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10.5.2017 1 Separation processes Separation processes Separation of heterogeneous and homogeneous mixtures of chemical compounds Based on different physically-chemical properties Commonly mixture of products (main and secondary) or mixture of product and unconverted reactants Mixture systems: heterogeneous homogeneous g – g g – g (gas mixture) g – l (fog, foam) g – l (gas solved in liquid) g – s (smoke) g – s l – l (emulsion) l – l (mixture liquids) l – s (slurry) l – s (solution) s – s s – s (metal alloy) Separation of heterogeneous mixtures When fluid phase is dominant (g, l), separation is based on: - different density (sedimentation) - flow of fluid thru porous separator (filtration, membrane separation) - ionization of particles (electrostatic precipitation) Small amount of liquid phase - vitalization (drying) System s – s - different density, magnet. properties (sedimentation) - different solubility (crystallization) - different wettability (flotation)

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  • 10.5.2017

    1

    Separation processes

    Separation processesSeparation of heterogeneous and homogeneous mixtures of chemical compoundsBased on different physically-chemical propertiesCommonly mixture of products (main and secondary) or mixture of product and unconverted reactants

    Mixture systems:heterogeneous homogeneous

    g – g g – g (gas mixture)

    g – l (fog, foam) g – l (gas solved in liquid)

    g – s (smoke) g – s

    l – l (emulsion) l – l (mixture liquids)

    l – s (slurry) l – s (solution)

    s – s s – s (metal alloy)

    Separation of heterogeneousmixtures

    When fluid phase is dominant (g, l), separation is based on:- different density (sedimentation)- flow of fluid thru porous separator (filtration, membrane separation)- ionization of particles (electrostatic precipitation)Small amount of liquid phase- vitalization (drying)System s – s- different density, magnet. properties (sedimentation)- different solubility (crystallization)- different wettability (flotation)

  • 10.5.2017

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    Separation of homogeneousmixtures

    Mixture of gases- sorption (absorption, adsorption)- different molecule diameter (membrane separation)Mixture of miscible liquids

    - liquids with different vapour preassure (destilation, rectification)- liquids with close vapour preassure (extraction)

    Non-volatile solids soluted in (evaporation and crystalization)- solubility is not dependent on temperature- solubility is strongly dependent on temperature

    Sedimentation (l-s, l-l, g-s, g-l, s-s)

    • rl is different than rs• gravitational acceleration

    • settling rate in gravity field =

    • possibility to separate particles with different diameter (trough separator)

    • possibility to separate particles with different density rs1> rl> rs2

    • Dorr sedimentation (l-s)

    Filtration (l-s, g-s)

    • porous separator – filter• proper pores diameter

    • cake / deep filtration• continuous / discontinuous filtration• driving force – pressure difference at front / behind filter

    • artificial (pressure/vacuum f.)• hydrostatic

    • resistance against filtration – viscosity of fluid, filter/f. cake pressure drop

    • pressure difference – stable / variable= filtration rate - variable / stable

    rotation vacuum cylinder filter, filter press, belt filter, candle filter, sand filter

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    centrifugation (l-s, l-l)

    • same principle as sedimentation (filtration)• centrifugal acceleration (3 orders of magnitude higher than g)

    • density difference can be only 1%• higher performance of device (mass flow)• continual / discontinual• centrifuges (sedimentation/filtration/separation)

    • cyclones, lamella separator

    Membrane separation (l)

    • analogy with filtration• selectivity on particle dimension basis (molecule mass)• „cross-flow“ / „death-end“ arrangement• retentate (rich solution) / permeate = filtrate (poor s.)• pressure processes

    • microfiltration (10-0,1 µm, up to 0,2MPa) – microorganisms, colloid particles• ultrafiltration (10-3 nm, 0,1-0,5 MPa) – macromolecules, viruses• nanofiltration (3-1 nm, 0,5-3,5 MPa) – pesticides, carbohydrates• reverse osmosis (1,5-15 MPa) – all dissolved salts

    • not only molecule sieve effect, but also selective interactions between particles and membrane (NF, RO)

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    Membrane separation - Filtration

    Electrostatic precipitation (g-s, g-l)

    • principle – ionization of particles (-) in strong DC electric field, migration to (+) electrode

    • negative electrode – wire in the middle • positive electrode – inner wall of precipitator• particles after discharge stay on (+) electrode (vibration)• up to 99.9% effectivity

    Drying (g-l, s-l)

    • flow of drying gas (little amount of vapors)• heat of vaporization• free / conventional drying – flow of heated gas• flows – parallel , counter or cross

    • static, sprinkled, linear, drifting

    • heatingconvectional, contact, radiant, electric, steam, ‘lyofilization’

    • important – relative humidity of gas is lower than dried material• dryers: spraying, rotary cylindric, fluid

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    h-xMolliérediagram

    Flotation (s-s)• one of most important separ. process• for ore processing• different interfacial parameters in three-phase system

    • wettability, production and carrying of bubbles• foam flotation – unwettable material form foam, wettable material

    sediment• additives (changing of surface properties)• electroflotation (electrolysis of water)

    Sodium Dodecylsulphatechem-physical parameters1) wettability2) density3) conductivity4) surface tension5) osmotic pressure6) eq. conductivity7) interphase tension

    Evaporation, crystalisation (l-s)

    • to separate nonvolatile solids solute in solvent• Increase of concentration above solubility

    • dependence of solubility on temperature• evaporation (vacuum)• change of T

    • particle properties• cooling rate, mixing

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    Distillation

    • for miscible liquids separation• vapors are rich for more volatile liquid

    • vapor composition is different than liquid• ideal mixtures – zoetrope mixtures (Raoult law small differences)• non ideal – azeotrope mixtures (interaction – H-bonds)

    • composition of azeotrope vapor is same as composition of liquid azeotrope• separation by distillation is not possible (can be done by pressure change,

    addition of third liquid)

    Rectification

    • multiple distillation with counter flow

    • number of theoretical stages• McCabe-Thiele method

    • columns – hat, mesh, packed

    p1: = + = ̇̇

    q: = − =

    q > 1 – feed is l at T < Tbpq = 1 – feed is l at Tbp0 < q < 1 – feed is mix of l and gq = 0 – feed is saturated vaporq < 0 – feed is superheated vapor

    Rectification stages/columns

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    Extraction (l-s, l-l)

    • separation of liquids with close boiling point• extractor ex

    • good slubility of one of the liquids l1 in ex (better than in l2)• non miscible with l2 (or partially miscible)• l1 and ex do not result to azeotrope

    • separation coeficient =

    • continual, discontinual, cascade• supercritic extraction (CO2, Tc=31 °C, pc=74 bar)• sepparation of ex and l2 (decanter) and destilation of l1 and ex

    Absorption (g-g)

    • sorption of one (or all except one) gas from the mixter in the liquid• physical and chemical• Henry law = • positive effect of low temperature and high pressure• difussion process – driving force: difference of concentration of A in

    gas and liquid is• important factorem is contact area of gas and liquid• columns like for rectification

    Adsorption (g-g, l-g, l-l)

    • for separation of homogeneous mixtures• sorption at solids with high specific surface (hundrets of m2/g)• selectivity can be affected by process parameters and by adsorbent

    type• positive effect of high pressure and lower temperature• physical ads. – low act. energy, exotermal, fast, multilayer, reversible• chemical ads. – higher act. energy, exothermal, slower, monolayer,

    only on active sites, selective, irreversible• adsorbers with fixed bed, fluid adsorbers