【作者】 李春香；

【导师】 董占能；

【作者基本信息】 昆明理工大学 ， 应用化学， 2002， 硕士

【摘要】 双(对-羧苯基)苯基氧化膦(BCPPO)是一种适用于PET纤维阻燃改性的新型有机磷阻燃剂，本文主要研究了其合成工艺，整个合成路线分为三步，通过Friedel-Crafts烷基化反应制备了苯基二氯化膦(DCPP)，进而通过Friedel-Crafts酰基化反应合成了双(对-甲苯基)苯基氧化瞵(BMPPO)，经氧气、高锰酸钾氧化得到了产品BCPPO。 通过一一考察各种因素对产品收率的影响，改进和优化了工艺路线；产品经过元素分析、热分析、质谱分析、气相色谱、红外光谱、酸值等分析方法进行了表征；测定了中间体的物性参数，为实验及工业化设计提供了依据。 本论文合成方案与文献报道相比，有如下改进：第一，在DCPP产物分离过程中，采用细颗粒氯化钠作为络合剂，与文献中采用的吡啶和三氯氧磷相比，络合效果好，反应比较平缓，易于控制，减少了对环境的污染，降低了生产成本；第二，氧化剂用廉价的双氧水和氧气代替部分高锰酸钾，降低了生产成本；第三，在双氧水和氧气氧化过程中采用醋酸作为反应溶剂，与采用甲苯和吡啶相比，减少了环境污染，降低了生产成本。更多还原

【Abstract】 The main work of the article was to synthesize a suitable monomer, bis(4-carboxyphenyl)phenyl phosphine oxide (BCPPO), as the retardant for poly(ethylene terephthalate) (PET) fibre. The procedures were divided into three steps: dichloride phenyl phosphine oxide (DCPP) was synthesized and bis(4-methyl phenyl)phosphate oxide(BMPPO) was prepared from DCPP by Friedel-Crafts reaction. BCPPO was produced by two steps of oxidizing BMPPO with KMnO4 and O2.The procedures were improved and optimized by reviewing different factors effects. The product was identified by elements analysis, DSC analysis, MS analysis, GAS chromatogram, infrared chromatogram, acid number and so on. The physical constants of products were measured, which provided evidences for experiment and industrialization plan.Some improvements were made in this synthesis method. First, sodium chloride was adopted as the separation reagent in the process of DCPP synthesis, which had approving effect and the reaction is easy to control. The environment pollution was decreased and production cost was reduced. Second, the H2O2 and 67 were substituted for KMnO4 as oxidant in the oxidation process. Third, acetic acid was adopted as solvent, which made environment pollution reduced and production cost decreased, too.更多还原