂,NaBH4在NiCo-NC上形核长大,得到NaBH4负载的附有NiB催化剂的纳米碳笼,记为NaBH4@NiB-CNC,该NaBH4均匀负载在NiB-CNC的空隙中。
本发明步骤(1)中,所述Ni盐采用醋酸镍、Ni(NO3)2、NiCl2或其水合物,Ni盐和NaBH4的摩尔比为1:1.3到1:1.5的范围内。
本发明步骤(1)中,通过调节反应物Ni源和NaBH4的加入量,控制NiB-CNC中催化剂NiB的含量:NiB-CNC中,NiB的质量百分比为10~40wt%。
本发明步骤(2)中,通过调节NaBH4和NiB-CNC的比例,控制两组分的含量:NaBH4的质量百分比为30~75wt%,NiB-CNC的质量百分数为70~25wt%,两部分总量满足100%。
本发明步骤(2)中,所述有机溶剂优选乙二醇二甲醚、二乙二醇二甲醚或四氢呋喃。
本发明制备的NaBH4@NiB-CNC是一种高效复合储氢材料,具有优异的放氢性能。加热到300℃即开始快速放氢,加热至400℃基本完全放氢。
本发明具有以下几个方面显著优点:
(1)本发明使用的NaBH4作为氢源材料价格低廉。
(2)本发明所用的负载方法对设备要求不高,易于实现。
(3)工艺简单,合成方便。
(4)放氢温度相对较低,在400℃可实现完全放氢。
附图说明
图1为不同阶段产物的SEM和TEM图。其中,(a)CNC的SEM图,(b)NiB-CNC的SEM图,(c)NiB-CNC的TEM图,(d)NiB-CNC的HRTEM图,(e)NaBH4@NiB-CNC的SEM图,(f)NaBH4@NiB-CNC的TEM图,(g)NaBH4@NiB-CNC的HRTEM图,(h)NaBH4@NiB-CNC的STEM及对应元素分布图。
图2为不同产物的XRD谱图。其中BM NaBH4为球磨的NaBH4,NaBH4/CNC为质量比1:1球磨的NaBH4和纳米碳笼,NaBH4/NiB-CNC为质量比1:1球磨的NaBH4和附有NiB催化剂的纳米碳笼,NaBH4@CNC为用溶液负载法制备的NaBH4负载在纳米碳笼中,NaBH4@NiB-CNC为用溶液负载法制备的NaBH4负载在有NiB催化剂的纳米碳笼中。
图3为不同样品的TPD放氢曲线。其中,带正方形的曲线为球磨的NaBH4,带菱形的曲线为添加10wt%NiB催化剂的NaBH4,带五角星的曲线为质量比1:1球磨的NaBH4和纳米碳笼,带六边形的为质量比1:1球磨的NaBH4和附有NiB催化剂的纳米碳笼,带三角形的曲线为溶液负载法制备的NaBH4@CNC,带空心圆的曲线为溶液负载法制备的NaBH4@NiB-CNC。测试的升温速率为3℃/min,样品的放氢量均为相对NaBH4的质量进行计算。
图4为NaBH4@NiB-CNC在氩气气氛下的MS曲线,升温速率为3℃/min。
图5为NaBH4@NiB-CNC在不同温度下的恒温放氢曲线。
图6为NaBH4负载量为67wt%和75wt%时,67%NaBH4@NiB-CNC和75%NaBH4@NiB-CNC的TPD放氢曲线。
具体实施方式
下面通过实例进一步说明本发明,但不因此而限制本发明的内容。
实施例1:
(1)NiB-CNC的制备
在室温(25℃)下,称取60mg纳米碳笼于40mL去离子水中,超声分散10min使纳米碳笼在去离子水中分散均匀。向其中加入84mg六水合硝酸镍,搅拌10分钟。将0.4mmol硼氢化钠溶于20mL去离子水中。在搅拌状态下将硼氢化钠溶液逐滴滴入有纳米碳笼的硝酸镍溶液中。滴加完毕后继续搅拌30min。将反应后的产物离心并用去离子水清洗3次,在60℃下真空干燥12h,得到的黑色粉末即为NiB-CNC。
(2)NaBH4负载量为50wt%的NaBH4@NiB-CNC的制备
在氩气手套箱中,将100mg NaBH4加入到50mL乙二醇二甲醚中,搅拌1h后得到透明澄清溶液。向其中加入100mg NiB-CNC后在超声机中持续超声0.5h,将超声后的产物转移到反应管中,在80℃下将溶剂抽干并持续抽真空12h,得到的产物即为50wt%负载量的NaBH4@NiB-CNC。
所制备的NaBH4@NiB-CNC在300℃左右就开始快速放氢,在400℃基本完全放氢,如图3所示,而且放出的气体为纯氢气,没有硼烷的生成,如图4所示。如图5所示,NaBH4@NiB-CNC在350℃下,3h内的放氢量可以达到9.2wt%;在400℃下保温,可实现完全放氢。
实施例2:
用实施例1中步骤(1)相同的方法制备带有NiB催化剂的纳米碳笼NiB-CNC。在氩气手套箱中,将40mg NaBH4加入到20mL乙二醇二甲醚中,搅拌1h后得到透明澄清溶液。向其中加入20mg NiB-CNC后在超声机中持续超声0.5h,将超声后的产物转移到反应管中,在80℃下将溶剂抽干并持续抽真空12h,得到的产物为NaBH4负载量为67wt%的NaBH4@NiCo-NC,即67%NaBH4@NiCo-NC。如图6所示,所制备的67%NaBH4@NiCo-NC在加热到400℃时,可以放出7.3wt%(相对于NaBH4的质量)的氢气,远高于球磨NaBH4的放氢量(0.5wt%)。
实施例3:
用实施例1中步骤(1)相同的方法制备带有NiB催化剂的纳米碳笼NiB-CNC。在氩气手套箱中,将60mg NaBH4加入到30mL乙二醇二甲醚中,搅拌1h后得到透明澄清溶液。向其中加入20mg NiB-CNC后在超声机中持续超声0.5h,将超声后的产物转移到反应管中,在80℃下将溶剂抽干并持续抽真空12h,得到的产物为NaBH4负载量为75wt%的NaBH4@NiCo-NC,即75%NaBH4@NiCo-NC。如图6所示,所制备的75wt%负载量的NaBH4@NiCo-NC在加热到420℃时可以放出7.3wt%(相对于NaBH4的质量)的氢气,远高于球磨NaBH4的放氢量(0.7wt%)。
Claims (6)
1.一种复合储氢材料的制备方法,其特征在于,具体步骤如下:
(1)附有NiB催化剂的纳米碳笼的制备:
以去离子水为溶剂,以Ni盐作为Ni源,以硼氢化钠为还原剂,在持续搅拌状态下将硼氢化钠溶液逐滴滴入Ni盐溶液中,室温下反应25-35分钟;将反应后的产物离心清洗、真空干燥得到附有NiB催化剂的纳米碳笼,记为NiB-CNC;
(2)溶液法将NaBH4负载到NiB-CNC:
将NaBH4溶于有机溶剂中,搅拌溶解得到无色澄清溶液;向其中加入NiB-CNC,超声分散均匀;通过抽溶剂的方法去除溶剂,NaBH4在NiB-CNC上形核长大,得到NaBH4负载的附有NiB催化剂的纳米碳笼材料,记为NaBH4@NiB-CNC;该复合材料中NaBH4均匀负载在NiB-CNC的空隙中。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述Ni盐采用醋酸镍、Ni(NO3)2、NiCl2或其水合物;Ni盐和NaBH4的摩尔比为1:1.3到1:1.5的范围内。
3.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,通过调节反应物Ni源和NaBH4的加入量,控制得到的NiB-CNC中NiB催化剂的含量:使NiB-CNC中NiB的质量百分比为10~40 wt%。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,通过调节NaBH4和NiB-CNC的加入量,控制两组分的含量:NaBH4的质量百分比为30~75 wt%,NiCo-NC的质量百分比为70~25 wt%,两部分总量满足100%。
5.根据权利要求1所述的制备方法,其特征在于,步骤(2)中所述有机溶剂为乙二醇二甲醚、二乙二醇二甲醚或四氢呋喃。
6.一种由权利要求1-4之一所述制备方法得到的复合储氢材料,为NaBH4负载于附有NiB催化剂的纳米碳笼而得到的复合材料,记为NaBH4@NiB-CNC。
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