摘要
通过油氨柱成型法制备了球形铅-锰复合氧化物载体,并利用X射线衍射(XRD)、BET法比面积测试等技术对球状载体进行了表征。结果表明,在焙烧温度为450℃、活性炭添加量为2%(质量分数)条件下,制得的球状载体的性能最优。此时,载体的主要成分为氧化锰和四氧化三铅;同时,前驱体碳酸盐完全分解生成的二氧化碳气体,在逸出的过程中在载体内部形成了大量的孔道结构,使得载体的比表面积达到129.80 m^2/g;同时,载体的机械抗压强度达到17.8 N,使得反应后的载体仍具有完整的球状形貌。以氯化钯溶液为钯源,利用沉淀法将球形铅-锰复合氧化物载体负载0.5%(质量分数)钯后,用于苯酚氧化羰基化合成碳酸二苯酯的催化反应,碳酸二苯酯的收率可达14.34%,选择性在99.20%以上。
A series of spherical Pb-Mn composite oxide supporters have been prepared via oil-ammonia column method.The crystal structure, surface area, pore volume, and pore size distribution of spherical supporters were characterized by XRD and BET techniques.Results showed that the spherical supporters prepared at ealeination temperature of 450 ℃ and active carbon additive amount of 2% （mass fraction）, had the best properties.At this time the main components of the supporter were MnO and Pb304.Meanwhile, CO2 gas produced in the totally decomposition of precursor carbonate, made a lot of pore canal structures inside the supporters during the emitting process,and the specific surface area of the supporter reached 129.80 m^2/g. Meanwhile, the crushing strength of supporter reached 17.8 N, which grantee the supporter still had complete spherical morphology after reaction.Taking palladium chloride as the palladium source,0.5% （mass fraction） Pd was loaded on spherical supporters and used in the oxidative carbonylation of phenol to diphenyl carbonate （DPC）,the best DPC yield reached 14.34% and the selectivity was up to above 99.20%.
出处
《无机盐工业》
CAS
北大核心
2016年第9期74-78,共5页
Inorganic Chemicals Industry
基金
国家自然科学基金(51474160)
湖北省自然科学基金资助项目(2013CFB322)
武汉工程大学研究生教育创新基金项目(CX2014003)
关键词
油氨柱成型
球形载体
氧化羰基化
碳酸二苯酯
oil-ammonia column shaping
spherical supporters
oxidative carbonylation
diphenyl carbonate
