Preparation of Mesoporous MCM-41 in Open-Vessel for Catalytic Synthesis of Geranyl Propionate

2012 ◽  
Vol 550-553 ◽  
pp. 358-361
Author(s):  
Xiao Hong Tang ◽  
Bao Jun Li ◽  
Chun Liang Han ◽  
Jin Wang ◽  
Cheng Wei Li

In this paper, the synthesis of mesoporous molecular sieves MCM-41 was carried out in an open-vessel. The mesoporous structure of as-synthesized MCM-41 was characterized by X-ray diffraction (XRD) pattern, Fourier transform infrared (FT–IR) spectrum, NH3-Temperature Programmed Desorption (TPD), and N2 adsorption-desorption isotherms. The catalytic performances of MCM-41 for the synthesis of geranyl propionate (GP) with geraniol and propionic acid as reagents also were investigated. The characterization results show that the as-synthesized MCM-41 possesses typical hexagonal mesoporous structure with high long-range order and crystalline degree. The high GP selectivity of 64.25% with geraniol conversion of 17.21% was achieved under optimum conditions.

2012 ◽  
Vol 550-553 ◽  
pp. 1391-1394
Author(s):  
Xiao Hong Tang ◽  
Bao Jun Li ◽  
Cheng Wei Li

In this paper, rice straw (RS) and rice straw ash (RSA) were employed to synthesize mesoporous molecular sieves MCM-41 in an open-vessel. The structure of as-synthesized MCM-41 was characterized by X-ray diffraction (XRD) pattern, Fourier transform infrared (FT–IR) spectrum, NH3-Temperature Programmed Desorption (TPD), and N2 adsorption-desorption isotherms. RS-MCM-41 and RSA-MCM-41 possess the same typical hexagonal mesoporous structure with high long-range order and crystalline degree as those of MCM-41 from water glass (SDS-MCM-41).


2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Michal Horňáček ◽  
Pavol Hudec ◽  
Agáta Smiešková

AbstractIn the synthesis of mesoporous molecular sieves of the type MCM-41, different cationactive surfactants and sources of silicon were used. Moreover, Al-MCM-41 samples with different content of aluminium were synthesized. MCM-41 and Al-MCM-41 were synthesized at elevated temperature in stainless-steel autoclaves. Prepared mesoporous molecular sieves were characterized by powder X-ray diffraction (XRD), physical adsorption of nitrogen at the temperature of −197°C, sorption capacity of benzene, and by infrared spectroscopy (FTIR). Acidity was measured for Al-MCM-41 by temperature programmed desorption of ammonia (TPDA) and by FTIR of adsorbed pyridine. Acid catalytic activity of Al-MCM-41 was tested by isomerization of o-xylene. Influence of the synthesis reproducibility, surfactant used, source of silicon, synthesis time, source of aluminium, and Si to Al mole ratio on the properties of mesoporous molecular sieves were evaluated.


2011 ◽  
Vol 233-235 ◽  
pp. 234-237 ◽  
Author(s):  
Sa Liu ◽  
Jian Wei Guo ◽  
Chu Fen Yang ◽  
Long Huan Li ◽  
Yi Hua Cui

Al-containing mesoporous molecular sieves(Al-MCM-41) were synthesized at ambient temperature. The structures of samples were characterized by XRD, N2-adsorption/desorption isotherms and FT-IR, etc. The evaluation results showed that Al-MCM-41 had higher catalytic activity for isomerization conversion of endo-tetrahydrodicyclo-pentadiene (endo-TCD) into exo-tetrahydrodicyclo-pentadiene (exo-TCD) and adamantane (AdH). Loading inorganic acid on the surface of Al-MCM-41 led increase of its catalytic activity and the yield of adamantane.


2013 ◽  
Vol 662 ◽  
pp. 214-217 ◽  
Author(s):  
Li Qin Wang ◽  
Yang Han ◽  
Xiu Jun Fu ◽  
Hai Tao Wu ◽  
E Chang ◽  
...  

Nanoparticals of MCM-41 molecular sieves were synthesized at near room temperature with cetyltrimethylammonium bromide (CTAB) as template agent. The prepared samples were characterized by the means of scanning electron microscopy (SEM), X-ray powder diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), N2 adsorption tests, thermogravimetric and differential thermal analysis (TG-DTA). The results suggested that morphology of MCM-41 molecular sieves samples with high crystallinity was almost uniform spherical, and the particles size was almost less than 100 nm. The adsorption-desorption isotherms were corresponded to typical type IV isotherms with the hysteresis loop of type H2, which showed the samples had mesoporous structure. The pore size distribution of samples were 1.69 nm and 3.58 nm, and the specific surface areas was up to 752.23 m2/g. The decomposition temperature of template agent CTAB was around 327 °C, while the framework for MCM-41molecular sieves was stable. So MCM-41 molecular sieve samples synthesized at near room temperature had excellent physical properties.


Catalysts ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 155 ◽  
Author(s):  
Zhenheng Diao ◽  
Lushi Cheng ◽  
Xu Hou ◽  
Di Rong ◽  
Yanli Lu ◽  
...  

Hierarchical HZSM-5 membranes were prepared on the inner wall of stainless steel tubes, using amphiphilic organosilane (TPOAC) and mesitylene (TMB) as a meso-porogen and a swelling agent, respectively. The mesoporosity of the HZSM-5 membranes were tailored via formulating the TPOAC/Tetraethylorthosilicate (TPOAC/TEOS) ratio and TMB/TPOAC ratio, in synthesis gel, and the prepared membranes were systematically characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), N2 adsorption–desorption, N2 permeation, inductively coupled plasma (ICP), in situ fourier transform infrared (FT-IR), ammonia temperature-programmed desorption (NH3-TPD), etc. It was found that the increase of the TPOAC/TEOS ratio promoted a specific surface area and diffusivity of the HZSM-5 membranes, as well as decreased acidity; the increase of the TMB/TPOAC ratios led to an enlargement of the mesopore size and diffusivity of the membranes, but with constant acid properties. The catalytic performance of the prepared HZSM-5 membranes was tested using the catalytic cracking of supercritical n-dodecane (500 °C, 4 MPa) as a model reaction. The hierarchical membrane with the TPOAC/TEOS ratio of 0.1 and TMB/TPOAC ratio of 2, exhibited superior catalytic performances with the highest activity of up to 13% improvement and the lowest deactivation rate (nearly a half), compared with the microporous HZSM-5 membrane, due to the benefits of suitable acidity, together with enhanced diffusivity of n-dodecane and cracking products.


2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
André E. Nogueira ◽  
Isabela A. Castro ◽  
Amanda S. Giroto ◽  
Zuy M. Magriotis

In this work, MCM-41, magnetite (MAG), and a composite of magnetite and MCM-41 (MCM-MAG) were synthesized by a simple route for the production of active systems in the decomposition of organic waste. The materials were characterized by N2 adsorption/desorption, X-ray diffraction analysis (XRD), temperature programmed reduction (TPR), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM). Our results indicated that the decolorization kinetics of the dyes were in the order of MCM-MAG > MCM-41 > magnetite. Mineralization of the dyes was monitored by total organic carbon (TOC) decrease. The dye solutions could be completely decolorized and effectively mineralized, with an average overall TOC removal 43% for a Fenton-like reaction time of 180 min. The degradation activity of the MCM-MAG was stable during four consecutive experiments, confirming their stability and reusability of the composite. The great advantage of this composite is that it may be easily magnetically recovered and reused.


2008 ◽  
Vol 8 (1) ◽  
pp. 400-404 ◽  
Author(s):  
Ayyamperumal Sakthivel ◽  
Kenichi Komura ◽  
Yoshihiro Sugi

Fe(III) containing mesoporous materials (FeMMSH) with zeolite building units were first time synthesized. XRD and N2 adsorption/desorption analysis confirm the mesoporous characters similar to MCM-48. FT-IR analysis of FeMMSH showed an additional band at about 530–550 cm− 1, characteristic of double five-membered ring of zeolite (ZSM-5) secondary building unit. The Fe(III) in FeMMSH materials is present in tetrahedral, and distorted tetrahedral framework are evident from EPR and DRUV-VIS spectra.


2011 ◽  
Vol 480-481 ◽  
pp. 159-164 ◽  
Author(s):  
Li Qin Wang ◽  
Xiang Ni Yang ◽  
Yang Han ◽  
Ning Yu ◽  
Xiu Li Zhao

The Y/MCM-41 composite molecular sieves were synthesized in the method of hydrothermal crystallization with cetyltrimethylammonium bromide (CTMABr) as the template agent. The as-prepared composite molecular sieves were characterized by the means of X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), the thermogravimetric and differential thermal analysis (TG-DTA) and the nitrogen adsorption test. The experimental results were shown as follows: the Y/MCM-41 composite molecular sieves kept properties of Y-zeolites and MCM-41 molecular sieves. In the XRD and FT-IR spectra, it can be found both characteristic peaks of Y-zeolites and MCM-41 molecular sieves. The pore size distribution plot indicated that the Y/MCM-41composite molecular sieves had micro-mesoporous structure, and the average pore size were about 1.5 nm and 15 nm. The decomposition temperature of the template agent was at 320 °C, and the calcined temperature of Y-zeolites was at about 560 °C. There showed an endothermic process constantly in the DTA curve, and there was little mass loss in the TG curve, indicating the obtained Y/MCM-41 composite molecular sieves had higher thermal stability.


2012 ◽  
Vol 457-458 ◽  
pp. 1283-1286 ◽  
Author(s):  
Yong Hong Yang ◽  
Cheng Yang ◽  
Jin Hu Wu

In this paper, various amine-modified CO2 adsorbents were prepared by incorporating tetraethylenepenthamine (TEPA) onto SBA-15(P) by controlling dynamic impregnation process. The materials were characterized by X-ray diffraction (XRD), nitrogen adsorption/desorption, elemental analysis (EA) and Fourier transform infrared (FT-IR) experiments. Moreover, the adsorption capacities and cycle life were evaculated by CO2 temperature programmed desorption (CO2-TPD). Various characterization results indicate that the morphology and loading amount of TEPA on the support material were controlled by adjusting dynamic impregnation times. Under given conditions, there is an optimum dynamic impregnation times.


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