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

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以聚丙二醇二缩水甘油醚(PPGDGE)和CO_2为原料,在离子交换树脂催化剂D296的作用下,通过环加成反应合成了聚丙二醇二缩水甘油醚型环状碳酸酯(5CC-PPGDGE)。采用均匀设计法,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PPGDGE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为:催化剂用量12%(以PPGDGE质量计,下同),反应时间38 h,反应温度125℃,反应压力1.0 MPa,催化剂活化时间24 h,在该条件下PPGDGE的转化率几乎为100%,并对产物进行FTIR、~1HNMR、~(13)CNMR、GPC和TGA表征,证明得到目标产物。 Polypropylene glycol diglycidyl ether cyclic carbonate (5CC-PPGDGE) was synthesized by the cycloaddition of polypropylene glycol diglycidyl ether (PPGDGE) and CO 2 under the action of ion exchange resin catalyst D296. The uniform design method was used to investigate the effect of catalyst D296 dosage, reaction time, reaction temperature, reaction pressure and catalyst activation time on PPGDGE conversion. By using sequential uniform design experiments, the main factors influencing the conversion rate were determined, and the relationship between each influencing factor and the conversion rate was obtained according to the fitted regression model. The optimal reaction conditions were as follows: catalyst dosage 12% (PPGDGE The reaction temperature was 125 ℃, the reaction pressure was 1.0 MPa and the activation time of the catalyst was 24 h. Under these conditions, the conversion of PPGDGE was almost 100%. The products were characterized by FTIR, 1HNMR, ~ (13) CNMR, GPC and TGA characterization, to obtain the target product.
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