氟硅酸铵处理KL沸石对有关指标的影响

KL(湖南师范大学长沙410081)用(NH4)2SiF6处理了KL沸石结果表明:无NH4Ac缓冲剂时,所得样品具有较多的中间孔,但孔分布不集中;加入NH4Ac作为缓冲剂,或延长反应时间,所制备的样品不仅可获得较高的结晶度,而且孔分布集中程度也得到明显改善但无论如何,中间孔的孔质及孔分布集中程度均远不如一次合成的MCM-41中孔材料KL沸石(NH4)2SiF6中间孔结晶度TQ127TreatmentofKLwith(NH4)2SiF6EffectsoftreatmentconditionsonCrystallinityandtextoralpropertiesofsamplesXiongShirongYangZhishuYangJunliangHeNongyue(HunanNormalUniversityChangsha410081)AbstractInthispaper,KLwastreatedwith(NH4)2SiF6,SomemesoporesweregeneratedintheabsenceofNH4Acasabufferagent,butthemesoporesizedistributionwasbroad.InthepresenceofNH4Acorelongatedthecorrosiontime,notonlyahigherCrystallinityofSampleswasobtained,butalsothemesoporesizedistributionwasimproved.However,inanycasetheporesizedistributionandmesoporevolumeisnotasgoodasthoseofthedirectlysynthsizedmesoporousmaterialMCM41.KeywordsKL(NH4)2SiF6mesoporeCrystallinity1,MobilMCM-41,[1,2],,,,,,,((NH4)2SiF6Si/Al(NaACaANaX)[3],10~30nm(NH4)2SiF6Y[4],(NH4)2SiF6274199712HUNANCHEMICALINDUSTRYVol.27No.4December1997KL221原料KL[5]Na2O05%,Si/Al2.9(NH4)2SiF6,AFS22样品制备和表征30g120KL200ml,,0.5mol/lAFS,100(2h),(FKL)NH4Cl48h,X-(XRD5DX)(ASAP-2000)221~32(2,2,1),(1,0,2),(3,2,1),(3,0,2)(2,2,2)5XRD331KL沸石分子筛处理前后的XRD图谱1KLAFSXRD,KLAFS,,Al-OSi-O,AFS,XRD,,,AFSNaNH4Y[4],AFS2=5~632处理条件的影响321AFS/Al1KL(a,Si/Al=2.90)FKL(b,Si/Al=3.94)XRD1AFS/AlAFS/Al[1]Si/Al(%)Vmicro[2](cm3/g)(m2/g)Vmes[3](cm3/g)Vtotal[4](cm3/g)dav[5](nm)1-2.891000.104304---20.33.941050.1043490.1150.11512.930.55.49990.0723200.1440.11210.740.77.32730.0603110.1750.15111.850.97.37590.0562960.1880.14010.3:1AFS/Al!!!AFSKLAlmol234(Vtotal=-KL)5BJH1,AFS,Al,1XRD1,AFS,Si/Al,,MaoAFSA274:KLX[3],21,KLAl,AFS322AFS2AFSAFS/Al(mol)speed*(1)(mol∀AFS/mol∀Al∀h)Si/Al(XRD%)Vmicro(cm3/g)(m2/g)Vmeso(cm3/g)dav(nm)Vtotal(cm3/g)40.70.17.31730.0603110.17511.80.15150.70.037.44880.0442980.20811.20.14860.70.37.27670.0742990.16611.20.132*AFSAFS/Al,AFS(2),,,,AFS,,,,AFS,,,,,,333pH3pH,pH,pH,,Si,,,,,,,pH,3pHAFS/Al(mol)pHSi/Al(mol)(XRD%)Vmicro(cm3/g)(m2/g)Vmeso(cm3/g)Vtotal(cm3/g)dav(nm)70.73.0~3.54.94460.0412790.1330.06212.480.74.74.94680.0502900.1210.05913.290.75-66.14830.0663050.1070.05313.6334NH4Ac4NH4Ac,NH4AcpH,AFS/Al(0.5),NH4AcAFS/Al(0.7),(NH4)Ac,,NH4Ac,,,2,NH4Ac,(14),NH4Ac(313),NH4Ac,F-KL,28274NH4AcAFS/Al(mol)NH4Ac/KL(mol)Si/Al(mol)(XRD%)Vmicro(cm3/g)(m2/g)Vmeso(cm3/g)Vtotal(cm3/g)dav(nm)100.51.33.241010.0793120.0810.023613.4110.504.01990.0722830.1440.095813.0120.72.27.281090.0642480.0550.003214.1130.706.04670.0662700.1070.052613.62FKL14BJH(NH4Ac/KL=0)3a[13(NH4Ac/KL=2.2)]b(BMCM-41)BJHa.3hb.9h4NH4Ac/KL=12.65BJH45,NH4Ac,(25NH4Ac/KL0,2.2,0.61.2),NH4Ac,(4a),AFS(4b),5NH4Ac/KL=1.2,13BJH,35,MCM-411KresgeCT,leonowiczME,RothWJetal.orderedmesoporousmolecularsievessynthesizedbyaliquid-crystaltemplatemechanism.Nature,1992,(359):7102,,Y,1993,(1):153HeNongyue,Baoshulin.XuQinhua.IncorporationofFe(#)inFrameworkofzeoliteL.ChineseJ.Chem,1997,(1):1~74,,AiSiMCM-41,1996,(3):315收稿日期:1997年8月25日294:KL