【作者】 姚强；

【导师】 朱明乔；

【作者基本信息】 浙江大学 ， 化学工程， 2015， 硕士

【摘要】 N,N’-双(4-氨基-2,2,6,6-四甲基哌啶基)-1,3-苯二甲酰胺(简称NN-BTP-BDCA)是一种受阻尼龙稳定剂。受阻胺光稳定剂(HALS)是20世纪70年代末研制开发出的新型高效光稳定剂,表现出优异的光稳定性,因此受到广泛的关注,是近几十年来国内外研究最活跃的光稳定剂之一本论文分为四章。主要研究了HALS典型产品(NN-BTP-BDCA)的合成反应工艺,通过探究了不同合成工艺来确定最佳合成路线,为之后的放大设计奠定了基础。论文的具体内容如下：第一章为文献综述,主要概括了近二十年HALS的发展过程以及未来的发展趋势,其中重点介绍了HALS的作用机理和未来发展趋势。第二章总结了实验原料、实验设备的使用,以及表征手段和合成工艺的确定,具体为：分别研究了羧酸与胺的缩合酰化工艺、酯交换转换为酰胺工艺和酰氯与胺的酰化工艺等三种工艺,以及将反应转移到高压釜中研究在加压的条件下对反应结果的影响。实验结果表明：采用间苯二甲酰氯与哌啶胺在0～5℃下,以二氯甲烷为溶剂,三乙胺为有机碱,滴定1h,然后升温至20℃再反应2h,得到产物,采用元素分析以及红外光谱分析等方法对所得产物进行确定,产物的收率达到95%以上。第三章对小试结果进行了设计放大并作出了可行性研究,内容主要包括工艺技术方案的选择、物料平衡、水平衡以及工程消耗。第四章对本文的主要研究内容进行了归纳总结,对未来HALS的合成工艺提出了一些建议。更多还原

【Abstract】 N,N’-bis(4-amino-2,2,6,6-tetramethyl-piperidyl)-1,3-benzenedicarboxamide (abbreviated NN-BTP-BDCA) is a hindered nylon stabilizer. Hindered amine light stabilizers (HALS) are a new class of light stabilizers developed at the end of 1970s, which have been one of the most intensively studied classes of stabilizers during the last several decades due to their high photo-stabilization efficiency.This thesis was divided into four chapters. It mainly includes the synthesis reaction process of HALS typical products (NN-BTP-BDCA) to determine the best route of synthesis by exploring different synthesis techniques, laid the foundation for subsequent amplification design. Specific contents are as follows:The first chapter is the literature review which summarized of HALS development and future trends in nearly two decades. This chapter focuses on the mechanism of HALS and future trends.The second chapter summarized the experimental materials, the use of laboratory equipments, as well as characterization method and experimental methods. It is mainly about:condensation acylated process of a carboxylic acid with an amine, the transesterification process which is converted to an amide and acylation process of acid chloride with an amine and so on. The reaction is transferred to an autoclave to study the effect of pressure on the results. The results indicate that:the yield of product was 95% under the reaction condition of reaction temperature 0～5 ℃, using isophthaloyl chloride with piperidine amine, methylene chloride as solvent and triethylamine as the organic base titration, reaction time 1 h, then warmed to 20℃ reacted for 2 h giving the product. The product is determined by elemental analysis and IR spectroscopy and other methods.The third chapter designed amplication according to the small scale experiments and made a feasibility study which includes selecting technology solutions, material balance, water balance and engineering consumption.The fourth chapter summarized the main contents of this paper, and put forward some suggestions for the synthsis process of HALS in future.更多还原