CN110404558B - 一种用于肼分解产氢的NiPt-Ni(OH)2/La(OH)3催化剂及其制备方法 - Google Patents
一种用于肼分解产氢的NiPt-Ni(OH)2/La(OH)3催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000001257 hydrogen Substances 0.000 title claims abstract description 40
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000000354 decomposition reaction Methods 0.000 title description 11
- 239000002184 metal Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 3
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- -1 rare earth hydroxide Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910018661 Ni(OH) Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 3
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 abstract 1
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 239000012279 sodium borohydride Substances 0.000 abstract 1
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 38
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 14
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002131 composite material Substances 0.000 description 6
- 239000011943 nanocatalyst Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 239000011232 storage material Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000002186 photoelectron spectrum Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
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Abstract
本发明提供了一种用于肼分解产氢的NiPt‑Ni(OH)2/La(OH)3催化剂及其制备方法。该催化剂由金属Ni、金属Pt、金属氢氧化物Ni(OH)2和稀土元素氢氧化物La(OH)3载体组成,结构式为NiPt‑Ni(OH)2/La(OH)3。该催化剂采用沉淀还原法,先通过加碱沉淀得到Ni(OH)2和Pt(OH)2,然后加入硼氢化钠还原得到。该催化剂能在常温常压不添加任何助剂的条件下快速催化肼分解产氢,选择性高达95%,转换频率高达303h‑1。该催化剂制备简单,催化活性高,是一种很有应用前景的催化剂。
Description
技术领域
本发明方法涉及一种用于肼分解产氢的复合纳米催化剂及其制备方法,属于储氢材料领域。
背景技术
氢能由于具有高燃烧热值和燃烧产物无污染的特点,被认为是一种理想的二次能源。但是如何安全高效的储存氢气仍然是制约着氢能的大规模使用的瓶颈。化学储氢材料由于具有较高的储氢密度,便于运输和储存,是可以替代传统增压或者低温液化储氢的新型储氢方式。在所有的化学储氢材料中,水合肼具有较高的含氢量,且可以在现有设备上直接使用,是一种极具应用前景的化学储氢材料。
水合肼(N2H4·H2O),室温下物理化学性质稳定,便于运输和储存,储氢含量为8.0wt.%,远超美国能源部制定的2017年储氢材料的要求指标(5.5wt%),具有良好的实际应用前景。有合适的催化剂存在时,水合肼的分解在温和的条件下就能进行。理论上1摩尔的水合肼分解可以产生2摩尔的氢气和氮气(反应1)。但是水合肼的分解往往伴随有生成氨气的副反应的发生(反应2),会大大降低水合肼产氢的效率。因此,水合肼产氢的关键在于制备高活性,高选择性的催化剂。
N2H4(l)→N2(g)+2H2(g) (1)
3N2H4(l)→4NH3(g)+N2(g) (2)
通常提高水合肼分解的氢气选择性的方法有升高反应温度以及添加碱作为助剂(J.Am. Chem.Soc.2010,49,6148;Eur.J.Inor.Chem.2011,2011,2232)。然而,升高温度意味着生产成本和能源消耗的增加,而氢氧化钠的引入会腐蚀设备,对设备和操作提出了更高的要求。因此,如何在室温以及无碱的条件下高效催化水合肼产氢,是实现水合肼产氢实际应用的关键。目前,已有一些报道的催化剂能够实现在室温下高选择性的催化水合肼脱氢(Angew. Chem.,Int.Ed.2012,51,1;J.Mater.Chem.A 2016,4,6595),但是这些催化剂的催化活性仍然很低,无法满足实际生产的需要。因此,制备出一种在室温无碱条件下,可高活性高选择性催化水合肼产氢的催化剂具有非常重要的理论和实际意义。
发明内容
本发明的目的在于提供一种复合纳米催化剂及其制备方法,该复合纳米催化剂可以用于液相催化肼产氢。在本文中,所述的复合纳米催化剂又称为NiPt-Ni(OH)2/La(OH)3催化剂。
本发明所述的NiPt-Ni(OH)2/La(OH)3催化剂由金属Ni、金属Pt、金属氢氧化物Ni(OH)2以及稀土氢氧化物La(OH)3组成,其化学式为NiPt-Ni(OH)2/La(OH)3,其中Ni的含量为2.1~13.0wt.%,Pt的含量为8.1~54.1wt.%,Ni(OH)2的含量为0.8~5.1wt.%,La(OH)3的含量为27.7~88.5wt.%。
本发明所述的NiPt-Ni(OH)2/La(OH)3催化剂采用沉淀还原法在常温常压下制得,具体包括以下步骤:
1)在水中加入La(OH)3并混合均匀;
2)向步骤1)得到的溶液中加入Ni和Pt的前驱体溶液,超声处理并混合均匀;
3)向步骤2)得到的溶液中加入NaOH,超声处理并混合均匀;
4)向步骤3)得到的溶液中加入NaBH4,混合均匀并反应一段时间;
5)从步骤4)得到的溶液中分离出固态物质,洗涤并干燥,得到所述的 NiPt-Ni(OH)2/La(OH)3催化剂。
上述制备方法中,Ni和Pt的前驱体溶液为Ni盐和Pt盐的水溶液,优选为NiCl2和K2PtCl4的水溶液。
上述制备方法中,Ni盐和Pt盐的摩尔比为1:1。
上述制备方法中,步骤4)所述的反应时间为10min。
上述的NiPt-Ni(OH)2/La(OH)3催化剂可以用于催化肼产氢,其催化性能优异。其中, NiPt-Ni(OH)2/La(OH)3催化剂是一种黑色粉末状物质,可通过离心从反应体系中回收,具有催化活性高,稳定性好等特点;在室温(298K)无碱的条件下能够高效催化肼产氢,其转化频率(TOF)高达303.2h-1,TOF值比目前报道的无碱添加剂下活性最高的催化剂要高一个数量级。如果加入2M NaOH,其TOF值在298K和303K下分别达到857.1h-1和1034.5h-1,比目前报道的活性最高的催化剂更好。
本发明的优点是:1)制备方法简单易行;2)所制备的复合纳米催化剂在室温无碱的情况下可高效催化肼产氢,其转化频率高达303.2h-1,氢气选择性为95%;3)该催化剂具有良好的循环稳定性;4)催化剂易于回收,可重复使用,具有良好的应用前景。
附图说明
图1是本发明实施例1所得NiPt-Ni(OH)2/La(OH)3催化剂及其对比样品的多晶X射线衍射图。
图2是本发明实施例1所得NiPt-Ni(OH)2/La(OH)3催化剂的透射电镜图。
图3是本发明对比例1所得NiPt-Ni(OH)2催化剂的拉曼光谱和红外光谱图。
图4是本发明实施例1所得NiPt-Ni(OH)2/La(OH)3催化剂的光电子能谱图(左图为Ni 2p 谱图,右图为Pt 4f谱图)。
图5是本发明实施例1所得NiPt-Ni(OH)2/La(OH)3催化剂的光电子能谱图(O 1s谱图)。
图6是本发明实施例1、对比例1和对比例2所得NiPt-Ni(OH)2/La(OH)3催化剂、NiPt-Ni(OH)2催化剂和NiPt-Ni(OH)2+La(OH)3混合物在室温下催化肼分解性能测试图。
图7是本发明实施例1所得NiPt-Ni(OH)2/La(OH)3催化剂不同温度下催化肼分解性能测试图。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例1:
1)在4mL水中加入40mg La(OH)3超声搅拌10min,得到均一溶液;
2)向步骤1)的溶液中加入含有0.05mmol氯化镍和0.06mmol四氯铂酸钾的溶液,超声搅拌10min;
3)向步骤2)的溶液中加入36mg的NaOH,搅拌超声10min;
4)向步骤3)的溶液中加入30mg的NaBH4,搅拌至反应完全;
5)将步骤4)所得产物离心洗涤至中性,分离干燥得到NiPt-Ni(OH)2/La(OH)3催化剂。
对比例1:
将实施例1的步骤1)的加入40mg La(OH)3改为加入0mg La(OH)3。其他步骤同实施例 1,得到NiPt-Ni(OH)2催化剂。
实施例2:
将实施例1的步骤1)的加入40mg La(OH)3改为加入5mg La(OH)3。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
实施例3:
将实施例1的步骤1)的加入40mg La(OH)3改为加入100mg La(OH)3。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
实施例4:
将实施例1的步骤3)的加入36mg的NaOH改为加入5mg的NaOH。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
实施例5:
将实施例1的步骤3)的加入36mg的NaOH改为加入50mg的NaOH。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
实施例6:
将实施例1的步骤4)的加入30mg的NaBH4改为加入15mg的NaBH4。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
实施例7:
将实施例1的步骤4)的加入30mg的NaBH4改为加入100mg的NaBH4。其他步骤同实施例1,得到NiPt-Ni(OH)2/La(OH)3催化剂。
对比例2:
将实施例1的步骤改为加入0mg La(OH)3。其他步骤同实施例1,得到NiPt-Ni(OH)2催化剂,并加入步骤6):将所得NiPt-Ni(OH)2催化剂与40mg La(OH)3搅拌均匀,得到 NiPt-Ni(OH)2+La(OH)3混合物。
实施例9-11
采用实施例1、对比例1和对比例2所得的复合纳米催化剂用于肼分解制氢(分别对应实施例9、10和11),将催化剂置于含4mL超纯水的50mL三口烧瓶中,然后加入水合肼。在298K下进行反应(结果如图6所示),结束后得如下结果(表一):
表一
实施例12-16:
采用实施例1所得的NiPt-Ni(OH)2/La(OH)3催化剂在五个不同的反应温度下催化肼分解制氢(分别对应实施例12-16)。将催化剂置于含5mL超纯水的三口烧瓶中,然后加入水合肼。在不同温度下进行反应(结果如图7所示),结束后得如下结果(表二)
表二
Claims (7)
1.NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,所述NiPt-Ni(OH)2/La(OH)3催化剂由金属Ni、金属Pt、金属氢氧化物Ni(OH)2以及稀土氢氧化物La(OH)3组成,其化学式为NiPt-Ni(OH)2/La(OH)3,其中Ni的含量为2~15 wt.%,Pt的含量为8~55wt.%,Ni(OH)2的含量为0.5~6 wt.%,La(OH)3的含量为27~89 wt.%。
2.根据权利要求1所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,Ni的含量为2.1~13.0 wt.%,Pt的含量为8.1~54.1 wt.%,Ni(OH)2的含量为0.8~5.1wt.%,La(OH)3的含量为27.7~88.5 wt.%。
3.根据权利要求1所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,所述NiPt-Ni(OH)2/La(OH)3催化剂的制备方法具体包括以下步骤:
1)在水中加入La(OH)3并混合均匀;
2)向步骤1)得到的溶液中加入Ni和Pt的前驱体溶液,超声处理并混合均匀;
3)向步骤2)得到的溶液中加入NaOH,超声处理并混合均匀;
4)向步骤3)得到的溶液中加入NaBH4,混合均匀并反应一段时间;
5)从步骤4)得到的溶液中分离出固态物质,洗涤并干燥,得到所述的NiPt-Ni(OH)2/La(OH)3催化剂。
4.根据权利要求3所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,Ni和Pt的前驱体溶液为Ni盐和Pt盐的水溶液。
5.根据权利要求4所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,Ni和Pt的前驱体溶液为NiCl2和K2PtCl4的水溶液。
6.根据权利要求4所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,Ni盐和Pt盐的摩尔比为1:1。
7.根据权利要求3所述的NiPt-Ni(OH)2/La(OH)3催化剂在催化肼产氢中的应用,其特征在于,步骤4)反应时间为10 min。
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