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1. Introduction 2. History of Distillation 3. Types of Stages 4. Control Schemes 5. Trouble Shooting 6. Industry Incidents 7. Conclusions
Distillation Is a unit operation in which a mixture of two or more molecular substances are separated into different products. Distillation is one of the most common separation techniques. Distillation can also be called fractional distillation or fractionation. Other types of separation techniques includes, crystallization and membrane separation.
The separation of components from a mixture by distillation depends on the difference in boiling points of the individual components, sometimes called relative volatility. For close boiling mixtures many stages are required to reach the desired purity.
Early Distillation was basically batch stills to produce ethanol. The Crude ethanol was placed in a still and heated, the vapor condensed for consumption. Later crude oil was placed in batch stills to produce lamp oil.
The next progression was to continually feed the still and recover the light product. Notice the separation that can be accomplished in one stage.
.Distillation History Next was a series of stills with a continuous feed that flowed through the series. Recovery was low.
Distillation History .
Still low recovery. .Distillation History The next progression was to return the vapor back to the upstream still.
Distillation History .
Distillation History The next progression was to place the stills in a column and interchange the vapor and liquid to improve recovery. . To obtain good separation you need many stills in series.
Distillation History .
Early flow measurement was made by counting the strokes of a positive displacement pump. .Distillation History Early small towers has one or two large bubble caps per tray.
. All instrumentation was local.Distillation History Early still men set their reflux rates in strokes per minute. You ran the units by sound and feel.
Distillation History A Kerosene Hydrotreater built in 1952 had one bubble cap per tray on the Stripper Tower which was one meter in diameter. .
Distillation History 1 Bubble cap per Tray 1m .
. Early trays were dual flow trays which then progressed to bubble cap trays and down comers were added.Distillation History The liquid and vapor traveled through the center of the column and mixed on the outer ring of each bubble cap.
Distillation History Later when tray efficiency became more important. flow on the tray began to be studied and several types of trays with changed flow patterns were developed. .
Reactive Distillation . Continuous Distillation A.Types Of Distillation Columns 1. Multiple Feeds and Products B. Extractive Distillation C. Batch Distillation 2.
.Types Of Distillation Columns Batch Distillation processes on a dis-continuous basis. Feed is processed in batches and distilled by selectively removing the more volatile fractions over time.
Additional variations may be utilized in a Continuous Distillation Column. The column may have multiple feed points and products. .Types Of Distillation Columns Continuous Distillation has a constant feed rate and is the most common of the two types.
Types Of Distillation Columns The column may have a solvent added to the system to help increase the separation. this type of column is named an extractive distillation column. . this type of column is named a reactive distillation column. The column may have a catalyst bed and reaction occurring in the column.
Trays A. Reboiler / Condenser 3. Sieve Deck Tray D. Structured . Bubble Cap Tray C. Random B. Packing A. Valve Tray E. Down comer Advances 4. Flash Drum 2.Types of Stages 1. Dual Flow Tray /Ripple Tray B.
Flash Drum The simplest type of distillation device is the flash drum. An example of where we utilize a flash drum for separation in an ethylene plant is in the hydrogen / methane drum.Types of Stages 1. . It is a single stage and can approach 100% of equilibrium limits it there is sufficient residence time.
Flash Drum An over head receiver is an example of a flash drum.Types of Stages 1. The separation of a single flash drum is limited. A 50:50 mixture of ethylene and propylene can only be separated to about 80:20 in a single flash drum. .
Types of Stages Vapor Liquid .
. and kettle drums. The three normal types of reboilers are horizontal thermosyphon. vertical thermosyphon.Types of Stages 2. The best design is for the liquid from the bottom tray to pass through the reboiler at least once before being drawn off as tower bottoms. It can approach 100% of equilibrium limits it there is sufficient residence time. Reboiler / Condenser A reboiler is a flash drum with heat exchange.
partial. total. Reboiler / Condenser A Condensers is a flash drum with heat exchange There are three major types of condensers. and hot vapor by-pass. Each has its best application. .Types of Stages 2.
For example when there is a small amount of methane and hydrogen mixed in a propylene stream. Partial Condenser The partial condenser is best used when there is a large difference in the overhead vapor compositions.Types of Stages A. The partial condenser condenses the propylene and leaves the methane and hydrogen as a vapor to be vented from the overhead receiver. like in the propylene towers. .
The system needs to be reviewed to address the potential build of on non-condensable gases in the heat exchanger that can reduce the cooling potential of the exchanger. Partial Condenser This type of condenser works well for most applications. .Types of Stages A.
Types of Stages Vent .
Types of Stages B. . This system also needs to be reviewed to address the potential build of non-condensable gases in the heat exchanger that can reduce the cooling potential of the exchanger. The overhead vapors can be condensed at approximately the same temperature. Total Condenser The total condenser is best used when there is a small difference in the overhead vapor compositions.
Types of Stages Vent .
The hot vapor by pass condenser also has a lower installed cost due to the heat exchanger being installed on the ground level. Hot Vapor By Pass Condenser The hot vapor by pass condenser is best utilized when there is the potential for large changes of overhead vapor composition. The vapor by pass can be used to maintain the pressure in the tower system when the light components are lower than design. .Types of Stages C.
because of the physical location of the exchanger. increasing the temperature of the reflux.Types of Stages C. which makes hydrocarbons harder to separate. has even higher potential to build noncondensable gases in the heat exchanger that can reduce the cooling potential of the exchanger. . Hot Vapor By Pass Condenser The negatives of the Hot Vapor By Pass Condenser is that the by pass can be opened too much. and raises the tower pressure. This system. This reduces the tray efficiency in the top of the tower.
Types of Stages Vent .
Valve Tray F. Trays A. Bubble Cap Tray D. Dual Flow Tray /Ripple Tray C. Tray advances . Sieve Deck Tray E. Baffle Trays B.Types of Stages 3.
The vapor must over come this liquid head to move up the column. For most trayed columns. On the tray the vapor and liquid are contacted and then above the tray they are separated. Tray design Trayed Columns utilize a pressure and temperature differential to separate the products.Types of Stages 3. the weir holds a liquid level of each tray. .
Types of Stages 3. . Trays utilize the staged contact principle to separate products. Tray design Any deviation that develops that restricts the vapor and liquid from contacting and then separating will deteriorate the column’s ability to meet design specifications.
For trays to function they need to mix the vapor and the liquid. valve trays. Tray design One of the first trays developed was the dual flow tray. . to bubble caps. and to directional flow valve trays.Types of Stages 3. The liquid and vapor traveled up and down the column in the same tray opening. Each function must be as complete as possible. then separate the vapor and the liquid. Tray design then moved to sieve decks.
The vapor disengages and move to the tray above. • The steps are repeated in the next tray. • The bulk liquid flows down the downcomer to the next tray.Staged Equipment: the mechanism • • • • Vapor and liquid mixes to form a froth. The froth overflows across a weir. Mass transfer occurs within the froth. .
Types of Stages B. Bubble Cap Tray Is a tray that has cap over the opening of the tray deck. . They are used in palm oil reactive distillation. but they are more expensive than other types of trays. with a bubbling ring in the bottom of the cap. The advantage of bubble cap trays is that they do not weep.
Types of Stages .
which maintains a set liquid level on the tray.Types of Stages C. . Sieve Deck Tray A sieve tray is essentially a plate with holes punched into the plate. The number and size of the holes is based on the vapor flow up the tower. a dam and overflow device on the side of the plate. The liquid flow is transported down the tower by down comers.
Typically sieve deck trays have a minimum capacity. .Types of Stages C. or the liquid level on the tray will weep down to the next tray through the holes punched on the plate. Sieve Deck Tray To maintain the liquid level on the tray a minimum amount of vapor traffic up the tower must be maintained. or downturn. of approximately 70%.
The advantage to this design was the ability to maintain the liquid level on the tray deck. or downturn. Valve Tray One of the next developments was to add a variable valve opening to the tray deck. This valve would open in relation to the vapor flow. of approximately 60%. . Typically valve deck trays have a minimum capacity.Types of Stages D.
Types of Stages Tray Advancements The latest in tray advancements involve the flow across the tray and the down comer design. .
Types of Stages Tray Efficiency is a function of 1.V:L . 4. 2. 5. 3. Path Flow Length Elimination of stagnant zones Bubbling Promoters Weir Heights Hydraulic Rates .
Types of Stages 1. The path flow lengths less than 500 mm should be avoided. On of the reason the multiple down comers trays has less efficiency is path flow length. An advantage of swept back weirs is that it increases the path flow length. Path Flow Length The efficiently of a tray is a function of path flow length. .
Elimination of stagnant zones The elimination of stagnant zones on the tray will improve tray efficiency. .Types of Stages 2.
Types of Stages
• • • • • • Eddy flows Caused by the round shape of columns. Liquid flows in straight directions across a tray. The rounded edge becomes dead zones Poor mass transfer and high residence time. “flow directioner” to change the flow pattern at the edge
Types of Stages
3. Bubbling Promoters The clear liquid exiting the downcomer has some resistance to the vapor, as compared to the froth developed later on the tray path.
Types of Stages
3. Bubbling Promoters On a tray with long flow path length and short weir heights, you can develop vapor and liquid channeling, causing weeping at the down comer outlet.
Types of Stages Froth Pusher Stepped Outlet Weir Existing DC Bolting Bar Down Comer Adaptor Existing Tray Support Ring .
. Weir Heights The weir height has an effect on the tray efficiency.Types of Stages 4. Recommendations are not to exceed 100 mm or 1/6 of tray spacing. and 50 to 75 is suggested for all services except vacuum services.
. Hydraulic Rates The hydraulic rate has an effect on the tray efficiency. efficiency will decrease. When the V:L ratios are not equal molar. at high rates froth touches the next tray.Types of Stages 5. At low rate trays will weep.
Packing utilizes a continuous contacting principle to separate products.Types of Stages 4. A major advantage to packed columns is the reduction in pressure across the column. Packing Random and Structured Packed Columns generate a mass transfer area by providing a large surface area over which the liquid can transfer heat and mass to the vapor. .
Liquid accumulation for a packed column is lower than that of a trayed column. Packing Typically the column pressure drop for a packed column is less than that of a trayed column because of the percent open area. Typical percent open area of a trayed column is 8 to 15%. whereas a packed column can approach 50%. .Types of Stages 4.
Packing has been used successfully in lowpressure applications. less than 150 psig. reducing entrainment when foaming agents are present. Packing generates thin films instead of fine droplets for mass and heat transfer.Types of Stages 4. . Packing Another advantage of packed column is reduced foaming.
Random Packing .Types of Stages A.
Structured Packing .Types of Stages B.
Non-staged Equipment: the mechanism • Bulk liquid is broken into fine droplets when in contact with packings. • Appears as a continuous froth across the height of the packed bed. • Provides large surface area for effective heat and mass transfer. .
Trays will normally eventually equalize whatever mal-distribution is developed by the vapor and liquid feeds.Non-staged Equipment: the mechanism The introduction of vapor and liquid to the packing is very important. . Packing will enhance whatever mal-distribution is developed by the introduction of the vapor and liquid feeds.
2. Up till this point we have discussed hardware. In distillation the hardware was developed and then a study was conducted to understand why it might work. Now let us discussed why the hardware might work.Concepts 1. 3. .
.Concepts 1. The nature of hydrocarbons is such that they separate better at lower pressure. Normally the pressure of a tower is set as low as possible based on the ability of the over head condenser to condense the over head vapor. Hydrocarbons separate better at lower pressure. The preferred cooling medium is water and the tower pressure is raised until the over head vapor can be condensed at 90 degrees F / 45 degrees C.
Concepts 1. Hydrocarbons separate better at lower pressure. A balance must be done between the construction cost and the utility cost. which is a construction cost. Some C2 Splitters run at lower pressure than other designs utilizing this lower pressure separation ability. The ability to separate determines the number of trays. To utilize lower pressure can require refrigeration. which is a utility cost. . Low pressure DeMethanizers with Methane Refrigeration can be shown to be cost effective.
When energy is added to a substance. . that energy is called latent heat. The motion of molecules causes heat energy. Heat is a form of energy. Heat is a form of energy caused by the motion of molecules. When energy is added to a substance and the substance changes phases from a liquid to a gas.Concepts 2. When energy is added to a substance and the temperature of the substance increases. this is called sensible heat. the motion of the molecules increases.
Concepts 2. To raise 1kg of water 1 degree requires 1000 calories. The unit of measurement of energy is called a calorie. . Heat is a form of energy caused by the motion of molecules. To change the phase of ethylene from liquid to a gas requires 114 calories. which is about 500 times the sensible heat value. 1 degree C. To change the phase of water from liquid to a gas requires 537 calories. It is the amount of energy to raise one gram of water.
Concepts 2. the temperature and pressure change are the energy carriers. The availability and large latent heat value are the reasons we use water as a heat carrier. Because we do not use the latent heat in pumps and compressors. . Heat is a form of energy caused by the motion of molecules. The large latent heat value can be utilized in reboilers.
if given enough time. . A vessel filled with two hydrocarbons is said to be at equilibrium if the number of light molecules escaping from the liquid is equal to the number returning to the liquid. total separation of two similar hydrocarbons cannot be obtained.Concepts 6. Equilibrium is the state which systems will establish. In one vessel because of the transfer of molecules from the liquid to the vapor.
Equilibrium is the state which systems will establish. if given enough time.Concepts 6. .
7 / 36.0159 -426.070 -127.00 Methane CH4 16.0 Ethylene C2H4 28.46 12.0 Propylene C3H6 42.5 Iso Butane C4H10 58.62 2.02 2.043 -258.123 10.53 1.53.65 5.71 13.0 / 11.0 / 9.0 Ethane C2H6 30.73 8.61 2.0 / 15.081 .8 / 8.9 / 13.83 9.097 .43.5 .7 Propane C3H8 44.25 2.130 188.78 6.3 / 4.53 2.054 -154.Concepts Hydro Carbon Formula Molecular Weight Boiling Point (F) Density (ft3/lb) Flammability Limits Low/High Hydrogen H2 2.71 23.
C Mass Balance Energy Balance Composition Balance . B.Tower Balances A.
Mass Balance All vessels will eventually reach a material balance. mass in equals mass out. Mass In = Mass Out + Accumulation . For distillation towers the material balance is.
Side Draws and Tower Bottoms flows.Mass Balance Sources of material into the tower normally are the feed points. Overhead Liquid. Sources of material out of the tower include Overhead Vapor. .
and level of hydrocarbons on the trays. Tower Bottoms Reservoir. .Mass Balance Sources of accumulation include Overhead Receiver or Reflux Drum. the Overhead Receiver and the Bottoms Reservoir. Two of the accumulations are straight forward.
.Mass Balance The third accumulation. is much more difficult to quantify. To build the inventory in the C2 Splitter Tower takes 8 hours. It is by far the largest accumulation in the tower. but less than one hour for the over head receiver to be filled. the level on the trays.
Mass Balance The tower delta P is a guide to how much level is on the trays. therefore the level on the trays is determined by reboiler. . The reflux is made in the reboiler. A stable reboiler heat input will stabilize the tower. The tower delta P is based on the amount of reflux that is added to the tower.
Mass Balance One of the first tower control schemes was the Material Balance that was developed in 1930s. . A field operator looking at sight glasses controlled the overhead and bottoms levels.
The Material Balance Control Scheme does not address the accumulation of level on the trays. the tower energy. and composition balance. the Material Balance Control Scheme can be utilized if the product specifications are lax.Mass Balance Today with level controls. .
.Mass Balance For most high purity product this is not the best control scheme due to the large number of trays in product fractionators.
Mass Balance PI TI .
energy in equals energy out. The feed can also be a source of energy if it is preheated. Energy In = Energy Out + Accumulation The main source of energy into the tower normally is the reboiler. . For distillation towers the energy balance is.Energy Balance All vessels will eventually reach an energy balance.
Overhead Liquid. the Overhead Receiver and the Bottoms Reservoir. Two of the accumulations are straightforward. and level of hydrocarbons on the trays. Smaller sources include Overhead Vapor. Tower Bottoms Reservoir.Energy Balance The main sources of energy out of the tower are the Overhead Condenser and the Tower Bottoms Flow. Side Draws and Tower Feed if it is cooled. Sources of accumulation include. .
the level on the trays. The first is the level on the tray changes. Three things happen on a tray when a reflux move is made. It is by far the largest energy accumulation in the tower.Energy Balance The third accumulation. . is much more difficult to quantify.
The third is that the composition on the tray changes. it takes one hour and thirty minutes for the change to be seen at the tower bottoms.Energy Balance The second is the energy or temperature on the tray changes. If each of these changes takes one minute and there are 30 trays in the column. .
it takes five hours for the change to be seen in the tower bottoms.Energy Balance If there are 100 trays in the column like in the C2 Splitter. . it takes 12 hours and thirty minutes for the change to be seen in the tower bottoms. If there are 250 trays like in a Polymer Grade C3 Splitter.
if they are installed correctly and calibrated.Energy Balance The Energy Balance Control Scheme was developed in 1960s. Instrumentation was improving and flow meters were becoming more accurate. A current orifice plate flow meter can approach 1.0% accuracy. .
01% accuracy. . which uses the vibrations of a tube as the fluid flows by can approach 0. The latest flow meters.5% accuracy.Energy Balance An average field orifice plate flow meter is normally considered to have 2.
The energy to the reboiler was measured and used as a control point. The energy was removed in the overhead condenser. . the heat input to the tower could be measured and controlled.Energy Balance Because of the improved instrumentation. This led to the Tower Energy Balance Control Scheme.
Energy Balance The overhead product was sampled and the product was changed by the sample results. . The sample results were returned typically four to five hours after the samples were caught. This meant that the tower adjustments were always behind what the tower actual operation was. To compensate for this lag time the products were always kept above the specification to ensure on test product.
reducing your cash margin. The main problem with the energy balance control scheme is that is does not take into account the composition balance.Energy Balance To be consistently above the sell specification gives away product. .
Energy Balance PI .
At constant pressure the temperature can be an indication of the composition and the product flow can be controlled by the difference in the two temperature points. .Energy Balance A later variation of the energy balance control scheme was the Delta T Energy Balance.
This will reduce the delta T between the temperature points. which will increase the reflux to the tower. . resulting in the toluene composition being decreased at the Benzene Product.Energy Balance For example in a Benzene Toluene Splitter the lower temperature point will began to increase as the toluene concentration increases. The product flow can then be decreased.
but ignores the composition balance.Energy Balance The advantage of a delta T over a single point is that the delta T takes the pressure deviations out of the control scheme. . This control scheme works.
Energy Balance PI TI DT TI .
This is the design of 1980s ethylene plants. It works. . minimizes reflux. but ignores the composition balance.Energy Balance A third variation of the Energy Balance Control Scheme is the Ratio Energy Balance.
Energy Balance PI TI DT TI .
composition in equals composition out. Composition In = Composition Out + Accumulation . For distillation towers the composition balance is.Composition Balance All vessels will eventually reach a composition balance.
Tower Bottoms Reservoir. .Composition Balance For the Propylene Tower a propylene balance can be developed. The propylene in the feed must equal the propylene that leaves the tower plus the accumulation of propylene in the tower. Sources of accumulation include. Overhead Receiver and level of hydrocarbons on the trays.
the level on the trays. is much more difficult to quantify.Composition Balance Two of the accumulations are straightforward. The third accumulation. . the Overhead Receiver and the Bottoms Reservoir. It is again the largest accumulation in the tower.
Composition Balance In the 1970s analyzers were becoming reliable and control schemes that utilized them became common. . A composition balance could be maintained by utilizing the mass flows and the analyzer results leading to better distillation control.
.Composition Balance The tower feed and composition are analyzed and used as a feed forward control for the product. The product rate and composition are analyzed and used as a feed back control. The sum of these two is used to balance the tower considering all three balances.
Composition Balance PI AI AI .
Foaming Entrainment Weeping / Dumping Flooding .Tower Problem Solving 1. 2. 3. 4.
Tower Problem Solving Do simple checks first. 1. Calculate column pressure drop and then measure pressure drop. Survey column temperature profile. 3. . 2. Ensure that levels are accurate. Review survey temperature reading to operation’s readings.
2. Have engineers simulate these results.Tower Problem Solving Verify Tower Operations. If no problems are identified consider scanning the column. 4. Calculate mass balance to within 2% accuracy. if not calibrate flow meters. 3. 1. . Survey heating and cooling temperatures. Sample Feeds and Products.
The first is normally obvious. . the over head receiver. the second is the bottom section of the tower. This internal surge drum creates an inventory to act as a buffer.Tower Problem Solving In distillation towers there are actually two accumulators. These accumulators are used to stabilize the operation of the tower and down stream operations.
which is not a true indication of the condition of the liquid within the tower. or feed inlet. The sight glass and level instrumentation contain non aerated liquid. . There is an inherent error built into sight glass and level instrumentation.Tower Problem Solving If this internal level is allowed to rise above the reboiler return. stripping inlet. flooding can occur. called clear liquid.
the tower level will be higher than the instrumentation indicates. entrained liquid can be carried to the next stage causing flooding. Because the aerated level will have lower specific gravity than the clear liquid within the instrumentation. a clear liquid level below the aerated liquid level. If the level in the tower is higher than the feed or reboiler return. .Tower Problem Solving The liquid within the tower will have two levels.
5. 2. 4. 3. Fouling.Tower Incidents Attached is a list of tower incidents that was found in the literature from HZ Kister “ Recent Trends in Distillation Tower Malfunctions” 1. plugging and Coking issues Tower Bottoms and Reboiler Return issues Packing Liquid Distributors issue Intermediate Draws Assembly Mishaps .
B.Tower Incidents 1. corrosion products Solids in feeds . D. Fouling. C.salts Scale. plugging and Coking issues A. Coking Precipitation .
plugging and Coking issues location A. E. C. D. B. Packing beds and Distributors Trays. Fouling. active areas and down comers Draw lines Instrument lines Feed lines .Tower Incidents 1.
B.Tower Incidents 2. D. High liquid levels Impingement by vapor inlets Vapor Mal-distribution Water induced pressure surges Leaking reboiler draw Gas entrainment in liquid bottoms . Tower Bottoms and Reboiler Return issues A. C. E. F.
G. F. D.Tower Incidents 3. C. E. Distributor Overflow Plugging Fabrication mishaps Feed entry problems Damage Poor hole pattern Poor irrigation quality . Packing Liquid Distributors issues A. B.
Tower Incidents 4. Leakage at draw Restriction of vapor . C. B. Intermediate Draws A.choking of draw line Plugging .
Product recovery and purity can be improved by understanding the principles of distillation. It is energy intensive and has opportunities to be optimized. . These principles need to be understood in advance of operating and trouble shooting a distillation column for the operator or problem solving to be effective.Conclusions Distillation is one of the major unit operations in processing plants.
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