Template-Free Synthesis of ZSM-5 Type Zeolite Layers on Porous Alumina Disks
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1 Turk J Chem 31 (2007), c TÜBİTAK Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on Porous Alumin Disks Hlil KALIPÇILAR nd Ali ÇULFAZ Chemicl Engineering Deprtment, Middle Est Technicl University, Ankr-TURKEY e-mil: culfz@metu.edu.tr Received ZSM-5 crystls were synthesized from templte-free tches on mcroporous α-lumin disks. The SiO 2/Al 2O 3 rtio of the synthesis gel influenced the crystl morphology, surfce coverge nd intergrowth mong the crystls. Prismtic ZSM-5 crystls covered the disk surfce when the SiO 2/Al 2O 3 rtio of the tch ws higher thn 100, wheres sphericl polycrystlline prticles of ZSM-5 were otined from tches with SiO 2/Al 2O 3 rtio of 80. Mordenite type zeolite ws formed on the disk surfce due to the incorportion of lumin dissolved from the disk when the time of crystlliztion ws extended. The effects of silic source nd seeding of the support surfce with 0.3 nd 2 µm ZSM-5 crystls on the morphology of zeolite lyer were lso investigted. The purity, surfce coverge nd SiO 2/Al 2O 3 rtio of ZSM-5 crystls incresed in the order of silic sol contining methnol, silic sol, nd silicic cid. Seeding decresed the length of prismtic ZSM-5 crystls from 45 µm 10 µm nd incresed the surfce coverge. Key Words: ZSM-5, templte-free synthesis, zeolite lyer, zeolite memrne. Introduction Zeolites, with their uniform pore structure nd high therml nd chemicl stility, re considered good cndidtes for memrne friction. Zeolite memrnes were usully synthesized y direct contct of support mteril, such s lumin or stinless steel, with rective synthesis mixture. 1 4 Considerle effort hs een devoted to prepre ZSM-5 type memrnes ecuse of their potentil in the seprtion of light hydrocrons. The syntheses were usully performed in the presence of n orgnic structure directing ction, typiclly tetrpropylmmonium (TPA + ). 1 5 These ctions trpped in the zeolite pores during crystl growth re lter removed y clcintion t C. However, clcintion my cuse the development of microcrcks on the memrne surfce due to the thermomechnicl incomptiility etween ZSM-5 crystls nd the support mteril. 6 8 Templte-free synthesis of ZSM-5 cn e n lterntive to the templte contining synthesis to eliminte clcintion. Mintov et l. 9 synthesized ZSM-5 lyers on non-porous qurtz sustrtes from templte-free tches. Prior to the synthesis, the qurtz surfce ws covered y siliclite seed crystls to promote crystlliztion. Corresponding uthor 233
2 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR, A. ÇULFAZ Hedlund et l. 10 prepred templte-free ZSM-5 memrnes in similr mnner on porous lumin supports covered with seed crystls. These memrnes showed selectivities for H 2 /i-c 4 H 10 s high s memrnes synthesized from templte including tches. The permetion of molecules lrger thn the ZSM-5 pores, such s m-xylene, lso showed tht memrnes contined non-zeolitic pores. Few studies were lter reported concerning the synthesis of ZSM-5 memrnes from templte-free tches All those studies were performed using seeded supports. The crystlliztion of ZSM-5 powder from templte-free tches requires more defined synthesis conditions thn the crystlliztion of ZSM-5 from tches contining templte molecule. 16,17 Templte-free ZSM-5 ws crystllized from tches with SiO 2 /Al 2 O 3 rtios of 40 to 70 nd N 2 O/SiO 2 rtios of 0.13 to The tches hving compositions outside these rnges usully resulted in impurity phses such s mordenite 13 or nlcime 16 type zeolites, qurtz, 19 nd unrected morphous solid. 20 In the present study, ZSM-5 crystls were grown on porous α-al 2 O 3 disks from templte-free tches with nd without seeding. The effects of the nture of the silic source nd the SiO 2 /Al 2 O 3 rtio of the tch on the purity nd morphology of crystls were investigted. Experimentl Methods Preprtion of sustrtes Home-mde α-al 2 O 3 disks, which were used s support, were prepred with dimeter of 21 mm nd thickness of 1 mm. Disks were mde y pressing out 0.8 g of α-al 2 O 3 powder (Riedel de Hen) under 128 MP. A smll mount of sodium silicte solution (Merck) ws dded to the lumin powder s inder. The green disks were dried overnight t mient conditions nd sintered t 1200 Cfor 22 h. Sintered α-al 2 O 3 disks consisted of 5.5% y weight dry sodium silicte. The sintered disks hd void volume of 0.20 cm 3 /g nd verge pore dimeter of 1.6 µm, which were mesured y Micromeritics Pore Sizer 9310 mercury porosimeter. Before the synthesis of zeolite lyer, oth sides of the disks were polished y sndpper nd wshed with distilled wter in n ultrsonic th for 5 min; this procedure ws repeted 3 times. The polished disks were dried t room temperture. Synthesis of templte-free ZSM-5 lyers without seeding The gel composition, 6.5 N 2 O:Al 2 O 3 :80SiO 2 :3196H 2 O, reported y Grose nd Flnigen 21 for the synthesis of templte-free powder of ZSM-5 ws used to prepre the zeolite lyers. The synthesis gel ws prepred using 3 silic sources: silicic cid (Merck), silic sol (Ludox HS40, Aldrich), nd silic sol contining 15% methnol y weight (Merck). The other rectnts were Al(OH) 3, NOH, nd distilled wter. The crystlliztion ws crried out t 200 Cfor 24 h to 172 h in stinless steel utoclves with PTFE cup inserts. The cpcity of PTFE cup ws out 35 ml nd 85% of this volume ws filled with the synthesis gel. Two lumin disks, one t the top nd the other t the ottom, were verticlly plced in PTFE cup y PTFE holders. After crystlliztion, the disks were wshed with distilled wter nd dried t room temperture. Synthesis of templte-free ZSM-5 lyers with seeding The disk surfces were covered with siliclite seed crystls efore crystlliztion. Siliclite with n verge size of 0.3 µmnd2µmws synthesized from tch with molr composition of 6.5 N 2 O:30SiO 2 :6.9TPABr: 234
3 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR,A.ÇULFAZ 1136H 2 O t 100 Cfor 72 h nd t 200 Cfor 24 h, respectively. 22 The crystls were clcined t 500 Cfor 10 h nd were used to prepre the seed suspension, which hd concentrtion of 0.3% y weight for 0.3 µm nd of 0.2% y weight for 2 µm crystls. For seed coting, n lumin disk ws slowly dipped into the seed suspension nd kept for 10 min, nd then slowly removed. The disk ws dried t 50 Cfor 30 min. Dipping ws repeted 5 times. The seed deposited disks were kept t 250 Cfor 2.5 h to fix the seed crystls onto the lumin surfce. 23 The synthesis on seeded disks ws performed y following the sme procedure pplied for the synthesis of templte-free ZSM-5 lyers on the re disks. Chrcteriztion of zeolite lyers The crystlline phses formed on the support surfce were determined y X-ry diffrctometer (Philips PW 1840) using Ni filtered CuKα-rdition. Scnning electron microscopy (JEOL JSM-330) ws used to exmine the morphology of the zeolite lyer. The chemicl nlysis of the lyer ws performed y energy dispersive X-ry spectrophotometer (EDX, Norton Instruments Series II). Results nd Discussion Effect of lumin content of tch on the morphology of crystls Btches hving SiO 2 /Al 2 O 3 rtios etween 80 nd infinity (Al 2 O 3 -free) were prepred to synthesize templtefree ZSM-5 lyers y using Ludox HS-40 s the silic source. The SiO 2 /Al 2 O 3 rtios were djusted y incresing the lumin content of the gel. Tle 1 shows the crystlliztion conditions s well s the crystlline phses tht ppered on the lumin disk surfce fter specified times of crystlliztion. The only crystlline phse tht formed on the disk surfces ws ZSM-5 except for the tch with SiO 2 /Al 2 O 3 rtio of 80, which yielded mordenite in ddition to ZSM-5 when no seeds were used. Tle 1. Synthesis conditions of templte-free ZSM-5 lyers nd the crystlline phses formed on α-al 2O 3 disks. Code SiO 2 /Al 2 O 3 Silic Synthesis Seed size 1 Phses formed 2 rtio in tch source time (h) D1 80 Silicic cid 96 - ZSM-5+MOR (minor) D2 80 C.S ZSM-5 D3 80 Ludox 96 - ZSM-5+MOR (minor) D4 100 Ludox 96 - ZSM-5 D5 160 Ludox 72 - ZSM-5 D6 Ludox 72 - ZSM-5 D7 Ludox MOR+ZSM-5 (minor) D8 80 Ludox ZSM-5 D9 80 Ludox 96 2 ZSM-5 1 D1-D7 synthesized without seeds 2 MOR: mordenite type zeolite 3 Colloidl silic contining 15% methnol Figure 1 shows the SEM imges of disk surfces prepred from tches with different SiO 2 /Al 2 O 3 rtios. The surfce of smple D6 tht ws synthesized from the lumin-free tch ws extensively covered y ZSM-5 crystls of prismtic shpe with n verge length of 8 µm nd n spect rtio of 5. Although the 235
4 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR, A. ÇULFAZ coverge ws very high, the cross-section imge of the disk (not given) showed tht the interction etween the ZSM-5 crystls nd the lumin disk is wek. Most of the crystls detched from the surfce fter the disk ws treted in n ultrsonic th for 5 min. 100 µm 100 µm c d 100 µm 10 µm Figure 1. SEM imge of templte-free synthesized ZSM-5 lyers on α-lumin disk surfce with SiO 2/Al 2O 3 rtio of () 80, D3 () 100, D4, (c) 160, D5, (d), D6. The surfces of smples produced from tches D4 nd D5 were extensively covered y ZSM-5 crystls (Figure 1 nd c). Although the intergrowth mong the crystls ws still low, the interction etween the ZSM-5 lyer nd the lumin disk incresed. The crystls on smples D4 nd D5 hd the typicl prismtic shpe of ZSM-5, which ws similr to the shpe of ZSM-5 crystls otined from the lumin-free tch. However, the crystls were significntly lrger thn the crystls otined from the lumin-free tch. The verge crystl size on oth D4 nd D5 ws 20 x 45 µm. The lumin ddition to the synthesis gel did not chnge the crystl shpe significntly; however, the prticle size considerly incresed s the SiO 2 /Al 2 O 3 rtio of tch decresed to 100. Upon further decrese in the SiO 2 /Al 2 O 3 rtio of the tch to 80, lrge sphericl prticles, consisting of smller cue-like ZSM-5 crystls, formed with dimeter of pproximtely 40 µm s shown on the imge of smple D3 (Figure 1d). Persson et l. 28 showed tht the crystl size increses with incresing lumin concentrtion in the synthesis of sumicron ZSM-5 crystls from cler solutions. Similrly, Yn et l. 29 showed tht ddition of lumin to the synthesis medium increses the size of prticles covering the lumin support during the synthesis of ZSM-5 memrnes from templte-contining tches. The lrger crystls formed from tches with SiO 2 /Al 2 O 3 rtios of 100 nd 160 cn e ttriuted to the higher lumin concentrtion of tch compred to the lumin-free tch. 236
5 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR,A.ÇULFAZ The holes seen on the ZSM-5 crystls, which usully ppered t the crystl edges (Figure 1 nd c), re proly ecuse of the dissolution of the ZSM-5 crystls. The metstle nture of ZSM-5 my cuse the dissolution of crystls nd recrystlliztion into more stle phse. 24 On the other hnd, Shirlkr nd Clerfield 17 ttriuted the dissolution of the ZSM-5 crystls synthesized without templtes to the excess sodium trpped in the zeolite pores during the synthesis. The lumin-free tch yielded pure ZSM-5 lyer fter 72 h of crystlliztion (smple D6), wheres the powder tht formed in the ulk solution nd settled during the crystlliztion ws pure qurtz. Extending the crystlliztion time to 168 h resulted in the complete coverge of surfce with mordenite (smple D7) s shown in Figure 2. Although no ZSM-5 crystls cn e detected from the surfce imge, the cross-section imge (Figure 2) showed tht there re some ZSM-5 crystls mong the mordenite crystls. The SiO 2 /Al 2 O 3 rtio of crystls on the surfce ws 28.4 nd 8.8 fter 72 nd 168 h of crystlliztion, respectively. Note tht the lumin surfce ws covered y luminum-contining zeolites, either mordenite or ZSM-5, lthough the synthesis hd een performed with n lumin-free tch. The formtion of lumin-contining zeolites from n lumin-free tch suggests the prtil dissolution of the support mteril nd incorportion of dissolved luminum into the crystlliztion medium. 10 µm 10 µm Figure 2. Surfce () nd cross-section () SEM imges of ZSM-5 lyers synthesized from lumin-free tch D7 for 168 h. Geus et l. 6 prepred zeolite films on vrious supports including porous α-lumin, zirconi nd cly from the sme templte contining gel. ZSM-5 crystls were seen only on cly nd insolule zirconi support while lumin-rich nlcime type zeolite phse ws formed on α-lumin support tht ws leched during crystlliztion. Similrly, Pn et l. 12 nd Lssinntti et l. 25 oserved dissolution of lumin support nd incorportion of leched luminum into the zeolite lyer during the synthesis of templte-free ZSM-5 memrnes. The gel tht ws presumed to e formed on the disk surfce 7,23 is enriched in luminum s result of leching such tht n luminum-rich zeolite like nlcime my form on the memrne surfce. ZSM-5 nd mordenite type zeolites were formed on the disk surfce, wheres the settled powder ws qurtz since the luminum concentrtion is likely to e the highest round the lumin support nd its pores, while the ulk of crystlliztion solution ws rich in silic. 237
6 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR, A. ÇULFAZ Effect of the nture of the silic source on the morphology of crystls Figure 3 shows the XRD ptterns of disk surfces fter 96 h of crystlliztion in templte-free gels tht were prepred using different silic sources. The peks tht elong to the lumin disk re mrked with n sterisk. Silicic cid (D1) nd silic sol contining methnol (D2) yielded only ZSM-5 s the crystlline phse on the disk surfce; however, the templte-free synthesis of ZSM-5 in powder form using the sme silic sources hd yielded ZSM-5 with qurtz. 26 The ZSM-5 (smple D3) synthesized from Ludox, which is silic sol without methnol, contined mordenite s minor phse, the peks of which re mrked with rrows on Figure 3. Strong XRD pek intensities for smples D2 nd D3 indicted tht lrger mount of ZSM-5 crystl ws deposited on the disk surfce compred to smple D1. However, the hump centered t round 23 Brgg ngle on the ckground reflections 27 of ll smples lso suggests the presence of morphous gel residue on the sustrte surfce. * lumin * * mordenite c d Brgg Angle Figure 3. XRD ptterns of templte-free synthesized ZSM-5 lyers on α-lumin disk surfce with () silicic cid, D1, () silic sol with methnol, D2, (c) Ludox, D3, (d) pttern of ZSM-5 from ICDD PDF No: Figure 4 shows the SEM imges of disk surfces. The disk surfce ws fully covered y ZSM-5 crystls in smple D2 nd prtly covered in smple D3 (Figure 1); however, few crystl deposits were seen on the surfce of smple D1. The crystls on smple D2 hd morphology resemling the typicl prismtic shpe of ZSM-5. The lrge sphericl prticles on the imge of D3 re ZSM-5 prticles. The prticles on D1 nd D3 re the gglomertes of cue-like ZSM-5 crystls. The size of gglomertes is round 20 µm ond1nd 40 µm on D3. The minor mordenite phse, which ws detected y XRD on smple D3, could lso e seen s needle-like unches in Figure
7 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR,A.ÇULFAZ 100 µm 100 µm Figure 4. SEM imges of templte-free synthesized ZSM-5 lyers on α-lumin disk surfce with () silicic cid, D1, () silic sol with methnol, D2. Di et l. 18 showed tht silic sources hving smll prticles fvored the formtion of ZSM-5 more thn the silic sources hving lrge prticles. Klıpcılr nd Çulfz 26 studiedtheeffectofthentureof the silic source nd the presence of orgnic stilizing gents in the silic source on the crystlliztion of templte-free ZSM-5 in powder. The methnol present in the silic sol promoted the crystlliztion. Silic sol tht does not contin n orgnic stilizing gent or silicic cid yielded ZSM-5 with qurtz s minor phse. The nture of the silic source is significnt for product purity in templte-free synthesis of ZSM-5. The chemicl nlysis of ZSM-5 prticles on the disk surfce is shown in Tle 2. Smples D1 nd D2 hve SiO 2 /Al 2 O 3 rtios of 18.6 nd 19.2, nd N 2 O/Al 2 O 3 rtios of 0.4 nd 0.6, respectively. The SiO 2 /Al 2 O 3 rtio of the smples ws similr ut much lower thn the SiO 2 /Al 2 O 3 rtio of the synthesis gel, which ws 80. Although ny type of zeolite contining luminum within its frmework needs ction to compenste for the negtive electricl chrge of the frmework, the N 2 O/Al 2 O 3 rtio of these smples ws lower thn one, proly due to the contriution of lumin sustrte to the chemicl nlysis. The SiO 2 /Al 2 O 3 nd N 2 O/Al 2 O 3 rtios of crystls on D3 were mesured s 33.3 nd 1.4, respectively. The presence of morphous solid on the surfce or the excess sodium tht remined in the crystl pores re possile resons for the high N 2 O/Al 2 O 3 rtio. 17 Tle 2. Surfce composition of the lumin disk surfce performed y EDX. Code Silic source SiO 2 /Al 2 O 3 rtio N 2 O/Al 2 O 3 rtio D1 Silicic cid D2 Silic sol with methnol D3 Ludox Effect of seeding on lyer properties Templte-free synthesis of ZSM-5 without seed crystls showed tht ZSM-5 crystls usully formed with low degree of intergrowth, proly due to the low numer of nuclei tht formed on the surfce. ZSM-5 seed crystls were emedded in the disk surfce in order to increse the numer of nucletion sites on the surfce nd to promote crystlliztion on the surfce. The seeding technique ws often used for the production of zeolite memrnes oth from templte contining tches 1 nd from templte-free tches The synthesis conditions for seeded synthesis of ZSM-5 lyers re lso given in Tle
8 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR, A. ÇULFAZ The SEM imge of the disk surfce fter seed coting showed tht the sumicron seed crystls were minly deposited on the lumin prticles ut did not fill the lrge support pores, wheres the lrger seed prticles were rndomly distriuted on the surfce (Figure 5). 1µm 1µm Figure 5. SEM imges of α-lumin disk surfces covered with siliclite seed crystls () 0.3 µm ()2µm. Figure 6 shows the SEM imge of disks crystllized for 72 h using seed crystls. The disk surfces were fully covered y ZSM-5 crystls. The surfce coverge ws significntly higher thn the surfce coverge of the smples synthesized on unseeded disks. The ZSM-5 crystls synthesized with sumicron seed crystls (Figure 6) were of prismtic shpe nd exhiited nrrow prticle size distriution with typicl size of 2 y 10 µm. The crystls were much smller thn those produced on the unseeded lumin disks. When the micron size seed crystls were used for synthesis (Figure 6), the crystls exhiited cue-like morphology with n verge size of 4-5 µm. 10µm 10µm Figure 6. SEM imges of templte-free synthesized ZSM-5 lyers from tch with SiO 2/Al 2O 3 rtio of 80 on α-lumin disk surfce coted with seed prticles, () 0.3 µm, D8 nd () 2 µm, D9. Conclusion ZSM-5 crystls were synthesized on seeded nd unseeded mcroporous α-al 2 O 3 disks from templte-free tches prepred using silicic cid, silic sol, nd silic sol contining methnol s stilizer with different SiO 2 /Al 2 O 3 rtios. The nture of the silic source influenced the purity, surfce coverge, nd morphology. ZSM-5 crystls fully covered the sustrte surfce when silic sol contining methnol ws used s silic 240
9 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR,A.ÇULFAZ source. ZSM-5 crystls on the α-al 2 O 3 disks dissolved t long crystlliztion times, nd mordenite crystls were formed due to the luminum leched from the disk. Seed coting on the sustrte surfce efore crystlliztion decresed the crystl size nd incresed the surfce coverge. Acknowledgment The uthors cknowledge the finncil support provided y the Stte Plnning Orgniztion nd METU Reserch Fund (DPT-97K122080) nd TÜBİTAK (TBAG-1532) for this work. References 1. Z.A.E.P. Vroon, K. Keizer, M.J. Gilde, H. Verweij nd A.J. Burggrf, J. Memr. Sci. 113, (1996). 2. H. Klıpçılr nd A. Çulfz, Micropor. Mesopor. Mter. 52, (2002). 3. F. Jremn, J. Hedlund nd J. Sterte, Sep. Purif. Tech. 32, (2003). 4. G. Xomeritkis, S. Nir nd M. Tsptsis, Micropor. Mesopor. Mter. 38, (2000). 5. K. Kuske, T. Kurod, A. Murt nd S. Morook, Ind. Eng. Chem. Res. 36, (1997). 6. E.R. Geus nd H. vn Bekkum, Zeolites 15, (1995). 7. M.J. den Exter, H. vn Bekkum, C.J.M. Rijn, F. Kpteijn, J.A. Moulijn, H. Schellevis nd C.I. N. Beenkker, Zeolites 19, (1997). 8. J.H. Dong, Y.S. Lin, M.Z.C. Hu, R.A. Pescoe nd E.A. Pyznt, Micropor. Mesopor. Mter. 34, (2000). 9. S. Mintov, J. Hedlund, V. Vltchev, B.J. Schoemn nd J. Sterte, J. Mter. Chem. 8, (1998). 10. J. Hedlund, M. Nock, P. Kolsch, D. Creser, J. Cro nd J. Sterte, J. Memr. Sci. 159, (1999). 11. R. Li nd G.R. Gvls, Micropor. Mesopor. Mter. 38, (2000). 12. M. Pn nd Y.S. Lin, Micropor. Mesopor. Mter. 43, (2001). 13. J.H. Dong, E.A. Pyznt, M.Z.C. Hu, D.W. Depoli nd Y.S. Lin, J. Mter. Sci. 38, (2003). 14. G. Li, E. Kikuchi nd M. Mtsukt, Micropor. Mesopor. Mter. 60, (2003). 15. S. Goplkrishnn, T. Ymguchi nd S.I. Nko, J. Memr. Sci. 274, (2006). 16. B.M. Lowe, J.R.D. Nee nd J.L. Csci, Zeolites 14, (1994). 17. V.P. Shirlkr nd A. Clerfield, Zeolites 9, (1989). 18. F.Y. Di, M. Suzuki, H. Tkhshi nd Y. Sito Crystlliztion of Pentsil Zeolite in the Asence of Orgnic Templtes in Zeolite Synthesis, ACS Symp. Series, Vol. 398, eds. M.L. Occelli nd H.E. Roson, pp , Wshington DC, R. Aiello, F. Cre, A. Nstro nd C. Pellegrino, Zeolites 7, (1987). 20. M. Otke, Zeolites 14, (1994). 21. R.W. Grose nd E.M. Flnigen, US Ptent 4,257,885 (1981). 22. H. Klıpcılr nd A. Çulfz, Cryst.Res.Technol.35, (2000). 241
10 Templte-Free Synthesis of ZSM-5 Type Zeolite Lyers on..., H. KALIPÇILAR, A. ÇULFAZ 23. R. Li nd G.R. Gvls, Ind. Eng. Chem. Res. 37, (1998). 24. A. Ary nd B.M. Lowe, Zeolites 6, (1986). 25. M. Lssinntti, F. Jremn, J. Hedlund, D. Creser nd J. Sterte, Ctl. Tody 67, (2001). 26. H. Klipcilr nd A. Culfz, Cryst.Res.Technol.36, , (2001). 27. K.G. Fegn nd B.M. Lowe, J. Chem. Soc., Frdy Trns. I 82, (1986). 28. A.E. Persson, B.J. Schoemn, J. Sterte nd J.E. Otterstedt, Zeolites 15, (1995). 29. Y.S. Yn, M.E. Dvis nd G.R. Gvls, Ind. Eng. Chem. Res. 34, (1995). 242
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