端羟基聚环氧氯丙烷与叠氮聚醚的后处理研究

Post-Processing for Hydroxy Terminal Polyepoxy Chloropropane and Azido Polyethers

以端羟基聚环氧氯丙烷(CTP)、叠氮聚醚(ATP)和高分子量叠氮聚醚(HATP)等三种粗产品为后处理物对象,分别开展了减压蒸馏和溶剂萃取两种方法的后处理研究。结果表明,通过减压蒸馏除掉环状冠醚和低分子齐聚物难度较大,仅能蒸出少量环状三聚体;而溶剂萃取法则能得到较为理想的结果。本研究选取异丙醇、石油醚(60～90℃)和二者的混合溶剂等三种溶剂作为萃取溶剂。萃取结果表明:(1)三种萃取剂的萃取效果依次为:混合溶剂>异丙醇>石油醚。(2)异丙醇倾向于优先萃取小分子多元醇,石油醚倾向于优先萃取环状冠醚,而混合溶剂则能兼顾二者的优点。(3)对CTP、ATP和HATP来说,萃取后产品的数均分子量(Mn)与官能度(f)均有一定幅度的提升。具体到HATP,混合溶剂萃取可使Mn由2500～3200上升到3000～4000;f由1.99～2.00上升到2.46～2.97;低分子聚合物的含量由4.1%～8.2%下降到0.3%～2.3%。

The two post-processing methods distilled under negative pressure and extraction were studied with the rude products of hydroxy terminal polyepoxy chloropropane （CTP）,azido polyethers （ATP） and high-molecular-weight azido polyethers （HATP） as the post-processing thing. Results show that it is very difficuh to get rid of cyclic crown ether and low-molecule-weight oligomer by distillation under negative pressure. But extraction can get ideal post-processing result. Iso-propyl alcohol, petroleum ether （60 -90℃） and the mixed solvent （mixed by iso-propyl alcohol and petroleum ether） were chosen as extraction solvents. Extraction results indicate： （ 1 ） The extracting power of three extracting agents is in proper order： the mixed solvent 〉 iso-propyl alcohol 〉 petroleum ether; （2） Iso-propyl alcohol extracts low-molecule-weight polyols preferably, and petroleum ether extracts cyclic crown ether preferably,while the mixed solvent has two extraction results at the same time; （3） For the rude products of CTP,ATP and HATP, the number average molecular-weight （Mn） and functionality （f） can be increased after extraction by the mixed solvent. For HATP, MR can be increased from 2500 - 3200 to 3000 - 4000 ; f can be increased from 1.99 - 2. O0 to 2.46 - 2.97 ; the content of low-molecule-weight oligomer can be decreased from 4.1% -8.2% to 0.3% -2.3%.