Nghiên cứu chế tạo xúc tác zeolity chứa mao quản trung bình từ nguyên liệu trong nước ứng dụng trong phản ứng alkyl hóa benzene bằng isopropanol

B GIO DC V O TO TRNG I HC BCH KHOA H NI Lấ VN DNG NGHIấN CU CH TO XC TC ZEOLIT Y CHA MAO QUN TRUNG BèNH T NGUYấN LIU TRONG NC NG DNG TRONG PHN NG ALKYL HểA BENZENE BNG ISOPROPANOL LUN N TIN S HểA HC H Ni 2017 B GIO DC V O TO TRNG I HC BCH KHOA H NI Lấ VN DNG NGHIấN CU CH TO XC TC ZEOLIT Y CHA MAO QUN TRUNG BèNH T NGUYấN LIU TRONG NC NG DNG TRONG PHN NG ALKYL HểA BENZENE BNG ISOPROPANOL Chuyờn ngnh: Húa Hu c Mó s: 62440114 LUN N TIN S HểA HC NGI HNG DN KHOA HC: GS.TS T Ngc ụn GS.TS V Th Thu H H Ni 2017 LI CAM OAN Tụi xin cam oan, õy l cụng trỡnh nghiờn cu ca riờng tụi, cỏc s liu v kt qu nghiờn cu nờu lun ỏn l trung thc, c cỏc ng tỏc gi cho phộp s dng v cha tng c cụng b bt k mt cụng trỡnh no khỏc Tỏc gi Lờ Vn Dng T A M TT PT I O VI N NG DN GS.TS T Ngc ụn LI CM N Trc ht, tụi xin by t lũng bit n sõu sc ti GS.TS T Ngc ụn v GS.TS V Th Thu H ó tn tỡnh hng dn, ch o nghiờn cu khoa hc v giỳp tụi sut quỏ trỡnh thc hin lun ỏn Xin chõn thnh cỏm n cỏc cỏn b ca B mụn Húa Hu c - Vin K thut Húa hc - i hc Bỏch Khoa H Ni v Phũng thớ nghim trng im Cụng ngh Lc, Húa du - Vin Húa hc Cụng nghip Vit Nam ó luụn h tr, giỳp tụi thi gian lm lun ỏn Xin trõn trng cm n Vin K thut Húa hc, Vin o to sau i hc i hc Bỏch Khoa H Ni ó luụn to mi iu kin v c s vt cht v th tc hnh chớnh cho tụi thc hin lun ỏn Xin trõn trng cm n cỏc PTN phõn tớch mu ca Khoa Húa hc - i hc Khoa hc T nhiờn - i hc Quc gia H Ni, Khoa Húa hc - i hc S phm H Ni, Vin V sinh Dch t Trung ng v cỏc n v khỏc ó to iu kin thun li cho tụi cú c kt qu thc hin lun ỏn Xin chõn thnh cỏm n gia ỡnh, bn bố, ng nghip ó ng viờn giỳp tụi hon thnh lun ỏn ny Tỏc gi Lờ Vn Dng MC LC DANH MC CH VIT TT V K HIU DANH MC BNG BIU DANH MC HèNH V M U CHNG TNG QUAN 1.1 QU TRèNH ALKYL HểA HYDROCACBON THM VI XC TC TRấN C S ZEOLIT 1.1.1 Phn ng alkyl húa hydrocacbon thm 1.1.2 Xỳc tỏc cho quỏ trỡnh alkyl hoỏ hydrocacbon thm 1.1.3 Xỳc tỏc trờn c s zeolit Y cho quỏ trỡnh alkyl hoỏ hydrocacbon thm 1.1.4 Quỏ trinh alkyl hoa san xuõ t cumene 1.2 GII THIU ZEOLIT Y CHA MAO QUN TRUNG BèNH 13 1.2.1 Gii thiu zeolit Y 13 1.2.2 Gii thiu zeolit Y cha mao qun trung bỡnh 17 1.2.3 Cỏc phng phỏp tng hp zeolit Y cha mao qun trung bỡnh 17 1.2.4 Cỏc yu t nh hng ti quỏ trỡnh tng hp zeolit Y cha MQTB 25 1.2.5 ng dng ca zeolit Y cha mao qun trung bỡnh 33 1.3 NGUYấN LIU CAO LANH V V TRU 34 1.3.1 Cao lanh 34 1.3.2 V tru 37 CHNG THC NGHIM V PHNG PHP NGHIấN CU 41 2.1 CHUN B NGUYấN LIU V HểA CHT 41 2.1.1 Hoỏ cht v dng c 41 2.1.2 Nguyờn liu cao lanh 41 2.1.3 Nguyờn liu v tru 41 2.2 NGHIấN CU TNG HP NANO-ZEOLIT Y T CAO LANH 42 2.2.1 Thc nghim 42 2.2.2 Nghiờn cu mt s yu t nh hng 43 2.3 NGHIấN CU TNG HP MESO-ZEOLIT Y T CAO LANH 2.3.1 Thc nghim 44 44 2.3.2 Nghiờn cu nh hng ca thnh phn v iu kin phn ng giai 45 on mt 2.3.3 Nghiờn cu nh hng ca thnh phn v iu kin phn ng giai on hai 46 2.4 NGHIấN CU TNG HP MESO-ZEOLIT Y T V TRU V CAO 47 LANH 2.4.1 Thc nghim 47 2.4.2 Nghiờn cu mt s yu t nh hng 48 2.5 NGHIấN CU TNG HP MSU-S(Y) T V TRU V CAO LANH 49 2.5.1 Thc nghim 49 2.5.2 Nghiờn cu mt s yu t nh hng 50 2.6 NGHIấN CU PHN NG ALKYL HểA BENZENE BNG ISOPROPANOL S DUNG XC TC TRấN C S CC VT LIU ZEOLIT Y CHA MQTB 2.6.1 Nghiờn cu ch to xỳc tỏc 51 51 2.6.2 Thc nghim phn ng alkyl húa benzene bng isopropanol s dng xỳc tỏc trờn c s cỏc vt liu zeolit Y cha MQTB 52 2.7 CC PHNG PHP C TRNG VT LIU NGHIấN CU 54 2.7.1 Phng phỏp nhiu x Rnghen 54 2.7.2 Phng phỏp hin vi in t quột 55 2.7.3 Phng phỏp hin vi in t truyn qua 55 2.7.4 Phng phỏp ph hp th hng ngoi 55 2.7.5 Phng phỏp ng nhit hp ph - nh hp ph Nit 55 2.7.6 Phng phỏp phõn tớch nhit 56 2.7.7 Phng phỏp kh hp ph Amoniac theo chng trỡnh nhit 56 2.7.8 Phõn tớch thnh phn húa hc 56 2.7.9 Xỏc nh tng dung lng trao i CEC 56 CHNG KT QU V THO LUN 58 3.1 KT QU X Lí NGUYấN LIU U 58 3.1.1 X lý cao lanh 58 3.1.2 X lý v tru 59 3.2 TNG HP NANO-ZEOLIT Y T CAO LANH BNG PHNG 60 PHP KT TINH MT BC, Cể MT CHT TO PHC HU C 3.2.1 Mt s yu t nh hng 60 3.2.2 c trng mu nano-zeolit NaY c tng hp t cao lanh iu 72 kin thớch hp 3.3 TNG HP MESO-ZEOLIT Y T CAO LANH BNG PHNG 78 PHP KT TINH HAI BC Cể MT CHT TO PHC HU C V CHT TO CU TRC MQTB 3.3.1 nh hng ca thnh phn v iu kin phn ng giai on mt 78 3.3.2 nh hng ca thnh phn v iu kin phn ng giai on hai 85 3.3.3 c trng mu meso-zeolit NaY c tng hp t cao lanh iu 90 kin thớch hp 3.4 TNG HP MESO-ZEOLIT Y T V TRU V CAO LANH 3.4.1 Mt s yu t nh hng 95 95 3.4.2 c trng mu meso-zeolit NaY c tng hp t v tru v cao lanh 100 iu kin thớch hp 3.5 TNG HP MSU-S(Y) T V TRU V CAO LANH 3.5.1 Mt s yu t nh hng 103 103 3.5.2 c trng vt liu MSU-S(Y) c tng hp t v tru v cao lanh 109 iu kin thớch hp 3.6 PHN NG ALKYL HểA BENZENE BNG ISOPROPANOL S 114 DUNG XC TC TRấN C S CC VT LIU ZEOLIT Y CHA MQTB 3.6.1 Ch to v c trng xỳc tỏc 114 3.6.2 Xac inh hot tớnh cua cac xỳc tỏc phan ng alkyl hoa benzene b ng isopropanol 118 3.6.3 Xỏc nh nhit phn ng i vi xỳc tỏc thớch hp 120 3.6.4 Xỏc nh thi gian phn ng i vi xỳc tỏc thớch hp 121 3.6.5 bn hot tớnh xỳc tỏc 122 3.6.6 ỏnh giỏ kt qu s dng xỳc tỏc ch to c phn ng alkyl húa benzene bng isopropanol iu ch cumene 123 KT LUN 129 IM MI CA LUN N 131 TI LIU THAM KHO 132 DANH MC CC CễNG TRèNH CễNG B CU A LUN AN 145 PH LC 146 DANH MC CH VIT TT V K HIU STT Kớ hiu Ting Anh Ting Vit ACAC Acetylacetone BEA CMT Critical Concentration CNTs Carbon nanotubes CTAB Cetyltrimethylammonium bromide DIPN diisopropylnaphtalene DIPB diisopropylbenzene DTA Differential Thermal Analysis Phng phỏp phõn tớch nhit vi sai DLS Dynamic Light Scattering Phng phỏp tỏn x lazer 10 EDTA Ethylenediamine tetraacetic acid 11 FAU Faujasite Zeolit ho Faujasit 12 FCC Fluid catalytic cracking Cracking xỳc tỏc tõ ng sụi 13 FTIR Fourier transform spectroscopy 14 GC/MS Gas Chromatography Spectometry 15 HexTEOS Hexadecyltriethoxysilane 16 HBM 17 ICPMS Inductively-Coupled Mass Spectrometry 18 IPA Isopropanol 19 IPB Isopropylbenzene 20 IR Infrared Hng ngoi 21 LTA Lipoteichoic acid Zeolit loa i LTA 22 MCF Mesostructured cellular foams Cu trỳc mao qun trung bỡnh dng bt 23 MKN 24 MQTB Zeolit loa i Beta Micellization Nng mixen ti hn ng nano cacbon infrared Phng phỏp ph hng ngoi bin i Fourier Mass Phõn tớch sc ký ghộp ph Hot ng b mt Plasma - Phng phỏp ph lng plasma cm ng Lng mu mt nung mesoporous Mao qun trung bỡnh Michigan State University Ho võ t liờ u MSU Trng i hc Bang Michigan -M phat minh 25 MSU 26 MSU-S Ho võ t liờ u MSU-S co mao quan trung binh va tng cha mõ m tinh thờ ho c tinh thờ zeolit 27 MSU-S(Y) Ho võ t liờ u MSU-S co mao quan trung binh va tng cha mõ m tinh thờ ho c tinh thờ zeolit Y 28 NMR Nuclear magnetic resonance 29 n-PB n-propylbenzene 30 SBU Secondary building unit n v cu trỳc th cp 31 SEM Scanning electron microscope Hin vi in t quột 32 TEA (Tri) Triethanolamine 33 TEAOH Tetraethylammonium hydroxide 34 TEM Transmission electron microscopy Hin vi in t truyn qua 35 TEOS Tetraethyl orthosilicate 36 TGA Therno Gravimetry Analysis 37 TIPB Triisopropyl benzene 38 TMA Trimethylamine 39 TMAOH Tetramethylammonium hydroxide 40 TMB 1,2,4 Trimethylbenzene 41 TMABr Tetramethylammonium bromide 42 TPA Tripropylamine 43 TPAOH Tetrapropylammonium hydroxide 44 TPD-NH3 Temperature-Programmed Desorption - NH3 Kh hp ph Amoniac theo chng trỡnh nhit 45 XRD X ray diffraction Nhiu x tia X (Nhiu x Rnghen) 46 ZSM-5 Zeolite Socony Mobil5 Zeolit ZSM-5 Phng phỏp phõn tớch ph cng hng t ht nhõn Phõn tich nhit trng lng DANH MC BNG BIU Tờn bng Trang Bng 1.1 Cu trỳc pha MQTB ph thuc vo g 31 Bng 1.2 Sn lng tru Vit Nam theo tng nm 37 Bang 1.3 Thanh phõ n cac nguyờn tụ vo trõ u (% lng) 38 Bang 1.4 Thanh phõ n hoa ho c mt sụ loa i vo trõ u (% lng) 38 Bng 3.1 Thnh phn hoỏ hc ca mu cao lanh s ch (Kao-SC), cao lanh ó x lý axit (Kao-AX) v Metacaolanh (Meta-Kao), % trng lng 58 Bng 3.2 Thnh phn hoỏ hc ca tro tru, % trng lng 59 Bng 3.3 nh hng ca hm lng kim n kớch thc tinh th nano-zeolit Y 60 Bng 3.4 nh hng ca hm lng silic n kớch thc tinh th nano-zeolit Y 66 Bng 3.5 nh hng ca thi gian gi húa n s kt tinh nano-zeolit Y 67 Bng 3.6 nh hng ca nhit kt tinh n quỏ trỡnh tng hp nano-zeolit Y 70 Bng 3.7 nh hng ca thi gian kt tinh n kớch thc tinh th nano-zeolit Y 71 Bng 3.8 So sỏnh c trng mu Nano-NaY, Nano-NaY [177] v Micro-NaY 76 Bng 3.9 Cỏc mu kho sỏt nh hng ca pH 88 Bng 3.10 Kt qu c trng mu meso-zeolit Y tng hp t cao lanh cú s dng CTAB 95 Bng 3.11 c trng cỏc mu vt liu trc v sau bin tớnh v dng axit 115 Bng 3.12 Kt qu TPD-NH3 ca Nano-HY, Meso1-HY, Meso2-HY v MSUHY 115 Bng 3.13 c trng cỏc mu xỳc tỏc trc v sau tỏch nhụm 116 Bng 3.14 Kt qu TPD-NH3 ca cỏc mu xỳc tỏc trc v sau tỏch nhụm 117 Bng 3.15 ỏnh giỏ hot tớnh ca cỏc xỳc tỏc phn ng alkyl húa benzene bng IPA 119 Bng 3.16 nh hng ca nhit phn ng trờn xỳc tỏc MSU-USY 121 Bng 3.17 nh hng ca thi gian phn ng trờn xỳc tỏc MSU-USY 122 Bng 3.18 bn hot tớnh ca xỳc tỏc MSU-USY 123 Bng 3.19 ỏnh giỏ kt qu s dng xỳc tỏc phn ng alkyl húa benzen bng IPA to sn phm cumen 127 132 TI LIU THAM KHO A Ti liu tham kho ting Vit: Bechechin A G (1962), Giỏo trỡnh khoỏng vt hc (Nguyn Vn Chin dch), NXB Giỏo dc, H Ni Dựng v tru sn xut pin in, bỏo Khoahoc.tv (http://khoahoc.tv/doisong/ moi-truong/giai-phap/48401_dung-vo-trau-de-san-xuat-pin-dien.aspx) o Vn Tng (2006) ng hc xỳc tỏc, NXB Khoa hc v K thut, H Ni ng ỡnh Bch, Nguyn Quang Tựng, Mai Tuyờn (2006), Ankyl húa toluen bng metanol trờn xỳc tỏc zeolit, Tp khoa hc v Cụng ngh, 44(2), 44-48 Xu n ng, Nguyn Th Thanh Loan, Nguyn Ngc Trỡu, V nh Tu n, Lờ Th Hoi Nam (2007), Nghiờn cu tng hp, c trng vt liu mao qun trung bỡnh Al -MSU v xỏc nh hot tớnh xỳc tỏc phn ng crackinh phõn t ln Phn Nghiờn cu tng hp, c trng vt liu mao qun trung bỡnh Al MSU, Tp Húa hc, 45(3), 294 - 298 H Th Lan Anh, T Ngc ụn (2011), nh hng ca cỏc cht to phc hu c v natri clorua n thi gian lm gi v thi gian kt tinh vt liu nano-zeolit NaX, Tp Húa hc, 49(5AB), 542-548 Hong Trng Mai (1970), Khoỏng vt hc, NXB i hc v THCN, H Ni H S Thong (1974), Nghiờn cu tớnh axit v hot tớnh xỳc tỏc ca cỏc zeolit cú hm lng SiO2 cao v cỏc cht xỳc tỏc cú cha zeolit, Lun ỏn tin s khoa hc húa hc (Bn dch ting Vit), Matxcva Hunh Quyn, Trung t m Nghiờn cu cụng ngh lc húa du Trng i hc 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zeolit NaY t cao lanh Vit Nam mụi trng kim Phn I Tng hp, c trng vt liu meso - zeolit NaY t cao lanh, nh hng ca thi gian kt tinh giai on mt v nh hng ca hm lng nc gel ban u, Tp Xỳc tỏc v Hp ph, 3(3), 51-58 T Ngc ụn, Lờ Vn Dng, T Ngc Hựng, T Ngc Thin Huy, Nguyn Th Xuõn, Nguyn Hu c, Nguyn c Ngha, Ninh Th Phng (2014), Chuyn húa thy nhit tro tru v metacaolanh thnh mesozeolit NaY, Tp Xỳc tỏc v Hp ph, 3(3), 59-63 Lờ Vn Dng, T Ngc Hựng, Nguyn Mnh Tun, Nguyn Th Phng Hũa, V Th Thu H, T Ngc ụn (2015) Tng hp vt liu meso-zeolit NaY t cao lanh: nh hng ca t l mol Na2O/Al2O3, CTAB/(Si+Al) v thi gian gi húa, Tp Húa hc, 53(4e2), 107-111 Lờ Vn Dng, Nguyn Th Phng Hũa, V Th Thu H, T Ngc ụn (2015), Tng hp meso-zeolit Y t cao lanh Vit Nam: nh hng ca pH v kh nng m rng mao qun trung bỡnh bng 1,2,4-trimetylbenzen, Tp Húa hc, 53(4e2),112-117 T Ngc ụn, Trnh Xuõn Bỏi, Lờ Vn Dng, T Ngc Hựng, Nguyn Mnh Cng, Trn Vn Hng, Nguyn Hu c (2015) Nghiờn cu tng hp vt liu MSU-S(Y) t tro tru v metacaolanh, Tp Xỳc tỏc v Hp ph, 4(3), 131-137 T Ngc ụn, Lờ Vn Dng, T Ngc Hựng (2016), Xỳc tỏc MSU-USY v MesoUSY t tro tru v metacao lanh phn ng alkyl húa benzen bng isopropanol, Tp Xỳc tỏc v Hp ph, 5(2), 40-46 ... ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI LÊ VĂN DƯƠNG NGHIÊN CỨU CHẾ TẠO XÚC TÁC ZEOLIT Y CHỨA MAO QUẢN TRUNG BÌNH TỪ NGUYÊN LIỆU TRONG NƯỚC ỨNG DỤNG TRONG PHẢN ỨNG ALKYL HÓA BENZENE BẰNG ISOPROPANOL. .. nguyên liệu đầu cao lanh vỏ trấu mẻ giới Trong luận án này, nghiên cứu chế tạo hệ xúc tác từ nguồn nguyên liệu vỏ trấu cao lanh nước, sử dụng làm xúc tác cho phản ứng alkyl hóa benzene nhằm tạo. .. TRÊN CƠ SỞ CÁC VẬT LIỆU ZEOLIT Y CHỨA MQTB 2.6.1 Nghiên cứu chế tạo xúc tác 51 51 2.6.2 Thực nghiệm phản ứng alkyl hóa benzene isopropanol sử dụng xúc tác sở vật liệu zeolit Y chứa MQTB 52 2.7