水性聚氨酯交联剂的合成、表征及其应用.pdf

石油化工
2011年第40卷第8期
PETROCHEMIICAL TECHNOLOGY
901
水性聚氨酯交联剂的合成、表征及其应用
刘藴慧,张庆思,李鹏,贺军,石翠磊
(山东轻工业学院化学工程学院,山东济南250353)
摘要]以二乙醇胺和5-氯-2ー成酮为原料、合成了5-[ニ(B-羟乙基)胺基」ー2-戊酮(BHAP);探讨了反应温度、反应时间
及溶剂、催化剂和缚酸剂种类等因素对BHAP收率的影响;采用FTIR,NMR,MS等方法表征了BHAP的结构并测定了BHAP的
相对分子质量及元素组成;同时将BHAP接枝到水性聚氨酯分子中,测试了交联收性聚氮酯胶膜的性能。实验结果表明,BHAP
的适宜合成条件为以N,Nー二甲基甲酰胺为溶剂、Na2CO3为缚酸剂、NaI为催化剂、反应温度73℃、反应时间30b。在此条件下,
BHAP收率达90.74%,产品纯度为89.66%。以BHAP为交联剂改性聚氨酯,当BHAP用量为7%(占改性聚氨階胶膜的质量分
数)时,与未交联的聚氨酯胶膜相比,交联改性聚氨酯胶膜的吸水率下降了64.70%,吸甲苯率下降了15.12%,拉伸强度提高了
1.81MPa,凝胶质量分数增加了4.43%。
关鍵词」5ー[二(B-羟乙基)胺基1-2ー成門;水性聚氮脂交联剂;と醇胺;5一氯-2-戊酮;交联聚氮酯胶膜
文章编号」1000-8144(2011)08-0901-06
中图分类号]TQ413.15
文献标识码」A
Synthesis, Characterization and Application of a erborne Polyurethane Crosslinker
Liu Yunhui, Zhang Qingsi, Li Peng, He Jun, Shi Cuilei
School of Chemical Engineering, Shandong Institute of Light Industry, Jinan Shandong 250353, China)
Abstract] A novel waterborne polyurethane(WPU)crosslinker, 5-bis(b-hydroxyethyl )amino-2
pentanone(BHAP), was synthesized from diethanolamine(DEA and 5-chloro-2-pentanone(CPE)
and characterized by mcans of FMR, NMR and MS. The effects of reaction temperature, reaction
timc, solvent, catalyst and acid binding agent on the yield of BHAP were investigated. The results
showed that under the optimal reaction conditions of dimethylformamide as the solvent. Na,CO, as the
acid binding agent, Nal as the catalyst, reaction temperature 73 C and reaction time 30 h, the yield
and the purity of BHAP were 90.74% and 89. 66%, respectively. After BHAP was linked to the main
chain of WPU, the properties of the WPU latex films were studied. Compared with the non-crosslinked
WPU, under BHAP dosage(mass fraction in the modified WPU latex film )7%, the water absorption
and the toluene absorption of the WPU latex films modified by BHAP decreased by 64.70% and
15. 12% respectively, and their ensile strength and gel mass fraction increased by 11.81 Mpa and
4.43 %o respectively
L Keywords J 5-bis (b-hydroxyethyl ) amino-2-pentanone; waterborne polyurethane crosslinker
diethanolamine: 5-chioro-2-pentanone: crosslinking polyurethane latex tilm
自乳化型水性聚氨附(WPU)由于合成条件的化学性能的目的“2。如陈广祥等?合成了聚氨
限制,聚合物相对分子质量较低,分子侧链存在较酯(PU)一丙烯酸酯复合型水分散体,通过双丙酮丙
多的亲水基团,致使其胶膜的力学性能及耐水性不烯酰胺引入酮羰基并与己二酸二酰肼发生酮肼交
好,这在一-定程度上限制了其应用范围シ。近年联反应,使胶膜的耐水性能和力学性能得到提高。
来,大量研究结果表明,交联改性是提高WPU性能
最直接、最有效的方法之一4-7
收稿日期』2011-01-28;[修改稿日期]2011-06-08。
将羰基引人WPU分子链段中,利用羰基
L作者简介]刘蕴慧(1983-),女,山东省青岛市人,硕士,电话
15866756257。联系人:张庆思,电话0531-89631618,电邮zqs(
的反应活性(如肼反应)制备成膜时再度发生交ic.cm
联反应的WPU,可以达到改善此类聚合物胶膜物理
基金项目山东省自然科学基金项目(2009ZRBO1128)。