CN107715883A - 一种Ni3FeN@石墨烯/海藻气凝胶电催化剂的制备方法 - Google Patents
一种Ni3FeN@石墨烯/海藻气凝胶电催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000661 sodium alginate Substances 0.000 claims abstract description 19
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 19
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 14
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 238000005342 ion exchange Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910001453 nickel ion Inorganic materials 0.000 claims description 9
- 235000010443 alginic acid Nutrition 0.000 claims description 8
- 239000000783 alginic acid Substances 0.000 claims description 8
- 229920000615 alginic acid Polymers 0.000 claims description 8
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- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims 1
- PXCKGGKGXIORDT-UHFFFAOYSA-L dichloroiron;iron Chemical compound [Fe].Cl[Fe]Cl PXCKGGKGXIORDT-UHFFFAOYSA-L 0.000 claims 1
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- 238000010189 synthetic method Methods 0.000 description 2
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 229910001415 sodium ion Inorganic materials 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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Abstract
本发明公开了一种Ni3FeN@石墨烯/海藻气凝胶电催化剂的制备方法,该方法是将石墨烯/海藻酸钠与Fe3+,Ni2+进行离子交换,将交换后的水凝胶冷冻干燥,再经管式炉氨气下高温焙烧后制得。该制备方法所用海藻为生物质材料,是绿色环保的新材料,而且制备方法简单,所得Ni3FeN@石墨烯/海藻气凝胶因其金属性和特殊的三维立体气凝胶结构而具有较高的活性位点和高催化性能。
Description
技术领域
本发明属于电催化剂领域,具体涉及一种离子交换法制备的Ni3FeN@石墨烯/海藻气凝胶电催化剂的制备方法。
背景技术
Ni3FeN电催化材料,由于具有金属导电性,催化活性高,双官能催化活性等优点,受到广泛的关注。已报道的Ni3FeN电催化剂的合成方法包括,共沉淀法、原位生长法,水热和溶剂热法等。然而,这些方法多依赖于以基底为原料的生长,合成方法单一,从而导致催化活性降低,而且在强碱性电解质下稳定性较差,制约着Ni3FeN在全水解实际应用中的的广泛应用。
考虑到以上等问题,本发明利用海藻为模版,首先海藻酸钠是从天然海藻中提取的,其次海藻酸钠中的羧基和羟基能够与铁离子和镍离子形成稳定的蛋盒结构螯合物,经高温处理后海藻酸的碳,氮,氢会热分解,从而形成核壳结构的Ni3FeN封装在氮掺杂无定形碳中,且均匀分布在三维石墨烯海藻气凝胶上,该材料的石墨烯增加了材料导电性和稳定性,同时由于Ni3FeN的金属性质及核壳结构,提供了更多的活性位点,从而有效提高Ni3FeN@石墨烯/海藻气凝胶电催化剂的催化效率。其次,三维多层介孔纳米气凝胶结构提供了更多的孔道,有助于提高材料的比表面积。因此,Ni3FeN@石墨烯/海藻气凝胶将是一个高催化活性,低成本,环保的电催化剂。
发明内容
本发明的目的在于制备一种代替传统贵金属催化剂,克服传统贵金属催化剂成本高,存量少的缺点。制备一种具有高催化活性,超强稳定性的Ni3FeN@石墨烯/海藻气凝胶电催化剂。
本发明提出的Ni3FeN@rGO/海藻气凝胶电催化剂的制备方法,包括以下步骤:
1.一定量的海藻酸钠与一定的还原氧化石墨烯混合分散在去离子水中,加入氯化镍和氯化铁的混合溶液,镍离子和铁离子交换掉海藻酸钠中的钠离子。
2.将步骤1处理好的海藻酸盐/rGO水凝胶进行真空冷冻干燥24h。
3.将步骤2的水凝胶驱体在管式炉中氨气中高温焙烧。
4.将步骤3的产物充分干燥,得到Ni3FeN@rGO/海藻气凝胶电催化剂。
所述的海藻酸钠为阿拉丁试剂。
步骤1所述氯化镍和氯化铁浓度为1mol/L,比例为10∶1。
步骤2所述真空冷冻干燥时间为48h。
步骤3所述焙烧温度为600-800℃。
与现有技术相比,本发明的有益效果是使用一种绿色环保的海藻酸作为模板,利用海藻酸的螯合作用得到的核壳结构的Ni3FeN@rGO/海藻气凝胶材料的三维气凝胶结构有利于精确调整Ni-Fe比,容易实现Ni3FeN二元协同互补效应;高度多孔和三维相互作用的气凝胶结构可以增强分子转运和催化活性。
附图说明
图1 Ni3FeN@石墨烯/海藻气凝胶的电镜图片
图2 Ni3FeN@石墨烯/海藻气凝胶的XRD图片
图3 Ni3FeN@石墨烯/海藻气凝胶的OER线性扫描曲线
图4 Ni3FeN@石墨烯/海藻气凝胶的HER线性扫描曲线
实施例
实施例一:1g的海藻酸钠99g水配置成1%的海藻酸钠溶液,与0.1g石墨烯(质量比为海藻酸钠的10%)混合均匀,随后将混合液加入200mL去离子水配置成的浓度为0.1mol/L的铁离子和镍离子混合溶液中,静止三十分钟,得到的Ni,Fe-石墨烯/海藻酸水凝胶。将上述水凝胶真空冷冻干燥12小时。将材料在管式炉中氨气氛围下升温到700℃,升温速率为5℃/min,焙烧1h,后冷却到室温,得到Ni3FeN@石墨烯/海藻气凝电催化剂。
实施例二:1g的海藻酸钠99g水配置成1%的海藻酸钠溶液,与0.2g石墨烯(质量比为海藻酸钠的20%)混合均匀,随后将混合液加入200mL去离子水配置成的浓度为0.1mol/L的铁离子和镍离子混合溶液中,静止三十分钟,得到的Ni,Fe-石墨烯/海藻酸水凝胶。将上述水凝胶真空冷冻干燥12小时。将材料在管式炉中氨气氛围下升温到700℃,升温速率为5℃/min,焙烧1h,后冷却到室温,得到Ni3FeN@石墨烯/海藻气凝电催化剂。
实施例三:1g的海藻酸钠99g水配置成1%的海藻酸钠溶液,与0.3g石墨烯(质量比为海藻酸钠的30%)混合均匀,随后将混合液加入200mL去离子水配置成的浓度为0.1mol/L的铁离子和镍离子混合溶液中,静止三十分钟,得到的Ni,Fe-石墨烯/海藻酸水凝胶。将上述水凝胶真空冷冻干燥12小时。将材料在管式炉中氨气氛围下升温到700℃,升温速率为5℃/min,焙烧1h,后冷却到室温,得到石墨烯/海藻气凝电催化剂。
实施例四:1g的海藻酸钠99g水配置成1%的海藻酸钠溶液,随后将混合液加入200mL去离子水配置成的浓度为0.1mol/L的铁离子和镍离子混合溶液中,静止三十分钟,得到的Ni,Fe-石墨烯/海藻酸水凝胶。将上述水凝胶真空冷冻干燥12小时。将材料在管式炉中氨气氛围下升温到700℃,升温速率为5℃/min,焙烧1h,后冷却到室温,得到Ni3FeN@石墨烯/海藻气凝电催化剂。
Claims (5)
1.一种Ni3FeN@石墨烯/海藻气凝胶电催化剂的制备方法,其特征在于:使用环保的生物质新材料海藻作为模版,通过离子交换作用和高温热处理制备Ni3FeN@石墨烯/海藻气凝胶电催化剂的方法。
2.根据权利要求1所述的Ni3FeN@石墨烯/海藻气凝电催化剂的制备方法,其特征在于:通过离子交换实现铁离子、镍离子与海藻酸钠结合,进而得到Ni3FeN@石墨烯/海藻气凝胶电催化剂。
3.根据权利要求2所述的Ni3FeN@石墨烯/海藻气凝电催化剂的制备方法,其特征在于:首先将质量分数1%的海藻酸钠溶液与石墨烯混合,随后将混合液加入浓度为0.1mol/L的铁离子和镍离子混合溶液中,得到的Ni,Fe-石墨烯/海藻酸水凝胶。将上述水凝胶真空冷冻干燥12小时。将材料在管式炉中氨气氛围下升温到700℃,升温速率为5℃/min,焙烧1h,后冷却到室温,得到Ni3FeN@石墨烯/海藻气凝胶电催化剂。
4.根据权利要求3所述制备方法,其特征在于:铁离子/镍离子的盐混合溶液为氯化铁铁、氯化镍。比例为1∶10。
5.根据权利要求3所述制备方法,其特征在于:焙烧温度为700℃-800℃,碳化时间为1-2h,升温速率为1-5℃/min。
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CN109939705B (zh) * | 2019-04-15 | 2021-09-28 | 福建农林大学 | 一种用于光催化还原二氧化碳的多元生物质复合气凝胶材料及其制备方法 |
CN110860688A (zh) * | 2019-11-19 | 2020-03-06 | 中国科学院生态环境研究中心 | 一种核壳结构双金属共价键合三维石墨烯宏观体及其制备方法 |
CN115722219A (zh) * | 2022-11-14 | 2023-03-03 | 浙江工业大学 | 一种颗粒炭材料负载金催化剂及其制备方法和在乙炔氢氯化制氯乙烯反应中的应用 |
CN115722219B (zh) * | 2022-11-14 | 2024-05-28 | 浙江工业大学 | 一种颗粒炭材料负载金催化剂及其制备方法和在乙炔氢氯化制氯乙烯反应中的应用 |
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