碳载高分散钯纳米粒子的制备及催化Suzuki反应

doi:10.11944/j.issn.1000-0518.2020.01.190161

摘要/Abstract

摘要：

利用三聚氰胺甲醛预聚物中N原子与Pd²⁺的相互作用,将Pd²⁺化学锚定在预聚物中;并以二氧化硅水凝胶为造孔剂、2,4-二氨基苯磺酸为预聚物缩合促进剂,在水溶液中制备出锚定了Pd²⁺的胶体纳米球;再经摩尔分数5%氢气焙烧、HF腐蚀,得到Pd质量分数为1.37%、平均粒径为(2.4±0.87) nm的碳载高分散Pd纳米粒子催化剂Pd@C。将其应用于Suzuki反应,在加入Pd与碘苯物质的量比为1:100的催化剂时,反应5 min收率为99.3%,且经8次循环后活性未降低,表现出良好的催化效果和重复使用性。

关键词: 三聚氰胺, 钯纳米粒子, 碳载体, Suzuki反应

Abstract:

Firstly, Pd²⁺ ions are anchored on melamine-formaldehyde prepolymer by the coordination with N atoms on the prepolymer. Then the colloidal nanospheres grow on silica hydrogel via the simultaneous condensation reaction accelerated by 2,4-diaminobenzenesulfonic acid. Finally, the carbon-supported highly dispersed palladiumPd@C catalyst is obtained after calcination in an atmosphere of 5%(molar fraction) H₂ and 95%(molar fraction) N₂ gases, followed by being treated with 5% HF solution. The prepared highly dispersed Pd nanoparticles with a loading amount of 1.37%(mass fraction) have an average diameter of (2.4±0.87) nm, and the catalytic performance of Pd@C has been further evaluated by Suzuki reaction. With the addition of molar ratio 1:100 catalyst, Pd@C performs both good catalytic activity with a yield of 99.3% achieved within 5 minutes, and excellent durability after 8 cycles.

Key words: melamine, palladium nanoparticles, carbon-support, Suzuki reaction

刘明辉, 刘盈岑, 吕荣文. 碳载高分散钯纳米粒子的制备及催化Suzuki反应[J]. 应用化学, 2020, 37(1): 61-68.

LIU Minghui, LIU Yingcen, Lü Rongwen. Preparation of Carbon-Supported Highly Dispersed Palladium Nanoparticles and Their Performance for Suzuki Reaction[J]. Chinese Journal of Applied Chemistry, 2020, 37(1): 61-68.

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