【作者】 崔丽丽；

【导师】 李巧玲；

【作者基本信息】 中北大学 ， 应用化学， 2008， 硕士

【摘要】 由于双(对-羧苯基)苯基氧化膦(BCPPO)分子结构中含有两个羧基和阻燃元素磷,因此可用作聚酯、聚酰胺、棉纤维等多种聚合物的反应型阻燃剂或阻燃单体以制得阻燃聚合物材料,它可同时赋予聚合物较好的阻燃性、抗静电性和染色性,较高的热稳定性和氧化稳定性以及较高的玻璃化转变温度等性能,具有广阔的应用前景。本论文通过优化BCPPO的各步合成工艺条件,缩短实验周期,减少贵重溶剂的用量,以降低成本,为其工业化生产提供依据,主要工作及创造性研究有以下几个方面:(1)苯基二氯化膦的合成(DCPP)合成中间体苯基二氯化膦,确定原料最佳的摩尔比及苯的投料方式,探索最佳的工艺条件。(2)双(对-甲苯基)苯基硫化膦(BMPPS)的合成优化BMPPS的合成工艺,确定各种原料的最佳配比并缩短反应时间,提高BMPPS的收率。(3)不同配比的水-吡啶混合液中BMPPS的溶解度的测定研究了同一配比的吡啶-水溶液中,BMPPS的溶解度与温度的关系;以及相同温度下,BMPPS的溶解度随着吡啶-水溶液中吡啶摩尔数的增加的变化趋势。(4)BCPPO的合成选择了合适的高锰酸钾的加料温度及反应氧化温度,在保证BCPPO较高收率的前提下,用廉价的水替代部分吡啶,降低昂贵溶剂吡啶的用量,得出最佳的吡啶和水的配比,缩短反应周期,降低生产成本。(5)产物的表征通过显微熔点测定仪,IR,UV,DSC,1H-NMR对制得的中间物BMPPS和目标物BCPPO进行结构表征及定量分析。更多还原

【Abstract】 Because two carboxyl group and flame retardant element phosphorus exist in the molecular structure, Bis(4-carboxyphenyl) phenyl phosphine oxide(BCPPO) was applied as the reactive-type flame retardant for plastics of many polymers such as polyester , polyamide , cotton fiber and so on, or as flame retardant monomer to obtain flame retardant polymer material. Polymers had the properties of flame retardance, antistatic electricity, dyeability, thermal stability, oxidation stability and high glass transition temperature because of BCPPO, so it had a broad application prospect.This topic provided the basis of industrialization, according to optimizing every process condition, decreasing the production cycle and the consumption of expensive solvent to reduce production costs. The work and the study were as follows:(1) The synthesis of phenylphosphorus dichloride (DCPP)DCPP was synthesized, the feeding style of C6H6 and the appropriate mol ratio of all kinds of raw materials was determined.(2) The synthesis of bis(4-methylphenyl)phenyl Phosphine Sulfid (BMPPS)Process conditions of BMPPS were optimized. The appropriate mol ratio of all kinds of raw materials was determined, the reaction time was shortened, and rate of production of BMPPS was improved at the same time.(3) The measurement of the solubility of BMPPS in water and pyridine solutionHow the solubility of BMPPS would change was studied when the temperature elevated in the same solution and when mole fraction of pyridine increased at the same temperature.(4) The synthesis of productThe appropriate feeding temperature and reaction temperature were chosen. Some pyridine was replaced by low-cost water to cut down the consumption of expensive pyridine, the reaction time was shortened and the mole ratio of pyridine and water was determined, when the yield of BCPPO was high. So production costs were cut down.(5) The characterization of productThe ultimate product and intermediate product were inspected and synthesized by micro-melting point inspector, IR, UV, DSC, 1H-NMR technology.更多还原