以双二苯基膦甲烷(DPPM)为合成单元,采用超交联法制备超交联双二苯基膦甲烷(HCPs-DPPM),并以其为载体用水合肼还原制备负载Ni纳米粒子催化剂HCPs-DPPM-Ni,Ni纳米粒子的尺寸通过改变Ni的负载量和pH来调节。同时,制备了商业活性炭(AC)负载Ni的催化剂Ni/AC作为对比催化剂。通过FT-IR、BET、SEM和XRD等对催化剂进行表征,结果表明催化剂HCPs-DPPM-Ni具有大量微孔和介孔结构,比表面积能够达到626m2/g,其中Ni的负载量为50%的催化剂HCPs-DPPM-Ni(50%)具有最优的催化活性,当反应温度为25℃,4-硝基苯酚(4-NP)初始浓度为0.5mmol/L时,HCPs-DPPM-Ni(50%)催化剂加入量为0.83mg/mL、NaBH4加入量为0.125mol/L的条件下反应4min,4-NP的转化率能够达到99%。
The polymerization of commercial 1,2-diphenylphosphine-methane monomers adopted the method of hyper crosslinking prepared microporous organic polymer(HCPs-DPPM).HCPs-DPPM used as carrier the loaded Ni nanoparticle catalyst(HCPs-DPPM-Ni) was prepared with hydrazine hydrate reduction,through changing the load of Ni and the pH to adjust the size of Ni nanoparticles.The catalyst of commercial activated carbon(AC) loaded Ni was prepared.The catalysts were characterized by FT-IR,BET,SEM and XRD.The results showed that the HCPs-DPPM-Ni had a large number of microporous and mesoporous structure,the surface area of 626m2·g-1.HCPs-DPPM-Ni(50%) with the best catalytic activity.When the reaction temperature 25℃,initial concentration of 4-NP 0.5mmol·L-1,the nickel load of 50%,HCPs-DPPM-Ni 0.83mg·mL-1,the NaBH4 addition amount of 0.125mol·L-1,after 4min,4-NP conversion rate can reach 99%.
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基金资助
西华师范大学一般培育项目(17C038);西华师范大学英才科研基金项目(17Y031)
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