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Study on Calcination Method for Preventing Removal of Structural Aluminum from β Zeolite
Kong Dejin,Xing Yu*,Chen Bo,Wang Hui,Li Chenglie
Author NameAffiliationE-mail
Kong Dejin Shanghai Research Institute ofPetrochemical Technology, Shanghai 201208  
Xing Yu* Shanghai Research Institute ofPetrochemical Technology, Shanghai 201208 engineeryuxing@yahoo.com  
Chen Bo Shanghai Research Institute ofPetrochemical Technology, Shanghai 201208  
Wang Hui Shanghai Research Institute ofPetrochemical Technology, Shanghai 201208  
Li Chenglie East China University of Science and Technology, Shanghai 200037  
Abstract:
The pyrogenic decomposition of template within zeolite Beta was greatly influenced by growth rate of calcination temperature. Inappropriate calcination methods would cause serious dealuminization from framework ofβzeolite and severe reduction in β zeolite’s crystallinity. Components of tail gas producing from calcination process were analyzed by chromatography. β zeolites calcined with different temperatures and as synthesized β zeolite were characterized by TG-DTG, FTIR, XRD, 29SiNMR and 27AlNMR. Hofmann degradation of organic amine took place chiefly at temperature range from 260℃to 420℃. Then the oxidation of organic amine reacted mainly at temperature higher than 492℃. A stage by stage calcining method was presented by using above research results. Firstly, calcination carried at low temperature stage within range from 110℃to 180℃ could eject water absorbed by β zeolite with air stream from the system, and hydrothermal dealuminization from framework of β zeolite that might occur at latter high temperature stage was able to be avoided. Secondly, one or two constant temperature stages placed at middle temperature range from 260℃ to 420℃ could make Hofmann degradation of organic amine react adequately, and moreover, combustible gas such as ethylene yielded from Hofmann degradation could be removed from the system and decomposition heat could be sent out stage by stage. Finally, a small quantity of residual was burned away at high temperature stage which is higher than 492℃. Temperature inside the pores of β zeolite wouldn’t heighten excessively to destroy framework of β zeolite because heat energy produced from residual combusting was limited. By this method, removal of structural aluminum from β zeolite could be restrained effectively, furthermore, amine free β zeolite was able to be produced with high crystallinity.
Key words:  Zeolite beta, Template removal, Calcination, Dealuminization
FundProject:
抑制β沸石骨架脱铝的焙烧研究
孔德金,邢宇*,陈波,王辉,李承烈
摘要:
研究了因焙烧过程升温速率对β沸石模板剂的热分解过程的影响,不同升温速率下Naβ沸石焙烧的尾气组成;还测定了Naβ沸石的TG-DTG谱,400℃下Naβ沸石的FIIR谱图,以及在不同温度下焙烧4 h后的XRD谱图及29Si、27Al的NMR结果.根据这些结果,提出了分段焙烧脱胺方法,使有机胺在260~420℃间的两个恒温段充分发生Hofmann降解反应,从而使分解产生的乙烯和水蒸气能够随空气流自然排出焙烧体系,可使焙烧过程中产生的热能得到分阶段逐步地释放,同时可避免高温下沸石骨架水热脱铝的负作用,得到骨架脱
关键词:  β沸石  模板剂脱除  焙烧  脱铝
DOI:10.1088/1674-0068/15/2/127-131
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