废FCC触媒负载纳米氧化锌的制备及其松香催化酯化反应的研究
发布时间:2018-01-16 19:01
本文关键词:废FCC触媒负载纳米氧化锌的制备及其松香催化酯化反应的研究 出处:《高校化学工程学报》2016年06期 论文类型:期刊论文
【摘要】:以石油催化裂化(FCC)废触媒为载体,充分利用废触媒原有的分子筛结构与L酸中心,采用溶胶-凝胶法制备非均相的负载型纳米氧化锌酯化催化剂(ZnO/FC3R);通过SEM,XRD,FT-IR和Py-IR技术对Zn O/FC3R的表面形貌、粉体与基团结构和酸种类及酸强度进行了表征;以松香和甘油的酯化为指针反应,研究了负载量、醋酸锌水解反应温度、煅烧温度和负载时间等制备条件对催化剂酯化反应活性的影响;考察了催化剂的失活特性。结果表明,焙烧后制得的再生FCC催化剂(FC3R)载体为Y型分子筛结构,表面积炭得到一定程度的去除,ZnO晶粒呈锥状结构,颗粒的平均粒径为42 nm,添加ZnO固体酸可获得更多的L酸中心;ZnO/FC3R催化剂的适宜制备条件为:Zn O负载量为25%(wt),水解反应温度为35℃,煅烧温度为500℃,负载时间为1 h,所制备的催化剂用于松香酯化反应产率达96.1%,松香甘油酯产品的加纳色度为6、酸值为6.5 mg KOH×g~(-1)、软化点为85.3℃、残留锌含量为0.02%(wt),符合138#松香甘油酯国家技术指标;催化剂重复使用5次后仍具有良好的催化活性。
[Abstract]:The waste catalyst of FCC FCCs was used as the carrier to make full use of the original molecular sieve structure and L-acid center of the waste catalyst. ZnO / FC3RN catalyst was prepared by sol-gel method. The surface morphology, structure, acid species and acid strength of ZnO / FC3R were characterized by means of SEM-XRD- FT-IR and Py-IR. With the esterification of rosin and glycerol as the pointer reaction, the effects of the amount of loading, the hydrolysis temperature of zinc acetate, the calcination temperature and the loading time on the esterification activity of the catalyst were studied. The deactivation characteristics of the catalyst were investigated. The results showed that the regenerated FCC catalyst (FC3R) supported by calcination was Y-type molecular sieve structure, and the carbon deposition on the surface was removed to a certain extent. The average particle size of ZnO grain is 42 nm, and more L acid centers can be obtained by adding ZnO solid acid. The optimum conditions for preparation of ZnO/FC3R catalyst are as follows: the loading amount of Zn O is 25 鈩,
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