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9-苯甲酸甲酯基芴的合成与表征
SYNTHESIS AND CHARACTERIZATION OF 9-METHYL BENZOATE FLUORENE
【摘要】 以9-羟甲基芴和苯甲酰氯为原料、以三乙胺为吸收剂合成了聚丙烯催化剂内给电子体9-苯甲酸甲酯基芴。采用红外光谱和核磁共振氢谱等分析测试手段对产品进行了结构表征。考察了原料配比、反应时间、反应温度及吸收剂用量等因素对9-苯甲酸甲酯基芴收率的影响。结果表明,合成9-苯甲酸甲酯基芴的最佳工艺条件为:9-羟甲基芴用量0.1mol,n(9-羟甲基芴):n(苯甲酰氯)=1.0:2.0,三乙胺吸收剂用量40mL,反应温度10℃,反应时间5.0h。在此条件下,9-苯甲酸甲酯基芴收率可达87.3%。
【Abstract】 9-methylbenzoate fluorene(as polypropylene catalyst internal donor) was synthesized from 9-hydromethylfluorene(A) and benzoyl chloride(B) with N(CH2CH3)3 as absorbent.The structure of 9-methylbenzoate fluorene was characterized by means of FT-IR and 1HNMR.The effects of reactants mole ratio,absorbent dosage,reaction temperature and reaction time on the yield of 9-methylbenzoate fluorene were investigated.Results showed that under the optimal reaction conditions of a A dosage of 0.1 mol,a A/B mole ratio of 0.5,a N(CH2CH3)3 dosage of 40 mL,a reaction temperature of 10℃and a reaction time of 5.0 h,the yield of 9-methylbenzoate fluorene reached 87.3%.
【Key words】 9-methylbenzoate fluorene; 9-hydromethylfluorene; N(CH2CH3)3; synthesis; structure characterization;
- 【文献出处】 石油炼制与化工 ,Petroleum Processing and Petrochemicals , 编辑部邮箱 ,2010年08期
- 【分类号】TQ245.2
- 【下载频次】83