单分散间苯二酚-甲醛气凝胶微球的制备工艺

Preparation of Monodisperse Resorcinol-formaldehyde Aerogel Microspheres

采用T型微流体注射成型技术,以邻苯二甲酸二丁酯、液体石蜡和司班80为油相,间苯二酚/甲醛(RF)溶液为水相,经过溶胶-凝胶、溶剂交换、超临界干燥等过程制备了单分散RF气凝胶微球,并就制备过程中RF溶液与分散剂油相的选择、预聚时间、流速比、搅拌速率、固化温度等影响因素进行了初步讨论。当RF溶液质量分数为10%,60℃预聚1.5h,间苯二酚与碳酸钠的物质的量之比为100,邻苯二甲酸二丁酯与液体石蜡的质量比为8∶1,流速比控制在8～16,搅拌速率为65～90r/min,固化温度为35℃时,制备得到了RF乳液,其粒径分布系数小于2%。

Based on a novel T-shaped microfluidic device, monodisperse RF aerogel microspheres are prepared by using dibutyl phthalate,atoleine and spanS0 as oil phase, RF solution as water phase, and by sol-gel, solvent exchanging and supercritical drying. The factors such as the ehoice of RF solution and oil, prepolymerization time, the flow rate ratio of oil to water phase, stirring rate and solidification temperature, which affect the process have been preliminarily discussed. When the polymerization reaction oecur in the following conditions： RF solution is 10%, prepolymerization time is 1.5 hours at 60℃, the molar ratio of resorcinol to sodium carbonate is 100, the mass ratio of dibutyl phthalate to atoleine is 8, the flow rate ratio of oil to water phase is 8-16, stirring rate is 65-90r/rain and solidification temperature is 35℃, the experiment has fabricated monodisperse RF aerogel microspheres, whose coefficient of variation （CV value） of all the RF droplets is below 2%.