摘要
以二乙醇胺和5-氯-2-戊酮为原料,合成了5-[二(β-羟乙基)胺基]-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,测试了交联改性聚氨酯胶膜的性能。实验结果表明,BHAP的适宜合成条件为以N,N-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30h。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%(占改性聚氨酯胶膜的质量分数)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11.81MPa,凝胶质量分数增加了4.43%。
A novel waterborne polyurethane (WPU) crosslinker, 5-bis (fl-hydroxyethyl) amino-2- pentanone ( BHAP), was synthesized from diethanolamine (DEA) and 5-chloro-2-pentanone ( CPE), and characterized by means of PTIR, NMR and MS. The effects of reaction temperature, reaction time, 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, Na2CO3 as the acid binding agent, NaI as the catalyst, reaction temperature 73℃ 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 tensile strength and gel mass fraction increased by 11.81 MPa and 4.43% respectively.
出处
《石油化工》
CAS
CSCD
北大核心
2011年第8期901-906,共6页
Petrochemical Technology
基金
山东省自然科学基金项目(2009ZRB01128)