Nitrobenzene Plant Report

Detail Process of Manufacturing Nitrobenzene
CHAPTER 1 INTRODUCTION TO COMPANY

COMPANY BACKGROUND: HINDUSTAN ORGANIC CHEMICALS LTD A leader in Indian chemical industry for over three decades is future expanding its horizons in near future. Earlier company has to depend upon the important of its vital organic chemical needs till the government with a view to making the company self reliant in this field setup HOC in 1960. Making a beginning as a small chemical unit HOC now is a multi-unit company with three fast growing units. HOC has following manufacturing units: 1. 2. 3. The main organic chemical complex at Rasayani at Raigad district (Maharashtra) The phenol complex at Kochi (Kerala). The poly tetra Fluroethylene plant (Hyderabad) Initially an era in basic chemical intermediates, incorporated at Rasayani, a backward area in Maharashtra, HOCs first plant started production in 1970. Between 1970 and 1974 a total of twelve plants were commissioned. Together they produce a large number of products that serve a wide spectrum of industries, ranging from pharmaceuticals to defense and space. After stabilization of first phase in the sixth plane period (1980-85), a number of expansion and diversification plans were launched at Rasayani. Expansion phase included doubling of Hydrogen, Aniline, Nitro Benzene and Nitro toluene and substantial expansion of Nitrochlorobenze. HOCL was established on 12th dec 1960 by the government of india with the view of making our country self sufficient in the field of organic chemical manufacture. Initiating an era in basic chemical complex as a leader in Indian chemical industries manufacturing a wide range of high quality basic organic chemical which are required for variety of chemical and pharmaceutical products such as drugs, medical dyes, plastics, resins, paints, textile and explosives. The company has a continuous manufacturing process and works for 24hrs. A day in 3 shifts in all, around 11 plants are manufacturing in at Rasayani. HOC has its head office situated at Mumbai. The company provides various facilities to its employees like canteen, transport, residential quarter, library and hospital etc.
Department of Chemical Engineering, Dr. BATU, Lonere. 1
MISSION: To be dynamic market leader committed to quality and customer satisfaction. Companys mission is also to be a prime representative of India in Global Chemical business. GROWTH STRATEGY: The fast changing business environment and the need for not only sustaining but also accelerating the growth process, dictated the long term perspective in planning coupled with flexibility to make strategic decisions. Organizations are expected to be resilient enough to respond to the emerging challenges. Hence, the company concentrates on the core business on Nitro Aromatics and Phenol/Acetone and certain Phenol based downstream products. ENERGY CONSERVATION: Energy and its important have been duly recognized by the organization. While acquiring technology to that effect energy conservation efforts have been made with remarkable achievements every year. Energy conservation awards from the ministry of power have been received continuously by the Rasayani unit for the past several years.
Department of Chemical Engineering, Dr. BATU, Lonere.
CHAPTER 2 NITROBENZENE PLANT

INTRODUCTION: Nitrobenzene plant phase-III in HOCL is designed to produce 15000 TPA of Nitrobenzene. The raw material is nitration grade benzene, 98% Nitric Acid and 98% Sulphuric acid which is used as the dehydrating agent and recovered as spent acid. The raw material is stored in the HOCL complex and the nitric acid required for the plant is taken from utility grid of HOCL complex.
Capacity of plant: This plant is designed to produce 15000 TPA of Nitrobenzene in 300 streams days. The plant is in continuous operation and produces approximately 2087 Kg/hr. of Nitrobenzene.
The entire plant is divided into three sections; 1. NITRATION SECTION: here nitration reaction is carried out. Nitration of benzene
is done with 98% HNO3. 98% H2SO4 is used as a dehydrating agent. The process is carried out in Nitration pump.
2.
WASHING SECTION: Here washing is done with the help of process water and
caustic lay. Washing is carried out in five different stages.
3.
DISTILLATION SECTION: Here distillation of crude nitrobenzene is done. Crude
nitrobenzene contains traces of benzene and water, hence to obtain pure nitrobenzene it is distilled in distillation column. Benzene and water are obtained in the form of vapour through the top of the distillation column, and distilled nitrobenzene is obtained from the bottom.
CHAPTER 3 RAW MATERIAL, FINISHED PRODUCT AND BY PRODUCT SPECIFICATION
RAW MATERIAL:A. 1. 2. BENZENE COLOUR APPEARANCE :Colorless :Not darker than solution of 0.1N of potassium dichromate and 12cc of 0.1N cobalt sulphate made with distilled water. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. SPECIFIC GRAVITY MELTING POINT CRYSTALLIZATION POINT DISTILATION RANGE(at 1 atm) VAPOUR DENSITY (Air=1) FLASH POINT EXPLOSIVE LIMIT IGNITION TEMPERATURE THRESHOLD LIMIT VALUE ACIDITY HYDROGENE SULPHIDE CARBON SULPHIDE :0.8814 at 150C : -5.20C :Not below 50C :Not more than 100C including temp of 80.10C : 2.8 :110C :1.3 to 7% :5620C :1-10 ppm :None :0.035% (by wt) :0.035% (by wt)
B.
NITRIC ACID :Colorless to Yellow liquid with acidic odour. :98% HNO3 by weight. :860C :-170C (20%) :1.115 (20%), 1.3667 (60%) :2 Approx.
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1. COLOUR 2. COMPOSITION 3. BOILING POINT 4. MELTING POINT 5. SPECIFIC GRAVITY 6. VAPOUR DENSITY
C.
SULPHURIC ACID 1. APPEARANCE 2. COMPOSITION : Colourless (pure) to dark brown oily liquid with acidic odour. : 98% by weight H2SO4(Min) Iron as Fe 0.05% by wt. Arsenic as 0.004 % by wt (Max). Heavy material as Pb 0.005% (Max). 3. BOILING POINT : 3300C
4. SPECIFIC GRAVITY: 1.84
D.
CAUSTIC LYE 1. SPECIFICATION 2. COMPOSITION : Rayon grade caustic lye. : Total alkali 45% (min) as NaOH, Sodium carbonates 0.2% (Max), sodium chloride 0.1%, sodium sulphate 0.1%, and silica 75 ppm as SiO2, Iron 10 ppm, Aluminum 2 ppm., Calcium 25 ppm., Magnesium 15 ppm.
3. RESIDUE ON IGNITION
:0.05% by wt. (Max.)
E.
PRODUCT: NITROBENZENE 1. APPEARANCE :Pale to dark yellow liquid free from visible impurities 2. RELATIVE DENSITY 3. pH 4. CRYSTALLIZATION POINT 5. DISTILATION RANGE : 1.197 to 1.2 at 270C : 5.5 (Min.) : 5.50C :9% (by volume) shall be distilled between 2090C To 2210C 6. FLASH POINT :87.80C
7. VAPOUR DENSITY (OF AIR 1) :4.3 8. EXPLOSIVE LIMIT 9. IGNITION TEMPERATURE 10. THRESHOLD LIMIT VALUE 11. MOISTURE :1.8% :4820C :1.2 ppm : 0.05% by wt (Max.)
F.
BY PRODUCT: SPENT SULPHURIC ACID 1. APPEARANCE 2. SPECIFIC GRAVITY 3. TOTAL ACIDITY 4. FREE NITRIC ACID :Varying from deep orange to dark brown. :1.640 to 1.675 :74 to 77% (Max) :0.5% (Max)
The nitrobenzene plant consist of mainly three sections; 1. NITRATION SECTION. 2. WASHING SECTION. 3. DISTILLATION SECTION. AND TWO SUBSECTIONS. 1. Tank farm and feed preparation unit. 2. Nitric acid extraction. The plant equipments and control system is described in the following section. The tank farm and feed preparation unit are described along with the nitration section.
The tank farm consist of following tanks.

SR NO. DESCRIPTIN NO. OF TANKS DIAMETER (cm) HEIGHT (cm) LENGTH (cm) CAPACITY (m3) MOC
Nitric Acid Day Tank
300
360
25
Aluminium 99.9%
Sulphuric acid Day tank
270
360
20
C.S
Benzene Underground Tank
240
860
40
C.S Gr, C
Crude Nitrobenzene
360
400
40
S.S
Product Nitrobenzene
360
400
40
C.S
Caustic Lye Tank
150
225
S.S
7 8
NaOH tank Nitrobenzene Hold vessel
1 1
150 100
115 120
2 1
C.S C.S
Distilled NB Hold vessel
110
220
2.3
C.S
10
Spent Acid Day tank
240
775
35
C.S
11
Caustic preparation Tank
130
150
C.S
12 13
Separation tank Benzene Intermediate tank 1
160 140
150
190 -
4.5 2.5
S.S S.S
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Effluent Tank
150
155
S.S
Pumps: SR NO. DESCRIPTION CAPACITY (m3/hr) 1 Nitric acid metering pump 2 Sulphuric acid metering pump 1.5 Alloy 20 Metering 1.5 Alloy 20 Metering M.O.C. TYPE
Benzene transfer pump
C.I
Centrifugal, Self priming
4 5 6 7 8
Effluent pump Nitration pump Spent acid pump Benzene metering pump Nitrobenzene washing Pump
20 60 20 3 3
S.S Alloy C.I S.S S.S
Centrifugal Centrifugal Centrifugal Metering Centrifugal
9 10 11
Process effluent pump Caustic transfer pump Crude nitrobenzene pump
50 4 3
S.S C.I C.I
Centrifugal Centrifugal Centrifugal
12
Nitrobenzene transfer pump
30
C.I
Centrifugal
13
Nitrobenzene circulation pump
2.5
C.I
Centrifugal
CHAPTER 4 USES OF NITROBENZENE

1) The most significant use of nitrobenzene is in the manufacture of aniline. Approximately 97-98% by weight of nitrobenzene produced is converted to aniline. 2) Nitrobenzene is used for the preparation of intermediate chemicals for azo and substituted diazo dyes including benzidine, m-dinitrobenzene and m-
nitrochlorobenzene. 3) It is also used in the manufacture of quinoline and magenta. 4) It is also used in the manufacture of rubber chemicals and hydroquinone, drugs, herbicides and fibers. 5) Nitrobenzene is used as selective solvent in petroleum industry. 6) It is used as ingredient in shoe polishes. 7) It is used for preparation of dinitrobenzene and as a component of liquid explosive.
CHAPTER 5 PROCESS SELECTION

The Mononitration of benzene is probably the most basic and familiar nitration process despite the importance of nitration process. Few changes in nitration method have been proposed for year. The various method which can be used for the manufacture of nitrobenzene are explained as below.
1) NITRATION OF BENZENE USING NITRIC ACID ALONE:This process involves the utilization of 40-60% by weight of nitric acid and temperature of 50-90oc. molar ratio of HNO3 to benzene is 6:1 to 15:1 and it is necessary to reconcentrate the nitric acid by distillation. The plant usually consist of a relatively small reaction tower, a nitration stripper and accessory and heat transfer equipments. The main disadvantage of this process is The water formation, after nitration reaction retards the rate of reaction considerably. 2) NITRATION OF BENZENE USING MIXED ACID:In this process, benzene is nitrated using a mixture of nitric acid and sulphuric acid commonly referred as Mixed acid or Nitrating Mixture. The reaction vessel is acid resistant, cast iron or steel vessel that are equiped with efficient agitator. By vigorous agitation the interfacial area of heterogeneous reaction mixture is maintained as high as possible enhancing mass transfer of reactants. Cooling coil or jacket are used to control the temperature of highly exothermic reaction. Industrial practice has been to operate with excess benzene, this is done to ensure that little or no nitric acid remains in the spent acid. It is much easier, to remove or recover benzene from crude nitrobenzene than, to recover nitric acid from spent acid. Beside of this, operating with excess nitric acid would lead to increase in the formation of impurities or byproducts (like dinitrobenzene). The spent acid strength in conversion isothermal nitrobenzene plant is usually kept at about 75% H2SO4 and residual nitric acid level is typically 0.1% HNO3 (by Weight). The spent acid strength drop much below 68% H2SO4 , nitration rates will drop to an extent that the increase in unreacted nitric acid and its subsequent loss will become an unacceptable economic penalty.
The process of manufacturing nitrobenzene using nitric acid alone as nitrating agent has been replaced by the one using mixed acid because of following reactions. 1. Nitric acid alone is generally poor nitrating agent, since the water produced in
reaction suppresses nitronium ion formation to yield a much less active nitrating agent. Hence the equilibrium is shifted away from the product to reactant this result in slowness and incompleteness of nitration reaction. 2. Nitric acid is further most a good oxidizing agent, its activity becoming more
pronounced at higher temperatures. Part of raw material may thus be converted to value less products which not only lowers the direct yield, but also makes the purification of nitrocompounds imperative. Where as in mixed acid process, the sulphuric acid present in mixture acts as dehydrating agent by isolating the water formed in nitration reaction, thus preventing the suppression of active nitrating agent and undesirable displacement of equilibrium. Employment of mixed acid rather than an excess of nitric acid results in certain technical advantages. 1. Since nitric acid is much more expensive than sulphuric acid, a considerable saving
is effected. 2. 3. The sulphuric acid moreover is recovered from the spent acid with only a slight loss. In addition of an serving as an economical dehydrating agent, the presence of
sulphuric acid makes it easier to keep the reaction under control and milder conditions that are thus provided are instrumental in inhabiting the formation of oxidation products.
Two different mixed acid processes are used in industry for the manufacture of nitrobenzene. 1) Conventional isothermal process. 2) Adiabatic process. Both processes have difference only in nitrating section, where as adiabatic process integrates nitration with sulphuric acid concentration. Here the heat of nitration is utilized for the concentration of sulphuric acid (spent acid). This is achieved by circulating a large volume of sulphuric acid through nitrators, absorbing heat of nitration without much temperature rise. The spent sulphuric acid is flash concentrated under vaccum. In the areas of
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nitrobenzene purification, effluent treatment and fume control, the both process employ the equivalent design concept. The convential isothermal plant usually operate at about 550C. this temperature is selected so that the Nitrator can be operated at atmospheric pressure without danger of having benzene flash (Boiling point 80.10C.) at higher temperature nitration would be much faster in the adiabatic process where final temperature is 105-1450C; but Nitrator would then have to be pressured. Also control of high temperature and pressure is comparatively very difficult. Hence most of plants, all over the world, employs conventional isothermal process. 3) AZEOTROPIC NITRATION OF BENZENE:Here the reaction is carried out at 120-1600C with excess of water being distilled from a Nitrator as an azeotrope with benzene. After being separated from product, the sulphuric acid recycled to the Nitrator without being concentrated an excess of benzene used to facilitate the removal of excess water as an azeotrope. After azeotrope is condensed, water is separated and benzene return to Nitrator. In duplex process the nitration is carried out in an azeotropic first stage which is followed by a lower temperature, mixed acid second stage. All or part of the benzene resulting from the azeotrope of first stage is taken to second stage for further nitration. SELECTED PROCESS Continuous, conventional isothermal process. Reasons:1. Always continuous process offers low capital cost and capacity advantages over batch process. 2. The continuous isothermal process utilizes lower nitric acid concentration and because of rapid and efficient mixing in reactors, higher reaction rates are observed. 3. It operates at lower temperature (550C). hence it need not required pressurized reactor (to avoid benzene vapor loss). 4. The heat of nitration is removed by cooling and hence excess sulphuric acid (as heat absorbing medium) is not essential.
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CHAPTER 6 CHEMISTRY AND MECHANISM

The lack of contrary evidence in the literature suggest that all commercial nitrobenzene plants use the mixed acid process. Mixed acid, also called as nitrating acid is obtained by blending sulphuric acid (or oleum or reconcentrated sulphuricacid ), nitric acid and water , the latter usually added as a part of the acids. Nitration, which is the introduction of the nitrogroup or the NO2 group into the molecule ,is achieved by bring mixed acid and the compound to be nitrated into intimate contact under vigorous agitation. Care must be taken to remove the heat of nitration .The acid left on completion of the nitration reaction is called as spent acid .In benzene nitration the reaction is heterogeneous, benzene and nitrobenzene have very low solubilities in mixed and spent acid. The overall stoichiometry for the reaction of benzene and nitric acid to form nitrobenzene and water is
Here the sulphuric acid acts as catalyst and does not enter directly into the stoichiometry of the reaction. It also acts as dehydrating agent by absorbing water formed in the nitration reaction and it is responsible for the dissociation of nitric acid through which the reactive species, nitronium ion forms.
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REACTION MECHANISM :The nitration of benzene involves the following steps 1. Formation of nitronium ion (electrophile) NO2+ HNO3 + 2H2SO4 --------- NO2+ + 2HSO4- + H3O+ 2. The electrophile attacks the benzene ring to give to carboniumion . This carbonium ion is resonance stabilized.
3. Removal of proton gives nitrobenzene.
The rate controlling step is second reaction. The rate of reaction is function of many factors , most importantly it is a function of sulphuric acid strength. The change in sulphuric acid strength changes the rate by the several order of magnitude because it affects the formation of nitronium ions and it is nitronium ion which is reactive species in rate controlling step.
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The main by products formed in commercial nitrobenzene plants are 1. Dinitrobenzene (C6H4(NO2)2
2. Dinitrophenol (C6H3OH(NO2)2
3. Picric acid (C6H2OH(NO2)3
The fraction of nitrobenzene obtained is usually well below 100 ppm , but can reach a few hundred ppm if the nitration is accidently operated with excess nitric acid . The introduction of nitro groups into the benzene ring lowers the electron density, thereby impeding electrophile attack . Substantial rate of conversion to dinitrobenzene are possible only at high spent acid strengths. Furthermore, commercial nitrobenzene plant usually operates with excess benzene which will consume most of the nitric acid well before significant quantities of dinitrobenzene can be formed.
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CHAPTER 7 THERMODYNAMICS
The economy of chemical manufacture depends largely upon establishing high rates of production of desired products and minimizing the production of undesired product. Thermodynamics principles may permits the selection of conditions which will results in favourable production if the equilibrium is reached but gives no clues as the rates at which the various reaction occurs. Thus displacement of system from equilibrium condition may be considered as potential which may cause a flow reaction to proceed. If other condition are favourable, similarly reaction rates depends on kinetic properties of the system as well as on driving potential. Quantitative knowledge of these kinetic properties is desirable in the design and intelligent operation of a chemical process.
THERMODYNAMIC FEASIBILITY :The object of thermodynamic analysis of a real process is the determination of the efficiency of the process from the stand point of energy utilization. further it is useful to calculate the influence of each irreversibility individually on the overall efficiency of the process. Thermodynamics can indicate whether a particular process is possible or not under a given set of parameters. However no information can be obtained from the pure thermodynamics as to the rate at which reaction will take place. Thermodynamics gives
who important pieces of information needed in design, the heat liberated accompanied by the liberation or absorption of heat. The magnitude of which must be know for proper design. Thermodynamics also allows calculation of the equilibrium constant k from the standard free energies G0 of the reaction materials. Thus for the reaction just given with equilibrium constant known the expected maximum attainable yield of the products of reaction can be estimated.
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Heat Capacity and heat of formation :The ideal gas heat capacity Cp0 is the function of temperature. A number of
analytical equation have been suggested to relate Cp0 to temperature. The most common is a simple polynomial. Cpo = a + bT + CT2 + dT3 Where, A,b,c,d are constant T = absolute temperature k The simple and reasonably accurate additive group contribution method of Rihani and Doraiswamy make use of values to determine the constant in equation, from which Cp0 can be calculated. The standard heat of formation Hf0 in the ideal gas state is required to determine heat of reaction. For other temperature H0ft = H0 f 298 + Gibbs free energy :The standard Gibbs free energy of formation Gf0 is used to determine the extent of reaction . vankrevelen and chermin suggest G0f = A + BT Where A & B can be found from the group contribution. If the gibbs free energy is found to be negative it is an indecation of feasibility of the reaction. Also the heat of reaction give an idea where the reaction is endothermic ( H positive ) or exothermic ( H - negative).
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Feasibility calculation:Main Reaction:C6H6 + HNO3 H2SO4 C6H5NO2 + H2O (Temp.=550C=3280K)
1.
Benzene:-
Group CH (6 groups) Total
A 3.047 18.282
B 0.61510-2 0.0369
G0fT = A+BT G0f 328 =18.282 + (328)(0.0369) =30.3852 Kcal/mol
2.
Nitrobenzene:-
Group CH (5 groups) C (1 group) NO2 (1 group) Total
A 3.047 4.675 -9.000 10.91
B 0.61510-2 1.15010-2 3.7010-2 0.07925
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G0fT = A+BT G0f 328 =10.91+ (328)(0.07925) =36.904 Kcal/mol
G0f of water = 56.678831 Kcal/mol G0f of HNO3 = -19.11363 Kcal/mol G0f of Reaction =G0f(product) + G0f(Reactant) =(-56.678831+36.904) (-19.5163+30.3852) =-19.774832 (10.87157) =30.646401 Kcal/mol
The free energy change is negative and hence therefore the reaction is theorotically feasible Now G0f = -RT ln K ln K = 0.0470227 103 K = 2.64 1020
Hence it shows that the conversion is good and high K value shows that reaction is irreversible.
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Heat of Reaction:Heat of reaction at reaction temperature gives us clear idea whether the reaction is exothermic or endothermic in nature.
Heat of formation For benzene at 298 K (liquid state)
H0f
298
= 49.0 0.6 KJ/mol = 49.0 KJ/mol (Mean) = 11.7035 Kcal/mol
For benzene heat capacity equation can be given as
C0p = -8.79 + (116.0 10-3) T + (-76.0 10-6) T2 + (18.9 10-9) T3 Hence, C0p 328 = -8.79 + (116.0 10-3) (328) + (-76.0 10-6) (328)2 + (18.9 10-9) (328)3 =21.75 Kcal/(Kgmol.k) =21.75 cal/(gmol.k)
Heat of formation of benzene at 328 K
H0f
328
= 11.7035 103 + = 11.7035 103 + 21.75(328-298)
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= 12.356 103 Cal/mol = 12.356 KCal/mol Nitrobenzene:H0f at 298 K = 2.9856 Kcal/mol
Temperature (0C) 10 30 50 70 90 120
Specific heat (cal/(g. 0C)) 0.358 0.339 0.330 0.330 0.343 0.394
By interpolation specific heat at 55 0C = 0.330 Cal/g0C = 0.330 123 Cal/mol0C = 40.59 Cal/mol0C
H0f 328 = 2.9856 103 + (40) (30) = 4.2033 Kcal/mol
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Water:-
H0f 298 = -285.83 KJ/mol = -68.27 Kcal/mol
C0p of water (30-60 0C) = 1 Cal/(gm 0C )
H0f 328 = -68.27 103 + 18.0001 30 = -67.73 Kcal/mol
HNO3:-
H0f = -173.22 KJ/mol = -41.373 Kcal/mol
Temperature (0K) 400 600 800 1000
Specific heat (J/(mol. 0K)) 63.19 76.77 85.04 90.43
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By extrapolation C0p = 58.3012 J/(mol. 0K) = 13.93 Cal/(mol 0K) H0f 328 = -41.373 103 + (13.93) (30) = -40.96 Kcal/mol H (Heat of Reaction at 328 K):=H0f(product) + H0f(Reactant) = (-67.73) + (4.2033) ((12.356) + (-40.96)) = -35.103 Kcal / mol Heat of reaction is negative that means that the reaction is exothermic.
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CHAPTER 8 PROCESS DESCRIPTION

1) NITRATION SECTION: The raw materials Benzene, Sulphuric acid (98%) and Nitric acid (98%) from main tank farm are received in their respective day tanks. 98% H2SO4 and 98% HNO3 are pumped to the mixing tee. Two air eggs are provided for HNO3 & H2SO4 heads respectively to dampen the pulsation. Benzene from underground day tanks is pumped to the benzene intermediate tank by C6H6 transfer pump. The C6H6 day tank is provided with flame arrestors and level indicators. The pipelines contacting volatile fluids are provided with jumpers to prevent the accumulation of electrostatic charges which is risky. The HNO3and H2SO4 are pumped at predetermined flow ratio to the mixing tee. The flow rates of the acids are measured by the respective flow meter. The temperature of mixing acid rise from 350C to 600C -700C due to the heat of mixing (Exothermic reaction). The hot mixed acid is passed through the water-cooled exchanger. The cooled mixed acid from the exchanger is sprayed in the nitration tee. In mixing tee, the feed C6H6 is sprayed against circulating spent acid and mixed thoroughly with mixed acid and delivered to nitration pump suction. The metering pump the C6H6 from the intermediate storage tank. The metering pumps are provided with air egg to dampen the pulsation. The reaction takes place at temperature and pressure of 580C -630C & 6.0 kg/cm2g. The vigorous agitation during the pumping helps the reaction to take place, and keeps the reaction at constant agitation so the nitrations pumps are more effective than a reactor for the reaction. The pumps are of centrifugal type provided with mechanical seals. The reaction product from the nitration pump passes through a nitration cooler cooled by cooling water, where the heat of reaction is removed by cooling water and the temperature is controlled at 500C. Regulation of the cooling water flow through the mixed acid cooler and nitration cooler controls the reactor temperature and the reactor products outlet temperature from the cooler. Cooler water passes in the series through the exchanger. The nitration product stream from the nitration cooler passes through nitration coils where it is given an additional residence time, under constant agitation, to complete the reaction. The heat evolved is being disspated to the atmosphere. The nitration coil is 4 inch diameter pipe approximately 170mt long and coil diameter of 1.8mt. The reaction mass from coil pass to the overflow weir. The
total quantity of reaction mass is measured and kept at a constant rate. The measurement is done by means of a rectangular overflow weir. The nitration mass then pass through a gravity separator where the part heavier that is spent acid is sent back to the nitration tee. While the lighter fractions, crude acidic C 6H5NO2 and the remaining spent acid mass is sent to the next gravity separator where the spent acid is separated and sent to the nitric acid recovery mixers. Decanter maintains the interface level in the gravity separator. The lighter fraction containing the crude acidic C 6H5NO2 Is sent to washing section by gravity. The spent acid in the mixer are mixed with a part of fresh C6H6 from benzene day tank through pump. The mixers are operated in series. The unreacted HNO3 gets extracted with the benzene leaving the spent acid with traces of HNO3. The spent acid & C6H6 along with the extracted HNO3 and separated in a gravity separator decanter. The overflow is sent to benzene intermediate tank and under flow is sent to the acid day tank. The C6H6 intermediate tank is equipped with an agitator and limpet coil for the cooling water. In spent acid day tank material is allowed to settle and any carried over nitrobenzene is taken out from top boot of the tank. The gravity separator in the plant is trapezoidal type construction packed with horizontal grid type plant bundle and are made out of stainless steel. All the process lines, equipments and nitration pumps are made out of stainless steel. All the equipment from overflow to the gravity separator is arranged in such a way that flow to successive equipment is by gravity to next equipment. NORMAL OPERATION CONDITIONS : (NITRATION SECTION) 1) Spent acid circulation rate 2) Benzene feed to nitration pump 3) H2SO4 feed rate 4) HNO3 feed rate 5) Temperature 6) Pressure
:60m3/hr :1567kg/hr :1044kg/hr :1127kg/hr :50-600C :6 kg/hr

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7) Spent acid composition
:74% H2SO4 (By wt.) &1% HNO3 (By wt)
2) WASHING SECTION: Crude acidic nitrobenzene from the gravity separator is sent to the washing section to wash the acidity and the phenolic nitro bodies. The 1st washing tower is packed with ceramic 20mm interlocks saddle (and ten layers of 25mmranching ring at bottom). The crude nitrobenzene is subjected to counter current washing by using wash water from the stage 4th. The acid nitrobenzene stream enters from the top & wash water from the bottom. The interface in the tower is maintained in the decanter. The organic phase containing crude nitrobenzene from the tower then flows to 2nd stage tower. The overflow from the top of the last 1st stage tower flows flows in to the gravity separator carried over organic phase is separated and the organic phase to the 2nd wash tower along with the 1st stage tower bottom organic phase are obtained . The water from the separator is drained out into effluent tank as yellow water. Decanter maintains the interface level in the separator. In second stage washing, the crude nitrobenzene is treated with dilute NaOH solution along with process water to remove acidity. The washing is done in counter current way i.e caustic soda solution from the bottom and crude nitrobenzene from the top. The maintains the interface in the washing tower. The organic phase from the top of the tower then overflow into the mixer (i.e 3rd stage washing) through gravity separator and decanter. The water from the separator overflows and drained out as RED WATER into the effluent tank. This treatment removes acidity of the crude nitrobenzene to make it alkaline and also converts the phenolic bodies (in crude nitrobenzene) to their respective sodium salt. The crude nitrobenzene from the 2nd stage wash goes to the mixer for 3rd wash using wash water from the 4th stage. Dilute NaOH solution is added to the mixer to adjust the pH6.5-7.0. The mixer is equipped with an agitator for through mixing of the two phases. From the mixer, the mixture is continuously fed to dynamic separator to separate crude nitrobenzene from water. The separate crude nitro benzene is fed 4th stage wash. The after phase from dynamic separator drained into the effluent tank as neutral water. The crude nitrobenzene
26
from the dynamic separator is washed in the 3rd tower counter current. The wash water is similar 1st &2nd stage wash organic phase from the tower is send to NB washing pump suction via decanter. Pump delivers this organic phase to the mixer. The mixer equipped with agitators. A measured amount of fresh process water is added to the mixer continuously. The water and crude nitrobenzene are thoroughly mixed to wash the last traces of alkalinity of the crude nitrobenzene. The wash water and crude nitrobenzene overflow from the mixer to the gravity separator where crude nitrobenzene and water are separated. The separate crude nitrobenzene flows by gravity to the separating tank through the decanter. Wash water from the last stage gravity separator goes to first tower. A pH meter is installed in the line to measures and record the pH of water. All the vents from the wash tower, mixers and gravity separators are provided with flame arresters. The elevations of successive washing stage equipments are arranged in such ways that all the flow are by gravity. A process effluent tank is provided to collect the effluent i.e. red water, yellow water and neutral water from the washing section. The nitro phenols formed in small amount during nitration step. They are removed in the washing section and found as yellow and red water.
NORMAL OPERATINGCONDITIONS: (WASHING SECTION) 1) Process water to 2nd washing tower 2) Process water to 3rd washing tower 3) Process water to mixer 4) Caustic addition to 2nd washing tower :1885lit/hr :800lit/hr :2454lit/hr :68.2kg/hr
27
3. DISTILLATION SECTION: Crude nitrobenzene from the washing section flows into the separation tank where carried over water along with the wash crude nitrobenzene is allowed to settle and the water is decanted out from the tank. Crude nitrobenzene from the bottom of the tank overflow, is equipped with panel level indicators and flame arresters. Crude nitrobenzene is then pumped to distillation column through crude nitrobenzene filter. It is then passed through NB/NB exchanger where it is preheated up to about 700C by outgoing hot nitrobenzene stream from the reboiler. Crude nitrobenzene contains unreacted benzene, water and traces of dinitrobenzene. The distillation column is provided with bubbles cap. Distillation column is provided with a specially constructed steel reboiler. The HP steam is available at 20kg/cm2g and is supplied to the reboiler under the PCV & FCV control at 14kg/cm2g. The column is at an absolute pressure of 500mm Hg. The column temperature varies from about 60 0C at top to around 1630C middle and about 1720C at the bottom. The overhead vapors containing benzene and water are condensed in cooling water condenser and separated in reflux drum. Reflux drum is provided with bootleg to collect water. The benzene is refluxed back partially to the column. The benzene product is drawn on level control from the reflux drum to benzene intermediate tank. The bottom product from the reboiler, overflow to distilled nitrobenzene hold vessel. The nitrobenzene is pumped by column bottom pump to day storage tank through the feed product heat exchanger, nitrobenzene cooler. In order to minimize the benzene vapors going to the vacuum pumps, a chilled water vent condenser has been provided in the vapour line. The vacuum pumps are of liquid ring type, with nitrobenzene used as a liquid ring. PVC controls the pressure of the distillation column by bleeding in air at the vacuum pump section. A shutdown valve is provided in the vaccum line to prevent air entry into the column. An automatic nitrogen flowing system is provided to the distillation column from safety point of view, whenever column stop functioning air enters into the column at this point of time and leads to a hazardous situation, for this a shutdown valve on the steam, nitrogen and vacuum line, high pressure switch on vacuum line and low and high pressure switch are provided on the nitrobenzene hold vessel. All the shutdown valves and high-
28
pressure switch are interlock with vacuum pump. Hence when ever power failure or instrumental air failure or vacuum trip or vacuum failure (i.e. drop in vacuum) occurs; the steam and vacuum line shutdown valves will close. At this time vacuum In the column will start dropping down. When the vacuum in the column drops to 0.7kg/cm2g, the pressure switch, PSL on vessel will open the shutdown valve on nitrogen line till the pressure in the column reaches 1.1kg/cm2. At this pressure the PSL on vessel will close the shutdown valve on nitrogen line. This system pressure is kept above atmosphere so that air cannot enter in the system. NB distillation column consists of total 22 trays, the feed points are 15th, 16th, 17th trays.
NORMAL OPERATING CONDITIONS: (DISTILLATION SECTION) 1) Feed temperature: 2) Top temperature : 3) Bottom temperature: 4) Top pressure: 5) Bottom pressure : 6) Feed flow rate: 7) Reflux flow rate: 8) Steam flow rate: 9) NB product draw rate: 10) Top product draw rate: 900C 50-600C 1730C 0.3kg/cm2 0.45kg/ cm2 2305kg/hr 458kg/hr 368kh/hr 2087kg/hr 213kg/hr
29
CHAPTER 9 MATERIAL BALANCE

INTRODUCTION:The overall material balance around any system can be given by the equiation. Input - Output + Generation - Consumed = Rate of Accumulation At steady state, rate of accumulation = 0 DATA:Substance Benzene Nitric acid Nitrobenzene Sulphuric acid Water Sodium hydroxide Molecular weight 78.065 62.99 123.059 98.065 18 39.997
REACTION:
From the stoichiometry of reaction, 1 mole of Benzene Reacts with 1 mole of nitric acid to give 1 mole of Nitrobenzene and 1 mole of water.
30
The side reactions are nearly negligible. hence Production of byproducts (nitrophenol, dinitrobenzene etc.) is considered commonly under the label Impurities.
Conversion of Benzene Yield of Nitrobenzene Yield of nitric acid
98.5% 99.5% 99.1%
Capacity of Nitrobenzene plant =50 Tons/day. That means than production rate= 2083.333 kg/hr We are taking the hourly production as basis of calculation for convenience. Consider losses in the amount of nitrobenzene due to washing, incomplete considers to be 1%. Actual nitrobenzene production = =2104.167 kg/hr From reaction, we can write 1 mole of Benzene corresponds to 1 mole of nitrobenzene. 123.059 kg of nitrobenzene corresponds to 78.065 kg of Benzene. Amount of Benzene utilized = 1334.821 kg/hr
But, yield of nitrobenzene is 99.5%. 0.995= Total benzene reacted = 1341.529 kg/hr.
31
Conversion of Benzene = 98.5% Total Benzene charged = =1361.958 kg/hr For complete conversion of nitric acid, 16% Excess benzene is charged. Total Benzene charged = =1579.871 kg/h Benzene balance:Total Benzene charged (with 16% excess) = 1579.871 kg/hr. Total Benzene reacted =1341.529 kg/hr. Benzene reacted for formation of nitrobenzene =1334.821 kg/hr. Benzene reacted for formation of impurities = 1341.529-1334.821 = 6.708 kg/hr. Total unreacted Benzene = Total Benzene charged Total Benzene Reacted =1579.871 1341.529 = 238.342 kg/hr.
Mixed Acid Balance: 123.059 kg nitrobenzene corresponds to 62.99 kg Nitric acid For the 2104.167 kg/hr production of Nitrobenzene Amount of nitric acid required = 1077.056kg/hr The Yield on the basis of nitric acid is 99.1% Total nitric acid reacted =
32
=1086.837 kg/hr Nitric acid balance:Total nitric acid charged = 1086.837 kg/hr (Considering 100% conversion of nitric acid) Nitric acid for nitrobenzene production= 1077.056 kg/hr Nitric acid for Impurity production = 9.781 kg/hr
Mixed acid balance:We are using acid with 60% H2So2, 32% HNO3 and 8% H2O (All percentage are wt% basis) Amount of H2SO4 in mixed acid = 2037.819kg/hr Amount of HNO3 in mixed acid = 1086.837kg/hr Amount of H2O in mixed acid = 271.709kg/hr Total mixed acid charged = 3396.366Kg/hr Impurity Balance Let consider the benzene and nitric acid reacts to hive impurity without formation of water. Impurity= 9.781 + 6.708 =16.489kg/hr Water balance 1 mole nitrobenzene corresponds to 1 mol water formation. Amount of water formed =307.781kg/hr (Considering impurity formation leads to zero water formation).
33
Material Balance across the Nitrator Input (kg/hr) Benzene HNO3 H2SO4 H2O Nitrobenzene Impurity Total 1579.871 1086.837 2037.819 271.709 ___ ___ 4976.236 Output (kg/hr) 238.342 ___ 2037.819 579.49 2104.167 16.489 4976.307
The error corresponds to error of approximation. 2. Gravity separator:Here two phases, Acid and organic phases are separated from each other. Consider overall efficiency of Gravity separator to be 99.5%. (The percentage of nitrobenzene removed in waste acid depends on temperature and efficiency of separation and it is approximately 0.5% of yield. These losses are excess of true solubility losses (They are neglected as they are much small in range.)) The Benzene in organic layer = 237.15 kg/hr Similarly we can write the Balance across the Gravity separator. Organic layer will content Benzene, NB and Impurities. And Acid layer will content the remaining (In excess ) As follows,
34
Input (kg/hr)
Output (kg/hr) Organic layer
Output (kg/hr) Acid layer 1.191 2027.063 576.593 10.521 0.082 2616.017
Benzene H2SO4 H2O Nitrobenzene Impurities Total
238.342 2037.819 579.49 2104.167 16.489 4976.307
237.15 10.189 2.897 2093.646 16.407 2360.289
The mixture of H2SO4 and water is called as spent acid, it contains 77.9% wt H2SO4.
3. Water washing tower Let 1000 kg/hr washing water is used to Assumptions. 1. The sulphuric acid will get completely washed. 2. The water will remain in benzene and nitrobenzene according to their solubility data and same excess water 2.0% of the added water. Solubility of Nitrobenzene at 30oc in water 0.257% . That means 100 grams water corresponds to 0.257 gm NB Total water in system/hr. 1000 + 2.897 =1002.897kg/hr 2.0 of water will remain as free water present = 20.058 kg water washing contains = 982.839 kg of water at output. Hence Nitrobenzene entrained with water = 2.526kg/hr
35
Similarly 1% of Impurities (Approximately) entrained with water. Benzene entrained with water (Solubility 0.07 part/100 part water at 220c) =0.688 kg/hr.
The Material balance is written as Input washing Benzene H2SO4 H2O Nitrobenzene Impurities Washing water Total 237.15 10.189 2.897 2093.646 16.407 1000.00 3360.289 0.688 10.189 ------2.526 0.104 982.839 996.346 Output Washed product 236.462 ----------2091.12 16.243 20.058 2363.883
4. Mixer:NaOH required for washing purpose 7 Kg/Ton Overall Requirement will be = 14.729 kg/hr Here the NaOH only reacts with impurity to form the sodium salts (other reactions are neglected)
36
Input (kg/hr) Benzene Nitrobenzene Impurities H2O NaOH Salts Total 236.462 2091.12 16.242 20.058 14.729 ------2378.61
Output (kg/hr 236.462 2091.12 -------20.058 -------30.972 2378.61
5. Dynamic Separator :Here again two phase will separated from each other organic phase contains -
Nitrobenzene, Benzene Acid/ Aq. Phase contains H2O +Salts in excess Calculation are similar as for first separator overall efficiency = 99.5% Material Balance Input (kg/hr) Output (kg/hr) Organic phase Benzene Nitrobenzene H2O Salts Total 236.46 2091.12 20.058 30.972 2378.602 235.278 2080.664 0.1 0.155 2316.197 Aq. Phase 1.182 10.456 19.95 30.817 62.405
37
6. Water washing Tower:Again 1000 kg/hr water is used. Total water = 1000.1 kg.hr let us consider Total traces of salts get washed away in this stage. Free water remained 30% Excess As it is required for further process of distillation = 300 kg/hr Nitrobenzene entrained with water = 1.799 kg/hr Benzene entrained with water = 0.49kg/hr
Material Balance Across washing Tower Input (kg/hr) washing Benzene Nitrobenzene H2O Salts Wash water Total 235.278 2080.664 0.1 0.155 1000 3316.197 0.49 1.799 -----0.155 700.1 702.544 Output (kg/hr) Product 234.788 2078.865 300.0 ----------2613.653
7.
Separator:Here the organic layer is much excess than aqueous layer hence higher degree of
separation is not possible. Hence, instead of considering overall efficiency Considering (approximately) individual efficiencies for organic phase =99.5% Aqueous phase = 94.5% (Approximate consideration)
38
Material Balance across separator Input (kg/hr) Output (kg/hr) Organic phase Benzene Nitrobenzene Water Total 234.788 2078.865 300.0 2613.653 233.614 2068.471 18.00 2320.085 Aq. Phase 1.174 10.394 282.0 293.568
8. Distillation column:As stated, 91% wt Benzene and 9% water forms azeotrope which boils at constant temperature. Hence extra benzene addition is required 9 kg water corresponds to 91.
Benzene 18 kg water corresponds to 182 kg Benzene : Benzene required = To be added for Azeotrope formation = 182 152.119 Input Benzene Nitrobenzene Water Kg/hr 233.614 2068.471 18 = 29.881 kg/hr Kmol/hr 2.995 16.809 1.0
39
XF = 0.192 Let XD = 0.998 XW =0.002
(More volatile basis)
( Approximately)
F = 20.804 Kmol /hr We can write F=D+w D + W = 20.804 XF *F = D* XD -----------(1) + W*XW
0.192 (20.804) =0.998D + 0.002 W 0.998D + 0.002W = 3.323 Solving equation (1) and (2) D = 3.9686 kmol/hr W = 16.8354 kmol/hr Material Balance (kmol /hr) Feed Nitrobenzene Water-Benzene TOTAL 16.801 3.995 20.804 Distillate 0.0079 3.9607 3.9686 Bottoms 16.8017 0.0337 16.8354 ------------(2)
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Material Balance (kg/hr) Feed Nitrobenzene Water-Benzene TOTAL 2068.471 251.614 2320.085 Distillate 0.9722 249.4536 250.4258 Bottoms 2067.6004 2.1225 2069.7229
Average molecular weight of water Benzene Azeotrope = 62.9822
Mixed acid preparation unit Mixed aced (3396.366 kg/hr) is produced with strength 60% H2SO4, 32% HNO3 and 8% H2O (by wt%) by blending. 1.98% H2So4 2.98% HNO3 and water if essential Mixed Acid = 3396.366 kg/hr It Contains 60% H2SO4 (100%) 32% HNO3(100%) 8% water Hence 98% H2SO4 Required 90% HNO3 Required H2O required = 2079.408kg/hr = 1109.017 kg/hr = 207.941 kg/hr 2037.820Kg/hr 1086.837Kg/hr 271.709Kg/hr
41
CHAPTER 10 ENERGY BALANCE

The nitration reaction is controlled by system additional cooling designed to withdraw the energy evolved. Additional cooling designed to withdraw the energy evolved. When all the energy set free by an exothermic reaction is forced to appear as heat the quantity of it lost to the cooling mechanism equals the decrease in enthalpy. Q=-H Here Q, the heat of reaction, represents the total energy i.e. amount of heat lost by the reacting system from start to end of the reaction. Kate for energy balance * * Cp of water = 1 kcal / kg 0C Cp of Benzene = -8.79 + (116.0 10-3) T + (-76.0 106 ) T2 + (18.9 10-9) T3 Where T = temperature (k) * Cp for nitrobenzene (kcal/(kg At At At At At * 300c 500c 700c 900c 1200c = = = = =
0
(Cal/(mol.k))
c ))
0.339 0.330 0.330 0.343 0.342
Cp of HNO3 = 13.438 cal /(mol k ) ( at 250c) = 13.930 cal/(mol k) (at 550c)
* *
Cp of H2SO4 = 139.1 + 15.59 10-2T J/(G mol 0c) X of water = 540 kcal/ kg
42
* *
X of Benzene = 94.4 kcal/ kh Enthalpy (specific) of steam = 668.2 kcal/kg At 19 khf/cm2 (saturation temp. 208.810c
1.
Acid mixing unit
The acids mixed are 1. 2. 3. 2079.408 kg/hr ; 98% H2SO4 1109.017 kg/hr ; 98% HNO3 207.941 kg/hr ; H2O
Consider room temperature at 250c 1. Enthalpy of 98% H2SO4 Total acid content = 98% HNO3 Content of unhydrous acid = 0% Enthalpy at 00c = -9.45 kcal/ kg C = 0.34 kcal/ (kg 0C) Enthalpy at 250c = - 9.45 + (0.34) (25) = -0.95 kcal/kg 2. 98% HNO3 Total acid content = 90% HNO3 Content of anhydrous acid = 100% Enthalpy at 00c = - 5 Kcal/kg. C = 0.47 kcal/ (kg
0
c)
Enthalpy at 250C = -5 + (0.47) (25) = 6.75 kcal/kg
43
3.
H2O
Enthalpy at 00c = 0 kcal /kg C = 1.0 kcal/(kg 0c) Enthalpy at 250C = 25 kcal / kg
4.
Final mixed acid Total mixed acid = 92% HNO3 Content of anhydrous acid = 32.6% Enthalpy at 00c = -34.5 Kcal/kg C= 0.43 kcal/(kg 0c) Enthalpy at 250c = -34.5 + 25 (0.43) = - 23.75 kcal/ kg.
Heat of mixing : = 3396.366 (-23.75) [(2079.408) (-0.95) +1109.017 (6.75) +207.941 (25)] = -91372.65 kcal/ hr
Amount of heat required to raise temperature of mixed acid to 550C. T=300C. Q=(3396.366)(0.43)30 Q = 43813.12 kcal/hr
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Excess heat can be utilize to heat the raw reactant Benzene from 25 0c to reaction temperature 550c. Specific heat of Benzene at ( )
0
=20.642 kcal/ (kmol) Total feed of Benzene =1579.871 kg/ hr =20.254 kmol/ hr Amount of heat required to heat the benzene =20.254 20.642 30 =12542.492 kcal/hr Excess heat = 91372 - (12542.492 + 43813.12) = 35016.958 kcal/hr This heat is removed by water cooling. Let temperature of water increases by 150c mCp T = 35016.958
=2334.46 kg/hr
2.
Nitration reactor -
H2 at 550c = -35.103 kcal/ mol Nitrobenzene formed To
calculate the heat balance around the reactor 1. 2. 3. 4. Enthalpy of feed mixed acid at 550c Heat of reaction at 550c Enthalpy of spent acid at 550c Heat removed by water cooling.
Nitrobenzene formed = 2104.167 kg/hr =17.10 kmol/ hr
45
Heat of reaction
HR = 17.099 103 (-35.103) HR = -600226.19 kcal/ hr
2.
Enthalpy of mixed acid at 550c = 3396.366 (-23.75) + 43813.12 = -36850.572 kcal/ hr
3.
Enthalpy of spent acid It contains 2037.319 H2SO4 (100%) and 579.497 kg H2O Total spent acid = 2616.816 kg/ hr Total acid content = 77.86% HNO3 Content of unhydrous acid = 00c Enthalpy at 00c = -65.5 kcal/ kg C = 0.45 kcal/(kg oC) Enthalpy at 550c = -65.5 + (55) (0.45) = -40.750 kcal/ kg
Total enthalpy associated with spent acid = -40.750 2626.816 = -106635.25 kcal/ hr Total heat change = HR at 550c + Enthalpy of mixed feed acid at 550c - Enthalpy of spent acid at 550c. = -6002261.3 - 36850.572 + 106634.966 = -530476.906 kcal /hr This excess heat is removed from the Nitrator by circulation of water at room temperature T = 100c mCp T = 530476.906 kcal /hr Let outlet temperature of water be 350c
46
4. Washing tower :Feed to the washing tower consist of crude nitrobenzene, benzene and spent sulphuric acid with traces of other impurities. Water added is at 250c and at a flow rate of 1000 kg/hr consider the products leaves washing tower at room temperature. Hence mCp (product) = mCp T(water) (Neglecting impurities) mCpT (product) = 1000 1 T 1000 T Taking cp0 at avg. temp = 400c
= [(237.15 20.625) / 78.065] 30 +[(10.189 44.878) / 98.065] 30 +[(2.897 1 ) 30 ] +[(2093.846 0.335) 30 ]
1000 T
= 23152.079
T = 23.152 23.20C Water leaves at 48.20c products leaves at room temperature.
3.
Preheater
(mCp T) feed to Preheater = (mCp T) bottoms from distillation column (The column temperature varies from 750c at top 1600c at middle and 1700c at bottoms.) Feed to Preheater enters at 250c leaves at 700c Bottoms enters the Preheater at 1700c
Average temperature (for feed) =42.50c =315.5 k [45 (2.995 20836 )] + 2068.471 0.333 45) +(18 1 45 )
47
= T (2062 .441 0.333) (Neglecting water-benzene Azeotropefraction ) T = 50.399 0c The bottoms leaves the Preheater = 170 - 50.399 = 119.6010c . 4. * Distillation column Enthalpy of feed at 700c = mcp T = (2.995 20.836 45 ) + (2068.471 0.333 45) +(18 1 45) = 34614.209 kcal/hr.. * Enthalpy of vapors = mCp T+ m
0
Average of temperature (neglecting Nitrobenzene fraction )
Boiling point of Benzene water fraction = 700c Hence, Neglecting the first term. = mX = 17.775 (540) + (233.614 94.4) = 31651.661kcal/hr.
Condenser load : Since there is no subcooling in condenser, cooling in condenser, cooling water is required to remove the heat of vaporization. Condenser load = mw X w + mB X w = 31651.661 kcal/hr.
Cooling water required Assume 150c change in water temperature mCp T = 31651.661 m = 2110.110 kg/hr Enthalpy of distillate at 700c (Average temp . = 480c) = (17.775 1 45 ) + (233.614 0.264 45) = 3575.209 kcal/hr Enthalpy of Bottoms (at 1700C) = = =
.
mCp T 2067.609 0.330 145 98935.091 kcal/hr
Reboiler duty = QB = Enthalpy of distillate + Enthalpy of bottoms + Condenser heat load enthalpy of feed .
= 3575.209 + 98935.041 + 31651.661 - 34614.209 = 99547.702 kcal/hr Flow rate of steam to reboiler. mH = QB m = 99547.702/668.2 = 148.9789 kg/hr
49
CHAPTER 11 DESIGN OF DISTILLATION COLUMN

Composition of feed: Component Benzene Nitrobenzene Total Molecular weight of Benzene = 78.065 Molecular weight of Nitrobenzene = 123.059 Flow rate 251.614 Kg/hr 2068.471 Kg/hr 2320.088 Kg/hr
Kg moles of Benzene = Kg moles of Nitrobenzene =
= 3.223 Kg moles = 16.80 Kg moles
Total moles of feed = 3.223 + 16.80 = 20.034 Kg moles
Composition of distillate: Component Benzene Nitrobenzene Total Flow rate 249.491 Kg/hr 0.9766 Kg/hr 250.4636 Kg/hr
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Composition of Residue: Component Benzene Nitrobenzene Total Flow rate 2.1225 Kg/hr 2067.609 Kg/hr 2069.7315 Kg/hr
Mole fraction of Benzene in Feed: Mole fraction of Benzene = = = 0.1609 Mole fraction of Benzene in Distillate (XD): = = 0.9975
Mole fraction of Benzene in Residue (XB): = = 0.0016
Mole fraction of Nitrobenzene in Residue: = Average molecular weight: = Of Feed = Of Distillate = Of Residue = = 0.9983
= 115.80 = 78.177 = 122.99

51
For vapour liquid equilibrium of Benzene Nitrobenzene system: According to Roults Law:Partial pressure = vapour pressure X mole fraction But, relative volatility = Ratio of partial pressure of one component to other component So here relative volatility of Benzene Nitrobenzene calculated: Vapour pressure of Benzene at 600C = 392.73 mm of Hg Vapour pressure of Nitrobenzene at 1700C = 261.771 mm of Hg Mole fraction of Benzene = 0.9975 Mole fraction of Nitrobenzene = 0.9983 Partial pressure of Benzene = 392.73 X 0.9975 = 391.7481 Partial pressure of Nitrobenzene = 261.771 X 0.9983 = 261.325 Relative volatility () = = Now from formula y= where y = mole fraction in vapour phase. x = mole fraction in liquid phase. So by varying values of x from 0.1 to 1 we can get different values of y and by getting x and y values x-y equilibrium curve can be plotted. e.g. calculation of No.1 x = 0.1 = 1.50 = 1.50
52
y= = 0.143 Like this X 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 y 0 0.143 0.272 0.391 0.5 0.6 0.693 0.778 0.887 0.931 1
Procedure details for finding the number of plates in the column: 1) First plot the equilibrium curve i.e. mole fraction of benzene in vapour (on Y axis) against mole fraction of water in liquid (on X axis). 2) Plot points (XD,XD),(XF,XF) and (XB,XB) XD = 0.9975 XF = 0.830 XB = 0.0016 3) Draw q line from point (XF,XF) 4) Calculate Y intercept i.e.
= 0.166
5) Joint Y intercept and (XD,XD)

6) Draw a line from point (XB,XB) through intersection of q line and (XD,XD) and Y intercept. 7) Draw right angle triangle (steps) between curve and operating lines. Both for stripping and rectification. Total number of triangle from point (XD,XD) to (XB,XB) will be the number of plates and step straddling line is the correct feed plate location.
Result from graph: Total no. of plates = 24 Number of feed plate = 8
Determination of column diameter: Vapour mass flow rate (top): i.e. VW = D (R+1) Where D = Distillate = 250.4636 Kg/hr R = Reflux ratio =5 VW = 250.4636(5+1) = 1502.7816 Kg/hr = 0.4174 Kg/s Liquid mass flow rate (Bottom): LW = (R*D) + F = (5*250.4636) + 2320.88 = 3573.198 Kg/hr = 0.9926 Kg/s Pressure at top of the column = 0.3 Kg/cm2 = 0.2904 atm Pressure at Bottom of the column = 0.45 Kg/cm2 = 0.4355 atm
54
Top condition: Temperature at top = 600C = 333.150K Average molecular weight = 78.177Kg/Kg of moles Liquid density = 881 Kg/m3 Vapour density = 2.8 Kg/m3
Bottom condition: Temperature at top = 1700C = 443.150K Average molecular weight = 122.99Kg/Kg of moles Liquid density = 1197 Kg/m3 Vapour density = 4.25 Kg/m3
Plate spacing = 0.3048 (1 ft) The overall height of the column will depend on the plate spacing. Plate spacings from 0.15 m (6 in.) to 1 m (36 in.) are normally used. The spacing chosen will depend on the column diameter and operating conditions. Close spacing is used with small-diameter columns, and where head room is restricted; as it will be when a column is installed in a building. For columns above 1 m diameter, plate spacings of 0.3 to 0.6 m will normally be used, and 0.5 m (18 in.) can be taken as an initial estimate. This would be revised, as necessary, when the detailed plate design is made. A larger spacing will be needed between certain plates to accommodate feed and side streams arrangements, and for man ways. Column diameter:
Where, uv = maximum allowable vapour velocity, based on the gross (total) column crosssectional area, m/s, l = plate spacing, m, uv = (-0.171*0.30482 + 0.27*0.3048 0.047)* uv = 0.40 m/s +
55
The column diameter, Dc, can then be calculated:
=* =1.062m Column height
= number of trays X (tray spacing + thickness of tray) = 23*(0.3048+0.005) = 7.1254 m
56
CHAPTER 12 HAZARDOUS CHEMICAL SAFETY DATA CLASSIFICATION
A. a) b) c) B. a) C. a)
CORROSIVE SUBSTANCES Sulfuric acid. Nitric acid Caustic soda lye/flakes. FLAMMABLE LIQUIDS. Benzene. TOXIC CHEMICALS. Nitrobenzene.
The health hazards, fire hazards, handling and first aid to be taken during spillage if any, are dealt with a under. A. CORROSIVE SUBSTANCES
a.
SULFURIC ACID Health Hazard: Due to its corrosive oxidizing and sulphonating properties, sulfuric acid produces
rapid destruction of tissues and severe burns. On contact with body causes skin irritation. Contact with eyes rapidly causes severe damage to the eye lens. Inhalation of concentrated vapor or mist from hot acid will cause damage to the upper respiratory tract and even to the lung tissue. Explosion hazard: No naked flame of any kind should ever be permitted near an opening of the tank for any purpose otherwise it may result in the ignition of hydrogen gas likely to be present near the opening and create an explosion. For this reason portable electic lights should be of the explosion proof type for use in hazardous locations.
Preventive health measures: Sulfuric acid is not a serious industrial hazard. Contact with skin and eyes, inhalation of vapors or mists should be avoided. Protective equipment as goggles, face shield, gloves, shoes, apron, air respirator are to be worn while handling acid depending upon the area of operation.
b.
NITRIC ACID
Health hazards: The vapor will consist mixture of various oxides of nitrogen and nitric acid. Nitric acid vapor is highly irritant to the mucus membrane of the eyes and respiratory tract and to the skin. Severe burn may be caused on contact with the acid. Hazardous properties: The fire hazard is moderate by chemical reaction with reducing agents. It is a powerful oxidizing agent. The explosion hazard is slight by chemical reaction to evolve oxidizing of nitrogen. It can explode on contact with powerful reducing agent and other organic material. It is highly corrosive and attacks large number of metals. In case of contact: If a person comes in contact with this acid, wash the affected part immediately with plenty of water at least for 15-20 min. He should rub the part while washing with water. If he has inhaled fumes of nitric acid, remove him from the work place to have sufficient fresh air and send to hospital for medical treatment. In case of oral poisoning dilution is much more important than an antidote. Therefore large quantities of water should be given. It is dangerous to induce vomiting when the patient has swallowed corrosive acid. Neutralizing drinks as milk, magnetia can be given. Carbonates or bicarbonates should not be given for acid oral poisoning.
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c. CAUSTIC SODA Hazardous properties, precautionary measures with first aid: The most common injuries suffered with caustic soda are burns of the skin or eyes when containers are opened. Another common source of injury is the splashing of the concentrated solution caused by attempts to dissolve the flakes in hot water. First aid consist of washing away the flakes or solution with large amount of cold water for about 1 hour preferably under the safety shower and then treating the injury. The washing of alkali burns should be done well, because of the tendancy of the alkalies to penetrate into the skin and continue to burn even after washing. Eyes injured by caustic soda should be washed with a gentle stream of water for at least 15 mints and then, be immediately brought under medical care.
Precautions: 1. Containers into which caustic is to be run should be absolutely dry and free of acid
in order to guard against explosions. 2. 3. People who are exposed to caustic should wear personal protective equipments. Spent caustic solution should not be let into sewers.
Oral poisoning and first aid: If taken internally, it causes severe burns of the mucous membranes of the mouth, throat and stomach. Dilute vinegar or 5% solution of ammonium chloride should be administered. If not, allow drinking plenty of water without delay. As a soothing agent whites of eggs or mineral oil may be given.
59
B) FLAMMABLE LIQUIDS : a) BENZENE : Health hazards : The greatest hazard of benzene is chronic poisoning by inhalation of comparatively small amounts over a long period of time . It is one of the most dangerous organic solvents in use. Chronic absorption of benzene may lead to a fall in red blood cell count . The maximum acceptable concentration of benzene in air for an 8 hrs, has been set at 25 ppm by volume (MAC) by American Conference of Governmental Industrial Hygienists. Important points in preventing the blood changes due to exposure of benzene are (1) the physical prevention of absorption of benzene vapors. (2) The maintenance of diet rich in protein. Explosion Hazards : Benzene is highly flammable and its vapor forms explosive mixtures with air . Benzene when it comes in contact with skin produces dryness and cracking of the skin. Contact with eyes : If benzene enters the eye, flush thoroughly with plenty of water for at least 15 minutes. If irritation persists get medical aid soon. Protective wears includes goggles, Benzene
gloves, safety shoes, face shield, airline masks for respiratory protection etc.
attacks natural rubber hence all protective equipments must be cleaned inside and outside, each time before and after thet are used. Equipment cleaning : The tank or equipment should be steamed to remove residual benzene and vapors. The steaming should be done above the boiling point of benzene (80 0c) it should be
continued till the benzene vapors have been removed. Then the tank or vessel is to be cooled with water by filling once or twice and then purged with fresh air.
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C) TOXIC CHEMICALS : a) NITROBENZENE Health hazards : Nitrobenzene is highly toxic and its maximum allowable concentration is I ppm in air (5m3). But it can be handled safely with proper precautions. It is readily absorbed by direct contact through the skin, by inhalation of vapor or by ingestion . Absorption in toxic quantities leads to cyanosis or blue lip. The probability of poisoning by inhalation of vapor from cold liquid is not great . nitrobenzene is primarily a blood and nervous system poison. Contact with skin : Wash the affected area thoroughly with warm water and soap. contaminated clothing and launder before using again. Contact with eyes : Through nitrobenzene is not highly irritatiog to the eyes, on receiving a splash, eyes should be washed well with water for at least 15 minutes and immediate medical attention should be obtained . Ingestion : If swallowed administer lukewarm water or lukewarm emulsion of soap. General: A complete bath with warm water and soap and complete change of clothing is a must at the end of each shift. Bo food or tobacco should be permitted in the work area. Protective equipments : Goggles, hand gloves, apron, shoes, air line masks are to be used while working in nitrobenzene area. Severe exposure is likely to escaping vapors. After use, the protective equipment must be thoroughly cleaned and well ventilated. Remove the
61
Spills and Leakages : Spilled nitrobenzene should never be left unattended. Flush with plenty of water till the smell of nitrobenzene disappears. The absorbed liquid can then be washed with hot water. Tank and equipment cleaning : Drain the tank completely. Rinse thoroughly with cold water with a view to remove any mud, as it mat tend to hold traces of nitrobenzene. Then introduce live steam and allow the condensate to drain ort. Increase steam to heat the tank thoroughly till all nitrobenzene smell is gone. Cool the equipment/tank.
b) NITROPHENOLS: These are formed in small amounts in nitration step. They are removed in the washing section and are found in the red and yellow water. Nitrophenols are very toxic compounds not only when ingested but also when inhaled or absorbed through skin. The toxicity is enhanced by increase in external temperature and by thyroxin, so people with hyperthyroid activity should not be exposed to nitro phenols. Permissible 4 mg/m3 of air.
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CHAPTER 13 QUALITY CONTROL
SAMPLE
LOCATION
TEST
STANDARD VALUES
Spent acid Before extraction
Separator S-5709 Bottom
Sp.Gr@ 27-300C T.A% H2SO4% HNO3%
1.660-1.690 74.30-77.00 74.00-77.00 0.20% Max 1.140-1.159 11.00-16.00 0.18% Max 5.5 Min 1.197-1.200 0.18% Max 5.5 Min 5.50C 0.1% Max
Crude Nitrobenzene
Separator S-5815 Top
Sp.Gr@ 27-300C Benzene% DNB% pH
Product Nitrobenzene
Sp.Gr@ 27-300C DNB% E-5912 pH Set point
Sp. Acid after extraction
Separator S-5713
HNO3
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CHAPTER 14 PLANT LOCATION

CONCEPT AND FACTORS GOVERNIG PLANT LOCATION:A plant is a place where men, money, equipment, machinery ect. Brought together for manufacturing products. Plant location means deciding a suitable location area, plan etc. , where the plant or factory start functioning. Activities involves, first to select a proper geographic region and second selecting a specific site within region. Plant location plays a major role in the design of production system as it determines the cost of, 1) 2) 3) Getting suitable raw material. Processing raw material to finished goods. Finished product distribution to customers.
VARIOUS FACTORS, AFFECTING PLANT LOCATION:1) Nearness to raw material:- especially those plants, which consume raw material in
bulk or raw material is heavy, is cheap but loses a good amount of its weight during processing (trees and coal, saw mills) must be located close to the sources of the raw material. 2) Transport facilities:- depending upon the size of the raw material and finished goods,
a suitable method of transportation like roads, rail, water or air is selected and the plant location is decided. 3) Nearness to market:- it reduces cost of transportation as well as the chances of the
finished product getting damaged and spoiled in the way (especially perishable products). Also for catching big market and an render quick service to customers. 4) Availability of labors:- stable labor face, of right kind of adequate size (number) and at reasonable rates with its proper attitude towards work. The purpose of management is to face less boycotts, strikes to achieve lower labor cost per unit of production. 5) Availability of fuel and power (utility):- because of the wide spread use of electric
power in most cases fuel (coal, oil, etc.) has not remained as a deciding factor for plant
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location. It is of course essential that electric power should remain available continuously, in proper quantity and at reasonable rates. 6) Availability of water (utilities or services):- water is used for processing as in paper
and chemical industries and required for drinking and sanitary purpose. A chemical industry should not be set up at a location which is famous for water shortage. 7) Climate conditions:- as development in the field of heating, ventilation and air
conditioning, climate of the region does not present much problems of course, control of climate needs money. 8) Financial and other aids:- certain states gives aids as loans, feed money, machinery,
built sheds etc., to attract industries. 9) Land:- topography area, the shape of the site cost, drainage and other facilities, the
probability of floods, earthquakes etc. influences the selection of plant location. 10) Community attitude:- success of industry depends very much on the attitude of the
local people and whether they want work or not. 11) 12) 13) 14) 15) 16) 17) Presence of related industries. Existence of facilities: bank, hospitals, schools, post office etc. Local bye laws, building, ordinance taxes etc. ordinance: house of military vapons. Housing facilities. Security. Facilities for expansion. Effluent disposal :- All industrial process produces waste products and full
consideration must be given to the difficulties and cost of their disposal. The disposal of toxic and harmful effluent will be covered by local regulations and the appropriate authorities must be consulted during the initial site survey to determine the stad that must be met. 18) Political strategic considerations :- capital grants, tax concessions and other
inducements are often given by government to direct new investment to preferred locations, such as areas of high unemployment. The availability of such grants can be the overriding consideration in the site selection. 19) Flood and Fire protection :- Many industrial plants are located along rives or near
large bodies of water and there are risks of flood or hurricane damage (violent storm wind). Before choosing a plant site, the regional history of natural events of this type should be examined and consequence of such occurrence considered. Protection from losses by fire is another important factor in selecting a plant location. In case of major fire assistance from
65
outside fire department should be available. Fire hazards in the immediate area surrounding the plant site must not be overlooked. 20) Ordinance :- chemical plants are not usually looked upon as desirable neighbors.
They may be regarded as source of danger from possible explosion or because of fumes as a detriment to the health of community and to its vegetation. The result of propaganda against the industry has been that may. It is advisable to ascertain whether the attitude of community is particularly unfriendly to chemical manufacturing. If this is the case it is good policy to go elsewhere even though no restricting ordinances are in effect at that time. 21) Community factor :- the character and facilities of community can have quite effect
on the location of the plant. If the sufficient facilities not available than it become burden for the plant to subsidize such facilities. Cultural facilities of the community are important to sound growth. The problem of recreation deserves special consideration. The efficiency, character and history of both state and local government should be evaluated.
LOCATION OF NITROBENZENE PLANT :Considering all above factors, ideas location for this plant are Rasayani, M.I.D.C, Roha , Late Parshuram or any chemical zone in konkan reagion (Because transportation facilities are good i.e. Railway Road transportation going to available).
66
CHAPTER 15 PLANT LAYOUT

INTRODUCTION:Plant layout means the disposition of various facilities (equipments, material, etc.) and services of the plant with in the area of site selected previously plant layout begins of the factory buildings and goes upto the location and movement of the work table PRINCIPLES OF PLANT LAYOUTS :The research work is being continued in order to develop scientific approach for solving plant layout problems. Mathematical models and computer aided computer
techniques for balancing assembly lines. 1. Integration :- Integration of production facilities material etc., are logical and balance manner. 2. Minimum movements and material Balancing:- Numbers of movement of workers and material should be minimized. It is better to transport material in optimum bulk rather than in small accounts. 3. Smooth and continuous flood :- Bottle necks congestion. Points and back tracking should be removed by proper line balancing techniques. 4. Cubic space utilization :- Besides using the floor space of a room, If the ceiling height is used, more material can be accommodated in the same room. Boxes or bags containing raw material or goods can be staiked one above the other to place some more items in the same room. Overhead material handling equipment save a lot of valuable floor space. 5. Safe and Improved Environment:working places safe, well ventilated and free like workers, machinery, raw
from dust, noise, fumes, odour, and other hazardous conditions decidedly increases the operating efficiency of workers and improve their morale. All this leads to satisfaction amongst the workers and thus better employer-employee relations. 6. Flexibility :- In automotive and other industries where models of products change often possible flexibility in the layout. The machinery is arranged in such a way that the changes of production process can be achieved at the least cost or disturbance.
67
LAYOUT :Process units and ancillary buildings should be laid to hive most economical flow of contents and personnel around the site. Hazardous process must be located at a safe distance from other buildings. The ancillary buildings and service required on a site in addition to the main processing units (Buildings) will include a) b) c) d) e) f) g) h) i) Storage of raw material and products. Maintenance workshops. Store, for maintenance operating supplies. Laboratory for process control. Fire stations and other emergency services. Effluent treatment plant. Utilities, steam boiler, compressed air, power generation, refrigeration Office for general administration. Canteen, medical centers and parking facilities.
1. When laughing out the preliminary site layout the process units will normally be sited first and arranged to give a smooth flow of materials through the various processing steps, from raw material to final product storage. 2. The ancillary building should be arranged so as to minimize the spent time , by personnel travelling between buildings. Administration offices, laboratories were a large number of peoples will be working should be located well away from potentially hazardous process area. 3. Control rooms should be normally locate adjacent to the processing units, but with potentially hazardous process may have control room at a safer distance. 4. The siting of the main building will determine the layout of the plant roads. Access roads will be needed to each building for construction operation and maintenance. 5. The main storage area placed between the loading and unloading facilities and the process units they serve. 6. Storage tanks containing hazardous material should be sited away from the site boundary
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7. Base of the columns should elevated to provide the necessary net positive suction head to a pump. 8. Equipment that need to have frequent operating attention should be located bear to the control room, valve sample points, instruments should be located at a convenient position and heights. 9. Equipment that require dismantling for maintenance such as compressors and large pumps should be placed under cover. 10. Blast walls may be placed to isolate potentially hazardous equipment and continue the effect of an explosion. 11. At least two escape counts for operators must be provided from each level in process building. 12. Equipment should be located in such a way that it can be conveniently tied in with ant future expansion of process. Space should be left on pope alloys for future needs.
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70
CHAPTER 16 D.C.S SYSTEM

The NB phase 3 plant uses the DCS system for operating the plant. A distributed control system (DCS) refers to system a control usually of a manufacturing system, process or any kind of dynamic system, in which the controller elements are not central in location (like the brain) but are the distributed through the system with each component sub-system controlled by one or more controllers. The entire system of controllers is connected by networks for communication and monitoring. 1) DCS is a very broad term used in a variety of industries, to monitor and control distributed equipment. 2) Electrical power grids and electrical generation plants. 3) Environmental control systems 4) Traffic signals 5) Radio signals 6) Water management systems 7) Oil refining plants 8) Metallurgical process plants 9) Chemical plants 10) Pharmaceutical manufacturing 11) Dry cargo and bulk oil carrier ships
Elements: A DCS typically uses custom designed processors as controllers and uses both proprietary interconnections and communications protocol for communication. Input and output modules from component part of the DCS. The processor receives information from input modules and send information to output modules. The input modules receive information from input instrument in the process (or filed) and transmit instructions to the output instruments in the field. Computer buses or electrical buses connect the distributed controllers with the central controller and finally to the human-machine interface (HMI) or control consoles.
71
Elements of distributed control system may directly connect to physical equipment such as switches, pumps and valves or may work through an intermediate system such as a SCADA system.
Applications: Distributed control systems (DCSs) are dedicated systems used to control manufacturing processes that are continuous or batch oriented, such as oil refining, petrochemicals, central station power generation, fertilizers, pharmaceuticals, food and beverage manufacturing, cement production, steel making and paper making. DCSs are connected to sensors and actuators and use set point control the flow of material through the plant. The most common example is a set point control loop consisting of a pressure sensor, controller and control valve. The pressure or flow measurements are transmitted to the controller, usually through the aid of a signal containing input/output (I/O) device. When the measured variable reaches a certain point, the controller instruct the valve or actuation device to open or close the unit the fluidic flow process reaches the desired set point. Large oil refineries have many thousands of I/O points and employ very large DCSs. Processes are not limited to fluidic flow through pipes, however and can include things like paper machines and their associated quality controls, variable speed drives and motor control centers, cement kilns, mining operations, ore processing facilities and many others. A typical DCS consists of functionally and/or geographically distributed digital controllers capable of executing from 1 to 256 or more regulatory control loops in one control box. The input/output devices (I/O) can be integral with the controller or located remotely via a field network. Todays controllers have extensive computational capabilities and in additional to proportional, integral and derivative (PID) control can generally perform logic and sequential control. Modern DCSs support also neural networks and fuzzy application. DCSs may employ one or several workstations and can be configured at the work station or by an off-line personal computer. Local communication is handled by control network with transmission over twisted pair, coaxial or fiber optic cable. A server and/or application processor may be included in the system for extra computational data collection and reporting capability.
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CHAPTER 16 CONCLUSION
My project is called as the Detail Process Of Manufacturing Nitrobenzene in practical sense. It gave me opportunity to correlate theoretical knowledge obtained at University and practical things obtained at plant. With project, I able to visualize work situation better and find it easier to adopt factory working later. I am also able to study relevant subject better and integrated teaching. For us, on job, training period also reduced. As a student of B.Tech chemical engineering I tried my level best to achieve maximum during my project and I am sure that this will greatly helpful to me as an engineer.
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REFERENCES
1) Perry P.H., Don Green (Ed.) Perrys Chemical Engineering Handbook, McGraw Hill. 2) Banga T.R., Sharma S.C., Industrial Organization and Engineering Economics, Eighteenth edition, Khanna publishers. 3) Bhatt B. I., Vora S.M., stoichiometry third edition, Tata McGraw Hill Publishing Company Ltd. 4) Himmelblue, David. M, Basic Principles and Calculations in Chemical Engineering, prentice hall of India pvt. Ltd., New Delhi. 5) Coulson J.M, Richardson R.K., Sinott R.K., Chemical Engineering Vol. 6 Third Edition. 6) Rao, M. Gopala, sitting Marsall Drydens outlines of chemical technology, second Edition. 7) J. M. Smith, H. C. Van Ness, M. M. Abbott, Introduction to Chemical Engineering Thermodynamics, Seventh Edition. 8) Robert E. Treybal, Mass-Transfer Operations, Third Edition, McGraw Hill. 9) H. Scott Fogler, Elements of Chemical Reaction Engineering, Fourth Edition. 10) Albright, L.F. Process for Nitration of Aromatic hydrocarbons - part I, chemical Engineering. 11) Albright, L.F. Process for Nitration of Aromatic hydrocarbons - part II, chemical Engineering.
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Detail Process of Manufacturing Nitrobenzene

CHAPTER 1 INTRODUCTION TO COMPANY

Detail Process of Manufacturing Nitrobenzene

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

CHAPTER 2 NITROBENZENE PLANT

caustic lay. Washing is carried out in five different stages.

DISTILLATION SECTION: Here distillation of crude nitrobenzene is done. Crude

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

CHAPTER 3 RAW MATERIAL, FINISHED PRODUCT AND BY PRODUCT SPECIFICATION

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

4. SPECIFIC GRAVITY: 1.84

:0.05% by wt. (Max.)

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

The tank farm consist of following tanks.

Nitric Acid Day Tank

Sulphuric acid Day tank

Benzene Underground Tank

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

Caustic Lye Tank

NaOH tank Nitrobenzene Hold vessel

Distilled NB Hold vessel

Spent Acid Day tank

Caustic preparation Tank

Separation tank Benzene Intermediate tank 1

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

Benzene transfer pump

Centrifugal, Self priming

S.S Alloy C.I S.S S.S

Centrifugal Centrifugal Centrifugal Metering Centrifugal

Process effluent pump Caustic transfer pump Crude nitrobenzene pump

S.S C.I C.I

Centrifugal Centrifugal Centrifugal

Nitrobenzene transfer pump

Nitrobenzene circulation pump

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

CHAPTER 4 USES OF NITROBENZENE

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

CHAPTER 5 PROCESS SELECTION

Detail Process of Manufacturing Nitrobenzene

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

CHAPTER 6 CHEMISTRY AND MECHANISM

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

3. Removal of proton gives nitrobenzene.

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

3. Picric acid (C6H2OH(NO2)3

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene

Department of Chemical Engineering, Dr. BATU, Lonere.

Detail Process of Manufacturing Nitrobenzene