异氰酸酯室温下与醇、水反应及较高温度下与纤维素反应的研究
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摘要
论文首先详细研究了室温下醇浓度、异氰酸酯基浓度、摩尔比、酸碱、溶剂等对异氰酸酯与醇的反应规律的影响。基于异氰酸酯与醇的反应规律以及不同浓度醇溶液的红外光谱特征，论文提出了异氰酸酯与醇反应的醇缔合作用机理，即异氰酸酯主要与n聚体缔合醇反应，反应后释放出(n—1)聚体缔合醇，反应实质上仍是二级反应。利用醇缔合作用机理能够合理解释反应速率、活化能、指前因子、活化熵等动力学参数随醇浓度增加而增加的规律，以及解释溶剂种类对异氰酸酯与醇反应的影响规律。醇浓度、酸碱、溶剂和温度对异氰酸酯与醇反应的速率常数有着显著的影响，异氰酸酯基浓度变化对之基本没有影响。碱氢氧化钠对异氰酸酯与醇的反应有着极显著的催化作用，其催化作用的本质是醇钠催化。
接着论文研究了室温下异氰酸酯与水的反应规律。通过理论推导和大量实验证明，室温下异氰酸酯与水的反应可以使用准二级方程描述，水和异氰酸酯基的分级数都是1。通过大范围内改变水浓度、异氰酸酯基浓度和摩尔比，异氰酸酯与水的反应都符合理论推导得的动力学速率方程。体系水浓度、溶剂种类、温度对反应速率常数有着明显的影响，酸碱和异氰酸酯基浓度变化对异氰酸酯与水的反应规律基本没有影响。在极限加速水浓度以前，增加体系的水浓度将使反应速率随之线性增加。在氢键化作用较强的溶剂中，加入基本没有氢键作用的烃类溶剂，或氢键作用较小的溶剂，会使异氰酸酯与水的反应速率增加。
接下来对异氰酸酯与醇和水竞争反应的研究表明，为了提高异氰酸酯与醇反应的比例，可以通过提高体系醇浓度或降低体系水浓度实现。由于异氰酸酯与水的反应速率比较快，若要使反应中绝大多数异氰酸酯与醇反应，要求体系醇的浓度要明显地高于水的浓度；当体系水的浓度是醇的2倍以上时，将有90％以上的异氰酸酯基与水反应。
最后论文利用DSC、FTIR和ESCA等研究了异氰酸酯与不同含水率纤维素的反应规律。发现：异氰酸酯主要分布于纤维素表层；异氰酸酯与含水纤维素反应时，异氰酸酯主要与水反应，而且随着纤维含水率增加，与水反应异氰酸酯的量就越多，当含水率达到9.78％时，绝大部分异氰酸酯与水反应。异氰酸酯与不同含水率纤维素反应机理很复杂，存在多种机理同时存在；当与绝干纤维素反应时主要是相界面机理。
The thesis firstly studies the reaction rules of isocyanate with alcohol in room temperature in which some factors are discussed such as the concentration of alcohol and isocyanate, the mole ratio, acid, alkali, solvent, temperature. Based on the reaction rules and the IR spectroscopy of alcohol solution, the paper puts forward a new mechanism, Alcohol Polymer Reacting Mechanism(APRM), to explain the reaction kinetics of isocyanate with alcohol. That is, the isocyanate mainly react with n polymeric alcohol, then release n-1 polymeric alcohol. The reaction is still second order. With APRM, the phenomena can be well understood that the kinetic parameters, such as the rate constant, activating energy, pre-exponential factor, activating entropy, are increasing when alcohol concentration increases. The APRM will explain the effects of solvents on the reaction. The alcohol concentration, acid, alkali, solvents and temperature have obvious effects on the rate constant. The alkali, sodium hydroxide, has a good catal
ysis on the reaction, however the essence of catalysis is alcohol sodium.
Secondly, the reaction rules of iscocyanate with water are undertaking in room temperature. The theoretical deduction and many experiments discovered that reaction of isocyanate with water is second order in room temperature, and the water and isocyanate are first order to the rate respectively. Water concentration, solvents and temperature greatly affect the rate constant, while the acid, alkali and isocyanate concentration has no effects. Before the critical accelerating water concentration, rate constant increases linearly with water content. The rate will accelerate when part of strong hydrogen-bonding solvent replaced with hydrocarbon solvent or weak hydrogen-bonding solvent.
The following study on the competing reaction of isocyanate with alcohol and water indicates that high alcohol concentration or thin water content will improve the reaction of isocyanate with alcohol. If one wants that isocyanate reacted extremely with alcohol, the alcohol content should be greatly more than water for isocyanate reacts with water is quite fast. However, if watev concentration is 2 times as alcohol, more than 90% of consumed isocyanate reacted with water.
Finally, the thesis studies the reaction rules of isocyanate with cellulose
containing different water content by DSC, FTIR and ESCA. It shows that isocyanate distributes mainly on the cellulose surface. When cellulose contain some water, most isocyanate react with water, and the more water the cellulose contains, the more isocyanate consumed by water. When the moisture content of cellulose is up to 9.78%, about 92.98% isocyanate are consumed by water. The phase interface mechanism controls the reaction of isocyanate with dry cellulose, when water exists, the mechanism is very complicated, and some mechanisms coexist.
接着论文研究了室温下异氰酸酯与水的反应规律。通过理论推导和大量实验证明，室温下异氰酸酯与水的反应可以使用准二级方程描述，水和异氰酸酯基的分级数都是1。通过大范围内改变水浓度、异氰酸酯基浓度和摩尔比，异氰酸酯与水的反应都符合理论推导得的动力学速率方程。体系水浓度、溶剂种类、温度对反应速率常数有着明显的影响，酸碱和异氰酸酯基浓度变化对异氰酸酯与水的反应规律基本没有影响。在极限加速水浓度以前，增加体系的水浓度将使反应速率随之线性增加。在氢键化作用较强的溶剂中，加入基本没有氢键作用的烃类溶剂，或氢键作用较小的溶剂，会使异氰酸酯与水的反应速率增加。
接下来对异氰酸酯与醇和水竞争反应的研究表明，为了提高异氰酸酯与醇反应的比例，可以通过提高体系醇浓度或降低体系水浓度实现。由于异氰酸酯与水的反应速率比较快，若要使反应中绝大多数异氰酸酯与醇反应，要求体系醇的浓度要明显地高于水的浓度；当体系水的浓度是醇的2倍以上时，将有90％以上的异氰酸酯基与水反应。
最后论文利用DSC、FTIR和ESCA等研究了异氰酸酯与不同含水率纤维素的反应规律。发现：异氰酸酯主要分布于纤维素表层；异氰酸酯与含水纤维素反应时，异氰酸酯主要与水反应，而且随着纤维含水率增加，与水反应异氰酸酯的量就越多，当含水率达到9.78％时，绝大部分异氰酸酯与水反应。异氰酸酯与不同含水率纤维素反应机理很复杂，存在多种机理同时存在；当与绝干纤维素反应时主要是相界面机理。
The thesis firstly studies the reaction rules of isocyanate with alcohol in room temperature in which some factors are discussed such as the concentration of alcohol and isocyanate, the mole ratio, acid, alkali, solvent, temperature. Based on the reaction rules and the IR spectroscopy of alcohol solution, the paper puts forward a new mechanism, Alcohol Polymer Reacting Mechanism(APRM), to explain the reaction kinetics of isocyanate with alcohol. That is, the isocyanate mainly react with n polymeric alcohol, then release n-1 polymeric alcohol. The reaction is still second order. With APRM, the phenomena can be well understood that the kinetic parameters, such as the rate constant, activating energy, pre-exponential factor, activating entropy, are increasing when alcohol concentration increases. The APRM will explain the effects of solvents on the reaction. The alcohol concentration, acid, alkali, solvents and temperature have obvious effects on the rate constant. The alkali, sodium hydroxide, has a good catal
ysis on the reaction, however the essence of catalysis is alcohol sodium.
Secondly, the reaction rules of iscocyanate with water are undertaking in room temperature. The theoretical deduction and many experiments discovered that reaction of isocyanate with water is second order in room temperature, and the water and isocyanate are first order to the rate respectively. Water concentration, solvents and temperature greatly affect the rate constant, while the acid, alkali and isocyanate concentration has no effects. Before the critical accelerating water concentration, rate constant increases linearly with water content. The rate will accelerate when part of strong hydrogen-bonding solvent replaced with hydrocarbon solvent or weak hydrogen-bonding solvent.
The following study on the competing reaction of isocyanate with alcohol and water indicates that high alcohol concentration or thin water content will improve the reaction of isocyanate with alcohol. If one wants that isocyanate reacted extremely with alcohol, the alcohol content should be greatly more than water for isocyanate reacts with water is quite fast. However, if watev concentration is 2 times as alcohol, more than 90% of consumed isocyanate reacted with water.
Finally, the thesis studies the reaction rules of isocyanate with cellulose
containing different water content by DSC, FTIR and ESCA. It shows that isocyanate distributes mainly on the cellulose surface. When cellulose contain some water, most isocyanate react with water, and the more water the cellulose contains, the more isocyanate consumed by water. When the moisture content of cellulose is up to 9.78%, about 92.98% isocyanate are consumed by water. The phase interface mechanism controls the reaction of isocyanate with dry cellulose, when water exists, the mechanism is very complicated, and some mechanisms coexist.
引文
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