A PROJECT REPORT ON

PRODUCTION OF METHYLACETATE

BY REACTIVE DISTILLATION

ACKNOWLEDGEMENT

We are extremely thankful to Prof. C. Muthamizh Chelvan, Associate Director, SRM

Engineering College, for permitting us to carry out this project and providing us with all

facilities.

We would like to thank Dr. R. Karthikeyan, Head of Department of Chemical

Engineering, for allowing us to work on this project and for all support and guidance he

has provided us.

We take pride in expressing our deepest gratitude to our project guide, Mr. K.

Anbalagan, Senior Lecturer, Department of Chemical Engineering, for his invaluable

guidance and encouragement at every stage of this project.

We extend our thanks to all the staff members of the Chemical Engineering Department

for the technical assistance and support.

We would like to thank the staff of the DTP and Xerox section of SRM Engineering

College for their assistance in the project documentation.

CONTENTS

S.No. CHAPTER Page No.

Acknowledgement

Abstract

1. Introduction 2

2. Properties 3

3. Processes of Manufacture 7

4. Selection of Process 9

5. Process Description 10

6. Material Balance 11

7. Energy Balance 18

8. Design Analysis 23

9. Cost Estimation 28

10. Control Structures 30

11. Safety Aspects 34

12. Flow Sheets & Graphs 39

13. Conclusion 51

Bibliography

PROCESS FLOWSHEET 1. Process Flow Sheet for Reactive Distillation Column.

2. Effect of Reflux Ratio on Conversion of Acetic Acid

3. Comparison of Two Models w.r.t. Mole Fraction of Various Components and

No. of Trays

4. Effect of Damkohler Number on Conversion of Acetic Acid

5. Conversion of Acetic Acid and Average Stage Volume Holdup for Different Da

6. Volume Holdup Distribution and Reactive Status Throughout The Column Based

on 280.0 Kmol MeOAc /hr

7. Effect of Reflux Ratio on Equilibrium Design

8. Effect of Reflux Ratio on the Composition of MeOAc and Water in Distillate and

Bottom Respectively for Different value of Da.

9. Heat Effect Model

10. Control Structure 1

11. Control Structure 2

12. Control Structure 3

ABSTRACT

It is a continuous system where the reaction and separation are performed in the Distillation column. Reaction takes place in the vessel and Separation is

done in the column attached to it. The design of Reactive Distillation systems is much

more complex then conventional reactors and distillation columns. It includes several

steps such as feasibility analysis, conceptual design, equipment selection and design,

operability and control studies. In the limit of reaction and phase equilibrium, we show

(1) the existence of both a minimum and a maximum reflux, (2) there is a narrow range

of reflux ratios that will produce high conversions and high purity methyl acetate, and (3)

the existence of multiple steady states throughout the entire range of feasible reflux

ratios. For finite rates of reaction, we find (4) that the desired product compositions are

feasible over a wide range of reaction rates, up to and including reaction equilibrium, and

(5) that multiple steady states do not occur over the range of realistic reflux ratios, but

they are found at high reflux ratios outside the range of normal operation. The conceptual

design estimates feed locations, flow rates, determines of column size and liquid holdups

etc.

INTRODUCTION

The production of methyl acetate is a classic example of successful reactive distillation

technology. Soon after the invention and commercial application of this technology for

methyl acetate synthesis it was used as a model system for testing a new design and

synthesis framework that was developed for the limiting case of equilibrium chemical

reactions, i.e. fast reactions or large holdups. In recent years, the focus of research has

turned to kinetically controlled reactive distillations and the kinetics of methyl acetate

synthesis have been studied extensively for both homogeneously and heterogeneously

catalyzed reactions. Methods have also been developed recently for the design, synthesis,

and feasibility analysis of kinetically controlled reactive distillation, and methyl acetate

synthesis has commonly been used as a model system .Extensive experimental data have

been reported for many different configurations of reactive distillation devices for methyl

acetate synthesis, which provides a good database for testing design and Simulation

models. These project also contain extensive literature reviews with special reference to

methyl acetate synthesis and Models and calculation techniques that have been developed

to support the design of reactive distillation columns. The models, which are hierarchical,

require increasingly sophisticated data needs as the hierarchy is implemented. Methyl

acetate synthesis is used as a model system to demonstrate the approach. The results show

the effects of reflux ratio and kinetic parameters on the conversion in reactive distillation,

in good agreement with measurements reported for this system.

PROPERTIES

Physical properties of Methyl acetate:

They are neutral colourless liquids possessing characteristic fruity odours.

The boiling point of Methyl Esters are much lower than the parent acid, since the former are unassociated liquids. Boiling point of

Methyl Acetate= 57 0C

Specific gravity of Methyl Acetate is 0.93(150C). Vapor density is 135.9 mbar (9.40C). Melting point by Methyl Acetate is obtained at -980C. Viscosity is obtained at 0.403mPa.S (150C). Flash point is obtained at -140C. Generally insoluble in water and soluble in most organic solvents. Many esters are excellent solvents for other organic substance.

Example-methyl acetate.

In the IR spectrum, esters show characteristic C=0 stretching frequency at 1735 cm-1.

Chemical properties of Methyl Acetate

9 Esters give nucleophillic substitution reactions similar to acid halides and anhydrides.

9 The carbonyl carbon in their molecule is electron deficient owing to the electron withdrawing effect of OH-1and carries a partial positive charge.

9 Esters undergo nucleophillic reactions less readily unlike acid halides or anhydrides. This is due to the Resonance effect.

9 Delocalization of unshared electrons pair on Oxygen atom, decreases the electron deficiency of carbonyl carbon which becomes less prone to

nucleophillic attack.

General Reactions are listed below:

Hydrolysis:

Esters when heated with water in the presence of an acid

catalyst (Sulphuric acid or Hydrochloric acid) are hydrolysed to give

the parent carboxylic acid and alcohol. Reactions are reversible.

Methyl acetate + water Acetic acid+ Methanol. CH3COOCH3 + H2O CH3COOH + CH3OH Hydrolysis of an ester can also be achieved by refluxing

with aqueous solution of a strong base such as Sodium Hydroxide.

Methyl Acetate + Sodium Hydroxide Sodium Acetate + Methanol.

CH3COOCH3 + NaOH CH3COONa + CH3OH The above reaction is called Saponification.

Transesterification:

Esters of an alcohol can react with another lower

alcohol in the presence of a mineral acid, to give the ester of second

alcohol. The interchange of alcohol portions of the esters is termed as

Transesterification.

Ethyl Acetate + Methanol Methyl Acetate + Ethanol.

CH3COOC2H5 + CH3OH CH3COOCH3+ C2H5OH

Reaction with Ammonia(Ammonylysis):

Methyl Acetate + Ammonia Ethanamide+ Methanol.

CH3COOCH3 + NH3 CH3CONH2 + CH3OH

Reduction to Alcohols:

Esters can be reduced to the primary alcohol

corresponding to the acid from which it was derived by Lithium Aluminum

Hydride or by Sodium and Alcohol.

Methyl Acetate+ 4(hydrogen) Ethanol+Methanol.

CH3COOCH3 + 4(H) C2H5OH + CH3OH

Reaction with Grignard Reagents :

Esters react with Grignard

reagents to form Ketones which at once react with another molecule of

Grignard Reagent to yield a tertiary alcohol.

Methyl Acetate Ketones tertiary alcohol.

CH3COOCH3 CH3COOMgCl (CH3)2 CH3COCH3 + ClMgOCH3

CH3COCH3 CH3COMgCl (CH3)2 CH3COH (CH3)2

Claisen Condensation:

Esters that have hydrogen atoms on the alpha

carbon atom undergo condensation reactions to form Beta-Keto Esters,

in the presence of a strong base (Sodium Acetate).

Methyl Acetate + Methyl Acetate Methyl AcetoAcetate.

CH3COOCH3 + CH3COOCH3 CH3COCH2COOCH3

USES OF METHYL ACETATE

It is used as a solvent in industry, notable for lacquers and resins.

It is used in artificial fruit flavors. In organic solvents .Example-Methyl AcetoAcetate. Synthetic products such as perfumes, pesticides, fibres,

solvents and plasticizers.

VARIOUS MANUFACTURING PROCESSES OF METHYL ACETATE

1) Fischer Esterification:

Acetic acid reacts with Methanol to give Methyl acetate.

Acetic acid+ Methanol Methyl Acetate + Water CH3COOH + CH3OH CH3COOCH3 + H2O

2) By reaction of Acid Anhydrides with Alcohols: Acetic anhydride reacts with Methanol to give Methyl Acetate.

Acetic anhydride + Methanol Methyl Acetate + Acetic acid. CH3COOCOCH3 + CH3OH CH3COOCH3 + CH3COOH 3) By reaction of Acid anhydrides with alcohols:

Acetyl Chloride reacts with Methanol to give Methyl Acetate.

Pyridine is used to remove HCl formed.

Acetyl Chloride + Methanol Methyl Acetate + Hydrochloric acid.

CH3COCl + CH3OH CH3COCH3 + HCl 4) By reaction of Carboxylate salts and Alkyl Halides: Sodium Carboxylate reacts with Methyl Chloride to give Methyl

Acetate.

Sodium Carboxylate + Methyl Chloride Methyl Acetate + Sodium Chloride.

CH3COONa + CH3CL CH3COOCH3 + NaCl 5) By Transesterification (Esterification): Ethyl Ethanoate reacts with Methanol to give Methyl Acetate.

Ethyl Ethanoate + Methanol Methyl Acetate + Ethanol. CH3COOC2H5 + CH3OH CH3COOCH3 + C2H5OH

6) By reaction of a carboxylic acid with Diazomethane: Ethanoic acid reacts with Diazomethane to give Diazomethane.

Ethanoic acid + Diazomethane Methyl ethanoate + Nitrogen. CH3COOH + CH2NH2 CH3COOCH3 + N2 7) Reactive Distillation:

It is a continuous system where the reaction and separation are

performed in the Distillation column. Reaction takes place in the vessel and Separation is

done in the column attached to it. It includes several steps such as feasibility analysis,

conceptual design, equipment selection and design, operability and control studies. The

conceptual design estimates feed locations, flow rates, determines of column size and

liquid holdups etceteras, and usually is based on geometric method.

Acetic acid+ Methanol Methyl Acetate + Water CH3COOH + CH3OH CH3COOCH3 + H2O

2Methanol Dimethyl Ether + Water 2CH3OH CH3COCH3 + H2O

SELECTION OF PROCESS OF MANUFACTURE Reactive Distillation is a continuous system where the reaction and separation are performed in the Distillation column. Reaction takes place in the vessel and Separation is done in the column attached to it. It includes several steps such as feasibility analysis, conceptual design, equipment selection and design, operability and control studies. The conceptual design estimates feed locations, flow rates, determines of column size and liquid holdups etceteras, and usually is based on geometric method.

Advantages of Reactive Distillation column:-

Potential of separating mixtures involving Azeotropes or isomers. Reducing energy costs: - Separation of these mixtures by

conventional distillation requires high energy costs while separation with solvent based distillation requires a suitable solvent, which may not be available in all the cases.

Increases product yield: - It allows separation of the reaction products from the reactants in the same unit operation. So ultimately increasing product yield.

Fewer problems: - Problems in Reactive distillation are particularly less due to the dynamic interaction of the reaction kinetics and thermodynamic properties. Allows overcoming the limitations caused by Chemical equilibrium.

100% Removal of cycle streams. Avoidance of Azeotropes. Significant reduction of capital and operating costs. Higher product purity.

Disadvantages of Reactive distillation:-

This process can only be understood with the aid of computer simulation.

Complicated modeling. Carrying out of expensive and time consuming sequences of

laboratory and pilot plant equipments.

Applications of Reactive distillation:-

9 Used for Esterification process. 9 Used in the manufacture of Anti-knock enhances such as MTBE and

TAME.

9 Used in the pharmaceutical industry. 9 Used in the preparation of Nylon-6 production.

PROCESS DESCRIPTION

Reactive Distillation is a continuous system where the reaction and separation are performed in the Distillation column. One interpretation of the column is that simultaneous reaction and separation occurs in the catalytic section (i.e., below the feed point for the Sulfuric acid catalyst) producing water as a bottom product and the methanol/methyl acetate Azeotropes in the vapor stream leaving the top of this section. This stream then enters a (non-reactive) extractive section placed on the top of the reactive column, which purifies the methyl acetate and forces the methanol down into the reaction zone. The third design is a novel reaction equilibrium device with two feeds, where acetic acid is fed near the top of the column and methanol near the bottom in equimolar amounts. The column simultaneously produces methyl acetate as distillate, and water as bottom product. In this design, the rectifying section is a non-reactive extractive section separating methyl acetate and acetic acid. This can be seen from the rectifying profile in the Flow sheet which lies on the non-reactive edge between methyl acetate and acetic acid it.

MATERIAL BALANCE

1. Reflux ratio range is 1.3 ~ 2.8. 2. Outside this range of reflux ratio, even an infinite number of equilibrium

reactive stages will not accomplish the desired separation 3. There is no infinite number of equilibrium reactive stages at (rmin & rmax ) due

to saddle pinch and node pinch in the middle profile. 4. We have to select best middle profile to minimize the total no. of stages in the

column. 5. Increasing the pressure increases the minimum number of stages required and

reduces the range of feasible reflux ratio. 6. Design with a practical no. of stages are not possible and pressure greater than

1atm and are not feasible at pressure greater than ~ 1.3 atm.

XD = 0.985 XB =0.985 Scaled Damkohler Number, D=(Da ) / (1 + Da) Da = (HRT /F)/(1/KF ) For no-reactive limit, Da =0 At reaction equilibrium limit, Da = The fixed point equations for the stripping cascade and for the rectified cascade by

Fixed points are calculated using an arc-length continuation procedure starting at the non-reactive Azeotropes and pure components at D=0

parameter is introduced to calculate the total reactive holdup within a reactive column when reaction occurs on stage j, is set to unity otherwise is zero when , non reactive distillation is recovered when , the equilibrium limit is approached.

when , it implies non-reactive distillation As , phase and reaction and equilibrium distillation is achieved The total rate of generation of moles at stage j is given by

Where R is the numbers of reactions

Terms Unit Methanol Water Methyl Acetate Acetic acid DMEMolecular weight 32.04 18.02 74.08 60.05 46.07

Molar density kgmole/m3 23.49 54.6 11.89 17.04 3.703*10^-2Mass density kg/m3 752.7 983.6 881 1023 1.706

Actual volume flow m3/hr 11.92 5.1 23.67 16.43 7604Mass enthalpy kJ/kg -7359 -15680 -5903 -7621 -3952Mass Entropy kJ/kg*c 2.184 0.7816 2.028 1.465 4.361Heat capacity kJ/kgmole*c 119 75.92 141.5 94.95 70.2

Mass heat capacity kJ/kg*c 3.714 4.215 1.19 1.581 1.525Lower Heating value kJ/kgmole 63810 0 1450000 786400 1328000

Mass lower heating value kJ/kg 19910 19570 13100 28840Phase fraction(Vol. basis) 1 1 1 1 1

Phase fraction(Mass basis) 2.122*10^-314 1 1 1 1Avg. Liquid density kgmole/m3 24.83 55.4 12.68 17.51 14.55

Specific heat kJ/kgmole*c 119 75.92 141.5 94.95 70.28Standard gas flow m3/hr 6620 6584 6657 6620 6657

Std. ideal liquid mass density kg/m3 795.7 998 939.3 1052 670.3Actual liquid flow m3/sec 3.311*10^-3 1.417*10^-3 6.576*10^-3 4.565*10^-3

Z factor 1.576*10^-3 6.782*10^-4 3.113*10^-3 2.173*10^-3 1Watson K 10.63 8.935 8.443 11.38

Heat of Vaporization kJ/kgmole 35290 40650 30150 23330 21520Kinematic viscosity centistoke 0.4837 0.5012 0.2968 0.7147 5.639

Liquid mass density(Std.cond.) kg/m3 796.4 1015 936 1072 617.8Molar volume m3/kgmole 0.04257 0.01832 0.08409 0.05869 27.01

Mass heat of vaporization kJ/kg 1101 2256 407 388.5 467.1Phase fraction(Molar basis) 1 1 1 1

Surface tension dyne/cm 24.69 66.67 27.95 28.11 Thermal conductivity w/m k 0.1666 0.6496 0.1506 0.164 0.01858

Absolute viscosity centipoise 0.3641 0.493 0.2615 0.7312 0.009618CV (semi-ideal) kJ/kgmole*c 110.7 67.61 133.2 86.64 61.96

MassCV (semi-ideal) kJ/kg*c 3.455 3.753 1.798 0.9557 1.345CV kJ/kgmole*c 93.21 65.01 107.4 61.96

MassCV 2.909 3.609 1.449 1.345True Vapour press. at 37.8*c kpa 32 6.553 49.59 4.184 831.3

Liquid Vol flow (std. cond.) m3/hr 11.27 4.943 22.28 15.69 20.99

CALCULATION OF ACTIVITY COEFFICIENT: Acetic Acid-component 1 Methanol- component 2 Methyl Acetate-component 3 Water- component 4 Dimethyl Ether- component 5

Components

Specific volume in cm3/mole

Acetic Acid 57.54 Methanol 44.44 Methyl Acetate 79.84 Water 18.07 Dimethyl Ether 69.07

WILSON PARAMETERS: a11=0 a21= -547.3248 a31= -696.5031 a41= 658.0266 a51=96.7797 a12=2535.2019 a22=0 a32= -31.1932 a42=469.5509 a52= -418.649a13=1123.1444 a23=813.1843 a33=0 a43=1918.232 a53= -21.2317a14=237.5248 a24=107.3832 a34=645.7225 a44=0 a54=522.2653 a15= -96.7798 a25=900.9358 a35= -17.2412 a45=703.3566 a55=0

where aij is interaction energy in Cal/mol

12= (V1/V2) exp (-a12/RT) =(57.54/44.44) exp (-2535.2019/(0.08206*329.15)) =2.2319*10-41

11=1 12=2.2319*10-41 13=6.29*10-19 14=4.8289*10-4 15=29.9779 21=491420768.3 22=1 23=4.6813*10-14 24=0.04615 25=2.1*10-15 31=2.015*1011 32=5.7 33=1 34=1.166*10-10 35=2.188 41=8.2524*10-12 42=1.1462*10-8 43= 33067* 10-31 44=1 45=1.2835*10-12 51=0.03335 52=8374737.23 53=1.8986 54=1.53*10-8 55=1

ln a1 = 1- ln(.000339*1 + 0.007845*1.33 * 10^(-44) + 0.985055 * 1.2119 * 10 ^ (-18) + 0.0069 *4.762 * 10^ (-5) +.000071 * 0.0333) a1 = 1.676 a2 = 1.545 a3 = 1.7892 a4 = 1.2455 a5 = 1.3450 The total rate of generation of moles at stage j is given by :-

E1,1 = 0.20385 E1,2 = 0.19024

Assumptions:- Extent of the reaction is constant at all stages in reactive zone. Liquid holdup at each stage or tray holdup = 3 m3 for maximum conversion of

reactant. X1 = 0.000339, X2 = 0.007845, X3 = 0.985055, X4 = .00669, X5 = 0.000071. V1 = 57.54 cm3/ mole, V2 = 44.44 cm3/ mole, V3 = 79.87 cm3/ mole, V4 = 18.07 cm3/mole, V5 = 69.07 cm3 / mole. Average specific molar volume V = X1 V1 + X2 V2 +X3 V3 + X4 V4 + X5 V5 = 79.1445 cm3 / mole or 79.1445 * 10 ^ (-3) m3 / kmole. Since 79.1445 * 10 ^ (-3) m 3 of liquid mixture = 1kmole. Therefore 3 m3 of liquid mixture = 38 kmole. HJ = 38 kmole , HT = 1444 kmole. The total rate of generation of moles at stage j is given by

when = 0, RJ = 1

when = 1, RJ = 1*38*(4*0.20385 + 4 * 0.19024) = 60 kmole. Overall Material Balance:- F1 + F2 = D + B = 280 + 280 = 281.544 + B B = 278.453 kmol / hr D= 281.547 kmol/ hr Liquid Phase:- LO = rD r = 1.9 , s = 1.9858 , F3 = 280 kmol/hr, Da = 21.74 LO = 534.9393 kmol/ hr L1 = rd + Q1 F1 + R1 , where Q1 is feed quality = 1.3 Since F1 = 0 & no reaction takes place at 1st stage. So R1 = 0. L1 = r * D = 534.9393 kmol/hr. L1 = L1 + Q2F2 + R2

F2 = 0, R2 = 0. L2 = L1 = 534.9393 kmol/hr L3 = L2 + Q3F3 + R3 R3 = 60 kmol/ hr, F3 =kmol/hr. L3 = 958.9393 kmol / hr. L4 = L3 + Q4F4 + R4 = 1018.9393kmol/hr. LN-1 = LN-2 + QN-1 FN-1 + RN-1 L36 = L35 + Q36 F36 + R36 = 3302.9393kmol/hr. L38 = B= 278.453 kmol / hr. Vapour Phase: - VO =VD = (r + 1) D =(1.9 + 1) * 281.547 = 816.48 63 kmol / hr. V1 = (r + 1) D R0 F0 Since F0 = 0, RO = 0 V1 = 816.4863 kmol/ hr. V2 = V1 + (QV 1) F1 = (r + 1) D + (Q1 1) F1 R0 F0 = 816.4863 kmol/ hr V3 = V2 + (Q 2 1) F2 = 816.4863 kmol/hr V4 = V3 + (Q3 1) F3 = 816.48 63 + (1.3 1) * 280 = 00.486 kmol/hr VN = SB = 1.9858 * 278.453 = 552.95 kmol/hr

ENERGY BALANCE

In the steady state, enthalpy balance enclosing stage J (! =0, N) is given by

For CH3OH, V=0.127 m3/ kmol, f = -2.013 * 10 ^ 5 kJ / kmol,

= -2.109 * 10^ 5 Kj /kmol.

Calculating : -

Neglecting enthalpy of mixing in Vapour-Phase. hjv, mix = 0. HJv, mix = (y1 * h1v + y2 * h2v + y3* h3v + y4 * h4v + y5 * h5v ) y1 = 0.000339, y2 = 0.007845, y3 = 0.985055, y4 = 0.00669, y5 = 0.000071 hVI, J = [(Mass Enthalpy * Molecular Weight) + Heat of Vaporization ] hv1CH3COOH = (-7621 * 60 +23330) = - 433930 kJ/ kmol hv2CH3OH = (-7359 * 32.04 + 35290) = - 200492kJ/kmol hv3CH3COOCH3 = (-5903 * 74.08 + 30150) = - 407144.24 kJ / kmol hv4H2O = (-15680 * 18.02 + 40650) = -241903.6 kJ / kmol hv5DME = (-3952 * 46.09 + 21520) = -203588.64 kJ/ kmol HJv, mix = (0.000339 * -433930) + (0.007845 * - 200492) + (0.985055 * - 407144.24) + (0.00669 * -241903.6) + (0.000071 * -203588.64) = -404412.2212 kJ / kmole. Calculating HJL , mix:-

Neglecting hLj,mix = 0

=(x1 * hL1 + x2 * hL2 + x3 * hL3 + x4 * hL4 + x5 * hL5) = (0.000339*-7621*60 + 0.007845 * -7359 * 32.04 + 0.985055 * -5903 * 74.08 + 0.00669 * - 15680 * 18.02 + 0.000071 * -3952 * 46.07) = -434670.4532 kJ /kmole.

For stage 1 values are: x1 = 0.000353, x2 = 0.007860 , x3 = 0.98 , x4 = 0.00705 , x5 = 0.004737. Assuming hv mix = 0 hV1 mix = ( x1 * hV1CH3COOH + x2 * hV2CH3OH + x3 * hV3CH3COOCH3 + x4 * hV4H2O + x5 * hV5DME) = (0.000353 * -433930 + 0.00786 * -200492 + 0.985055 * -407144.24 + 0.00705 * -241903.6 + 0.004737 * -203588.64) = - 403262.3598 kJ/ kmole. Heat and free energy formation of Inorganic and Organic compounds Reaction undergoing in the Reactive distillation column CH3COOH + CH3OH CH3COOCH3 + H2O For Liquid Hfl = Hfr - Hfp = (-57.04-116.2) (-98.72-68.3174) = -6.2026kcal/mole = -25951.7kj/kmole For Gas Hfg =Hfr - Hfp =(-48.08-104.72)-(-57.7979-94.06) = -0.9421 kcal/mole 2CH3OH CH3OCH3 + H2O For Liquid Hfl = Hfr - Hfp = (2*-57.04) (-51.3-68.3174) =5.5374kcal/mole For Gas Hfg =Hfr - Hfp = (2 * -48.08) (-43.06-57.7979) = -4.6979kcal/mole. Calculation of Qc

Parameters Units values

VD kj/kmole 816.4863

HJv, mix kj/kmole -404412.22

LD kmole/hr 281.547

LO kmole/hr 534.9393

HJL, mix kj/mole -434670.4532

H1v, mix kj/mole -403262.3598

V1 kmole/hr 816.4863

1 HO kmole 38

0.20385 0.19024 Qc= (816.4863 * -404412.22) + (281.547 + 534.9393) * (434670.4532) (816.4863 * -403262.3598) 0 1 * 38 * (-25951.7 * 0.20385 + 23168.48 * 0.19024) = -3.558*10^7 kj/hr. Calculation for Qr

LN-1 = LN-2 + QN-1FN-1 + RN-1 When N=38, QN-1FN-1 = 0, L36 =3302.9393 kmol/hr L37 = L36 + Q37F37 + R37 = 3302.9393 + 60 = 3362.9393kmol/hr hVT = hv1CH3COOH + hv2CH3OH + hv3CH3COOCH3 + hv4H2O + hv5DME = (-433930 * 0.009027) + (-200492 * 0.001081) + (-407144.24 * 0.000012) + (-241903.6 * 0.98988) + (-203588.64 * 0) = -243594.2437kj/kmole hL = hLCH3COOH + hLCH3OH + hLCH3COOCH3 + hLH2O + hLDME = (-7621*60*0.009027) + (-7359 * 32.04 * 0.001081) + (-5903 * 74.08 * 0.000012) + (-15680*18.02 * 0.98988) + 0

= -284081.9711kj/kmole. At (N-1) stage, i.e. 37th stage. X1 = 0.0015 , X2 = 0.002056 , X3 = 0.00009 , X4 = 0.9853 , X5 =0. hL37, mix = (0.0015 * -7621 * 60) + (0.002056 * -7359 * 32.04) + (0.00019 * -5903 *74.08) + (0.9853*-15680*18.02) = -279653.8065kj/kmole Parameters required for calculating Qr Parameters Units Values

V38 kmole/hr 552.95hV38,mix kj/kmole -243594.2437

L38 kmole/hr 278.453L37 kmole/hr 3362.9393

hL38,mix kj/kmole -284081.9711H38 kmole 38F38 kmole/hr 0

Or = (552.95 * -243594.2437) + (278.453 * -284081.9711) (3362.9393 * -279653.8) - 0 [1 * 38 * {-25951.7 * 0.20385 23168.48 * 0.19024 }] = 7.26 * 10^8 kj/hr.

DESIGN ANALYSIS Determination of number of Equilibrium stages by Fenske-Underwood-Gilliland method Nmin = ln [(xLK/xHK) D (xHK/ xLK) B] / ln (LK/HK) avg Where, xLK = Mole fraction of the light key xHK = Mole fraction of the heavy key Nmin = Minimum number of stages (LK/HK) avg = Average geometric relative volatility of the Light key to the Heavy key. . (LK/HK) avg = [(LK/HK)D (LK/HK)B ](1/2) Reactions undergoing in the column are:- CH3COOH + CH3OH CH3COOCH3 + H2O 2CH3OH CH3OCH3 + H2O In distillate & bottom product Light key (LK) = Methyl Acetate (CH3COOCH3) Heavy key (HK) = Water (H2O) In feed stream Light key (LK) = Methanol(CH3OH) Heavy key (HK)=Acetic acid(CH3COOCH3) To determine the minimum reflux ratio by Underwood:- (i * XF, i)/ (i ) = 1 q , where i = 1 to n i = Average geometric relative volatility of component i in the mixture relative to the heavy key. (XF,i) = Mole fraction of component i in the feed. q = Moles of saturated liquid on the feed tray per mole of feed. Value of is determined by trial and error method and lies between the relative volatility Of 2 key components. Minimum Reflux (Rmin) Rmin + 1 = (i * XD i)/ (i ), where i = 1 to n n = No. of individual components in the feed. XD i = Mole fraction of component i in the distillate.

N = Number of Equilibrium stages. i = Average geometric relative volatility of component i in the mixture relative to the heavy key. Eduljee Equation (N-Nmin)/ (N+1) = 0.75 [1 (R-Rmin)/(R+1) ^0.566} Where R = Operative reflux selected by design. We know, 12 = (y1/y2)/(x1/x2) = (P1S)/ (P2S) L/H = (yL/yH)/ (xL/xH) Operating temperature: 56*C = 329K Determining Saturated Pressure (PS) By Antoine Equation: lnPsat = A + (B/T+C) Where Psat =saturated pressure (Pascal) T=Operating temperature (Kelvin) A, B, C are Antoine Coefficients. Values of Antoine Coefficients

ln PsatCH3COOH = 22.1001 (3654.62/(329-45.392)) = 9.2139 PsatCH3COOH = 10035.6597 pa ln PsatCH3OH = 23.4999-(3643.3136/(329-33.434)) = 11.1733 PsatCH3OH = 71206.166 pa ln PsatCH3COOCH3 = 21.1520-(2662.78/(329-53.460)) =11.4881 PsatCH3COOCH3 = 97551.9 pa ln PsatH2O =23.2256 (3835.18/(329-45.343)) = 9.7051 PsatH2O = 16401.298 pa Determination of average geometric relative volatility LK/HK = PLKS /PHKS In Distillate and Bottom product : LK/HK = PsatCH3COOCH3 / PsatH2O

= (97551.9/16401.298) = 5.9478 In Feed stream : LK/HK = PsatCH3OH / PsatCH3COOH = (71206.166/10035.6597) = 7.095 (LK/HK)avg =[(LK/HK)D(LK/HK)B]^(0.5) =(5.9478*5.9478)^0.5 =5.9478 Number of Equilibrium stages Nmin = ln [ (xLK/xHK)D (xHK/xLK)B ] / ln (LK/HK)avg (xLK)D = (xCH3COOCH3)D = 0.985055 (xHK)D = (xH2O)D = 0.006690 (xLK)B = (xCH3COOCH3)B = 0.000012 (xHK)B = (xH2O)B = 0.989881 (LK/HK)avg =5.9478 Nmin = ln [ (0.985055) / (0.006690)D * (0.989881) / (0.000012)B ] / ln (5.9478) = 9.1487 9 So No. of Equilibrium stages = 9 Calculation to obtain Rmin (i * XF, i)/ (i ) = 1 q , where i = 1 to n i = Average geometric relative volatility of component i in the mixture relative to the heavy key. (XF,i) = Mole fraction of component i in the feed. q = Moles of saturated liquid on the feed tray per mole of feed. Value of is determined by trial and error method and lies between the relative volatility Of 2 key components. Assuming Feed is in Vapour.q = 0 (5.9478 * 1) /(5.9478 x ) + (1*1)/(1-x) = 1 2 + 5.9478 = 0 = 1.9895 Now, . Rmin + 1 = (i * XD i)/ (i ), where i = 1 to n n = No. of individual components in the feed. XD i = Mole fraction of component i in the distillate. N = Number of Equilibrium stages. i = Average geometric relative volatility of component i in the mixture relative to the heavy key Rmin + 1 = (5.9478 * 0.985055)/(5.9478 1.9895) + (1 * 0.006690) / (1-1.9895) =1.4734 So Rmin = 0.4734 For normal distillation processes , R = 1.2Rmin = 0.56808 Incase of Reactive Distillation , R = 4Rmin = 4 * 0.4734 = 1.8936 1.9

(N-Nmin)/(N+1) = 0.75 (1 (0.56808 0.4734)/(0.56808 + 1) ) ^ (0.566) = 0.724 (N-9) / (N+!) = 0.724 N = 35.234835 Determination of location of Feed Log (ND/NB) = 0.206 Log { (B/D) (xHK/xLK)F [(xLK)B/ (xHK)D]^2 } D= 281.457kmol/hr = 0.07821 kmol/s B= 278.451 kmol/hr = 0.0773 kmol/s (xHK)F = 1 (xLK)F = 1 (xLK)B = 0.000012 (xHK)D = 0.006690 Log (ND/NB) = -1.13251 (ND/NB) = 0.07370 We know N = ND + NB 35 = ND + NB ND = 0.07370NB Substituting ND=0.0737NB in 35 = ND + NB NB = 33 ND = 2 Calculating Vapour velocity Vnf = CSb (/ 20)^0.2 ((L V)/V)^0.5 CSb = 0.075 = Surface tension of Methyl Acetate = 27.95 dyne/cm. L = Average liquid density of Methyl Acetate (kmole/m3) V = Average vapour density (kmole /m3) V = (PM/RT) By Ideal gas law where P = Pressure of the vapour = 1atm M = Molecular weight of the vapour = 74 T = operating temperature = 329k R = universal gas law constant V = (1 * 74) / (0.08206 * 329 ) = 2.7413g/litre. Vnf = 0.075 * (27.95/20) ^0.2 ((938.32 2.7413)/2.7413)^0.5 =1.4814 m /s Assuming 80% Flooding So actual Vapour velocity , Vn = 0.8 Vnf =( 0.8 * 1.4814) = 1.18512 m/s. Volumetric flow rate = Vn * An 23.67 = 1.185 * An An= 19.97 m2

Assuming the Down comer occupies 15% of cross sectional area of the reactive distillation column. Ac = An/0.85 =19.97/0.85 =23.49m2 Diameter of the Distillation Column D=(4Ac/)^0.5 =(4 *23.49/3.14)^0.5 = 5.469m Height of the tray H= (Tray holdup / Ac) =(3/23.49) =12.77cm Column Length LC (ft) = 2.4 NT Where NT = Total no. of trays = 35 = (2.4 * 35) = 84 ft. Fd = Factor for Design type. Fm = Factor for radiant tube material. Fp = Factor for design Pressure. Fc = FmFp = 3.67

COST ESTIMATION Reboiler Heat Transfer area (AR) AR(ft2) = (QR / UR * TR) Where QR = Reboiler duty (Btu/hr) = 6.88 * 10^8 Btu UR = Overall heat transfer coefficient = 250 Btu/ hr * ft2 TR= Temperature Driving force = 28 AR = (6.88 * 10^8) / (250 * 28) = 98285.71ft2 Condenser Heat Transfer area (AC) AC(ft2) = (QC / UC*TC) Where QC = Condenser duty (Btu/hr) = -3.3 * 10^ 7 Btu UC = Overall heat transfer coefficient = 150Btu/hr * ft2 TC = Temperature Driving force =19 AC = (-3.37 * 10^7) / (150 * 19) = 11824.56ft2 Column cost [$] = (M&S) / 280 (101.9 DC1.066 LC0.802 (2.18 + FC)) LC = 84ft, FC = FMFD = 3.67 , DC = 5.469m = 17.94ft , M&S = 1108.1(2002,3 year payback) = (1108.1/280) (101.9 (17.94)^1.066 (84)^0.802(2.18 + 3.67) ) = $1788947.851 Tray cost [$] = (M&S) / 280 (4.7 DC ^1.55 LC FC) Where FC = FS + FT + FM = 1+1.8+1.7 = 4.5 = [(1108.1/280) (4.7 (17.94) ^1.55(84) (4.5)] = $617213.42 AR = 98285.71ft2 AC = 11824.56ft2 AT = AR + AC = 110110.27ft2 Heat Exchanger cost [$] = (M&S) / 280 (A ^ 0.65 (2.29 + FC)) For Reboiler: FC = (FD + FP) FM = (1.35 + 0) * 3.75 = 5.0625 = (1108.1 / 280) [98285.71) ^0.65 (2.29 + 5.0625)] = $51165.2 For Condenser: FC = (FD + FP) FM = (1 + 0) * 3.75 = 3.75

= (1108.1 / 280) [(11824.56) ^0.65(2.29 + 3.75)] = $10611.29 Considering total area AT = AR + AC = 110110.27 ft2 For Reboiler: =(1108.1 / 280 ) [(110110.27) ^0.65 (2.29 + 50.625 )] = $55086.356 For Condenser: = (1108.1 / 280) [ (110110.27)^0.65 (2.29 + 3.75)] =$45252.85 Cooling Water cost: [$1 year] = ($1.03 /1000gal) (1gal/8.34lb) (QC/30) (8150 h/year) =$33035.24

CONTROL STRUCTURE Control structure 1

CS1 in which three compositions are measured and controlled. The purities of the distillate and bottoms are controlled by manipulating reflux and reboiler heat-input, respectively. A composition inside the reactive zone of the column is measured and controlled by manipulating one of the fresh feeds. This loop permits the neat operation of the column (no excess of one of the reactants is used). Exact stoichiometric amounts of the two reactants must be fed, and this can only be achieved by some type of feedback of composition information about the amounts of the reactant components in the system. Any imbalance in the inflow of the two reactants will result in a gradual buildup of the reactant that is in excess. This will lead to an unavoidable drop in product purity when one or more of the manipulated variables hit a constraint.

In practical applications, it is impossible to simply ratio the two feed streams, as has been

proposed in some of the literature papers. Flow measurement inaccuracies and feed

composition changes doom to failure any ratio structure that does not somehow

incorporate information about compositions inside the system and feed this information

back to adjust fresh feed.

Control structure 2 CS5 in which only one composition is controlled (the column internal composition) and a temperature is controlled in the stripping section. This temperature controller maintains bottoms purity at or above its specified value by keeping light components from dropping out the bottom with the heavy product component (HOAc). The setpoint of the temperature controller must set high enough to make sure the bottoms purity is at or above its specification value under worst-case conditions. A RR control scheme is used, with the RR set high enough to guarantee the distillate purity under worst-case conditions

The CS2 control structure is a more practical approach since it does not require three

composition analyzers. In both CS1 and CS2 there is a direct production-rate handle, the

flowrate of one of the fresh feeds.

Control structure 3

A new structure, which was not studied in the previous work, features the use of two temperatures that manipulate the two fresh feeds. Reboiler heat-input is flow controlled and serves as the production rate handle. RR is controlled. The selection of the tray temperatures to control is a central issue in this structure The gain matrix between the inputs (the two fresh feed flowrates) and the outputs (the temperatures on all trays) is calculated numerically RESULTS

Control structure 1

The composition of methyl acetate in the distillate is controlled by the reflux flow rate.

The composition of the water in the bottoms is controlled by the heat input to the

reboiler. The acetic acid flow rate is flow controlled. The levels in the reflux drum and

the base of the column are controlled by the distillate flow rate and the bottoms flow rate,

respectively. The concentration of methanol on the tray it is being fed to (Tray 11) at the

bottom of the reactive zone is measured and controlled by manipulating the fresh

methanol feed flow rate.

The steady-state multiplicity analysis predicts that the system is open loop unstable. It

will drift to either a higher-conversion state or a lower-conversion state if no feedback

control is used. This structure controls purities at both ends of the column, and for the

high-conversion case, these purities are high. High product purities produce columns that

are highly nonlinear in their dynamic behavior and present difficult control problems.

In order to study the basics of this structure, we turn off the composition controller in the reactive zone. We are left with only the two composition controllers in the top and bottom of the column. It is also interesting to note that the system is closed loop stable when the third composition controller is put on automatic. It appears that this controller acts to reduce interaction. However, the performance of this structure is poor in the face of load disturbances and changes in set points. The level of conversion and purity set the degree of system's nonlinearity. This is an important design variable that affects the controllability of the column directly. This nonlinearity makes dual composition very difficult even in conventional distillation columns. The interaction of this design variable on the controllability of the column is

examined by changing the conversion and purity levels. Cases were studied over a range of conversions and product purities. Only one case is presented here in which the design conversion level is 95% and the design methyl acetate purity is 95 mol%. This 95/95 design should be compared with the high-conversion case with 99.2% conversion and 96 mol% methyl acetate purity. The 95/95 design was analyzed for input and output multiplicity as discussed before. Results predicted the system should be open loop stable for the control structure CS1.

Control structure 2

The temperature on the third tray and the composition of methanol in Tray 11 are

controlled RR is held constant. Even for the high-conversion/high-purity case, this

control structure handles disturbances in the acetic acid feed flow rate. It gives results for

a 20% step increase in the acetic acid flow rate. The system settles in around 4 h.

Although methyl acetate and water purities are not controlled directly, this structure is

able to indirectly maintain them very close to their desired levels. Temperature set point

changes of 2 K were tested. Even with these set point changes this structure is able to

hold the methyl acetate and water purities close to their desired levels. For these

temperature set point changes, methyl acetate ranges between 95.98% and 96.03% while

water ranges between 98.55% and 99.00%.

These tests indicate that the CS3 control structure provides effective control even at high

purity and conversion levels. Controlling an internal composition and one temperature

reduces loop interaction. Controlling an intermediate tray temperature instead of a

product purity significantly reduces the nonlinearity, even for high-purity levels. The

temperature loop sees much more linear dynamics than does a composition loop. It

should be kept in mind that there is no direct control of product compositions, so the

temperature controller set point and the reflux ratio must be set to handle worst-case

conditions. The low-conversion design is easier to control than the high-conversion

design as discussed above. CS2 is effective on the high-conversion design and would be

expected to perform as well in the low-conversion design.

Control structure 3

Temperature controllers on two trays in the column manipulate the two fresh feed flow

rates. The reflux drum level is controlled by the reflux flow rate, and the base level by the

bottoms flow rate The distillate flow rate is adjusted to give a constant RR. The heat

input is fixed. This control structure has the very significant advantage of not requiring

any composition measurement.

Singular value decomposition is used to select the most sensitive trays to be controlled,

which are Tray 3 and 15. Closed loop response tests show that this control structure

handles load disturbance very effectively, even for the high purity/conversion case

A 20% increase in the reboiler heat input (the production handle) is handled by this

structure very well. The temperature controllers increase both feeds flow rates by the

same magnitude which balances the increase in the reboiler heat input. The methyl

acetate and water purities at both ends are maintained close to the desired levels. Set

point changes of 2 K in the temperature controllers were tested. The results of these

changes show that the structure is not sensitive to inaccuracies in temperature sensors.

Under these temperature set point changes, methyl acetate ranges between 95.9% and

96.1% while water ranges between 98.2% and 99.2%.

Unlike CS1, this structure is effective for the high-conversion design. To explore the

effect of the conversion level on the controllability of this system, we tested the CS3

structure on the low-conversion design. Since this structure works well for the high-

conversion design, which presents a more difficult control problem, one would expect it

to perform well at low-conversion levels, and simulation results confirmed this. Since this

structure does not control product purities directly, large disturbances can drive products

off-spec unless the system is designed for purities that are higher than specifications.

More reactive trays, higher tray holdups or catalyst loading are required to handle the

worst-case conditions.

SAFETY AND SAFETY APPLIANCES

Nothing can be more important than the safety of the worker and safe conditions must be maintained at all the times. No amount of compensation can compensate the human life or the loss of any limb or part of the body. At the turn of the century, a great many human lives were lost due to unsafe working conditions but with the passage of time, the general awareness to ensure safe working conditions have been realized and the trend is to make any working place 100% accident free. To ensure this, both the supervisor and the worker must be vigilant at all times and any unsafe act or unsafe working condition must be reported to the higher authorities immediately. A good worker is basically a safe worker because unsafe practices cause untold misery to all concerned, the worker himself who is the victim, his family and the company for whom he works for. Medical care, no matter how advanced, can never bring back the original splendor and grace of the human limb, scarred or maimed by accidents. INDUSTRIAL ACCIDENTS An accident has been defined as an unplanned or unexpected event which causes or is likely to cause an injury. The basic theory of accident prevention takes the following sequence:

1. A personal injury. 2. An accident occurs as a result of unsafe action or exposure to an unsafe

environment. 3. Unsafe actions or unsafe mechanical or physical conditions exist only because of

faults of the part of person. 4. Faults of persons are inherited from the environment and reasons for the faults

are: a. Improper attitude. b. Lack of knowledge or skill. c. Physical unsuitability. d. Improper Mechanical or Physical environment.

ACCIDENT PREVENTION From the foregoing, it will be seen that the occurrence of an injury is the natural culmination of a series of events or circumstances which invariably occur in a fused and logical order.

Knowledge of the factors in the accident sequence guides and assists in selecting the point of attack in prevention work. It permits simplification without sacrifice of effectiveness. The most important point is that unsafe actions and unsafe mechanical or physical conditions are the immediate causes of accidents. The supervision and management can control the actions of employed persons and so prevent unsafe acts and so prevent unsafe acts and so also guard or remove unsafe conditions, even though previous events or circumstances in the sequence are unfavorable. The four factors that converge to cause accidents are:

a) Personal factor b) Hazard factor c) Unsafe factor d) Proximate causal factor

The solution under the following four factors would also lead to two steps. These are planning and organizing to

a) Prevent unsafe actions being committed. b) Remove unsafe mechanical or physical conditions.

Unsafe conditions Examples:

a) Operating without securing, warning etc. b) Operating or working at unsafe speed. c) Making safety devices inoperative. d) Using unsafe equipment. e) Unsafe loading, placing, mixing etc. f) Taking unsafe position or posture. g) Working on moving or dangerous equipment.

Unsafe Mechanical and Physical conditions example a) Inadequately guarded. b) Unguarded. c) Defective condition. d) Unsafe design or construction. e) Hazardous arrangement, process etc. f) Inadequate or improperly distributed ventilation. g) Unsafe dress or apparel. h) Unsafe method, processes, planning etc.

The most important means of accident prevention are:

a) Engineering Revision

b) Instruction c) Persuasion d) Appeal e) Personal adjustment f) Discipline

INDUSTRIAL VENTILATION AND LIGHTING: The main functions are:

1. To prevent harmful concentration of Aerosols. 2. To main reasonable condition of comfort for operators at workplace.

It maintains the body heat balance and to provide reasonable conditions of comfort. Ventilation should aim at:

1. Keeping the air temperature of the workroom low enough to enable body heat to be dissipated by convection.

2. Preventing excessive humidity so as to assist body heat loss by evaporation. 3. Regulating the rate of air movement so that loss of body heat by convection is

facilitated. The amount of ventilation depends generally on the following factors:

1. Size and type of room or building and its usage. 2. Duration and type of occupants and their activities. 3. Heat gains from Sun, hot manufacturing. 4. Temperature conditions. 5. The operators of the ventilating system.

Types of Ventilation

a) Natural ventilation. b) Mechanical ventilation.

Natural Ventilation: Forces which operate to induce natural ventilation in building are due to

a) Pressure exerted by outside wind. b) The temperature difference of the air within and without the building.

Types

i. Cross Ventilation

ii. Roofed Ventilation iii. Cool type roof Ventilation

Mechanical Ventilation: It is brought about by either one or both of the following two methods:

a) Ventilation through windows or other openings owing to the suction created by the exhaust air.

b) Positive ventilation by means of a fan or blower. Types

I. Exhaust Ventilation. II. Combined plenum and extraction systems.

III. Mechanical roof ventilators. PERSONAL PROTECTIVE DEVICES: Protective devices are required by regulation; the employers are required to provide it free cost and also be responsible to ensure its usage, maintenance and renewal. Once it is decided to use protective devices, we must

1. Select the proper type of device. 2. Make sure that the employees use and maintain these correctly.

For selection of device, two criteria should be used:

1. The degree of protection a particular piece affords under varying condition. 2. The ease with which it may be used.

Protective devices are divided into two groups.

1. Respiratory devices. 2. Non-Respiratory devices.

SAFETY APPLIANCES:

1. Helmets: Every employee working inside the factory should always wear the safety helmet to avoid head injuries. No person will be allowed to enter any plant building without the helmet.

2. Safety Goggles: The goggles must be worn while entering the process areas. Special goggles must be worn for gas welding and grinding operations.

3. Safety Shoes: All employees working in the plant should always wear safety

shoes as a matter of rule rather than exception. When required Gumboots must be used while handling acids and alkalies.

4. Hand Gloves: While operating any equipment or valve and also while executing

any maintenance work, the employees should wear appropriate type of safety gloves.

5. Dust Mask: While working in a dusty atmosphere, the employees must always

wear dust masks to prevent dust and fumes from entering the sensitive respiratory organs, which can cause a lot of irritation and misery and in the long run painful and incurable diseases.

6. Gas mask with chemical cartridge: This is to be used when doing any

maintenance work which may involve leakage of gases like chlorine, Hydrofluoric acid gas, sulphurdioxide, oleum, fumes etc.

7. Face shield: All the operation and maintenance staff doing plant operations or

plant maintenance should always wear these items particularly while handling hazardous materials under pressure.

8. Plastic Aprons: This handling with the hood gives protection to the operation and

maintenance staff while handling dangerous acids and other hazardous chemicals particularly when there is possible leakage.

9. Safety showers: The safety showers are provided at strategic points in the main

plant to enable the employees who have come in contact with acid or any hazardous material to immediately wash the affected parts with running water. As soon as a person steps on the shower platform the water spray will function automatically and this will enable the affected person to wash the affected part immediately.

Inspite of these safety appliances, the companys medical center is equipped to meet any emergency and any employee coming in contact with the acid or any hazardous chemical must be treated at medical center immediately.

PROCESS FLOW SHEET FOR REACTIVE DISTILLATION COLUMN

EFFECT OF REFLUX RATIO ON CONVERSION OF ACETIC ACID

COMPARISION OF TWO MODELS W.R.T. MOLE FRACTION OF VARIOUS COMPONENTS AND NUMBER OF TRAYS

EFFECT OF DAMKOHLER NUMBER ON CONVERSION OF

ACETIC ACID

CONVERSION OF ACETIC ACID AND AVERAGE STAGE VOLUME HOLDUP FOR DIFFERENT Da

Volume Holdup Distribution and Reactive Status throughout the Column Based on 280.0 kg mol MeOAc/h.

EFFECT OF REFLUX RATIO ON EQUILIBRIUM DESIGN. FIG. SHOWS THE NUMBER OF STAGES REQUIRED AS A FUNCTION OF REFLUX RATIO AT THREE DIFFERENT PRESSURE

INFLUENCE OF REFLUX RATIO ON THE COMPOSITION OF MeOAc AND WATER IN DISTILLATE AND BOTTOM

RESPECTIVELY FOR DIFFERENT VALUE OF Da

HEAT EFFECT MODEL

CONTROL STRUCTURE 1

CONTROL STRUCTURE 2

CONTROL STRUCTURE 3

CONCLUSION Methyl Acetate is commercially important chemical as far as Reactive Distillation technology is concerned. The demand for Methyl Acetate by the various industries has led to its increased production rate. Methyl Acetate is still difficult to synthesize, mainly for kinetic reasons and application of computer simulation makes this techniques price much higher. This project has analyzed the salient features of the process of manufacture by Reactive Distillation. It has also dealt with design aspects as well as control structure for the Methyl Acetate production by Reactive Distillation.

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ABSTRACT