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机构地区:[1]江南大学化学与材料工程学院,江苏无锡214122 [2]常州大学江苏省精细石油化工重点实验室,江苏常州213164
出 处:《精细化工》2011年第4期396-399,416,共5页Fine Chemicals
基 金:国家"十一五"重点科技支撑计划项目(2007BAE52B01);中央高校基本科研业务费专项资金(JUSRP20905);江苏省精细石油化工重点实验室开放基金(KF0903)~~
摘 要:开发了一条从天然脂肪酸合成α-羟基脂肪酸(α-HFA)的高产率、低污染且低成本的合成路线,即从天然脂肪酸制备α-氯代脂肪酸(α-CFA),再以α-CFA为原料通过水热法中性水解合成α-HFA。用GC-MS和IR鉴定了产物的结构,ESI-MS表征了产物的相对分子质量(以下简称分子量),纯化后α-HFA纯度达99%(GC)以上。探讨了水热中性水解反应中原料配比、反应加水量、反应温度、反应时间等因素对该水热工艺的影响,结果表明,当n(CaCO3)∶n(α-CFA)=1.05∶1,m(H2O)∶m(α-CFA)=2∶1,C12~C18的α-氯代天然脂肪酸在155℃水热条件下反应4 h后,α-HFA同系物的产率均高达98%~99%。α-Hydroxyl fatty acids(α-HFA) were hydrothermally synthesized through the neutral hydrolysis of α-chloro fatty acids(α-CFA) derived directly from natural fatty acids,which is a novel green route to synthesize α-HFA from natural fatty acids with the characteristics of a high yield,low-cost and environmental-friendly.In this paper,the structure of α-HFA was identified by FTIR and GC-MS and the relative molecular weight was confirmed by ESI-MS.The purity of purified α-HFA was examined by GC as high as 99%.Moreover,the influence of molar ratios of reactants,water dosages,reaction temperatures and reaction time on the hydrothermal synthesis has been investigated.The results indicate that the yield of α-hydroxyl natural fatty acid(C12~C18) can reach 98%~99% under the following conditions:n(CaCO3)∶n(α-CFA)=1.05∶1;m(H2O)∶m(α-CFA)=2∶1 at 155 ℃ for 4 hours.
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