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Influence of the amount of catalyst and initial pH on the phenolic resol resin formation

机译:催化剂用量和初始pH值对酚醛酚醛树脂形成的影响

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The influence of the added amount of triethylamine as phenolic resol resin catalyst and that of the initial pH were studied for resols synthesized at 80deg C with F/P1.8. The evolution of phenol and first formed addition products were quantitatively followed by highperformance liquid chromatography (HPLC) and final prepolymers were analyzed by ~(13)C NMR spectroscopy. The catalyst amount kinetically and mechanistically affected the prepolymer formation.The higher the amount of added catalyst the higher reactant consumption rates and product formation rates. The ortho directing characteristics of triethylamine for the addition of formaldehyde onto phenoli sites were observed. It could be stated that two mechanisms for the addition of formaldehyde occurred simultaneously. On the one hand, hydroxyl groups favoured the formation of phenolate ions, which would favour addition onto para phenolic positions.On the other hand, formaldehyde, phenol, and triethylamine could be involved in the formation of an intermediate transition state, favouring addition onto ortho sites, due to the ortho directing properties of triethylamine. The influence of the studied pH range did not give rise to significant differences on the resol resin prepolymer formation.
机译:研究了三乙胺作为酚醛可熔酚醛树脂催化剂的添加量和初始pH值对80°C F / P1.8合成的甲阶酚醛树脂的影响。通过高效液相色谱(HPLC)定量分析苯酚和第一个形成的加成产物的演变,并通过〜(13)C NMR光谱分析最终的预聚物。催化剂的量在动力学和机械上影响预聚物的形成。催化剂的加入量越高,反应物的消耗速率和产物形成速率越高。观察到三乙胺的向苯酚位置加甲醛的邻位定向特性。可以说,添加甲醛的两种机理同时发生。一方面,羟基有利于酚盐离子的形成,有利于加成到对酚位置;另一方面,甲醛,苯酚和三乙胺可能参与中间过渡态的形成,有利于加成到邻位位置,由于三乙胺的邻位定向性质。研究的pH范围的影响对可熔酚醛树脂预聚物的形成没有明显的影响。

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