DICP Course - Dalian, 2012 Preparation of solid catalysts Part 8 Supported by the Chinese Academy of Sciences
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1 DICP Course - Dalian, 2012 Preparation of solid catalysts Part 8 Supported by the Chinese Academy of Sciences Charles Kappenstein, Professor Emeritus, University of Poitiers, France Preparation of catalysts 8 Dalian, March-April /xx
2 Outline Introduction and general aspects Interfacial chemistry Electrostatic adsorption Impregnation, drying, calcination and/or reduction Sol-gel chemistry processing Deposition Precipitation and Coprecipitation Bimetallic catalysts Preparation of catalysts 8 Dalian, March-April /xx
3 Outline Shaping of solid catalysts Monolith-based catalysts Zeolite-based catalysts Ordered mesoporous materials Case studies: - Noble metal catalysts - Methanol catalysts - Hydrotreating catalysts - Preparation of catalysts 8 Dalian, March-April /xx
4 Zeolite-based catalysts 1) Introduction - hydrothermal synthesis 2) Acidity - zeolites - aluminophosphates Outline 3) Synthesis - overall steps in zeolite crystallization - model for zeolite growth - aluminophosphates Preparation of catalysts 8 Dalian, March-April /xx
5 Introduction Zeolite = "boiling stone" Definition: crystalline material with micropores and cation-exchange capacity, insoluble in water and with sufficient thermal stability About 200 different framework types Most important zeolites: - ultrastable Y (USY) (FAU = faujasite) - ZSM-5 (MFI), ZSM-35 (FER = ferrierite) (ZSM = Zeolite Socony Mobil) - mordenite (MOR) - zeolite omega (MAZ = mazzite) - SAPO-34 (CHA = chabazite) Applications: FCC: fluid catalytic cracking (particles µm) Hydro-isomerization, hydrocracking Preparation of catalysts 8 Dalian, March-April /xx
6 Introduction: hydrothermal synthesis Ex.: M I x [Al x Si y O 2(x+y )] zh 2 O Na 2 SiO 3 + NaOH + Al 2 (SO 4 ) 3 + C 3 H 7 -NH 2 + (C 3 H 7 ) 4 N + Br - + H 2 O 160 C, several days zeolites ZMS-5 Solvent: H 2 O Parameters: - Temperature: T > boiling temperature (up to 300 C) - Pressure: increase with temperature Ex.: water T / C P /bar (kitchen pressure cooker) use of autoclaves First autoclave: 1645, Papin s pot Preparation of catalysts 8 Dalian, March-April /xx
7 Introduction: hydrothermal synthesis Schematic representation of zeolite formation process, from reactants to final crystalline product. SDA = structure-directing agent (Handbook heterogeneous catalysis) Preparation of catalysts 8 Dalian, March-April /xx
8 Introduction: exemple of structure LTA framewotk Preparation of catalysts 8 Dalian, March-April /xx
9 Zeolite-based catalysts 1) Introduction - hydrothermal synthesis 2) Acidity - zeolites - aluminophosphates Outline 3) Synthesis - overall steps in zeolite crystallization - model for zeolite growth - aluminophosphates Preparation of catalysts 8 Dalian, March-April /xx
10 Acidity: zeolites Maximum number of protons (USY, ZSM-5 ) 0.2 till 1.2 mmol g -1 Depends on the Si/Al ratio Formal charge of the bridging oxygen atoms: Si-O-Si Si-OH-Si Si-O-Al Si-OH-Al Effect of structure on acid strength: Si-O-Al angle The higher the angle, the higher the acid strength of the proton Angle between 130 (medium Brönsted acidity) and 180 (strong Brönsted acidity) Acid strength is maximal at low Al concentration (high Si/Al ratio) isolated Al Acis strength is minimal at the highest Al concentration Preparation of catalysts 8 Dalian, March-April /xx
11 Acidity: aluminophosphates (AlPO 4 -n) P 5+ and Al 3+ cations alternate in T sites O-P-O-Al-O-P-O-Al-O no acidity Si substitution to P SiAlPO 4 (or SAPO) variable acid properties see figure Ex.: SAPO-37 (FAU) T-atom % Si 12.5 % Al 50 % P 37.5 % Environment: Si: 4 Al P: 4 Al Al: 3 P + 1 Si Preparation of catalysts 8 Dalian, March-April /xx
12 Zeolite-based catalysts 1) Introduction - hydrothermal synthesis 2) Acidity - zeolites - aluminophosphates Outline 3) Synthesis - overall steps in zeolite crystallization - model for zeolite growth - aluminophosphates Preparation of catalysts 8 Dalian, March-April /xx
13 Synthesis: overall steps in zeolite crystallization Hydrothermal conversion in supersaturated conditions Ex. sodium silicate Na 2 SiO 3 + sodium aluminate NaAl(OH) 4 + organic bases NR 4+ OH - M n x/n [Al x Si y O 2(x+y) ] zh 2 O Si/Al ratio adjustable low (close to 1) C high hydrothermal synthesis gels, C, autoclave M: column 1 or 2 Parameter: - Si/Al ratio - H 2 O/Si ratio - HO-/Si ratio - inorganic cations/si - organic additives/si templates - structure directing agent - structure determining effect Preparation of catalysts 8 Dalian, March-April /xx
14 Synthesis: overall steps in zeolite crystallization Ex.: synthesis of ZSM-5 TPABr = [(C 3 H 7 ) 4 N] + Br - TPEABr = [(CH 3 -C 3 H 7 ) 4 N] + Br - TPAOH = [(C 3 H 7 ) 4 N] + HO - Composition of the gel 4.38 (TPA) 2 O, 27.6 Na 2 O Al 2 O 3, 87.7 SiO 2, 3262 H 2 O Ion exchange with NH 4 NO 3 Drying, calcination 550 C Binding: binder alumina (50 wt.-%) + plasticizer (1 %) + peptizer (1 %) Forming by extrusion pellets C Perego, P. Villa, Catalysis Today 34 (1997) Preparation of catalysts 8 Dalian, March-April /xx
15 Synthesis: overall steps in zeolite crystallization Induction period Primary amorphous phase Local order via successive depolymerization/polymerization Secondary amorphous phase Scheme of equilibration and change of order during a zeolite synthesis Preparation of catalysts 8 Dalian, March-April /xx
16 Synthesis: model for zeolite growth Classical nucleation-crystallization theory Viable nucleus: between one and eigth unit cells Role of structure directing agents (SDA) Tetrapropylammonium ions (TPA, N(C 3 H 7 ) 4+ ) at interphase between aqueous and organosilicon (TEOS) phases. Silicate condenses around TPA ions Zeolitization parameters: composition, basicity (ph 9 to 13), presence of mineralizing agents and template molecules x SiO 2 : y Al 2 O 3 : z Na 2 O : u R : v H 2 O R = organic species Schematic representation of successive agglomerations of Si O intermediates synthesis of MFI structures, with nanoslabs as key intermediates Preparation of catalysts 8 Dalian, March-April /xx
17 Synthesis: model for zeolite growth Role of template (structure directing agent SDA) Influence zeolitization process SDA species surrounded by aluminosilicates in a particular geometry building units - Na + (aq) templates four-rings (4Rs). - TMA (tetramethyl ammonium) two 4Rs form D4R Si-rich of Al-rich zeolite A (LTA) Low Al content three 4R form D6R NaY zeolite high Al content and K + (aq) NaX zeolite - 18-crown-6 D6Rs EMT zeolite (in de Jong, 2009) Preparation of catalysts 8 Dalian, March-April /xx
18 Synthesis: AlPO4-n-based molecular sieve zeolites Phosphate source: phophoric acid H 3 PO 4 (pk a 2, 7, 12) ph 3 to 10 Al source: pseudoboehmite AlO(OH) nh 2 O Ex. Pr 3 N : Al 2 O 3 : P 2 O 5 : 40 H 2 O Acronyms and T atom composition of AlPO4-n-based molecular sieve zeolites. Acronym AlPO4-n SAPO-n MAPO-n MAPSO-n ElAPO ElAPSO T atoms Al, P Si, Al, P M (Co, Fe, Mg, Mn, Zn) M, Al, P, Si El (As, B, Be, Ga, Ge, Li, Ti) El, Al, P, Si Preparation of catalysts 8 Dalian, March-April /xx
19 Outline Shaping of solid catalysts Monolith-based catalysts Zeolite-based catalysts Ordered mesoporous materials Case studies: - Noble metal catalysts - Methanol catalysts - Hydrotreating catalysts - Preparation of catalysts 8 Dalian, March-April /xx
20 Outline Ordered mesoporous materials 1) Introduction 2) mesoporous silica - synthesis strategy - pore models - exemples - pore size control - functionalization 3) mesoporous carbon Preparation of catalysts 8 Dalian, March-April /xx
21 Introduction New class of porous solids with uniform pore size 1.5 to 40 nm, large surface area (up to 2500 m 2 g -1 ) and tunable structure Driving force self-assembly of molecules Weak bonds: van der Waals bonds, electrostatic bonds, hydrogen bonds, hydrophobic interactions, π-π stackings. Pore wall remain amorphous (mesoporous silica) 1-D porosity cylindrical channels 2-D porosity lamellar silica sheets 3-D porosity cubic structure, channels extending in 3 directions Synthesis - use of amphiphilic molecules (surfactants) Evolution of structure versus the surfactant concentration Figure Cmc = critical micelle concentration Preparation of catalysts 8 Dalian, March-April /xx
22 Introduction Evolution of structure versus surfactant concentration Cmc = critical micelle concentration Top to Bottom: Increasing concentration of surfactant forming a layer on the surface and forming micelles above the CMC The forming 1-D-tubes, 2-D bilayer and 3-D cubes Preparation of catalysts 8 Dalian, March-April /xx
23 Introduction: exemple of preparation (MCM-41) (i) Surfactant (cetyltrimethylammonium bromide, CTAB, (CH 3 ) 3 N(CH 2 ) 15 CH 3 Br) form liquid crystalline micelles in water (ii) Ceramic sol-gel precursor (tetraethoxysilane, TEOS, (C 2 H 5 O) 4 Si) is added silica network around the micelles upon hydrolyses and condensation (iii) Removal of the organic template by calcination or solvent extraction mesoporous ceramic material Preparation of catalysts 8 Dalian, March-April /xx
24 Outline Ordered mesoporous materials 1) Introduction 2) mesoporous silica - synthesis strategy - pore models - exemples - pore size control - functionalization 3) mesoporous carbon Preparation of catalysts 8 Dalian, March-April /xx
25 Mesoporous silica: synthetic strategy Route (a): cooperative self-assembly due to interaction between inorganic and organic species at the molecular scale 3D ordered arrangements. Route (b): true liquid-crystal template pathway forms 3D ordered arrangements, and then incorporates the inorganic precursors. Most of the mesostructure belong to hexagonal or cubic phases Preparation of catalysts 8 Dalian, March-April /xx
26 Mesoporous silica: pore models Pore models of mesostructures with symmetries of (a) p6mm, (b) Ia3d, (c) Pm3n, (d) Im3m, (e) Fd3m, and (f) Fm3m. Preparation of catalysts 8 Dalian, March-April /xx
27 Mesoporous silica: examples MCM-41 = Mobil Catalytic Material #41 Quaternary cationic surfactants [(CH 3 ) 3 NC n H 2n+1 ] + X - Cell parameters from XRD and TEM: about 4 nm Symmetry: P6mm Pore channel geometry: cylinders Pore wall thickness about 1 nm BET surface area > 1000 m 2 g -1 (n even, 8 to 16; X = Cl, Br) SBA-15 = Santa Barbara Amorphous #15 Symmetry: P6mm Prepared from P123 at C (triblock copolymer) Pluronic123 = HO(CH 2 CH 2 O) 20 (CH 2 CH(CH 3 )O) 70 (CH 2 CH 2 O) 20 H, Uniform pore size 6.5 to 10 nm Pore wall thickness 3.1 to 4.8 nm higher thermal stability MCM-48 Symmetry: Ia-3d Preparation of catalysts 8 Dalian, March-April /xx
28 Mesoporous silica: SBA-15 SBA-15 = Santa Barbara Amorphous #15 Left: representation of the pore topology, synthesis (a) between 35 C and 60 C; (b) at 100 C; and (c) at 130 C. pore size increases channels progressively interconnected Preparation of catalysts 8 Dalian, March-April /xx
29 Mesoporous silica: pore-size control Pore sizes of ordered silica mesostructures obtained by various methods. Pore size (nm) Method 2 5 Surfactants with different chain lengths 4 7 Long-chain quaternary cationic salts as surfactants High-temperature hydrothermal treatment 5 8 Charged surfactants with addition of organic swelling agents such as TMB and midchain amines 2 8 Nonionic surfactants 4 20 Triblock copolymer surfactants - Adding swelling agents expand pore sizes (ex.: dodecane, trimethyl benzene (TMB) - Hydrothermal treatment: pore size of SBA-15 can be tuned from 4.6 to 10 nm by increasing the temperature from 70 to 130 C Preparation of catalysts 8 Dalian, March-April /xx
30 Mesoporous silica: functionalization Schematic diagram for (a) Grafting (b) Co-condensation with surfactants Preparation of catalysts 8 Dalian, March-April /xx
31 Outline Ordered mesoporous materials 1) Introduction 2) mesoporous silica - synthesis strategy - pore models - exemples - pore size control - functionalization 3) mesoporous carbon Preparation of catalysts 8 Dalian, March-April /xx
32 Carbon: hard templating approach by nanocasting Ordered mesoporous silicates employed as templates for formation of other materials Precursor incorporated in the channels (impregnation, ion-exchange, adsorption;;;) Heat treatment precursors are decomposed, nanoparticles are formed and growth in the channels Mesoporous silica templates are dissolved Pore size distribution wider than the silica template Preparation of catalysts 8 Dalian, March-April /xx
33 End of part 8 Preparation of catalysts 8 Dalian, March-April /xx
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