均匀设计在聚丙二醇二缩水甘油醚型环状碳酸酯合成中的应用

Application of Uniform Design Method on Synthesis Investigation of Poly(propylene oxide) bis-carbonate

摘要:

采用均匀设计法，对影响聚丙二醇二缩水甘油醚型环状碳酸酯（5CC-PPGDGE）合成的主要因素进行了考察。以聚丙二醇二缩水甘油醚（PPGDGE）和CO2为原料，在离子交换树脂D296 的作用下，通过环加成反应合成了5CC-PPGDGE。考察了催化剂D296用量、反应时间、反应温度、反应压力以及催化剂的活化时间对产物转化率的影响。采用序贯均匀设计实验，确定了对转化率影响的主要因素，并且根据实验结果拟合回归模型得到各影响因素与转化率之间的关系，得到了最优反应条件：催化剂用量=12%，反应时间=38h，反应温度=125℃，反应压力=1MPa，催化剂活化时间=24h。在最优反应条件下的产物转化率几乎为100 %， 并对产物进行FTIR、1HNMR、13CNMR、GPC和TGA分析表征，证明得到目标产物。

Abstract:

The main factors which had significant effects on the synthesis of carbonated polypropylene glycol diglycidyl ether (5CC-PPGDGE) were investigated by using uniform design. The 5CC-PPGDGE was synthesized from polypropylene glycol diglycidyl ether (PPGDGE) and CO2 by using quaternary ammonium salt modified amberlyst D296 as catalyst. Effect of D296 catalyst content, reaction time, reaction temperature, reaction pressure and catalyst activation time on conversion efficiency of PPGDGE were investigated. By two uniform design experiments, the main factors for PPGDGE conversion were determined: catalyst content = 12 %, reaction time = 38 h, reaction temperature = 125 ℃, reaction pressure= 1 MPa and catalyst activation time = 24 h, and the optimum conditions were obtained based on the relationship between experimental factors and conversion which was acquired through regression. The conversion of product from the optimum condition was almost 100 % and product was confirmed by FTIR, 1HNMR, 13CNMR, GPC and TGA analysis.