Simulation of Manufacturing Process of Nitrobenzene

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

INDEX SR.NO.

CONTENTS

PAGE NO.

1

Chapter 1

4

2

Introduction Chapter 2

6

Literature Review 2.1. Process For Production Of Nitrobenzene 2.2. Selection Of Process 2.3. Manufacturing Process Of Nitrobenzene 2.4. Chemical And Physical Properties 3

Chapter 3

15

4

Thermodynamic Feasibility 3.1. Reaction Data For Formation Nitrobenzene 3.2. Calculations Chapter 4

23

5

Design Of Distillation Column Chapter 5

29

Simulation Using Aspen 5.1 Introduction to Aspen 5.2 Starting With Process Simulation 6

Chapter 6

49

Result summary 6.1 Material Balance Over Reactor 6.2 Material Balance Over Decanter 6.3 Material Balance Over Distillation Column 6.4 Overall Material Balance 7

Chapter 7

53

8

Conclusion Chapter 8

55

9

References APPENDIX A

58

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FIGURE INDEX FIGURE

FIGURE NAME

PAGE NO.

NO. 1

2.1 Manufacturing Process Of Nitrobenzene

11

2

4.1 Rectification section

27

3

4.2 Stripping Section

28

4

5.1 Flowsheeting

34

5

5.2 Title Page

35

6

5.3 Component Entry

36

7

5.4 Selection Of Property Method

37

8

5.5 Mixer

38

9

5.6 Reactor

39

10

5.7 Reaction Input

40

11

5.8 Decanter

41

12

5.9 Distillation

42

13

5.10 Result Summary

43

14

5.11 Strem Result Over Mixer

44

15

5.12 Strem Result Over Reactor

45

16

5.13 Strem Result Over Decanter

46

17

5.14 Strem Result Over Distilation Column

47

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TABLE INDEX TABLE NO.

TABLE NAME

PAGE NO

1

2.1 Properties Of Benzene

11

2

2.2 Propetries Of Suphuric Acid

12

3

2.3 Properties Of Nitric Acid

13

4

2.4 Properties Of Nitrobenzene

14

5

2.5 Enthalpy Data At Standard State

16

6

2.5 Entropy Data At Standard State

16

7

2.5 Specific Heat Data At Standard State

17

8

5.1 Stream Result Overall

48

9

6.1 Material Balance Over Reactor

50

10

6.2 Material Balance Over Decanter

50

11

6.3 Material Balance Over Distillation Column

51

12

6.4 Overall Material Balance

52

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CHAPTER-I

INTRODUCTION

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INTRODUCTION Nitrobenzene (some time called the oil of Mira-bane) C6H5NO2 is pale yellow liquid with an odour that resembles bitter almonds, Depending upon the compounds purity. Its colour various from pale yellow to yellowish brown liquid boiling at 483 K (101 KPa) and freezing at 287.7 K as bright yellow crystals. It is quite toxic to human system. Nitrobenzene was first synthesized in 1834 by treating benzene with fuming nitric acid. And it was first produced commercially in England in 1856. The elective‟s ease of aromatic nitration has contributed significantly to the large and varied industrial application of nitrobenzene, other aromatic nitro- compounds and their derivatives A continues process for the production for the production has been developed by M/S.Biazzi of Switzerland. The advantages of this process are lower concentration of mixed said used and higher reaction rate. The reactants are kept mixed under high speed agitation (600 rpm) and cooling due to control feed rate and rapid agitation. The reaction time is about 15 – 20 minutes, where the yield is higher than 99% of theoretical

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.[4][5]

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CHAPTER-II

LITERATURE REVIEW 2.1. Process For Production Of Nitrobenzene 2.2. Selection Of Process 2.3. Manufacturing Process Of Nitrobenzene 2.4. Chemical And Physical Properties

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LITERATURE REVIEW 2.1 PROCESS FOR PRODUCTION OF NITROBENZENE Nitrobenzene is manufactured by nitration of benzene using mixture of Nitric and sulphuric acid. Nitration can be done by two processes. Via. [1]

Batch Process.

[2]

Continuous process.

2.1.1 BATCH PROCESS In batch process the nitrator is charged with benzene and mixed acid (HNO 3 32 – 39 %, H2SO4 60 -53 %, H2O 8%) is added slowly below surface of benzene. The rate of agitation is such that both the acid & benzene phases are in intimate contact. The feed rate of mixed acid and the rate of cooling are such that during the entire period of acid addition, the temperature of nitrator is maintained at 323 -328 K. after complete addition of acid, The acid and organic layers are drained into separate vessel from where spent acid is drawn off for reconcentration. This crude product is washed with water to remove contamination in the nitrobenzene and the aqueous sodium carbonate solution to remove small traces of nitro phenols formed during nitration. Particularly when the product is to be further nitrated, removal of nitrophenolic impurities is important, since they way undergo unwanted side reaction during subsequent nitration. The product is further purified by distillation and the yield is 95 – 98% of the theoretical.

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[4][5]

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2.1.2 CONTINUOUS PROCESS A continuous process for the production of nitrobenzene has been developed by M / S.Biazzi of Switzerland. The advantages of this process are the lower concentration of mixed acid is used and higher reaction, rates though the sequence of operations is the same as in bath process. Continuous nitrator with capacity of 150 lit. Can produce as a 7500 capacity batch nitrator, but at the same time of quantity a reactants in nitrator is considerably small, unlike the batch process. Mixed acid and benzene are fed to nitrator in such that all nitric acid is utilized for nitraton of benzene. The reactants are kept mixed under high speed agitation (600 rpm) and cooling. Due to the controlled feed rate and rapid agitation, the reaction time is 15 to 20 minutes only at reaction mixture is drawn off side of nitrator. The mixture is sent to decanter, where the, product is separated from spend acid for further processing.

[4][5]

2.2 SELECTION OF PROCESS Continuous process, in general, will be found to have the following to have the following advantages over batch process. [1]

Lower Capital Cost.

[2]

Safety

[3]

Labour Usage.

2.2.1 LOWER CAPITAL COST For a given rate of production, the equipment needed for a continuous process is smaller than for a batch process. This is usually the striking different between the two types of process. The reason for that is obvious since, it is not necessary to accumulate material in a continuous process anywhere; the vessel is designed with capacity dictated by the rate of reaction process step which they must accommodate. Alternatively, because of relatively FAMT ,Ratnagiri

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small size of continuous process equipment, it is often possible and excessively high in cost for batch scale equipment. Thus for example Corrosion resistance alloys such as appropriate S.S. may be detected for a batch plant because of cost. In case of S.S. corrosion problems are completely eliminated.

2.2.2 SAFETY Because of relatively small size of continuous process equipment, there is less material in process at any time than at certain in a comparable batch process. At the completion of batch process nitration and during its normal separation of product from spent nitrating acid, the entire batch of an often hazardous compound will be present in the equipment. In the continuous process, only as much material need be present in hazardous conditions as needed to again sufficient reaction of process time. In case of high explosive made by nitration, this process has inherent safety factor is very attractive

[3].

2.2.3 LABOUR USAGE In the nitration filed the continuous process is usually more efficient labour usage than a batch process. This is particularly true for small or medium scale production and for hazardous products, since continuous processing

minimizes the amount the material in

process on average. It is often possible to handle operations at one place that efficiency tends to disappear as the scale of operations increases.

2.3 MANUFACTURING PROCESS OF NITROBENZENE Nitrobenzene is manufactured commercially by direct nitration of benzene using a mixture of nitric acid and sulphuric acid, which is commonly referred to as mixed acid for nitrating acid. The reaction is conducted is specially build cast iron are S.S. reaction vessel FAMT ,Ratnagiri

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provided with agitator, external jacket and internal coils. Since two phases ate formed in reaction mixture and reactant ate distributed between them. Rate of nitration is controlled by transfer between the phases as well as by chemical kinetics. Benzene used is of commercial quality. Mixed acid contain of 56 – 60 wt % H2SO4, 20 – 26 wt% nitric acid and 15 – 18% water. Sulphuric acid used is of 94% - 98% concentration and nitric acid commercial grade of 55% - 60% concentration. Benzene is charged to the nitrator. Mixed acid is slowly added on surface of benzene from dosing tank with stirring. The ratio of mixed acid to benzene is kept around 2.5 : 1.0. The temperature mass is maintain initially at 25 – 30°C. So by high speed agitator and proper cooling coils reaction temperature can maintained upto 50 – 55°C. By obvious agitation, the interfacial area, of the reaction mixture is maintained as high as possible, thereby enhancing the mass transfer of reactants and cooling coils, which control the temperature of highly .[4]

exothermic reaction

A slight excess of benzene usually is fed into the nitrator of ensure that the nitric acid in mixed acid is formation of denitrobenzene. Reaction time is only 15 – 20 minutes because of rapid and efficient agitation. Nitrobenzene and spent acid are removed from the side reactor and send to decanter unit. Organic and aqueous layers are formed, where two layers are separate in 10 to 20 minutes. The aqueous phase or spent acid is drawn from the bottom and is concentrated in a sulphuric acid is drawn from the bottom and is concentrated in a sulphuric acid reconcentration step or is recycled to the nitrator, where it is mixed nitric acid and sulphuric acid immediately prior to being fed into nitrator. The crude Nitrobenzene can used directly for production of aniline if required, otherwise the crude nitrobenzene flows through a series of washer – separators, where residual acid is removed by washing with a dilute sodium carbonate solution followed by final washing with water.The product is then distilled to remove benzene and the nitrobenzene can be refined by vacuum distillation. Theoretical yields are 96 – 99 %. The nitration process is unavoidably associated with the disposal of waste water from washing step. This water principally contains Nitrobenzene, some sodium carbonate and inorganic salts from the neutralized spent FAMT ,Ratnagiri

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acid which was present in the product. Generally, the waste water is extracted with benzene to remove the nitrobenzene and the benzene that is dissolved in the water is stripped from water prior to the final waste treatment.

[6]

Fig No-2.1 Manufacturing Process Of Nitrobenzene

2.4 CHEMICAL AND PHYSICAL PROPETRIES

[7]

2.4.1 PROPERTIES OF BENZENE PHYSICAL PROPERTYPROPERTY

VALUE

Molecular Weight

78.11

Melting Point, °C

5-533

Boiling Point, °C

80.1

Density, Kg/cum

873.7

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Refractive index

1.49792

Viscosity (absolute, at 20°C)

0.6468

Flash point, °C

-11.1

Heat of fusion, kJ/kmole

9.847 Table No-2.1 Properties Of Benzene

CHEMICAL PROPERTY

[14][15][16]

REACTION WITH WATER:Water and benzene are non-reactive unless high and pressure are applied.

2.4.2 PROPETRIES OF SUPHURIC ACID PHYSICAL PROPERTY-

PROPERTY

VALUE

Molecular Weight

98.08

Boiling Point, °c

330.0

Density, at 20°C, gm/cc

1.834

Flash Point

None

Vapour pressure at 145°C mmHg

1.0

TLV, mg/cum.

1.0

Freezing Point, °C

10.48 Table No-2.2 Propetries Of Suphuric Acid

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CHEMICAL PROPERTY

[14][15][16]

REACTION WITH WATER:Has great affinity for water, absorbs atmospheric moisture and absorbs water from organic material causing charring. Sulphuric Acid reacts with water vigorously liberating large amount of heat. REACTION WITH METAL AND OTHER ELEMENTS:When cold, it reacts with metal including platinum when not, reactivity is intensified. Sulphuric acid on reaction with metals causes liberations of flammable hydrogen. Cu + H2SO4 →

CuSO4 + H2

Zn + H2SO4 →

ZnSO4 + H2

2.4.3 PROPERTIES OF NITRIC ACID PHYSICAL PROPERTYPROPERTY

VALUE

Molecular Weight

63.02

Boiling Point

86.0

Melting point °C

-42.0

Density, at 20°C,gm/cc

1.502

Flash point

None

Solubility in water

Soluble in water

TLV, mg/cum.

2-5

Freezing point, °C

10.48 Table No. 2.3 Properties Of Nitric Acid

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CHEMICAL PROPERTIES :REACTION WITH WATER :Nitric Acid reacts with water to produce heat, toxic and corrosive fumes. REACTION WITH METALS AND OTHER ELEMENTS :Nitric acid is corrosive to most of metals like zinc to form nitrate with evolution of hydrogen. Cu + 2HNO3 → Cu (NO3)2 + H2 Zn + 2HNO3 → Zn (NO3)2 + H2

2.4.4 PROPERTIES OF NITROBENZENE PHYSICAL PROPERTYPROPERTY

VALUE

Molecular Weight

123.0

Boiling Point, °C

201.9

Melting point, °C

5.85

Density, at 20°C, gm/cc

1.344

Flash point

88.0

Auto ignition temp., °C

482.0

Explosive limit (at 93°)

1.8 Vol % in air

Vapour density

4.1 Table No. 2.4 Properties Of Nitrobenzene

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CHAPTER III

THERMODYNAMIC FEASIBILITY 3.1. Reaction Data For Formation Nitrobenzene 3.2. Calculations

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THERMODYNAMIC FEASIBILITY 3.1 REACTION DATA FOR FORMATION NITROBENZENE[7] REACTION:C6H6

+

HNO3



C6 H5 NO2 +

H2 O

DATA :HEAT OF FORMATION

( kcal/gmole)

Benzene (liquid)

11.71

Nitrobenzen (liquid)

13.76

Nitric acid (liquid)

-41-61

Water (liquid)

-68.315 Table No. 2.5 Enthalpy Data At Standard State

ENTHROPY

kJ/(kmol.K)

Benzene (liquid)

172.915

Nitrobenzene (Liquid)

364.61

Nitric acid (liquid)

110.113

Water (liquid)

69.92 Table No. 2.6 Entropy Data At Standard State

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SPECIFIC HEAT AT 25 °C

kJ/(kmol.K)

Benzene (liquid)

91.73

Nitrobenzene (liquid)

185.361

Nitric acid (liquid)

111.113

Water (liquid)

75.362 Table No. 2.7 Specific Heat Data At Standard State

3.2 CALCULATIONS[11] From heat of formation data: ∆HR = HPRODUCTS - HREACTANTS = ( HNB + HWATER ) - ( HBENZENE + HNITRIC ACID ) = ( 13.76 – 68.315 )

- (11.71 – 41.61)

∆HR = -24.655 kcal/gmmole

∆HR = -103157 kJ/(kmol)

From specific heat data:

Cpavg = CpPRODUCT - CpREACTANT = ( CpNB + CpWATER ) - ( CpBENZENE + CpNITRIC ACID ) FAMT ,Ratnagiri

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= ( 185.361 + 75.362 ) - ( 91.73 + 111.113 ) Cpavg =

57.88 kJ/(kmol.K)

From entropy data:

∆S

= SPRODUCTS - SREACTANTS = ( SNB + SWATER ) - ( SBENZENE + SNITRIC ACID ) = ( 364.61 + 69.92 ) - ( 172.91 + 110.113 )

∆S

= 151.507 kJ/(kmol.K)

For ∆HR At Reaction Temperature: ∆HR = ∆H° - Cp.T ∆H° = ∆HR + Cp.T = -103157 + 57.88 × 298 = -85908.76 kJ/(kmol) Therefore, ∆HR at 323 K, ∆HR = -85908.76 – ( 57.88 ×323 ) = -104604 kJ/(kmol)

Similarly, for ∆S At Reaction Temperature: ∆S = ∆S° + CplnT FAMT ,Ratnagiri

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∆S°= ∆S - CplnT = 157.507 - 57.88 ×In (298) = -178.24 kJ/(kmol.K) Therefore, ∆S at 323 K, ∆S = -178.507 + 57.88 ×In (323) = 156.17 kJ/(kmol.K)

Now using Standard free energy change relation, ∆G° = ∆HR - T∆S = -104604 – (323×156.17) = -155046.91 kJ/(kmol) Since ∆G° is negative it can thermodynamically feasible Reaction By using Van‟t Hoff Isotherm, ∆G° = -RT lnKp lnKp = = = 57.73 Kp = 1.18 ×1025 Since Kp = Kx×P∆n For our reaction, ∆n = (1+1)-(1-1) FAMT ,Ratnagiri

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= 0 Kp =

×P0

Kp =

= Kx

Now,taking material balance, Composition of mixed acid(Weight basis):

25%

Nitric acid

58%

Sulphuric acid

17%

Water

Consider 1000 kg of mixed acid.

Nitric acid 250 kg

=

3.97 kmole

Water 170kg

=

9.44 kmole

Sulphuric acid 580 kg

=

5.92 kmole

----------------------------

Total moles

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19.33 kmole

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Mole % of

Nitric acid

=

20.5 %

Water

=

48.8 %

Sulphuric acid

=

30.7 %

But benzene mixed acid

1---------------------------->

400kg

19.314

Moles of benzene

=

1

---------------->

3.766 moles of

Moles of acid

=

3.766

X

0.205

= 0.772 moles

Reaction of nitrobenzene C6H6 FAMT ,Ratnagiri

+

HNO3

→

C6 H5 NO2 +

H2 O Page 21

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

Initially

1

0.772

Reacted

X

X

At. equilibrium

Kx

(1-X)

(0.772-X)

0

0

X

X

X

X

X2

=

----------------------(1 - X) (0.772 - X)

X2 1.18 ×1025 =

---------------------------------------

X2 - 1.73 X + 0.73

X2 - 1.772 X + 0.772 X

=

=

0

0.772

Extent of reaction = 0.772

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CHAPTER IV

DESIGN OF DISTILLATION COLUMN

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DESIGN OF DISTILLATION COLUMN

[10]

Basis ; 1 hour of operation. Mass flow rate of feed = 740.75 kg/hr. Mass flow rate of distillate = 32.3 kg/hr. Mass flow rate of bottom = 708.38 kg/hr. Xf = = 0.317/1.401 = 0.226 Xd = 2.8075/3.048 = 0.92 Xw = 0.0036/1.08667 = 0.003 Average Molecular weight of feed = 110.556 Feed rate = 593.568 kg/hr Slope of q-line ; We know that q = Hg-Hf / Hg-Hl q=1 slope of q-line: slope of q-line = q/q-1 = 1/1-1 Tan-1(α) = 0 FAMT ,Ratnagiri

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q line is st.line Xd / Rm+1 = 0.05 Rm+1 = 1/0.05 Rm+1 = 20 Rm = 19 R = 1.2 Rm R = 22.8 ∼ 23 Xd = 1 = 0.042 Rm+1= 23+1 =24

From Mc-cabe Thile Graph

X 0 0.01 0.02 0.03 0.045 0.07 0.10 0.155 0.20 0.30 Y 0 0.03 0.485 0.63 0.74 0.82 0.88 0.92 0.94 0.964 Ideal Plate = 16 (From Graph) Actual Plate = Ideal/n = 16/0.6 Actual Plate = 26.66 Height: Plate Spacing = 450 mm = 0.45m Ht = (Actual Plate-1)×0.45 + 2(0.45) = 12.45m

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Diameter : Vap rate = v = D(R+1) = 0.0087(23+1) n = 0.21 kmole/hr Top Column : Vol.rate = nRT/P = 0.21×8.314×103×(82+273)/ 1.01325×105 = 6.1170 m3/hr Vol rate = 1.7×10-3 m3/sec Velocity = 1 m/sec Area = Vol rate / Velocity = 1.7×10-3 /1 = 1.7×10-3 m2 Area = π D2 /4 D2 = 4A /π D = 0.047 m Bottom column: Vol.rate = nRT/P = 0.21×8.314×103×(210+273)/ 1.01325×105 = 8.32 m3/hr Area = Vol .rate / Velocity Velocity = 1 m/sec Area = 2.31×10-3 m2 2

A=πD /4

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D2 = 4A /π D = 0.054 m Both diameters are approximately same , we choose the larger diameter (i.e) bottom diameter Bottom diameter D= 0.054 m DESIGN SUMMARY Ideal plate = 16.00 Actual Plates = 26.66 Column Height = 12.45 m Column Diameter = 0.054 m

Fig No. 4.1 Rectification Section

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Fig No-4.2 Stripping Section

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CHAPTER V

SIMULATION USING ASPEN

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SIMULATION USING ASPEN 5.1 INTRODUCTION TO ASPEN[8] 5.1.1

What is a Process Flowsheet? Process flowsheet can simply be defined as a blue print of a plant or part of it. It

identifies all feed streams, unit operations, streams that inter-connect the unit Operations and finally the product streams. Operating conditions and other technical Details are included depending on the detail level of the flowsheet. The level can vary from a rough sketch to a very detailed design specification of a complex plant. For steady-state operation, any process flowsheet leads to a finite set of algebraic equations. For a case where we have only one reactor with appropriate feed and Product streams the number of equations may be manageable by manual hand calculations or simple computer applications. However, as the complexity of a flowsheet Increases and when distillation columns, heat exchangers, absorbers with many purge and recycle streams come into the picture the number of equations easily approach many ten thousands. In these cases, solving the set of algebraic equations becomes a Challenge in it. However, there are computer applications called process flowsheet simulators specialized in solving these kinds of large equation sets. Some well-known process flowsheet simulators are Aspen Plus, ChemCad and PRO/II.These products have highly refined user interfaces and on-line component databases. They are used in real world applications from interpreting laboratory scale data to monitoring a full scale plant.

5.1.2 Advantages of using a process flowsheet simulator The use of a process flowsheet simulator is beneficial in all the three stages of aPlant: research & development, design and production. In research & development they help to cut down on laboratory experiments and pilot plant runs. In design stage they enable a speedier development with simpler comparisons of various alternatives. FAMT ,Ratnagiri

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Finally, in the production stage they can be used for risk-free analysis of various what-if scenarios

5.1.3 Disadvantages of using a process flowsheet simulator Disadvantages of using a process flowsheet simulatorManual solution of a problem usually forces someone to think deeper on theProblem, find novel approaches to solve it, and evaluate and re-evaluate the Assumptions closer. A drawback of process flowsheet simulators may be cited as the Lack of this detailed interaction with the problem. This might act as a double edged Sword. On one side it hides the complexities of a problem so you can concentrate on the real issues at hand. On the other side this hiding may also hide some important Understanding of the problem as well,

[8]

5.1.4 History In 1970s the researchers at MIT‟s Energy Laboratory developed a prototype forProcess simulation. They called it Advanced System for Process Engineering (ASPEN).This software has been commercialized in 1980‟s by the foundation of a companyNamed AspenTech. AspenTech is now a publicly traded company that employs 1800People worldwide and offers a complete

integrated solution to

chemical

processIndustries.This sophisticated software package can be used in almost every aspect of processengineering from design stage to cost and profitability analysis. It has a built-in modelLibrary for distillation columns, separators, heat exchangers, reactors, etc. Custom orPropriety models can extend its model library. These user models are created with FORTRAN subroutines or Excel worksheets and added to its model library. Using VisualBasic to add input forms for the user models makes them indistinguishable from theBuilt-in ones. It

has a

built-in property databank for thermodynamic and

physicalParameters. During the calculation of the flow sheet any missing parameter can beestimated automatically by various group contribution methods.In this workshop we will only scratch the surface of this tool. We will discuss itsAdvantages and disadvantages. Our focus will be on reactors and our goal is to provideyou with a smooth and simple introduction

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to Aspen Plus. Let‟s start our workshop bylearning how to access Aspen Plus at the University of Michigan.

5.1.5 What is an Aspen plus Process Simulation Model? A process consists of components being mixed, separated, heated, cooled a Converted by unit operations. These components are transferred from unit to unitthrough process stream you can translate a process into an Aspen plus process simulation model bydoing the following steps: 1. Define the process flowsheet configuration. To do this step, you: Define the unit operations in the process Define the process streams that flow between these unit operations Select unit operation models from the Aspen Plus model library to Describe each unit operation 2. Specify the chemical components in the process. You can take these Components from the Aspen Plus databanks, or you can define them. 3. Choose appropriate thermodynamic models from those available in Aspen Plus, to represent the physical properties of the components and mixtures in The process. 4. Specify the component flow rates and the thermodynamic conditions (for Example, temperature and pressure) of feed streams to the process. 5. Specify the operating conditions for the unit operations in the flowsheet. When you have specified this information, you have defined an Aspen Plus Process simulation model of your process. You can use the Aspen plus processSimulation model to predict process behaviour. FAMT ,Ratnagiri

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With

Aspen

Plus

you

can

interactively

change

specifications,

such

as

flowsheetConfiguration, operating conditions, and feed compositions, to run new cases andAnalyse alternatives. In addition to process simulation, Aspen Plus allows you to perform a wide rangeof other tasks such as estimating and regressing physical properties, generatingCustom graphical and tabular output results, data-fitting plant data toSimulation models, costing your plant, optimizing your process, and interfacingResults to spread sheets.

5.1.6 Why Use Process Simulation?

Process simulation allows you to predict the behaviour of approves by using basicEngineering relationships, such as mass and energy balances, and phase and Chemical equilibrium. Given reliable thermodynamic data, realistic operating Conditions, and rigorous equipment models, you can simulate actual plant Behaviours. Process simulation enables you to run many cases conduct "what if" Analyses, and perform sensitivity studies and optimization runs. With simulation, you can design better plant and increase profitability in existing plants.

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

5.2 STARTING WITH PROCESS SIMULATION 1] First stating with Blank Simulation we must design our required flowsheet with proper stream names & block names .each stream is properly connect to the proper unit.After doing this we click Next to the required input step by step.

Fig No 5.1-Flowsheeting FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

2] we input Title of our simulation with all units are in SI units.

Fig No 5.2-Title Page

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

3] We input our components that takes part in process operation,all conventional types It involves nitrobenzene,benzene,water,sulphuric acid,nitric acid.

Fig No 5.3 –Component Entry

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

4] This is the step where you put property method.From our investigation in aspen running plant we know that NRTL is the best property method applied where large water usage in operation or process.

Fig No 5.4- Selection Of Property Method

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

5] Then we come at Block of Mixer where we fed H2SO4, H2O, HNO3 in desired proportion to make Mixed acid.In mixer we operate at normal temperature & pressure.

Fig No 5.5-Mixer

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

6] Next to we selected stoichiometric reactor since we know only the extent of reaction & stoichiometric reaction coefficients operating at 50 °C

Fig No 5.6-Reactor

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

7] Insert our reaction in new option with correct coefficient

Fig No 5.7 Reaction Input

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

8] Moving on to decanter we fed extra water to this unit in order to remove sulphuric acid effectively.we select nitrobenzene is our key component

Fig No 5.8-Decanter

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

9] Distillation column is where we obtained our desired product in Bottom stream from data we find out optimum feed ratio

Fig No 5.9- Distilation

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

10] Final next to Run the simulation Summary obtained,

Fig No 5.10-Result Summary

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

11 Now we take stream result over each block First is Mixer which has 3 inlet stream & 1 outlet stream

Fig No 5.11-Strem Result Over Mixer

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

12] Second block is stoichiometric reactor where we provide benzene with mixed acid in 1:2.5 proportion.Crude nitrobenzene is obtained .

Fig No 5.12-Strem Result Over Reactor

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

13] Third stream result over Decanter

Fig No 5.13 -Strem Result Over Decanter

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

14] Last stream result over a distillation column in the bottom stream we get our final product

Fig No 5.14 -Strem Result Over Distilation Column

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

15] Steam result obtained from overall result

Table No 5.1-Strem Result Overall

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

CHAPTERVI RESULT SUMMARY

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

RESULT SUMMARY 6.1 MATERIAL BALANCE OVER REACTOR SR. NO

COMPONENTS

INPUT (kg/hr)

OUTPUT (kg/hr)

1

BENZENE

400

91.07

2

NITROBENZENE

-

486.2

3

WATER

241.84 1000

4

NITRIC ACID

5

SULPHURIC ACID

0.89 580

TOTAL

1400

1400

Table No.6.1 Material Balance Over Reactor

6.2 MATERIAL BALANCE OVER DEACNTER INPUT (kg/hr) SR. NO

COMPONENTS

1

BENZENE

OUTPUT (kg/hr) SPENT ACID STREAM

ORGANIC PHASE

91.07

2.09

88.98

2

NITROBENZENE 486.2

9.88

476.32

3

WATER

241.84+2000

2241.43

0.41

4

NITRIC ACID

0.89

0.89

-

5

SULPHURIC ACID

580

553.51

26.49

3400

3400

TOTAL

Table No.6.2 Material Balance Over Decanter

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

6.3 MATERIAL BALANCE OVER DISTILLATION COLUMN

INPUT (kg/hr) SR. COMPONENTS NO

OUTPUT (kg/hr) TOP PRODUCT

BOTTOM PRODUCT

1

BENZENE

88.98

78.6

10.38

2

NITROBENZENE

476.32

-

476.32

3

WATER

0.41

0.41

-

4

NITRIC ACID

-

-

-

5

SULPHURIC ACID

26.49

-

26.49

592.2

592.2

TOTAL

Table No.6.3 Material Balance Over Distillation Column

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

6.4 OVERALL MATERIAL BALANCE

SR.

COMPONENTS

INPUT

OUTPUT

(kg/hr)

(kg/hr)

TOTAL

NO

SPENT

TOP PDT

BOTTOM

ACID

STREAM

PDT

STREAM

STREAM

1

BENZENE

400

2.09

78.6

10.38

2

NITRIC ACID

250

0.89

-

-

3

SULPHURIC

580

553.51

-

26.49

ACID 4

WATER

170 + 2000

2241.43

0.41

-

5

NITROBENZENE

-

9.88

-

476.32

TOTAL(kg/hr)

3400

3400

Table No. 6.4 Overall Material Balance Conversion of benzene is 77 % Purity of Nitrobenzene in bottom product is 92.8 %.

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

CHAPTER VII

CONCLUSION

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

CONCLUSION It is very important for any process to kow that parameters like composition, streams, temperature, pressure etc may affect the production rate.One must have perform pilot plant in order to know this, so each time we need manual calculation to get desired results,this is so time consuming. So the use of simulaters like ASPEN, CHEMCAD are helpful.Simulation & modeling useful in doing risk analysis in production process. In our project we simulate continuous process for nitrobenzene production using benzene nitration.In that we know about how actually parameters mention above may affect each stream.For example we first added calculated amount of extra water to decanter,but from that action we know that how much extent it affect the each stream,so we are finaly able to find the optimum amount of water required for operation. Generally it is difficult to obtain desired result manually that is why we simulate it using ASPEN PLUS .And we searching new techniques as possible in order to get the optimum production. Also we can check where is the opportunity to increase the conversion & reduce the losses as well as maintenance cost.

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

CHAPTER VIII

REFERENCES

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

REFERENCES Books, [1]B.I. Bhatt & S.M. Vora. “ Stoichiometry”, Tata – Mcgraw Hill Publishing Co. Ltd. [2]Dryden C. E., “Drydens Outline Of Chemical Technology”. East – West Press Pvt. Ltd;(536) [3]G. D. Muir, “Hazardous In Chemical Laboratory” The Chemical Society, London. [4]Kirk – Othmer „Encyclopedia Of Chemical Technology‟.Vol. – 15. Wiley Intenscience Publications, 1979.(138-139) [5]P.H.Groggins .„Unit Process In Porganic Synthesis.‟ Mcgraw – Hill International Book Co. [6]R.Norris Shreve & Joseph A. Brink Jr.„Chemical Process Industries‟.Mcgraw – Hill International Publications.(776-778) [7]Robert H. Perry „Perry‟s Chemical Engineering Handbook‟.Mcgraw – Hill International Publications.(642-644) [8]Amiya K. Jana. „Process Simulation And Controle Using Aspen‟.PHI Learning Private Limited ,Second Edition ,2012 [9]Bhattacharya A., Purohit V. C., Suarez, V.; Tichkule, R; Parmer, G.; Rinaldi, F. (2006). "One-step reductive amidation of nitro arenes: application in the synthesis of Acetaminophen" Volume 47, Issue 11, 13 March 2006, Pages (1861–1864) [10]M.V.Joshi,Mahajani, Joshi's Process Equipment Design, Macmillan, 2009 [11]K.A.Gavane,”Chemical Reaction Engineering-I”,Nirali Publication,2012, Chapter 6 (6.1-6.15) Journal Papers, [12]R. D. BIGGS and R. R. WHITE „ Rate of Nitration of Benzene with Mixed Acid‟ University of Michigan, Ann Arbor, Michigan 2000 [13]J. Chil. Chem. Soc. vol.57 no.2 Concepción 2012, págs: 1194-1198.

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

[14]V. Dubois, G. James, J.L. Dallons, A. Van Geysel, In Catalysis of Organic Reactions, M. Ford, Ed; Marcel Dekker, New York, 1994, Vol.82, p. 1. [15]Laali, Kenneth K., and Volkar J. Gettwert. “Electrophilic Nitration of Aromatics in Ionic Liquid Solvents.” The Journal of Organic Chemistry 66 (Dec. 2000): 35-40. American Chemical Society. [16]Sauls, Thomas W., Walter H. Rueggeberg, and Samuel L. Norwood. “On the Mechanism of Sulfonation of the Aromatic Nucleus and Sulfone Formation.” The Journal of Organic Chemistry 66 (1955): 455-465. American Chemical Society.

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

APPENDIX A

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

SIMULATION REPORT

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 1

MANUFCTURING OF NITROBENZENE RUN CONTROL SECTION

RUN CONTROL INFORMATION -----------------------

THIS COPY OF ASPEN PLUS LICENSED TO

TYPE OF RUN: NEW

INPUT FILE NAME: _0812ogh.inm

OUTPUT PROBLEM DATA FILE NAME: _0335nde VERSION NO. 1 LOCATED IN:

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

PDF SIZE USED FOR INPUT TRANSLATION: NUMBER OF FILE RECORDS (PSIZE) = NUMBER OF IN-CORE RECORDS

= 256

PSIZE NEEDED FOR SIMULATION

CALLING PROGRAM NAME: LOCATED IN:

0

=

1

apmain

C:\PROGRA~2\ASPENT~1\ASPENP~1.2\Engine\xeq

SIMULATION REQUESTED FOR ENTIRE FLOWSHEET ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 2

MANUFCTURING OF NITROBENZENE INPUT SECTION

INPUT FILE(S) -------------

; ;Input Summary created by Aspen Plus Rel. 10.2.1 at 19:39:35 Sun Apr 27, 2014 ;Directory G:\Aspen new\aspen save Filename _0812ogh.dan ;

FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

TITLE 'MANUFCTURING OF NITROBENZENE'

IN-UNITS SI

DEF-STREAMS CONVEN ALL

SIM-OPTIONS IN-UNITS ENG SIM-OPTIONS NPHASE=1 PHASE=L ATM-PRES=101325.

DATABANKS PURE10 / AQUEOUS / SOLIDS / INORGANIC / & NOASPENPCD

PROP-SOURCES PURE10 / AQUEOUS / SOLIDS / INORGANIC

COMPONENTS C6H5NO2 C6H5NO2 / H2SO4 H2SO4 / H2O H2O / HNO3 HNO3 / C6H6 C6H6 FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

FLOWSHEET NBMFG BLOCK RSTO IN=C6H6 MIXACID OUT=CNB BLOCK DECANTER IN=CNB OUT=SPA ORGANIC BLOCK DIST IN=ORGANIC OUT=TOP BOTTOM BLOCK MIXER IN=HNO3 H2O H2SO4 OUT=MIXACID

DEF-STREAMS CONVEN NBMFG

PROPERTIES NRTL

PROP-DATA NRTL-1 IN-UNITS SI PROP-LIST NRTL BPVAL C6H5NO2 H2O -5.154900000 2270.617200 .2000000000 0.0 & 0.0 0.0 273.1500000 379.7500000 BPVAL H2O C6H5NO2 5.854700000 229.4967000 .2000000000 0.0 & 0.0 0.0 273.1500000 379.7500000 BPVAL C6H5NO2 C6H6 -.8730000000 630.1689000 .3000000000 0.0 & 0.0 0.0 343.1500000 484.1500000 BPVAL C6H6 C6H5NO2 -1.289300000 98.83280000 .3000000000 0.0 & 0.0 0.0 343.1500000 484.1500000 FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

BPVAL H2O C6H6 140.0874000 -5954.307100 .2000000000 0.0 & -20.02540000 0.0 273.9500000 350.1500000 BPVAL C6H6 H2O 45.19050000 591.3676000 .2000000000 0.0 &

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 3

MANUFCTURING OF NITROBENZENE INPUT SECTION

INPUT FILE(S) (CONTINUED)

-7.562900000 0.0 273.9500000 350.1500000

STREAM C6H6 SUBSTREAM MIXED TEMP=298. PRES=101325. MASS-FLOW=400. MASS-FRAC C6H6 1.

STREAM H2O SUBSTREAM MIXED TEMP=298. PRES=101325. MASS-FLOW=170. MASS-FRAC H2O 1.

STREAM H2SO4 FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

SUBSTREAM MIXED TEMP=298. PRES=101325. MASS-FLOW=580. MASS-FRAC H2SO4 0.98

STREAM HNO3 SUBSTREAM MIXED TEMP=298. PRES=101325. MASS-FLOW=250. MASS-FRAC HNO3 0.6

BLOCK MIXER MIXER PARAM PRES=101325. T-EST=298.

BLOCK DECANTER DECANTER PARAM TEMP=298. PRES=101325. L2-COMPS=C6H5NO2

; ;Input file created by Aspen Plus Rel. 10.2.1 at 00:20:55 Mon Apr 28, 2014 ;Directory G:\Aspen new\aspen save Runid simu1 ;

BLOCK DIST DISTL PARAM NSTAGE=26 FEED-LOC=16 RR=0.45 PTOP=101325. & FAMT ,Ratnagiri

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DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

PBOT=101325. D:F=0.205

BLOCK RSTO RSTOIC PARAM TEMP=323. PRES=101325. STOIC 1 MIXED C6H6 -1. / HNO3 -1. / C6H5NO2 1. / H2O & 1. CONV 1 MIXED C6H6 0.772

REPORT INPUT ; ; ; ; ; ; ;Input file created by Aspen Plus Rel. 10.2.1 at 00:16:43 Mon Apr 28, 2014 ;Directory G:\Aspen new\aspen save Runid simu1 ;

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 4

MANUFCTURING OF NITROBENZENE FAMT ,Ratnagiri

Page 65

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

INPUT SECTION

INPUT FILE(S) (CONTINUED)

STREAM EXH2O SUBSTREAM MIXED TEMP=298. PRES=101325. MOLE-FLOW=0.0309 MOLE-FRAC H2O 1. ; ;Input file created by Aspen Plus Rel. 10.2.1 at 00:05:56 Mon Apr 28, 2014 ;Directory G:\Aspen new\aspen save Runid SIMU1 ;

FLOWSHEET NBMFG BLOCK RSTO IN=C6H6 MIXACID OUT=CNB BLOCK DECANTER IN=CNB EXH2O OUT=SPA ORGANIC BLOCK DIST IN=ORGANIC OUT=TOP BOTTOM BLOCK MIXER IN=HNO3 H2O H2SO4 OUT=MIXACID ; ;Input file created by Aspen Plus Rel. 10.2.1 at 00:26:14 Mon Apr 28, 2014 ;Directory G:\Aspen new\aspen save Runid simu1 FAMT ,Ratnagiri

Page 66

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

;

FLOWSHEET NBMFG BLOCK RSTO IN=C6H6 MIXACID OUT=CNB BLOCK DECANTER IN=CNB EXH2O OUT=SPA ORGANIC BLOCK DIST IN=2 OUT=TOP BOTTOM BLOCK MIXER IN=HNO3 H2O H2SO4 OUT=MIXACID BLOCK B1 IN=ORGANIC OUT=2 ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 5

MANUFCTURING OF NITROBENZENE FLOWSHEET SECTION

FLOWSHEET CONNECTIVITY BY STREAMS ---------------------------------

STREAM

SOURCE

DEST

STREAM

EXH2O

----

DECANTER

H2SO4

----

MIXER

H2O

----

HNO3

----

MIXER

CNB

RSTO

SPA

DECANTER ----

FAMT ,Ratnagiri

C6H6

ORGANIC

SOURCE

----

DEST

RSTO

MIXER DECANTER

DECANTER DIST Page 67

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

TOP

DIST

MIXACID

----

MIXER

BOTTOM

DIST

----

RSTO

FLOWSHEET CONNECTIVITY BY BLOCKS --------------------------------

BLOCK RSTO

INLETS C6H6 MIXACID

DECANTER DIST MIXER

OUTLETS CNB

CNB EXH2O

ORGANIC

SPA ORGANIC TOP BOTTOM

HNO3 H2O H2SO4

MIXACID

COMPUTATIONAL SEQUENCE ----------------------

SEQUENCE USED WAS: MIXER RSTO DECANTER DIST

OVERALL FLOWSHEET BALANCE -------------------------

*** MASS AND ENERGY BALANCE *** FAMT ,Ratnagiri

Page 68

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

IN

OUT

GENERATION RELATIVE DIFF.

CONVENTIONAL COMPONENTS (KMOL/SEC) C6H5NO2

0.000000E+00 0.109812E-02 0.109812E-02 -0.336175E-06

H2SO4

0.164266E-02 0.164266E-02 0.000000E+00 -0.189866E-08

H2O

0.335212E-01 0.346193E-01 0.109812E-02 0.138954E-07

HNO3

0.110207E-02 0.395223E-05 -0.109812E-02 -0.680900E-11

C6H6

0.142243E-02 0.324314E-03 -0.109812E-02 -0.764627E-07

TOTAL BALANCE MOLE(KMOL/SEC)

0.376884E-01 0.376884E-01 0.000000E+00 0.000000E+00

MASS(KG/SEC )

0.945561

ENTHALPY(WATT

) -0.110013E+08 -0.111195E+08

ASPEN PLUS PLAT: WIN32

0.945561

VER: 10.2.1

-0.482081E-07 0.106313E-01

04/28/2014 PAGE 6

MANUFCTURING OF NITROBENZENE PHYSICAL PROPERTIES SECTION

COMPONENTS ----------

ID

TYPE FORMULA

C6H5NO2 C H2SO4 C FAMT ,Ratnagiri

C6H5NO2 H2SO4

NAME OR ALIAS C6H5NO2 H2SO4

REPORT NAME C6H5NO2 H2SO4 Page 69

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

H2O

C

H2O

H2O

HNO3

C

HNO3

C6H6

C

C6H6

H2O

HNO3

HNO3

C6H6

ASPEN PLUS PLAT: WIN32

C6H6

VER: 10.2.1

04/28/2014 PAGE 7

MANUFCTURING OF NITROBENZENE U-O-S BLOCK SECTION

BLOCK: DECANTER MODEL: DECANTER -------------------------------INLET STREAMS:

CNB

EXH2O

FIRST LIQUID OUTLET: SPA SECOND LIQUID OUTLET: ORGANIC PROPERTY OPTION SET: NRTL

RENON (NRTL) / IDEAL GAS

*** MASS AND ENERGY BALANCE *** IN

OUT

RELATIVE DIFF.

TOTAL BALANCE MOLE(KMOL/SEC)

0.376884E-01 0.376884E-01 0.000000E+00

MASS(KG/SEC ) ENTHALPY(WATT FAMT ,Ratnagiri

0.945561 )

0.945561

-0.482081E-07

-0.111411E+08 -0.111630E+08 0.196334E-02 Page 70

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

*** INPUT DATA ***

LIQUID-LIQUID SPLIT, TP SPECIFICATION SPECIFIED TEMPERATURE

K

SPECIFIED PRESSURE

298.000

N/SQM

101,325.

CONVERGENCE TOLERANCE ON EQUILIBRIUM

0.10000E-03

MAXIMUM NO ITERATIONS ON EQUILIBRIUM

30

EQUILIBRIUM METHOD

EQUATION-SOLVING

KLL COEFFICIENTS FROM

OPTION SET OR EOS

KLL BASIS

MOLE

KEY COMPONENT(S):

C6H5NO2

*** RESULTS ***

OUTLET TEMPERATURE OUTLET PRESSURE

K

N/SQM

CALCULATED HEAT DUTY

WATT

MOLAR RATIO 1ST LIQUID / TOTAL LIQUID

FAMT ,Ratnagiri

298.00 0.10132E+06 -21917. 0.96043

Page 71

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

L1-L2 PHASE EQUILIBRIUM : COMP

F

C6H5NO2

0.029137

H2SO4 H2O

X1

K

0.00061841 0.72129

0.043585 0.91857

X2

0.043344 0.95573

0.049433 0.016631

1,166.36 1.14047

0.017401

HNO3

0.00010487 0.00010429 0.00011894

C6H6

0.0086051

0.00020300 0.21253

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

1.14047

1,046.96

04/28/2014 PAGE 8

MANUFCTURING OF NITROBENZENE U-O-S BLOCK SECTION

BLOCK: DIST

MODEL: DISTL

----------------------------INLET STREAM:

ORGANIC

CONDENSER OUTLET: REBOILER OUTLET:

TOP BOTTOM

PROPERTY OPTION SET: NRTL

RENON (NRTL) / IDEAL GAS

*** MASS AND ENERGY BALANCE *** IN

OUT

RELATIVE DIFF.

TOTAL BALANCE FAMT ,Ratnagiri

Page 72

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

MOLE(KMOL/SEC)

0.149140E-02 0.149140E-02 0.000000E+00

MASS(KG/SEC ) ENTHALPY(WATT

0.164883 )

0.164883

-34983.6

0.338098E-08

8548.66

-1.24436

*** INPUT DATA *** THEORETICAL STAGES

26

FEED STAGE NO. FROM TOP

16

REFLUX RATIO

0.45000

TOP STAGE PRESSURE (N/SQM )

101,325.

BOTTOM STAGE PRESSURE (N/SQM )

101,325.

DISTILLATE TO FEED RATIO

0.20500

CONDENSER TYPE: TOTAL CONDENSER

*** RESULTS *** FEED-QUALITY

-0.31849

FEED STAGE TEMPERATURE (K TOP STAGE TEMPERATURE (K

)

365.058

)

BOTTOM STAGE TEMPERATURE (K

324.418 )

478.860

CONDENSER COOLING REQUIRED (WATT NET CONDENSER DUTY (WATT

)

REBOILER HEATING REQUIRED (WATT NET REBOILER DUTY (WATT FAMT ,Ratnagiri

)

)

14,284.2 -14,284.2

)

57,816.5 57,816.5 Page 73

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

BLOCK: MIXER

MODEL: MIXER

----------------------------INLET STREAMS:

HNO3

OUTLET STREAM:

H2O

H2SO4

MIXACID

PROPERTY OPTION SET: NRTL

ASPEN PLUS PLAT: WIN32

RENON (NRTL) / IDEAL GAS

VER: 10.2.1

04/28/2014 PAGE 9

MANUFCTURING OF NITROBENZENE U-O-S BLOCK SECTION

BLOCK: MIXER

MODEL: MIXER (CONTINUED)

*** MASS AND ENERGY BALANCE *** IN

OUT

RELATIVE DIFF.

TOTAL BALANCE MOLE(KMOL/SEC)

0.536596E-02 0.536596E-02 0.000000E+00

MASS(KG/SEC ) ENTHALPY(WATT

0.277778 )

0.277778

-0.199840E-15

-0.224319E+07 -0.224319E+07 0.415178E-15

*** INPUT DATA *** ONE

PHASE

FAMT ,Ratnagiri

FLASH SPECIFIED PHASE IS LIQUID Page 74

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

MAXIMUM NO. ITERATIONS

30

CONVERGENCE TOLERANCE

0.00010000

OUTLET PRESSURE N/SQM

BLOCK: RSTO

101,325.

MODEL: RSTOIC

-----------------------------INLET STREAMS:

C6H6

OUTLET STREAM:

CNB

MIXACID

PROPERTY OPTION SET: NRTL

RENON (NRTL) / IDEAL GAS

*** MASS AND ENERGY BALANCE *** IN

OUT

GENERATION RELATIVE DIFF.

TOTAL BALANCE MOLE(KMOL/SEC)

0.678839E-02 0.678839E-02 0.000000E+00 0.000000E+00

MASS(KG/SEC )

0.388889

0.388889

ENTHALPY(WATT

) -0.217334E+07 -0.231317E+07

0.000000E+00 0.604497E-01

*** INPUT DATA ***

SIMULTANEOUS REACTIONS STOICHIOMETRY MATRIX:

FAMT ,Ratnagiri

Page 75

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

REACTION # 1: SUBSTREAM MIXED : C6H5NO2

1.00 H2O

1.00 HNO3

-1.00 C6H6

REACTION CONVERSION SPECS: NUMBER=

-1.00

1

REACTION # 1: SUBSTREAM:MIXED

KEY COMP:C6H6

ASPEN PLUS PLAT: WIN32

CONV FRAC: 0.7720

VER: 10.2.1

04/28/2014 PAGE 10

MANUFCTURING OF NITROBENZENE U-O-S BLOCK SECTION

BLOCK: RSTO ONE

MODEL: RSTOIC (CONTINUED)

PHASE TP FLASH SPECIFIED PHASE IS LIQUID

SPECIFIED TEMPERATURE K SPECIFIED PRESSURE

N/SQM

MAXIMUM NO. ITERATIONS CONVERGENCE TOLERANCE FAMT ,Ratnagiri

323.000 101,325. 30 0.00010000 Page 76

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

*** RESULTS *** OUTLET TEMPERATURE OUTLET PRESSURE HEAT DUTY

K

323.00

N/SQM

WATT

0.10132E+06 -0.13983E+06

REACTION EXTENTS:

REACTION

REACTION

NUMBER

EXTENT KMOL/SEC

1

0.10981E-02

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 11

MANUFCTURING OF NITROBENZENE STREAM SECTION

BOTTOM C6H6 CNB EXH2O H2O ------------------------FAMT ,Ratnagiri

Page 77

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

STREAM ID

BOTTOM

FROM :

DIST

TO :

----

C6H6

----

CNB

RSTO

RSTO

EXH2O

----

H2O

----

DECANTER DECANTER MIXER

SUBSTREAM: MIXED PHASE:

LIQUID

LIQUID

LIQUID

LIQUID

LIQUID

COMPONENTS: KMOL/SEC C6H5NO2

1.0757-03

H2SO4 H2O

7.3724-05 3.1510-18

0.0

1.0981-03

0.0 0.0

1.6427-03

0.0 0.0

0.0 0.0

3.7193-03 3.0900-02 2.6212-03

HNO3

1.9992-11

0.0

3.9522-06

C6H6

3.6209-05 1.4224-03 3.2431-04

0.0 0.0

0.0 0.0

TOTAL FLOW: KMOL/SEC

1.1857-03 1.4224-03 6.7884-03 3.0900-02 2.6212-03

KG/SEC

0.1424

CUM/SEC

1.4003-04 1.2713-04 3.2101-04 5.6022-04 4.7524-05

0.1111

0.3888

0.5566 4.7222-02

STATE VARIABLES: TEMP K PRES N/SQM

478.8604 298.0000 323.0000 298.0000 298.0000 1.0133+05 1.0133+05 1.0133+05 1.0133+05 1.0133+05

VFRAC

0.0

LFRAC

1.0000

FAMT ,Ratnagiri

0.0

0.0

1.0000

0.0 1.0000

0.0 1.0000

1.0000 Page 78

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

SFRAC

0.0

0.0

0.0

0.0

0.0

ENTHALPY: J/KMOL

2.7788+05 4.9107+07 -3.4075+08 -2.8569+08 -2.8569+08

J/KG

2312.1927 6.2866+05 -5.9481+06 -1.5858+07 -1.5858+07

WATT

329.4732 6.9851+04 -2.3132+06 -8.8279+06 -7.4887+05

ENTROPY: J/KMOL-K

-3.3127+05 -2.5267+05 -2.3857+05 -1.6272+05 -1.6272+05

J/KG-K

-2756.4033 -3234.6200 -4164.5254 -9032.4484 -9032.4484

DENSITY: KMOL/CUM

8.4673 11.1885 21.1467

KG/CUM

55.1564 55.1564

1017.6101 873.9777 1211.4430 993.6590 993.6590

AVG MW

120.1805 78.1136 57.2873

ASPEN PLUS PLAT: WIN32

18.0152 18.0152

VER: 10.2.1

04/28/2014 PAGE 12

MANUFCTURING OF NITROBENZENE STREAM SECTION

H2SO4 HNO3 MIXACID ORGANIC SPA ------------------------------

STREAM ID FAMT ,Ratnagiri

H2SO4

HNO3

MIXACID

ORGANIC

SPA Page 79

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

FROM : TO :

----

----

MIXER

MIXER

MIXER

DECANTER DECANTER

RSTO

DIST

----

SUBSTREAM: MIXED PHASE:

LIQUID

LIQUID

LIQUID

LIQUID

LIQUID

COMPONENTS: KMOL/SEC C6H5NO2

0.0

0.0

H2SO4

1.6427-03

H2O

0.0

0.0

0.0

HNO3

0.0

C6H6

0.0

0.0

1.0757-03 2.2385-05

1.6427-03 7.3724-05 1.5689-03

2.6212-03 2.4803-05 3.4595-02

1.1021-03 1.1021-03 1.7738-07 3.7748-06 0.0

0.0

3.1697-04 7.3479-06

TOTAL FLOW: KMOL/SEC

1.6427-03 1.1021-03 5.3660-03 1.4914-03 3.6197-02

KG/SEC

0.1611 6.9444-02

CUM/SEC

8.8976-05 4.5735-05 2.0328-04 1.4334-04 7.5076-04

0.2777

0.1648

0.7806

STATE VARIABLES: TEMP K PRES N/SQM

298.0000 298.0000 298.0000 298.0000 298.0000 1.0133+05 1.0133+05 1.0133+05 1.0133+05 1.0133+05

VFRAC

0.0

LFRAC

1.0000

SFRAC

0.0

0.0

0.0

1.0000 0.0

0.0

0.0 1.0000 0.0

0.0 1.0000

1.0000

0.0

ENTHALPY: FAMT ,Ratnagiri

Page 80

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

J/KMOL

-7.9337+08 -1.7338+08 -4.1804+08 -2.3457+07 -3.0743+08

J/KG

-8.0891+06 -2.7516+06 -8.0755+06 -2.1217+05 -1.4254+07

WATT

-1.3032+06 -1.9108+05 -2.2432+06 -3.4984+04 -1.1128+07

ENTROPY: J/KMOL-K

-3.3300+05 -3.1260+05 -2.3701+05 -3.7927+05 -1.6879+05

J/KG-K

-3395.2154 -4960.9513 -4578.3531 -3430.5411 -7826.0507

DENSITY: KMOL/CUM

18.4618 24.0968 26.3970

KG/CUM

10.4047 48.2138

1810.7264 1518.4146 1366.4855 1150.2998 1039.8510

AVG MW

98.0794 63.0128

ASPEN PLUS PLAT: WIN32

51.7666 110.5555 21.5674

VER: 10.2.1

04/28/2014 PAGE 13

MANUFCTURING OF NITROBENZENE STREAM SECTION

TOP ---

STREAM ID FROM : TO :

TOP DIST ----

SUBSTREAM: MIXED FAMT ,Ratnagiri

Page 81

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

PHASE:

LIQUID

COMPONENTS: KMOL/SEC C6H5NO2

0.0

H2SO4 H2O

0.0 2.4803-05

HNO3

1.7736-07

C6H6

2.8076-04

TOTAL FLOW: KMOL/SEC

3.0574-04

KG/SEC

2.2389-02

CUM/SEC

2.6121-05

STATE VARIABLES: TEMP K

324.4181

PRES N/SQM

1.0133+05

VFRAC

0.0

LFRAC

1.0000

SFRAC

0.0

ENTHALPY: J/KMOL J/KG WATT

2.6883+07 3.6711+05 8219.1914

ENTROPY: FAMT ,Ratnagiri

Page 82

DESIGN & SIMULATION OF NITROBENZENE MANUFACTURING PROCESS

J/KMOL-K

-2.3016+05

J/KG-K

-3142.9623

DENSITY: KMOL/CUM

11.7048

KG/CUM

857.1411

AVG MW

73.2293

ASPEN PLUS PLAT: WIN32

VER: 10.2.1

04/28/2014 PAGE 14

MANUFCTURING OF NITROBENZENE PROBLEM STATUS SECTION BLOCK STATUS -----------*************************************************************************** * *

*

* Calculations were completed normally *

* *

* All Unit Operation blocks were completed normally *

*

* All streams were flashed normally *

*

* *

***********************************************************

FAMT ,Ratnagiri

Page 83