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 Copyright 2004 International Human Resources Development Corporation
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Distillation Principles 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. Vapour Pressure and Boiling The vapour pressure of a liquid at a particular temperature is the equilibrium pressure exerted by molecules leaving and entering the liquid surface. Here are some important points regarding vapour pressure: 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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UNIT 1
DEFINITIONS OF WORDS AND TERMS USED IN THE GAS PROCESSING INDUSTRY

Absorber A tower or column that provides contact between natural gas being processed and a liquid solvent Absorption Absorption Factor 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. It is generally expressed as A = L/KKV where L and V are the moles of liquid and vapor, and K is the average value of the vapor liquid equilibrium constant for the component of concern. Absorption Oil A hydrocarbon liquid used to absorb and recover components from the natural gas being processed. Acid Gas The hydrogen sulfide and/or carbon dioxide contained in, or extracted from, gas or other streams. Adiabatic Expansion 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. Adsorbent A solid substance used to remove components from natural gas being processed. Adsorption The process by which gaseous components are adsorbed on solids because of their molecular attraction to the solid surface
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Amine (alkanolamine) 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 Gas Gaseous hydrocarbons occuring as a free-gas phase under original oil-reservoir conditions of temperature and pressure. Atmospheric Pressure The pressure exerted on the earth by the earth's atmosphere. A pressure of 760 mm of mercury or 101.3250 kPa 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 English - unit measure of liquid volume which, in the petroleum industry, equals 42 U.S. liquid gallons for petroleum or natural gas liquid products measured at 60F and equilibrium vapor pressure. One barrel equals 0.159 cubic meters, or 6.29 barrels per cubic meter (See Fig, 1-2). Blanket gas A gas phase maintained in a vessel containing liquid to protect the liquid against air contamination, to reduce the hazard of detonation, or to maintain pressure of the liquid. The source of the gas is external to the vessel. Blow Case A small tank in which liquid is accumulated and then forced from the tank by applying as or air pressure above the liquid level. Blowdown 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. Boilaway Test Sometimes used to describe the GPA weathering test for LPgas. Refer 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 mix A liquefied hydrocarbon product composed chiefly of butanes and propane. If it originates in a refinery, it may also contain butylenes and propylene. More specifically, it conforms to the GPA specifications for commercial B-P mixes as described in GPA Standard 2140. Breathing The movement of vapor in or out of an atmospheric pressure storage tank 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&W (basic sediment and water) Waste that collects in the bottom of vessels and tanks containing petroleum or petroleum products. Bubble Point The temperature at a specified pressure at which the first stable vapor forms above a liquid. Commercial Butane, A liquefied hydrocarbon consisting predominately of butane and/or butylene and which conforms to the GPA specification for commercial butane defined in GPA Standard 2140. Normal Butane, In commercial transactions, a product meeting the GPA specifications for commercial butane and, in addition, containing a minimum of95 liquid volume percent normal butane. Chemically, normal butane is an aliphatic compound of the paraffin series having the chemical formula C4HlO and having all of its carbon atoms joined in a straight chain. Calorimeter An apparatus which is used to determine the heating value of a combustible material.
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Carbonyl Sulfide A chemical compound of the aldehyde group containing a carbonyl group and sulfur (COS). Sometimes a contaminant in natural gas and NGL. It may need to be removed in order to meet sulfur specifications. Casinghead Gas Unprocessed natural gas produced from a reservoir containing oil. It contains heavier hydrocarbon vapors and is usually produced under low pressure from a casing head on the well. Charcoal Test A test standardized by the Gas Processors Association and the American Gas 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 distillation. The test is prescribed in Testing Code 101-43, joint publication of AGA and GPA. Chromatography A technique for separating a mixture into individual components by repeated adsorption and desorption on a confined solid bed. It is used for analysis of natural gas and NGL. Claus Process A process to convert hydrogen sulfide into elemental sulfur by selective oxidation. Compressibility Factor A factor, usually expressed as "Z," 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. Compression Ratio The ratio of the absolute discharge pressure from a compressor to the absolute intake pressure. Also applies to one cylinder of a reciprocating compressor and one or more stages of a rotating compressor. Condensate The liquid formed by the condensation of a vapor or gas; 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. In a steam system it may be water that is condensed and returned to the boilers.
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Convergence Pressure The pressure at a given temperature for a hydrocarbon system of fixed composition at which the vapor-liquid equilibrium K-values of the various components in the system become, or tend to become, unity. The convergence pressure is used to adjust vaporliquid equilibrium K-values to the particular system under consideration. Copper Strip Test A test using a small strip of pure copper to determine qualitatively the hydrogen sulfide corrosivity of a product. Refer to GPA LP-gas copper strip test (Copper Strip Method), ASTM D-1838 test procedure. Critical Density The density of a substance at its critical temperature and critical pressure. Critical Pressure The vapor pressure of a substance at its critical temperature. Critical Temperature For a pure component, the maximum temperature at which the component can exist as a liquid. Cryogenic Plant A gas processing plant which is capable of producing natural gas liquid products, including ethane, at very low operating temperatures, usually below minus 50C. Cubic Meter A unit of volume measurement commonly used in international commerce for petroleum, petroleum products and natural gas. One cubic meter measured at 15.56C = 264.172 U.S. gallons = 6.29 barrels = 35.315 cubic feet measured at 15.56C. 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. Debutanizer A fractionator designed to separate butane (and more volatile components if present) from a hydrocarbon mixture.
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Dehydration The act or process of removing water from gases or liquids. Demethanized Product A product from which essentially all methane and lighter materials have been removed. Demethanizer A fractionator designed to separate methane (and more volatile components if present) from a hydrocarbon mixture. Depropanizer 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. Desulfurizationf A process by which sulfur and sulfur compounds are removed from gases or liquid hydrocarbon mixtures. Dew Point The temperature at any given pressure, or the pressure at any given temperature, at which liquid initially condenses from a gas or vapor. It 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 vaporize a portion and then cooling to liquefy a part of the vapor. Materials to be separated must differ in boiling point and/or relative volatility. Doctor Test A qualitative method for detecting hydrogen sulfide and mercaptans in NGL. The test distinguishes between "sour" and "sweet" products.
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Dry Gas (1) Gas whose water content has been reduced by a dehydration process. (2) Gas containing little or no hydrocarbons commercially recoverable as liquid product. Gas in this second definition preferably should be called lean gas. End Point The maximum temperature observed on the thermometer during an ASTM distillation test. EP-Mix (ethane-propane mix) A product consisting of a mixture of essentially ethane and propane. Expansion Turbine A device which converts part of the energy content of a gas or liquid stream into mechanical work by expanding the gas or liquid through a turbine from which work is extracted. Extraction The process of transferring one or more components from one liquid phase to another by virtue of different solubility in the two liquids. It is also used to indicate removal of one or more constituents from a stream. Field Separator A vessel in the oil or gas field for separating gas, hydrocarbon liquid, and water from each other. Flash Point The lowest temperature at which vapors from a hydrocarbon liquid will ignite. See ASTM D-56. Fractionation See definition of "distillation." Generally used to describe separation of a mixture of hydrocarbons into individual products based on difference in boiling point and/or relative volatility. Freeze Valve A specially constructed and calibrated valve designed and used solely for determining the water content in propane product. See ASTM D-2713.
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Gas Constant (R) The constant multiplier in the Ideal Gas Law. Numerically, R=PV/T, if V is the volume of one mole of an ideal gas at temperature T and pressure P. Gas Hydrate Refer to definition of "hydrate". Gas Injection The injection of natural gas into a reservoir to maintain or increase the reservoir pressure or reduce the rate of decline of the reservoir pressure. Gas Lift A method for bringing crude oil or water to the surface by injecting gas into the producing well bore. Gas-Oil Ratio (GOR) 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 stock tank liquid. Gas Processing The separation of constituents from natural gas for the purpose of making salable products and also for treating the residue gas to meet required specifications. Gas Processing Plant A plant which processes natural gas for recovery of natural gas liquids and sometimes other substances such as sulfur. Gas-Well Gas The gas produced or separated at surface conditions from the full well stream produced from a gas reservoir. Gas-Well Liquid The liquid separated at surface conditions from the full well stream produced from a gas reservoir. Gathering System The network of pipelines which carry gas from the wells to the processing plant or other separation equipment.
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Heat Media (Heating Media) A material, whether flowing or static, used to transport heat from a primary source such as combustion of fuel to another material. Heating oil, steam, and an eutectic salt mixture are examples of heat media. Heating Value (Heat Of Combustion) 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. Heavy End The portion of a hydrocarbon mixture having the highest boiling point. Usually hexanes or heptanes and all heavier hydrocarbons are the heavy ends in a natural gas stream. Hexanes Plus (Or Heptanes 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). Hydrate A solid material resulting from the combination of a hydrocarbon with water under pressure. Immiscible Liquids that will not mix nor blend to give homogeneity are said to be immiscible. Inerts Elements or compounds not acted upon chemically by the surrounding environment. Nitrogen and helium are examples of inert constituents of natural gases. Isobutene In commercial transactions, a product meeting the GPA specification for commercial putane and, in addition, containing a minimum of 95 liquid volume percent isobutane. Chemically, a hydrocarbon of the paraffin series with the formula C4HlO and having its carbon atoms branched. Jacket Water Water 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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Joule-Thomson Effect 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 ASTM D-2420. Lean Gas (1) The residue gas remaining after recovery of natural gas liquids in a gas processing plant. (2) Unprocessed 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 Gas Gas used in a gas lift operation. Light Ends The low-boiling, easily evaporated components of a hydrocarbon liquid mixture. Light Hydrocarbon The low molecular weight hydrocarbons such as methane, ethane, propane and butanes. LNG (liquefied natural gas) The light hydrocarbon portion of natural gas, predominately methane, which has been liquefied. Loading Rack A structural and piping installation alongside a railroad track or roadway used for the purpose of filling railroad tank cars or transport trucks. LPG (liquefied petroleum gas) Refer to definition of "LP-gas".
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LP-gas (Liquefied petroleum gas) Predominately propane or butane, either separately or in mixtures, which is maintained in a liquid state under pressure within the confining vessel. LRG (liquefied refinery gas) Liquid propane or butane produced by a crude oil refinery. It may differ from LP-gas in that propylene and butylene may be present. LTX (low temperature extraction 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 LTS (low temperature separation) unit. Mercaptan, Any of a homologous series of compounds of the general formula RSH. All mercaptans possess a foul odor. Miscible Flood A method of secondary recovery of fluids from a reservoir by injection of fluids that are miscible with the reservoir fluids. Natural Gas Gaseous form of petroleum. Consisting predominately of mixtures of hydrocarbon gases. The most common component is methane. Natural Gasoline 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 GPA. See GPA Standard 3132. Natural Gas Processing Plant Term used for gas processing plant, natural gasoline plant, gasoline plant, etc. NGL (natural gas liquids) Natural gas liquids are those hydrocarbons liquefied at the surface in field facilities or in gas processing plants. Natural gas liquids include ethane, propane, ,butanes, and natural gasoline.
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Odorant An odoriferous compound added to natural or LP-gas to impart a distinctive odor for detection of fugitive vapors. Ethyl mercaptan is the most widely used odorant for LPgas, while tertiary butyl mercaptan, usually mixed with small amounts of other compounds, is the predominant odorant for natural gas. Oil-Well Gas Gas that is produced from an oil well. On-Stream Factor The percentage of time a unit is on-stream. Operating Factor 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. Packaged Unit A shop-assembled group of equipment and accessories which needs only foundations, inlet and outlet piping, and utility connections to make an operating unit. Packed Column A fractionation or absorption column filled with packing designed to give the required contact between the rising vapors and the descending liquid. Peak Shaving 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 (C5H12) 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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Pipeline Gas Gas which meets a transmission company's minimum specifications. Propane A normally gaseous paraffinic compound (C3H8). The term includes all products covered by GPA specifications for commercial and HD-5 propane. See GPA Standard 2140. Commercial Propane, A liquefied hydrocarbon product consisting predominately of propane and/or propylene and which conforms to the GPA specification for commercial propane as defined in GPASt andard 2140. Propane HD-5 A special grade of propane consisting predominately of propane and which conforms to the GPA specification for HD-5 propane as defined in GPA Standard 2140. Raw Gas Unprocessed gas, or the inlet gas to a gas processing plant. Raw Mix Liquid A mixture of natural gas liquids prior to fractionation. Also called "raw make". Recovery That percent or fraction of a given component in the plant feed which is recovered as plant product. Recycle Return of part of a process stream to a point upstream from where it was removed to enhance recovery or control. Reflux In fractionation, the portion of condensed overhead returned to the column to enhance achievable purity of the overhead product. Reflux Ratio A way of giving a relative measurement to the volume of reflux. Usually referred either to the feed or overhead product.
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Relative Density The ratio of the mass of a given volume of a substance to that of another equal volume of another substance used as standard. Unless otherwise stated, air is used as the standard for gases and water for liquids, with the volumes measured at 15.56C and atmospheric pressure (101.325 kPa). Relief System The system for safely relieving excess pressure to avoid exceeding equipment design pressure. Residue The material which remains after a separation process. (1) Residue gas is that gas remaining after the recovery of liquid products. (2) Residue may also be the heaviest liquid or solid remaining after distillation or reclaiming process. Retrograde Condensation (vaporization) Condensation or vaporization that is the reverse of expected behavior. Condensation caused by a decrease in pressure or an increase in temperature. Vaporization caused by an increase in pressure or a decrease in temperature. Rich Gas Gas feed to a gas processing plant for liquid recovery. Rich Oil The oil leaving the bottom of an absorber. It is the lean oil plus the absorbed constituents. RVP (Reid Vapor Pressure) The vapor pressure of a material measured by the Reid Method and apparatus as detailed in ASTM Test Procedure D-323. S & W (See bs&w) Saturated compounds hydrocarbon compounds having no unsaturated carbon valence bonds. Natural gas and natural gas liquids are saturated compounds. Saturated Liquid Liquid which is at its boiling point or is in equilibrium with a vapor phase in its containing vessel.
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Saturated Vapor Vapor at its dew point. shrinkage The reduction in volume of a gas stream by removal of some of its constituents such as for recovered products, fuel, or losses. SNG (Synthetic or Substitute Natural Gas) The gas product resulting from the gasification of coal and/or gas liquids or heavier hydrocarbons. Solution Gas Gas which originates from the liquid phase in an oil reservoir. Sour Liquids and gases are said to be "sour" if they contain hydrogen sulfide, carbon dioxide, and/or mercaptans above a specified level. It is also used to refer to the feed stream to a sweetening unit. Sour Gas Gas containing undesirable quantities of hydrogen sulfide, mercaptans, and/or carbon dioxide. It is also used to refer to the feed stream to a sweetening unit. Splitter 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). Sponge Absorbent An absorbent for recovering vapors of a lighter absorbent that is used in the main absorption process of a gas processing plant. Stabilized Condensate Condensate that has been stabilized to a definite vapor pressure in a fractionation system. Stabilizer A fractionation column designed to reduce the vapor pressure of a liquid stream.
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Stage Separation System 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. In plants using a low molecular weight absorption oil, the still is designed as a fractionation column. In 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. Strapping A term applied to the process of calibrating liquid storage capacity of storage tanks in increments of depth. Stream Day A continuous 24 hour period of plant operation. Stripper 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. Stripping Factor An expression used to describe the degree of stripping. Mathematically, it is KVfL, the reciprocal of the absorption factor. Stripping Medium As stated under "stripper", the medium may be steam, gas, or other material that will increase the driving force for stripping. Sulfur A yellow, non-metallic chemical element. In its elemental state, it exists in both crystalline and amorphous forms. In many gas streams, sulfur may be found as volatile sulfur compounds, such as hydrogen sulfide, sulfur oxides, mercaptans, and carbonyl sulfide. Reduction of the concentration of these gaseous sulfur compounds is often necessary for corrosion control and possibly for health and safety reasons. Sulfur Dioxide (SO2) A heavy, colorless, suffocating gas that is chemically an oxide of sulfur. Conversion 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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Sweet Gas containing essentially no objectionable sulfur compounds. Also, treated gas leaving a sweetening unit. Sweet Gas Gas which has no more than the maximum sulfur and/or CO2 content defined by (1) the specifications for the sales gas from a plant; (2) the definition by a legal body. Also, the treated gas leaving a sweetening unit. Temperature Correction Factor A factor for correcting volume at a given temperature to that at a specific reference temperature. Reference temperature most commonly used in the petroleum industry is 15.56C. Therm A unit of gross heating value equivalent to (1.055) X 107 kJ. Tonne A unit of mass measurement, commonly used in international petroleum commerce; an expression for the metric ton, or 1000 kilograms. Trayed Column A vessel wherein gas and liquid, or two partially miscible liquids, are contacted, usually concurrently on trays. Also refer to packed column. Turboexpander Refer to definition of "expansion turbine." ullage (See outage) Unsaturated Compounds Hydrocarbon 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. Unsaturates are produced by a thermal cracking or chemical reaction and can be found in synthetic gas (SNG) or light refinery gases (LRG). Vapor Pressure (true vapor pressure) The pressure exerted by the equilibrium vapor of a liquid when confined in a closed previously evacuated tank or test apparatus.
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Vapor Pressure Gasoline A descriptive phrase for natural gasoline meeting a specified vapor pressure. Vapor Pressure, GPA Vapor pressure as specified by GPA procedures. Vapor Recovery Equipment or process for the recovery of desired components from stock tank vapors or vapors from some other source. Volatile Sulfur An obsolete term referring to sulfur compounds that will vaporize readily (See sulfur). Weathering The evaporation of liquid caused by exposing it to the conditions of atmospheric temperature and pressure. Partial evaporation of liquid by use of heat may also be called weathering. Weathering Test A GPA test for LP-gas for the determination of heavy components in a sample by evaporation under specified conditions. Weight In Air Weight compared to a standard with no correction for air buoyancy. Wellhead 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. Wet Gas (1) A gas containing water, or a gas which has not been dehydrated. (2) A term synonymous with rich gas. Refer to definition of "rich gas". Wobbe Number A number proportional to the heat input to a burner at constant pressure. In British practice, it is the gross heating value of a gas divided by the square root of its gravity. Widely used in Europe, together with a measured or calculated flame speed, to determine interchangeability of fuel gases.
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UNIT 2
PHASE BEHAVIOR
PHASE BEHAVIOR Introduction: In planning, design and operation of modem petrochemical processes, engineers, technologists and process operators must know with- reasonable accuracy the properties of the fluids with which they deal. If 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 thickness and even the specifications for the control devices. 1.1 Vapor-Liquid Equilibrium : Terms/Definitions: Property - 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. Equilibrium - a state in which there is no tendency toward change, Phase - a completely homogeneous and uniform state of matter. Ideal Gas - is an imaginary gas which obeys exactly certain simple laws such as the laws of Boyle, Charles, Dalton. No real gas obeys these laws exactly over all ranges of temperature, although "lighter" gases (hydrogen, oxygen, air, etc.) under ordinary circumstances obey the ideal gas laws with but negligible deviations. Ideal Gas Law - from the work of Boyle and Charles, scientists developed the relationship now called the Ideal Gas Law. The equation used is pV = n RT. This equation can relate the volume, pressure, temperature, and the amount of a given gas. Equations of State - relate the p- V - T properties of a pure substance (or mixture) by theoretical or empirical relations. The Ideal Gas Law is a simple example of an equation of state. Vapor - a gas below its critical point which can condense (i.e change its phase).
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Gas - a substance which is above its critical point and is noncondensable. Vapor Pressure - the pressure at which vaporization and condensation are at constant temperature and pressure under equilibrium conditions for a pure substance or mixture. "Normal" Boiling Point - the temperature at which boiling will take place under a pressure of 1 atmosphere [101.3 kPa, 760 mm Hg]. Dew Point - the temperature at which a vapor starts to form a liquid during the process of condensation. Bubble Point - the temperature at which a liquid starts to form vapor during the process of vaporization. Saturated - when a vapor or liquid is just about to condense a drop of liquid or vaporize a 'puff of vapor respectively. Superheated - 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. Subcooled - when a substance is below its saturated liquid region. Triple 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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Multiphase Systems Water 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. For instance: liquid to solid : freezing solid to liquid : melting liquid to vapor : boiling vapor to liquid : condensation sublimation : solid to vapor At 101.325 kPa pressure, 1 atmosphere, the boiling point of water is 100 C. 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 vaporization. The boiling point of water changes with a change in pressure. For example; as pressure is lowered, the boiling point of water decreases, There are several points of specific interest on a P-T diagram. The first of these is the critical point, Tc and Pc, 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. If a substance above Tc and Pc is cooled, there will be no condensation of vapor to liquid, rather there is a slow change in physical properties. Critical pressures and temperatures can be found in the Physical Properties 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 101.325 kPa, the temperature rises to 100 C, then remains constant at 100 C until enough energy is added to vaporize the liquid, (heat of vaporization, hv) then the temperature will begin to increase once more. It is important to realize 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. Vapor pressure is very important for expressing the volatility of a substance at fixed conditions. For instance, the volatility of petrol is defined by the vapor pressure. Vapor pressure is also very useful in performing calculations involving vapors and liquids. It is usually given the symbol p* and can be found in tables or charts.
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Multicomponent Systems: Most systems in processing facilities are mixtures of components, not pure components. For our purposes, we will limit our discussion to two components to simplify matters although the same principles apply for systems containing multiple components. For mixtures, there are now three variables to plot, pressure, temperature and composition. For simplicity, only two of these variables are plotted at once and the third is kept constant: For example: Pressure versus temperature constant composition Temperature versus composition - constant pressure Pressure versus composition - constant temperature
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Critical Point for a Pure Substance ( Water )
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UNIT 3
DISTILLATION COLUMN COMPONENTS
Overview This topic is aimed at all process operations staff wanting to expand their knowledge about the various internals and externals to a distillation column. Objectives On completion of this topic, the trainee will : know the components of a distillation column and understand their function understand the physical limitations of trays and packings (flooding and jet flooding) know the common process variables and understand their meaning
Contents notes and diagrams on distillation column components
Components of Distillation Columns: The modem distillation column is comprised, of a tall column with trays mounted internally, an overhead system and a reboiler system. In some cases, packing may be used rather than individual trays.
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Figure 2 : Distillation Column with Trays and Packing
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Sic Distillation Equipment And Operation Main Components of Distillation Columns 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 major components: a vertical shell where the separation of liquid components is carried out column internals such as trays/plates and/or packings 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 back 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 below:
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Basic Operation and Terminology The liquid mixture that is to be processed is known as the feed and this is introduced usually somewhere near the middle of the column to a tray known 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. Heat 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. In 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 known 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 known as the reflux drum. Some of this liquid is recycled back to the top of the column and this is called the reflux. The condensed liquid that is removed from the system is known 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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Column Internals
Trays and Plates The terms "trays" and "plates" are used interchangeably. There are many types of tray designs, but the most common ones are : 1. Bubble cap trays
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. Vapour 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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2.
Valve trays
In valve trays, perforations are covered by liftable caps. Vapour flows lifts the caps, thus creating a flow area for the passage of vapour. The lifting cap directs the vapour to flow horizontally into the liquid, thus providing better mixing than is possible in sieve trays.
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3.
Sieve trays
Sieve trays are simply metal plates with holes in them. Vapour passes straight upward through the liquid on the plate. The arrangement, number and size of the holes are design parameters.
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Because 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. Liquid and Vapour Flow in a Tray Column The next few figures show the direction of vapour and liquid flow across a tray, and across a column.
Each tray has 2 conduits, one on each side, called downcomers. Liquid 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. Being 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. In 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. Tray Designs A tray essentially acts as a mini-column, each accomplishing a fraction of the separation task. From 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. Less 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 packings. Packings Packings are passive devices that are designed to increase the interfacial area for vapour-liquid contact. The following pictures show 3 different types of packings.
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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 packed section. This is important because a high pressure drop would mean that more energy is required to drive the vapour up the distillation column. Packings versus Trays A tray column that is facing throughput problems may be de-bottlenecked by replacing a section of trays with packings. This is because: packings provide extra inter-facial area for liquid-vapour contact efficiency of separation is increased for the same column height packed columns are shorter than trayed columns
Packed 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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Column Reboilers
There are a number of designs of reboilers. It is beyond the scope of this set of introductory notes to delve into their design principles. However, 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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UNIT 4
PRINCIPLES OF GAS PROCESSING OPERATION
Overview Natural gas liquids (or "NGLs), are hydrocarbons in a liquid state. There are many reasons for removing NGL's from the gas stream, including: 1. 2. 3. 4. The hydrocarbon components may be more valuable in their liquid state, either mixed or separated into their different individual elements. Pipeline gas quality specifications may restrict the amount of NGL is allowed. Heavier NGLs can separate from the gas stream in pipelines as temperatures drop, thus restricting flow in the pipeline. The NGLs may be used for re-injection on enhanced oil recovery projects. That is, they will be injected into a formation to help "sweep" 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 NGLs from the natural gas stream. The three most common are: Cryogenics, refrigeration and lean oil absorption.
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1.
Cryogenics
In the cryogenic process, a natural gas stream is cooled to extremely low temperatures to liquefy the ethane and heavier hydrocarbons. When a gas stream is chilled to below -50 F (-45 C ), 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
CRYOGENICS
Cryogenic processing of a natural gas stream involves three basic steps: dehydration, chilling and fractionation. Because of the very cold temperatures in cryogenic processing, the gas stream must be almost totally dehydrated to prevent the formation of Hydrates. 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. But 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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NATURAL GAS STREAM
DEHYDRATION DRY GAS CHILLING - 150 F ( - 101 C ) GAS AND LIQUID
WATER
FRACTIONATION
GAS ( METHANE)
NATURAL GAS LIQUID
CRYOGENIC PROCESSING
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Chilling 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 ( "J.T or Joule- Thompson), provides cold temperatures in the range of -50 F (-45 C) to -100 F (-73 C). To obtain the lowest temperatures, -100 F (-73 C) to -200 F (-129 C), pressure reduction with energy removal is accomplished using an expander -compressor. Cryogenics has relatively moderate energy requirements, and is considered the most efficient method for removing NGLS from the gas stream.
METHOD
TEMPERATURE RANGE 0 to 20 F ( - 18 to 29 C )
TYPICAL PERCENT RECOVERY Ethane Propane Butanes Heavier Ethane Propane Butanes Heavier Ethane Propane Butanes Heavier 25 55 93 97 70 80 97 99 80 96 99 100
Refrigeration
Pressure Reduction ( J.T Process )
- 50 to 70 F ( - 46 to 57 C )
Expander Process
- 125 to 150 F ( - 87 to 101 C )
HIGH PRESSURE GAS COMMON SHEET LOW PRESSURE GAS COMPRESSOR
HIGH PRESSURE GAS LOW PRESSURE GAS
EXPANDER
EXPANDER PROCESS
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2.
Refrigeration
Refrigeration 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 0F (-18 C) to -20 F (-29 C). Chilling causes the heavier hydrocarbons to liquefy, and then these NGLS can be separated from the gas.
COMPRESSOR
CONDENSER
REFIRGERANT VAPOR
WARM NATURAL GAS SURGE TANK CHILLER

COLD GAS AND LIQUIDS REFIRGERANT LIQUID
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Refrigerant The energy requirements of refrigeration are primarily for compressing the refrigerant and driving the condenser. While 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, making it a more economical method than lean oil absorption. 3. Lean Oil Absorption
In 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 "rich" oil. Once the NGLs are distilled, the lean oil is recycled back through the system.
GAS
LEAN OIL
LEAN OIL
CHILLER
NATURAL GAS LIQUIDS

METHANe
NATURAL gAS
SEPARATO R PUMP RICH OIL
ABSORBER LEAN OIL ABSORPTION
STILL
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High percentages (90-95%) of propane and heavier hydrocarbons (98-100%) can be recovered using lean oil absorption. Lean 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 takes its place.
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FRACTIONATION FLOW
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4.
Fractionation ( Deethanizer & Depropanizer & Debutanizer)
Fractionation is a. downstream treatment option for NGLs after they have been separated from the gas stream. By definition, fractionation consists of separating two components in a mixture of two or more components. For example, a depropanizer separates propane from a stream that contains propane and one or more heavier hydrocarbons. The propane is cooked out of the mixture and is the overhead product from the tower. The bottom stream is practically free of propane. Fractionation is essentially a distillation process. As you can see on the pervious diagram, different NGLs are cooked 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. Generally speaking, pressure and feed rate cannot be changed, since this would change conditions in the rest of the plant. Whether to fractionate is a question of economics. Is there a profitable market for the fractionated product? Because market conditions change rapidly and often, this question must constantly be answered to determine if fractionation will be done. There are times when the mixed NGLs will be more valuable than their separate components.
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UNIT 5
PRODUCT SPECIFICATIONS
Overview This topic is aimed at all process operations staff wanting to expand their knowledge about the control of distillation columns and the impact to product separation. Objectives On completion of this topic, the trainee will: understand how a distillation column is controlled (the six independent variables)
Contents 5.1 5.2 Distillate and Bottoms Specifications Control of Product Composition
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5.1
Distillation and Bottoms Specifications:
This topic is devoted to a discussion of measurement and control techniques common is distillation. For purposes of discussion, it will be assumed that: 1. 2. 3. 4. A column already exists. Many 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 making only two products a
distillate and bottoms product. If the assumptions are held for the above, there are eight (8) variables 1. 2. 3. 4. Column Pressure Feed Flow Rate Feed Composition Feed Temperature 5. 6. 7. 8. Heat Added (boil-up) Bottom Product Flow Rate Heat Removed (reflux) Distillate Product Flow Rate
only six (6) of these variables can be controlled independently. Compositions for distillate and bottom products are called dependent variables since they are not controlled directly but rather through the other variables mentioned above. Pressure Control Most distillation columns are maintained at some kind of constant pressure. This helps in keeping the condensation loading to the condenser as even as possible (dew point). The specific pressure is determined from economic considerations- For example, if operating pressure increases, the column temperature increases thus increasing the condenser cooling requirements and decreasing the reboiler heating requirements. Feed Control The first variable fixed would be the column pressure (as discussed above). If the feed conditions were fixed, this would necessitate that three (3) 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. 'Unfortunately, the feed composition is seldom subject to adjustment. For this reason, it is necessary to make 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. For efficient separation, it usually is desirable to have the feed at its bubble point when it's enters the column. If the feed composition varies, its bubble point also varies. It is a common practice to set the temperature control at a point which is equivalent to the bubble point of the heaviest feed. Reboiler Control: 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. Frequently, the boil-up 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. In kettle reboilers, the heating medium (e.g. steam) is added as required to try and achieve the bottom product specification Reflux Control: For 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 just 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. Conclusion: By 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. 5.2 Control of Product Purity & Fulfilling demands
A distillation unit operates between two extremes. In one case, insufficient separation is reflected in unacceptable product purity. In 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. When composition of the bottom product is the important consideration, it is desirable to maintain a constant temperature in the lower section of the column. When composition of the distillate product is the important consideration, it is desirable to maintain a constant temperature in the upper section of the column. Measuring 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. In 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. Laboratory analysis can be done to confirm and/or adjust 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 (G.c / s). If the distillate and/or bottoms streams could be sampled continuously and fed through an analyzer, the stream compositions could be used for column control.
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UNIT 6 DISTILLATION COLUMN CONTROL & INSTRUMENTATION Instrumentation -Measurement Points, Alarm Points. Safety Equipment, Relief Devices: Measurement Points, Alarm Points: As discussed in topic #5, 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) Feed Control: Reboiler Control: Bottoms Control: Tower Pressure Control: Reflux Control: Distillate Control:
Safety Equipment, Relief Devices: Distillation columns requires safety systems in order to function within the plant environment without creating risk to plant personal and other process equipment. These safety systems may range in complexity from simple alarms to interlock systems. Examples of areas that should have alarms are: Reflux Drum : high and low level alarms, high pressure alarm
Column Bottom : high and low level alarms Feed Flow Reflux Flow Reboil : high and low flow alarms : high and low flow alarms : high temperature alarm, high and low flow alarms (steam ) low flow alarms (process).
A major concern in the operation of distillation systems is overpressure of the equipment and possible catastrophic failure , A partial list of the causes of overpressure is found below:
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a)
Utility failure loss of coolant loss of electric power loss of steam loss of instrument air
b)
Controller failure ( human error in opening valve) failure of reboiler controller failure of pressure controller failure of feed controller failure of pump around controller
c)
Extraneous 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 pockets of water flashing to steam internal explosions
Methods of relieving overpressure which should be included in the column design are: properly sized 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 Column Control: Distillation column control schemes may be broken into two major types, material balance systems and heat balance systems. Of the two, the material balance system or some variation of it, is the most common. Material Balance System: In 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. It is a common practice to have both distillate and bottoms on level control, thus making accumulation in the column unlikely. 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 known as direct control. Energy Balance System: In 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. For these reasons, energy balance controls are only used if a satisfactory material balance system cannot be implemented or in conjunction with an advanced computer control system.
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UNIT 7
DISTILLATION COLUMN OPERATION

Startup / Shutdown: Once 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 take preventative measures against performance deterioration. Line Blowing: Normally 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 joints. Most blowing is done to atmosphere and not into the distillation column itself. Pressuring and Depressuring: This is done with the same utility mentioned above. The column, connecting equipment, piping, along with all instrumentation is checked for leakage. The column system must be leak proof and can be checked by monitoring the column pressure [no drop in transmitter signal] and also by "snooping" or checking for leaks 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 [especially on vacuum systems] on the column as it allows explosive mixtures to occur. The column should be kept under a nitrogen "pad" prior to startup so as not to cause any problems on startup. Blinding and Unblinding: Most 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 [safety concerns]. 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.. Leak Testing: Per above "pressuring and depressuring " step. A soapy water solution can be used as a "snoop" test. Most times this solution is placed in a bottle [or can be purchased as "snoop"]. All flanges and equipment / instrument connections are squirted with the soapy water solution. If any leaks occur, the solution will bubble vigorously.
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Washing: 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 "deadspots" that cause problems with the process material to be put through the column itself. A "water run" can be done to help calibrate instruments and check for pump seal problems, leaks, etc.. Steaming: Some columns can be purged with steam to exclude air. This can be done especially in warm climates ( no freezing problems). Also, steam makes a good leak check since it can "find" leaks better than any external testing. Dryout: Normally done with dry air or nitrogen utility. Can also be a solvent drying as well depending on the application. Once 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 availab1e 1) Final elimination of undesirable materials.
The distillation column system should be clean, leak checked, and ready to run. 2) Bringing column to normal operating pressure.
Depending on what the desired pressure is, this may be done by use of vacuum pumps/ejectors [if vacuum column] or by allowing the pressure control system to respond to column liquid boil up. 3) Column 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. 4) Introduction of feed.
This is done once all the above are done. 5) Starting up 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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6)
Bringing column to desired operating 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 [if the distillate/forwards can be recycled], If the forwards can not be recycled, then a total reflux can be done for a short time until the specifications are okay, then reflux ratio can be set along with a feed increase and required reboiler/heating load increase [to keep the bottoms on spec], Column shutdown also follows a similar series of steps, typically: 1) Reducing 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 keep the reboiler running on a liquid inventory [i.e. no . bottoms being pumped forward either. 2) Shutting down heating and cooling sources.
The feed can be stopped per step (3) 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. 3) Stopping feed.
The feed can be stopped sooner than the heating source shutdown if the level rise in the column becomes too high [alarm point]. This will help minimize the pump-out of excess liquid inventory from the bottom of the column if required for any shutdown activity. 4) Draining liquids.
Both the condenser [reflux inventory] and reboiler [bottoms inventory] can be pumped out or drained to storage inventory prior to any column decommissioning activities. 5) Cooling or heating column.
If required for maintenance and/or vessel entry work, the column may need to be further cooled or heated using the process material and/or utility as required. 6) Bringing column to atmospheric pressure.
For vacuum systems, nitrogen is used to repressure the column. For 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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7)
Eliminating undesirable materials.
In most cases, nitrogen is used to purge out any remaining vapors and liquids Prior to vessel work. 8) Prepare the column for opening to atmosphere.
Hopefully 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. Operations staff should be aware of any specific hazards or potential problems with the specific column prior to startup/shutdown. Prior to startup/shutdown, there are several other items that should be considered: 1) 2) 3) 4) 5) 6) 7) 8) 9) Prepare adequate procedures for operation, startup, shutdown and maintenance. Ensure the startup/shutdown team consists of personnel who have all the required skills for the procedure. Adequate training for the startup team, supervisors and operators is required. Proper startup/shutdown planning must be complete. Secure any raw materials, equipment or spares required. Develop adequate procedures for last minute modifications, safety checks and audits, inspections and recordkeeping. Develop adequate procedures for emergency response in case of accident Develop individual tasks and objectives for each member of the startup team and ensure these are well understood Ensure proper checklists are available for each phase of the startup/shutdown.
Operation of Distillation Columns: There are several fundamental process variables in a distillation column which must be controlled in order to get proper separation of components: Overhead Temperature: 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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Temperature 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. If 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 taking 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. Column 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. If 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. If 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. Reflux Ratio: 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 known as the optimum reflux ratio. This value is different for each application. Easy separations may require a reflux ratio as low as 0.5 while difficult separations may require as high as 8 or 9. Once a column is running, the reflux ratio is fine tuned for the specific operating conditions of the plant. . Bottoms Temperature: 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 jet flooding will result. As the bottoms temperature is increased, the reflux ratio may require adjustment 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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UNIT 8
DISTILLA TION COLUMN TROUBLESHOOTING

Flooding: Distillation column capacity is usually restricted by flooding. Flooding is excessive accumulation of liquid inside the column. This accumulation is generally caused by one of the following mechanisms: Spray Entrainment Flooding - 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 bulk of these drops is entrained into the tray above. The liquid accumulates on the tray above instead of flowing to the tray below. Froth Entrainment flooding - At higher liquid rates, the dispersion of the tray is in the form of a froth. When vapor flow rate is raised, froth height increases. When 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. For large tray spacing [18 - 24 inches], the froth envelope seldom approaches the tray above. Given enough vapor velocity, the froth would turn into spray and cause spray entrainment flooding per above. Downcomer Backup Flooding - Aerated liquid is backed up into the downcomer because of tray pressure drop, liquid height on the tray, and frictional losses in the downcomer apron. Downcomer Choke Flooding - As liquid flow rate increases, so does the velocity of aerated liquid in the downcomer. When 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. Generally, at low tray spacing (less than 12 - 15 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. Finally, when downcomers are small or downcomer backups are high, downcomer flooding is favored.
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Flooding can be determined by one or more of the following symptoms: 1) 2) 3) 4) 5) Excessive column differential pressure [delta pressure is greater than 3 inches of water per foot of packed bed] Sharp rise in column differential pressure Loss of bottoms Rapid rise of entrainment from column top tray [large rise in reflux vs normal] Loss of separation as can be detected by temperature profile or product analysis.
Operation Difficulties: Dislodging and Damage of Trays: Most tray or packing damage comes from excessive liquid in the bottom of the column. In some cases, totally flooded trays will get damaged if vapor slugs are allowed to "bubble" through the column. Reliable bottoms level indication is essential for safe. column operation. Some techniques for preventing tray damage due to excessive liquid levels: 1) 2) 3) 4) 5) 6) Pump out liquid vs boil it out. Construct the bottom seal pan to be strong. Construct the bottom 25 percent of trays for extra mechanical strength. Provide a liquid level differential pressure measurement for the bottom Provide facilities for easy diversion of bottom liquid to either the feed tank or storage tank so that liquid level can be readily reduced. Ensure smooth and stable automatic control of boil up to the tower.
Liquid Level in Reflux Accumulators: An overflowing accumulator will usually backup liquid into the condenser, flooding some tubes. Often, column pressure will rise and the relief valve may possibly lift A low accumulator level can cause pump damage due to lack of liquid [cavitation]. Proper level indication with interlocks to pump operation or column operation should be available. Sources and Effects of Water Problems: 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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Typical sources of water are: 1) 2) 3) 4) 5) 6) 7) The feed stream. Water may be found in the feed storage tank or from a leaking heat exchanger. Undrained water in a stripping steam line. "Dry" steam is required prior to column introduction. Chemical reaction. A condensation reaction forming water may occur between organic chemicals A leaking heat exchanger [reboiler, condenser]. A pre startup wash. leak -test, pr steam-water operation. Condensate formed in previous operations. It could have remained trapped in pipelines or pockets inside the equipment. A water-containing stream that found its way to the column [a typical example is water discharged from the desalter safety valve and ends up in a refinery crude column].
Leaking Heat Exchangers: Tube leaks may occur in the reboiler, condenser, pre heater, precooler or any other heat exchanger linked with the distillation column. Effects of heat exchanger tube leaks into the column include off-spec products and/or undesirable chemical reactions. In some cases, this reaction may lead to rapid corrosion or plugging. It is important to realize that leaked material may cause vapor slugs and tray damage if conditions permit. Leaks can be detected by heat exchange equipment sampling and/or off-line drain/vent checks. A leaking tube on an exchanger will show the heating material on the other side of the heat exchanger.
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Distillation

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Distillation

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DISTILLATION

DEFINITIONS OF WORDS AND TERMS USED IN THE GAS PROCESSING INDUSTRY

Critical Point for a Pure Substance ( Water )

DISTILLATION COLUMN COMPONENTS

Contents notes and diagrams on distillation column components

Figure 2 : Distillation Column with Trays and Packing

PRINCIPLES OF GAS PROCESSING OPERATION

NATURAL GAS HEAT EXCHANGER N. GAS LIQUID

NATURAL GAS STREAM

DEHYDRATION DRY GAS CHILLING - 150 F ( - 101 C ) GAS AND LIQUID

NATURAL GAS LIQUID

Pressure Reduction ( J.T Process )

- 125 to 150 F ( - 87 to 101 C )

HIGH PRESSURE GAS COMMON SHEET LOW PRESSURE GAS COMPRESSOR

HIGH PRESSURE GAS LOW PRESSURE GAS

WARM NATURAL GAS SURGE TANK CHILLER

NATURAL GAS LIQUIDS

SEPARATO R PUMP RICH OIL

ABSORBER LEAN OIL ABSORPTION

Fractionation ( Deethanizer & Depropanizer & Debutanizer)

Distillation and Bottoms Specifications:

Internal sources noncondensables chemical reaction closed column outlets

Transient sources pockets of water flashing to steam internal explosions

DISTILLATION COLUMN OPERATION

Bringing column to desired operating rates.

Eliminating undesirable materials.

DISTILLA TION COLUMN TROUBLESHOOTING

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