聚丙烯催化剂内给电子体9,9-双(乙酸甲酯基)芴的合成与表征

SYNTHESIS AND CHARACTERIZATION OF 9,9-BIS(METHYL ACETATE) FLUORINE,AN INTERNAL DONOR OF POLYPROPYLENE CATALYST

以自制的9,9-双羟甲基芴(BHMF)和乙酸酐为原料,以碘为催化剂,在无溶剂条件下合成了9,9-双(乙酸甲酯基)芴,考察了原料配比、反应时间、反应温度及催化剂用量等因素对9,9-双(乙酸甲酯基)芴收率的影响。采用红外光谱和核磁共振谱等分析测试手段对产品进行了结构表征并逐一归属。实验结果表明,合成9,9-双(乙酸甲酯基)芴的最佳工艺条件为n(BHMF):n(乙酸酐):n(碘催化剂)=1.0:6.0:0.016,反应温度25℃,反应时间5 h,在此条件下,9,9-双(乙酸甲酯基)芴收率可达78.6%,产品纯度为98.7%。

9,9-bis （methyl acetate） fluorene was synthesized from 9,9-bis （hydromethyl） fluorine （BHMF）and acetic anhydride under a solvent-free condition using 12 as catalyst. The structure of 9,9-bis （methyl acetate）fluorene was characterized by means of FT-IR and NMR. The effects of reaction conditions,such as reactants mole ratio, reaction time,reaction temperature and catalyst dosage,on the yield of 9,9-his（methyl acetate）fluorene were investigated. Test results showed that under the optimal reaction conditions of mole ratios of BHMF/acetic anhydride/I2 = 1. 0 ： 6. 0 ： 0. 016, a reaction temperature of 25 ℃ and a reaction time of 5 h,the yield and purity of 9,9-bis（methyl acetate）fluorene reached 78.6% and 98.7% ,respectively.