Abstract:

Sulfonic acid type waterborne polyurethane chain extender (N,N-bis(2-hydroxyethyl)-2-aminopropane sulphonate) was synthesized by sulfonation of self-made intermediate (N,N-bis(2-hydroxyethyl)-2-amine-propenyl) and adjusting temperature, time and molar ratio. Composition, structure and crystallinity of the synthesized product were characterized with nuclear magnetic resonance (¹H NMR), infrared spectroscopy (FTIR), elemental analysis, and XRD. Thermal stability of the product was characterized with TGA. The best synthesis process was determined by sulfonation degree of the product. When temperature of reaction was 90℃, time of reaction was 8 h, and materials ratio of N,N-(2-hydroxyethyl)-2-amino propylene, and NaHSO₃ was 1:2.5, the sulfonation degree of the product was above 94%. With DMPA and as-prepared sulfonic acid type monomer as hydrophilic chain extenders respectively, CWPU and SWPU were synthesized. Performance comparison showed that compared with CWPU, SWPU had good hydrophilicity and heat resistance, solid content and stability of SWPU were also better than those of CWPU.

Key words: N,N-bis(2-hydroxyethyl)-2-amine-propenyl, N,N-bis(2-hydroxyethyl)-2-aminopropane sulphonate, sulfonation, synthesis, characterization

摘要：

以自制的中间体N,N-二(2-羟乙基)-2-氨基丙烯为原料,对其进行磺化反应,控制温度、时间和摩尔比反应合成磺酸型水性聚氨酯扩链剂N,N-二(2-羟乙基)-2-氨基丙磺酸钠,借助核磁氢谱(¹H NMR)、红外光谱(FTIR)、元素分析、X射线衍射(XRD)等手段对合成产物进行了组成、结构和结晶性表征,用热重分析仪表征了产物的热稳定性。根据产物的磺化度确定最佳的合成工艺:反应温度为90℃,反应时间为8 h,N,N-二(2-羟乙基)-2-氨基丙烯和亚硫酸氢钠(NaHSO₃)的物料比为1:2.5,磺化率可达到94%以上。分别以二羟甲基丙酸(DMPA)和自制磺酸型单体作为亲水扩链剂制备羧酸型水性聚氨酯(CWPU)和磺酸型水性聚氨酯(SWPU),其性能对比结果表明:SWPU相比于CWPU具有较好的亲水性和耐热性能;固含量及稳定性方面,SWPU也是优于CWPU的。

关键词: N,N-二(2-羟乙基)-2-氨基丙烯, N,N-二(2-羟乙基)-2-氨基丙磺酸钠, 磺化, 合成, 表征