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甲苯和甲醇制二甲苯催化剂的失活与再生
中国石油化工股份有限公司上海石油化工研究院 绿色化工与工业催化国家重点实验室,上海 201208
Deactivation and Regeneration of Catalyst from Toluene and Methanol to Xylene
State Key Laboratory of Green Chemical Engineering and Industrial Catalysis, Shanghai Research Institute of Petrochemical Technology, SINOPEC, Shanghai 201208, China
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摘要 针对甲苯甲醇甲基化反应催化剂失活快的问题,对ZSM-5分子筛催化的甲基化反应的反应行为进行了分析,并结合X射线衍射(XRD)、N2吸附–脱附、傅里叶红外光谱(FT-IR)和吡啶吸附红外光谱(Py-IR)等方法对失活催化剂以及积炭物种进行了表征。结果表明,固定床甲基化反应中催化剂经历平稳期和快速失活期,二甲苯的选择性随着反应的进行持续上升,甲苯歧化反应持续受到抑制。积炭物种主要由羰基以及羟基化合物、烷基芳烃和复杂的稠环芳环等物质组成。积炭物种会堵塞分子筛孔道以及覆盖表面酸性位,孔道阻塞是造成催化剂快速失活的原因。在此基础上提出了一种操作简单的梯度氧化烧焦再生方式,能使催化剂的结构性质以及催化性能得到有效地恢复。
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李华英
董 骞
石张平
邹 薇
孔德金
关键词 甲基化ZSM-5催化剂甲苯甲醇二甲苯    
Abstract:In view of the rapid deactivation problem of catalyst for methylation of toluene with methanol, the methylation reaction was investigated in detail over ZSM-5 zeolite, and the deactivated catalyst and deposited carbon species were characterized by using X-ray diffraction (XRD), N2 adsorption-desorption, Fourier infrared spectroscopy (FT-IR) and pyridine absorption infrared spectroscopy (Py-IR). The results showed that the catalyst experienced a stable period and a rapid deactivation in the fixed-bed reactor, and the selectivity of xylene kept rising with toluene disproportionation reaction being inhibited. The deposited carbon species on the deactivated catalyst were mainly composed with carbonyl and hydroxyl compounds, alkylaromatic, polycyclic aromatic hydrocarbons. Carbon deposition could block the pore channels of ZSM-5 zeolite and cover its surface acid sites, and the blockage of the active site was the mainly reason for the catalyst deactivation. Furthermore, a simple regeneration method was proposed by a temperature programmed coke burning-off, and the structure and performance of the catalyst could be recovered efficiently.
Key wordsmethylation    ZSM-5 catalyst    toluene    methanol    xylene   
收稿日期: 2019-08-17     
作者简介: 李华英(1968—),女,高级工程师;孔德金(1965—),男,教授级高级工程师,通讯联系人。E-mail: kongdj.sshy@sinopec.com。
引用本文:   
李华英,董 骞,石张平等. 甲苯和甲醇制二甲苯催化剂的失活与再生[J]. 化学反应工程与工艺, 2019, 35(5): 402-409.
LI Huaying,DONG Qian,SHI Zhangping et al. Deactivation and Regeneration of Catalyst from Toluene and Methanol to Xylene[J]. 化学反应工程与工艺, 2019, 35(5): 402-409.
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