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7-47 Physical Operations in Chemical Plants
Page 2 FM Global Property Loss Prevention Data Sheets
List of Figures
Fig. 1. Conventional distillation column. ........................................................................................................ 7
Fig. 2. Plate-tower absorber. .......................................................................................................................... 9
Fig. 3. Typical shell and tube heat exchanger. ............................................................................................ 14
List of Tables
Table 1. Typical Commercial Gas Absorption Systems ................................................................................. 9
Table 2. Properties of High Temperature, Inorganic Heat Transfer Media .................................................. 13
1.0 SCOPE
This document provides an overview of the hazards of the various physical operations conducted in chemical
plants (and often in other occupancy classes) as well as some basic loss prevention recommendations. The
common hazards are large quantities of flammable liquids and gases, high pressures and temperatures,
and operations that cause hazardous components to interact in an unintended manner. In many cases, there
also are references to other FM Global Loss Prevention data sheets that provide additional criteria for loss
prevention.
1.1 Changes
September 2010. Minor editorial changes were done for this revision.
2.1.2 Occupancy
2.1.2.1 Process vessels should be designed and installed in accordance with applicable recommended
practices for process vessel design; for example the ASME Boiler & Pressure Vessel Codes (or Interna-
tional equivalent).
2.1.2.2 Flammable liquid pumping and piping systems should be in accordance with Data Sheet 7-32,
Flammable Liquid Operations.
2.1.2.3 If the quantity of flammable liquid used in the process and the topography are such that escaping
liquid and water from fire protection systems would flow to surrounding installations, the processing area
should be curbed and emergency drainage to a safe location provided in accordance with Data Sheet 7-83,
Drainage Systems for Flammable Liquids.
2.1.2.4 Electrical equipment should be installed in accordance with NFPA 70, National Electrical Code®.
2.1.2.5 Inspection and maintenance procedures, operator training, and emergency procedures should be in
accordance with applicable recommendations in Data Sheet 7-43/17-2, Loss Prevention in Chemical Plants.
2.1.2.6 Safe limits of temperature, pressure, chemical composition of components, liquid levels, and flow
rates should be established for each process. Instrumentation and control equipment should be designed to
ensure that the process is operated within the specified safe limits at all times, including during shut-
downs, startups, and foreseeable malfunctions of equipment.
2.1.2.7 Where equipment operates with a flammable atmosphere, but must be converted to an air atmo-
sphere for maintenance, inerting or other FM Approved (see Appendix A for definition) procedure should be
established to avoid passing through the explosive range, unless the equipment is designed to withstand
the pressures developed by an internal vapor-air explosion.
2.1.2.8 Where materials in the process are subject to violent decomposition, polymerization, or runaway
reactions, they should be maintained safely diluted, inerted, or inhibited so that the reaction cannot take place;
or the process should be isolated so that an explosion or fire cannot affect other facilities.
2.1.3 Protection
2.1.3.1 Where flammable liquids or liquefied flammable gases are present in significant quantities, automatic
sprinkler or water spray protection should be provided in accordance with Data Sheet 7-14, Fire & Explo-
sion Protection for Flammable Liquid, Flammable Gas, & Liquefied Flammable Gas Processing Equipment
& Supporting Structures.
2.1.3.2 Where internal fires are possible, as with plastic packing materials or charcoal adsorption beds,
provide for manual internal water flooding.
2.2.2 Protection
2.2.2.1 Where flammable liquids or liquefied flammable gases are present in significant quantities, automatic
sprinkler or water spray protection should be provided in accordance with Data Sheet 7-14, Fire & Explo-
sion Protection for Flammable Liquid, Flammable Gas, & Liquefied Flammable Gas Processing Equipment
& Supporting Structures. If the process does not fall within the scope of Data Sheet 7-14, sprinklers should be
installed in accordance with Data Sheet 2-0, Installation Guidelines for Automatic Sprinklers (NFPA), with
water supplies in accordance with Data Sheet 3-26, Fire Protection Water Demand for Nonstorage Sprin-
klered Properties.
2.3.2 Occupancy
2.3.2.1 All equipment in the heat transfer system, including heat exchangers, piping, pumps, valves, relief
devices, and instrumentation should be suitable for the heat transfer media being used and for the tempera-
ture and pressure extremes anticipated.
2.3.2.2 Safe limits of operation should be established, both for the heat transfer system and the process it
serves, as to temperature, pressure, liquid level, flow rates, and chemical composition. Instrumentation and
control equipment should be provided to ensure that safe limits of operation are not exceeded.
2.3.2.3 Inspection and maintenance schedules should be established to maintain the heat transfer sur-
faces in satisfactory condition for efficient and safe operation of the process. Equipment should be arranged
to permit inspection and cleaning where corrosion, fouling, or deterioration is expected.
2.3.3 Protection
2.3.3.1 Where flammable liquids or liquefied flammable gases are present, automatic sprinklers or water
spray protection should be provided in accordance with Data Sheet 7-14, Fire & Explosion Protection for Flam-
mable Liquid, Flammable Gas, & Liquefied Flammable Gas Processing Equipment & Supporting Struc-
tures, as it applies.
2.3.3.2 Where combustible heat transfer equipment is used (as in cooling towers), automatic protection should
be provided in accordance with Data Sheet 1-6, Cooling Towers.
Materials used for the construction of operating equipment should not be affected by or react violently with
material being processed. For example, some halogens and halogenated compounds have reacted vio-
lently with aluminum parts on equipment when rubbing of the parts has dislodged the protective oxide or other
coating on the aluminum. Where practical, materials should be resistant to mechanical damage.
Gasket, packing, and lubrication materials in equipment should not react with or contaminate process
chemicals.
Vaporization and diffusion of flammable liquids or gases is the primary hazard in this group of operations.
The basic principle of safety for these operations is containment of the materials within the system, and keep-
ing the contents of the system out of the explosive range. Except for drying, these operations should be con-
ducted outdoors wherever possible. Adequate ventilation and explosion venting should be provided for
buildings and equipment. Precautions must be taken to eliminate sources of ignition.
3.3.1 Distillation
Distillation is the separation of a mixture into two or more fractions that have different normal boiling points.
The liquid mixture is normally heated; the vapor that comes off has a higher concentration of the lower-
boiling material than the liquid from which it was evolved. The system is often operated under a vacuum so
that the materials will boil at lower temperatures.
A condensed liquid that runs countercurrent to the uncondensed vapors is called reflux. Equipment in which
bubbles of vapor rise through descending condensate or reflux is called a rectifier.
A distillation column normally is a series of plates or trays. Each plate has some liquid on it and rising vapors
pass through and make contact with it. The reflux descends over a weir and through a downcomer to the
plate below. (See Fig. 1.)
After vapors leave the top plate they are condensed. The liquid runs to an accumulator. Some of this distillate
may be refluxed to the top of the column.
The feed normally enters near the center of the column.
The liquid from the bottom plate is partially vaporized in the reboiler at the bottom and partially drawn off
as bottoms or bottom product.
Packed towers containing stoneware such as Raschig rings may be used rather than plates. Normally, this
is in small diameter columns or for highly corrosive conditions. Column packing can also be plastic
construction.
A more complex column can have more than one feed or one or more streams withdrawn in addition to the
distillate and bottoms. Columns can be combined into systems, interconnected by recycle streams.
Where flammable liquids are being distilled, the distillation equipment will have a flammable vapor, above
the upper explosive limit, during operation. When opened up for maintenance, the flammable vapor must be
replaced with air. Unless inerting is done, the vapor will pass through the explosive range on startup and
shutdown.
If one or more components being distilled is subject to violent decomposition, explosive reaction, or polymer-
ization, the concentration of the component in either the vapor or liquid phase may produce a hazardous con-
dition. This may occur during operation, while temporarily shut down on total reflux, or when unforeseen
process upsets occur.
Failure of the distillation column, associated piping, or equipment may release substantial quantities of vapors
or liquids above their normal boiling points. This can result in a flammable vapor cloud explosion or flash
fire. If the column is under vacuum, air may enter the column and bring it into the explosive range.
3.3.2 Evaporation
Evaporation is the removal of a liquid from a solution or slurry by vaporization. It differs from distillation in
that no attempt is made to separate volatile components. It differs from drying in that it starts with a liquid while
drying normally starts with a solid. (Spray drying starts with a liquid but is normally classified as a drying
operation because of the equipment used.)
In evaporation, the vapor removed is usually water. Applications include the concentration of black liquor in
paper mills, concentration of juices and milk (dehydration), and conversion of sea water to fresh water.
Most evaporators are vessels containing bundles of tubes through which steam or other heat transfer fluid
is passed to supply heat and boil off the liquid. The vessel is often under a vacuum to lower the boiling tem-
perature. Several evaporators may be connected together, later stages operating at lower temperatures and
pressures to evaporate greater quantities from a given heat input (multiple effect evaporators).
If the liquid being evaporated is water, the process is normally low in hazard. If the vapors are flammable,
the hazards are similar to those of distillation with flammable liquids and vapors.
3.3.3 Drying
Drying is the removal of liquid from a substance by the application of heat or vacuum. (Processes that remove
a liquid without heat include filtration, decanting, and centrifuging.)
For descriptions of drying operations, discussion of hazards and recommended practices, see FM Global rec-
ommended practices for ovens and dryers (Data Sheet 6-9, Industrial Ovens and Dryers), spray dryers (Data
Sheet 7-76, Prevention and Mitigation of Combustible Dust Explosions and Fires).
Absorption processes are usually carried out in vertical counter-current flow through packed, plate, or spray
towers. The conventional packed tower is simply an empty shell filled with commercially available packing
materials. The liquid flows down over the packing and thus exposes a large surface to the gas flowing upward
through the interstices. In plate towers the liquid flows down in cascade fashion from plate to plate, counter
to gas bubbling up through each plate (Fig. 2). In spray towers the liquid is sprayed in fine droplets which
pass downward counter to the gas flow. (See also Data Sheet 7-48, Disposal of Waste Materials.)
Where either stream is flammable, the hazards are similar to those found in distillation. If the gas stream is
at a high temperature, such as flue gas from a combustion process, the liquid also may be acting as a cool-
ant. Interruption of liquid flow without interruption of the gas flow may lead to overheating, and fire if com-
bustibles are present.
Adsorption
Adsorption is the transfer of material from a gaseous or liquid mixture to the surface of a solid. The pur-
pose may be solvent or product recovery or pollutant removal. The solid is usually a material having a large
surface area, such as finely divided charcoal or silica gel. For additional information and safeguards see
Data Sheet 7-2, Waste Solvent Recovery.
3.4.1 Mixing
Mixing operations are found in nearly all chemical processes. They can include all possible combinations
of gas, liquid, and solid.
Gas-gas Mixtures. Gases can be mixed with simple jets, baffled columns, or tubes or by propellers or tur-
bines. Most operations are continuous. An example is diluting propane vapors with air to produce a fuel gas
similar to natural gas.
The primary hazard is a possible explosive mixture involving gases that react with one another.
Gas-solid Mixtures. The primary application of gas-solid mixing is in solid fuel burners, such as air-pulverized
coal mixing.
The primary hazard is a possible dust explosion when a combustible dust is mixed with air or other oxidiz-
ing material.
Gas-liquid Mixtures. Gas-liquid mixing is accomplished by producing small droplets in a gas stream or bubbles
in a liquid phase. This can be done by spray atomizing or churning.
Liquid-liquid Mixtures. Liquid-liquid mixing is very common, not only to achieve a homogeneous composi-
tion but also to achieve homogeneous temperature in heat transfer operations. Agitation may be achieved by
propellers, turbines, paddles, jets, pumps, turbulent flow tubes, and by shaking or revolving the container.
Liquids of very high viscosity such as pastes, doughs, or resins can be mixed by rollers or kneaders.
Frictional overheating of high speed agitators can occur if they are operated for a long period without suffi-
cient cooling. A side mounted horizontal propeller shaft can be bent if operated when it is partially submerged.
Liquid-solid Mixtures. Liquid-solid mixing produces slurries or suspensions such as paint, paper pulp in water,
ores in water, sewage sludge, and grain mash. Mixing may be done with paddles, propellers, turbines, air
bubbling, and rotating containers.
3.4.2 Filtration
Filtration is the separation of a liquid-solid or gas-solid mixture by means of a filter medium such as a screen,
cloth, or porous bed that permits the flow of fluid but retains the solid particles.
The most common example of a gas-solid mixture filtration system is an ordinary cloth-bag dust collector.
(See Data Sheet 7-73, Dust Collectors and Collection Systems.)
Liquid-solid mixtures may be filtered by passing the slurry under pressure through filter cloths laid on a series
of frames clamped together on a press or by drawing the liquid through a flat or cylindrical screen under
vacuum. Many products are separated by filtration including sugar, inorganic salts, rayon, dyes, sewage
sludge, and ceramics. Hazards of liquid-solid filtration are limited primarily to the possible escape of flam-
mable liquids or the accumulation of unstable chemicals.
3.4.3 Centrifuging
Centrifuging is the speeding up of gravitational separation of liquid and liquid-solid mixtures by high speed
rotation of the material.
Centrifuging is used in recovering sugar and inorganic salts; purifying animal, vegetable, and mineral oils;
separating milk and cream; ‘‘drying’’ laundry; and reclaiming cutting oils from metal chips.
The primary hazard is internal fires and explosions in equipment handling flammable liquids. The atmo-
sphere inside the machine can get into the explosive range, and the vapors can be ignited by frictional heat,
static sparks, or mechanical sparks.
Centrifuges present the problem of high speed equipment, and have seals and lubrication systems that must
be properly designed and protected.
3.4.5 Screening
Screening is the method of separating coarse from fine solid particles by passing them through various sized
meshes. The operation is used in producing cement, sugar, soap powder, crushed stone, sand and coal.
The operation is low in hazard unless combustible dusts are present.
3.4.6 Crystallization
Crystallization is the separation of solid material from solution by formation of nuclei and crystal growth. The
process is used in the production of inorganic and organic crystals. Where the solvent is water, the pro-
cess is low in hazard.
Where heated flammable liquids are used, the hazards are similar to those of flammable liquid distillation
and absorption.
Liquid-Solid Extraction and Leaching. A liquid may be used to extract a soluble constituent within a solid.
Where the constituent is a liquid bound up within cells of the solid, such as animal or vegetable oil, the pro-
cess is liquid-solid extraction. This process is common in the recovery of oils from grain or animal prod-
ucts, see Data Sheet 7-30N, Solvent Extraction Plants (NFPA). Where the constituent is a soluble mineral
material in an ore, the process is leaching.
3.6.1.1 Molten Salt for Heat Transfer. The most used molten salt (heat transfer salt), is a mixture of sodium
nitrite, sodium nitrate, and potassium nitrate. The mixture has a relatively low melting point for a salt, and
is noncorrosive to ordinary steels at temperatures below 850°F (455°C). At temperatures from 850°F to 1100°F
(455°C to 593°C), 18-8 stainless steel, Type 347, will satisfactorily withstand corrosion. At temperatures
above 850°F the salt is normally kept under an inert atmosphere to minimize oxidation and adsorption of car-
bon dioxide and water. The salt is noncombustible and stable, but it is an oxidizing agent, and can erupt
when molten if contaminated with organic material.
3.6.1.2 Molten Metals for Heat Transfer. Molten metals can be used for heat transfer at temperatures above
that for molten salts or organic fluids, but their use is rare outside of nuclear reactors because of cost and
because few processes require such temperatures.
Mercury is nonflammable, but is costly and highly toxic.
Sodium and its alloys burn in air and react violently with water. Special designs must be used and special
pumps provided to minimize this hazard, which add substantially to the cost.
Equipment Function
Chiller Cools a fluid to a temperature below that obtainable if water only were used as a
coolant. It uses a refrigerant.
Condenser Condenses a vapor or mixture of vapors, either alone or in the presence of a
noncondensable gas.
Exchanger Performs a double function: 1) heats a cold fluid by (2) using a hot fluid which it cools.
Reboiler Connected to the bottom of a fractionating tower, it provides the reboil heat necessary
for distillation. The heating medium may be either steam or a hot process fluid.
Steam generator or waste Generates steam for use elsewhere in the plant by using the available high-level heat
heat boiler in a process fluid.
Superheater Heats a vapor above the saturation temperature.
The basic principle of heat transfer equipment design is to provide a large surface area with minimum resis-
tance to heat flow. This is most often accomplished through standard shell and tube heat exchangers (Fig.
3). Concentric tubes can be used as well as hollow plates. Air-cooled heat exchangers are similar in con-
struction and operation to an ordinary automobile radiator. Process vessels can have internal or external coils
or a hollow jacket for heating or cooling. Heat transfer can be conducted without maintaining a separation
between the media, as in an ordinary cooling tower where air contacts and cools water droplets directly.
An accumulation of materials that reduce the rate of heat flow across a boundary means a reduction in the
effectiveness of heat transfer equipment and increased difficulty in maintaining temperature control. Where
heat transfer is very rapid, such as in a furnace, this could lead to a rapid increase in temperature in spots
and ultimate softening and failure. Instrumentation can usually detect general deterioration of heat transfer
surfaces, but careful inspection and maintenance is necessary to detect localized deficiencies.
A dangerous situation can occur if the level of the liquid being heated falls below the heating coils, since
heat transfer is reduced and overheating of the heat transfer surface above the liquid level can result.
4.0 REFERENCES
4.1 FM Global
Data Sheet 1-6, Cooling Towers.
Data Sheet 1-44, Damage-Limiting Construction.
Data Sheet 2-0, Installation Guidelines for Automatic Sprinklers.
Data Sheet 3-26, Fire Protection Water Demand for Nonstorage Sprinklered Properties.
Data Sheet 6-9, Industrial Ovens and Dryers.
Data Sheet 7-2, Waste Solvent Recovery.
Data Sheet 7-13, Mechanical Refrigeration.
Data Sheet 7-14, Fire & Explosion Protection for Flammable Liquid, Flammable Gas, & Liquefied Flammable
Gas Processing Equipment & Supporting Structures.
Data Sheet 7-30N, Solvent Extraction Plants.
Data Sheet 7-32, Flammable Liquid Operations.
Data Sheet 7-43/17-2, Loss Prevention in Chemical Plants.
Data Sheet 7-48, Disposal of Waste Materials.
Data Sheet 7-49/12-65, Emergency Venting of Vessels.
Data Sheet 7-55/12-28, Liquefied Petroleum Gas.
Data Sheet 7-59, Inerting and Purging of Tanks, Process Vessels, and Equipment.
Data Sheet 7-73, Dust Collectors and Collection Systems.
Data Sheet 7-76, Prevention and Mitigation of Combustible Dust Explosions and Fires.
Data Sheet 7-83, Drainage Systems for Flammable Liquids.
Data Sheet 7-88, Flammable Liquid Storage Tanks.
Data Sheet 7-95, Compressors.
Data Sheet 7-98, Hydraulic Fluids.
Data Sheet 7-99/12-19, Heat Transfer By Organic and Synthetic Fluids.
Data Sheet 7-100/13-16, Dynamic Compressors.
4.3 Others
ASME Boiler and Pressure Vessel Code.