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通过表面交换反应,以多巴胺为偶联剂,将三苯基膦担载到磁性纳米氧化铁表面制得磁性纳米三苯基膦配体,其结构通过红外光谱、元素分析以及热重分析进行了表征。初步考察了表面交换反应条件对三苯基膦在纳米粒子表面担载量的影响;提高多巴胺-三苯基膦衍生物与磁性纳米氧化铁粒子比例以及延长超声时间有助于提高三苯基膦的担载量。在优化后的反应条件下,即苯乙烯1.25 m L,30 mg磁性纳米三苯基膦,1.8 mg Rh(OAc)2,12 m L无水四氢呋喃,3 MPa合成气VCO∶VH2=1∶1,纳米三苯基膦配体中的三苯基膦含量为0.21μmol/mg,该配体能够与Rh(OAc)2一起催化苯乙烯的氢甲酰化反应并能重复使用4次,且仅有4.8%的三苯基膦配体从纳米粒子表面脱落。
By the surface exchange reaction, dopamine as coupling agent, the triphenylphosphine supported on the surface of magnetic nano-iron oxide magnetic nano-triphenylphosphine ligand, the structure of which was characterized by IR, elemental analysis and thermogravimetric analysis Characterization. The effects of surface exchange reaction conditions on the loading of triphenylphosphine on the surface of nanoparticles were investigated. It was found that increasing the ratio of dopamine-triphenylphosphine derivatives to magnetic nano-iron oxide particles and prolonging the sonication time could improve the yield of triphenylphosphine Of the load. Under optimized reaction conditions, styrene 1.25 m L, 30 mg of magnetic nanometer triphenylphosphine, 1.8 mg of Rh (OAc) 2,12 m L of anhydrous tetrahydrofuran, 3 MPa of syngas VCO: VH 2 = 1: 1 , The triphenylphosphine content in the nano-triphenylphosphine ligand was 0.21 μmol / mg, which can catalyze the hydroformylation of styrene together with Rh (OAc) 2 and can be reused for 4 times, and only 4.8% of the triphenylphosphine ligands are released from the surface of the nanoparticles.