Abstract:-Al-MCM-41, 16%Ba/Al-MCM-41 and 1.4%Cr-16%Ba/Al-MCM-41 were used as catalysts in the vapor-phase catalytic conversion of ethanol. Physical-chemical properties of the catalysts and the effect of barium and chromium on the Al-MCM-41 activity and 1,3-butadiene yield were studied. The catalysts were characterized by X-ray diffraction (XRD), N 2 physisorption (BET method), CO 2 chemisorption and Fourier transform infrared spectroscopy (FT-IR). When ethanol was completely converted on Al-MCM-41 and 16%Ba/Al-MCM-41, … Show more
“…The nitrogen adsorption/desorption isotherms of Fe 3 O 4 @MCM‐41@Zr‐MNPs before and after modification with piperazine are shown in Figure . The isotherms correspond to type IV (in the IUPAC classification), which is typical of mesoporous materials, and further confirm that the piperazine was loaded into the pore channels of the MCM‐41 support. The Brunauer‐Emmet‐Teller (BET) surface areas, total pore volume and Barret‐Joyne‐Halendu (BJH) pore diameter were 597.42 m 2 .g −1 , 0.3912 cm 3 .g −1 , and 2.6196 nm, respectively.…”
Fe3O4@MCM‐41@Zr‐MNPs modified with piperazine is easily prepared and characterized using Fourier transform infrared spectroscopy (FT‐IR), X‐ray powder diffraction (XRD), N2 adsorption–desorption, Transmission electron microscopy (TEM), Energy‐dispersive X‐ray (EDX), Vibrating sample magnetometry (VSM) and Thermogravimetric analysis (TGA) techniques. The characterization results showed that Zr highly dispersed in the tetrahedral environment of silica framework and piperazine is successfully attached to the surface of the nanocatalyst in connection with zirconium. The prepared nanosized reagent (10–30 nm), shows excellent catalytic activity in the synthesis of tetrahydro‐4H‐chromene and pyrano[2,3‐d]pyrimidinone derivatives. All reactions are performed under mild and completely heterogeneous reactions conditions in high yields during short reaction times. On the other hand and due to its superparamagnetic nature the catalyst can be easily separated by the application of an external magnetic field and reused for several times.
“…The nitrogen adsorption/desorption isotherms of Fe 3 O 4 @MCM‐41@Zr‐MNPs before and after modification with piperazine are shown in Figure . The isotherms correspond to type IV (in the IUPAC classification), which is typical of mesoporous materials, and further confirm that the piperazine was loaded into the pore channels of the MCM‐41 support. The Brunauer‐Emmet‐Teller (BET) surface areas, total pore volume and Barret‐Joyne‐Halendu (BJH) pore diameter were 597.42 m 2 .g −1 , 0.3912 cm 3 .g −1 , and 2.6196 nm, respectively.…”
Fe3O4@MCM‐41@Zr‐MNPs modified with piperazine is easily prepared and characterized using Fourier transform infrared spectroscopy (FT‐IR), X‐ray powder diffraction (XRD), N2 adsorption–desorption, Transmission electron microscopy (TEM), Energy‐dispersive X‐ray (EDX), Vibrating sample magnetometry (VSM) and Thermogravimetric analysis (TGA) techniques. The characterization results showed that Zr highly dispersed in the tetrahedral environment of silica framework and piperazine is successfully attached to the surface of the nanocatalyst in connection with zirconium. The prepared nanosized reagent (10–30 nm), shows excellent catalytic activity in the synthesis of tetrahydro‐4H‐chromene and pyrano[2,3‐d]pyrimidinone derivatives. All reactions are performed under mild and completely heterogeneous reactions conditions in high yields during short reaction times. On the other hand and due to its superparamagnetic nature the catalyst can be easily separated by the application of an external magnetic field and reused for several times.
“…Incidentally, the use of an incorrect support resulted in undesired properties. In particular, MCM-41 was shown to be a poor support, as it structural integrity was repeatedly compromised by post-synthetic modifications, once as silica source for an MgO-SiO 2 catalyst, another time as an acidic support for Cr 2 O 3 and BaO 2 [7,40]. In both case, the ordered mesoporous structure of the silicate was lost.…”
Section: Discussionmentioning
confidence: 99%
“…Another aspect that will grow in importance is the too-often ignored time-on-stream stability of the catalytic materials. Currently, it is believed the coke deposition is the principal source of deactivation [36,40,50,54]. As the performances of the catalysts improve, growing attention will be devoted to minimizing this phenomenon.…”
1,3-Butadiene is traditionally produced as a byproduct of ethylene production from steam crackers. What is unusual is that the alternative production route for this important commodity chemical via ethanol was developed a long time ago, before World War II. Currently, there is a renewed interest in the production of butadiene from biomass due to the general trend to replace oil in the chemical industry. This review describes the recent progress in the production of butadiene from ethanol (ETB) by one or two-step process through intermediate production of acetaldehyde with an emphasis on the new catalytic systems. The different catalysts for butadiene production are compared in terms of structure-catalytic performance relationship, highlighting the key issues and requirements for future developments. The main difficulty in this process is that basic, acid and redox properties have to be combined in one single catalyst for the reactions of condensation, dehydration and hydrogenation. Magnesium and zirconium-based catalysts in the form of oxides or recently proposed silicates and zeolites promoted by metals are prevailing for butadiene synthesis with the highest selectivity of 70% at high ethanol conversion. The major challenge for further application of the process is to increase the butadiene productivity and to enhance the catalyst lifetime by suppression of coke deposition with preservation of active sites.
“…Purely siliceous MCM-41 and Al-containing samples with Si/Al molar ratios of 50 and 15 named Al-MCM-41(50) and Al-MCM-41(15), respectively, were synthesized according to the procedure described previously 20 . …”
Purely siliceous MCM-41 and Al-containing MCM-41 (Al-MCM-41) mesoporous materials were synthesized by non-hydrothermal method in alkali-free ions medium at room temperature and short reaction times. Under these synthesis conditions, it was also investigated the influence of Al incorporation in the crystal structure of MCM-41. The solids were characterized by ICP-OES, AAS, N 2 adsorption at 77 K, XRD, TEM, NH 3 -TPD, 27 Al and 29 Si-MAS-NMR, FT-IR and TGA. The resulting mesoporous materials showed a well-defined hexagonally ordered pore geometry maintaining a uniform and unimodal pore size distribution with high specific surface areas (1000-1400 m 2 g -1 ). The Al +3 ions were introduced successfully in the structure of the purely siliceous MCM-41 expanding the unit cell parameter and forming four-coordinated Al species, and in a less extent, forming six-coordinated Al species. In addition, the surface acidity of the MCM-41 increased with Al loading. Contrary, the presence of Al in the MCM-41 mesoporous structure resulted in a decrease of the crystallinity and specific surface area possibly due to the presence of Al species in highly distorted tetrahedral structures and Al extra-framework or amorphous alumina occluded in the pores. The MCM-41 type mesoporous materials obtained in this work show similar characteristics of those synthesized by conventional hydrothermal methods.
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