无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2016, Vol. 48 ›› Issue (9): 74-.

• 论文 • 上一篇    下一篇

球形铅-锰复合氧化物载体制备及性能评价

殷超凡,杨小俊,吴元欣,陈启明   

  1. 武汉工程大学化工与制药学院,绿色化工过程教育部重点实验室,湖北武汉 430074
  • 出版日期:2016-09-10 发布日期:2016-09-18

Preparation and properties of spherical Pb-Mn composite oxide supporters

 YIN  Chao-Fan, YANG  Xiao-Jun, WU  Yuan-Xin, CHEN  Qi-Ming   

  1. Key Laboratory for Green Chemical Process of Ministry of Education,School of Chemical Engineering and
    Pharmacy,Wuhan Institute of Technology,Wuhan 430074,China
  • Online:2016-09-10 Published:2016-09-18

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 m2/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。

关键词: 油氨柱成型, 球形载体, 氧化羰基化, 碳酸二苯酯

Abstract: 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 calcination 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 Pb3O4.Meanwhile,CO2 gas produced in the totally decomposition of precursor carbonate,made a lot of pore canal struc- tures inside the supporters during the emitting process,and the specific surface area of the supporter reached 129.80 m2/g. Meanwhile,the crushing strength of supporter reached 17.8 N,which grantee the supporter still had complete spherical mor- phology 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%.

Key words: oil-ammonia column shaping, spherical supporters, oxidative carbonylation, diphenyl carbonate

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