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Synthesis of mordenite by solvent-free method and its application in the dimethyl ether carbonylation reaction

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Chinese Journal of Chemical Engineering 2024年第2期66卷 216-223页

作者： Yinghui Liu Shaoduo Liu Xiaosheng Wang Hongjing Wang Ranjia Li Changchun Yu Chunming Xu Yuxiang Liu Zhengqiu Xie Yongqiang Wang Pan Tang State Key Laboratory of Heavy Oil Processing College of New Energy and MaterialsChina University of Petroleum-BeijingBeijing 102249China Synfuels China Technology Co. LtdBeijing 101400China College of Chemical Engineering Qingdao University of Science&TechnologyQingdao 266042China Yueyang Jucheng Chemical Co. LtdYueyang 414009China

Mordenite with different Si/Al ratios were synthesized by solvent-free method and used for dimethyl ether(DME)carbonylation *** influence of Si/Al ratio in the feedstock on the structure,porosity and acid sites were systematically *** characterization results showed that with the increase of Si/Al ratio in the feedstock,part of silicon species fail to enter the skeleton and the specific surface area and pore volume of the samples *** amount of weak acid and medium strong acid decreased alongside with the increasing Si/Al ratio,and the amount of strong acid slightly *** Al atoms preferentially enter the strong acid sites in the 8 member ring(MR)channel during the crystallization *** high Si/Al ratio sample had more acid sites located in the 8 MR channel,leading to more active sites for carbonylation reaction and higher catalytic *** increasing the Si/Al ratio was beneficial for the improvement of carbonylation reaction activity over the mordenite(MOR)catalyst.

关键词： Carbonylation dimethyl ether Solvent-free Zeolite Synthesis Catalysis

Shaped binderless ZSM-11 zeolite catalyst prepared via a dry-gel conversion method:Characterization and application for alkylation of benzene with dimethyl ether

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Journal of Energy Chemistry 2017年第3期26卷 380-389页

作者： Wanshuo Zhang Shuang Zhang Wenjie Xin Hui Liu Yongchen Shang Xiangxue Zhu Shenglin Liu Longya Xu College of Chemistry and Chemical Engineering Harbin Normal University State Key Laboratory of Catalysis Dalian Institute of Chemical PhysicsChinese Academy of Sciences Research and Development Center Sinochem Quanzhou Petrochemical Co.Ltd.

Shaped binderless ZSM-11 zeolite catalysts were synthesized via a dry-gel conversion technique from 70ZSM-11/30 SiO;mix extrudates. 1,6-hexanediamine combined with tetrabutylammonium bromide was proved to be the best structure directing agent for the synthesis of the binderless ZSM-11 catalyst, without adding other alkaline materials. The 70HZSM-11/30 SiO;mix serials materials crystallized for different times were detected by X-ray diffraction（XRD）, nuclear magnetic resonance（NMR）, scanning electron microscopy（SEM）, transmission electron microscopy（TEM）, scanning transmission electron microscopy–energy dispersive spectroscopy（STEM–EDS） techniques, and so on. In order to investigate the possible crystallization mechanism, the textural and structural properties of 70HZSM-11/30 SiO;mix serials samples were further characterized by N;adsorption–desorption. Acid properties were determined by temperature-programed desorption of NH;（NH;-TPD） and pyridine adsorption-infrared（Py-IR） measurements. In the alkylation of benzene with dimethyl ether, the serials catalysts exhibited different benzene conversions. 70HZSM-11/30 SiO;mix showed the lowest benzene conversion while sample 70HZSM-11/30 SiO;mix-6.5h synthesized only for 6.5h displayed a higher benzene conversion, even higher than the value over 70HZSM-11/30Al;O;mix. Extending the crystallization time, the obtained samples displayed the increased benzene conversion in general under the same reaction conditions. In the end, the relation of physicochemical properties with the reaction performance was investigated.

关键词： Shaped binderless ZSM-11 Crystallization mechanism Mechanical strength Acidity Alkylation dimethyl ether

Optimization of hydrothermal synthesis of H-ZSM-5 zeolite for dehydration of methanol to dimethyl ether using full factorial design

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Journal of Natural Gas Chemistry 2012年第3期21卷 344-351页

作者： Samaneh Hosseini Majid Taghizadeh Ali Eliassi Chemical Engineering Department Babol University of TechnologyP.O.Box 484*** BabolIran Chemical Technologies Research Department Iranian Research Organization for Science and TechnologyTehranIran

H-ZSM-5 zeolite was synthesized by hydrothermal method. The effects of different synthesis parameters, such as hydrothermal crystallization temperature （170-190 ℃） and Si/A1 molar ratio （100-150）, on the catalytic performance of the dehydration of methanol to dimethyl ether （DME） over the synthesized H-ZSM-5 zeolite were studied. The catalysts were characterized by N2 adsorption-desorption, XRD, NH3-TPD, TGA/DTA, and SEM techniques. The full factorial design of experiments was applied to the synthesis of H-ZSM-5 zeolite and the effects of synthesis conditions and their interaction on the yield of DME as the response variable were determined. Analysis of variance showed that two variables and their interaction significantly affected the response. According to the experimental results, the optimized catalyst prepared at 170℃ with the Si/A1 molar ratio of 100 showed the best catalytic performance among the tested H-ZSM-5 zeolite.

关键词： full factorial design H-ZSM-5 synthesis methanol dehydration dimethyl ether

Synthesis of ethylidene diacetate from dimethyl ether,CO and H_2

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Journal of Natural Gas Chemistry 2010年第2期19卷 165-168页

作者： Dianhua Liu Xin Huang Lei Hu Dingye Fang Weiyong Ying Dasheng Chen Engineering Research Center of Large Scale Reactor Engineering and Technology Ministry of Education State Key Laboratory of Chemical Engineering East China University of Science and Technology Shanghai 200237 China Shanghai Wujing Chemical Co. Ltd. Shanghai 200241 China

Ethylidene diacetate was prepared by reacting dimethyl ether,acetic acid and syngas in the presence of a catalytic system comprising RhI3,PPh3 and *** effects of reaction temperature,pressure,time and the CO/H2 molar ratio on the conversion of dimethyl ether and the product selectivity were investigated under the same catalyst *** showed that a maximum conversion of dimethyl ether was obtained when a mixture consisting of 0.3 mol dimethyl ether and 120 ml acetic acid was reacted at 180 ℃ and 3.0 MPa for 10 h at a stirring speed of 600 rpm under a syngas flow with a CO/H2 molar ratio of 2.5,which was catalyzed by a catalyst mixture comprising 0.3 g RhI3,6 g PPh3 and 1.3 g *** selectivity of ethylidene diacetate increased with temperature,decreased with the CO/H2 molar ratio and exhibited a maximum with pressure.

关键词： dimethyl ether carbonylation ethylidene diacetate reaction condition

Effect of Calcination Temperature on Catalytic Activity and Textual Property of Cu/HMOR Catalysts in dimethyl ether Carbonylation Reaction

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Chinese Journal of Chemical Physics 2013年第2期26卷 220-224,I0004页

作者：张雪李宇萍仇松柏王铁军马隆龙张琦定明月中国科学院广州能源研究所可再生能源与天然气水合物重点实验室广州510640 中国科学院大学北京100049

The effect of calcination temperature on the catalytic activity for the dimethyl ether （DME） carbonylation into methyl acetate （MA） was investigated over mordenite supported copper （Cu/HMOR） prepared by ion-exchange process. The results showed that the catalytic activity was obviously affected by the calcination temperature. The maximal DME conversion of 97.2% and the MA selectivity of 97.9% were obtained over the Cu/HMOR calcined at 430 ℃ under conditions of 210 ℃, 1.5 MPa, and GSHV of 4883 h^-1. The obtained Cu/HMOR catalysts were characterized by powder X-ray diffraction, N2 absorption, NH3 temperature program desorption, CO temperature program desorption, and Raman techniques. Proper calcination temperature was effective to promote copper ions migration and diffusion, and led the support HMOR to possess more acid activity sites, which exhibited the complete decomposing of copper nitrate, large surface area and optimum micropore structure, more amount of CO adsorption site and proper amount of weak acid centers.

关键词： dimethyl ether Methyl acetate Calcination temperature Carbonylation HMOR

Importance of metal location in M-H zeolite for synergistically catalyzing dimethyl ether carbonylation

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Chinese Journal of Chemical Engineering 2022年第1期35卷 350-357页

作者： Shiyue Li Shouying Huang Kai Cai Ying Li Jing Lv Xinbin Ma Key Laboratory for Green Chemical Technology of Ministry of Education Collaborative Innovation Center of Chemical Science and EngineeringSchool of Chemical Engineering and TechnologyTianjin UniversityTianjin 300350China

Mordenite(MOR)has shown great potential to catalyze dimethyl ether(DME)carbonylation to methyl acetate(MA)in *** synergy between metal species and Brønsted acid sites accelerates DME *** we designed and prepared two catalysts with different Ag locations by seed-directed growth method and two-step impregnation method(named as Ag@HMOR and Ag/HMOR-out,respectively),to explain the effect of Ag location on catalytic *** results of TEM,XPS,CO-IR and UV–Vis showed that Ag species mainly presented as Ag^(0) species over both Ag@HMOR and Ag/***,Ag^(0) species mainly located in the micropores of Ag@HMOR,while as for Ag/HMOR-out,Ag^(0) mainly existed on external *** comparing the performance of the catalysts with different Ag positions,we confirmed that the Ag^(0) species encapsulated in the channels of HMOR promoted the DME carbonylation,which revealed the importance of spatial adjacency on the acid-metal catalysts.

关键词： dimethyl ether Carbonylation Silver modification Metal location

Production of Light Olefins from Biosyngas by Two-stage Catalytic Conversion Process via dimethyl ether

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Chinese Journal of Chemical Physics 2014年第2期27卷 227-232,I0004页

作者：李宇萍涂军令王铁军马隆龙张兴华章青蔡炽柳中国科学院广州能源研究所可再生能源重点实验室广州110640 中国科学院大学北京100049

NiSAPO-34 and NiSAPO-34/HZSM-5 were prepared and evaluated for the performance of dimethyl ether （DME） conversion to light olefins （DTO）. The processes of two-stage light olefin production, DME synthesis and the following DTO, were also investigated using biosyngas as feed gas over Cu/Zn/A1/HZSM-5 and the optimized 2%NiSAPO-34/HZSM- 5. The results indicated that adding 2%Ni to SAPO-34 did not change its topology structure, but resulted in the forming of the moderately strong acidity with decreasing acid amounts, which slightly enhanced DME conversion activity and C2=-C3= selectiw ity. Mechanically mixing 2%NiSAPO-34 with HZSM-5 at the weight ratio of 3.0 further prolonged DME conversion activity to be more than 3 h, which was due to the stable acid sites from HZSM-5. The highest selectivity to light olefins of 90.8% was achieved at 2 h time on stream. The application of the optimized 2%NiSAPO-34/HZSM-5 in the second-stage reactor for DTO reaction showed that the catalytic activity was steady for more than 5 h and light olefin yield was as high as 84.6 g/m3syngas when the biosyngas （H2/CO/CO2/N2/CH4=41.5/26.9/14.2/14.6/2.89, vol%） with low H/C ratio of 1.0 was used as feed gas.

关键词： Light olefins Two-stage conversion dimethyl ether Biosyngas NiSAPO-34/HZSM-5

Enhanced catalytic performance for direct synthesis of dimethyl ether from syngas over a La_2O_3 modified Cu-ZrO_2/γ-Al_2O_3 hybrid catalyst

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Journal of Natural Gas Chemistry 2012年第3期21卷 360-365页

作者： Zhuo Li Jianqing Li Cheng Yang Jinhu Wu Key Laboratory of Biofuels Qingdao Institute of Bioenergy and Bioprocess Technology Chinese Academy of Sciences Qingdao 266101 Shandong China Graduate School of Chinese Academy of Sciences Beijing 100039 China

A series of hybrid catalysts were made by physically mixing Cu-ZrO2 and γ-A12O3, for former it was modified with different loadings of La2O3 prepared by co-precipitation method. The catalysts were characterized by BET, XRD, N2O-adsorption, EXAFS, H2-TPR, NH3-TPD techniques and evaluated in the synthesis of dimethyl ether from syngas. The results show that La2O3 promoted catalysts displayed a significantly better catalytic performance compared with Cu-ZrO2#y-A12O3 catalyst in CO conversion and DME selectivity, and the optimum catalytic activity was obtained when the content of La2O3 was 12 wt%. The characterizations reveal that high copper dispersion, facile reducibility of copper particles and appropriate amount of acidic sites are responsible for the superior catalytic performance.

关键词： dimethyl ether syngas hybrid catalyst Cu-ZrO2 La2O3

Inhibition Effects of CH_(4)/CH_(3)OH on dimethyl ether Cool Flames

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Journal of Thermal Science 2023年第6期32卷 2284-2296页

作者： ZHOU Xun ZHANG Rui YANG Shenghua LIU Dong Key Laboratory of Thermal Control of Electronic Equipment Ministry of Industry and Information TechnologyNanjing210094China Advanced Combustion Laboratory School of Energy and Power EngineeringNanjing University of Science and TechnologyNanjing210094China

CH_(4)/DME mixtures can be used for engines and gas turbines,and have already been studied for many ***,DME has a strong cool flame phenomenon,which will greatly influence the ignition and combustion characteristics of following hot ***,the cool flame characteristics of CH_(4)/DME mixture are very important for their ***,the inhibition effect of CH_(4)on DME cool flames has been discovered,but the mechanisms of the inhibition effects lack further verification and *** this study,the inhibition effects were investigated via both experiments and *** order to validate the inhibition effects,a comparison fuel of CH_(3)OH/DME was also used in this *** extinction limits,flame temperatures and combustion products of the cool flames of the CH_(4)/DME and CH_(3)OH/DME mixtures were measured using a counterflow burner,and the reaction paths and heat release rate were derived from the *** results indicate that CH_(4)and CH_(3)OH will both inhibit the cool flame of DME via competing with DME for OH and O radicals,and CH_(3)OH has stronger inhibition effects than CH_(4),because it is more competitive and produces more CH2O,which inhibits the oxidation of *** HPMech-v3.3 closely agrees with the experimental data,but still needs to be improved.

关键词： cool flame dimethyl ether methane methanol non-premixed counterflow flame