【作者】 范海平；

【导师】 方云进；

【作者基本信息】 华东理工大学 ， 化学工程， 2012， 硕士

【摘要】 本文较全面的综述了双酚A型聚碳酸酯的主要合成工艺,通过对比筛选,确定了以非光气熔融酯交换法合成聚碳酸酯预聚体的工艺路线。通过烧瓶中的小试实验,对预聚反应的催化剂进行了考察,确定了以氢氧化四丁基铵为催化剂时得到的产品综合性能最佳,然后分别考察了主要影响因素如催化剂用量、物料配比、抗氧剂、调色剂的加入量、碳酸二苯酯和双酚A纯度,以及猝灭剂的加入量对预聚产品性能的影响。在此基础上,在不锈钢反应釜中进行了条件探索,如电机转速,猝灭剂用量等。最后还对预聚反应体系进行了动力学的研究,实验结果符合假定动力学模型,对后续实验有一定的指导作用。较佳的预聚工艺条件为：催化剂选用氢氧化四丁基铵,用量5×10-5mol/molBPA,DPC结晶后使用,使用K7抗氧剂,用量0.6%,猝灭剂采用有机酸,用量5ppm,催化剂在150℃时加入,前期酯交换反应30min,最终温度230℃,并保持10min,制备的PC预聚体分子量达到缩聚要求,色泽和透光率达国内领先水平。更多还原

【Abstract】 This paper comprehensive reviews the methods for synthesis of bisphenol-A polycarbonate(PC). The non-phosgene synthesis route of melt transesterification method is determined for polycarbonate prepolymer process by comparing the other methods. Syhthesis of prepolymer of polycarbonate by melt transesterification with diphenyl carbonate and bisphenol-A is studied in a flask. Through the small scale experiments in the flask, the pre-polymerization catalyst was investigated to determine the tetrabutylammonium hydroxide as a catalyst to get the best overall performance of the product. Then the main factors were investigated such as the amount of catalyst, the material ratio, the kind of antioxidant, the amount of toner, purity of diphenyl carbonate and bisphenol A, and the amount of quencher on the prepolymer product performance. On this basis, the pre-polymerization conditions such as motor speed, quenching agent dosage were investigated in the stainless steel reactor. Finally, the kinetic was studied for the pre-polymerization system, and the experimental results shows a good agreement with the assumed kinetic model. The results have some guidance for the follow-up experiment. The optimal conditions of the reaction are as follows: catalyst tetrabutyl ammonium hydroxide, the amount of 5×10-5 mol/molBPA, DPC used after crystallization, using K7 as antioxidants, the amount of 0.6%; using organic acid as quencher, the amount of 5ppm; the catalyst was added at 150℃, preliminary transesterification reaction 30 min, the final temperature of 230℃, and keeping 10 min. The molecular weight of PC prepolymer preapred meets the requirements of polycondensation, the color and light transmission rate of PC prepolymer reaches world-class level.更多还原