有机胺催化制备聚碳酸酯二元醇

The Preparation Technology of Polycarbonate Diols Catalyzed by Amines

以碳酸二甲酯(DMC)和1,4-丁二醇(BDO)为原料,在三乙胺等有机胺类催化剂催化下,酯交换制备出聚碳酸酯二元醇(PCDL)。采用核磁共振和红外光谱等分析手段鉴定产物的结构;凝胶渗透色谱分析减压时间对PCDL分子量分布的影响。详细研究了原料摩尔比(DMC/BDO)、催化剂用量、减压时间等因素对反应过程的影响,优化了PCDL的合成工艺参数。实验结果表明,当DMC/BDO的摩尔比为1.2～1.25,催化剂用量占BDO的质量分数为0.5%,采用阶段控温方式制备出数均分子量在1600g/mol左右的PCDL。

Polycarbonate diols（PCDL） was synthesized by carbonate interchange reaction of dimethyl carbonate with 1,4-butanediol in the catalysis of amines. The structure of PCDL was determined by Fourier transform infrared spectroscopic（FT-IR） and hydrogen nuclear magnetic resonance spectrum（1H-NMR）,it is confirmed that the chemical structures of product are consistent with that of pure polycarbonate diols. The process parameters affecting the characters of product,such as molar ratio of DMC/1,4-BDO,the dosage of catalyst,vacuum reaction time,were studied extensively. The experimental results show that desired polycarbonate diols with excellent technical specifications is prepared by means of stage temperature under the conditions of molar ratio for n（DMC）∶n（1,4-BDO）=1.2～1.25,temperature of under 190 ℃ and amines accounting for 0.5 mass percent of 1,4-BDO.