Production of Diethyl Ethere
Production of Diethyl Ethere
Engineering College
           Chemical Engineering Department
                           2021-2022
CHAPTER
1 INTRODUCTION 5
                                                                                                                        |Page2
      2          MATERIAL BALANCE                                                          16
3 ENERGY BALANCE 41
                                                                                    |Page3
        4        CHEMICAL DESIGN                                                            71
REFRENCES 163
                                                                                      |Page4
 CHAPTER I
INTRODUCTION
               |Page5
1.1 INTRODUCTION
Diethyl ether is a colorless, highly volatile flammable liquid and organic
compound. Diethyl ether is also called ethoxyethane, ethyl ether, sulfuric ether,
or ether. It is part of the ether class, meaning it contains an ether group or an
oxygen atom connected to two alkyl or aryl groups. The general formula for the
ether group is R-O-R. Ethers are typical in organic and biochemistry, because
they are common links in carbohydrates and lignin. Technical-grade ether and
anesthetic ether are the two grades available for commercial use. Technical-grade
ether standardly does not contain peroxides, though no worldwide parameters
exist. Anesthetic diethyl ether must pass the tests for aldehydes and peroxides,
have a natural reaction, contain no foreign odors, and have a water content of
0.2% or below.
                                                                         |Page6
1.2 PHYSICAL PROPERTIES OF DIETHYL ETHER –
(C2H5)2O:
             TABLE (1.1) : physical properties of D.E.E
Property Value
Color Colorless
                                                                 |Page7
                      TABLE(1.2): physical properties
                                                                        |Page8
        form                                        Liquid
       color                                        max. 10
  Specific Gravity                     0.714 (20/4℃) ; 0.712 (25℃)
  Relative polarity                                   2.9
        Odor                    Pungent odor detectable at 0.33 ppm
   explosive limit                                1.7-36%(V)
  Water Solubility                               69 g/L (20 ºC)
   FreezingPoint                                   -116.3℃
       Merck                                        14,3806
                                  -4         3
Henry's Law Constant   12.50(x 10 atm?m /mol at 25 °C) (Signer et al., 1969)
   Exposure limits        TLV-TWA 1200 mg/m3 (400 ppm) (ACGIH and
                          OSHA); STEL 1500 mg/m3 (500 ppm) (ACGIH).
      Stability:       Stable, but light-sensitive, sensitive to air. May contain
                       BHT (2,6-di-tert-butyl-4-methylphenol) as a stabilizer.
                           Substances to be avoided include zinc, halogens,
                        halogen-halogen compounds, nonmetals, nonmetallic
                       oxyhalides, strong oxidizing agents, chromyl chloride,
                          turpentine oils, turps substitutes, nitrates, metallic
                                            chlorides. Extre
                                                                     |Page9
1.4 USES OF DIETHYL ETHER
1.Diethyl ether is a common laboratory solvent. It has limited solubility in water
(6.05 g/100 mL at 25°C) and dissolves in 1.5 g/100 mL of water at 25°C.
Therefore, it is commonly used for liquid liquid extraction. When used with an
aqueous solution, the organic layer is on top because diethyl ether has a density
lower than that of water. . It is also a common solvent for the Grignard reaction
as well as other reactions involving organometallic reagents.
3.It is a good solvent or extractant for fats, waxes, oils, perfumes, resins, dyes, .
gums and alkaloids.
4.When mixed with ethanol, ethyl ether becomes an excellent solvent for
cellulose nitrate in the manufacture of guncotton (see Explosives and propellants)
collodion solutions (see Membrane technology), and pyroxylin plastics (see
Cellulose derivatives, esters).
5.Another important use is as an extractant for acetic acid as well as other organic
acids, eg, in the cellulose acetate (qv) and plastic industries to recover acetic acid
from dilute aqueous systems.
7.It has been used as a starting fuel for diesel engines and as an entrainer for
dehydration of ethanol and isopropyl alcohol.
8.It may be used as an anhydrous, inert reaction medium for the Grignard and
Wurtz-Fittig reactions.
                                                                             | P a g e 01
1.5 PRODUCTION
Most diethyl ether is produced as a byproduct of the vapor-phase hydration of
ethylene to make ethanol. This process uses solid-supported phosphoric acid
catalysts and can be adjusted to make more ether if the need arises. Vapor-phase
dehydration of ethanol over some alumina catalysts can give diethyl ether yields
of up to 95%.
This reaction must be carried out at temperatures lower than 150 °C in order to
ensure that an elimination product (ethylene) is not a product of the reaction. At
higher temperatures, ethanol will dehydrate to form ethylene. The reaction to
make diethyl ether is reversible, so eventually an equilibrium between reactants
and products is achieved. Getting a good yield of ether requires that ether be
distilled out of the reaction mixture before it reverts to ethanol, taking advantage
of Le Chatelier's principle.
Another reaction that can be used for the preparation of ethers is the Williamson
ether synthesis, in which an alkoxide (produced by dissolving an alkali metal in
the alcohol to be used) performs a nucleophilic substitution upon an alkyl halide.
                                                                           | P a g e 00
Figure 1.1 unit 1200 diethyl ether process
                                             | P a g e 02
TABLE(1.4) : united states production and price of ETHYL ETHER, 1940_1977
1. Halogenation:
 When diethyl ether treated with Cl2 or Br2 in the dark, substitution product are
obtained. The extent of substitution depends upon the reaction condition.
Halogenations preferentially take place at ά- carbon atoms.
                                                                         | P a g e 03
2. Formation of peroxide:
3. Combustion:
Diethyl ether
                                                           | P a g e 04
1.7 EFFECTS OF DIETHYL ETHER
Health Effects
diethyl ether is a severe eye and moderate skin irritant. Irregular breathing,
hypothermia, and bradycardia have been noted as early effects in industrial
exposures. Excessive salivation has been reported. Prolonged exposure to high
vapor concentrations may cause eye injury. Exhaustion, dizziness, excitation,
headache, CNS depression, and seizures have occurred.
High exposure can cause unconsciousness and even death. High exposure may
affect the kidneys. Repeated or prolonged skin contact can cause drying, scaling
and cracking of the skin. Diethyl Ether is a highly flammable liquid and a serious
fire hazard.
Diethyl ether is highly flammable (NFPA rating = 4) and is one of the most
dangerous common fire hazards in the laboratory, due to its volatility and
extremely low ignition temperature. Ether vapor can be ignited by hot surfaces
such as hot plates and static electricity discharge, and since vapor is heavier than
air, it may travel a great distance to the source of ignition and flash back. Ether
vapor forms an explosive mixture with air in concentrations from 1.9 to 36% (by
volume). Carbon dioxide or dry chemical extinguishers should be used for ether
fires. Diethyl ether forms unstable peroxides upon exposure to air in a reaction
enhanced by light; The presence of these peroxides may cause an explosive
residue upon distillation.
Behavior in Fire: Steam is heavier than air and may travel a great distance to the
source of ignition and flash back. It decomposes violently when heated.
                                                                           | P a g e 05
               Chapter II
       MATERIAL BALANCE
                                             | P a g e 06
2.1 MASS BALANCE AROUND REACTOR (R-1201)
Selectivity = 80
X = 0.8
Input Output
2 3
FA°? FA ?
FB°? FB+FD1+FD2 ?
FC1-FC2 ?
FF ?
( )
                                                              | P a g e 07
  Abbreviations used in the reactor:
Basis:
Feed:70% ethanol
30% water
The productivity of the project was determined diethyl ether is 25000 ton/year
FC=FA°(𝜃c + )
FB°= mole/sec
                                                                          | P a g e 08
                               (       )
C 2F + D
                   (       )
Selectivity =          (       )
C D + 2F
1 1 2
? ? 0.1478
2X = 0.1478
X(FD) = = 0.0739mole/sec
X(FC) = = 0.0739mole/sec
                                                                       | P a g e 09
INPUT :
Sum=1590.5
OUTPUT :
Sum=1590.5
                                                                     | P a g e 21
2.2 MASS BALANCE AROUND FLASH VESSEL ( V-1202 )
                                     Yi
                          4
                                             Ethylene
Water
D.E.E
                                            Ethanol
             3
Zi
                           5
                          Xi
Water
Ethanol
Ethylene
D.E.E
                                                | P a g e 20
Assume      ℃
     Component     A               B             C
     Ethanol       16.8958         3795.17       230.918
     Ethylene      6.74756         585           255
     D.E.E         14.0735         2511.29       231.200
     Water         16.3872         3885.70       230.170
                             ( )
                                             ℃
                                                       | P a g e 22
10.489*0.171+109.39*2.60*    +86.406*0.547 + 4.271*0.27 =
= 50.495 Kpa
Assume ℃
      Component        A               B                C
      Ethanol          16.8958         3795.17          230.918
      Ethylene         6.74756         585              255
      D.E.E            14.0735         2511.29          231.200
      Water            16.3872         3885.70          230.170
                                                              | P a g e 23
                                            ℃
29.517*0.171+125.085*2.6* +171.057*0.547+12.403*0.27=
                                                          | P a g e 24
- Assume ( 0.002 ) from D.E.E , ethanol and water out with ethylene from the top
- Assume ( 0.001 ) from ethylene out with D.E.E and water from the bottom
Input
= 272.48
= 871.288
= 442.611
= 4.145
SUM.= 1590.5
Top product
( )
SUM.=7.3134
                                                                       | P a g e 25
Bottom product
SUM.=1583.2099
                                          Output
                  input
                                                                  Output
                 Steam
                                           Steam                     Steam
                  3
                                            4                         5
            Mass flow     Molar flow   Mass flow    Molar flow   Mass flow       Molar
Component   rate g/sec       rate      rate g/sec      rate      rate g/sec    flow rate
                           mol/sec                   mole/sec                   mol/sec
  D.E.E      871.288       11.7550      1.7425        0.0235      869.545       11.7315
                                                                              | P a g e 26
   2.3 MASS BALANCE AROUND DISTILATION ( T_1201)
                                             Ethylene
                           6
                                               D.E.E
Water
Ethanol
Ethylene
Ethanol
D.E.E
Water
           5
Ethylene
Water
D.E.E
Ethanol
                                             | P a g e 27
(The feed)
FDEE =
= 11.7316
Fwater =
= 24.5266 mole/sec
Fethanol =
= 5.9026
Fethylene =
= 1.4777 mole/sec
∑= 42.1610 mole/sec
Composition:-
XDEE = 0.2782
Xwater = 0.5817
Xethanol = 0.1400
Xethylene = 3.5048
∑= 0.9999
                                      | P a g e 28
TBP = ∑ Xi * TBPi
TBP = 78.5334 C
TBP = 351.5334 K
ᶯDEE = 0.99 =
DDEE = 0.99 * 11.7316 = 11.6142 mole/sec
ᶯWater = 0.01 =
Dwater = 0.01 * 24.5267 = 0.2452 mole/sec
                                  (    )
                                                     ℃
                                                                   | P a g e 29
      (        )
( )
( )
                              (                   )
                          (                       )
Nm = 4.2
                   (                      )
ᶯethanol =
              ( (                         )           )
              (                   )
ᶯethanol =    ((                  )           )
                                                          = 0.2464
                       (                      )
ᶯethylene =
               ( (                            )           )
                  (                   )
ᶯethylene =    ((                     )           )
                                                              = 0.6109
                                                                         | P a g e 31
(THE TOP PRODUCT)
∑= 13.3138 mole/sec
Composition:-
XDEE = 0.8723
Xwater = 0.0184
Xethanol = 0.1092
Xethylene = 6.7803 *
∑= 0.9999
                                               | P a g e 30
)THE BOTTOM PRODUCT)
W=F–D
∑= 28.8471 mole/sec
Composition:-
XDEE = 4.0697 *
Xwater = 0.8417
Xethanol = 0.1541
Xethylene = 3.03*
∑= 0.9999
                                                             | P a g e 32
  TABLE (2.5) : SUMMARY OF MATERIAL BALANCE OF DISTILATION
                           COLUMN
  Sum
            1583.2087                                         1583.2234
                                                                          | P a g e 33
2.4 MASS BALANCE AROUND DISTILATION( T-1202 )
D.E.E
Ethanol
Ethylene
Water
D.E.E
Ethanol 7
Ethylene
Water
D.E.E
Ethanol
Ethylene
Water
                                                | P a g e 34
 )(The feed
FDEE = 0.1174
Fwater = 24.2815
Fethanol = 4.4482
Fethylene = 5.7498
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
∑= 28.8471
Composition:-
XDEE = 4.0697
Xwater = 0.8417
Xethanol = 0.1541
Xethylene = 1.9931
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
∑= 0.9999
TBP = ∑ Xi * TBPi
                                                                                                           | P a g e 35
ᶯethanol = 0.99 =
Dethanol = 0.99 * 4.4482 = 4.4037 mole/sec
ᶯWater = 0.01 =
Dwater = 0.01 * 24.2815 = 0.2428 mole/sec
( )
 -The volatility of ethylene is calculated from the scheme used for flash process
thermodynamic:
                                                                         | P a g e 36
       (              )
( )
( )
                                      (           )
                              (                   )
Nm = 11.389
ᶯDEE =
                  (           )
( ( ) )
ᶯDEE =     (
              (
                          )
                                          )
                                                  = 0.9999
ᶯEthylene =
                      (               )
( ( ) )
ᶯDEE =     (
              (
                          )
                                          )
                                                  =1
                                                             | P a g e 37
))THE TOP PRODUCT
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
Composition:-
XDEE = 0.0246
Xwater = 0.0509
Xethanol = 0.9243
Xethylene = 1.2069
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
∑= 0.9998
                                                                                                                                            | P a g e 38
)) THE BOTTOM PRODUCT
W=F–D
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
Composition:-
XDEE = 4.1522
Xwater = 0.9981
Xethanol = 1.8477
Xethylene = 0
ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ
∑= 0.9999
                                                                                                                                            | P a g e 39
  TABLE (2.6) : SUMMARY OF MATERIAL BALANCE OF DISTILATION
                           COLUMN
                                                                           | P a g e 41
            CHAPTER III
        ENERGY BALANCE
                                            | P a g e 40
GENERAL EQUATION FOR ENERGY
CONSERVATION
Ĥ=∫
H=n∫
CP = A + BT + C D +E (for gas)
H= ( −          𝑓) + /2 ( −        𝑓 ) + /3 (      −       𝑓 ) + /4 (    −     𝑓
)+ /5 ( −        𝑓 )     (for gas)
      Component         A           B             C              D          E
         DEE          35.979     2.8444 *     -1.2673 *      -1.0128 *   3.4529 *
                                                                         | P a g e 42
CP = A + BT + C      +D             (for liquid)
H= ( − 𝑓) + /2 ( − 𝑓 ) + /3 ( − 𝑓 )
+ /4 ( − 𝑓 ) (for liquid)
         Component            A                 B               C          D
           DEE              75.939           7.7335 *        -2.7936    4.4383 *
                                                             *
           Ethanol          59.342           3.6358 *       -1.2164 *   1.8030 *
           Water
          Ethylene          25.597           5.7078 *       -3.3620 *   8.4120 *
ΔH = ∑Hout -
T : temperature, k
                                                                        | P a g e 43
3.1 ENERGY BALANCE AROUND OF FEED DRUM ( V-1201 )
              =298 k
                          1
v-1201
         29
         99
                                         2              =?
                                         2
   =116.1499 k
                                                             | P a g e 44
               TABLE (3.3) : Energy Flow on Streams (1) and (29)
                            Stream1                         Stream29
    Stream         n                     H         N                          H
  component     (mol/sec)   (J/mol)   (J/sec)   (mol/sec)    (J/mol)       (J/sec)
T3 = 336.5 K = 63.5 °C
                                                                          | P a g e 45
3.2 ENERGY BALANCE AROUND OF FEED HEATER
( E-1201)
2 3
Q = ΔH = ∑H3 - ∑H2
            Stream2                                     Stream3
   N                             H           N                              H
(mol/sec)    (J/mol)          (J/sec)     (mol/sec)     (J/mol)          (J/sec)
     0        ..........         0            0          ...........         0
 29.5725    4230.9331       125119.2691    29.5725    11659.74486       344807.805
  12.673    2897.0454       36714.25635    12.673      5188.1268       65749.13094
     0       ............        0            0          ...........         0
 42.2455    7127.9785       161833.5255    42.2455    16847.87166      410556.9359
Q = ΔH = ∑H3 - ∑H2
Q = 410556.9359 – 161833.5255
Q = 2487723.4104 J/sec
                                                                           | P a g e 46
   3.3 ENERGY BALANCE AROUND OF REACTER( R-1201 )
𝛥 298 = ∑ⱱ𝛥
ⱱ = Stoichiometric Coefficient.
                                            | P a g e 47
                TABLE (3.5) : heat of formation of components
(Ethanol) (DEE)
(DEE) )ethylene)
                                                                 | P a g e 48
                     TABLE (3.6) : Energy Flow on Streams (3)
            Stream                 N                                  H
           Component            (mol/sec)         (J/mol)          (J/sec)
               DEE                  0             ............        0
             Ethanol             29.5725        11659.74486      344807.805
              Water               12.673         5188.1268       65749.13094
             Ethylene               0             ............        0
              Total              42.2455                         410556.9359
T4 = 410.6 K = 137.6 °C
                                                                     | P a g e 49
 3.4 ENERGY BALANCE AROUND OF EFFLUENT COOLER
                                   ( E-1202 )
4 5
                         Stream4                            Stream5
              n                         H          n                      H
 Component (mol/sec)     (J/mol)     (J/sec)    (mol/sec)    )J/mol(    )J/sec(
Q = 69077.6205 – 319603.4108
Q = - 250525.7903 ⁄
                                                                        | P a g e 51
3.5 ENERGY BALANCE AROUND OF FLASH SEPRTER
                  ( V-1202 )
          5       V-12023
          5
( )
( )
                                       | P a g e 50
            TABLE (3.8) : Energy Flow on Streams (6) and (7)
Stream 6 Stream 7
               N            H                       N            H
Component
            (mol/sec)     (J/sec)     (J/mol)    (mol/sec)     (J/sec)       (J/mol)
                                                                     | P a g e 52
    3.6 ENERGY BALANCE AROUND OF DEE COLUMN (T-1201)
66
99
ا
                                              | P a g e 53
          Component           Α
                  DEE         2.2544           0.2782         0.8723
               Ethanol        0.5800          0.14000         0.1092
                Water         0.2534            0.5817         0.0184
              Ethylene        0.8426      3.5048*        6.7803*
q at boiling point =1
Rmin + 1 =
R = 3*Rmin =0.806001
                                                                  | P a g e 54
From volume 6 , chapter 11 ,figure (11.11)
N=6.176
                                              | P a g e 55
        3.7 ENERGY BALANCE AROUND OF DEE CONDENSER
                                  (E-1203)
E-1203
14 15
Cw
Component Α
                                                                 | P a g e 56
Composition and Amount (TOP) :-
 T bubble
̅ ∑
Log =A -
Log (1454.58)=6.96559 -
=53.9959 C֩
                                                               | P a g e 57
     T dew
* +
= 255.503 kpa
= 63.166 C֩
Q=V ( )
Component             Cp
Dee                   1031.9465
Ethanol               704.4715
Water                 817.0099
Ethylene              450.9329
∫ =A+BT+C +D
CP= ( ) + /2 ( ) + /3 ( ) + D/4 ( )
Q = 121138.7441 J/sec
                                                            | P a g e 58
3.8 ENERGY BALANCE AROUND OF DEE REBOILER (E-1204)
E-1204
10 11
Component α
                                                                  | P a g e 59
Composition and Amount (Bottom) :-
 T bubble
̅ ∑
Ln =A -
Ln (1066.90)=18.3036 -
=109.94 C֩
                                                            | P a g e 61
      T dew
* +
=628.0762 kpa
Ln =A -
= 113.32 C֩
Q=V ( )
Component             Cp
Dee                   228.4193
Ethanol               137.1547
Water                 112.6949
Ethylene              112.4969
∫ =A+BT+C +D +E
Q =11401.8068 J/sec
                                                                 | P a g e 60
3.9 ENERGY BALANCE AROUND OF ETHANOL COLUMN
                    (T-1202)
19
                                      | P a g e 62
  Component             Α
           DEE          2.2544   4.0697*              0.0246
       Ethanol          0.5800        0.1541          0.9243
        Water           0.2534        0.8417          0.0509
      Ethylene          0.8426   1.9931*         1.2069*
q at boiling point =1
Rmin + 1 =
Rmin+1 = 5.70912
Rmin= 4.70912
R = 3*Rmin =14.12736
                                                               | P a g e 63
From volume 6 ,chapter 11 ,figure (11.11)
N=14.9855
                                               | P a g e 64
3.10 ENERGY BALANCE AROUND OF ETHANOL
CONDENSER (E-1206)
E-1206
24 25
Component α
                                        0.9243
 Ethanol     1.13620           1
 Ethylene      46                       2.98104*
                            40.4858
                                                         | P a g e 65
Composition and Amount (TOP) :-
 T bubble
̅ ∑
Log =A -
Log (1283.9153)=7.68117 -
=92.11 C֩
                                                               | P a g e 66
     T dew
* +
= 183.1227 kpa
Log (1373.8721)=7.68117 -
= 93.9942 C֩
Q=V ( )
Component            Cp
Dee                  239.8349
Ethanol              158.4497
Water                163.8101
Ethylene             106.2838
∫ =A+BT+C +D
CP= ( ) + /2 ( ) + /3 ( ) + D/4 ( )
Q = 123357.6881 J/sec
                                                             | P a g e 67
3.11 ENERGY BALANCE AROUND OF ETHANOL REBOILER
                     (E-1207)
E-1207
20 21
Component Α
                                                          | P a g e 68
Composition and Amount (Bottom) :-
 T bubble
̅ ∑
Ln =A -
Ln (1309.7883)=18.3036 -
= 116.149 C֩
                                                              | P a g e 69
      T dew
* +
=174.81178 kpa
Ln =A -
= 116.043 C֩
Q=V ( )
Component               Cp
Dee                     729.61
Ethanol                 420.018
Water                   353.31
Ethylene                362.63
∫ =A+BT+C +D +E
Q = 16523.8364 J/sec
                                                                     | P a g e 71
  CHAPTER IV
CHEMICAL DESIGN
                  | P a g e 70
4.1 CHEMICAL Design of Heat Exchanger (E_-1201)
The temperature inlet in the shell side is 63. 5°C and the outlet temperature is
177°C.
The temperature of the heat exchanger tube inlet is 200°C and the outlet
temperature is 150°C.
The pressure equals to 10bar.
The flow is counter current.
             (            ) (       )
                      (         )
                      (         )
             (            ) (           )
                                        =50°C
    (             )
     (           )
     (           )
    (            )
         (       )         (        )
         (        )        (        )
                                                                          | P a g e 72
Figure 4-1 Correction-factor plot for exchanger with one shell pass and two, four,
or any multiple of tube passes.(Reference: Holman , Heat Transfer 10th edition
By using the values of P and R through the above figure the value of correction
factor is obtained.
                                                                        | P a g e 73
Assuming the overall heat transfer coefficient equals 500 by using Table
12.1
Where:
Select :
                     Tube length            16 ft   4.83 m
                     Tube out side diameter 20 mm   0.02 m
                     Tube thickness         16 mm   0.016 m
                                                                   | P a g e 74
_The recommend tube pitch distance between
( )
K1=0.319,n1=2.142
( )
Where:
Clearnace=61mm
Ds=527+61=588mm
                                                        | P a g e 75
Tube_side coefficient:
Mean water temperature =         ℃
Where:
   ∶ ℎ       𝑢𝑏
         ∶        𝑓
203428.57
( )
                                     | P a g e 76
                                (       )
( )
( ) )
( )
                                                        | P a g e 77
                     ρ(   ) Cp(J/kg °C(         μ (pa.s)   K(w/m. °C(
Cptotal=4251*0.3+3482*0.7=3712.7J/kg. °C
μ total=0.000229*0.3+0.0002*0.7=2.087
Ktotal =0.684*0.3+0.123*0.7=0.29 w/m. °c
Re=
Re= 60827.98
Hs=ho= ( )
ho=3303.7(w/m.°C(
Checking:
Hod=5000,Hid=3000 from table (12.2) volume6
From table (12.6)for steel kw=35w/   . °C
                                                                        | P a g e 78
overall heat transfer coefficient based on the outside area of the tube.
                      (   )
       ℃
                                             ℃
   ∶                                         ℃
   ∶                           (                 )       ℃ )
           ∶                             ℃
       ∶                                                           ℃
  ∶
   ∶
                                             (                 )       (
           )
Uo=500.638
[ ( )( ) ]
Where
                                                                           | P a g e 79
                        (   )
[( ( ) ) ]
                                            | P a g e 81
Pressure drop of shell side
                                                𝑢
                                    (   )( )         (   )
                                          𝑏
Where
L = tube length=4.83mm ,
De=14.2mm
= baffle spacing .
For Re = 60827.98
Number of baffles ( )
                                                             | P a g e 80
Summary
                         Tube length       4.83 m
                      Tube thickness     0.016 m
             Shell inlet temperature        63.5C
            Shell outlet temperature         177C
           Tube inlet temperature            200C
            Tube outlet temperature          150C
                    Number of tubes            353
                    Bundle diameter      527 mm
                   Number of baffles      196mm
                  Overall coefficient          500
          Pressure drop of tube side    17.66 psi
          Pressure drop of shell side    25.6 psi
                      Shell diameter          14.2
                                              mm
                                                     | P a g e 82
4.2 CHEMICAL DESIGN OF REACTOR :
                                   | P a g e 83
Conditions                                 Value
Inlet Temperature (K)                       450
Inlet Pressure (kpa)                       1200
Outlet Temperature (k)                     410.6
Outlet pressure (kpa)                      1200
Molar flow rate (A)                       29.5725
(mole/sec)
Other information
Type of Reactor                      Packed bed rector
operating condition                  Adiabatic reactor
Density of catalyst                       3950
(Kg/m3)
E                                           0.5
                (        )
ethanol         diethyl ether
A            1/2 C +         1/2 D
θA = 1 , θc = 0 , 𝜃d =
Fc = 11.829 mole/sec
FC=FA°(θc + 1/2 X)
                                                         | P a g e 84
PA = Pt * y
              °(          )
PA = Pt *
              (           )
PA = 840 (1-x)
              (               )
Pc = Pt *         (           )
Pc = 420.168 x
              °(                  )
PD = Pt *         (           )
              (                       )
PD = 1200 *
PD = 359.663 + 420.168x
                      (               )
Ethanol               diethyl ether
ΔHr = ∑(n ΔHf)product - (n ΔHf)react
ΔHr(298) = (1 * -241.8) + (1 * -252.7)⦌ - (2 * -234.81)⦌
ΔHr(298) = - 24.88 KJ/mole = - 24880 J/mole
                                                             | P a g e 85
Substance                                                   Cpi (J/Kmol . K)
    A                    1             27.091+1.1055*10-1T + 1.0957*
                                       10-4T2 - 1.5046 *10-7T3 + 4.6601 * 10^-11
                                       T4
    C                    0             35.979 + 2.8444 * 10^-1 T- 1.2673 * 10^-6
                                       T^2 – 1.0128 * 10^-7 T^3 + 3.4529*10^-11
                                       T^4
    D            0.428                 33.933 – 8.4186 * 10^-3T + 2.9906 * 10^-5
                                       T^2 – 1.7825 * 10^-8T^3 + 3.6934 *10^-12
                                       T^4
                 °(              )                      (   )                 °(           )
CPmix = CPA *
                                                    (           )
                                                                  + CPD *          (   )
                     (           )
                 (           )                  (   )                 (            )
CPmix = CPA *                               (           )
                                                          + CPD *         (    )
                 (           )
CPmix(average) = =
                                                                                               | P a g e 86
        ∫
∫ 𝑓( ) (𝑓 𝑓 𝑓 𝑓 )
∫ 𝑓( )
Weight of catalyst
W=V*d
W = 6.196 * 3950
W = 24474.2 kg
Volume of reactor =
                      (   )
Vr =
             (   )
Vr = 12.392
                                          | P a g e 87
12.392 =        * 4D
12.392 = 3.14
L = 4 * 1.580
L = 6.32 m
Summary of Reactor :
   Catalyst volume      6.196 m3
    Catalyst weight    24474.2 kg
    Reactor volume     12.392 m3
   Reactor diameter     2.451 m
    Reactor Length      1.634 m
                                    | P a g e 88
4.3_ CHEMICAL DESIGN OF HEAT EXCHANGER (E_1202)
E_1202
                                                                        | P a g e 89
Where
              (                )           (       )
                           (                   )
                           (                   )
         (         ) (             )
                                                   ℃
= 0.8667
= 0.15366
                                                       | P a g e 91
* From figure 4.1 : F = 0.91
fig. 4.1 . temperature correction factor; one shell pass; two or more tube pass
Select :
                                                                                              | P a g e 90
      𝑢 𝑓                𝑓        𝑢𝑏 ( )
𝑢 𝑏 𝑓 𝑢𝑏 ( )
𝑏𝑢 ( ) ( )
( )
                                                                 | P a g e 92
* Bundle diameter clearance = 77.9
𝑏 𝑓𝑓 ( )
                                      | P a g e 93
Tube side coefficient ( )
ρ ⁄
𝑢𝑏
𝑢𝑏
𝑢𝑏 𝑢𝑏
𝑢 ⁄
                                          | P a g e 94
𝑢
                         | P a g e 95
                                                       (       )
Where
𝑓 𝑓
𝑢 𝑓 𝑢𝑏 𝑓𝑢
𝑓 𝑓𝑢 𝑢
[ ]
( )
( )
= 1.5905 kg
Cp = 1835.7118 J/Kg.K
                                                                         | P a g e 96
    K = 0.02286 w/m.℃
( )
( )
( )
                                                        | P a g e 97
Overall coefficient U
( )
Where
U = the overall coefficient based on the out side area of the tube ℃
℃ ℃
                                                                     | P a g e 98
Pressure drop of tube side
                                                             𝑢
                                 [   ( )(      )         ]
Where
𝑢𝑏 𝑢 ( )
𝑢 𝑏 𝑓 𝑢𝑏
𝑢 𝑢𝑏
𝑓 𝑢𝑏
                                                                 | P a g e 99
             [(                          ( )    )           ]
                                                    𝑢
                                     (   )( )           (       )
                                           𝑏
Where
L = tube length ,
= baffle spacing .
For Re = 50525.95078
                                                                    | P a g e 011
Number of baffles   ( )
                          | P a g e 010
Summary
                                                           | P a g e 012
4.4 CHEMICAL DESIGN OF ETHANOL COLUMN (T-1202):
                       4.70912
                       11.389
             Ø         0.953
             R         14.12736
                       72.05917
                       67.2956
                       72.0594
                       96.1427
                       0.8248
0.9338
0.76
N 14.9855
                                          | P a g e 013
Cloumn diameter :
Top section
FLV= √
Vapor density: =
              =(74.12*0.0246)+(46.07*0.9243)+(18*0.0509)+(28*1.2069*       )
=45.25g/mol
=2.61 kg/
                                                                 | P a g e 014
           (     )
ρl=A*
SO
FLV= √ =0.048 
( -0.047) *√
=0.87 m/s
                                                                        | P a g e 015
           From figure 11.27 find value of K1.
K1 = 0.08
√ =0.855 m
Bottom section
FLV= √ 
Vapor density: =
                                                                   | P a g e 016
                                                 ℃
=2.11 kg/
         (      )
ρl=A*
comp                    Ρl(kg/m^3)                   Xw
Diethyl ether           583                          4.1522*
H2O                     939.257                      0.9981
ethanol                 691.10                       1.8477*
ethylene                259.4                        0
SO
FLV= √ =0.063 
( -0.047) *√
                                                               | P a g e 017
           From figure 11.27 find value of K1
K1 =0.088
√ =0.998m
Plates efficiency :
(∑
𝑓 ∶
component
DEE                         0.126               4.0697*10^-3
ethylene                    0.0057              1.9931*10^-6
Ethylene                    0.36                0.1541
Water                       0.29                0.8417
( )=0.50 
                                                               | P a g e 018
          Column High
                𝑓
                    𝑓      𝑢
0.5=
Column diameter
Column Area ( )=
= ( )
=0.77
At 12 percent of area 
=0.0924
                                                           | P a g e 019
      Weir length:
(Ad/Ac) *100%= 12
Lw=0.99*0.76=0.7524m
Take Hd=5mm 
Plate thickness=55mm 
                                   | P a g e 001
Take weir hight =50mm=hw 
Cheek weeping :
=0.482 kg/s
=750( )
                                                          | P a g e 000
K2 = constant = 32 figure 11.30
           (      )
Ûh =                  = 9.39m/s
                                                                  | P a g e 002
plate pressure drop :
                                                                | P a g e 003
The pressure drop through the dry plate can be estimated using an expression ;
=30.67+(50+5.78)+12.67
=30.67+55.78+12.67
=99.12mm liquid
hap=50 – 10 = 40 mm
= 0.0474mm
=0.155m
So:
 ( plate spacing + weir height )
=1/2(0.5+(50*10^-3))
                                                                      | P a g e 004
=0.275
Tr=
 Check entrainment:
For FLV=0.063
 Trail Layout:
50 mm
                    0.7524                                   0.99 m
                                         Өc
                        m
                              50 mm
                                                                         | P a g e 005
perforated area
                                                                   | P a g e 006
-area of calming zones= 2( 0.714×0.05) =0.0714 m2
 Number of holes:
Number of holes =
                                                      | P a g e 007
   CHAPTER V
MECHANICAL DESIGN
                    | P a g e 008
5.1 MECHANICAL DESIGN OF HEAT EXCHANGER (E_1201)
                     Condition
                     Operating pressure     10 bar
                     Material               Stainless steel
                     Density of material    7800     ⁄
                     Shell temperature               ℃
                     Tube temperature       200_150 ℃
                     Corrosion allowance    2 mm
                     Shell diameter         588 mm
                     Number of tubes        353
                     Insulation thickness   75 mm
Pi=1.2N/m
Determining        ℎ
Choosing Tori spherical
( )
                                                              | P a g e 009
      (          √   )
.771
( )
t=4.361 hv=4.83m
                         (H       )
                              (       )
3.549kN
= 3.05kN
                                          | P a g e 021
Determining Weight of insulation
=2.2
= 2.9000kN
Double=2.9000*2=5.8KN
Total weight
Shell                  3.549
Insulation             5.8
Pipes                  3.05
Total                  12.399
                    (H              )
                   (            )
                                        | P a g e 020
            (H       )
Where
         ℎ 𝑏                         𝑏
Analysis of stresses
                                         .
( ) ( )
( )
( )
                                                 | P a g e 022
       (          )
( )
( ) ( ) ⁄
The maximum compressive stress will occur when the vessel is not under
pressure .
                                                                     | P a g e 023
Support design
Choose saddle support must be designed to withstand the load imposed by the
weight of the vessel and content . they are constructed of bricks or concrete, or
are fabricated from steel plate . the contact angle should not be less than 120° ,
and will not normally be greater than 150° . wear plates are often welded to the
shell wall to reinforce the wall over the area of contact with the saddle .
The dimensions of typical "standard" saddle designs are given in figure 13.26
chemical engineering Vol.6 page 847.
Choose the design that fit that diameter frim fig 13.26.
                                                                         | P a g e 024
Flange design
Where:
                 𝑓    𝑏
                          | P a g e 025
2-For shell inlet:
        ℃.
  (        )
( )
                     | P a g e 026
4-For tube outlet:
T=150
( )
Summary
              Shell thickness          4.361 mm
              Head thickness           6.139mm
              Total weight             12.399kN
              Loading                  854.222 N/m
              Pressure stress          40.449 ⁄
              Pressure stress          80.898 ⁄
              Dead weight stress       0.00152 ⁄
              Bending stress           0.0083 ⁄
                (𝑢         )           40.456 ⁄
                (             )        -40.438 ⁄
                                                     | P a g e 027
5.2_ MECHANICAL DESIGN OF REACTOR :
            Condition
            Operating Pressure (bar)              12
            Material                              Carbon Steel
            Catalyst weight, kg                   24474.2
            Operating Temperature c               137-177
            Diameter, m                           1.58
            Height, m                             6.32
            Insulation thickness, mm              75
                                       (      )
                       ethanol             diethyl ether
Elliposoidal head
                                                                 | P a g e 028
Dead weight
Take =1.08
     =   +e
Dm =1.58 + 1(0 * 10^-3) = 1.59
𝑊v=240        (       +0.8       )
                         (                )
Wv =36288.7577 N = 36.2887 KN
Weight of insulation:
mineral wool density = 130 kg/m3
𝑊         𝑓       𝑢          =                𝑢    9.81
     𝑢   of insulation =
     𝑢   of insulation = 3.14 * 1.58 * 6.32 * 75 * 10^-3 = 2.35 m^3
𝑊e        𝑓       𝑢          = 130 * 2.35 * 9.81
𝑊         𝑓       𝑢          = 2996.955 N = 2.996 KN
Double this to allow for fitting = 2.996 * 2 = 5.992 KN
Wt = 𝑊 +𝑊
Wind loading
Take dynamic wind pressure as 1280 N/m2.
Mean diameter, including insulation                (      + 75) 0.001= 1 75
( )
                                                                   | P a g e 029
Analysis of stresses
( ) ( )
Bending stresses:
Do = Di + 2t
    0=1.58 *
         (                )       (           )
            (         )
    𝑏                         (           )
= + ∓ 𝑏
                                                      | P a g e 031
The greatest difference between the principal stresses will be on the
down-wind side
95.59 – 43.7556 = 51.8344 N/
well below the maximum allowable design stress
F = 115 N/mm^2
Skirt high = hs = 3 m
Skirt thickness = ts = 10 mm
Weigt of skirt
Approximate weight = H
                                                                | P a g e 030
Analysis of stresses of skirt .
          (      )
                             =   (       )
( ) ( )
operation = ( ) ( )
Maximum , ( )
Maximum , ( )
Maximum ( )
Maximum ( )
                                                         | P a g e 032
5 - Criteria for design
                                                                   | P a g e 033
          , 𝑏=                      ⦌
, 𝑏= ⦌
Ab = 90 mm^2
Use M24 bolts (BS 4190:1967) root area = 353 mm^2 (from figure 11.30
volume 6) (page – 849)
𝑏= ⦌
Where, Fb = the compressive load on the base ring, Newtons per linear
metre      Ds = skirt diameter, m
Where,
This is the minimum width required; actual width will depend on the
=chair design. Actual width required ( figure 13.30 v6 ) .
Lr + ts + 50 mm
= 76+12+50= 138 mm
                                                               | P a g e 034
            Actual bearing pressure on concrete foundation:
√ ---------- ref 7
    Lr = the distance from the edge of the skirt to the outer edge of the
     ring, mm.
    tb = base ring thickness, mm.
    f’c = actual bearing pressure on base, N/mm^2 .
    fr = allowable design stress in the ring material, typically 140
     N/mm^2.
      tb = 76 √          = 7.8 mm
      round off to 8 mm
The chair dimensions from figure 13.30 for bolt size M24.
                                                                | P a g e 035
  Flange Design
  For input steam at T = 450 k
  From material balance :
      =         ƒ            = 1.59 /s
Calculate =
  Material
      Ethanol            1.25             0.857             46.07           1.07
      Watwr             0.488             0.143             18.02         0.0698
       Total                                                                         =
                                                                            1.14
= 296
                                                                          | P a g e 036
                                  d1=323.9
d2=22
                                                       12
                                                                           h=44
                                                                    b=22
                                                             3
                                   d3=355
                                   d4=365
                                   K=395
                                   D=440
Calculate =
Material
     DEE                   2.20               0.548         74.12                 1.21
    ethanol                1.37               0.171         46.07                 0.234
    water                  0.535              0.278         18.02                 0.149
   ethylene                0.833             0.00261        28.05            2.17 * 10^-3
     total                                   ∑x=1                                     = 1.60
                                                                           | P a g e 037
  For carbon steel
       = 282 × (G)0.52 × (ρ) −0.37
       = 282 × (1.59)0.52 × (1.60) −0.37
       = 268
d1=273
d2=18
                                               12
                                                                 h=44
                                                          b=22
                                                     3
                            d3=295
                            d4=312
                            K=335
                            D=375
                                                                      | P a g e 038
Summary
Shell thickness           10        mm
Total weight              42.2807   KN
Loading fw                2240      N/m
Pressure stress   L       47.795
Pressure stress   H       95.59
Dead weight stress w      1.74
Bending stresses      b   2.2749
 z (upwind)               48.3344
 z (downwind)             43.7556
                                          | P a g e 039
5.3 MECHANICAL DESIGN OF HEAT EXCHANGER
(E_1202)
              Condition
              Operating pressure          10 bar
              Material                    Stainless steel
              Density of material         7800     ⁄
              Shell temperature           40 - 137.6 ℃
              Tube temperature            25 – 40 ℃
              Corrosion allowance         2 mm
              Shell diameter              947.0034 mm
              Number of tubes             1028.454
              Insulation thickness        75 mm
𝑏 ⁄
𝑓 ⁄
Shell thickness ( e ) ( )
Head thickness
   Elliposoidal
                                                              | P a g e 041
Dead weight of vessel
 Take Cv = 1.08
𝑊 ( )
𝑊 ( )
Weight of pipes
𝑊 𝑓
Weight of insulation
Weight of insulation 𝑓 𝑢
                                                             | P a g e 040
Total weight
Shell 75.2352
Pipe 8.9002
Insulation 2.7487
86.8841 KN
Wind loading
Mean diameter ( )
Mean diameter ( )
Analysis of stress
                                                             | P a g e 042
Dead weight stress
( )
                                        ⁄
       (                     )
Bending stress
( )
( )
( )
( ) ⁄
(𝑢 ) ⁄
( ) ⁄
                                                                 | P a g e 043
Check elastic stability (buckling)
Critical buckling stress:
( ) ( ) ⁄
The maximum compressive stress will occur when the vessel is not under
pressure .
                                                                  | P a g e 044
Support design
Choose saddle support must be designed to withstand the load imposed
by the weight of the vessel and content . they are constructed of bricks or
concrete, or are fabricated from steel plate . the contact angle should not
be less than 120° , and will not normally be greater than 150° . wear
plates are often welded to the shell wall to reinforce the wall over the area
of contact with the saddle .
 Choose the design that fit that diameter from fig 13.26.
                                                                  | P a g e 045
Flange design
   For stainless steel
Where
𝑓 ⁄
℃ ⁄
                                      | P a g e 046
 for out put gases from shell at :
       ℃                           ⁄
℃ ⁄
℃ ⁄
                                          | P a g e 047
Summary
    Shell thickness      6.00480 mm
    Head thickness       6 mm
    Total weight         86.8841KN
    Loading              1315. 84 N/m
    Pressure stress      47.35017 ⁄
    Pressure stress      94.70034 ⁄
    Dead weight stress   0.8112 ⁄
    Bending stress       3.6094 ⁄
      (𝑢         )       50.1483 ⁄
      (             )    42.9295 ⁄
                                        | P a g e 048
5.4_ MECHANICAL DESIGN OF ETHANOL COLUMN (T-
1202) :
Head thickness
Choose elipsoidal head :
3 mm
Supports:
Weight loads:
CV = constant = 1.15
                                                                 | P a g e 049
HV = height or length of shell m = 7.8 m
t = e= 3 mm shell thickness
Dm = Di + (t × 10-3) --------(ref 7)
Hv=16.5
Plates
WP = 1.2 Ac N
Weight of insulation:
W = v*g*ρ
W = 4946.8887N = 4.946 KN .
                                                                | P a g e 051
Wind load
Dm = 998+2(3+75) = 1154mm=1.154m
Analysis of stresses
Pressure stresses:
( ) ------------ ref 7
        (           )
                                         ( compressive) .
                                                                 | P a g e 050
Bending stresses
∓ ( ) ------------(ref 7)
Iv ( )= ----------- (ref 7 ).
∓ ( ) ∓
∓ 𝑏
( )
= 10.673-3.4837= 7.1893N/mm^2
( ) ( )
                                                             | P a g e 052
The maximum compressive stress will occur when the vessel is not under
pressure .
F 126 N/mm^2
Skirt high = hs = 4 m
Skirt thickness = ts = 9 mm
Weigt of skirt
Approximate weight =                          l
                     =                                    = 119909 N
Wapprox              = 119.9 KN.
                                                                  | P a g e 053
2-bending stress of skirt ,
            (        )
                                  =        (           )
( ) ( )
operation = ( ) ( )
Maximum , ( )
Maximum ( )
                                                                            | P a g e 054
                    (              )         (    )       Ө˚
, = 1 / 𝑏𝑓𝑏 × ((4 * )/ 𝑏 – 𝑊)
Use M24 bolts (BS 4190:1967) root area = 353 mm2 ( from figure
11.30 ref 7.
( ) ( * )
= 14.453 mm
                                                               | P a g e 055
Total compressive load on the base ring per unit length:
𝑏 = (( 4 / ^2) +( 𝑊 / ))--------ref 7
Ds = skirt diameter, m
(( * * ) ( * ))
=48.5248 KN/m
Where,
This is the minimum width required; actual width will depend on the
=chair design. Actual width required ( fihure 13 .30 ref 7 ) .
Lr + ts + 50 mm
= 76+16+50= 142 mm
                                                           | P a g e 056
The minimum thickness is given by.
𝑏 √ ---------- ref 7
     Lr = the distance from the edge of the skirt to the outer edge of
      the ring, mm.
     tb = base ring thickness, mm.
     ’
     fr = allowable design stress in the ring material, typically 140
      N/mm.
       tb = 76 √        = 6.487 mm .
       The chair dimensions from figure 13.30 for bolt size M24. Skirt
       is to be welded flush with outer diameter of column shell.
                                                             | P a g e 057
             Design of Nozzles:
Where:-
     G=flowrate, kg/s
     𝞺=density, kg/
   Feed Stream:
G=6.509 kg/s
𝞺=920.46 kg/
 dopt=293( ) ( ) = 62.3mm
 Nozzle thickness , t=
= ( )
=2+0.0048=2.0048mm
   Top Stream:
G=0.0216 kg/s
𝞺=2.61 kg/
 dopt=293( ) ( ) =47mm
                                                                 | P a g e 058
   Nozzle thickness , t=
= ( )
=2+0.0036=2.0036mm
   Bottom Stream:
G=4.35kg/s
𝞺=947 kg/
 dopt=293( ) ( ) = 70mm
 Nozzle thickness , t=
= ( )
=2+0.0053=2.0053mm
                                                      | P a g e 059
                Flange design:-
Feed stream:
d1=60.3
d2=14
                                                   12
                                                                            h=28
                                                                b=14
                                                            3
                            d3=80
                            d4=90
                            K=110
                            D=140
                                                                     | P a g e 061
 Top stream:
d1=48.3
d2=14
                                             12
                                                                h=26
                                                      b=14
                                                  3
                        d3=70
                         d4=80
                        K=100
                        D=130
                                                             | P a g e 060
 Bottom stream:
d1=76.1
d2=14
                                              12
                                                                 h=32
                                                       b=14
                                                   3
                        d3=100
                        d4=110
                        K=130
                        D=160
                                                              | P a g e 062
REFERENCES :
1- Chemical - Reaction - Engineering Third Editionn - Octave Levenspiel
7- https://diethyl-ether.weebly.com/weebly
8- https://webwiser.nlm.nih.gov/substance?substanceId=
11&identifier=Diethyl%20Ether&identifierType=name&menuItemId=62
&catId=83
9- https://www.slideshare.net/100003690100228/diethyl-ether-dee-
literature-review
10- https://byjus.com/chemistry/diethyl-ether/Byjus
| P a g e 063