Soran university

Faculty of engineering
Department of chemical

ACRYLONITRILE FROM PROPYLENE AND AMMONIA

Prepared by : Dlawar Mahmud

Supervisor :m. Ali hosin

1/12/2020
Flow sheet

FLOW SHEET FOR THE PRODUCTION OF METHYL ETHYL KETONE

Vaporization section

(a) Steam pre heater

The feed 2-butanol from storage tank at Temp 25oC is pumped through

pump at the shell side of the shell and tube type preheater. Dry

saturated Low pressure steam of the temp 140oC is used in tube side to

increase the 2-butanol temp up to 100oC and after that the condensate is

removed and recycled to make low pressure steam. The flow of steam is

controlled by FIC.
(b) horizatonal kettle vaporizer

Unsaturated butanol vapour at the temperature 100oC is fed in shell

side of Vertical thermo syphon vaporizer to attained the outlet

temperature 210oC by Reaction product from Reactor which is fed in

tube side at temperature 400oC .Temperature is observed through THI.

Saturated vapors are fed into Separator from where any liquid butanol

if any recycled to vaporizer again. Hot Butanol Vapour from separator

top is fed in two super Heaters at the temperature 210oC.

(c) Super heaters

The Hot Butanol Vapour is fed to two super heater to increase the

reactor feed inlet temperature up to 400-500oC by the flue gasses from

the furnace top . Reactor feed inlet temperature is controlled by the

extra tunnel burner in flue gases if required. Temperature is monitored

through thermocouple.
(d) Reactor

Dry Butanol from super heater is fed to the packed bed reactor having

Zno-Brass catalyst at the temperature 500oC ,where 90% of Sec –

Butanol is converted into MEK and Hydrogen . The dehydrogenation

reaction is endothermic and reversible and therefore a considerable

amount of heat is to be supplied and hence, a multi-tube reactor is

selected.

Reaction product having 10% unreacted Butanol and reaction

products (MEK and Hydrogen) at the minimum temperature is fed to

vaporizer.

(e) Cooling Section

Reaction products at the temperature 400olooses its temp with heat

exchange in Vertical thermo syphon vaporizer and is cooled up to 150oC

and then fed to condenser for further cooling.

(f) Partial condenser

It is used to condense the reaction products from vaporizer and

further sub cooled it .The 80% of reaction product (MEK and alcohol)

is condensed and sub cooled up to 32oC here and sent to Solvent

Extraction column for further separation of MEK from alcohol.

Rest 20% of reaction product (vapours of MEK, alcohol and Hydrogen)

is fed into the absorption columns for further separation of MEK.

(g) Absorbing section

The rest 20 % vapors from condenser is fed to the bottom of the

packed bed absorption column where MEK and 2-butanol will be

absorbed in Aqueous Ethanol. The Aqueous Ethanol will be recycled

from the extraction column. The hydrogen discharged from the top of

the absorption column is dried and fed to the furnace as fuel of burners.

The liquor Aq. Ethanol containing MEK and butanol goes to

distillation column from where Lean Ethanol is recycled back to

absorption column
(h) Solvent Extraction column

The 80 % of the condensed MEK and Butanol from partial condenser

along with the liquid( MEK and Butanol) from the absorption

distillation column is fed to a Solvent Extraction column where Tri

Chloro Ethane (TCE) is used to absorb MEK .

The Raffinate (Butanol) is recycled .

The Extract (TCE and MEK) from solvent Extraction column is fed

to distillation column for further purification.

(i) Distillation column

The extract(TCE and MEK) from solvent Extraction column is fed to the

Solvent Distillation column where TCE is separated from MEK and

recycled back to solvent extraction column , and final product MEK is

sent to storage tank.

Material Balance

Final Production of MEK =10⁷Kg/year

Let plant runs for 335 days in a year

then, Production = 10⁷/335Kg/Day

= 29850.75 Kg/Day

= 29850.75/24Kg/H = 1243.78 Kg/H

Let 7 % slippage and other losses then,

Production=1.071243.78=1330.85Kg/h

I.e. we will have to make / design a plant for final MEK production

= 1330.85Kg/h

Material Balance Overall Plant :

REACTOR STREAM 1

F M MEK Distillation

Column R

F=Feed M=Mixed STREAM

2 R=Recycle
 Alcohol Recycle

Alcohol=99%, MEK&OTHER=1%

REACTOR BLOCK MEK PROD.STILL

CH3CH2CH (OH) CH3 = CH3CH2C (O) CH3 +

H2 BUTANOL MEK H2

1 MOL 1MOL 1MOL

74 72 2

MEK Production = 1330.85Kg/h =

18.48Kmol 1Kmol MEK produced by 1Kmol

Butanol 18.48KmolMEK = 18.48Kmol

Butanol MEK=1330.85Kg/h=18.48Kmol
Some MEK and some Butanol is wasted with Hydrogen in absorption section

So taking some Excess Butanol

So Fresh Butanol =1369.63Kg/h

Butanol from Recycle=150.18Kg/h (99.0%)

MEK from Recycle = 1.48Kg/h (1.0%)

M=F+R

Total Butanol in mixed feed

=1369.63+150.18=1519.81Kg/h Total MEK in Mixed feed

=1.48 Kg/h
Material Balance over Reactor:-

Since 90% conversion as per problem given

Kg/H kmol %
Reactor
Kg/H kmol % 2-Butanol 151.85 2.05 9.98
(90% conversion)
2- 1519.81 20.54 99.9 MEK 1332.76 18.51 87.61
Butanol
Hydrogen 36.68 18.34 2.41
MEK 1.48 .02 .1
Total 1521.29 -- 100
Total 1521.29 -- 100

MEK produced =20.54kmol × 0 .9 =18.49kmol=1331.28 Kg/h

Total MEk = 1331.28+1.48 = 1332.76 Kg/h

Butanol remained unreacted = 1519.81 - (20.54×0.9×74) =151.73 Kg/h=2.05kmol

Hydrogen produced =36.68 kg/h = 18.34kmol

 Material Balance Over Condenser

As pergiven condition 80% of inlet is condensed and remaining 20

% Vapourgoes in absorption coloumn

KgpH kmol %

Butanol 30.37 0.41 9.10

MEK 266.55 3.70 79.90
Vapour Hydrogen 36.68 18.34 11.00

20%
Total 333.60 100
Partial
KgpH kmol %
Condenser
Butanol 151.85 2.05 9.98
80% condensate
MEK 1332.76 18.48 87.61
Hydrogen 36.68 18.34 2.41 (80%20% Vapour
condension)

TOTAL 1521.29 100

KgpH kmol %
Butanol 121.48 1.64 10.23
MEK 1066.21 14.51 89.77
Hydrogen 0 0 0
Total 1187.69 100
 Material Balance Over Absorption Coloumn-
Aqueous Ethanol absorb MEK and Butanol and releases Hydrogen gas

COMPONENT KG/Hr KgMOLE/HR %

BUTONAL 3.14 0.04 3.09

MEK 1.33 0.02 1.31

Kg/hr kmol % H2 36.68 18.34 36.14

butanol 30.37 .41 9.10 Absorption Coloumn

WATER 61.35 3.41 59.46
MEK 266.55 3.70 79.90
A
Total 101.5 100
hydrogen 36.68 18.34 11.00

Total 333.60 100

Kg/hr kmol %

Kg/hr kmol % Butanol; 27.23 0.37 3.29

Butanol; 0 0 0 MEK 265.72 3.69 32.15

MEK 0.5 .007 .18 hydrogen 0 0 0

Ethanol+ 533.6 99.82 Ethonal 533.6 64.56

water Total 826.55 100

Total 534.10 100

Material Balance Over Solvent Extraction Coloumn

Kg/hr kmol %

Butanol 0 0 0

MEK .05 - 0.09

Kg/hr kmol %
Ethanol 533.6 5.8 99.91
Butanol 27.23 0.37 3.29 Extraction
Coloumn
Total 534.10 100
MEK 265.72 3.69 32.15

Ethanol 533.6 64.56

Total 826.55 100

Kg/hr kmol %

Kg/hr kmol % Butanol 27.23 0.37 2.10

Butanol 0 0 0 MEK 266.17 3.70 20.58

MEK 0.5 .0007 .05 TCE 1000 - 77.32

TCE 1000 99.95 Total 1293.40 100

Total 1000.5 100

Material Balance Over Solvent Recovery Coloumn

Kg/hr kmol %

Butanol 0 0 0

MEK .05 -- .005

TCE 1000 -- 99.995

Kg/hr kmol %
Total 1000.05 100
Solvent Recovery
Butanol 27.23 0.37 2.10 Coloumn

MEK 266.17 3.70 20.58

TCE 1000 -- 77.32

Total 1293.45 100

Kg/hr kmol %
Butanol 27.23 0.37 9.28
MEK 266.12 3.70 90.72
TCE 0 0 0
Total 293.35 100
Material Balance OverMEKProduction Coloumn

Kg/hr kmol %

Butanol 150.18 2.03 99.02

MEK 1.48 .02 .98

Total 151.66 - 100

Kg/hr kmol %

Butanol 27.23 0.37 9.28

MEK Production
Column
MEK 266.12 3.70 90.28

Total 293.22 100

Kg/hr kmol %
Butanol 13.44 0.18 1.0
MEK 1330.85 8.68 99.00
Total 1344.29
Kg/hr kmol %

Butanol 121.48 1.64 10.23

MEK 1066.21 14.81 89.77

Total 1187.69 100

ENERGY BALANCE

Basis:- 1 Hr. Operation

ENERGY BALANCES ACROSS THE FEED PREHEATING

EQUIPMENT:-

The heating of cold 2-butanol feed is to be completed in three stages in

order to avoid large heat losses. The cold feed is first preheated to its

boiling point using steam as heating medium and then vaporized in a

thermo syphon reboiler utilizing the heat contained in the reaction

products. The vapor, which has entrained liquid is removed from the

knock out drum, and then heated to reaction temperature using flue gas.

COLD FEED PREHEATER:-

Total butanol =1369.63+150.18=1519.81Kg/h

MEK from recycle =1.48Kg/h

Total feed = 1519.81+1.48=1521.29Kg / hour of 2-

butanol+MEK (recycled) is to be preheated from 250C it boiling

point 107.50C.
Heat load on preheater, Q = (1519.81 × 1.497+1.48×1.664)(380.5

– 298)

= 187902.83 KJ/h

The heating medium is used is dry saturated steam at

413K Steam requirement =

= 88.49

Kg/hr BUTANOL

VAPORIZER:-

2-butanol feed is vaporized at 107.50C using reaction

products. Heat load on vaporizer is, Q = M × λ

= 1521.29× 557.43 KJ

= 848012.68 KJ/hr

Average Cp of reaction products = 2.304 KJ / Kg

K 848012.68 = 1521.29 ×2.304 (673 – T)

T = 431 K
FIRST SUPER HEATER:-

2-butanol vapors are to be heated from 380.5 K to 573K .using flue gas

which enters at 673 K & cools to 423K.

2-butanol vapors Cp = 2.038 KJ/Kg.K

Heat load on super heater, Q = M ×Cp × (T2 – T1)

= 1521.27 × 2.038 (573 – 380.5)

Q = 596817.04 KJ/h

Mass flow rate of flue gas =

= 1989.39 kg/h

SECOND SUPER HEATER:-

It raises the temperature of vapor from 573K to 773 K , using flue gas

which enters at 873K and cools to 623K

Cp = 2.674 KJ/KgK

Heat load on super heater Q = M × Cp × (T2 – T1)

= 1989.39 × 2.674× (773 – 573)

= 1063925.77KJ/h
Flue gas requirement, =

= 4451.57 Kg/h

ENERGY BALANCE ACROSS THE REACTOR:-

The feed enters the reactor at 773K and leaves at 673K. The conversion

obtained in the reactor is 90%. The heat balance includes two terms i.e ,

sensible heat change due to cooling of reaction mixture and heat

consume due to reaction.

Q = M ×Cp×(T2 – T1) + M×xi × ΔH

Mean Cp = 2.68 KJ/Kg.K

ΔH = 73900 KJ/Kgmol

Total 2-butanol feed = 1369.63+150.18=1519.81Kg/h

= 1519.81/74

=20.54 kmol/h

Q = 1521.29×2.68 × (673- 773) + 20.54×0 .90 × 73900

= 958409.68 KJ
It is assume that a flue gas is available at 800K & leaving 750K

Cp(flue gas) = 1.195 KJ/KgK

Flue gas requirement, =

=16040.33 Kg/h

ENERGY BALANCE ACROSS THE CONDENSER:-

The vapor enters condenser at 1270C (400K) at 1 bar pressure.

Liquid and the vapor leaving the condenser is in equilibrium.

At the mole fraction x = 0.80 of the condensate we get both liquid and

vapor temperature from the T- x- y diagram and temperature are

305K. = liquid temperature. 335.7K = vapor temperature

We take cooling water enters at 240C and leaving at 420C

CpH2 = 14650 J/ kg k

Cpalcohol = 1760 J/ kg k

CpMEK = 1664 J/ kg k

Cpmix =0.875 × 1664 + 0.0999 × 1760 +0 .025 × 14650

 = 1998.074 J/kg.K

Heat loss to reduction in vapor temperature from 400k to 335.7 k

Q1= 1529.27 ×1998.074 (400- 335.7)

=196474734.45J/ h=196474.73 Kj/h

Heat loss due to condensation

Q2 = 121.48 × 689.19 + 1066.21 × 486.11

= 602018.14 KJ/h

Heat loss due to further cooling of a part of vapor

is Q3 = 1187.69 ×1.987 × (335.7 – 305)

= 72450.16 KJ/h

Total heat lost = Q = Q1 + Q2 + Q3

196474.73+602018.14+72450.16

= 870943.03KJ/h

Mass flow of cooling water =

= 11556.18 Kg / h

ENERGY BALANCE ACROSS THE ABSORBER :-

Heat of condensation of MEK = 265.72 x 443.14

= 117751.16Kj/h

Heat of condensation of alcohol is = 27.23 x 560

= 0.15248.80Kj/h

Heat of solution = (265.72+27.23) x 0.35

= 102.53Kj/h

Heat loss in cooling gasses from 62.7 to 270C

= (1.33 x 1.47 + 3.14 x 1.53 + 36.68 x 14.65) (62.7 –

27)

= 19424.01Kj/h

Total heat released = 152526.50Kj/h

Heat removed by water vapor = (61.30 x 2437.9)

= 149565.17Kj/h

Heat gained by irrigating liquor

a) Water: 61.35 x 4.186 (T – 300)

b) MEK: 1.33 x 2.299 x ( T-300 )

c) Alcohol: 3.14 x 2.429 x (T- 300)

Heat gained by irrigating liquor =

(61.354.186+1.332.299+3.142.429)(T-

300)

=267.29(T-300)Kj/h

Total heat gained = 149565.17+ 267.29 x (T-300) Kj/h

Heat released = heat gained

152526.50 = 149565.17+ 267.29 x (T-300) Kj/h

2961.33=267.29x (T-300) Kj/h

11.07=T-300

T=311.07K

ENERGY BALANCES ACROSS THE EXTRACTION COLUMN:-

It is assume that the extraction process is isothermal. All that streams

come at 270C and

Leavesat 270C.

ENERGY BALANCE ACROSS THE SOLVENT RECOVERY &

UNIT:-
Feed is not saturated liquid it is sub-cool liquid. Saturation temperature

is 930C

From x-y diagram we get Rm = 0.38.

R= 2Rm = 0.76

Feed:

Alcohol = 27.23/74 = 0.37 kmol /h

MEK = 266.17/72 = 3.70 kmol/h

TCE = 1000/133.5 = 7.49kmol/h

Total = 11.56kmol /h

Mole fraction of MEK

XMEK = 0.32

Feed temperature = 270C

F . HF =0.37 x170.058 (27- 0) + 3.70x165.726 x 27+7.49 x148.56x27

 =1698.88+4478.30+30043.29

F . HF = 366220.47 Kj/h

Distillate:-

Alcohol = 27.23/74 = 0.37 kmol /h

MEK = 266.07/72 = 3.70 kmo/h

Total = 4.07 kmol/h

D = 4.07kmol/hr

Mole fraction of MEK, XMEK =3.70/4.07=0.91

from T-x-y diagram distillate temperature = 80.40C

Cp MEK = 170 Kj/kmol K

Cp alcohol = 228 Kj/kmol K

Cp water = 75.37 Kj/mol K

Cp TCE = 148.56 Kj/mol K

D. HD = [0.37 x 228 + 3.70 x 170 ] (80.4)

= 713.36Kj/h

Residue:

MEK = 0.5 kg = 0.0006 Kmol/h

TCE = 1000 kmol = 7.49 Kmol /h

Total = 7.4912 kmol/h

XMEK = 0.0006/7.4912 = 0.00008

From T-x-y diagram the temoeratureobtained .

T = 1120C = 385K (residue)

Cp MEK = 175 Kj/mol k

Cp alcohol = 260 Kj/kmol k

Cp water = 75.37 Kj/kmol k

Cp TCE = 148.56 Kj/kmol k

W. Hw = [.0006 x 175 + 7.49 x 148.56 + ] x (112)

= 124635.72Kj/h
Condenser:-

VHv =D.HD + L. HL + Qc.

VHv = (D + L ) . HL +Qc

Qc = V x (Hv - HL)

Qc = V x λ

V = (1 + R ) x D

D = 4.07 kmole/h

V = ( 1 + 0.76 )x 4.07 = 7.16 kmole/h

Vxλ= 7.16 x 3.18445 x104

= 22.81x104kj/h

Qc = 22.81 x 104kj/h

Cooling water requirement = 22.81 x 104/4.187(42-25)

= 3204.60Kg/h

Reboiler:-

Overall heat balance

F. HF + QB = Qc + D . HD + WHw

QB = Qc + D . HD + WHw - F. HF
QB = DHD = WHw + Qc - FHF

QB = 228100+713.36+ 124635.72– 36220.47

QB = 317228.61Kj/h

Steam is available at 2.00 bar steam temperature = 410 k

Steam Req.= 317228.61/2153.4=147.32Kg/h