摘要
以氯苯、金属钠和硼酸三异丙酯为原料,以甲苯为溶剂合成三苯基硼,考察了反应温度、物料配比、反应时间和加料方式对三苯基硼合成过程及其收率的影响。研究结果表明,以甲苯为溶剂,反应可在常压下进行,降低了对设备和操作的要求;采用逐滴加料的方式,可降低反应体系中氯苯和硼酸三异丙酯的浓度,减少副产物联苯和偏硼酸钠的生成。当温度较高时,钠砂的聚并速率较快,导致钠砂的比表面积下降,使产物收率降低;但温度过低又会降低主反应的选择性,导致产物收率下降。适宜的工艺条件为:反应温度65℃,反应时间4 h,n(钠)∶n(氯苯)∶n(硼酸三异丙酯)=7.00∶3.50∶1.00。在该条件下,产物三苯基硼的收率为85.04%。
Triphenylboron was prepared from chlorobenzene, sodium sand and triisopropyl borate（TIPB） with toluene as the solvent. The effects of reaction temperature, feeding ratio, reaction time and feeding modes on the triphenylboron yield were investigated. Using toluene as the solvent led to that the reaction could be conducted under atmospheric pressure, which would reduce the requirements of equipment and operation. The by-products biphenyl and sodium metaborate can be decreased by dropwise feeding which can lower the concentration of chlorobenzene and TIPB in the reaction system. The sodium sand easily coalesces at high temperature, which can lead to reducing its specific surface area so lowering the yield. On the other hand, too low temperature will reduce the selectivity of the main reaction. The yield of triphenylboron could reach 85.04% under the optimal reaction conditions of 65℃, n（sodium） ： n（chlorobenzene） ： n（TIPB）7.00 ： 3.50 ： 1.00 and reaction time 4 h.
出处
《石油化工》
CAS
CSCD
北大核心
2013年第4期415-418,共4页
Petrochemical Technology
关键词
三苯基硼
钠砂
氯苯
硼酸三异丙酯
甲苯
triphenylboron
sodium sand
chlorobenzene
triisopropyl borate
toluene
