苯基异氰酸酯与纤维素反应产物的定量研究
首发时间:2006-11-22
摘要:异氰酸酯基与纤维素和纤维素中的水分在一定条件下生成纤维素基氨基甲酸酯和取代脲的反应是采用异氰酸酯改性纤维素及其衍生物的研究基础,同时也是聚氨酯胶粘剂与木材胶接的基础反应之一。氨基甲酸酯和取代脲的生成量对改性效果和胶接强度的影响具有积极的理论意义和实践指导价值。 基于凯氏定氮法,本文首先提出并验证了一种可用于苯基异氰酸酯与纤维素反应产物的分离与分析方法;然后以苯基异氰酸酯为异氰酸酯模型物,研究了异氰酸酯与纤维素在不同反应条件下(即含水率、时间和温度),参与反应异氰酸酯总量、异氰酸酯与水反应生成取代脲量、以及异氰酸酯与生物质大分子反应生成氨基甲酸酯量的变化规律。 红外光谱证明论文所提出的实验方法是可行的,并获得了良好的分离效果;研究还表明:由于纤维素是一种高度结晶性高分子且不与异氰酸酯相溶,异氰酸酯只能在其接触表面与之发生反应,因此在纤维素含水率、反应时间和反应温度变化时,苯基异氰酸酯与纤维素体系中的羟基反应生成氨基甲酸酯的量较少且基本保持不变,消耗的异氰酸酯中有80.4-86.0%与纤维素体系中的水反应生成取代脲。苯基异氰酸酯与纤维素中的水和羟基反应的摩尔比在4.10-5.33之间。
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Quantitative study on the isocyanate-cellulose reacted resultants
Abstract:The reactions that isocyanate reacted to cellulose and water in cellulose to form the urethane (cellulose carbamates) and urea are basic knowledge for the adhesion of isocyanate-terminated polyurethane resins to wood, and for the modification of cellulose and cellulose derivatives with isocyanate. It has significant meaning to understand that different quantity of urethane and urea affect the strength of adhesive bond and modifying result. Based on the nitrogen content analysis by Kjeldahl, the paper proposed and confirmed a method, which was available to adequately separate and analyze of resultants of isocyanate reacted with cellulose. It regards phenyl isocyanates (BMI) as isocyanate model, and studies the variety rules of total isocyanates attending the reaction and the output of urea and urethane under different conditions (taking cellulose moisture content (MC)、reaction time、reaction temperature into account). FT-IR analysis conformed that the reactants of urethane and urea could be well separated by the method proposed in the study which allowed to be further quantitatively analyzed. The quantitative analysis indicated that phenyl isocyanate (PI) reacted with only a few hydroxyl groups (-OH) on the surface layer of cellulose powder to form urethane because of highly crystallization and poor solubility of cellulose, and the content of urethane formed under different conditions was almost constant, averaged 0.116mmol/g. It also revealed that most isocyanate groups consumed, 80.4-86.0%, reacted with water to form urea, and the mole ratios of PI reacted with water and with cellulose were ranged from 4.10 to 5.33.
Keywords: isocyanate cellulose urea urethane quantitative study
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No.9768706461164167****
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