CaO/Co-Al-O固体碱的制备、表征及其油脂醇解活性  

Preparation,characterization and oil alcoholysis activity of CaO/Co-Al-O solid base

作　　者：靳福全[1] 

机构地区：[1]太原工业学院化学与化工系,太原030008

出　　处：《中国油脂》2015年第11期64-68,共5页China Oils and Fats

基　　金：山西省高校科技开发项目(2010130);山西省高等学校大学生创新创业训练项目(2011370);太原工业学院大学生创新企业训练项目(2013年)

摘　　要：采用共沉淀、浸渍及高温焙烧的方法制备了Ca O/Co-Al-O固体碱催化剂。采用正交实验考察了制备条件对Ca O/Co-Al-O固体碱油脂醇解活性的影响,得到固体碱催化剂的优化制备条件为：Co与Al摩尔比3∶1、顺加法、Ca（Ac）2浸渍液质量分数0.25、焙烧温度700℃、焙烧时间6 h。以优化条件下制备的Ca O/Co-Al-O固体碱为催化剂,在甲醇与蓖麻油摩尔比9∶1、催化剂与蓖麻油质量比0.04∶1、搅拌速率400 r/min、反应温度65℃、反应时间3 h的条件下,蓖麻油转化率为94.74%。采用TG-DTA、FT-IR、BET及XRD技术对固体碱催化剂及其前驱体进行了表征。结果显示：固体碱催化剂前驱体Ca（Ac）2/Co-Al水滑石TG曲线有3个失重台阶,分别出现在100~200℃、200~300℃及680~730℃;Ca O/Co-Al-O固体碱催化剂的BET比表面积为42.7 m2/g,BJH脱附累积孔容为0.29 cm3/g,BJH脱附平均孔半径为11.4 nm;Ca O/Co-Al-O固体碱中的活性组分Ca O以无定形或微晶的形式高度分散于Co Al2O4及Co3O4表面。CaO/Co - Al - O solid base catalyst was prepared using coprecipitation, impregnation and cal- cination methods. The effects of preparation conditions on the activity of CaO/Co - Al - O solid base in oil alcoholysis were investigated by orthogonal experiment. The optimal preparation conditions were ob- tained as follows ： molar ratio of Co to Al 3： 1, forward addition, mass fraction of Ca （Ac） 2 impregnation solution 0.25, calcination temperature 700 ℃ and calcination time 6 h. When reaction temperature was 65 ℃, reaction time was 3 h, molar ratio of methanol to castor oil was 9： 1, mass ratio of catalyst to castor oil was 0.04：1 and stirring speed was 400 r/min, the conversion rate of castor oil reached 94.74% in the presence of the CaO/Co - AI - O catalyst prepared under the optimal conditions. The catalyst and its precursor were characterized using techniques of TG - DTA, FT - IR, BET and XRD. The results indica- ted that Ca（Ac）2/Co- Al hydrotalcite had three weight loss steps in the TG curve, respectively appea- ring at 100 - 200 ℃, 200 - 300 ℃ and 680 - 730 ℃ ; BET surface area, BJH desorption accumulativepore volume and BJH desorption average pore radius of CaO/Co - Al - O solid base catalyst were 42.7 m^2/g, 0. 29 cm^3/g and 11.4 nm respectively; the active component CaO in the solid base was highly dispersed on the surface of CoAl2O4and Co3O4.

关 键 词：氧化钙 复合氧化物 固体碱 制备 催化剂 生物柴油 

分 类 号：TE667[石油与天然气工程—油气加工工程] O643.36[理学—物理化学]