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WPU交联扩链剂5,6-二羟基-2-己酮的合成及表征
引用本文:贺军,张庆思,李鹏,刘蕴慧,石翠磊.WPU交联扩链剂5,6-二羟基-2-己酮的合成及表征[J].聚氨酯工业,2012(5):10-14.
作者姓名:贺军  张庆思  李鹏  刘蕴慧  石翠磊
作者单位:山东轻工业学院化学与制药工程学院,济南250353
基金项目:山东省自然科学基金(2009ZRB01128).
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(DH0),讨论了合成DHO的适宜条件及分离提纯的方法,并采用订-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8h,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。

关 键 词:5  6-二羟基-2-己酮  乙酰丙酮  环氧氯丙烷  WPU  交联扩链剂

Synthesis and Characterization of Waterborne Polyurethane Crosslinker-Chain Extender 5,6-Dihydrocy-2-Hexanone
He Jun Zhang Qingsi Li Peng Liu Yunhui Shi Cuilei.Synthesis and Characterization of Waterborne Polyurethane Crosslinker-Chain Extender 5,6-Dihydrocy-2-Hexanone[J].Polyurethane Industry,2012(5):10-14.
Authors:He Jun Zhang Qingsi Li Peng Liu Yunhui Shi Cuilei
Affiliation:He Jun Zhang Qingsi Li Peng Liu Yunhui Shi Cuilei (School of Chemistry and Pharmaceutical Engineering, Shandong Polytechnic University, Ji'nan 250353, China)
Abstract:A new crosslinker for waterborne polyurethane ( WPU ), 5,6-dihydroxy-2-hexanone ( DHO ) was syn- thesized by uueleophilie substitution and hydrolysis from acetylacetone (ACA) and epiehlorohydrin (ECH). The effects of reaction conditions on the yield of DHO and its separation, purification were investigated. DHO was char- actizated 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 opti- mal 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-ehain extender.
Keywords:5  6-dihydroxy-2-hexanone  acetylacetone  epichlorohydrin  WPU  crosslinker-chain extender
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