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构建了巯基/偶氮二异丁腈(—SH/AIBN)氧化还原引发体系,成功地实施了单体甲基丙烯酸缩水甘油酯(GMA)在微米级硅胶微粒表面引发接枝聚合,制得接枝微粒PGMA/SiO_2。然后,以4-羟基-2,2,6,6-四甲基哌啶氮氧自由基(4-OHTEMPO)为试剂,使PGMA/SiO_2微粒表面的环氧基团发生开环反应,从而制得TEMPO固载微粒PGMA/SiO_2-TEMPO,并研究了主要因素对固载化反应的影响,同时采用多种方法对产物进行表征。最后,将PGMA/SiO_2-TEMPO与Fe(NO_3)_3组成共催化体系,催化氧化肉桂醇。结果表明,共催化体系在适宜条件下可有效地催化氧化肉桂醇,得到单一产物肉桂醛,反应16 h肉桂醛的产率可达88%。此外,该催化剂具有良好的循环使用性能。
A thiol / azobisisobutyronitrile (-SH / AIBN) redox initiator system was constructed. The graft polymerization of monomeric glycidyl methacrylate (GMA) on the surface of micrometer silica particles was successfully carried out. Particle PGMA / SiO_2. Then, 4-hydroxy-2,2,6,6-tetramethylpiperidine nitroxide (4-OHTEMPO) was used as a reagent to ring-open the epoxy groups on the surface of PGMA / SiO 2 particles TEMPO particles were immobilized on PGMA / SiO_2-TEMPO. The effects of main factors on the immobilization reaction were also studied. At the same time, a variety of methods were used to characterize the product. Finally, PGMA / SiO_2-TEMPO and Fe (NO_3) _3 were co-catalyzed to catalyze the oxidation of cinnamyl alcohol. The results showed that under the proper conditions, the cocatalyst could catalyze the oxidation of cinnamyl alcohol effectively, and the single product cinnamaldehyde was obtained. The yield of cinnamaldehyde reached 16% in 16 h. In addition, the catalyst has good recycling performance.