CN113967478B - 一种高热稳定钌单原子催化剂及其制备方法 - Google Patents
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 11
- 239000010941 cobalt Substances 0.000 claims abstract description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 8
- IYWJIYWFPADQAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;ruthenium Chemical compound [Ru].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O IYWJIYWFPADQAN-LNTINUHCSA-N 0.000 claims description 5
- NQZFAUXPNWSLBI-UHFFFAOYSA-N carbon monoxide;ruthenium Chemical group [Ru].[Ru].[Ru].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] NQZFAUXPNWSLBI-UHFFFAOYSA-N 0.000 claims description 5
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 5
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 5
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910021603 Ruthenium iodide Inorganic materials 0.000 claims description 3
- YLPJWCDYYXQCIP-UHFFFAOYSA-N nitroso nitrate;ruthenium Chemical compound [Ru].[O-][N+](=O)ON=O YLPJWCDYYXQCIP-UHFFFAOYSA-N 0.000 claims description 3
- LJZVDOUZSMHXJH-UHFFFAOYSA-K ruthenium(3+);triiodide Chemical compound [Ru+3].[I-].[I-].[I-] LJZVDOUZSMHXJH-UHFFFAOYSA-K 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 239000001307 helium Substances 0.000 claims 1
- 229910052734 helium Inorganic materials 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- 238000005470 impregnation Methods 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 239000002105 nanoparticle Substances 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 5
- 229910003266 NiCo Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001889 high-resolution electron micrograph Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明公开了一种高热稳定钌单原子催化剂及其制备方法，所用载体为钴基氧化物，利用等体积浸渍法、吸附法或物理混合法将钌前驱体与载体混合后，在空气或惰性气氛中经700‑1000℃焙烧1‑72小时后，可获得单原子分散的钌催化剂，钌的质量分数为0.01‑3wt％。本发明方法合成的负载型钌催化剂具有在高温情况下钌单原子不烧结的特点。
Description
技术领域
本发明属于催化剂技术领域，特别涉及一种高热稳定钌单原子催化剂及其制备方法。
背景技术
近年来，负载型铂族金属催化剂在工业生产中发挥着不可替代的作用，为国民经济发展做出了巨大的贡献，具有广阔的应用前景。一方面，不同于价格昂贵的铑、钯、铱和铂，钌元素具有相对低廉的价格，其催化剂可有效降低生产成本。另一方面，相较于传统的负载型铂族金属纳米催化剂，单原子催化剂具有最大化的原子利用率、均一的活性位点，对特定反应优异的活性和/或选择性，目前已经成为催化领域的研究热点，但制备高热稳定的铂族单原子催化剂仍是巨大的挑战。Lang等(Nat.Commun.,2019,10,234)报道了在高温氧化气氛下，氧化铁载体上铂纳米粒子可以发生再分散，生成高热稳定的铂单原子催化剂。Corma等(J.Am.Chem.Soc.,2016,138,15743)发表文章，通过一步合成法将铂物种限域在分子筛内，切换氧化和还原气氛，可实现单原子与纳米粒子之间的转换。Hu等(Nat.Nanotechnol.,2019,14,851)通过高温冲击波法，将负载在载体上的金属前驱体转变为稳定的单原子。目前，高热稳定铂族单原子催化剂的制备主要集中在铂元素上，与高热稳定钌单原子催化剂制备相关的工作鲜有报道，对于该类催化剂的制备是仍是研究的一个难点。
发明内容
本发明公开了一种高热稳定钌单原子催化剂及其制备方法，载体为钴基氧化物，催化剂中钌质量分数为0.01-3wt％。解决了高温过程中钌单原子易团聚烧结的问题。
为了达到上述目的，本发明采用的技术方案是，一种钌单原子催化剂的制备方法，包括以下步骤：
将钴基氧化物(四氧化三钴、钴酸锌、钴酸镍、钴酸镁或钴酸镧)载体等体积浸渍在相应浓度的活性组分钌的前驱体溶液中，所述钌的前驱体为氯化钌、乙酰丙酮钌、羰基钌、碘化钌、亚硝酰硝酸钌等。室温干燥2-24小时，然后在60-150℃干燥2-24小时，最后在空气和/或惰性气氛下700-1000℃焙烧1-72小时，得到钌的重量百分含量为0.01-3wt％的单原子催化剂；
或，将钴基氧化物(四氧化三钴、钴酸锌、钴酸镍、钴酸镁或钴酸镧)载体浸渍于含有活性组分钌的前驱体溶液中，所述钌的前驱体为氯化钌、乙酰丙酮钌、羰基钌、碘化钌、亚硝酰硝酸钌等。搅拌1-24h，移至水浴60-90℃条件下搅拌至溶液完全蒸干，并在100-150℃干燥2-24小时，最后在空气和/或惰性气氛下700-1000℃焙烧1-72小时，得到钌的重量百分含量为0.01-3wt％的单原子催化剂；
或，按所需质量比例将钴基氧化物(四氧化三钴、钴酸锌、钴酸镍、钴酸镁或钴酸镧)载体直接与氧化钌粉末物理混合，然后在空气和/或惰性气氛下700-1000℃焙烧1-72小时，得到钌的重量百分含量为0.01-3wt％的单原子催化剂。
本发明方法合成的负载型钌单原子催化剂具有在高温(700-1000℃)情况下单原子抗团聚烧结的特点，具有高热稳定性。
附图说明
图1为采用本发明所述方法实施例1、2、3和4制备的1.0wt％Ru/Co3O4-RuCl3-800℃-5h(a)、2.0wt％Ru/ZnCo2O4-RuO2-Ar-900℃-24h(b)、1.2wt％Ru/NiCo2O4-Ru(acac)3-700℃-48h(c)和0.2wt％Ru/MgCo2O4-Ru3(CO)12-900℃-2h(d)的XRD图，所有样品中均未出现RuO2特征衍射峰。
图2为采用本发明所述方法实施例1制备的1.0wt％Ru/Co3O4-RuCl3-800℃-5h催化剂的高分辨电镜照片，催化剂中没有钌物种纳米粒子存在，说明钌以高度分散的形式存在。
图3为采用本发明所述方法实施例1制备的1.0wt％Ru/Co3O4-RuCl3-800℃-5h催化剂的球差校正电镜照片，钌单原子均匀分散在载体上，证实生成高热稳定的单原子催化剂。
图4为采用本发明所述方法实施例3制备的1.2wt％Ru/NiCo2O4-Ru(acac)3-700℃-48h催化剂的球差校正电镜照片，该催化剂中未发现钌物种纳米粒子存在，钌均以单原子形式存在。
具体实施方式
实施例1：以氯化钌作为前驱体的Co3O4负载的钌单原子催化剂制备
将2.0g Co3O4载体加入200mL含有99mmol/L的活性组分氯化钌溶液中，室温搅拌10小时，移至水浴80℃条件下搅拌至溶液完全蒸干，然后在120℃干燥5小时，最后在空气气氛下800℃焙烧5小时后，得到钌的理论重量百分含量为1.0wt％的Co3O4负载的钌单原子催化剂，通过电镜表征，该催化剂中没有钌物种纳米粒子存在，且钌均以单原子形式存在，证实制得高热稳定钌单原子催化剂。
实施例2：以氧化钌作为前驱体的ZnCo2O4负载的钌单原子催化剂制备
将2.5g ZnCo2O4载体与0.0676g氧化钌粉末物理混合，然后在氩气气氛下900℃焙烧24小时后，得到钌的理论重量百分含量为2.0wt％的ZnCo2O4负载的钌单原子催化剂，通过电镜表征，该催化剂中没有钌物种纳米粒子存在，且钌均以单原子形式存在，证实制得高热稳定钌单原子催化剂。
实施例3：以乙酰丙酮钌作为前驱体的NiCo2O4负载的钌单原子催化剂制备
将1.0g NiCo2O4载体等体积浸渍在0.4mL 303mmol/L的活性组分乙酰丙酮钌溶液中，室温干燥24小时，然后在80℃干燥10小时，最后在空气气氛下700℃焙烧48小时后，得到钌的理论重量百分含量为1.2wt％的NiCo2O4负载的钌单原子催化剂，通过电镜表征，该催化剂中没有钌物种纳米粒子存在，且钌均以单原子形式存在，证实制得高热稳定钌单原子催化剂。
实施例4：以羰基钌作为前驱体的MgCo2O4负载的钌单原子催化剂制备
将2.0g MgCo2O4载体等体积浸渍在0.9mL 44mmol/L的活性组分羰基钌溶液中，室温干燥6小时，然后在120℃干燥6小时，最后在空气气氛下900℃焙烧2小时后，得到钌的理论重量百分含量为0.2wt％的MgCo2O4负载的钌单原子催化剂，通过电镜表征，该催化剂中没有钌物种纳米粒子存在，且钌均以单原子形式存在，证实制得高热稳定钌单原子催化剂。
Claims (5)
1.一种高热稳定钌单原子催化剂，其特征在于：所述催化剂为负载型钌催化剂，载体为钴基氧化物材料，催化剂中钌质量分数为0.01-3wt%；钴基氧化物载体为四氧化三钴、钴酸锌、钴酸镍、钴酸镁、钴酸镧中的一种或二种以上；
可采用下述任一过程制备高热稳定钌单原子催化剂：
等体积溶液浸渍，将钴基氧化物载体等体积浸渍在相应浓度的活性组分钌的前驱体溶液中，室温干燥2-24小时，然后在60-150℃干燥2-24小时，最后在空气和/或惰性气氛下700-1000oC焙烧1-72小时，得到钌的重量百分含量为0.01-3wt%的单原子催化剂；
或吸附法，将钴基氧化物载体浸渍于含有活性组分钌的前驱体溶液中，搅拌1-24 h，移至水浴60-90oC条件下搅拌至溶液完全蒸干，并在100-150℃干燥2-24小时，最后在空气和/或惰性气氛下700-1000oC焙烧1-72小时，得到钌的重量百分含量为0.01-3wt%的单原子催化剂；
或物理混合法，按所需质量比例将钴基氧化物载体直接与氧化钌粉末物理混合，然后在空气和/或惰性气氛下700-1000oC焙烧1-72小时，得到钌的重量百分含量为0.01-3wt%的单原子催化剂。
2.根据权利要求1所述的催化剂，其特征在于：
所述钌的前驱体为氯化钌、乙酰丙酮钌、羰基钌、碘化钌、亚硝酰硝酸钌中的一种或两种以上。
3.根据权利要求1所述的催化剂，其特征在于：
惰性气氛为氩气、氦气或氮气气氛中的一种或二种以上。
4.根据权利要求1所述的催化剂，其特征在于：
所述的氧化钌粉末为商业试剂或实验室自制。
5.根据权利要求1所述的催化剂，其特征在于：所述催化剂中钌质量分数为0.1-2wt%。
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