氟化钾/镍铝复合氧化物的制备及催化合成生物柴油  

Preparation of potassium fluoride/nickel aluminum composite oxide and catalytic synthesis of biodiesel

作　　者：李晓红[1] 

机构地区：[1]太原工业学院化学与化工系,山西太原030008

出　　处：《可再生能源》2015年第9期1415-1421,共7页Renewable Energy Resources

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)

摘　　要：采用共沉淀、煅烧及研磨的方法制备氟化钾/镍铝复合氧化物,并利用正交实验考察制备条件对氟化钾/镍铝复合氧化物催化合成生物柴油活性的影响,得到优化后的制备条件：镍/铝摩尔比为2、煅烧温度为550℃、煅烧时间为2 h、氟化钾/镍铝复合氧化物质量比为1。以优化条件下制得的氟化钾/镍铝复合氧化物为催化剂,催化蓖麻油与甲醇的酯交换反应,结果蓖麻油转化率为98.9%。采用TG-DTA,FTIR,BET,XRD技术对镍铝水滑石、镍铝复合氧化物及氟化钾/镍铝复合氧化物催化剂进行了表征,结果表明：镍铝水滑石在30~220℃,220~380℃及500~520℃3个温区有3个失重台阶;氟化钾/镍铝复合氧化物催化剂BET表面积为34.42 m2/g,BJH累积孔容为0.128 cm3/g,BJH平均孔半径为5.46 nm;氟化钾/镍铝复合氧化物催化剂由Ni O晶体和K3Al F6晶体构成。Nickel aluminum hydrotalcite was synthesized by coprecipitation and nickel aluminum composite oxide was manufactured by calcination and then potassium fluoride/nickel aluminum composite oxide catalyst was prepared by grinding potassium fluoride and nickel aluminum composite oxide together and drying it. Effects of preparation conditions on the catalytic activity of biodiesel synthesis catalyzed by potassium fluoride/nickel aluminum composite oxide were investigated through orthogonal tests.The optimal conditions obtained were nickel/aluminum molar ratio of 2, calcination temperature of 550 ℃, calcination time of 2 h, potassium fluoride/ nickel aluminum composite oxide mass ratio of 1. Using potassium fluoride/ nickel aluminum composite oxide prepared under the optimal conditions as a catalyst, under the conditions of alcohol/oil molar ratio of 9, catalyst/oil mass ratio of0.04, reaction temperature of 65 ℃ and reaction time 2 h, castor oil conversion was 98.9%. Nickel aluminum hydrotalcite, nickel aluminum composite oxide and potassium fluoride/nickel aluminum composite oxide catalyst were characterized by techniques of TG-DTA, FTIR, BET and XRD. The results showed that TG curve of nickel aluminum hydrotalcite had three weight loss steps, arising respectively in 30~220 ℃, 220~380 ℃ and 500~520 ℃, and that BET surface area of potassium fluoride/nickel aluminum composite oxide catalyst was 34.42 m2/g, BJH cumulative volume of pores 0.128 cm3/g,BJH average pore radius 5.46 nm, and that potassium fluoride/nickel aluminum composite oxide catalyst was made up of crystals Ni O and K3 Al F6.

关 键 词：氟化钾 镍铝复合氧化物 催化剂 生物柴油 

分 类 号：O614[理学—无机化学] TK6[理学—化学]