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采用超声波在线测量溶液粘度的方法,研究了合成聚酰胺酸过程中实验条件的影响;对实验结果进行分析,由此确定了合成高分子量聚酰胺酸的最佳实验条件。研究表明:在加料次序为先加二胺后加二酐,二酐与二胺的摩尔比为(1.01～1.02)∶1,试剂中含水量尽可能少,反应温度在 0～5 ℃,反应时间以溶液粘度到达最大值为止的条件下,所合成的聚酰胺酸溶液粘度最大,可满足惯性约束聚变(ICF)充气腔靶端口膜的需要。
The influence of experimental conditions on the synthesis of polyamic acid was studied by measuring the viscosity of solution online with ultrasonic wave. The experimental results were analyzed, and the optimum experimental conditions for the synthesis of high molecular weight polyamic acid were determined. The results show that the molar ratio of dianhydride to diamine is (1.01 ~ 1.02): 1, the water content in the reagent is as little as possible, the reaction temperature is 0 ~ 5 ℃, Under the condition that the solution viscosity reaches the maximum, the synthesized polyamic acid solution has the highest viscosity and meets the needs of the target port membrane of inertial confinement fusion (ICF) inflation chamber.