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作 者:许庆博 陈梦 时爽 徐思思 周宝晗 唐强 徐保明 XU Qing-bo;CHEN Meng;SHI Shuang;XU Si-si;ZHOU Bao-han;TANG Qiang;XU Bao-ming(Hubei University of Technology,School of Materials and Chemical Engineering,Wuhan 430068,Hubei,China)
机构地区:[1]湖北工业大学材料与化学工程学院
出 处:《精细化工》2018年第9期1567-1572,1581,共7页Fine Chemicals
基 金:国家自然科学基金(21272086);科技部中小企业创业基金(12C26214204453)~~
摘 要:以聚苯乙烯马来酸酐共聚物(SMA)及六水合硝酸钴为原料,制备了苯乙烯.马来酸酐钴盐(SMA-Co),利用FTIR、元素分析、UV-vis、SEM、EDS、XRD、TG对催化剂结构与性能进行了表征与测试。将N-羟基邻苯二甲酰亚胺(NHPI)与SMA-Co组成复合催化体系,考察了NHPI与SMA-CO物质的量比、催化剂用量、反应温度、氧气压力、反应时间对NHPI/SMA-Co催化氧气氧化环己烷反应的影响。结果表明:当环己烷为5mL、乙腈为10mL、n(NHPI):n(SMA-Co)=10:3、NHPI/SMA-Co用量0.04g、反应温度120℃,初始氧气压力为1.0MPa、反应6h时,环己烷转化率最大,为19.84%,环己醇选择性为22.23%,环己酮选择性为38.65%,环己酮和环己醇(KA油)总选择性达60.88%。催化剂经过4次回收利用后,催化剂活性无明显降低。Styrene-maleic anhydride copolymer cobalt salt (SMA-Co) was prepared using styrene-maleic anhydride copolymer (SMA) and cobalt nitrate hexahydrate as raw materials. The sample was characterized by FTIR, elemental analysis, UV-vis, SEM, EDS, XRD and TG. Subsequently, a composite catalytic system composed of N-hydroxyphthalmide (NHPI) and SMA-Co for the oxidation of cyclohexane was constructed. The effects of molar ratio of NHPI to SMA-Co, catalyst dosage, reaction temperature, oxygen pressure, reaction time on the oxidation of cyclohexane were investigated. The optimized reaction conditions were obtained as follows: 5 mL cyclohexane, 10 mL acetonitrile, n(NHFI) : n(SMA-Co)=10 : 3,NHPI/SMA-Co dosage 0.04 g, reaction temperature 120 ℃, initial oxygen pressure 1.0 MPa, reaction time 6 h. Under these conditions, the conversion of cyclohexane was 19.84%, and the selectivities of cyclohexanol and cyclohexanone were 22.23% and 38.65%, respectively. The selectivity of KA oil (the mixture of cyclohexanone and cyclohexanol) Was 60.88%. The catalytic activity of the catalyst was not obviously reduced after being recycled four times, indicating that the catalyst could be recycled,
关 键 词:SMA-Co NHPI 环己烷 催化氧化 催化技术
分 类 号:TQ314[化学工程—高聚物工业]
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