CN116855999A - 一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法 - Google Patents
一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法 Download PDFInfo
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 29
- QZCHKAUWIRYEGK-UHFFFAOYSA-N tellanylidenecopper Chemical compound [Te]=[Cu] QZCHKAUWIRYEGK-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- 238000006722 reduction reaction Methods 0.000 claims abstract description 20
- 238000011056 performance test Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000012279 sodium borohydride Substances 0.000 claims description 10
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 10
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229920000557 Nafion® Polymers 0.000 claims description 5
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 235000010288 sodium nitrite Nutrition 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000002106 nanomesh Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(i) oxide Chemical compound [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009620 Haber process Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- DVOKWRXNWTZRDW-UHFFFAOYSA-N [Ru].[Ru]=O Chemical compound [Ru].[Ru]=O DVOKWRXNWTZRDW-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
本发明涉及一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法,催化剂的制备包括如下步骤:(1)反应溶液的配制;(2)多孔铜碲纳米网催化剂的制备;(3)电催化还原反应性能测试。本发明提供的有机无机复合催化剂的制备方法操作简单、成本低廉、绿色环保,适用于大规模化生产。多孔结构为分子渗透提供了丰富的通道,增加了反应物与催化剂之间的可达活性位点。另外,无定形的结构提供丰富的不饱和结构活性位点,从而提高了催化性能。
Description
【技术领域】
本发明属于催化材料技术领域,涉及一种无定型的海绵状纳米催化剂的制备方法,该催化剂可用于电催化亚硝酸根合成氨反应的研究。
【背景技术】
氨作为一种重要的化学产品,广泛应用于农业、工业和医药领域。由于其高氢密度(17.6wt%H2)、低液化温度和低运输成本,全球每年对氨的需求超过1.7亿吨,已成为世界第二大化学品,预计未来每年还将增长2.3%。另外,氨被视为一种有前景的无碳储能介质,可以作为能源载体分子,在未来的清洁能源社会,其需求有可能更加庞大。目前氨的生产主要是通过Haber-Bosch工艺在高温高压下将H和N催化合成NH3。由于所用H主要来源于天然气,每生产1吨氨气,会放出1.9吨CO2,这占了全球碳排放的总量的大约1.8%。因此,近年来人们积极探索各种绿色、可持续的合成氨路线。其中,由可再生能源驱动的电化学合成氨技术备受关注。
电催化硝酸盐还原制氨被认为是一种可持续发展的途径,但仍然存在一些基本的科学挑战。为了达到最优的电流效率,通常需要较高的还原过电位和能耗,同时竞争性析氢反应严重,导致合成氨的选择性低。通过精确调控催化剂的电子结构,可有效提升电催化性能。专利CN202110913241.5公开了一种电催化硝酸根或亚硝酸根合成氨的方法,该方法采用的电催化剂为金属-金属氧化物,所述金属-金属氧化物选自钌-氧化钌、铜-氧化铜、铜-氧化亚铜、等中的一种或多种组合。专利CN202110241969.8公开了一种金属磷化物在电催化亚硝酸盐合成氨中的应用,通过采用金属磷化物作为电催化剂,将亚硝酸盐催化还原为氨。本发明所提供的催化电极材料结构稳定,制备工艺简单,可有效实现其在将含硝酸根或亚硝酸根废水变为有价值的氨的应用。
【发明内容】
[要解决的技术问题]
为了解决需要还原过程中竞争性析氢反应严重,导致合成氨的选择性低合成氨的选择性低的问题,本发明提供了一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法。
[技术方案]
一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法,其特征在于铜碲催化剂的制备以及电催化还原反应应用,包括以下步骤:
(1)反应溶液的配制:
分别配制1mL浓度为20mM的亚碲酸钠水溶液、1mL浓度为20mM的氯化铜水溶液和20mL浓度为20mM的硼氢化钠水溶液;
(2)钯纳米颗粒催化剂的制备:
1mL亚碲酸钠溶液(20mM)和1mL氯化铜溶液(20mM)与10mL用冰超纯水新配制的硼氢化钠溶液(20mM)搅拌3min,还原过程中产生大量气体,并且观察到一种海绵状的黑色固体漂浮在溶液中,产品经过离心收集,超纯水、乙醇洗涤,并在60℃下干燥备用;
(3)电催化还原反应性能测试:
称取5mg的样品分散在490μL超纯水、490μL乙醇和10μL Nafion(5wt%)的混合溶液中,超声30分钟得到均匀的分散液,然后在面积1*1cm2的碳纸上滴加200μL催化剂溶液,载量为1mg/cm2。制成工作电极;同时铂片电极作为对电极,饱和甘汞电极作为参比电极组成三电极系统,在H型电解装置中进行还原性能测试;在测试前,电解槽的工作电极侧加入35mL 0.1M硫酸钠和0.01M亚硝酸钠溶液,对电极侧加入35mL 0.1M硫酸钠溶液,然后进行亚硝酸根还原合成氨的测试。
[有益效果]
(1)本发明以硼氢化钠为还原剂,制备了无定形海绵状铜碲纳米网催化剂。这种还原剂能有效简化催化剂的制备过程,显著降低催化剂的生产成本。
(2)本发明制备的海绵状铜碲电催化剂,无定形的结构提供丰富的不饱和结构活性位点,可以降低反应的能垒并增强中间体的吸附,从而提高了催化性能。
【附图说明】
图1为实施例1中铜碲海绵状催化剂的SEM图和TEM图。
图2为实施例1中铜碲海绵状催化剂的XRD和XPS图。
图3为实施例1中铜碲海绵状催化剂的LSV图。
图4为实施例1中铜碲海绵状催化剂的产氨率、FE和氨的选择性图。
图5为实施例1中铜碲海绵状催化剂的it图。
图6为实施例1中铜碲海绵状催化剂的BET图。
【具体实施方式】
实施例1:
(1)反应溶液的配制:
分别配制1mL浓度为20mM的亚碲酸钠水溶液、1mL浓度为20mM的氯化铜水溶液和20mL浓度为20mM的硼氢化钠水溶液;
(2)铜碲海绵状催化剂的制备:
1mL亚碲酸钠溶液(20mM)和1mL氯化铜溶液(20mM)与10mL用冰超纯水新配制的硼氢化钠溶液(20mM)搅拌3min,产品经过离心收集,超纯水、乙醇洗涤,并在60℃下干燥备用;
(3)电催化还原反应性能测试:
称取5mg的样品分散在490μL超纯水、490μL乙醇和10μL Nafion(5wt%)的混合溶液中,超声30分钟得到均匀的分散液,然后在面积1*1cm2的碳纸上滴加200μL催化剂溶液,载量为1mg/cm2。制成工作电极;同时铂片电极作为对电极,饱和甘汞电极作为参比电极组成三电极系统,在H型电解装置中进行还原性能测试;在测试前,电解槽的工作电极侧加入35mL 0.1M硫酸钠和0.01M亚硝酸钠溶液,对电极侧加入35mL 0.1M硫酸钠溶液,然后进行亚硝酸根还原合成氨的测试。
实施例2:
(1)反应溶液的配制:
分别配制1mL浓度为20mM的亚碲酸钠水溶液、1mL浓度为20mM的氯化铜水溶液和20mL浓度为20mM的抗坏血酸水溶液;
(2)铜碲海绵状催化剂的制备:
1mL亚碲酸钠溶液(20mM)和1mL氯化铜溶液(20mM)与10mL用冰超纯水新配制的抗坏血酸溶液(20mM)搅拌3min,产品经过离心收集,超纯水、乙醇洗涤,并在60℃下干燥备用;
(3)电催化还原反应性能测试:
称取5mg的样品分散在490μL超纯水、490μL乙醇和10μL Nafion(5wt%)的混合溶液中,超声30分钟得到均匀的分散液,然后在面积1*1cm2的碳纸上滴加200μL催化剂溶液,载量为1mg/cm2。制成工作电极;同时铂片电极作为对电极,饱和甘汞电极作为参比电极组成三电极系统,在H型电解装置中进行还原性能测试;在测试前,电解槽的工作电极侧加入35mL 0.1M硫酸钠和0.01M亚硝酸钠溶液,对电极侧加入35mL 0.1M硫酸钠溶液,然后进行亚硝酸根还原合成氨的测试。
实施例3:
(1)反应溶液的配制:
分别配制1mL浓度为20mM的亚碲酸钠水溶液、2mL浓度为20mM的氯化铜水溶液和20mL浓度为20mM的硼氢化钠水溶液;
(2)铜碲海绵状催化剂的制备:
1mL亚碲酸钠溶液(20mM)和2mL氯化铜溶液(20mM)与10mL用冰超纯水新配制的硼氢化钠溶液(20mM)搅拌3min,产品经过离心收集,超纯水、乙醇洗涤,并在60℃下干燥备用;
(3)电催化还原反应性能测试:
称取5mg的样品分散在490μL超纯水、490μL乙醇中和10μL Nafion(5wt%)的混合溶液中,超声30分钟得到均匀的分散液,然后滴加200μL溶液在面积1*1cm2的碳纸上,载量为1mg/cm2,制成工作电极;同时铂片电极作为对电极,饱和甘汞电极作为参比电极组成三电极系统,在H型电解装置中进行还原性能测试;在测试前,电解槽的工作电极侧加入35mL0.1M硫酸钠和0.01M亚硝酸钠溶液,对电极侧加入35mL 0.1M硫酸钠溶液,然后进行亚硝酸根还原合成氨的测试。
Claims (4)
1.一种用于电化学合成氨的海绵状铜碲电催化剂及其制备方法,其特征在于铜碲催化剂的制备以及电催化还原反应应用,包括以下步骤:
(1)反应溶液的配制
分别配制1mL浓度为20mM的亚碲酸钠水溶液、1mL浓度为20mM的氯化铜水溶液和20mL浓度为20mM的硼氢化钠水溶液;
(2)钯纳米颗粒催化剂的制备
1mL亚碲酸钠溶液(20mM)和1mL氯化铜溶液(20mM)与10mL用冰超纯水新配制的硼氢化钠溶液(20mM)搅拌3min,还原过程中产生大量气体,并且观察到一种海绵状的黑色固体漂浮在溶液中,产品经过离心收集,超纯水、乙醇洗涤,并在60℃下干燥备用;
(3)电催化还原反应性能测试
称取5mg的样品分散在490μL超纯水、490μL乙醇和10μL Nafion(5wt%)的混合溶液中,超声30分钟得到均匀的分散液,然后在面积1*1cm2的碳纸上滴加200μL催化剂溶液,载量为1mg/cm2;制成工作电极;同时铂片电极作为对电极,饱和甘汞电极作为参比电极组成三电极系统,在H型电解装置中进行还原性能测试;在测试前,电解槽的工作电极侧加入35mL0.1M硫酸钠和0.01M亚硝酸钠溶液,对电极侧加入35mL 0.1M硫酸钠溶液,然后进行亚硝酸根还原合成氨的测试。
2.根据权利要求1所述的铜碲催化剂的制备,其特征在于,其还原剂为硼氢化钠。
3.根据权利要求1所述的铜碲催化剂的制备,其特征在于反应时间为1min-5min。
4.根据权利要求1所述的铜碲催化剂的制备,其特征在于铜碲的摩尔比例为1:1、2:1、1:2、3:1或1:3。
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