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南开大学高分子研究所 吸附分离功能高分子材料教育部重点实验室,天津,300071
纸质出版日期:2013-9-20,
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昝慧宁, 侯志爱, 张丽轩, 施荣富, 王春红. 固载胍基的强碱树脂合成与表征及其在Knoevenagel缩合反应中的催化作用[J]. 高分子学报, 2013,(9):1204-1211.
Hui-ning Zan, Zhi-ai Hou, Li-xuan Zhang, Rong-fu Shi, Chun-hong Wang. SYNTHESIS,CHARACTERIZATION OF STRONG BASE RESIN WITH GUANIDYL GROUPS AND THE APPLICATION AS CATALYST IN THE KNOEVENAGEL CONDENSATION[J]. Acta Polymerica Sinica, 2013,(9):1204-1211.
昝慧宁, 侯志爱, 张丽轩, 施荣富, 王春红. 固载胍基的强碱树脂合成与表征及其在Knoevenagel缩合反应中的催化作用[J]. 高分子学报, 2013,(9):1204-1211. DOI: 10.3724/SP.J.1105.2013.12433.
Hui-ning Zan, Zhi-ai Hou, Li-xuan Zhang, Rong-fu Shi, Chun-hong Wang. SYNTHESIS,CHARACTERIZATION OF STRONG BASE RESIN WITH GUANIDYL GROUPS AND THE APPLICATION AS CATALYST IN THE KNOEVENAGEL CONDENSATION[J]. Acta Polymerica Sinica, 2013,(9):1204-1211. DOI: 10.3724/SP.J.1105.2013.12433.
利用一步原位反应由大孔聚苯乙烯苄胺树脂和单氰胺合成含有胍基官能团的强碱阴离子交换树脂(PG)
通过傅立叶红外、酸碱滴定、元素分析、SEM对胍基树脂进行了表征
同时考察了体系中pH值、投料比、温度对原位反应的影响
实验结果表明
在pH值为2的溶液中
大孔树脂氨基交换量与单氰胺的摩尔比为1:3时
110 ℃反应5 h
树脂的强碱交换量达3.54 mmol/g.以胍基强碱树脂为非均相催化剂
催化Knoevenagel缩合反应
探讨了催化剂用量、反应溶剂、反应时间、树脂重复使用等因素对产率的影响
确定了反应的最佳条件.实验结果表明
该树脂具有良好的催化活性
在以乙醇为溶剂
反应时间为5 h
强碱树脂固载胍基含量与反应底物的摩尔比为1:5时
胍基强碱树脂催化Knoevenagel缩合的反应产率达到83.1%~95.3%
胍基强碱树脂可循环使用
在5次重复实验中
其催化活性基本保持.
The strongly basic polymer-supported catalyst containing guanidine functional group has been synthesized.In order not to increase the complexity or cost of the synthetic process
macroporous polystyrene amine resin has been allowed to react nucleophilic addition with cyanamide in situ to generate strong basic guanidine resin from weak basic amine resin designated as PG.PG resin is characterized by FTIR and SEM
and the contents of the strongly basic functional groups bound to the PG resin are determined by acid-base titration and elemental analysis.The effects of pH value
material ratio and reaction temperature on the in situ reaction are also studied.The experimental results show that when pH value of solution is 2
the molar ratio of amine functional groups on the macroporous to cyanamide is 1:3
and reaction temperature is 110 ℃
the strong base exchange capacity is 3.54 mmol/g.The Knoevenagel condensation has been selected to investigate the catalytic activity of the synthesized solid-supported guanidine catalyst.The Knoevenagel condensation is an effective carbon-carbon bond-forming reaction between a carbonyl compound and any compound having an active methylene group.The obtained PG resin has been found to be efficiently catalyze the Knoevenagel condensation reactions with remarkably high yields
and even the reactions of relatively inactive substrates such as ketones can be accomplished at higher temperatures.The effects of the amount of PG resin
reaction solvent and reaction time on the Knoevenagel condensation reactions between benzaldehyde and ethyl cyanoacetate(molar ratio 1:1) are investigated.Optimum reaction conditions are obtained as follows:in ethanol media
reaction time 5 h
n(guanidine functional groups immobilized on the anion exchange resin):n(substrate)=1:5
the yields of 83.1%~95.3% are gained.Lastly
the PG resin has been reused under identical reaction conditions remaining basically the efficiency in catalytic activity at the fifth cycle.
胍强碱阴离子交换树脂原位反应Knoevenagel缩合反应
GuanidineStrong base anion exchange resinIn situ reactionKnoevenagel condensation
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