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Catalysts 2016, 6, 30 5 of 11 Figure 2: SEM images (1 μm scale‐bar) of zeolites synthesized for different durations. Figure 2. SEM images (1 μm scale-bar) of zeolites synthesized for different durations. The SAR based on the bulk composition was remarkably affected and values in the range of 25 to150weInretmheaZsSuMred-5.Mzeiocrloitpeosryosnithieessaisndwmithesboipomroassitsieesxatreacrtat(hoebrtasimneildarbfyorhayldlrzoeloylistiesiinline withNlaitOerHatu0.r5emdaotal/[L22,,a2g3e].dFdorutrhinegsa2k4eho,fZclSaMrit-y5,Dap),acroentvZenSMtio‐5nawlaMsFchIacroafcfitenr-iszheadpbeyctrhyesntaitlrsogen adsorption/desorption technique and similar microporous volumes were measured. ZSM‐5 prepared were formed, being larger than those observed without biomass-derived compounds in the presence of biomass derived‐compounds exhibited a slightly lower mesoporous volume (Refs. [1,2]). After extending the ageing time to 48 h (ZSM-5 E(48)) a further increase compared to its parent ZSM‐5 counterpart. The ZSM‐5 structure is orthorhombic (Pnma space group) in the crystal size was observed, but the common shape for ZSM-5 crystals was still when high thermal treatment is conducted [24,25], usually resulting in prismatic crystal formation [26] maintained. It seems however that the surface roughness diminished for ZSM-5 as observed for reference zeolites (Figure 2). The standard method used for preparing ZSM‐5 zeolite E(48) which may indicate a higher crystallinity. This assumption is in line with XRD resulted in 1‐3 μm range crystal size with no changes in morphology with ageing time. In contrast, both data (Table 2). In contrast, after an ageing time of 72 h, ZSM-5 F(72) exhibits a similar morphology and particle size were affected by the presence of biomass derived‐compounds. The extract morphology to ZSM-5 D(24) but with a high level of intergrowth. A peculiar crystal obtained at 0.1 mol/L led to regular (size and type) ZSM‐5 crystals at an ageing time of 24 h. A further raisaegignraegeaitnigontimectoha4n8ishmlesdeetomtshetoforcmcautri,onreosuflctriynsgtailnsheaxvteingsitvhetswaminensinizge,obbusteerxvterdemely difffeorernltoingteerrmsysnothfemsoisrpdhuorloagtiyonthsa.tTwhaismcoingshtrtubcetedubeytaondaisseomlubtliyonof/reelocnrgyasteadlliFzraetniochn‐fries having 100 nm in width. At longer ageing times, larger crystals were formed, exhibiting again a phenomena, involving peculiar self-assembly processes during the crystal growth. conventional morphology. In contrast to ZSM‐5 A(24) sample, ZSM‐5 C(72) sample exhibits sharper Since zeolites are metastable materials, it is possible to shift from one structure to crystal outer rim and appears to be more faceted. While studying the influence of alkali cation nature another one [28], or to crystallize in various morphologies by a simple change in and gel ionic strength, Petrik et al. were able to synthesize MFI zeolites with significant changes in the synthesis duration. This phenomenon was already observed for SiC substrate morphology and drawn the conclusion that minor alterations of the composition may lead to major self-reconstruction into zeolites [29,30]. changes in the crystal growth [27]. The cracking of n-hexane or so-called alpha test [31] is an useful tool for ranking In the ZSM‐5 zeolite synthesis with biomass extract (obtained by hydrolysis in NaOH 0.5 mol/L, ZSM‐5 E(48) which may indicate a higher crystallinity. This assumption is in line with XRD data 231 (Table 2). In contrast, after an ageing time of 72 h, ZSM‐5 F(72) exhibits a similar morphology to ZSM‐ 5 D(24) but with a high level of intergrowth. A peculiar crystal aggregation mechanism seems to occur, resulting in extensive twinning observed for longer synthesis durations. This might be due to dissolution/recrystallization phenomena, involving peculiar self‐assembly processes during the crystal growth. Since zeolites are metastable materials, it is possible to shift from one structure to the catalytic activity of acidic zeolites since catalytic activity is related to both the aged during 24 h, ZSM‐5 D), conventional MFI coffin‐shape crystals were formed, being larger than thosneuombsbeervr eadnwd ityhpouetobfioamciadss‐idtesriavnedcaolmsopotounthdes (mReofrsp. [h1o,2l]o).gAyfatenrdexctreynsdtianlgotrhgeaangieziantgiotnim. e to 48hTh(ZeSMn-‐h5eEx(a4n8e))acftuivrtihtyeriisncirnedaseedinltohweecrycsotamlspizaerewdastoobtsheervceodm,bmuterthcieacloZmSmMo-n5s[h2a2p]efor ZSM‐5 crystals was still maintained. It seems however that the surface roughness diminished forPDF Image | Zeolite Catalysis
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