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机构地区:[1]青岛科技大学化学与分子工程学院,山东青岛266042
出 处:《中国油脂》2017年第5期78-81,95,共5页China Oils and Fats
基 金:国家863重大项目(2012AA000100);国家自然科学基金(21406252);中科院青年创新促进会基金(2012170)
摘 要:采用一步水热法合成磷钨酸改性多孔配位聚合物(PCP(Cr)-PTA)催化剂,并对催化剂进行FTIR、XRD、N_2吸附脱附、透射电镜、扫描电镜和热重表征。将催化剂用于水相中合成棕榈酸甲酯,探讨了催化剂用量、反应温度、反应时间和醇水体积比对棕榈酸甲酯产率的影响。结果表明:磷钨酸成功负载并分散在多孔配位聚合物孔道之中,Keggin结构保持不变,且热稳定性良好。在醇水体积比1∶9,反应温度130℃,反应时间3 h,催化剂PCP(Cr)-PTA用量为反应物质量的5%的酯化反应条件下,棕榈酸甲酯产率达到84.7%。催化剂连续经过5个反应周期仍保持良好的催化活性。Catalyst of novel porous coordination polymers (PCPs) modified with phosphotungstic acid (PTA) were prepared by hydrothermal method via one-pot self-assembly.The catalyst was characterized by FTIR,XRD,N2 adsorption and desorption,TEM,SEM and TG.The catalyst was used in the synthesis of methyl palmitate in water.And the effects of catalyst dosage,reaction temperature,reaction time and volume ratio of methanol to water on the yield of methyl palmitate were discussed.The results showed that PTA dispersed finely in the sieves,and the structure of PTA was not destroyed,thermal stability was also great.Under the conditions of volume ratio of methanol to water 1∶ 9,reaction temperature 130 ℃,reaction time 3 h and catalyst dosage 5% (based on the mass of reactants),the yield of methyl palmitate was 84.7%,and the catalyst still exhibited good catalytic activity after five runs of reaction.
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