【作者】 丁树成；

【导师】 王永莉；

【作者基本信息】 天津大学 ， 化学工程， 2005， 硕士

【摘要】 抗氧剂1010是一种高分子量的受阻酚类抗氧剂,广泛应用于塑料、橡胶、合成纤维、弹性体、石油制品以及饲料领域中。目前,国内生产的抗氧剂1010与国外产品相比,在粒度、堆密度及晶型等方面都存在一定差距。因此,本论文对抗氧剂1010结晶过程进行了系统的理论分析和实验研究。采用扫描电镜观察了抗氧剂1010的晶体外部形态,利用DSC分析了其熔点、熔化焓、半峰宽,利用X-粉末衍射确定了晶体的晶型,利用文献单晶数据,运用Cerius2软件分别采用BFDH模型和AE模型预测了抗氧剂1010的晶习,利用DSC分析讨论了溶剂和降温速率对晶体晶型的影响。采用静态法测定了抗氧剂1010在不同配比溶剂中的溶解度,采用激光法测定了抗氧剂1010在乙醇-异丙醇-水物系中的介稳区和诱导期,由诱导期数据计算得到固液界面张力。考察了降温速率、搅拌速率、晶种对介稳区的影响。采用差式扫描量热分析仪测定了抗氧剂1010的熔点和分解热,利用简易仪器测定了其堆密度,为结晶工艺优化及工业放大提供了基础数据和理论依据。采用间歇动态法测定了抗氧剂1010冷却结晶动力学,运用分级模型对实验数据进行处理,建立了生长粒度无关、聚结粒度无关的动力学模型,推导出了抗氧剂1010生长、聚结和成核动力学方程。以DSC分析半峰宽小于5℃和粒度分布均匀为目标,实验考察了加与不加晶种、晶种加入温度、晶种加入量、晶种粒度、降温速率、搅拌速率、洗涤、溶剂、干燥、结晶时间等结晶条件对产品各性能的影响,最终确定了抗氧剂1010的经验最优结晶工艺条件。本文所做的以上所有研究工作尚未见报导。更多还原

【Abstract】 As one kind of high molecular weight suffocate hydroxybenzene antioxidant, antioxidant 1010 is widely used in plastic, rubber, synthetic fiber, elastomer, petroleum products and fodder fields. Up to now, the domestic antioxidant 1010 is not as good as those overseas products in granularity, stack-density and crystal form. Therefore, a systematic academic and laboratorial research on the crystallization processes was done in detail. The crystal appearance has been observed with the help of scanning electron microscope. The DSC instrument was used to measure the melting point, melting enthalpy and half-peak width of antioxidant 1010. The crystal form was determined by X-ray Diffraction. With single crystal data of patents, crystal habit of antioxidant 1010 was forecasted in Cerius2 software by BFDH model and AE model. In using of DSC, the effect of solvent and cooling speed on crystal form has been discussed. The static method was used to measure the solubility of antioxidant 1010 at different solvent ratios. The laser method was used to measure the inducement period and metastable zone of antioxidant 1010 at ethanol-isopropanol-water. With the data of inducement period, solid-liquid phase interface tension has been calculated. Effect of cooling speed, stirring speed, seeds on metastable zone has been reviewed. With the help of DSC instrument, melting point and decomposing heat have been measured. The stack-density has been determined with simple instrument. All these works will provide base data and academic foundation to crystallization processes optimization and industrial magnification. The cooling crystallization kinetics was measured by batch dynamic methods. The kinetic data were treated with a discretized population balance model. A size-independent growth and size-independent agglomeration kinetic model was established. The growth equations, agglomeration equation and nucleation equation of antioxidant 1010 have been deduced. Aiming at half-peak width less than 5 degree centigrade and a uniform granularity distribution of antioxidant 1010 produces, the effect of seeds putted or not, temperature of seeds inputted, quantity of seeds inputted, seeds granularity, cooling speed, stirring speed, washing up, solvent, drying, crystallization time on products performance have been reviewed experimentally. In using of these reviewing data, the experiential optimum crystallization conditions have been determined ultimately. There aren’t any similar literatures to above study results have been reported up to date.更多还原