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    Crystallization PDF

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    Crystallization is a process where a saturated solution is cooled or evaporated to form crystals of the solute. [1] It is important industrially because crystals formed are pure even from an impure solution, providing a practical method to obtain pure chemicals. [2] Solubility, yield, purity, size, and shape of crystals are important factors. [3] Solubility depends mainly on temperature and is represented by a solubility curve.

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    Crystallization PDF

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    Crystallization is a process where a saturated solution is cooled or evaporated to form crystals of the solute. [1] It is important industrially because crystals formed are pure even from an impure solution, providing a practical method to obtain pure chemicals. [2] Solubility, yield, purity, size, and shape of crystals are important factors. [3] Solubility depends mainly on temperature and is represented by a solubility curve.

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    Crystallization is a process where a saturated solution is cooled or evaporated to form crystals of the solute. [1] It is important industrially because crystals formed are pure even from an impure solution, providing a practical method to obtain pure chemicals. [2] Solubility, yield, purity, size, and shape of crystals are important factors. [3] Solubility depends mainly on temperature and is represented by a solubility curve.

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    198 views9 pages

    Crystallization PDF

    Uploaded by

    only. star
    Crystallization is a process where a saturated solution is cooled or evaporated to form crystals of the solute. [1] It is important industrially because crystals formed are pure even from an impure solution, providing a practical method to obtain pure chemicals. [2] Solubility, yield, purity, size, and shape of crystals are important factors. [3] Solubility depends mainly on temperature and is represented by a solubility curve.

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    of 9

    CRYSTALLIZATION

    •  saturated solution cooled/evaporated forms crystal

    •  important industrially because:

    i) a crystal formed from an impure solution and itself pure

    ii) Practical method of obtaining pure chemical substances in a


    satisfactory condition for packaging and storing

    •  solid-liquid separation process

    •  yield , purity, sizes & shapes of crystals important

    •  crystals - uniform in size


    FKKKSA

    SOLUBILITY CURVE

    FKKKSA

    1
    SOLUBILITY CURVE

    •  equilibrium is attained when the solution or mother liquor is saturated


    (represented by solubility curve)

    •  solubility dependent mainly on temperature (pressure negligible effect)


    •  solubilities of most salts increase slightly or markedly with temperature

    Solubility curve for some typical salts in water Solubility curve for sodium thiosulfate

    FKKKSA

    SOLID-LIQUID PHASE DIAGRAM

    Solid-liquid phase diagram for the MgSO4-nH2O system at 1 atm

    FKKKSA

    2
    YIELD & HEAT & MATERIAL BALANCES
    •  yield of crystals can be calculated by knowing:
    initial concentration of solute
    final temperature
    solubility at this temperature
    •  material balances Mass balance :
    kg H2O evaporate
    Water balance : Input = Output
    Solute balance : Input = Output
    F kg Hot solution S kg solution

    X1 kg solute/ X2 kg solute/
    100 kg H2O 100 kg H2O

    C kg Crystal
    solute crystals are anhydrous - simple water & solute material balances
    crystals are hydrated - some water in the solution is removed with crystals
    FKKKSA

    EXAMPLE 12.11-1

    A salt solution weighing 10 000 kg with 30 wt % Na2CO3 is cooled to 293K (20oC). The salt
    crystallized as the decahydrate. What will be the yield of Na2CO3.10H2O crystals if the
    solubility is 21.5 kg anhydrous Na2CO3/100 kg of total water?

    a) Assume that no water evaporated.

    b)  Assume that 3% of the total weight of the solution is lost by evaporation of water in
    cooling.
    Ans: 6370 kg, 6630 kg

    FKKKSA

    3
    EXAMPLE 12.11-1
    Solution:    
    Molecular weights: Na2CO3 = 106.0, 10H2O = 180.2, Na2CO3 •10H2O = 286.2

    (a)  W = 0, water balance:

    Na2CO3 balance:

    C = 6370 kg of Na2CO3 •10H2O crystals and S = 3630 kg solution


    (b) W = 0.03(10000) = 300 kg, water balance:

    C = 6630 kg of Na2CO3 •10H2O crystals and S = 3070 kg solution.


    FKKKSA

     
     
    EXAMPLE 27.1(McCabe,   Smith & Harriott)
    A solution consisting of 30 wt% MgSO   4 is cooled to 60oF. During cooling, 5 %
     
    of the total water in the system evaporates. How kg of crystals are obtained per
    1000 kg of original mixture?
    Data: Molecular weight of MgSO4 = 120.4
    Ans: 261 kg

    FKKKSA

    4
    EXAMPLE (P12.11-3)

    A hot solution containing 1000 kg of MgSO4 and water having a concentration


    of 30 wt% MgSO4 is cooled to 288.8 K (60oF) where crystals of MgSO4.7H2O
    are precipitated. The solubility at 288.8 K is 24.5 wt % anhydrous MgSO4 in
    the solution. Calculate the yield of crystals obtained if 5 % of the original
    water in the system evaporates on cooling.
    Data: Molecular weight of MgSO4 = 120.4
    Ans: 261 kg

    FKKKSA

    HEAT BALANCES IN CRYSTALLIZATION


    normally, crystallization is exothermic W kg H2O
    HV kJ/kg

    F kg Hot solution S kg solution

    hF kJ/kg hS kJ/kg

    Total heat absorbed, q (kJ): C kg Crystal


    hC kJ/kg
    When Tdatum = 32oF ,
    FhF + q = (S + C)hM + WHV
    or
    FhF + q = ShS + ChC + WHV
    When Tdatum = Tequil./sat. , FhF + q = Wλ + ChC = Wλ + CΔH∞crys
    #
    heat of crystallization, ΔHcrys = - heat of solution at infinite dilution, "H
    soln
    Heat absorbed, q = + ve ,Heat given off , q = - ve

    FKKKSA !

    5
    ENTHALPY-CONCENTRATION DIAGRAM

    Enthalpy-concentration diagram for the MgSO4-


    nH2O system at 1 atm
    FKKKSA

    ENTHALPY-CONCENTRATION DIAGRAM

    FKKKSA

    6
    EXAMPLE

    A 32.5% solution of MgSO4 at 120oF


    (48.9oC) is cooled, without appreciable
    evaporation to 70oF (21.1oC) in a batch-
    cooled crystallizer. How much heat must be
    removed from the solution per 100 Ib of the
    feed solution? The average heat capacity of
    the feed solution is 0.72 Btu/Ib oF and the
    heat of solution at 18oC is 23.2 Btu/Ib of
    MgSO4.7H20.
    Ans: -4260 Btu

    Enthalpy-concentration diagram for the MgSO4-


    nH2O system at 1 atm
    FKKKSA

    EXAMPLE 12.11-2

    A feed solution of 2268 kg at 327.6 K


    (54.4oC) containing 48.2 kg MgSO4/100
    kg total water is cooled to 293.2 K (20oC)
    where MgSO4.7H2O crystals are removed.
    The solubility of the salt is 35.5 kg
    MgSO4/100 kg total water. The average
    heat capacity of the feed solution can be
    assumed as 2.93 kJ/kg.K. The heat of
    solution at 291.2 K (18oC) is 13.31 x 103
    kJ/kg mol MgSO4.7H2O. Calculate the
    yield of crystals and make a heat balance
    to determine the total heat evolved and
    removed from the crystalliser, q,
    assuming that no water is vaporized.
    Data: Molecular weight of MgSO4•7H20
    is 246.49
    Ans: 616.9 kg crystal, -261 912 kJ
    Enthalpy-concentration diagram for the MgSO4-
    nH2O system at 1 atm
    FKKKSA

    7
    EXAMPLE 12.11-2
    Solution:    
    Molecular weights: MgSO4 = 120.4, 7H2O = 126, MgSO4 •7H2O = 246.4

    2268 kg S kg solution
    48.2 kg MgSO4/100 kg H2O 35.5 kg MgSO4/100 kg H2O

    C kg MgSO4 •7H2O

    ! 100 $ ! 100 $ ! 126 $


    W = 0, water balance: 2268 # &= S# &+C# &
    " 48.2 +100 % " 35.5+100 % " 246.4 %

    ! 48.2 $ ! 35.5 $ ! 120.4 $


    MgSO4 balance: 2268 # &= S# &+C# &
    " 48.2 +100 % " 35.5+100 % " 246.4 %

    Total balance: 2268 = C + S

    C = 631.9 kg MgSO4•7H2O crystals, S = 1636.1 kg solution.


    FKKKSA

     
     
     
     
     
    EXAMPLE 12.11

    Solu&on  
    Tref. = 293.2K (Tdatum)
    Heat balance :
    FhF + q = Wλ + ChC = Wλ + CΔH∞crys
    Enthalpy of the feed , hF = CpΔT = (2.93)(327.6-293)

    Heat of solution = 13.31x103/246.49 = 54.0 kJ/kg crystals.


    Heat of crystallization = -(54.0) = -54.0 kJ/kg crystals
    Total heat absorbed, q
    2268(2.93)(327.6-293) + q = 631.9(54.0)
    q = 631.9(54.0) - 2268(2.93)(327.6-293) = -262 689 kJ

    FKKKSA

    8
    EXAMPLE

    A solution of 500 kg of Na2SO4 in 2500 kg water is cooled from 333K to 283K in


    an agitated mild steel vessel. At 283K, the solubility of the anhydrous salt is 8.9
    kg/100kg water and the stable crystalline phase is Na2SO4.10H2O. At 291K, the
    heat of solution is -78.5 MJ/kmol and the specific heat capacity of the solution is
    3.6 kJ/kg.K. If, during cooling, 2% of the water initially present is lost by
    evaporation, estimate the heat which must be removed.
    Ans: 240 407 kJ

    FKKKSA

    CRYSTALLIZER

    FKKKSA

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