【作者】 汪建红；

【导师】 李巧玲；

【作者基本信息】 中北大学 ， 应用化学， 2006， 硕士

【摘要】 本文利用 Friedel—Crafts 反应合成了苯基二氯化膦(DCPP),并利用合成的 DCPP 制备了阻燃剂 2-羧乙基苯基次膦酸(CEPPA)。通过对中间体 DCPP 合成过程中催化剂用量、反应时间、络合剂种类、络合剂粒度、络合剂用量等影响条件的探讨及合成最终产物CEPPA 过程中原料添加顺序、丙烯酸用量、滴加温度、反应温度、反应时间、水解条件等影响因素的分析,找到了最为适宜的 CEPPA 的合成工艺条件。并利用红外光谱(FFIR)、差热扫描(DSC)、热重(TG)等分析手段对 CEPPA 的结构、熔点及热稳定性进行了分析,结果表明所制得的 CEPPA 具有较高的熔点和较高的热稳定性。为了尽早实现工业化,本课题还作了放大实验,制备了相当数量的产品 CEPPA,发现当搅拌情况良好,氯化钠添加速度合适时,效果更佳,CEPPA 的收率可达 78.4%。另外,还利用自制的阻燃剂 CEPPA 对尼龙-66 及棉纤维进行了阻燃改性处理,结果表明阻燃剂 CEPPA 阻燃性能优良,可使尼龙-66 的阻燃级别达到 V-0 级,使棉纤维的阻燃级别达到 B1 级。更多还原

【Abstract】 Dichlorophenylphosphine(DCPP) was synthesized byFriedel-Crafts method, and the 2-carboxyethyl (phenyl) phosphinicacid(CEPPA) was prepared with the synthesized DCPP. In the processof the preparation of the intermediate DCPP, the affecting conditions,such as the quantity of the catalyst, reacting time, the sort ofcomplexing agent, the granularity of complexing agent, the quantity ofthe complexing agent were explored, and in the process of thesynthesizing of the end product CEPPA, the affecting factors ,such asthe adding order of the reagent, the quantity of the acrylic acid, theadding temperature, the reacting temperature , the reacting time, thecondition of hydrolyzation, was analyzed, and the most suitabletechnological conditions of the CEPPA were got. The structure,melting point and thermal stability of the CEPPA were analyzed byFTIR, DSC, TG, and it indicated that the CEPPA has higher meltingpoint and higher thermal stability.In order to make its industrialization come true, the scale-upexperiments were done, and more product CEPPA was gotten. Itindicated that when the stirring was good and the adding rate wassuitable, the effect was better, and the yield of the CEPPA got to78.4%.Besides, the nylon-66 and the cotton fiber were modified withthe synthesized CEPPA. The results indicated that the flame-retardedproperty of the CEPPA was good, and could make the flame-retardedability of the nylon-66 on the level of V-0, the flame-retarded abilityof the cotton fiber on the level of B1.更多还原