【作者】 高庆平；

【导师】 李占双；

【作者基本信息】 哈尔滨工程大学 ， 应用化学， 2006， 硕士

【摘要】 双酚芴(BHPF)，学名9，9-双(4-羟苯基)芴，是一种重要的有机化工原料，主要用于合成聚碳酸酯、环氧树脂、聚酯、聚醚或多醚等缩聚产品。 本论文选择双酚芴合成反应作为研究对象，分别使用杂多酸和阳离子交换树脂作为催化剂对合成双酚芴进行研究，并与传统质子酸浓硫酸催化合成双酚芴的实验进行对比，取得了较好的结果。论文针对目前研究中存在的问题，通过新方法与传统方法的比较，对双酚芴合成工艺进行了系统的研究。对反应时间、反应温度、酚酮摩尔比、催化剂用量、助催化剂用量等影响因素进行了考察。分别对硫酸法、杂多酸法和离子交换树脂法催化合成双酚芴工艺的最佳反应条件进行优化。 本文首先对传统方法——硫酸法合成双酚芴进行研究，确定了最佳反应条件。结果表明，当苯酚与芴酮的物质的量的比为6：1，催化剂浓硫酸用量为8.5mL，助催化剂β—巯基丙酸用量为0.25mL时，在45℃反应3h，双酚芴的收率可达98.1％，液相色谱显示其纯度为98.2％。 实验中采用两种新方法——杂多酸法和离子交换树脂法合成双酚芴，并考察了其反应条件。磷钨杂多酸催化合成双酚芴的最佳工艺条件是：苯酚与芴酮的物质的量的比为10：1，催化剂磷钨杂多酸用量为9％(占总物料质量百分数)，助催化剂β—巯基丙酸用量为0.15mL，在115℃反应11h，双酚芴的反应收率为65.1％，液相色谱显示纯度为99.3％。阳离子交换树脂催化合成双酚芴的最优工艺条件：苯酚与芴酮的物质的量的比为10：1，催化剂阳离子交换树脂D-072用量为10％(占总物料质量百分数)，助催化剂β—巯基丙酸用量0.2mL，在温度100℃反应10h，双酚芴的反应收率为82.3％，液相色谱显示其纯度为99.8％。 从实验结果可以看出，不同的合成工艺路线对双酚芴的纯度和收率有较更多还原

【Abstract】 9,9-bis(4-hydroxyphenyl)-fluorene, is one kind of important organic industrial chemicals, mainly used in synthesizing polycarbonates, epoxy resins, polyesters, polyethers, some gathers polycondensation product and so on.The present paper chooses the synthesis reactions of BHPF as the research object, uses the heteropoly acid and the cation resin as the catalyst to conduct the research, in addition, there was a contrast with the traditional synthesis by using sulfuric acid as catalysis , better result has obtained. In view of the question which exists at present studies, the paper conducts the system research to the BHPF synthesis craft, through the comparison between new method and traditional method. The influence factor, reaction time, reaction temperature, phenol-fluorenone molar ratio, catalyst amount used, promote catalyst amount used, has reviewed, respectively. The optimum response conditions are optimized through studying the sulfuric acid method, the heteropolyacid and the ion exchange resin to catalyze and synthesize BHPF.Firstly, the paper studies the traditional method sulfuric acid method to synthesize BHPF, and determined the optimum reaction conditions. The result indicated, when the molar ratio of phenol and fluorenone is 6:1, the amount used of strong sulfuric acid is 8.5mL, the amount used of promote catalyst P-mercaptopropionic acid is 0.25mL, reaction time is 3h, the BHPF yield reaches 98.1% on 45 ℃, and the liquid chromatography demonstrated its purity is 98.2%.In the experiment, two new methods, heteropolyacid and the ion exchange resin method, are used to synthesize BHPF, and their response condition are reviewed. The optimum reaction conditions of catalyzing and synthesizing BHPF by phosphorus tungsten heteropoly acid as follows: the molar ratio of phenol and fluorenone is 10:1, the catalyst phosphorus tungsten heteropoly acid amount used is 9% (occupies total material mass percent), the promote catalyst P-mercaptopropionic acid amount used is 0.15mL, reaction time is 11h, the BHPF更多还原