CN116159561A - 一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法 - Google Patents
一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法 Download PDFInfo
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- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 238000006356 dehydrogenation reaction Methods 0.000 title claims abstract description 27
- 230000003301 hydrolyzing effect Effects 0.000 title claims abstract description 26
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 14
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 10
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 6
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000006722 reduction reaction Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 33
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 27
- 239000001257 hydrogen Substances 0.000 abstract description 27
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 27
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- 239000011232 storage material Substances 0.000 abstract description 3
- 229910000510 noble metal Inorganic materials 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- -1 salt copper chloride dihydrate Chemical class 0.000 description 1
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- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 238000009210 therapy by ultrasound Methods 0.000 description 1
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Abstract
一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,涉及储氢材料及催化剂的制备技术领域。将聚乙烯吡咯烷酮溶解于去离子水中,加入氧化石墨烯形成分散液,再将二水合氯化铜、四水合氯化亚铁和六水合氯化钴的水溶液加入到该分散液中,混合均匀后加入硼氢化钠和氨硼烷在15℃~35℃下进行还原反应1~5h,然后将所得混合物离心、洗涤、再离心,最后经冷冻干燥得到三元金属CuFeCo纳米催化剂。本发明制得的三元金属CuFeCo纳米催化剂对氨硼烷水解脱氢反应具有较高的催化活性,并且催化剂重复使用稳定性良好。
Description
技术领域
本发明涉及储氢材料及催化剂的制备技术领域,尤其涉及一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法。
背景技术
近年来,在工业化进程中,煤、石油等化石能源不可避免的大量消耗,它们的不可再生性导致的能源短缺和使用附带的污染问题日益严重。而随着社会发展对能源的需求量仍在不断增加,这使得高效清洁的能源开发显得更加重要。氢能作为一种清洁、高效和可再生的能源,被认为是化石能源的理想替代和21世纪最具发展潜力的二次清洁能源。
然而,大量氢气的储存和运输问题是制约氢能大规模应用的重大制约因素。高压气态储氢即使在50MPa的高压下,储氢密度只有40g/L,不仅储氢密度较小,而且成本高,存在安全问题。低温液态储氢虽然储氢密度比高压气态储氢有所增加,达到71g/L,但需要在-240℃、1.3MPa的条件下,极其苛刻。相比于上述物理储氢,化学储氢具有较大的储氢量,其中氨硼烷具有储氢密度大(152.9g/L)、释放氢气的条件温和、无毒以及常温下为稳定的固体而易于储运等特点成为最有前景的储氢材料之一。氨硼烷在合适的催化剂作用下,在常温下进行水解即可以释放3个当量的氢气。
氨硼烷水解脱氢反应的催化剂按所含金属种类可分为单金属与多元金属体系,其中单金属催化剂中贵金属的催化活性较好;非贵金属成本低、资源丰富,但活性普遍较弱;单金属催化剂易团聚,易氧化,催化活性较低,性能不稳定;多元金属体系活性普遍有所提升,含贵金属的催化剂活性更高,但是使用贵金属成本较高。
中国专利CN 113522288 B公开以P-Cu-Co-3O-4@C为催化剂,用于氨硼烷水解脱氢,其表观活化能为38.31kJ/mol,经过5次循环催化反应后,催化活性就降至68%,稳定性较差。中国专利CN 113083325 A公开以Ru(1-x)Cox/P25为催化剂,用于氨硼烷水解脱氢,贵金属Ru价格昂贵,催化剂成本很高。中国专利CN 113522312 A公开以Ru-Fe-Co合金为催化剂,用于氨硼烷水解脱氢,同样贵金属Ru价格昂贵,催化剂成本很高。上述催化剂在制备过程中温度较高,存在安全隐患,使用了贵金属的催化剂在成本上过高,并且催化剂的循环稳定性较差。
发明内容
本发明的目的在于解决现有技术中的上述问题,提供一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,操作简单安全,成本低廉,具有良好重复使用的稳定性。
为达到上述目的,本发明采用如下技术方案:
一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法:在室温下将聚乙烯吡咯烷酮溶解于去离子水中,加入氧化石墨烯形成分散液,再将二水合氯化铜、四水合氯化亚铁和六水合氯化钴的水溶液加入到该分散液中,混合均匀后加入硼氢化钠和氨硼烷在15℃~35℃下进行还原反应1~5h,然后将所得混合物离心、洗涤、再离心,最后经冷冻干燥得到三元金属CuFeCo纳米催化剂。
所述聚乙烯吡咯烷酮的重均分子量为44000~54000,商品规格为K30;
所述聚乙烯吡咯烷酮的用量为二水合氯化铜质量的10%~200%;
所述氧化石墨烯使用量为二水合氯化铜质量50%~200%;
所述四水合氯化亚铁、六水合氯化钴和二水合氯化铜的摩尔比为0.5~3.5:0.5~3.5:1;
所述硼氢化钠的摩尔数与二水合氯化铜、四水合氯化亚铁和六水合氯化钴的总摩尔数之比为0.2~5:1;
所述氨硼烷的摩尔数与二水合氯化铜、四水合氯化亚铁和六水合氯化钴的总摩尔数之比为5~15:1。
催化剂对氨硼烷水解脱氢的催化活性用转换频率(TOF)表示:
相对于现有技术,本发明技术方案取得的有益效果是:
1、本发明所使用的非贵金属盐二水合氯化铜、四水合氯化亚铁和六水合氯化钴廉价易得,催化剂成本较低。
2、本发明中,聚乙烯比咯烷酮具有优异的分散性能和胶体保护作用,也可以络合金属离子,氧化石墨烯可负载固定金属纳米粒子,它们使得金属纳米粒子的分散性均匀、不会发生团聚,既提高了催化活性,又使催化剂具有良好的重复使用稳定性。
附图说明
图1为三元金属CuFeCo纳米催化剂催化氨硼烷水解脱氢放出的氢气体积(Vgas)与时间(t)的关系图。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚、明白,以下结合附图和实施例,对本发明做进一步详细说明。
实施例1
向一个置于超声仪中的25mL两颈烧瓶中加入10mL去离子水和5mg聚乙烯吡咯烷酮,开启超声搅拌,待聚乙烯吡咯烷酮全部溶解后,加入10mg氧化石墨烯,继续超声搅拌1小时,分散均匀后加入由6.8mg(0.04mmol)CuCl2·2H2O、7.9mg(0.04mmol)FeCl2·4H2O与28.5mg(0.12mmol)CoCl2·6H2O溶于5mL去离子水而组成的水溶液,继续超声搅拌1h,充分混合均匀后,加入5mg(0.13mmol)硼氢化钠和51mg(1.65mmol)氨硼烷,在25℃下进行还原反应2h。然后,将所得混合物离心(离心机转速为8000r/min)、去掉上层清液,加10mL去离子水洗涤、再离心,重复3次。最后,将所得混合物在-20℃、-0.1MPa下冷冻干燥12h,即得三元金属CuFeCo纳米催化剂,金属纳米粒子平均粒径8nm,通过电感耦合等离子体质谱(ICP-MS)测得所得催化剂中三种金属的摩尔比为Cu:Fe:Co=0.2:0.2:0.6。
采用排水集气法测定该催化剂催化氨硼烷水解脱氢的性能。结果表明,在25℃下该催化剂对氨硼烷水解脱氢的催化活性(TOF)为30.12molH2mol-1min-1。改变氨硼烷水解反应的温度(20℃、25℃、30℃和35℃),采用排水集气法测定该催化剂催化氨硼烷水解脱氢性能,根据Arrhenius公式,得到该催化反应活化能为26.6kJ/mol。
实施例2
测试实施例1中三元金属CuFeCo纳米催化剂重复使用的稳定性。利用排水法集气法监测氨硼烷水解反应期间释放的氢气体积。测试在带有磁力搅拌的25m双颈烧瓶中进行。双颈烧瓶的一个颈部连接气体滴瓶,便于测量氢气释放量,另一颈部连接恒压漏斗。将20mg氨硼烷和5mg催化剂加入双颈烧瓶中,将5mL去离子水从恒压漏斗迅速注入双颈烧瓶中,记录放出的氢气量。当氢气释放完毕后,再称取20mg氨硼烷溶于1mL去离子水中,注入双颈烧瓶中,进行该催化剂的第二次催化氨硼烷水解释氢,记录放出的氢气量。重复上述步骤直到第10次,结果见图1,在催化剂重复使用10次后催化剂仍保留初始催化活性的90%以上,表明该催化剂具有良好的重复使用稳定性。
实施例3
反应装置和操作方法同实施例1。其不同在于氧化石墨烯的加入量为5mg。结果表明,该催化剂在25℃下对氨硼烷水解脱氢的催化活性(TOF)为28.3molH2mol-1min-1。
对比例1
反应装置和操作方法同实施例1。其不同之处在于本例中不添加氧化石墨烯。结果表明,所得催化剂在25℃下对氨硼烷水解脱氢的催化活性(TOF)为23.5molH2mol-1min-1。
对比例2
反应装置和操作方法同实施例1。其不同之处在于本例中不添加聚乙烯吡咯烷酮。结果表明,所得催化剂在25℃下对氨硼烷水解脱氢的催化活性(TOF)为19.8molH2mol-1min-1。
对比例3
反应装置和操作方法同实施例1。其不同之处在于本例中不添加聚乙烯吡咯烷酮和氧化石墨烯。结果表明,所得催化剂在25℃下对氨硼烷水解脱氢的催化活性(TOF)为9.6molH2mol-1min-1。
Claims (7)
1.一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:将聚乙烯吡咯烷酮溶解于去离子水中,加入氧化石墨烯形成分散液,再将二水合氯化铜、四水合氯化亚铁和六水合氯化钴的水溶液加入到该分散液中,混合均匀后加入硼氢化钠和氨硼烷在15℃~35℃下进行还原反应1~5h,然后将所得混合物离心、洗涤、再离心,最后经冷冻干燥得到三元金属CuFeCo纳米催化剂。
2.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述聚乙烯吡咯烷酮的重均分子量为44000~54000。
3.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述聚乙烯吡咯烷酮的用量为二水合氯化铜质量的10%~200%。
4.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述氧化石墨烯的用量为二水合氯化铜质量的50%~200%。
5.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述四水合氯化亚铁、六水合氯化钴和二水合氯化铜的摩尔比为0.5~3.5:0.5~3.5:1。
6.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述硼氢化钠的摩尔数与二水合氯化铜、四水合氯化亚铁和六水合氯化钴的总摩尔数之比为0.2~5:1。
7.如权利要求1所述的一种用于催化氨硼烷水解脱氢的三元金属CuFeCo纳米催化剂的制备方法,其特征在于:所述氨硼烷的摩尔数与二水合氯化铜、四水合氯化亚铁和六水合氯化钴的总摩尔数之比为5~15:1。
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