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聚氯乙烯三乙撑四胺负载钯配合物的制备及对Heck反应的催化性能 被引量:10

Synthesis of Polyvinyl Chloride-triethylene-tetramine Supported Pal- ladium Complex and Its Catalytic Properties for Heck Reaction
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摘要 以聚氯乙烯为原料,通过胺化反应制得聚氯乙烯三乙撑四胺,然后用较简单方法得到聚氯乙烯三乙撑四胺负载钯配合物(PVC-TETA-Pd),利用XPS,TG,DTA和TEM等手段对其进行了表征.热分析表明PVC-TETA-Pd在室温至250℃范围内有很好的热稳定性;TEM分析证实钯在PVC-TETA-Pd中分布比较均匀,钯颗粒呈球形,粒径在2~3nm.PVC-TETA-Pd不需在惰性气体氛围中就能有效地催化丙烯酸、苯乙烯与芳基碘的Heck芳基化反应,并且在较低的温度(40℃)或较少的催化剂用量(0.02%)下,对Heck反应仍有较好的催化性能.PVC-TETA-Pd便于回收,且有很好的重复使用性能,对于碘苯与丙烯酸的反应,重复使用十二次,肉桂酸的产率仍达到80.1%. Polyvinyl chloride-triethylene-tetramine was synthesized from polyvinyl chloride via amination, then polyvinyl chloride-triethylene-tetramine supported palladium complex (PVC-TETA-Pd) was prepared and characterized by XPS, TG, DTA, TEM, etc. PVC-TETA-Pd has good thermal stability from room temperature to 250 V. ITEM confirms that Pd particles are spherical and have uniform distribution with the size of 2 similar to 3 nm. The complex is an efficient catalyst for Heck arylation of acrylic acid and styrene with iodoarenes under atmospheric condition, even at the low temperature (40 degrees C) or few amount of the catalyst (0.02 mol% Pd). PVC-TETA-Pd can be easily separated and used repeatedly. Yield of cinnamic acid was 80.1% for Heck reaction of acrylic acid with iodoarene even though the complex was used 12 times.
作者 张磊 崔元臣
出处 《化学学报》 SCIE CAS CSCD 北大核心 2005年第10期924-928,i003,共6页 Acta Chimica Sinica
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