4th Stage/Chemical Industries Ch.1 Chemical Processes Asst. Professor: A.

Al-Mosawi 1

Chapter 1. Chemical Processes

1.1 Introduction
Chemical processes usually have three interrelated steps:
1. Transfer of reactants to the reaction zone.
2. Chemical reactions involving various unit processes.
3. Separation of the products from the reaction zone.
Processes may involve homogeneous or heterogeneous systems.
Homogeneous system, reactants are in same phase liquid, gases or solids.
Heterogeneous system include two or more phases; gas-liquid, gas-solid, liquid-
solid. The type of reactions may be reversible or irreversible, endothermic or
exothermic, catalytic or non-catalytic.
Operating variables affecting chemical reactions are temperature, pressure, initial
reactants concentration, pH, catalyst activity, hydrodynamics ….etc.
The reaction may be carried out in batch, semi batch or continuous reactor.
Reactors may be batch (tank with an agitator), plug flow (PFR), CSTR. It may be
isothermal or adiabatic. Catalytic reactors may be fixed bed, moving bed or
fluidized bed.
The most important factors in chemical processes are:
1. Basic data are the physical and chemical properties of reactants and products.
2. Yield is that fraction of raw material recovered as the main product, the yield is
frequently above 90% for most reactions.
3. Conversion is that fraction of material changed to another desired product. The
conversion is limited by equilibrium, changing the operating conditions, the
equilibrium can be shifted and the conversion enhanced.
4. Kinetics is the study of order and reaction rate. Such information is essential for
plant design, since reaction rate determines equipment size. Catalysts are materials that
increase reaction speed.
Along with knowledge of unit processes and unit operation, the following information
and requirements are very important for the development of a commercial process:
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1. Material and Energy Balances, and Process Flow and Piping and Instruments
Diagrams (PFD and P& ID).
2. Raw Material purity and Energy Consumption per Ton of Product.
3. Batch vs. Continuous.
4. Chemical Process Selection: design and operation, pilot plant data, equipment
required, material of construction.
5. Chemical Process Control and Instrumentation.
6. Chemical Process Economics: Material and Energy Cost, Labor, Overall Cost of
Production.
7. Market Evaluation: Purity and Uniformity of Products for Further Processing.
8. Plant Location (layout).
9. Environment Protection, Health, Safety and Hazardous Material.
10. Construction, Building and Commissioning.
11. Management for Productivity and Creativity, Training of Plant Personals.
12. Research and Development (R&D); the strategy for developing new
technologies or products is an important concern in research and development
(R&D) departments for the chemical industry.
The chemical process is a combination of unit process and unit operation:
1.2 Unit Processes
Unit process involves principle chemical conversions leading to synthesis of useful
products and provide basic information regarding;
1. the reaction temperature and pressure, 2. the extent of chemical conversions, 3.
the yield of product of reaction, 4. the nature of reaction whether endothermic or
exothermic, 5. and the type of catalyst.
Some unit processes in chemical industries are given in Table 1.1
Nitration
Nitration involves the insertion of one or more nitro groups (-NO2) into reacting
molecules using nitrating agents such as nitric acid or mixture of nitric acid and
sulfuric acid in batch or continuous process. Nitration products find wide
application in chemical industry as solvent, dyestuff, pharmaceuticals, explosive,
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chemical intermediates. Typical products: TNT, Nitrobenzene, m-dinitrobenzene,

Nitroacetanilide, Alpha Nitronaphthalene, Nitroparaffins.
Table 1.1: Unit Processes in Chemical Industries

Halogenation
Halogenation is the replacement of one or more hydrogen atoms in an organic or
inorganic compound by a halogen (fluorine, chlorine, bromine or iodine) for
making different halogen derivatives. Although chlorine derivatives find larger
application, however some of the bromine and fluorine derivatives are also
important. Important chlorinating agents are; Cl2, HCl, phosgene (COCl2),
hypochlorite (NaOCl). For bromination; bromine Br2, hydrobromic acid HBr,
bromide Br−, sodium bromate NaBrO3, alkaline hypobromite BrO−. In iodination;
iodine I2, hydroiodic acid HI and alkali hypoiodites NaIO. In fluorination; fluorine
F2, hydrofluoric acid HF, and silver tetrafluoroborate AgBF4.
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Sulfonation and Sulfation

Sulfonation is defined as the replacement of H atom of an organic compound with a
sulfonic acid group _SO3H or corresponding salt like sulfonyl halide RSO2X.
Sulfonating agents are SO3 and its compounds, SO2, and sulfoalkylating agents.
Sulfation involves the replacement of H atom of an organic compound with a
sulfate -OSO2OH or -SO4- and for inorganic involves salts of sulfuric acid
(sulfates) are formed. Sulfonation and sulfation are major industrial chemical
processes used to make a diverse range of products, including dyes and color
intensifiers, pigments, medicines, pesticides and organic intermediates. Typical
application of sulfonation and sulfation are production of lingo sulfonates, linear
alkyl benzene sulfonate, Toluene sulfonates, phenolic sulfonates, chlorosulfonic
acid, sulfamates for production of herbicide.
Oxidation
Oxidation used extensively in the organic and inorganic chemical industry for the
manufacture of a large number of chemicals. Oxidation using O2 are combinations
of several reactions like oxidation via dehydrogenation using O2, dehydrogenation
and the introduction of O2 and destruction of carbon, partial oxidation,
peroxidation, oxidation in presence of strong oxidizing agent like potassium
permanganate KMnO4, sodium chlorate NaClO3, potassium dichromate K2Cr2O7,
hydrogen peroxide H2O2, lead dioxide PbO2, MnO2, nitric acid, oleum, and O3.
Oxidation maybe carried out either in liquid phase or vapor phase. Some of the
important products of organic oxidation are aldehyde, ketone, benzyl alcohol,
phthalic anhydride, ethylene oxide, vanillin, benzaldehyde, acetic acid, cumene,
synthesis gas from hydrocarbon, propylene oxide, benzoic acid, maleic acid, etc.
Hydrogenation
Hydrogenation is a chemical reaction between hydrogen gas (H2) and another
compound or element, usually in the presence of a catalyst such as nickel,
palladium or platinum. Some reactions with H2 gas are: hydrodesulfurization,
hydrocracking, hydroformylation (is an industrial process for the production of
aldehydes from alkenes), hydroammonolysis (is a process in which NH3-H2 mixture
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is made in the presence of a hydrogenation catalyst), synthesis of ammonia NH3,

hydrogenation of vegetable oils.
Hydration
Hydration is the process of combining a substance chemically with water
molecules. Hydrate, a term used to indicate that a substance contains water, many
minerals and crystalline substances are hydrates. In organic chemistry, water is
added to an unsaturated substrate, which is usually an alkene or an alkyne. This type
of reaction is employed industrially to produce ethanol, isopropanol, and 2-butanol.
Hydrolysis
Hydrolysis is the chemical breakdown of a compound due to reaction with water.
The reaction mainly occurs between an ion and water molecule and often changes
the pH of a solution. Hydrolysis is used both in inorganic and organic chemical
industry. Typical application is in oil and fats industry during soap manufacture
where hydrolysis of fats are carried out to obtain fatty acid and glycerol followed
by addition of NaOH to form soap. The types of hydrolysis reaction may be pure
hydrolysis, hydrolysis with aqueous acid or alkali, dilute or concentrated.
Electrolysis
Electrolysis is a chemical decomposition produced by passing an electric current
through a liquid or solution containing ions. Electrolysis is a technique that uses a
direct electric current (DC) to drive non-spontaneous chemical reaction.
Electrolysis is commercially important as a stage in the separation of elements from
naturally occurring sources such as ores using an electrolytic cell.
Esterification
Esterification is the conversion of carboxylic acid into an ester by combination with
an alcohol and removal of a molecule of H 2O. It is an important process in the
manufacture of polyethylene terephthalate, methyl meta acrylate, cellulose ester in
viscose rayon manufacture, nitroglycerine.
Alkylation
Alkylation is the transfer of an alkyl group from one molecule to another
compound by substitution or reduction. Products from alkylation find application in
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detergent, lubricants, high octane gasoline, photographic chemicals, plasticizers,

synthetic rubber, etc. Some of the alkylating agents are olefins, alcohols, alkyl
halides. Although sulfuric acid and phosphoric acid were commonly used as
catalyst in alkylation processes.
Polymerization
Polymerization is a process of reacting monomer molecules together in a chemical
reaction to form polymer chains or three-dimensional networks. Polymerization is
one of the very important unit processes which find application in manufacture of
polymer (polyethylene, polypropylene, PVC), synthetic fiber (polyurethane,
polyester), synthetic rubber, paint epoxy resin, etc. Polymerization may be carried
out either with single monomer or with co-monomer. Polymerization reaction can
be addition or condensation reaction. Also, polymerization methods may be bulk,
emulsion, solution, suspension.
Pyrolysis
Pyrolysis is a thermochemical decomposition of hydrocarbon at elevated
temperatures in an inert atmosphere. It involves the simultaneous change of
chemical composition and physical phase and is irreversible. Application involves
plastic and tire pyrolysis at temperature of 400-450 °C, in absence of oxygen to
break down into smaller molecules of oil and gas. The pyrolysis of coal is the first
step of gasification. Biomass pyrolysis include biochar, bio-oil and gas production
like CH4, H2, CO, and CO2.
Carbonization is the term for the conversion of an organic substance into carbon or
a carbon-containing residue through pyrolysis or destructive distillation.
Carbonation
Carbonation is created by adding dissolved CO 2 and carbonic acid into the liquid.
Carbonation is added to soft drinks to give the soft drinks a "bite" to them.
Methanation
Methanation is the reaction by which carbon oxides CO x and hydrogen H2 are
converted to methane CH4 and water. The reaction is catalyzed by nickel catalysts.
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1.3 Unit Operations

Unit operations are very important in chemical industries for separation of products
formed during the reaction. Table 1.2 give some details of unit operation in
chemical industries.
Table 1.2 Unit Operations in Chemical Industries

Distillation
Distillation is the process of separating the components or substances from a liquid
mixture by successive evaporation and condensation steps and most widely used
separation technology. Distillation is used in petroleum refining and petrochemical
manufacture. Distillation is the heart of petroleum refining and all processes require
distillation at different stages of operations.
Membrane Technology membrane is a selective barrier; it allows some ions or molecules to pass through and prevent others

Membrane technology is a generic term for a number of different, very

characteristic separation processes. These processes are of the same kind, because a
membrane is used. Membranes are used more and more often for the creation of
water treatment. Membrane technology has finding increasing application in
desalination, wastewater treatment and gas separation and product purification.
Membrane separation processes operate without heating and therefore use less
energy than conventional thermal separation processes such as distillation,
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sublimation or crystallization. The separation process is purely physical and both

fractions (permeate and retentate) can be used.
Absorption
Absorption is a physical or chemical process in which molecules or ions of gaseous
stream enter another absorbing bulk phase of gas or liquid. Absorption is the most
commonly used separation technique for the gas cleaning purpose to remove
pollutants such as H2S, CO2, SO2 and NH3. Cleaning of solute gases is achieved by
transferring to a liquid solvent with good contact of the gas stream and liquid
stream which offers specific or selectivity for the gases to be recovered. The
absorption is mass transfer phenomena where the solute of a gas is removed from
being fed in contact with a nonvolatile liquid solvent that absorbs the components
from the gas.
Solvent: Liquid applied to remove the solute from a gas stream.
Solute: Components to be removed from entering streams.
Adsorption
Adsorption is the adhesion of molecules of gas, liquid, or dissolved solids to a
surface based adsorbent. This process creates a film of the adsorbate (the molecules
or atoms being accumulated) on the surface of the adsorbent. Adsorption is present
in many natural, physical, biological, and chemical systems, and is widely used in
industrial applications such as heterogeneous catalysts, activated charcoal, air
conditioning and other process requirements (adsorption chillers), synthetic resins,
and water purification. Adsorption process is often a much cheaper and easier
option than distillation, absorption or extraction. One of the most effective method
for recovering and controlling emissions of volatile organic compounds is
adsorption. Some of the commercial adsorbents are silica gel, activated carbon,
molecular sieve, charcoal, zeolites molecular sieves, polymer and resins, clays,
biosorbents. Some of the key properties of adsorbents are capacity, selectivity,
regeneration, kinetics, compatibility and cost.
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Crystallization
Crystallization is a chemical solid–liquid separation technique, in which mass
transfer of a solute from the liquid solution to a pure solid crystalline phase occurs.
Crystallization occurs in two major steps. The first is nucleation; the appearance of
a crystalline phase from either a supercooled liquid or a supersaturated solvent. The
second step is known as crystal growth, which is the increase in the size of particles
and leads to a crystal state. The most important application in the petroleum
industry for separation of wax. The process involves nucleation, growth, and
agglomeration and gelling. Some of the applications of crystallization is in the
separation of p-xylene from xylenes stream. Typical process of separation of p-
xylene involves cooling the mixed xylene feed stock to a slightly higher than that
of eutectic followed by separation of crystal by centrifugation or filtration.
Solvent Extraction
Solvent extraction is a method to separate compounds based on their relative
solubilities in two different immiscible liquids, usually water and an organic
solvent. It consists of transferring one (or more) solute(s) contained in a feed
solution to another immiscible liquid (solvent). The solvent that is enriched in
solute(s) is called extract. The feed solution that is depleted in solute(s) is called the
raffinate. Liquid-liquid extraction has been commonly used in petroleum and
petrochemical industry for separation of close boiling hydrocarbons. Some of the
major applications are: removal of sulfur compound from liquid hydrocarbons,
recovery of aromatics from liquid hydrocarbon, separation of butadiene from C 4
hydrocarbons, extraction of acetic acid, removal of phenolic compounds from
wastewater, recovery of copper from leach liquor, and extraction of glycerides from
vegetable oil. Some of the important property of a good solvent are: high solvent
power/capacity, high selectivity for desired component, sufficient difference in
boiling points of the solvent and the feed for effective separation, low latent heat of
evaporation an specific heat to reduce utility requirement, high thermal and
chemical stability, low melting point, relatively inexpensive, non-toxic and non-
corrosive.
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1.4 Engineering Flowsheets

The engineering flowsheet of a chemical process describe in general, equipment,
operating details, and all reactions as that occurred, which should include data
covering not only materials, but labor and utilities as well.

Fig. 1.1 Typical flowsheet symbols

Process Flow Diagrams (PFD) are usually prepared when the design is completed and
are used to coordinate all the data from the drawings of individual plant items, which
must be prepared separately. It is conventional to show pipes with flanges, heat
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exchangers with supports, flanges and nozzles and so on, each item being given a
code number, various companies have their own ideas on this, but E for exchangers,
C for columns, V for vessel and so on seems to be generally accepted. Some useful
and generally accepted symbols are shown in Figure 1.1.
Piping and Instrument Diagrams (P&ID) are mechanical flow diagrams allied to the
engineering flowsheets. These include all pipe sizes, size and type of valves, pipe
fittings, etc., and are necessary where this information, which is required by
mechanical, electrical and instrument engineers, is too complicated to be included in
the process flowsheet. A portion of a typical piping flow diagram is shown in Fig.1.2.
In such diagrams it is conventional to number the various pipelines and branches as
an aid to clarity and also in locating lines once the plant is completed. There are a
multitude of systems, though the following coding is fairly widespread: nominal pipe
size/material code/sequence number.

Fig. 1.2 Part of a typical piping flowsheets

For example, `2-Cl-6a'-represents a 2 in. diameter, number 6a carrying chlorine,

whilst `4-S150-21' refers to pipe 21, which is 4 in. diameter carrying steam at
1501b/in2 g. Other material codes are fairly obvious and a matter of personal
reference. In numbering pipes, letters are often used to indicate branches. Useful
symbols for incorporation in such diagrams are as in Figure 1.3.
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Fig. 1.3 Symbols used in piping flowsheets

1.5 Chemical Process Design

The process engineer is a specialist in current aspects of chemical process design.

Practical experience is a necessity if the senior design engineer is to be able to
foresee and solve plant problems of a less obvious nature, such as maintenance,
safety, and conformation to government environmental controls. Experienced
consultants, either individuals or professional consulting firms, are available to
advise, design, and/or erect chemical process plants.
1.5.1 Process Development
Process development is a continuous interaction between experimental programs,
process design, and economic studies. The starting point is a chemical reaction
discovered in the laboratory, often accompanied by a suitable catalyst, and the
outcome is the production plant. A large part of the development activities is
concerned with scaling up from laboratory to full-scale industrial plant, with the
intermediate miniplant and pilot plant stages.
1.5.2 Process Evaluation
After each development stage the status of the process should be evaluated. The basis
for this evaluation is the documentation of the knowledge of the process gained so
far. The important questions to be answered are:
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1. Is the production process technically feasible in principle?

2. What is the economic attractiveness of the process?
3. How big is the risk in economic and technical terms?
The technical feasibility of a process is proven by research in the laboratory,
miniplant, and pilot plant. If certain process steps present difficulties, these problems
should be solved either by improving these steps or by selecting a different
procedure. The technical evaluation of a process aims to steer the process research
and development in the right direction.
1.5.3 Miniplants /Pilot Plants
Miniplant serves to test the entire process, including all recycles, on a small scale. Its
design is based on laboratory unit project of the process. The miniplant technique has
the following characteristics:
1. The miniplant includes all recycling paths and it can consequently be extrapolated
with a high degree of reliability.
2. The components used (columns, pumps, etc.) are often the same as those used in
the laboratory. In addition, miniplants usually contain standardized equipment that
can be reused in other miniplants, resulting in reduced investment costs and high
flexibility.
3. The miniplant is operated continuously for weeks or months and, therefore is
automated to a large degree.
4. The miniplant is used in combination with the mathematical simulation of the
industrial scale process.
Pilot plants are small-scale units designed to allow experiments that obtain design
data and displays operation for larger plants and sometimes to produce significant
quantities of a new product to permit user evaluation of it. Pilot plants range in size
more than miniplant to less than an almost commercial unit but are usually
intermediate in size. The development of a new process or product usually requires
miniplant or pilot plant work, or both. In particular with novel processes, scale-up
problems can often only be solved by experimental demonstration. Pilot plant
development experiments are expensive but frequently essential.
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The use of a miniplant together with mathematical simulation often makes it possible
to skip the pilot plant stage, though retaining the same scale-up reliability. As a result
it is possible to speed up process development, which can have a noticeable effect on
the cost effectiveness of a new process.
1.5.4 Equipment
Equipment is emphasized in conjunction with descriptions of the various processes
and with flowcharts representing these processes. Any chemical engineer should start
early to become familiar with industrial equipment such as pumps, filter presses,
distillation towers, nitrators, evaporators, sulfonators, electrolyzers, and fuel cells.
The Chemical Engineering Catalog includes convenient information concerning the
actual equipment that can be supplied by various manufacturers.
1.5.5 Corrosion, Materials of Construction
Successful operation of chemical plants depends not only on the original strength of
the materials of construction but also upon proper selection to resist corrosion.
Mechanical failures are seldom experienced unless there has been previous corrosion
or weakening by chemical attack. Erosion is occasionally a factor in the deterioration
of equipment; it can be reduced by avoiding sudden changes in flow direction.
Corrosion cannot be prevented; it can only be minimized. Advances in materials
science have provided many corrosion-resistant materials: rubber-covered steel,
resin-bonded carbon, and tantalum to resist hydrochloric acid; stainless steel to resist
the action of aqueous nitric acid and organic acids even under pressure; and nickel or
nickel-clad steel to resist caustic solutions, hot or cold. Polymeric organic materials
have become important in the fight against corrosion. Among the construction
materials used by chemical engineers are many of the commonest substances and
some of the rarest-brick, cast iron, steel, wood, cement, platinum, tantalum, and
silver. Corrosion testing must be done with commercial chemicals rather than pure
laboratory chemicals since it frequently happens that a small amount of a
contaminant in a commercial raw material affects corrosion appreciably.
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1.6 Scale-up
Scale-up makes use of laboratory and/or pilot plant data, complemented by mock-up
studies and mathematical modeling, to determine the size and dimensions of the
industrial unit. Mock-ups or “cold flow models” are usually used to simulate those
aspects of the process related to fluid flow. As the reactor is the core of the process
plant, two reactor categories are mainly dealt with;
1. Scale-up of Batch Reactors
A laboratory unit can be transposed to an industrial unit based on the reaction time
alone, provided the temperatures and the concentration of all components involved
are identical in both units. However, in practice this is often difficult to achieve. One
reason is that for processes involving highly exothermic reactions maintaining the
same temperature in a large unit as in the small laboratory unit is difficult.
Furthermore, mixing and hydrodynamic conditions in a large tank are different from
those in a small tank, resulting in concentration differences. Especially when the
reaction networks are complex, unexpectedly low yields and/or selectivity may be the
result.
2. Scale-up of Continuous Flow Stirred-Tank Reactor
The scale-up of this type of reactor usually involves the transposition from a batch
laboratory reactor to a continuous stirred tank industrial reactor (or cascade of
reactors). If the kinetics are known from small scale experimentation, this
transposition is relatively easy because scaling up is possible on the basis of the
kinetic model. The reactor scale-up problems need to resolve questions, for instance
about the influence of impurities on the catalyst activity, the mechanical stability of
the catalyst particles, and catalyst removal, particularly in homogeneously catalyzed
systems.
1.7 Instrumentation and Process Control
Instruments are the essential tool for modern processing. Automatic and instrument
controlled chemical processes are common and essential. Data processing and
computing instruments actually take over the running of complex chemical
processing systems. Some instruments can even optimize plant conditions to meet
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changing feed conditions. Instruments should be chosen simply to record process

variables and to assure:
(1) Quality, usually by sensing.
(2) Controlling.
(3) Recording.
(4) Maintaining desired operating conditions.
In large-scale continuous operations, the function of the workers and the supervisory
chemical engineer is to maintain the plant in proper running order. Batch sequences
require few instruments, hence more supervision on the part of the workers and the
process engineer because conditions or procedures usually differ from start to finish.
Even these problems can be solved by programmed instruments if the expense can be
justified.
Instrumentation has been forced into this position of importance by the increase in
continuous procedures, by the increased cost of labor and supervision, by the relative
unreliability of human actions, and by the availability of many types of instruments
and monitors at decreasing price and increasing reliability. Instrument types include:
1. Indicating instruments-presenting current data, value, or deviation from a norm
2. Recording instruments-permit study and analysis
3. Indicating/ recording and controlling instruments.
Two types of instruments are currently used, analog and digital:
Analog instruments such pressure spring, thermometers and Bourdon pressure gages,
that show results by mechanical movement of some type of device which is
proportional to the quantity being measured.
Digital devices generally utilize a "transducer" a device to convert the quantity being
measured into some type of signal (usually electrical or pneumatic) and electronic
circuitry to this signal to readable numerical figures (digits) which are displayed
and/or recorded.
Instruments are indicated by appropriate symbols with the following typical
abbreviations:
RTC recording temperature controller
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RFM recording flowmeter

ILC indicating level controller
ORFM orifice for recording flowmeter
PG pressure gauge
HPA high pressure alarm
In most designs, diagrams of instrumentation lines, power supplies, and so on, have
to be prepared. Instruments and control lines should be presented on the piping flow
diagram and on the drawings of the plant items together with full mechanical.
1.7.2 Chemical analytical control has been used in factory procedures for analysis of
incoming material and outgoing product, but generally conventional procedures are
too slow, expensive, and dependent on frequently questionable sampling procedures.
With the advent of fast, reliable, and sensitive procedures capable of automation,
control based on analysis within the process has become economically feasible.
Quality devices are produced far more reliably than when human analyses are used.
Chromatographic systems, pH sensors, conductivity meters, even mass spectroscopy
have been automated and used industrially.