CN110624609A - 一种磁性纳米催化剂的制备方法 - Google Patents
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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Abstract
本发明提供了一种磁性纳米催化剂的制备方法,该方法为:先由多巴胺自聚反应在四氧化三铁(Fe3O4)亚微球表面形成聚多巴胺层(PDA),即得到Fe3O4@PDA亚微球,然后将该亚微球转移到溶剂中,加入过渡金属(M)盐溶液,在适当的温度下反应一定时间,得到金属纳米粒子(NPs)负载于Fe3O4@PDA表面的复合物,即Fe3O4@PDA‑M NPs。该方法中用到的溶剂可以是水或乙醇,过渡金属可以是钯、金、钌、铂等离子化合物,反应温度可以在30~100℃。该方法无需另加还原剂即可形成金属纳米粒子。
Description
技术领域
本发明涉及一种磁性纳米催化剂的制备方法。
背景技术
四氧化三铁(Fe3O4)微纳米粒子具有优良的磁学性质和微波吸收功能,在诸多领域具有广泛的应用,与其他金属微纳米粒子相比,其制备过程较为简单,且材料价格更低廉易得,适合工业化生产。但是单个四氧化三铁微纳米球通常会发生团聚等现象,不利于催化反应,因此常使用二氧化硅、多巴胺、表面活性剂等物质包裹四氧化三铁,使得Fe3O4粒子均匀分散,表现出良好的亲水性。尤其是Fe3O4亚微米粒子还具备超顺磁性,无外加磁场时可快速分散在反应体系中充分接触反应物参与反应,又可在外加磁场的作用下迅速聚集而从反应体系中分离,把纳米过渡金属负载在磁性亚微米级粒子上,提高了过渡金属的稳定性,同时可以保持其催化活性,催化剂的回收更为方便。
改性的Fe3O4亚微球表面可以引入铂、金、钯、银等高活性的过渡金属,这些金属可以是离子型的,也可以是零价态的。零价态的纳米过渡金属通常通过还原沉淀法负载在Fe3O4亚微球表面,常用还原剂有水合肼、硼氢化合物及抗败坏血酸等,过渡金属的形状、大小及分散度受还原剂种类及Fe3O4亚微球表面性质等条件影响。
发明内容
本发明的目的在于:提供了一种磁性纳米催化剂的制备方法,使Fe3O4亚微球负载过渡金属纳米粒子的工艺更加简便高效。本发明特点在于:改进了过渡金属离子还原形成纳米粒子的方法,Fe3O4亚微球表面负载纳米过渡金属离子时无需另加还原剂,通过Fe3O4亚微球表面的聚多巴胺层吸附过渡金属离子,并直接被聚多巴胺层还原成零价态的金属纳米粒子。
磁性纳米催化剂制备方案如下:先由多巴胺自聚反应在四氧化三铁亚微球表面形成聚多巴胺层(PDA),即得到Fe3O4@PDA亚微球,然后将该亚微球转移到溶剂中,加入过渡金属(M)盐溶液,在适当的温度下反应一定时间,得到金属纳米粒子(NPs)负载于Fe3O4@PDA表面的复合物,即Fe3O4@PDA-M NPs。该方案中用到的溶剂可以是水或乙醇,过渡金属可以是钯、金、钌、铂等离子化合物,反应温度可以在30~100℃。
附图说明
图1为Fe3O4@PDA-Pd NPs催化剂的电镜扫描图像;图2为Fe3O4@PDA-Au NPs催化剂的电镜扫描图像;图3为Fe3O4@PDA-Ru NPs催化剂的电镜扫描图像;图4为Fe3O4@PDA-Pt NPs催化剂的电镜扫描图像。
具体实施方式
实施例1Fe3O4@PDA的制备
取0.152g浓氨水溶解于50mL去离子水中,加入0.1gFe3O4,超声分散均匀,加入盐酸多巴胺0.13g,超声分散均匀,30℃机械搅拌24h。
反应结束磁铁分离固液,固体用去离子水25mL*3洗涤,得Fe3O4@PDA复合物。
实施例2Fe3O4@PDA-Pd NPs的制备
加入5.9mg醋酸钯、0.8mL去离子水,边晃动边滴加1.2mL氨水,溶清后得到醋酸钯氨溶液。40mL乙醇中加入实施例1得到的Fe3O4@PDA,超声分散均匀,滴加上述的醋酸钯氨溶液,滴毕恒温30℃,机械搅拌24h。反应结束磁铁分离固液,固体依次用乙醇25mL*3、去离子水25mL*3洗涤,得Fe3O4@PDA-Pd NPs复合物(可保存于25mL乙醇中,干燥后约0.1g固体),电镜扫描图像见附图1。能谱分析钯含量3.16%。
实施例3Fe3O4@PDA-Au NPs的制备
加入8.0mg三氯化金,2mL去离子水,搅拌溶清得到三氯化金水溶液。40 mL去离子水中加入实施例1得到的Fe3O4@PDA,超声分散均匀,滴加上述的三氯化金水溶液,滴毕100℃回流,机械搅拌24h。反应结束磁铁分离固液,固体用去离子水25mL*3洗涤,得Fe3O4@PDA-AuNPs复合物(可保存于25mL 乙醇中,干燥后约0.1g固体),电镜扫描图像见附图2。能谱分析金含量3.08%。
实施例4Fe3O4@PDA-Ru NPs的制备
加入6.0mg三氯化钌,2mL去离子水,搅拌溶清得到三氯化钌水溶液。40 mL乙醇中加入实施例1得到的Fe3O4@PDA,超声分散均匀,滴加上述的三氯化钌水溶液,滴毕80℃回流,机械搅拌24h。反应结束磁铁分离固液,固体依次用乙醇25mL*3、去离子水25mL*3洗涤,得Fe3O4@PDA-Ru NPs复合物(可保存于25mL乙醇中,干燥后约0.1g固体),电镜扫描图像见附图3。能谱分析钌含量1.30%。
实施例5Fe3O4@PDA-Pt NPs的制备
加入7.0mg二氯化铂、0.8mL去离子水,边晃动边滴加1.2mL氨水,溶清后得到二氯化铂氨溶液。40mL去离子水中加入实施例1得到的Fe3O4@PDA,超声分散均匀,滴加上述的二氯化铂氨溶液,滴毕恒温60℃,机械搅拌24h。反应结束磁铁分离固液,固体用去离子水25mL*3洗涤,得Fe3O4@PDA-Pt NPs 复合物(可保存于25mL乙醇中,干燥后约0.1g固体),电镜扫描图像见附图4。能谱分析铂含量1.93%。
Claims (4)
1.一种磁性纳米催化剂的制备方法,方法如下:先由多巴胺自聚反应在四氧化三铁(Fe3O4)亚微球表面形成聚多巴胺层(PDA),即得到Fe3O4@PDA亚微球,然后将该亚微球转移到溶剂中,加入过渡金属(M)盐溶液,在适当的温度下反应一定时间,得到金属纳米粒子(NPs)负载于Fe3O4@PDA表面的复合物,即Fe3O4@PDA-M NPs。
2.根据权利要求1所述的一种磁性纳米催化剂的制备方法,其特征在于:方法所述的溶剂为水或乙醇。
3.根据权利要求1所述的一种磁性纳米催化剂的制备方法,其特征在于:方法所述的过渡金属为钯、金、钌、铂。
4.根据权利要求1所述的一种磁性纳米催化剂的制备方法,其特征在于:方法所述的温度为30~100℃。
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Cited By (5)
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CN111605276A (zh) * | 2020-06-30 | 2020-09-01 | 江南大学 | 一种熔融共挤多层透明的紫外近红外屏蔽高分子材料、制备方法及其应用 |
CN111716833A (zh) * | 2020-06-30 | 2020-09-29 | 江南大学 | 一种涂覆型多层透明的紫外近红外屏蔽高分子材料、制备方法及其应用 |
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CN111605276A (zh) * | 2020-06-30 | 2020-09-01 | 江南大学 | 一种熔融共挤多层透明的紫外近红外屏蔽高分子材料、制备方法及其应用 |
CN111716833A (zh) * | 2020-06-30 | 2020-09-29 | 江南大学 | 一种涂覆型多层透明的紫外近红外屏蔽高分子材料、制备方法及其应用 |
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CN112868668A (zh) * | 2021-03-19 | 2021-06-01 | 常州英诺升康生物医药科技有限公司 | 一种Fe3O4-DA-AMP纳米复合抗菌材料及其制备方法和应用 |
KR102436881B1 (ko) * | 2021-05-17 | 2022-08-26 | 한양대학교 에리카산학협력단 | 폴리도파민 지지체를 기반으로 하는 유기화학반응 촉매 및 그 제조 방법 |
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