Cryogenic Distillation

DISTILLATION
Introduction
Distillation is defined as: a process in which a liquid or vapour mixture of two or more substances is separated into its component fractions of desired purity, by the application and removal of heat. Distillation is based on the fact that the vapour of a boiling mixture will be richer in the components that have lower boiling points. Therefore, when this vapour is cooled and condensed, the condensate will contain more volatile components. At the same time, the original mixture will contain more of the less volatile material. Distillation columns are designed to achieve this separation efficiently.
Integrated Training Program / Phase B Distillation "o#$right % &!!' International (uman )esources De*elo#ment "or#oration
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Distillation Princi#les Separation of components from a liquid mixture via distillation depends on the differences in boiling points of the individual components. Also, depending on the concentrations of the components present, the liquid mixture will have different boiling point characteristics. Therefore, distillation processes depends on the vapour pressure characteristics of liquid mixtures. +a#our Pressure and Boiling The *a#our #ressure of a li,uid at a #articular tem#erature is the e,uili-rium #ressure e.erted -$ molecules lea*ing and entering the li,uid surface/ (ere are some im#ortant #oints regarding *a#our #ressure: energy input raises vapour pressure vapour pressure is related to boiling a liquid is said to boil when its vapour pressure equals the surrounding pressure the ease with which a liquid boils depends on its volatility liquids with high vapour pressures !volatile liquids" will boil at lower temperatures the vapour pressure and hence the boiling point of a liquid mixture depends on the relative amounts of the components in the mixture distillation occurs because of the differences in the volatility of the components in the liquid mixture
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D12INITIONS O2 3O)DS AND T1)4S 0S1D IN T(1 5AS P)O"1SSIN5 IND0ST)6

A-sor-er A tower or column that provides contact between natural gas being processed and a liquid solvent A-sor#tion A-sor#tion 2actor The operation in which one or more components in the gas phase are transferred to !absorbed into" a liquid solvent A factor which is an indication of the tendency for a given gas phase component to be transferred to the liquid solvent. #t is generally expressed as A $ %&''( where % and ( are the moles of liquid and vapor, and ' is the average value of the vapor liquid equilibrium constant for the component of concern. A-sor#tion Oil A hydrocarbon liquid used to absorb and recover components from the natural gas being processed. Acid 5as The hydrogen sulfide and&or carbon dioxide contained in, or extracted from, gas or other streams. Adia-atic 1.#ansion The expansion of a gas, vapor, or liquid stream from a higher pressure to a lower pressure in which there is no heat transfer between the gas, vapor, or liquid and the surroundings. Adsor-ent A solid substance used to remove components from natural gas being processed. Adsor#tion The process by which gaseous components are adsorbed on solids because of their molecular attraction to the solid surface
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Amine 8al9anolamine: Any of several liquid compounds containing amino nitrogen generally used in water solution to remove, by reversible chemical reaction hydrogen sulfide and&or carbon dioxide from gas and liquid hydrocarbon stream Associated 5as )aseous hydrocarbons occuring as a free*gas phase under original oil*reservoir conditions of temperature and pressure. Atmos#heric Pressure The pressure exerted on the earth by the earth+s atmosphere. A pressure of ,-. mm of mercury or /./.012. 34a is used as a standard for some measurements. State regulatory bodies have set other standards for use in measuring the legal volume of gas. Atmospheric pressure may also refer to the absolute ambient pressure at any given location. Barrel common 5nglish * unit measure of liquid volume which, in the petroleum industry, equals 61 7.S. liquid gallons for petroleum or natural gas liquid products measured at -.89 and equilibrium vapor pressure. :ne barrel equals ../2; cubic meters, or -.1; barrels per cubic meter !See 9ig, /*1". Blan9et gas A gas phase maintained in a vessel containing liquid to protect the liquid against air contamination, to reduce the ha<ard of detonation, or to maintain pressure of the liquid. The source of the gas is external to the vessel. Blo; "ase A small tan3 in which liquid is accumulated and then forced from the tan3 by applying as or air pressure above the liquid level. Blo;do;n The act of emptying or depressuring a vessel. This may also refer to discarded material, such as blow down water from a boiler or cooling tower. Boila;a$ Test Sometimes used to describe the )4A weathering test for %4gas. =efer to the definition of weathering test
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Bottoms The liquid or residual matter which is withdrawn from the bottom of a fractionator or other vessel during processing or while in storage. B<P mi. A liquefied hydrocarbon product composed chiefly of butanes and propane. #f it originates in a refinery, it may also contain butylenes and propylene. >ore specifically, it conforms to the )4A specifications for commercial ?*4 mixes as described in )4A Standard 1/6.. Breathing The movement of vapor in or out of an atmospheric pressure storage tan3 because of a change of level of the stored liquid, a change in the temperature of the vapor space above the liquid, or a change of atmospheric pressure. BS=3 8-asic sediment and ;ater: @aste that collects in the bottom of vessels and tan3s containing petroleum or petroleum products. Bu--le Point The temperature at a specified pressure at which the first stable vapor forms above a liquid. "ommercial Butane> A liquefied hydrocarbon consisting predominately of butane and&or butylene and which conforms to the )4A specification for commercial butane defined in )4A Standard 1/6.. Normal Butane> #n commercial transactions, a product meeting the )4A specifications for commercial butane and, in addition, containing a minimum of;2 liquid volume percent normal butane. Ahemically, normal butane is an aliphatic compound of the paraffin series having the chemical formula A6Bl: and having all of its carbon atoms Coined in a straight chain. "alorimeter An apparatus which is used to determine the heating value of a combustible material.
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"ar-on$l Sulfide A chemical compound of the aldehyde group containing a carbonyl group and sulfur !A:S". Sometimes a contaminant in natural gas and D)%. #t may need to be removed in order to meet sulfur specifications. "asinghead 5as 7nprocessed natural gas produced from a reservoir containing oil. #t contains heavier hydrocarbon vapors and is usually produced under low pressure from a casing head on the well. "harcoal Test A test standardi<ed by the )as 4rocessors Association and the American )as Association for determining the natural gasoline content of a given natural gas. The gasoline is adsorbed from the gas on activated charcoal and then recovered by dis* tillation. The test is prescribed in Testing Aode /./*60, Coint publication of A)A and )4A. "hromatogra#h$ A technique for separating a mixture into individual components by repeated adsorption and desorption on a confined solid bed. #t is used for analysis of natural gas and D)%. "laus Process A process to convert hydrogen sulfide into elemental sulfur by selective oxidation. "om#ressi-ilit$ 2actor A factor, usually expressed as EF,E which gives the ratio of the actual volume of gas at a given temperature and pressure to the volume of gas when calculated by the ideal gas law. "om#ression )atio The ratio of the absolute discharge pressure from a compressor to the absolute inta3e pressure. Also applies to one cylinder of a reciprocating compressor and one or more stages of a rotating compressor. "ondensate The liquid formed by the condensation of a vapor or gasG specifically, the hydrocarbon liquid separated from natural gas because of changes in temperature and pressure when the gas from the reservoir was delivered to the surface separators. #n a steam system it may be water that is condensed and returned to the boilers.
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"on*ergence Pressure The pressure at a given temperature for a hydrocarbon system of fixed composition at which the vapor*liquid equilibrium '*values of the various components in the system become, or tend to become, unity. The convergence pressure is used to adCust vapor* liquid equilibrium '*values to the particular system under consideration. "o##er Stri# Test A test using a small strip of pure copper to determine qualitatively the hydrogen sulfide corrosivity of a product. =efer to )4A %4*gas copper strip test !Aopper Strip >ethod", AST> D*/H0H test procedure. "ritical Densit$ The density of a substance at its critical temperature and critical pressure. "ritical Pressure The vapor pressure of a substance at its critical temperature. "ritical Tem#erature 9or a pure component, the maximum temperature at which the component can exist as a liquid. "r$ogenic Plant A gas processing plant which is capable of producing natural gas liquid products, including ethane, at very low operating temperatures, usually below minus 2.8A. "u-ic 4eter A unit of volume measurement commonly used in international commerce for petroleum, petroleum products and natural gas. :ne cubic meter measured at /2.2-8A $ 1-6./,1 7.S. gallons $ -.1; barrels $ 02.0/2 cubic feet measured at /2.2-8A. Deaerator An item of equipment used for removing air or other non*condensible gases from a process stream or from steam condensate or boiler feed water. De-utani@er A fractionator designed to separate butane !and more volatile components if present" from a hydrocarbon mixture.
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Deh$dration The act or process of removing water from gases or liquids. Demethani@ed Product A product from which essentially all methane and lighter materials have been removed. Demethani@er A fractionator designed to separate methane !and more volatile components if present" from a hydrocarbon mixture. De#ro#ani@er Afractionator designed to separate propane !and more volatile components if present" from a hydrocarbon mixture. Desiccant A substance used in a dehydrator to remove water and moisture. Also a material used to remove moisture from the air. Desulfuri@ationf A process by which sulfur and sulfur compounds are removed from gases or liquid hydrocarbon mixtures. De; Point The temperature at any given pressure, or the pressure at any given temperature, at which liquid initially condenses from a gas or vapor. #t is specifically applied to the temperature at which water vapor starts to condense from a gas mixture !water dew point", or at which hydrocarbons start to condense !hydrocarbon dew point". Distillation The process of separating materials by successively heating to vapori<e a portion and then cooling to liquefy a part of the vapor. >aterials to be separated must differ in boiling point and&or relative volatility. Doctor Test A qualitative method for detecting hydrogen sulfide and mercaptans in D)%. The test distinguishes between EsourE and EsweetE products.
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Dr$ 5as !/" )as whose water content has been reduced by a dehydration process. !1" )as containing little or no hydrocarbons commercially recoverable as liquid product. )as in this second definition preferably should be called lean gas. 1nd Point The maximum temperature observed on the thermometer during an AST> distillation test. 1P<4i. 8ethane<#ro#ane mi.: A product consisting of a mixture of essentially ethane and propane. 1.#ansion Tur-ine A device which converts part of the energy content of a gas or liquid stream into mechanical wor3 by expanding the gas or liquid through a turbine from which wor3 is extracted. 1.traction The process of transferring one or more components from one liquid phase to another by virtue of different solubility in the two liquids. #t is also used to indicate removal of one or more constituents from a stream. 2ield Se#arator A vessel in the oil or gas field for separating gas, hydrocarbon liquid, and water from each other. 2lash Point The lowest temperature at which vapors from a hydrocarbon liquid will ignite. See AST> D*2-. 2ractionation See definition of Edistillation.E )enerally used to describe separation of a mixture of hydrocarbons into individual products based on difference in boiling point and&or relative volatility. 2ree@e +al*e A specially constructed and calibrated valve designed and used solely for determining the water content in propane product. See AST> D*1,/0.
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5as "onstant 8): The constant multiplier in the #deal )as %aw. Dumerically, =$4(&T, if ( is the volume of one mole of an ideal gas at temperature T and pressure 4. 5as ($drate =efer to definition of EhydrateE. 5as InDection The inCection of natural gas into a reservoir to maintain or increase the reservoir pressure or reduce the rate of decline of the reservoir pressure. 5as Lift A method for bringing crude oil or water to the surface by inCecting gas into the producing well bore. 5as<Oil )atio 85O): The ratio of gas to liquid hydrocarbon produced from a well. This may be expressed as standard cubic meters of gas per cubic meter of stoc3 tan3 liquid. 5as Processing The separation of constituents from natural gas for the purpose of ma3ing salable products and also for treating the residue gas to meet required specifications. 5as Processing Plant A plant which processes natural gas for recovery of natural gas liquids and sometimes other substances such as sulfur. 5as<3ell 5as The gas produced or separated at surface conditions from the full well stream produced from a gas reservoir. 5as<3ell Li,uid The liquid separated at surface conditions from the full well stream produced from a gas reservoir. 5athering S$stem The networ3 of pipelines which carry gas from the wells to the processing plant or other separation equipment.
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(eat 4edia 8(eating 4edia: A material, whether flowing or static, used to transport heat from a primary source such as combustion of fuel to another material. Beating oil, steam, and an eutectic salt mixture are examples of heat media. (eating +alue 8(eat Of "om-ustion: The amount of heat obtained by the complete combustion of a unit quantity of material. The gross, or higher, heating value is the amount of heat obtained when the water produced in the combustion is condensed. The net, or lower, heating value is the amount of heat obtained when the water produced in the combustion is not condensed. (ea*$ 1nd The portion of a hydrocarbon mixture having the highest boiling point. 7sually hexanes or heptanes and all heavier hydrocarbons are the heavy ends in a natural gas stream. (e.anes Plus 8Or (e#tanes Plus: The portion of a hydrocarbon fluid mixture or the last component of a hydrocarbon analysis which contains the hexanes !or heptanes" and all hydrocarbons heavier than the hexanes !or heptanes". ($drate A solid material resulting from the combination of a hydrocarbon with water under pressure. Immisci-le %iquids that will not mix nor blend to give homogeneity are said to be immiscible. Inerts 5lements or compounds not acted upon chemically by the surrounding environment. Ditrogen and helium are examples of inert constituents of natural gases. Iso-utene #n commercial transactions, a product meeting the )4A specification for commercial putane and, in addition, containing a minimum of ;2 liquid volume percent isobutane. Ahemically, a hydrocarbon of the paraffin series with the formula A6Bl: and having its carbon atoms branched. Eac9et 3ater @ater which fills, or is circulated through, a casing which partially or wholly surrounds a vessel or machine element in order to remove, add, or distribute heat in order to control the temperature within the vessel or element.
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Eoule<Thomson 1ffect The change in gas temperature which occurs when the gas is expanded at constant enthalpy from a higher pressure to a lower pressure. The effect for most gases at normal pressure, except hydrogen and helium, is a cooling of the gas. Lead Acetate Test A method for detecting the presence of hydrogen sulfide by discoloration of paper which has been moistened with lead acetate solution. See AST> D*161.. Lean 5as !/" The residue gas remaining after recovery of natural gas liquids in a gas processing plant. !1" 7nprocessed gas containing little or no recoverable natural gas liquids. Lean Oil Absorption oil as purchased or recovered by the plant, or oil from which the absorbed constituents have been removed. Lift 5as )as used in a gas lift operation. Light 1nds The low*boiling, easily evaporated components of a hydrocarbon liquid mixture. Light ($drocar-on The low molecular weight hydrocarbons such as methane, ethane, propane and butanes. LN5 8li,uefied natural gas: The light hydrocarbon portion of natural gas, predominately methane, which has been liquefied. Loading )ac9 A structural and piping installation alongside a railroad trac3 or roadway used for the purpose of filling railroad tan3 cars or transport truc3s. LP5 8li,uefied #etroleum gas: =efer to definition of E%4*gasE.
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LP<gas 8Li,uefied #etroleum gas: 4redominately propane or butane, either separately or in mixtures, which is maintained in a liquid state under pressure within the confining vessel. L)5 8li,uefied refiner$ gas: %iquid propane or butane produced by a crude oil refinery. #t may differ from %4*gas in that propylene and butylene may be present. LTF 8lo; tem#erature e.traction unit: A unit which uses the cooling of a constant enthalpy expansion to increase liquid recovery from streams produced from high pressure gas condensate reservoirs. Also called %TS !low temperature separation" unit. 4erca#tan> Any of a homologous series of compounds of the general formula =SB. All mercaptans possess a foul odor. 4isci-le 2lood A method of secondary recovery of fluids from a reservoir by inCection of fluids that are miscible with the reservoir fluids. Natural 5as )aseous form of petroleum. Aonsisting predominately of mixtures of hydrocarbon gases. The most common component is methane. Natural 5asoline A mixture of hydrocarbons, mostly pentanes and heavier, extracted from natural gas, which meets vapor pressure, end point, and other specifications for natural gasoline as adopted by the )4A. See )4A Standard 0/01. Natural 5as Processing Plant Term used for gas processing plant, natural gasoline plant, gasoline plant, etc. N5L 8natural gas li,uids: Datural gas liquids are those hydrocarbons liquefied at the surface in field facilities or in gas processing plants. Datural gas liquids include ethane, propane, ,butanes, and natural gasoline.
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Odorant An odoriferous compound added to natural or %4*gas to impart a distinctive odor for detection of fugitive vapors. 5thyl mercaptan is the most widely used odorant for %4* gas, while tertiary butyl mercaptan, usually mixed with small amounts of other compounds, is the predominant odorant for natural gas. Oil<3ell 5as )as that is produced from an oil well. On<Stream 2actor The percentage of time a unit is on*stream. O#erating 2actor The percentage of time a unit is performing the function for which it was designed. Outage The vapor volume in a liquid vessel left for liquid expansion. Sometimes referred to as ullage. Pac9aged 0nit A shop*assembled group of equipment and accessories which needs only foundations, inlet and outlet piping, and utility connections to ma3e an operating unit. Pac9ed "olumn A fractionation or absorption column filled with pac3ing designed to give the required contact between the rising vapors and the descending liquid. Pea9 Sha*ing The use of non*conventional fuels to supplement the normal supply of pipeline gas during periods of extremely high demand. Pentane<Plus A hydrocarbon mixture consisting of isopentane !A2B/1" and heavier components with higher boiling points. Pigging A procedure for forcing a device through a pipeline for cleaning purposes, separating products, or inspecting the line.
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Pi#eline 5as )as which meets a transmission company+s minimum specifications. Pro#ane A normally gaseous paraffinic compound !A0BH". The term includes all products covered by )4A specifications for commercial and BD*2 propane. See )4A Standard 1/6.. "ommercial Pro#ane> A liquefied hydrocarbon product consisting predominately of propane and&or propylene and which conforms to the )4A specification for commercial propane as defined in )4ASt andard 1/6.. Pro#ane (D<? A special grade of propane consisting predominately of propane and which conforms to the )4A specification for BD*2 propane as defined in )4A Standard 1/6.. )a; 5as 7nprocessed gas, or the inlet gas to a gas processing plant. )a; 4i. Li,uid A mixture of natural gas liquids prior to fractionation. Also called Eraw ma3eE. )eco*er$ That percent or fraction of a given component in the plant feed which is recovered as plant product. )ec$cle =eturn of part of a process stream to a point upstream from where it was removed to enhance recovery or control. )eflu. #n fractionation, the portion of condensed overhead returned to the column to enhance achievable purity of the overhead product. )eflu. )atio A way of giving a relative measurement to the volume of reflux. 7sually referred either to the feed or overhead product.
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)elati*e Densit$ The ratio of the mass of a given volume of a substance to that of another equal volume of another substance used as standard. 7nless otherwise stated, air is used as the standard for gases and water for liquids, with the volumes measured at 15.56C and atmospheric pressure !/./.012 34a". )elief S$stem The system for safely relieving excess pressure to avoid exceeding equipment design pressure. )esidue The material which remains after a separation process. !/" =esidue gas is that gas remaining after the recovery of liquid products. !1" =esidue may also be the heaviest liquid or solid remaining after distillation or reclaiming process. )etrograde "ondensation 8*a#ori@ation: Aondensation or vapori<ation that is the reverse of expected behavior. Aondensation caused by a decrease in pressure or an increase in temperature. (apori<ation caused by an increase in pressure or a decrease in temperature. )ich 5as )as feed to a gas processing plant for liquid recovery. )ich Oil The oil leaving the bottom of an absorber. #t is the lean oil plus the absorbed constituents. )+P 8)eid +a#or Pressure: The vapor pressure of a material measured by the =eid >ethod and apparatus as detailed in AST> Test 4rocedure D*010. S = 3 8See -s=;: Saturated compounds hydrocarbon compounds having no unsaturated carbon valence bonds. Datural gas and natural gas liquids are saturated compounds. Saturated Li,uid %iquid which is at its boiling point or is in equilibrium with a vapor phase in its containing vessel.
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Saturated +a#or (apor at its dew point. shrin9age The reduction in volume of a gas stream by removal of some of its constituents such as for recovered products, fuel, or losses. SN5 8S$nthetic or Su-stitute Natural 5as: The gas product resulting from the gasification of coal and&or gas liquids or heavier hydrocarbons. Solution 5as )as which originates from the liquid phase in an oil reservoir. Sour %iquids and gases are said to be EsourE if they contain hydrogen sulfide, carbon dioxide, and&or mercaptans above a specified level. #t is also used to refer to the feed stream to a sweetening unit. Sour 5as )as containing undesirable quantities of hydrogen sulfide, mercaptans, and&or carbon dioxide. #t is also used to refer to the feed stream to a sweetening unit. S#litter A name applied to fractionators, particularly those separating isomers !e.g., butane splitter refers to a tower producing most of the isobutane in the feed as overhead and most of the normal butane in the feed as bottoms". S#onge A-sor-ent An absorbent for recovering vapors of a lighter absorbent that is used in the main absorption process of a gas processing plant. Sta-ili@ed "ondensate Aondensate that has been stabili<ed to a definite vapor pressure in a fractionation system. Sta-ili@er A fractionation column designed to reduce the vapor pressure of a liquid stream.
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Stage Se#aration S$stem A system of separators where the liquid portion of the well effluent is separated from formation gas and flash vapors Still The column where the absorbed product is recovered from the lean absorption oil. #n plants using a low molecular weight absorption oil, the still is designed as a fractionation column. #n plants using a high molecular weight absorption oil, the still may use steam or other fluids as stripping medium. Also used to refer to regenerators in amine treating and glycol dehydration systems. Stra##ing A term applied to the process of calibrating liquid storage capacity of storage tan3s in increments of depth. Stream Da$ A continuous 16 hour period of plant operation. Stri##er A column wherein absorbed constituents are stripped from the absorption oil. The term is applicable to columns using a stripping medium, such as steam or gas. Stri##ing 2actor An expression used to describe the degree of stripping. >athematically, it is '(f%, the reciprocal of the absorption factor. Stri##ing 4edium As stated under EstripperE, the medium may be steam, gas, or other material that will increase the driving force for stripping. Sulfur A yellow, non*metallic chemical element. #n its elemental state, it exists in both crystalline and amorphous forms. #n many gas streams, sulfur may be found as volatile sulfur compounds, such as hydrogen sulfide, sulfur oxides, mercaptans, and carbonyl sulfide. =eduction of the concentration of these gaseous sulfur compounds is often necessary for corrosion control and possibly for health and safety reasons. Sulfur Dio.ide 8SO&: A heavy, colorless, suffocating gas that is chemically an oxide of sulfur. Aonversion of the gaseous sulfur oxides to sulfur is necessary for corrosion control, for health and safety reasons, and for complying with governmental standards.
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S;eet )as containing essentially no obCectionable sulfur compounds. Also, treated gas leaving a sweetening unit. S;eet 5as )as which has no more than the maximum sulfur and&or A:& content defined by !/" the specifications for the sales gas from a plantG !1" the definition by a legal body. Also, the treated gas leaving a sweetening unit. Tem#erature "orrection 2actor A factor for correcting volume at a given temperature to that at a specific reference temperature. =eference temperature most commonly used in the petroleum industry is /2.2-8A. Therm A unit of gross heating value equivalent to !/..22" I /., 3J. Tonne A unit of mass measurement, commonly used in international petroleum commerceG an expression for the metric ton, or /... 3ilograms. Tra$ed "olumn A vessel wherein gas and liquid, or two partially miscible liquids, are contacted, usually concurrently on trays. Also refer to pac3ed column. Tur-oe.#ander =efer to definition of Eexpansion turbine.E ullage 8See outage: 0nsaturated "om#ounds Bydrocarbon compounds having one or more unsaturated valence bonds, i.e., ethylene, propylene. These compounds are not found in natural gas streams or gas liquids because of their relatively high chemical reactivity. 7nsaturates are produced by a thermal crac3ing or chemical reaction and can be found in synthetic gas !SD)" or light refinery gases !%=)". +a#or Pressure 8true *a#or #ressure: The pressure exerted by the equilibrium vapor of a liquid when confined in a closed previously evacuated tan3 or test apparatus.
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+a#or Pressure 5asoline A descriptive phrase for natural gasoline meeting a specified vapor pressure. +a#or Pressure> 5PA (apor pressure as specified by )4A procedures. +a#or )eco*er$ 5quipment or process for the recovery of desired components from stoc3 tan3 vapors or vapors from some other source. +olatile Sulfur An obsolete term referring to sulfur compounds that will vapori<e readily !See sulfur". 3eathering The evaporation of liquid caused by exposing it to the conditions of atmospheric temperature and pressure. 4artial evaporation of liquid by use of heat may also be called weathering. 3eathering Test A )4A test for %4*gas for the determination of heavy components in a sample by evaporation under specified conditions. 3eight In Air @eight compared to a standard with no correction for air buoyancy. 3ellhead The assembly of fittings, valves, and controls located at the surface and connected to the flow lines, tubing, and casing of the well so as to control the flow from the reservoir. 3et 5as !/" A gas containing water, or a gas which has not been dehydrated. !1" A term synonymous with rich gas. =efer to definition of Erich gasE. 3o--e Num-er A number proportional to the heat input to a burner at constant pressure. #n ?ritish practice, it is the gross heating value of a gas divided by the square root of its gravity. @idely used in 5urope, together with a measured or calculated flame speed, to determine interchangeability of fuel gases.
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P(AS1 B1(A+IO)
P(AS1 B1(A+IO) Introduction: #n planning, design and operation of modem petrochemical processes, engineers, technologists and process operators must 3now with* reasonable accuracy the properties of the fluids with which they deal. #f a piece of process equipment is to be designed, the properties of the fluid which will be contained in that vessel must be determined in order to determine the required volume of the vessel, the operating+ pressure and thus the wall thic3ness and even the specifications for the control devices. 1/1 +a#or<Li,uid 1,uili-rium : Terms/Definitions: Pro#ert$ * any measurable characteristic of a substance, such as pressure, volume, or temperature, or a characteristic that can be calculated or deduced, such as internal energy. State * when a system possesses a unique set of properties, such as temperature, pressure, density, and so on, at a given time. Thus the system is said to be in a particular state. A change in the state of a system results in a change *in at least one of its properties. 1,uili-rium * a state in which there is no tendency toward change, Phase * a completely homogeneous and uniform state of matter. Ideal 5as * is an imaginary gas which obeys exactly certain simple laws such as the laws of ?oyle, Aharles, Dalton. Do real gas obeys these laws exactly over all ranges of temperature, although ElighterE gases !hydrogen, oxygen, air, etc." under ordinary circumstances obey the ideal gas laws with but negligible deviations. Ideal 5as La; * from the wor3 of ?oyle and Aharles, scientists developed the relationship now called the #deal )as %aw. The equation used is p( $ n =T. This equation can relate the volume, pressure, temperature, and the amount of a given gas. 1,uations of State * relate the p* ( * T properties of a pure substance !or mixture" by theoretical or empirical relations. The #deal )as %aw is a simple example of an equation of state. +a#or * a gas below its critical point which can condense !i.e change its phase".
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5as * a substance which is above its critical point and is noncondensable. +a#or Pressure * the pressure at which vapori<ation and condensation are at constant temperature and pressure under equilibrium conditions for a pure substance or mixture. GNormalG Boiling Point * the temperature at which boiling will ta3e place under a pressure of / atmosphere K/./.0 34a, ,-. mm BgL. De; Point * the temperature at which a vapor starts to form a liquid during the process of condensation. Bu--le Point * the temperature at which a liquid starts to form vapor during the process of vapori<ation. Saturated * when a vapor or liquid is Cust about to condense a drop of liquid or vapori<e a +puff of vapor respectively. Su#erheated < when a substance is above its saturated vapor region. The degrees of superheat refer to the difference in temperature between the solution temperature and the actual temperature of a substance above the saturation region. Su-cooled < when a substance is below its saturated liquid region. Tri#le Point * when a substance is at a set of conditions in which the solid, liquid, and vapor phases are all in equilibrium.
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4ulti#hase S$stems @ater can exist in many phases, solid, liquid and vapor. These states can change from one to another at the proper conditions with +the addition or removal of the correct amount of energy. 9or instanceM li,uid to solid : free<ing solid to li,uid : melting li,uid to *a#or : boiling *a#or to li,uid : condensation su-limation : solid to vapor At /./.012 34a pressure, / atmosphere, the boiling point of water is /.. A. This is usually referred to as the normal boiling point of a substance and the energy required to boil that water is referred to as the heat of *a#ori@ation. The boiling point of water changes with a change in pressure. 9or exampleG as pressure is lowered, the boiling point of water decreases, There are several points of specific interest on a 4*T diagram. The first of these is the critical point, Tc and 4c, critical temperature and critical pressure respectively. Above this point, the material no longer exhibits the properties of liquid or a gas, rather the properties change slowly from those of a gas to those of a liquid. There is no line which defines the difference between liquid and vapor. #f a substance above Tc and 4c is cooled, there will be no condensation of vapor to liquid, rather there is a slow change in physical properties. Aritical pressures and temperatures can be found in the 4hysical 4roperties section . The second point to mention is the triple point. This is defined as the one temperature and pressure where solid, liquid and vapor can coexist in equilibrium, This is of limited importance to the processing industries. The line running from the triple point to the critical point, the line representing the equilibrium between liquid and vapor, is the line of most interest to us, As water is heated at /./.012 34a, the temperature rises to /.. A, then remains constant at /.. A until enough energy is added to vapori<e the liquid, !heat of vapori<ation, hv" then the temperature will begin to increase once more. #t is important to reali<e that is true only for pure components and not mixtures. As the temperature increases in the above example, the liquid begins to exert a pressure on the vapor above it. This is referred to as the vapor pressure of that component. (apor pressure is very important for expressing the volatility of a substance at fixed conditions. 9or instance, the volatility of petrol is defined by the vapor pressure. (apor pressure is also very useful in performing calculations involving vapors and liquids. #t is usually given the symbol pN and can be found in tables or charts.
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4ulticom#onent S$stems: >ost systems in processing facilities are mixtures of components, not pure components. 9or our purposes, we will limit our discussion to two components to simplify matters although the same principles apply for systems containing multiple components. 9or mixtures, there are now three variables to plot, pressure, temperature and composition. 9or simplicity, only two of these variables are plotted at once and the third is 3ept constantM 2or e.am#le: 4ressure versus temperature O constant composition Temperature versus composition * constant pressure 4ressure versus composition * constant temperature
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"ritical Point for a Pure Su-stance 8 3ater :
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0NIT 7
DISTILLATION "OL04N "O4PON1NTS
O*er*ie; This topic is aimed at all process operations staff wanting to expand their 3nowledge about the various internals and externals to a distillation column. O-Decti*es On com#letion of this to#ic> the trainee ;ill : * * * 3now the components of a distillation column and understand their function understand the physical limitations of trays and pac3ings !flooding and Cet flooding" 3now the common process variables and understand their meaning
"ontents * notes and diagrams on distillation column components
"om#onents of Distillation "olumns: The modem distillation column is comprised, of a tall column with trays mounted internally, an overhead system and a reboiler system. #n some cases, pac3ing may be used rather than individual trays.
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2igure & : Distillation "olumn ;ith Tra$s and Pac9ing
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Sic Distillation 1,ui#ment And O#eration 4ain "om#onents of Distillation "olumns Distillation columns are made up of several components, each of which is used either to transfer heat energy or enhance material transfer. A typical distillation contains several maCor componentsM a vertical shell where the separation of liquid components is carried out column internals such as trays&plates and&or pac3ings which are used to enhance component separations a reboiler to provide the necessary vaporisation for the distillation process a condenser to cool and condense the vapour leaving the top of the column a reflux drum to hold the condensed vapour from the top of the column so that liquid !reflux" can be recycled bac3 to the column
The vertical shell houses the column internals and together with the condenser and reboiler, constitute a distillation column. A schematic of a typical distillation unit with a single feed and two product streams is shown belowM
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Basic O#eration and Terminolog$ The liquid mixture that is to be processed is 3nown as the feed and this is introduced usually somewhere near the middle of the column to a tray 3nown as the feed tray. The feed tray divides the column into a top !enriching or rectification" section and a bottom !stripping" section. The feed flows down the column where it is collected at the bottom in the reboiler. Beat is supplied to the reboiler to generate vapour. The source of heat input can be any suitable fluid, although in most chemical plants this is normally steam. #n refineries, the heating source may be the output streams of other columns. The vapour raised in the reboiler is re*introduced into the unit at the bottom of the column. The liquid removed from the reboiler is 3nown as the bottoms product or simply, bottoms.
The vapour moves up the column, and as it exits the top of the unit, it is cooled by a condenser. The condensed liquid is stored in a holding vessel 3nown as the reflux drum. Some of this liquid is recycled bac3 to the top of the column and this is called the reflux. The condensed liquid that is removed from the system is 3nown as the distillate or top product. Thus, there are internal flows of vapor and liquid within the column as well as external flows of feeds and product streams, into and out of the column.
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"olumn Internals
Tra$s and Plates The terms EtraysE and EplatesE are used interchangeably. There are many types of tray designs, but the most common ones are M 1/ Bu--le ca# tra$s
A bubble cap tray has riser or chimney fitted over each hole, and a cap that covers the riser. The cap is mounted so that there is a space between riser and cap to allow the passage of vapour. (apour rises through the chimney and is directed downward by the cap, finally discharging through slots in the cap, and finally bubbling through the liquid on the tray.
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&/
+al*e tra$s
#n valve trays, perforations are covered by liftable caps. (apour flows lifts the caps, thus creating a flow area for the passage of vapour. The lifting cap directs the vapour to flow hori<ontally into the liquid, thus providing better mixing than is possible in sieve trays.
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Sie*e tra$s
Sieve trays are simply metal plates with holes in them. (apour passes straight upward through the liquid on the plate. The arrangement, number and si<e of the holes are design parameters.
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?ecause of their efficiency, wide operating range, ease of maintenance and cost factors, sieve and valve trays have replaced the once highly thought of bubble cap trays in many applications. Li,uid and +a#our 2lo; in a Tra$ "olumn The next few figures show the direction of vapour and liquid flow across a tray, and across a column.
5ach tray has 1 conduits, one on each side, called downcomers . %iquid falls through the downcomers by gravity from one tray to the one below it. The flow across each plate is shown in the above diagram on the right. A weir on the tray ensures that there is always some liquid !holdup" on the tray and is designed such that the the holdup is at a suitable height, e.g. such that the bubble caps are covered by liquid. ?eing lighter, vapour flows up the column and is forced to pass through the liquid, via the openings on each tray. The area allowed for the passage of vapour on each tray is called the active tray area.
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As the hotter vapour passes through the liquid on the tray above, it transfers heat to the liquid. #n doing so, some of the vapour condenses adding to the liquid on the tray. The condensate, however, is richer in the less volatile components than is in the vapour. Additionally, because of the heat input from the vapour, the liquid on the tray boils, generating more vapour. This vapour, which moves up to the next tray in the column, is richer in the more volatile components. This continuous contacting between vapour and liquid occurs on each tray in the column and brings about the separation between low boiling point components and those with higher boiling points. Tra$ Designs A tray essentially acts as a mini*column, each accomplishing a fraction of the separation tas3. 9rom this we can deduce that the more trays there are, the better the degree of separation and that overall separation efficiency will depend significantly on the design of the tray. Trays are designed to maximise vapour*liquid contact by considering the liquid distribution and vapour distribution
on the tray. This is because better vapour*liquid contact means better separation at each tray, translating to better column performance. %ess trays will be required to achieve the same degree of separation. Attendant benefits include less energy usage and lower construction costs. There is a clear trend to improve separations by supplementing the use of trays by additions of pac3ings. Pac9ings 4ac3ings are passive devices that are designed to increase the interfacial area for vapour*liquid contact. The following pictures show 0 different types of pac3ings.
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These strangely shaped pieces are supposed to impart good vapour*liquid contact when a particular type is placed together in numbers, without causing excessive pressure*drop across a pac3ed section. This is important because a high pressure drop would mean that more energy is required to drive the vapour up the distillation column. Pac9ings *ersus Tra$s A tray column that is facing throughput problems may be de*bottlenec3ed by replacing a section of trays with pac3ings. This is becauseM pac3ings provide extra inter*facial area for liquid*vapour contact efficiency of separation is increased for the same column height pac3ed columns are shorter than trayed columns
4ac3ed columns are called continuous*contact columns while trayed columns are called staged*contact columns because of the manner in which vapour and liquid are contacted.
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"olumn )e-oilers
There are a number of designs of reboilers. #t is beyond the scope of this set of introductory notes to delve into their design principles. Bowever, they can be regarded as heat*exchangers that are required to transfer enough energy to bring the liquid at the bottom of the column to boiling point. The following are examples of typical reboiler types.
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0NIT '
P)IN"IPL1S O2 5AS P)O"1SSIN5 OP1)ATION
O*er*ie; Datural gas liquids !or ED)% s", are hydrocarbons in a liquid state. There are many reasons for removing D)%+s from the gas stream, includingM /. 1. 0. 6. The hydrocarbon components may be more valuable in their liquid state, either mixed or separated into their different individual elements. 4ipeline gas quality specifications may restrict the amount of D)% is allowed. Beavier D)% s can separate from the gas stream in pipelines as temperatures drop, thus restricting flow in the pipeline. The D)% s may be used for re*inCection on enhanced oil recovery proCects. That is, they will be inCected into a formation to help EsweepE crude oil through the reservoir by mixing with the oil and pushing the crude toward the well bore.
There are several different processes that can be used to separate D)% s from the natural gas stream. The three most common areM Aryogenics, refrigeration and lean oil absorption.
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"r$ogenics
#n the cryogenic process, a natural gas stream is cooled to extremely low temperatures to liquefy the ethane and heavier hydrocarbons. @hen a gas stream is chilled to below *2.P 9 !*62 P A ", heavier gas components are easily liquefied. The ethane and heavier hydrocarbons are then separated from the methane.
EXPANDER COMPRESSO R COMPRESS OR METHANE SEPARAT OR DEMETHANIZER
NATURAL GAS HEAT EXCHANGER N. GAS LIQUID
")6O51NI"S
Aryogenic processing of a natural gas stream involves three basic stepsM dehydration, chilling and fractionation. ?ecause of the very cold temperatures in cryogenic processing, the gas stream must be almost totally dehydrated to prevent the formation of Bydrates. Dehydration is usually accomplished with either a liquid or solid desiccant. The method depends on the water content of the inlet gas at your facility. Some cryogenic processes will use only dry*desiccant dehydration. ?ut if the water content of the inlet gas is*high, first there would be liquid desiccant dehydration, followed by dry*desiccant dehydration.
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NAT0)AL 5AS ST)1A4
D1(6D)ATION D=Q )AS "(ILLIN5 < 1?!H 2 8 < 1!1H " : )AS ADD %#R7#D
3AT1)
FRACTIONATION
5AS 8 41T(AN1:
NATURAL GAS LIQUID
")6O51NI" P)O"1SSIN5
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Ahilling of the gas is the cornerstone of the cryogenic process. The gas stream can be chilled by heat exchange with cold gas, and by pressure reduction or pressure reduction with energy removal. The pressure reduction method ! EJ.T S or Joule* Thompson", provides cold temperatures in the range of *2.P 9 !*62P A" to */..8 9 !*,0 P A". To obtain the lowest temperatures, */.. P 9 !*,0 P A" to *1..8 9 !*/1; P A", pressure reduction with energy removal is accomplished using an expander *compressor. Aryogenics has relatively moderate energy requirements, and is considered the most efficient method for removing D)%S from the gas stream.
41T(OD
T14P1)AT0)1 )AN51 . P to O 1. P 9 ! * /H P to O 1; P A "
T6PI"AL P1)"1NT )1"O+1)6 5thane 4ropane ?utanes Beavier 5thane 4ropane ?utanes Beavier 5thane 4ropane ?utanes Beavier 12 22 ;0 ;, ,. H. ;, ;; H. ;;; /..
)efrigeration
Pressure )eduction 8 E/T Process :
* 2. P to O ,. P 9 ! * 6- P to O 2, P A "
1.#ander Process
* /12 P to O /2. P 9 ! * H, P to O /./ P A "
B#)B 4=5SS7=5 )AS A:>>:D SB55T %:@ 4=5SS7=5 )AS A:>4=5SS:=
B#)B 4=5SS7=5 )AS %:@ 4=5SS7=5 )AS
5I4ADD5=
1FPAND1) P)O"1SS
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)efrigeration
=efrigeration is a separation process that has been in use for many years. The principle is to chill the natural gas stream by passing the gas through a chiller. Temperatures in this process range from .89 !*/H8 A" to *1.8 9 !*1;8 A". Ahilling causes the heavier hydrocarbons to liquefy, and then these D)%S can be separated from the gas.
A:>4=5SS:=
A:DD5DS5=
REFIRGERANT VAPOR
@A=> DAT7=A% )AS S7=)5 TAD' AB#%%5=

A:%D )AS ADD %#R7#DS =59#=)5=ADT %#R7#D
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)efrigerant The energy requirements of refrigeration are primarily for compressing the refrigerant and driving the condenser. @hile the volume of heavier hydrocarbons recovered is less than with lean oil absorption , the amount of equipment and energy used for recovery with refrigeration is much less, ma3ing it a more economical method than lean oil absorption. 7/ Lean Oil A-sor#tion
#n lean oil absorption, lean oil is flows through a natural gas stream, absorbing the heavier hydrocarbons as it contacts them. The hydrocarbons are then recovered by distilling them out of the now ErichE oil. :nce the D)% s are distilled, the lean oil is recycled bac3 through the system.
)AS
%5AD :#%
%5AD :#%
AB#%%5=
DAT7=A% )AS %#R7#DS

>5TBADe
DAT7=A% gAS
S54A=AT: = 47>4 =#AB :#%
A?S:=?5= L1AN OIL ABSO)PTION
ST#%%
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Bigh percentages !;.*;2T" of propane and heavier hydrocarbons !;H*/..T" can be recovered using lean oil absorption. %ean oil absorption is relatively expensive to operate because it requires a lot of energy& equipment compared to refrigeration or cryogenics. This process was the mainstay of the industry for years. Although still in use, it is gradually fading from the scene as cryogenics ta3es its place.
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2)A"TIONATION 2LO3
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2ractionation 8 Deethani@er = De#ro#ani@er = De-utani@er:
9ractionation is a. downstream treatment option for D)% s after they have been separated from the gas stream. ?y definition, fractionation consists of separating two components in a mixture of two or more components. 9or example, a depropani<er separates propane from a stream that contains propane and one or more heavier hydrocarbons. The propane is coo3ed out of the mixture and is the overhead product from the tower. The bottom stream is practically free of propane. 9ractionation is essentially a distillation process. As you can see on the pervious diagram, different D)% s are coo3ed out in various towers. There are usually two means of control ling the purity of the top and bottom streams of a given tower by varying the temperature at the top of the tower, or varying the temperature at the bottom of the tower. )enerally spea3ing, pressure and feed rate cannot be changed, since this would change conditions in the rest of the plant. @hether to fractionate is a question of economics. #s there a profitable mar3et for the fractionated productU ?ecause mar3et conditions change rapidly and often, this question must constantly be answered to determine if fractionation will be done. There are times when the mixed D)% s will be more valuable than their separate components.
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0NIT ?
P)OD0"T SP1"I2I"ATIONS
O*er*ie; This topic is aimed at all process operations staff wanting to expand their 3nowledge about the control of distillation columns and the impact to product separation. O-Decti*es :n completion of this topic, the trainee willM * understand how a distillation column is controlled !the six independent variables"
"ontents 2./ 2.1 Distillate and ?ottoms Specifications Aontrol of 4roduct Aomposition
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Distillation and Bottoms S#ecifications:
This topic is devoted to a discussion of measurement and control techniques common is distillation. 2or #ur#oses of discussion> it ;ill -e assumed that: /. 1. 0. 6. A column already exists. >any of the control variables will be fixed by the engineering design of the column. The column has a reboiler. The feed point to the column is fixed and ma3ing only two products O a
distillate and bottoms product. If the assum#tions are held for the a-o*e> there are eight 8B: *aria-les /. 1. 0. 6. Aolumn 4ressure 9eed 9low =ate 9eed Aomposition 9eed Temperature 2. -. ,. H. Beat Added !boil*up" ?ottom 4roduct 9low =ate Beat =emoved !reflux" Distillate 4roduct 9low =ate
only six !-" of these variables can be controlled independently. Aompositions for distillate and bottom products are called dependent variables since they are not controlled directly but rather through the other variables mentioned above. Pressure "ontrol >ost distillation columns are maintained at some 3ind of constant pressure. This helps in 3eeping the condensation loading to the condenser as even as possible !dew point". The specific pressure is determined from economic considerations* 9or example, if operating pressure increases, the column temperature increases thus increasing the condenser cooling requirements and decreasing the reboiler heating requirements. 2eed "ontrol The first variable fixed would be the column pressure !as discussed above". #f the feed conditions were fixed, this would necessitate that three !0" more independent variables would be determined * feed rate feed, composition, and feed temperature. The feed flow rate can be maintained at a constant rate by using flow control. The feed composition has a great influence upon the operation of a distillation unit. +7nfortunately, the feed composition is seldom subCect to adCustment. 9or this reason, it is necessary to ma3e changes elsewhere to the operation of the column in order to compensate for variations in feed composition.
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The thermal condition of the feed determines how much additional heat must be added to the column by the reboiler. 9or efficient separation, it usually is desirable to have the feed at its bubble point when it+s enters the column. #f the feed composition varies, its bubble point also varies. #t is a common practice to set the temperature control at a point which is equivalent to the bubble point of the heaviest feed. )e-oiler "ontrol: Since fixing the feed conditions and column pressure determines four of the variables listed earlier, only two other. variables remain to be controlled in order to fix the operation of the distillation column. 9requently, the -oil<u# rate is chosen as one of the two remaining independent variables. The boil*up rate is controlled by setting the flow of heat to the reboiler. #n 3ettle reboilers, the heating medium !e.g. steam" is added as required to try and achieve the bottom product specification )eflu. "ontrol: 9or total control of the distillation operation, reflux rate represents the sixth and last independent variable to be controlled. The reflux furnishes the continuous supply of liquid to the top and down through the column Cust as the boil*up from the reboiler provides a continuous supply of vapor up through the column. The rate of reflux is regulated by a flow controller on the reflux line The rate of distillate product withdrawal is controlled by the liquid level in the accumulator. "onclusion: ?y controlling the six independent variables and assuming constant feed conditions the separation efficiency of a distillation column can be controlled. The consistent and optimum specification for distillate and bottoms products can hence be achieved. ?/& "ontrol of Product Purit$ = 2ulfilling demands
A distillation unit operates between two extremes. #n one case, insufficient separation is reflected in unacceptable product purity. #n the other case, separation can be far in excess of what is demanded so that utilities and unit capacity are wasted. The goal of distillation then is to achieve a specified product purity without causing waste. To obtain this goal, some measure of product composition is needed. Since distillation separates materials according to their difference in vapor pressure and since vapor pressure is a temperature controlled function, temperature measurement can be used to indicate composition.
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The important consideration is to measure temperature on a tray which most reflects changes in composition. @hen composition of the bottom product is the important consideration, it is desirable to maintain a constant temperature in the lower section of the column. @hen composition of the distillate product is the important consideration, it is desirable to maintain a constant temperature in the upper section of the column. >easuring temperature in a column usually requires that the sensing device be in the liquid on the tray. Distillation temperature is an indication of composition only when column pressure remains constant. #n most cases, the controlling of pressures and temperatures can approximate the control of product ! the compositions should be close to specification with a given set point of pressure and temperature!s" in the column. %aboratory analysis can be done to confirm and&or adCust the pressure and temperature set points. Analytical or specific composition control is another way to sidestep the problems of temperature control. Several types of analytical instruments can be used for distillation column control. The most common ones used are infrared and gas .chromatographs !).c & s". #f the distillate and&or bottoms streams could be sampled continuously and fed through an analy<er, the stream compositions could be used for column control.
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0NIT DISTILLATION "OL04N "ONT)OL = INST)041NTATION Instrumentation <4easurement Points> Alarm Points/ Safet$ 1,ui#ment> )elief De*ices: 4easurement Points> Alarm Points: As discussed in topic V2, there are different variables that can be used to operate a given distillation column. The different locations, control loops, and alarm points. Notes: a" b" c" d" e" f" 9eed AontrolM =eboiler AontrolM ?ottoms AontrolM Tower 4ressure AontrolM =eflux AontrolM Distillate AontrolM
Safet$ 1,ui#ment> )elief De*ices: Distillation columns requires safety systems in order to function within the plant environment without creating ris3 to plant personal and other process equipment. These safety systems may range in complexity from simple alarms to interloc3 systems. 5xamples of areas that should have alarms areM )eflu. Drum : high and low level alarms, high pressure alarm
"olumn Bottom : high and low level alarms 2eed 2lo; )eflu. 2lo; )e-oil : high and low flow alarms : high and low flow alarms : high temperature alarm, high and low flow alarms !steam " low flow alarms !process".
A maDor concern in the o#eration of distillation s$stems is o*er#ressure of the e,ui#ment and #ossi-le catastro#hic failure > A #artial list of the causes of o*er#ressure is found -elo;:
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a:
0tilit$ failure * * * * loss of coolant loss of electric power loss of steam loss of instrument air
-:
"ontroller failure 8 human error in o#ening *al*e: * * * * failure of reboiler controller failure of pressure controller failure of feed controller failure of pump around controller
c:
1.traneous sources * * * * valve opening to external pressure source upstream upset !change in feed composition" exchanger failure !tube rupture" exterior fire
d:
Internal sources * * * noncondensables chemical reaction closed column outlets
e:
Transient sources * * poc3ets of water flashing to steam internal explosions
4ethods of relie*ing o*er#ressure ;hich should -e included in the column design are: * * * * properly si<ed relief valves on column adequate vapor vent from reflux drum properly specified control valves with correct failure mode manual bypass around control valves
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Standard "olumn "ontrol: Distillation column control schemes may be bro3en into two maCor types, material balance systems and heat balance systems. :f the two, the material balance system or some variation of it, is the most common. 4aterial Balance S$stem: #n a material balance control system , product composition is controlled by controlling the flow of material into and out of the column. The column pressure is controlled by the amount of cooling in the overhead condenser while the distillate and bottoms products are both controlled by level control. #t is a common practice to have both distillate and bottoms on level control, thus ma3ing accumulation in the column unli3ely. The temperature of the bottom is controlled by the steam flow on temperature control while the reflux is on flow control. This is referred to as indirect control as the tower top temperature is controlled by a flow controller. A variation of this is to use temperature control to manipulate the reflux. This is 3nown as direct control. 1nerg$ Balance S$stem: #n energy balance control system, the energy balance controls the product composition while the free variable is one of the product flows. The shortcoming of this scheme is that variations in the material balance interact with the control system. These controls are more sensitive to the changes in the material balance than the changes in the energy balance. 9or these reasons, energy balance controls are only used if a satisfactory material balance system cannot be implemented or in conCunction with an advanced computer control system.
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0NIT A
DISTILLATION "OL04N OP1)ATION

Startu# / Shutdo;n: :nce a column is bolted up after initial construction or a shutdown, a number of operations must occur to prepare the column for startup. These steps, referred to as column commissioning, are used to clear the system of undesirable materials, test the column and to ta3e preventative measures against performance deterioration. Line Blo;ing: Dormally done with a utility service such as air and&or water. This facilitates the removal and cleaning of any pipe scale, rust, and loose slag from weld Coints. >ost blowing is done to atmosphere and not into the distillation column itself. Pressuring and De#ressuring: This is done with the same utility mentioned above. The column, connecting equipment, piping, along with all instrumentation is chec3ed for lea3age. The column system must be lea3 proof and can be chec3ed by monitoring the column pressure Kno drop in transmitter signalL and also by EsnoopingE or chec3ing for lea3s in the field. Purging: This is done using an inert gas utility such as nitrogen. This is extremely+ important since air can+t be used Kespecially on vacuum systemsL on the column as it allows explosive mixtures to occur. The column should be 3ept under a nitrogen EpadE prior to startup so as not to cause any problems on startup. Blinding and 0n-lindingM >ost columns under construction and during vessel entry may have piping blind flanges or spades inserted so as not to have any utility and&or process materials enter the equipment Ksafety concernsL. The removal of blinds and spades are required prior to the purging step but may be left on during any line blowing activity if the location of the blinds and spades are connecting equipment to piping. The removal may be done after blowing so as not to contaminate the equipment with the blown out rust, scale, slag, etc.. Lea9 Testing: 4er above Epressuring and depressuring E step. A soapy water solution can be used as a EsnoopE test. >ost times this solution is placed in a bottle Kor can be purchased as EsnoopEL. All flanges and equipment & instrument connections are squirted with the soapy water solution. #f any lea3s occur, the solution will bubble vigorously.
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3ashing: Some columns and equipment may need to be washed with water or a solvent prior to operation as to eliminate any concerns with fouling, reactivity with dirt, rust, carbon, etc., as well as any EdeadspotsE that cause problems with the process material to be put through the column itself. A Ewater runE can be done to help calibrate instruments and chec3 for pump seal problems, lea3s, etc.. Steaming: Some columns can be purged with steam to exclude air. This can be done especially in warm climates ! no free<ing problems". Also, steam ma3es a good lea3 chec3 since it can EfindE lea3s better than any external testing. Dr$out: Dormally done with dry air or nitrogen utility. Aan also be a solvent drying as well depending on the application. :nce the column has been properly commissioned, the system is ready for startup. The sequence of steps used for startup is listed below although deviations are often required for specific distillation columns and the hardware availab/e 1: 2inal elimination of undesira-le materials/
The distillation column system should be clean, lea3 chec3ed, and ready to run. &: Bringing column to normal o#erating #ressure/
Depending on what the desired pressure is, this may be done by use of vacuum pumps&eCectors Kif vacuum columnL or by allowing the pressure control system to respond to column liquid boil up. 7: "olumn heating and cooling/
The condenser cooling medium should be on and functional. The reboiler&heating system should be ready to run once the liquid feed is introduced and a column bottom level established. ': Introduction of feed/
This is done once all the above are done. ?: Starting u# heating and cooling sources/
The cooling medium should already be running, The heating medium should be started slowly and carefully due to the thermal stress created in the equipment during the heatup.
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Bringing column to desired o#erating rates/
Depending on desired operating set points, the feed should be put on a minimum setting until the entire column is up to temperature, pressure, reflux ratio Kif the distillate&forwards can be recycledL, #f the forwards can not be recycled, then a total reflux can be done for a short time until the specifications are o3ay, then reflux ratio can be set along with a feed increase and required reboiler&heating load increase Kto 3eep the bottoms on specL, "olumn shutdo;n also follo;s a similar series of ste#s> t$#icall$: 1: )educing column rates/
Assuming all control systems are on line and at set point, the first step is to reduce column feed rates, This will gradually reduce heat and cooling loads as well as forwards and bottoms rates while still on spec.. The column may be put on total reflux so as to 3eep the reboiler running on a liquid inventory Ki.e. no . bottoms being pumped forward either. &: Shutting do;n heating and cooling sources/
The feed can be stopped per step !0" below first if the heating and cooling sources are ready to be shutdown. The heating source should be shutoff first as to help cool the column with any remaining reflux. 7: Sto##ing feed/
The feed can be stopped sooner than the heating source shutdown if the level rise in the column becomes too high Kalarm pointL. This will help minimi<e the pump*out of excess liquid inventory from the bottom of the column if required for any shutdown activity. ': Draining li,uids/
?oth the condenser Kreflux inventoryL and reboiler Kbottoms inventoryL can be pumped out or drained to storage inventory prior to any column decommissioning activities. ?: "ooling or heating column/
#f required for maintenance and&or vessel entry wor3, the column may need to be further cooled or heated using the process material and&or utility as required. : Bringing column to atmos#heric #ressure/
9or vacuum systems, nitrogen is used to repressure the column. 9or pressure systems, the condenser system is often vented to a recovery and&or flare system in order to get the column to atmospheric pressure.
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A:
1liminating undesira-le materials/
#n most cases, nitrogen is used to purge out any remaining vapors and liquids 4rior to vessel wor3. B: Pre#are the column for o#ening to atmos#here/
Bopefully the column has been purged correctly and all piping drained&blown to a vapor&liquid recovery system. Again, these steps may vary with each specific column or specific company procedure. :perations staff should be aware of any specific ha<ards or potential problems with the specific column prior to startup&shutdown. 4rior to startup&shutdown, there are several other items that should be consideredM /" 1" 0" 6" 2" -" ," H" ;" 4repare adequate procedures for operation, startup, shutdown and maintenance. 5nsure the startup&shutdown team consists of personnel who have all the required s3ills for the procedure. Adequate training for the startup team, supervisors and operators is required. 4roper startup&shutdown planning must be complete. Secure any raw materials, equipment or spares required. Develop adequate procedures for last minute modifications, safety chec3s and audits, inspections and record3eeping. Develop adequate procedures for emergency response in case of accident Develop individual tas3s and obCectives for each member of the startup team and ensure these are well understood 5nsure proper chec3lists are available for each phase of the startup&shutdown.
O#eration of Distillation "olumns: There are several fundamental process variables in a distillation column which must be controlled in order to get proper separation of componentsM O*erhead Tem#erature: The overhead temperature is determined by the composition of the liquid on the first tray, this liquid must be at its+ boiling point at the pressure of the column. The composition is controlled by the reflux ratio. The higher the reflux ratio, the higher the concentration of the lighter component on the top tray. As the lighter component boils, at a lower temperature, the temperature at the top of the column will be lower. There are limits to this which are dependent on the condenser temperature and the phase characteristics of the material in the column.
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Tem#erature Profile The temperature profile of a column is a plot of the temperature on each tray from the top of the column to the bottom. The lowest temperature should be at the top of the column, corresponding to the lightest components while the highest temperature should be at the bottom, corresponding to the heaviest component. The profile between the top and bottom of the column should be a smooth curve with no flat spots. This indicates that the composition is different on each tray and efficient separation is occurring. #f there is a section of the column in which the temperature profile is flat, the composition on those trays is very close and minimal separation is ta3ing place. The exception to this is often the feed area where a very cold !subcooled" or very hot !superheated" feed can cause the temperature profile to flatten. "olumn Pressure: The operating pressure in the column is determined by two factors, the composition of the overhead vapor being condensed and the cooling ! both amount and temperature" available in the overhead condenser. The condenser temperature must be cold enough to condense the lightest component in the overhead vapor to liquid. The pressure at which this occurs determines the operating pressure of the column. #f the lightest component is not condensed, the vapor in the overhead receiver will cause the system pressure to increase until the temperature in the condenser is low enough to condense the light component. #f this results in a pressure which is too high for the design of the column, the light end can be vented as vapor from the reflux drum. )eflu. )atio: The reflux ratio, along with the bottoms temperature, is the primary control variable for a distillation column. The definition of the reflux ratio is the ratio of liquid returned to the column divided by the distillate flow, the higher the value, the more liquid that is returned to the top of the column. The reflux ratio controls the tower top temperature, the degree of separation of the components and the amount of liquid flowing from tray to tray. As the reflux ratio is so important, the column is designed for a specific value 3nown as the optimum reflux ratio. This value is different for each application. 5asy separations may require a reflux ratio as low as ..2 while difficult separations may require as high as H or ;. :nce a column is running, the reflux ratio is fine tuned for the specific operating conditions of the plant. . Bottoms Tem#erature: The temperature at the bottom of the column determines the composition of the bottom product, the higher the bottoms temperature, the less light ends in the bottom product. The rate of heating also determines the vapor return rate to the column. The higher the bottoms temperature, the higher the vapor return rate. At some point the amount of vapor will become too great for the column and Cet flooding will result. As the bottoms temperature is increased, the reflux ratio may require adCustment to maintain the same overhead temperature. The bottoms temp is usually controlled by the amount of heating medium, such as steam of hot oil, flowing through the reboiler.
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0NIT B
DISTILLA TION "OL04N T)O0BL1S(OOTIN5

2looding: Distillation column capacity is usually restricted by flooding. 2looding is e.cessi*e accumulation of li,uid inside the column/ This accumulation is generall$ caused -$ one of the follo;ing mechanisms: S#ra$ 1ntrainment 2looding * at low liquid flow rates, trays operate in the spray form, where most of the liquid on the tray is in the form of liquid drops. As vapor velocity is raised, a condition is reached where the bul3 of these drops is entrained into the tray above. The liquid accumulates on the tray above instead of flowing to the tray below. 2roth 1ntrainment flooding * At higher liquid rates, the dispersion of the tray is in the form of a froth. @hen vapor flow rate is raised, froth height increases. @hen tray spacing is small, the froth envelope approaches the tray above. As this surface approaches the tray above, entrainment rapidly increases, causing liquid accumulation above. 9or large tray spacing K/H * 16 inchesL, the froth envelope seldom approaches the tray above. )iven enough vapor velocity, the froth would turn into spray and cause spray entrainment flooding per above. Do;ncomer Bac9u# 2looding * Aerated liquid is bac3ed up into the downcomer because of tray pressure drop, liquid height on the tray, and frictional losses in the downcomer apron. Do;ncomer "ho9e 2looding * As liquid flow rate increases, so does the velocity of aerated liquid in the downcomer. @hen this velocity exceeds a certain limit, friction losses in the downcomer and downcomer entrance become excessive, and the frothy mixture cannot be transported to the tray below. This causes liquid accumulation on the tray above. )enerally, at low tray spacing !less than /1 * /2 inches", froth entrainment flooding is favored. At higher tray spacing, and when conditions do not favor vapor cross flow, the froth regime will turn into a spray as vapor velocity increases, and spray entrainment flooding is favored. 9inally, when downcomers are small or downcomer bac3ups are high, downcomer flooding is favored.
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2looding can -e determined -$ one or more of the follo;ing s$m#toms: /" 1" 0" 6" 2" 5xcessive column differential pressure Kdelta pressure is greater than 0 inches of water per foot of pac3ed bedL Sharp rise in column differential pressure %oss of bottoms =apid rise of entrainment from column top tray Klarge rise in reflux vs normalL %oss of separation as can be detected by temperature profile or product analysis.
O#eration Difficulties: Dislodging and Damage of Tra$s: >ost tray or pac3ing damage comes from excessive liquid in the bottom of the column. #n some cases, totally flooded trays will get damaged if vapor slugs are allowed to EbubbleE through the column. =eliable bottoms level indication is essential for safe. column operation. Some techni,ues for #re*enting tra$ damage due to e.cessi*e li,uid le*els: /" 1" 0" 6" 2" -" 4ump out liquid vs boil it out. Aonstruct the bottom seal pan to be strong. Aonstruct the bottom 12 percent of trays for extra mechanical strength. 4rovide a liquid level differential pressure measurement for the bottom 4rovide facilities for easy diversion of bottom liquid to either the feed tan3 or storage tan3 so that liquid level can be readily reduced. 5nsure smooth and stable automatic control of boil up to the tower.
Li,uid Le*el in )eflu. Accumulators: An overflowing accumulator will usually bac3up liquid into the condenser, flooding some tubes. :ften, column pressure will rise and the relief valve may possibly lift A low accumulator level can cause pump damage due to lac3 of liquid KcavitationL. 4roper level indication with interloc3s to pump operation or column operation should be available. Sources and 1ffects of 3ater Pro-lems: The main adverse effects of water in distillation column service are pressure surges, flooding, cycling, corrosion, hydrates, and off*spec products.
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T$#ical sources of ;ater are: /" 1" 0" 6" 2" -" ," The feed stream. @ater may be found in the feed storage tan3 or from a lea3ing heat exchanger. 7ndrained water in a stripping steam line. EDryE steam is required prior to column introduction. Ahemical reaction. A condensation reaction forming water may occur between organic chemicals A lea3ing heat exchanger Kreboiler, condenserL. A pre startup wash. lea3 *test, pr steam*water operation. Aondensate formed in previous operations. #t could have remained trapped in pipelines or poc3ets inside the equipment. A water*containing stream that found its way to the column Ka typical example is water discharged from the desalter safety valve and ends up in a refinery crude columnL.
Lea9ing (eat 1.changers: Tube lea3s may occur in the reboiler, condenser, pre heater, precooler or any other heat exchanger lin3ed with the distillation column. 5ffects of heat exchanger tube lea3s into the column include off*spec products and&or undesirable chemical reactions. #n some cases, this reaction may lead to rapid corrosion or plugging. #t is important to reali<e that lea3ed material may cause vapor slugs and tray damage if conditions permit. %ea3s can be detected by heat exchange equipment sampling and&or off*line drain&vent chec3s. A lea3ing tube on an exchanger will show the heating material on the other side of the heat exchanger.
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Cryogenic Distillation

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DISTILLATION

D12INITIONS O2 3O)DS AND T1)4S 0S1D IN T(1 5AS P)O"1SSIN5 IND0ST)6

"ritical Point for a Pure Su-stance 8 3ater :

DISTILLATION "OL04N "O4PON1NTS

"ontents * notes and diagrams on distillation column components

2igure & : Distillation "olumn ;ith Tra$s and Pac9ing

P)IN"IPL1S O2 5AS P)O"1SSIN5 OP1)ATION

NATURAL GAS HEAT EXCHANGER N. GAS LIQUID

NAT0)AL 5AS ST)1A4

NATURAL GAS LIQUID

T14P1)AT0)1 )AN51 . P to O 1. P 9 ! * /H P to O 1; P A "

Pressure )eduction 8 E/T Process :

* /12 P to O /2. P 9 ! * H, P to O /./ P A "

B#)B 4=5SS7=5 )AS A:>>:D SB55T %:@ 4=5SS7=5 )AS A:>4=5SS:=

B#)B 4=5SS7=5 )AS %:@ 4=5SS7=5 )AS

@A=> DAT7=A% )AS S7=)5 TAD' AB#%%5=

DAT7=A% )AS %#R7#DS

S54A=AT: = 47>4 =#AB :#%

A?S:=?5= L1AN OIL ABSO)PTION

2ractionation 8 Deethani@er = De#ro#ani@er = De-utani@er:

Distillation and Bottoms S#ecifications:

Internal sources * * * noncondensables chemical reaction closed column outlets

Transient sources * * poc3ets of water flashing to steam internal explosions

DISTILLATION "OL04N OP1)ATION

Bringing column to desired o#erating rates/

1liminating undesira-le materials/

DISTILLA TION "OL04N T)O0BL1S(OOTIN5

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