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Synthesis and characterisation of 9,9-bis(4-hydroxyphenyl)-fluorene catalysed by cation exchanger

机译:阳离子交换剂催化的9,9-双(4-羟苯基)-芴的合成与表征

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摘要

Purpose - The purpose of this paper is to synthesise high-purity 9,9-bis(4-hydroxyphenyl)-fluorene (BHPF). Design/methodology/approach - 9,9-bis(4-hydroxyphenyl)-fluorene was prepared from phenol and fluorenone using cationic ion-exchange resin as the condensation catalyst. The purity and chemical structure of the resulting 9,9-bis(4-hydroxyphenyl)-fluorene were characterised by elemental analysis, MS, HPLC, FTIR, ~1H NMR and ~(13)C NMR spectroscopy, etc. Findings - The purity and weight yield of 9,9-bis(4-hydroxyphenyl)-fluorene reached up to 99.1 and 81.3 per cent, respectively, under the optimal reaction condition, that is, the molar ratio of phenol to fluorenone was 8-1, the reaction temperature was 100°C, reaction time was 10h, the mass percentage of cation exchanger accounting for the total reactants was 15 per cent and the co-catalyst quantity was 0.2 ml. Originality/value - The method for preparation was novel and could find numerous applications as monomer or modifier for heat-resistant adhesives, high-temperature coatings and matrix resin for advanced composites, etc.
机译:目的-本文的目的是合成高纯度的9,9-双(4-羟苯基)芴(BHPF)。设计/方法/方法-以阳离子交换树脂为缩合催化剂,由苯酚和芴酮制备9,9-双(4-羟苯基)-芴。通过元素分析,MS,HPLC,FTIR,〜1H NMR和〜(13)C NMR光谱等对所得9,9-双(4-羟苯基)-芴的纯度和化学结构进行表征。结果-纯度在最佳反应条件下,即苯酚与芴酮的摩尔比为8-1,9,9-双(4-羟基苯基)-芴的重产率分别达到99.1%和81.3%。温度为100℃,反应时间为10小时,阳离子交换剂占反应物总量的质量百分比为15%,助催化剂的量为0.2毫升。原创性/价值-制备方法新颖,可作为耐热胶粘剂的单体或改性剂,高温涂料和高级复合材料的基质树脂等获得广泛的应用。

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