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Transcript of Experimental Methods in Catalysis (EMC) M.Tech-Catalysis Technology II Semester CT-503...
![Page 1: Experimental Methods in Catalysis (EMC) M.Tech-Catalysis Technology II Semester CT-503 Dr.K.R.Krishnamurthy National Centre for Catalysis Research Indian.](https://reader036.fdocuments.in/reader036/viewer/2022062407/56649cb75503460f9497d1e8/html5/thumbnails/1.jpg)
Experimental Methods in Catalysis (EMC)
M.Tech-Catalysis Technology
II Semester
CT-503
Dr.K.R.Krishnamurthy
National Centre for Catalysis Research
Indian Institute of Technology
Chennai-600036
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Catalysts- FunctionalitiesCatalysts- Functionalities
BasicActivitySelectivityStability
AppliedManufacturingAgingDeactivationRegenerability
Evalua-tion
Character-izattion
Prepa-ration
CatalystDevelopment
Cycle
Why do we Characterize?Why do we Characterize? Provides answers to WHY & HOW Integral part of Catalyst development cycle
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Catalysts-CharacteristicsCatalysts-CharacteristicsChemical composition
Active elements, promoters, stabilizersStructural features
Crystalline/Amorphous, Crystal structurePhase composition, Phase transformations- TiO2—Anatase/Rutile
Surface PropertiesComposition, -Bulk Vs Surface, in-situ techniquesCo-ordination, Geometry/ Structure- Spectroscopic methods
Dispersion & distribution of active phasesConcentration profile, Crystallite size
Electronic propertiesRedox character, Chemisorption
Textural propertiesSurface area, Pore volume, Pore-size & distribution
Physical propertiesSize, Shape, Strength
Chemical properties Surface reactivity/Acidity/Basicity
Enabling Structure-Activity correlationsEnabling Structure-Activity correlations
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Catalysts- Shape factorCatalysts- Shape factor
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Catalysts- Shape effectCatalysts- Shape effect
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Characterization of CatalystsCharacterization of Catalysts
Preparation Characterization
Evaluation Ageing Spent
Concn. of active elements
Phase composition
In-situ Spectroscopy
Solid state transformations
Inactive
phases
Species in Solution phase
Electronic state Transient surface species
Structural transformations
Poisons
Solid state transformations
Structural features Reactants & Products
Surface composition
Analysis
of coke
Preparation techniques
Dispersion & Distribution
Kinetics & mechanism
Surface composition
Evolve active phase
Ensure desired characteristics
Surface reactions
Catalyst life Deactivation & Regeneration
Catalysts Characterization- From Cradle to Coffin
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Textural propertiesTextural properties
Catalysts Adsorbents
MetalsMetal oxidesMetal sulfidesMetal chloridesZeolitesHeteropoly acids
AluminaSilicaCarbonMol.sievesClays
Surface area
Pore structure
Pore size-Area-Volume-Distribution-Geometry
Textural propertiesTextural properties
Porous solids
External InternalGeometric shape/size
Porosity /Pores
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Textural properties- SignificanceTextural properties- Significance
Surface area/Pore volume - Dispersion of active phase
Pore size & distribution Molecular traffic-Diffusion of reactants & products
Heat & mass transfer
Diffusion rates- residence timeSelectivity
Extent of coking
Thermal & mechanical stability
Textural properties-Integral part of catalyst architectureTextural properties-Integral part of catalyst architecture
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Origin of poresOrigin of poresCrystal structure- Intrinsic voids
Atomic/molecular
Preparation- Voids due to leaving groupsHydroxides, carbonates, Oxalates- Ni(OH)2, MgCO3, ZnC2O4
Structural modifications-Intercalation/PillaringGraphite/ Clay
Aggregation/Coalescence- PreparationFormation of secondary particles from primary particlesFlexible pores- dispersion of particles
Agglomeration/Sintering- Pre-treatmentsRigid pores
CompactingShaping
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Origin of poresOrigin of pores
Pores Inherent in any solid structure
Intrinsic intra particle poresVoids created by specific arrangement of atoms / molecules- Zeolites- Cages & channels –Structurally intrinsic pores
Voids formed due to missing/removed molecules, atoms, particles- Dehydration of AlOOH to Al2O3
Removal of Na from Na silicate glass
Interstitial space between graphitic plates in CF
Extrinsic intra particle pores Voids created by removal of combustible additives- Addition of
surfactants-fillers in alumina precursor to increase pore volume/size
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Origin & types of poresOrigin & types of pores
K.Kaneko,J.Membrane Science, 96,59,1994
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Pore size % pore volume
% surface area
Micro 30 - 60 >95
Meso < 10 < 5
Macro 25 - 30 negligible
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Intrinsic pores in zeolitesIntrinsic pores in zeolites
ME Davis, Nature,412,813, (2002)
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Classification of poresClassification of pores
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Classification of poresClassification of pores
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Classification of poresClassification of pores
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Experimental techniquesExperimental techniques
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112/04/18 Aerosol & Particulate Research Lab
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Definition
The concentration of gases, liquids or dissolved substances (adsorbate) on the surface of solids (adsorbent)
Physical Adsorption (van der Waals adsorption): weak bonding of gas molecules to the solid; exothermic (~ 0.1 Kcal/mole); reversibleChemisorption: chemical bonding by reaction; exothermic (10 Kcal/mole); irreversible
Physical vs Chemical
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112/04/18 Aerosol & Particulate Research Lab
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Sorbent Materials• Activated Carbon• Activated Alumina
Air Pollution Engineering Manual., 1992
• Silica Gel
• Molecular Sieves (zeolite)
Polar and Non-polar adsorbents
Properties of Activated CarbonBulk Density 22-34 lb/ft3
Heat Capacity 0.27-0.36 BTU/lboFPore Volume 0.56-1.20 cm3/gSurface Area 600-1600 m2/gAverage Pore Diameter
15-25 Å
Regeneration Temperature (Steaming)
100-140 oC
Maximum Allowable Temperature
150 oC
http://www.activatedcarbonindia.com/activated_carbon.htm
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Adsorption Mechanism
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Measurement of Textural propertiesMeasurement of Textural properties• Adsorption isotherms- v = f (p/po)T
• Adsorbates – N2 Ar, Kr
• Methods – Volumetric – static/dynamic- Manual/automated
Gravimetric• Samples to be pre-treated to remove adsorbed impurities/moisture • Different molecules depending upon the size can be used as probes
to elucidate pore structure - Molecular resolution porosimetry • Isotherms/Isobars/Isosters – ( P,V,T)
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Measurement of adsorptionMeasurement of adsorption
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Types of adsorption isotherms -IUPACTypes of adsorption isotherms -IUPACReveal the type of pores & degree of adsorbate-adsorbent interactions
IUPAC classification – 6 types of isotherms
Type-I - Microporous solids Langmuir isothermType-II - Multilayer adsorption on non-porous / macroporous solidsType-III - Adsorption on non-porous /macro- porous solids with weak adsorptionType-IV - Adsorption on meso porous solids with hysteresis loopType-V - Same as IV type with weak adsorbate-adsorbent interactionType-VI - Stepped adsorption isotherm, on different faces of solid
Original classification by Brunauer covers upto Type-5
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Types of Isotherms - BrunauerTypes of Isotherms - Brunauer
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Origin of HysteresisOrigin of Hysteresis
• Normally observed in Type IV & V and sometimes in II &III• Absence of hysteresis- Type-I Micro porous structure
• At any given value for Va, p/p0 for in desorption branch is lower than that on adsorption
• Chemical potential of adsorbate during desorption is lower; hence true equilibrium exists
• Differences in contact angle during ads/des may lead to hysteresis• Presence of ink-bottle type pores-narrow neck & wide body. This
could mean that adsorption branch represents equilibrium• Differences in the shape of the meniscus in the case of cylindrical
pores with both ends open
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Types of hysteresis loops- de BoerTypes of hysteresis loops- de Boer
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Hysteresis Loops IUPACHysteresis Loops IUPAC
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Surface area by BET methodSurface area by BET method
p/v( p0-p) = 1/vmC + (C-1)p/ Cvmp0 - Plot of p/v(p0-p) Vs p/p0
P0- Sat. pressure; p- actual equilibrium Pressure; Vm-mono layer volumeV- adsorbed vol. at equilibrium pressure pC- constant signifying adsorbate-adsorbent extent of interaction
Applicable in the range p/p0- 0.05-0.35 & Only from Type II &IV isothermsSurface heterogeneity and interactions between adsorbates in adsorbed state are not accounted for
Slope + Intercept – 1/vm
Surface area = vmN Am/ 22414 x 10-20 m2
N- Avogadro’s number; Am-cross sectional area of adsorbate moleculeMono layer volume by Point B method in Type II isotherms
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Pore geometries- modelsPore geometries- models
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t- method of Lippens & deBoert- method of Lippens & deBoer
• Standard isotherms- Plot of Va/Vm Vs p/p0 gives a straight line
• t = 0.354( Va/Vm) = f1(p/p0) – for multilayer adsorption of nitrogen
t is independent of the nature of adsorbent if it is non-porous
• Plot of t Vs Va then passes through origin and the slope of the line can be used to calculate SA
• st = 1.547 x 106 dVa/dt with t expressed in nm
st Surface area by t-method
• As long as multilayer adsorption takes place, Va –t plot is a straight line passing through origin
• At higher t values deviations occur;
• Upward deviation – capillary condensation, cylindrical pores, ink-bottle type, spheroidal cavities
• Downward deviation- micro pores, with slit shaped geometry
• Higher the pressure at which deviation occurs, the larger the pore size
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ααss- method of Sing- method of Sing
• Comparison of experimental isotherm with that of standard one
• Thickness t replaced by a specific Va/Vm ratio for non-porous solid
• Ratio of volume adsorbed at specific p/p0 to volume adsorbed at p/p0 = 0.4 is designated as αs
• αs= Va/Vm = f(p/p0) ; αs= 1 at p/p0=0.4
• Basis - mono layer coverage completed and multilayer adsn. starts
at p/p0 = 0.4
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t - Plots for various pore size rangest - Plots for various pore size ranges
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Pore size distribution- BJH methodPore size distribution- BJH method• Based on Kelvin equation for capillary condensation for spherical
meniscus
• lnp/p0 = -2vλ Cosθ/ rkRT
– θ- contact angle
– λ- surface tension
– rk- Kelvin radius
– V-molar volumeWith θ =0, γ = 8.85.dynes/cm2 V= 34.6 cc/mole rk = 4.14/ln(p/p0)
• t = 3.5[5/ln(p/p0)]1/3
• Pore radius rp = rk+ t
rrpprrkk
tt
Model calculationsFor cylindrical pores - Gregg & Sing – p .164For parallel plates - RB Anderson - p.66
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Calculation of t, rCalculation of t, rkk & r & rpp
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dV = dvf +dvk
dVk= dV-dVf
dVf= 0.064xΔtx ∑dSp
dSp= 31.2 dVp/r*p
dVp= dVk(r*p/r*k)
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Micro porous solidsMicro porous solidsFollow Type I isotherm- Langmuir isotherm
Large uptake of adsorbate at very low pressures, up to p/p0=0.15
BET model applicable up to pores 1 nm
For <1nm Dubinin model applicable
Dubinin- Radushhkevich equation for micro porous solids
log10Va = log10V0 - D( log10X)2
Va- Vol adsorbed per unit mass of adsorbent
V0 – largest volume of adsorbate, total pore volume
X- p/p0 ; D- factor varying with temp & asorbent/adsorbate
Langmuir equation
1/n = 1/nm+ 1/(nmK) X 1/p/p0 n- moles adsorbed per gram of
adsorbent; nm- monolayer volume
Plot of 1/n .Vs. 1/p/p0 gives a straight line with intercept 1/nm
Surface area can be calculated from nm
Total pore volume from the uptake at horizontal plateau
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Mercury porosimetryMercury porosimetryIntrusion of mercury into the pores by applying pressure
rp= (2 γ/ P) cosθ - γ- Surface tension 480 dynes/ cm
θ - Contact angle, 141
rp = 7260/p with p-atmos. rp -nm
rp= 7x 10-4 cm = 70000Å ; 100Å – 700 atm.; 20Å- 3500 atm.
Pressure range – 0.1 to 400 KpaPore radius – 75000 to 18Å
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Pore structure Analysis - SummaryPore structure Analysis - Summary
Adsorption Isotherm
BET Plot
Isotherm Type
Pore size distribution
Hysteresis Type t-Curve
SurfaceSurface areaarea
Pore radius/Pore radius/Pore volumePore volume
Pore type, Shape, GeometryPore type, Shape, Geometry