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先用偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅对硅胶进行了表面化学改性
然后进行了4-乙烯基吡啶(4VP)的接枝聚合
制备了接枝微粒P4VP/SiO2
接着使接枝微粒表面的聚4-乙烯基吡啶与Cu(Ⅱ)离子进行配合作用
最终制备了接枝于硅胶表面的配合物催化剂P4VP-Cu(Ⅱ)/SiO2.用红外光谱与热分析法对产物的化学结构及热稳定性进行了表征
采用扫描电镜观察了微粒的形貌
并重点考察了各种反应条件对制备配合物催化剂关键步骤——接枝聚合的影响规律.接枝聚合适宜的反应条件为:乙醇为溶剂
4VP浓度为15~20 wt%
引发剂为单体质量的2 wt%
反应时间7 h
反应温度80℃
在此条件下接枝微粒的接枝度可达25 g/100 g.热失重(TG)测试结果表明:与未接枝的配合物P4VP-Cu(Ⅱ)相比
接枝在SiO2表面的配合物P4VP-Cu(Ⅱ)
热稳定性得到了显著的提高.
Micrometer-sized silica gel was modified chemically by using γ-methacryloxypropyl trimethoxysilane(MPTMS) as a coupling agent
and double bond was introduced onto silica gel particle surface.4-vinylpyridine was grafted from silica gel surfaces
and grafting particles P4VP/SiO2 was prepared.The coordination between grafted P4VP and cupric ions was performed
and the complex catalyst P4VP-Cu(Ⅱ)/SiO2 was obtained.The chemical structure and thermal stability of the product were characterized with infrared spectrum(IR) and thermogravimetry(TG) respectively
and the morphology of grafting particles P4VP/SiO2 was observed with scanning electron microscopy(SEM).The graft polymerization is a key step for the preparing of the complex catalyst P4VP-Cu(Ⅱ)/SiO2
so the effects of various factors on the graft polymerization were examined.The suitable conditions of reaction are as follows: a monomer concentration of 15~20 wt%
an initiator concentration of 2wt%(percent of monomer amount)
at 80 ℃ and for 7 h.Under these conditions
the grafting degree of P4VP could get up to 25 g/100 g.The results of TG determining showed that the complex P4VP-Cu(Ⅱ) grafted onto SiO2 has much better heat stability than the ungrafted complex P4VP-Cu(Ⅱ).
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