【摘要】 以乙酰丙酮(ACA)、环氧氯丙烷(ECH)为原料,通过氯代烃的亲核取代及环氧的水解开环反应合成了5,6-二羟基-2-己酮(DHO),讨论了合成DHO的适宜条件及分离提纯的方法,并采用FT-IR、NMR、HRMS等方法对DHO进行了表征。结果表明,ACA与ECH的最佳反应温度为60℃,中间产物5,6-环氧-2-己酮(EHO)收率达37.1%;EHO水解开环反应最佳反应温度为90℃,反应时间为8 h,DHO收率可达69.5%,且中间产物5-(乙酰氧基)-6-羟基-2-己酮经碱水解也可以得到DHO;分离与提纯采用制备液相色谱法可得到DHO产物,纯度达95.96%,并得到FT-IR、NMR、HRMS方法的证实,该产物可作为水性聚氨酯交联扩链剂。更多还原

【Abstract】 A new crosslinker for waterborne polyurethane(WPU),5,6-dihydroxy-2-hexanone(DHO) was synthesized by nucleophilic substitution and hydrolysis from acetylacetone(ACA) and epichlorohydrin(ECH).The effects of reaction conditions on the yield of DHO and its separation,purification were investigated.DHO was charactizated by FT-IR,NMR,HRMS.The results showed that,under the optimal reaction conditions of ethanol as the solvent,reaction temperature 60 ℃,the yield of intermediate A(5,6-epoxy-2-hexanone) was 37.1%.The optimal temperature of hydrolysis reaction was 90 ℃ and reaction time was 8 h,the DHO yield was 69.5%.DHO could also be synthesized by hydrolytic reaction of the intermediate B(5-(acetyloxy)-6-hydroxy-2-hexanone).FT-IR showed that the product DHO separated by preparative HPLC systems and the purity was 95.96%.DHO was characterized by means of FTIR,NMR and HRMS.The product was used as WPU crosslinker-chain extender.更多还原