4.

LEVEL 4: SYNTHESIS OF CHEMICAL SEPARATION SYSTEM Basically, effluent from reactor consists of product, by-products and un-reacted reactants.

In order to obtain the product in desired purity and recycle un-reacted reactant, separation has to be carried out. There will be two different separation processes for methanol production from glycerol. The first separation process is the high pressure separator after reformer reactor to separate the syngas and water before the methanol synthesis section. Second is the distillation column to purify methanol as the final product. This will involve methanol-water separation. 4.1 High Pressure Separator

The separation of the water and gas phase after the reformer section was performed in a high pressure separator (HPS). The product from the reactor is vapor phase at high temperature and pressure, the stream then is cooled down just before the stream entering the separator. The liquid phase in the HPS consist water and can be recycled via a recycle pump. The gas phase from the HPS which is syngas was directly fed to the methanol synthesis section without upgrading or selective removal of components. It is assumed as 100% recovery of syngas as the feed to methanol reactor. Figure 4.1 below shows the arrangement of separation system in the high pressure separator.
Carbon monoxide(CO) Carbon dioxide(CO2) Hydrogen (H2)

Water(H2O)

Carbon monoxide(CO) Carbon dioxide(CO2) Hydrogen(H2) Gly cerol(C3H8O3) Water(H2O)

Glycerol(C3H8O3)
Water(H2O)

Gly cerol(C3H8O3)

Figure 4.1: Separation of syngas and water

4.11

Flash Calculation for Phase Separator

The calculation procedures are as follows: 1. Assume key component recovery,

k .
n k

2. Calculate Kk and Kn by using Antoine Equation (4.1) and Equation (4.2) and Equation (4.3) at known temperature T. 3. Calculate

using

n using Equation (4.4).

4. Recalculate mass balance and mole fraction of liquid outlet using Equations (4.5) and (4.6). 5. If the calculated pressure using bubble-point equation (4.7) equals to the operating pressure, then the solution is achieved. 6. If not, reassumed the recovery of key component and repeat the procedure. Component vapor pressure Pon can be calculated from Antoine Equation given by:
ln Pno An Bn T Cn

(4.1)

where An, Bn, and Cn are the Antoine constants and T is the temperature. Assuming ideal condition, then
Kn Pno P

(4.2)

The relative volatility can be written by:

n k

Kn Kk

(4.3)

The recovery of component n, is calculated using:

1 n k 1 k

n kk

(4.4)

The vapor and liquid streams are calculated from:

vn n f n

(4.5) (4.6)

ln 1 n fn

At the known temperature T, the bubble-point pressure can be calculated using:

o P T n k n

(4.7)

where

n k xn
4.12 Annual Cost of Phase Separator Annual cost of a phase separator in RM/year can be calculated by using the following formula: ( Where, D = Diameter of column L = Length of column Fm = Design materials factor Fp = Pressure factor FI = Installation factor = 1.5 IMSk = Recent Marshall and Swift index IMSd = Early Marshall and Swift index = 280 )* ( ) + (4.8)

4.2

Distillation Column

In general, distillation is the least expensive means of separating mixtures of liquids. The separation of liquids by distillation relies on relative volatilities of components. If the relative volatility is larger the separation process becomes easier.
For methanol-water mixture, methanol is the light key, while water is the heavy key. At atmospheric pressure (1 atm), methanol boils at 64.65C, and water boils at 100.00C. Thus, the distillation separation of methanol from water is not a difficult one.

Carbon monoxide(CO) Carbon dioxide(CO2) Hydrogen (H2)

Carbon monoxide(CO) Carbon dioxide(CO2) Hydrogen(H2) Methanol (CH3OH) Water(H2O)

Methanol (CH3OH) Water(H2O)

Figure 4.12: Distillation column 4.21 Sizing Distillation Column Determination of Minimum Number of Stages Using the specified flow of light key (LK) and heavy key (HK) component, the minimum number of stages of column is calculated by using the following formula:
[( )( )]

(4.9)

Where, d = distillate flow rate b = bottom flow rate = mean relative volatility = [(LK,HK)N(LK,HK)1]1/2 and Nactual = 2Nmin Height of column is calculated by the following equation: H = (0.69 Nactual)/Eo + 4 (4.10) (4.11) Where, Eo= plate efficiency

Nt - number of theoretical equilibrium stages, Na - actual number of stage required

Minimum and Actual Reflux Ratio Minimum reflux ratio is estimated by using Underwood Equation:
[ ( )]

(4.12)

And actual reflux ratio for all column is set to R=1.2Rmin. Theoretical and Actual Number of Stages The theoretical number of stages, N is calculated by using Gilliland correlation:

*(
Where,

)(

)+

(4.13)

(4.14)

Column diameter is determined by using the following equation:

(4.15)

The area of condenser is calculated by the following equation:

(4.16)

while area of reboiler is calculated by: (4.17)

Where, Hv = Enthalpy heat of vaporization Uc = Overall heat transfer coefficient for condenser. UR = Overall heat transfer coefficient for reboiler. 4.22 Annual Cost of Distillation Column Annual cost of a distillation column in RM/year can be calculated by using the following formula: ( Where, D = Diameter of column L = Length of column Fm = Design materials factor Fp = Pressure factor FI = Installation factor = 1.5 IMSk = Recent Marshall and Swift index IMSd = Early Marshall and Swift index = 280 )* ( ) ( )+ (4.18)

4.3 Economy Potential Analysis of Level 4 The economy potential for level 4 is given by fPE4=fPE3-Kmt1(S-01)-Kmt2(S-02)-Kmt3(C-01) Hence, the economy potential of level 4 is shown as following: (4.19)