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作 者:刘振民[1,2] 王军威[2] 亢茂青[2] 殷宁[2] 王心葵[2] 谭猗生[3] 朱玉雷[3]
机构地区:[1]中国科学院研究生院化学与化学工程学院,北京100049 [2]中国科学院山西煤炭化学研究所应用催化与绿色化工实验室,山西太原030001 [3]中国科学院山西煤炭化学研究所煤转化国家重点实验室,山西太原030001
出 处:《精细化工》2012年第10期1026-1031,共6页Fine Chemicals
基 金:国家重点基础研究发展计划(973计划)(2012CB215305)~~
摘 要:采用等体积浸渍法制备了一系列氧化铝负载碱金属氟化物固体碱催化剂,用于甘油(丙三醇)与碳酸二甲酯酯交换反应合成碳酸甘油酯,其中KF/γ-Al2O3催化剂能够更好地促进碳酸甘油酯的生成。进一步考察了KF/γ-Al2O3催化剂的制备条件、反应条件对甘油与碳酸二甲酯酯交换反应的影响。当KF负载在γ-Al2O3的负载量为15%(质量分数,下同),于400℃焙烧5 h后制得固体碱催化剂,在n(碳酸二甲酯)∶n(甘油)=3∶1,反应温度80℃,反应时间1.5 h的条件下,甘油的转化率达96.1%,碳酸甘油酯选择性和收率分别达98.1%和94.3%。A series of alumina supported alkali metal fluoride solid base catalysts were prepared by impregnation method and were subsequently applied to the synthesis of glycerol carbonate(GC) via transesterification of glycerol with dimethyl carbonate(DMC).Among these catalysts,KF/γ-Al2O3 could promote the transformation of glycerol into GC more efficiently than other catalysts.The effects of the preparation conditions of KF/γ-Al2O3 and the reaction conditions on transesterification of glycerol with DMC were investigated.The results prove that the loading amount of KF over KF/γ-Al2O3,calcination temperature and time of catalyst and reaction conditions had significant impacts on the conversion of glycerol and the selectivity of GC.With the molar ratio of DMC to glycerol being 3∶ 1,the reaction being conducted at 80 ℃ for 1.5 h,KF/γ-Al2O3 as catalyst,15% KF loading amount and the calcination being conducted at 400 ℃ for 5 h,the conversion of glycerol,the selectivity and yield of GC attained 96.1%,98.1% and 94.3%,respectively.
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