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水热条件下合成了含M2+离子(Mg2+、Co2+、Ni2+和Zn2+)的介孔Smectite材料.经X射线粉末衍射和比表面积与孔隙率测定,确定了其晶体结构和孔性质.以配位体交换法固载金属Pd配合物———Pd(PhCH2CN)2Cl2,制备固载Pd配合物的Smectite介孔材料催化剂———SM(M)Pd.负载后平均孔径的测定结果表明,SM(M)Pd平均孔径均高于H-Mont-Pd平均孔径(3.70 nm),说明固载的Pd(PhCH2CN)2Cl2能够扩大H-Mont-Pd孔径.不同SM(M)Pd催化Heck偶联反应结果表明,SM(Co)Pd催化剂活性最好,这一方面与SM(Co)Pd具有最大的比表面积和孔容一致,另外也与Co2+电子结构有关.在该催化剂下,碘苯与丙烯酸甲酯的Heck偶联反应的适宜溶剂是N,N-二甲基乙酰胺(NMAC),反应温度为80℃,反应时间1 h,催化剂用量5 mg/mmol碘苯,5次重复使用催化剂活性没有下降,碘苯转化率接近100%.
The mesoporous Smectite material containing M2 + ions (Mg2 +, Co2 +, Ni2 + and Zn2 +) was synthesized under hydrothermal conditions.The crystal structure and pore properties of the mesoporous Smectite were determined by X-ray powder diffraction and specific surface area and porosity determination. The exchange method, Pd (PhCH2CN) 2Cl2, was used to prepare the Smectite mesoporous material supported on Pd complex, SM (M) Pd. The average pore size after loading showed that SM ) Pd average pore size is higher than that of H-Mont-Pd (3.70 nm), indicating that the immobilized Pd (PhCH2CN) 2Cl2 can enlarge the H-Mont-Pd pore size.The results of Heck coupling reaction catalyzed by different SM , The activity of SM (Co) Pd catalyst is the best, which is consistent with the largest specific surface area and pore volume of SM (Co) Pd on the one hand and the Co2 + electronic structure on the other hand.In this catalyst, iodobenzene and methyl acrylate Heck coupling reaction of N, N-dimethylacetamide (NMAC), the reaction temperature was 80 ℃, the reaction time 1 h, the amount of catalyst 5 mg / mmol iodobenzene, 5 times repeated use of the catalyst activity did not decline, Iodobenzene conversion is close to 100%.