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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
出 处:《石油化工》2016年第12期1441-1448,共8页Petrochemical Technology
基 金:江苏省重点研发计划(产业前瞻与共性关键技术)资助项目(BE2015204)
摘 要:采用共沉淀法,以逆滴的方式,制备了Cu-Zn-Al-Ba系列催化剂。通过ICP,TG,DTG,XRD,SEM等方法对催化剂进行表征;考察催化剂沉淀环境、各元素组分的配比、焙烧条件和还原条件等对活性的影响;并将催化剂用于硬脂酸甲酯催化加氢制硬脂醇的反应。实验结果表明,催化剂沉淀陈化过程中的优化条件为:催化剂组分n(Cu)∶n(Zn)∶n(Al)∶n(Ba)=8∶4∶4∶2,沉淀环境p H=8,陈化温度60℃,沉淀剂Na_2CO_3浓度0.80 mol/L,混合盐溶液浓度0.18 mol/L。表征和评价结果显示,焙烧和还原的优化条件为:焙烧温度400℃,焙烧时间3 h,还原温度270℃,还原时间1.5 h。评价结果表明,在反应温度为230℃、反应压力为氢压3 MPa、反应时间为4 h及优化条件下制备的催化剂用量5%(基于体系质量)的条件下,硬脂酸甲酯转化率超过96%,硬脂醇收率约为95%。Cu-Zn-Al-Ba catalysts were prepared through co-precipitation with inverse dropping and characterized by means of ICP, TG, DTG, XRD and SEM. The catalysts were used in the catalytic hydrogenation of methyl stearate to stearyl alcohol with n-hexane as the solvent. The effects of preparation conditions, namely ratio of raw materials, calcination conditions and reduction conditions, on the activities of the catalysts were studied. The results showed that the optimal conditions for the preparation were the ratio of elements n(Cu) : n(Zn) : n(Al) : n(Ba) 8 : 4 : 4 : 2, pH 8, aging temperature 60 ℃, Na2CO3 precipitant concentration 0.80 mol/L, mixed salt solution concentration 0.18 mol/L, calcination temperature 400 ℃, calcination time 3 h, reduction temperature 270 ℃ and reduction time 1.5 h. It was indicated that, under the hydrogenation reaction conditions of temperature 230 ℃, hydrogen pressure 3 MPa, reaction time 4 h and catalyst dosage 5%(w), the conversion of methyl stearate and the yield of stearic alcohol reached more than 96% and about 95%, respectively.
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