Memo 3 Cryogenic Air Separation Final Design

December 3, 1998
Carnegie Mellon University Chemical Engineering Department Group 5 Annie Devine Heide Eash Jennifer Moore

Abstract
A preliminary design for a cryogenic distillation plant was completed. The plant was to produce pure nitrogen for polymer applications. The system first compresses the inlet air isothermally to 1200 kPa using an oil-filled screw-type compressor (model GA90 from Atlas Copco). The feed then passes through a temperature swing adsorber (TSA) sieve to separate the water, oil, and carbon dioxide from the inlet air feed. It is necessary to remove these components because they will freeze at the operating conditions of the rest of the process, causing damage to the equipment. A multi-cell heat exchanger is used to cool the feed stream by cold process streams. The cold air stream (112 K, 1190 kPa) is then fed to the bottom of the distillation column, where it is separated into a pure nitrogen stream and an oxygen rich stream. The oxygen rich stream is used to provide cooling in the column condenser after being flashed adiabatically through a valve. This stream is then expanded through a turbine to produce electricity to reduce the utilities cost of the compresser. The product and waste streams act as the cold fluids in the main heat exchanger. A stream of 99% nitrogen with flow rate of 23.383 kgmol/hr (20230 SCFH) at 100 psig was produced. After all of the requirements were met for the process, a complete economic analysis was performed. The net present value of the plant was found to be $2.201 * 106 after taxes. The annual earnings was found to be $3.544 * 105 with a rate of return of 75.7%. A few ways to improve the economics of the design were discovered. The cost of the turbine in comparison to the utilities credit realized should be investigated. The column condenser is the most expensive piece of equipment in the process and ways to improve it should be investigated. The process is profitable and further development is recommended. However, the net present value is sensitive to the price of nitrogen and this market price should be monitored.

Table of Contents
Abstract Introduction Background Technical Discussion Basis of design Alternative processes Process description Figure 1: Qualitative version of flowsheet Assumptions and limitations Equipment design Economic Discussion Basic economics calculations Figure 2: Manufacturing capital breakdown Figure 3: Total capital investment breakdown Figure 4: Breakdown of annual manufacturing cost Table 1: Economic indicators for cryogenic process Sensitivity analysis Process Design Figure 6: Flowsheet with stream table Table 2: Mass and energy balance table Equipment specifications Economic Analysis Table 3: Table 4: Table 5: Table 6: 16 Capital investment Utilities summary Manufacturing cost Economic indicators 17 17 17 2 4 4 5

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Conclusions and Recommendations Acknowledgements References

Introduction
The Technology Division has requested a design and evaluation a nitrogen plant from the Chemicals Division. The nitrogen will be used by the Polymers Division for production applications. The plant will follow the recent industry trend of being on-site of the plant that it services. The economic advantage of building an on-site nitrogen plant becomes apparent when compared to the cost of shipping liquid nitrogen under high pressure in refrigerated tanks, which can be very expensive. An on-site is also more reliable than an offsite plant because our company will control its day-to-day operation. The polymer market is expected to grow significantly by the year 2005, so the calculations have been completed with 2005 as the target year to construct the plant. The Polymers Division has requested a dry nitrogen stream that is 99% pure, which is considered to be a moderately high purity in the air separation industry.

Background
Since nitrogen is a common gas used in many industrial processes because of its properties as an inert gas, it is necessary to produce pure nitrogen efficiently and inexpensively. Typical industrial uses of nitrogen are gas recovery and secondary oil recovery. In both recovery processes, the fluids, in this case nitrogen, are pumped into the contaminated soil to help remove the gas or oil. Because nitrogen is an inert there is not a concern about combustion once the fluid is introduced into the ground. This makes the process more environmentally sound.19 Nitrogen is also used for processes that require no oxygen in the system.2 Another application for nitrogen use is for purging or sweeping out machinery lines before repairs are made in many plants.14 Nitrogen is widely used in the polymer industry as an inert atmosphere in water and oxygen sensitive reactions. Free radical reactions, one of the most common ways to produce polymers such as ethylene, can be terminated by formation of oxygen free radicals. Reactions that rely on the Grignard mechanism for propagation are highly water sensitive. If Grignard reagents are exposed to water, an explosion can occur because the reaction is highly exothermic. Thus having a dry stream of pure nitrogen is important for blanketing polymer reactions. The most inexpensive process for producing nitrogen is air separation. There are three main types of air separation processes: cryogenic distillation, membrane separation, and pressure swing adsorption (PSA). Of these processes, the first one to be developed and put into industrial use was cryogenic distillation. Up until the late 1970s, this was the only process available to industries.12 Even then, the other types were not designed to produce enough nitrogen needed in most industrial processes. Therefore it was not a significant economic advantage for the manufacturers to switch from the cryogenic air separation to membrane separation or PSA. After the cryogenic process was in use a few years, advances were made in cost and energy efficiency. This was especially true after the energy crisis of the 1970s because the cost to build a cryogenic air separation system is very high. One company reduced the cost to build the system by about thirty-five percent and reduced the energy needed to operate the system by about twenty-five percent.12 The first cryogenic system that was placed into operation was the Linde single-column system in 1902. It is still considered to be the simplest type of cryogenic air separation system. As with most air separation systems, air is first brought into the system and compressed. Process streams are used to cool the incoming air. The air is further cooled by using it as the working hot fluid in the column reboiler. The advantage to this is that the air can be cooled at a lesser cost and the heat generated can be used to boil the liquid into the upward vapor instead of steam heat. After the air is cooled, it is mostly liquid and it is sent to the top of the column where it can pass through the plates. This process allows the liquid to be enriched with oxygen by the vapor phase, which captures the nitrogen and carries it to the top of the column. Both the oxygen and nitrogen streams are passed through the main heat exchanger where they are used to cool the incoming air.4

Even though the Linde single-column system is the simplest type of air separation, it does have several disadvantages. The first disadvantage is that in this process the desired product is usually pure oxygen. The second disadvantage is that part of the impurities contained within the nitrogen stream are oxygen, which means that a great deal of the oxygen produced is wasted in the nitrogen stream.4 Linde solved this problem in 1910 by designing a double-column system. In this system, the two columns are placed on top of one another. The boiling oxygen coming from the bottom of the first column can be used to condense the nitrogen at the top of the first column. The liquid nitrogen is then passed through the second column and sent through the system. Then as with the single-column design, the product streams are used to cool the incoming air.4 Many additions, changes and improvements to the cryogenic distillation process have been made since Linde set up the original design. One such change was to operate the single column under higher pressures than originally designed. This has been a common design since the 1960s for small to moderate plants, which have a pressure between six and ten bar. These processes use a waste expander cycle to save on operating costs. The waste stream is used to control the pressure of the nitrogen product. However, this process is inefficient because it can cause over refrigeration in the system. Also included in this double column design are two reboilers, designed as a solution to problems from the waste expander cycle.2 When dealing with a cryogenic air separation process, it is necessary to account for the water and hydrocarbons in the inlet air stream. If these compounds are allowed to remain in the process stream, they will freeze in the equipment and cause damage to the entire system. Therefore the air inlet stream must be prepurified before it enters the cryogenic system. The most common way to do this is to use a Temperature Swing Adsorber (TSA). The TSA has two beds of adsorbent that alternate to allow for regeneration of the bed.20 The most efficient sieves use a solid with a high surface area. The pores in the solid are used to adsorb the impurities. Different gases can be taken out based on their molecular size.18 Two types of adsorbents available to remove water and carbon dioxide are F-1 alumina and 13X zeolite molecular sieve, respectively. When designing a plant such as this one, it is necessary to look at the long run costs involved with running the plant for a period of time. This analysis includes estimates of economic outcome of the process using several economic indicators. In order to find this, the unit and installation costs must be compared to the operating and maintenance costs over the plants lifetime.5

Technical Discussion
Basis of Design
A request was made for the design of a nitrogen plant with the capacity to produce 20,000 SCFH of nitrogen at a minimum purity of 99 volume % inert. The available feedstock for this process is air at ambient conditions. Temperature: 100 F Pressure: 1 atm Composition: 78% nitrogen, 20.95% oxygen, 0.94% argon, 1% water, 0.035% carbon dioxide The available utilities include: 150 psig steam 600 psig steam Fuel oil Cooling water at 90 F Process water at 90 F Electricity Steam condensate

Alternatives considered
There are three main alternatives to purify nitrogen PSA, membrane separation, and cryogenic distillation. Cryogenic distillation is the oldest and most widely used method. It is the only one that will be considered here, because other groups in the Chemical Division are researching the more modern technologies of PSA and membrane separation. There are many small variations on the cryogenic distillation process, although in general the process is fairly uniform. Almost every process pretreats the air, cools it down and compresses it, distills it, and recycles streams from the distillation to cool other streams. The complexity increases as higher purity products are desired. This leads to greater equipment costs and potentially less profitable processes. As a process is designed, the product that is needed must be considered to have an economically viable process. Prepurification alternatives The first step is to remove from the air any components that could freeze in the rest of the cryogenic process. These compounds include water, carbon dioxide and hydrocarbons. Some processes include a knockout drum as an initial contaminant removal system. This is used to remove water and hydrocarbons so less adsorbent is needed. There are variations on how the adsorber is regenerated, but most include using a dry process waste stream to regenerate and having two beds with switching valves to ensure the continuity of the process. Distillation column alternatives The distillation column is absolutely necessary to the process, but the number of columns it is divided into is variable. In general, more columns produce higher purity nitrogen and oxygen streams. One of the most common schemes is the Linde process, which contains a two section column. Two sections are necessary if very high purity nitrogen is necessary.4 If a third section is added, the high pressure nitrogen in the top of the column can be recycled to decrease the load on the compressor at the beginning of the process. This third column also gives a slightly higher nitrogen recovery. Processes that wish to produce pure argon add a side-draw column. The nitrogen product that is drawn off can be removed as a liquid or vapor, depending on which side of the condenser it is taken from. If the product nitrogen is being supplied to a very sensitive on-site process a liquid nitrogen reservoir may be necessary. This reservoir would hold a quantity of liquid nitrogen that could supply the process for a few days until nitrogen could be ordered in. Energy recovery alternatives One of the ways to recover energy in the process is to expand one of the process fluids through a turbine. The standard way to do this, commonly called waste expansion, is to expand the oxygen enriched stream taken from the bottom of the column after it has passed through the condenser at the top of the column. Hybrid expansion is when both the feed and waste streams are expanded to produce energy. Energy costs are also lowered by using process streams to cool the feed stream. Depending on the complexity of the process, multiple heat exchangers may be used. In general, multi-cell heat exchangers are used in this process. Process streams can also be used as the working fluid in the condenser. They may or may not be recycled to the column after passing through the heat exchanger.

Process Description
Based on the specifications for the nitrogen supply, a single column distillation process was designed. The flow sheet shown in Figure 1 details this process. Pro/II was used to simulate the process. The feed to the system is ambient air at 310.93 K and 101.32 kPa. The feed is compressed, impurities are removed, and the clean feed is distilled to produced the required purity of nitrogen. The process streams are used to cool the inlet stream to cryogenic temperatures. The waste stream is first expanded through a turbine to recover energy for the process and is then used to regenerate the adsorber bed.

Figure 1: Qualitative description of cryogenic process The Peng-Robinson system was chosen for thermodynamic calculations because it was the closest system to the Gibbs-Duhem system requested. The option for decant water was turned off because there would be no water in the system after the temperature swing adsorber (TSA) had removed it from the air feed. A screw-type compressor (C1) was used to compress the air feed stream (S1). The pressure of the outlet stream (S2) of the compressor was set at 1200 kPa. The compressor contains an oil bath which removes the heat of compression, making it an isothermal process. The oil bath also introduces hydrocarbons to the air stream which are subsequently removed in the TSA bed. The TSA bed contains both alumina to remove water and a zeolite molecular sieve to remove carbon dioxide. The alumina is a product of Alcoa, product F-1, and the zeolite is a product of Union Carbide, product 13X. When the air stream (S3) leaves the TSA it is assumed to contain no water, carbon dioxide or hydrocarbons. After being cooled in the main heat exchanger (E1), the feed (S4) enters the distillation column (T1) at the bottom (tray 15). There is no reboiler in the column as the feed stream supplies the necessary vapor flow up the column. The column was specified to have 15 trays and that the vapor product from the condenser should be 20230 SCF/H (23.383 kgmol/hr) and contain 99% nitrogen. The pressure was set to operate at 1190 kPa. The product nitrogen (S11) exits the column as vapor from the condenser (E2). The oxygen-rich liquid stream (S5) from the bottom of the column provides the cooling for the condenser. The liquid bottom product (S6) was adiabatically flashed through a valve (V1) with a pressure drop of 900 kPa. On the flow sheet, this process was modeled by setting the duty in the simple heat exchanger (E2) equal to the duty in the column condenser. A four-cell heat exchanger was used to utilize the cold temperature of the product and waste streams. The cold streams in the main heat exchanger are the product nitrogen (S11) and the oxygen-rich waste stream (S7). The waste stream passes through this heat exchanger as a cold stream twice: once before (S7) and after (S9) it is expanded in the waste expansion cycle.

A waste expansion cycle is included in the process to make it more energy efficient. After the waste stream (S6) condenses the nitrogen product, it enters the main heat exchanger (S7) where it is warmed by the feed air (S8). The stream is then expanded in a turbine (EX1) to atmospheric pressure (S9). The work done by this turbine can be harnessed to provide energy to drive the compressor at the beginning of the process. The outlet oxygen-rich stream (S10) can then be used to regenerate the TSA membrane beds.

Assumptions, limitations, and errors

Certain assumptions had to be made in the design of this cryogenic air separation process in order to determine the final outcome. Errors can also be encountered when making assumptions. The first assumption made in this design was the thermodynamic model. Peng-Robinson was chosen because of the parameters it uses to calculate the values of certain equipment output such as the recoveries of compounds. If another thermodynamic model was chosen, then these values would be different. This would cause a change in the final economic outcome. Before the TSA was set up in the process design, it was necessary to determine the amount of water in the atmosphere. This was done by looking at a table that connected the relative humidity to the operating temperature. Since the relative humidity was determined to be high, the water content was also assumed to be on the high side of the possible range. Once this was determined to be one percent of the feed, the area needed for the TSA was calculated. Another assumption made for the TSA was that it perfectly separated from the feed stream all three impurities oil, water, and carbon dioxide. In reality, this would not happen because it is not feasible to obtain perfect separation and there will always be a small amount of impurities entering the system. These impurities could eventually cause damage to the column. Since this perfect separation was assumed, it was not necessary to take into consideration the wear on the equipment due to these impurities. One way to reduce the amount of impurities is to not use an oil-filled screw-type compressor. From the information gathered, it was apparent that most cryogenic air separation plants in operation today do not use such a compressor. They usually use an oil-free compressor16. These compressors are slightly more expensive than the oil-filled ones because not as much heat can be absorbed. This would change the final economic cost analysis. However, since the oil-filled screw-type compressor was part of the design requirements, it was applied to this design aspect of the process. The efficiency of the turbine was assumed to be eighty percent because this was a typical value used for calculations5. Since the efficiency depends on the particular turbine. In use, the actual efficiency was unknown. If the turbine efficiency were in fact lower than 80%, then more work for the compressor would have to be supplied by electrical power. The temperature at the outlet of the turbine would also be affected as a result of a change in efficiency. In order to find a definite estimate of how much electricity would be needed to run the compressor, the actual turbine efficiency would be needed. Pressure drop through different pieces of equipment can affect the results of a process. For this process, it was assumed that there was a 10 kPa pressure drop across each cell in the heat exchangers. A higher pressure drop would decrease the operating pressure in the column and therefore reduce the bottoms flow rate. Then working fluid in the condenser would have to do more work, which would be accomplished by increasing the pressure drop across valve V1. This would decrease the inlet pressure to the turbine and the work out of the waste expansion process. It was also assumed that there was no pressure drop across the column. If these pressure drops were changed, then the output of the equipment would change and thus change the economics of the plant. The limitation that affected the process the most was the minimum temperature difference necessary for heat transfer. This number was set at 5.5 K. If it was lower, more energy could have been recovered by the turbine because the condenser working fluid could have been flashed to a higher temperature and pressure. As is discussed in the next section, the minimum temperature approach determined many of the operating conditions.

Equipment design
The biggest constraints on the process were related to heat exchange. The minimum temperature difference for heat exchange was set at 5.5 K. A high flow rate for the bottom product of the distillation column was necessary to condense the tops product. The main variables that were adjusted include the outlet pressure of the compressor, the temperature of the column inlet stream, and the pressure drop across the valve that expands the waste before it condenses the top product. The main piece of equipment in the process is the distillation tower, which is what makes the separation possible. To design the tower, the number of trays was determined first. Trial and error simulation in Pro/II was found to be the easiest method to complete this task. Recovery of nitrogen was given as approximately 30% in much of the literature, so the process was simulated with different numbers of trays until that recovery was achieved. The number of trays was then set at 15. It was decided that there would be no pressure drop across the column. Next, the pressure in the column was determined. It was known that the working temperature would be around 110 K. The dew point pressure at that temperature was found through Pro/II calculations to be around 1200 kPa and this became the set point for trial and error simulations. An inlet temperature of 112K and pressure of 1190 kPa were found to give appropriate outlet temperatures from the column. The pressure is also high enough so that a significant pressure drop is possible across valve V1 to cool the waste stream enough that it can condense the product. The desired pressure drop across this valve will give a working fluid outlet temperature that is less than the condenser temperature by the set minimum temperature difference. But the fluid cannot simply be flashed to atmospheric pressure because then the turbine would not be able to expand the fluid at all. Thus energy recovery from waste expansion would not be possible. Trial and error simulation set the pressure drop at 900 kPa. The column condenser was designed by introducing another heat exchanger into the simulation and setting its duty equal to the duty of the column condenser. There is a 10 kPa pressure drop across the exchanger. The column condenser was set as a partial condenser, with the heat duty being the variable that was adjusted to achieve the required purity. The main multi-cell heat exchanger was designed by considering the temperature of the feed into the column and the minimum temperature difference possible across the exchanger. The feed stream is the hot stream. The product stream, condenser working fluid, and waste outlet serve as the cold streams. The outlet temperature of the hot stream was set at 112 K, which is at least 5.5 K warmer than the inlet temperatures of the cold streams. The outlet temperature of the product stream was set at 298 K, which was felt to be an appropriate delivery temperature. The outlet temperature of the stream which is fed to the turbine was set so that the final waste outlet temperature would not violate the minimum temperature difference. Each cell in the exchanger also has a 10 kPa pressure drop. The turbine was designed to drop the pressure of the waste stream to atmospheric pressure to extract as much energy from the process as possible. The adiabatic efficiency was set to 80%, an average value often used when equipment specifications are not available. Conveniently, the turbine also cools the stream further so it can be passed through the heat exchanger twice to aid in cooling the feed stream. The oil-filled screw-type compressor was chosen from models available from Atlas Copco. Model GA90 was chosen because it can handle the flow rate going through the system. The outlet pressure was calculated by adding any pressure drops the feed experienced to the working pressure of the column. This totaled 1200 kPa in the end. Because of this high working pressure, a second valve (V2) was added to the end of the system to drop the pressure of the product to the desired delivery condition, 100 psig.

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Finally, the temperature swing adsorber that pretreats the air was designed. The TSA unit was placed after the oil-filled screw-type compressor to remove any oil that was transferred to the air in the compressor. F-1 alumina was chosen to adsorb the water because it can be used at high pressures. 13X zeolite molecular sieve was chosen to remove the carbon dioxide. There are no real operating conditions to choose for the TSA. The sizing process is detailed in the economic section.

Economic Discussion
Basic economics calculations
The first step in determining the economic feasibility of the process is to size and cost the equipment. Standard design equations were used to size the heat exchangers and turbine. The distillation tower was sized using the Westerberg correlations and other empirical correlations found in the literature.5 The compressor was sized and a cost was found from information provided by the manufacturer.16 The Guthrie method was then used to cost each piece of equipment and the costs were updated to 2005 prices.13 Figure 2 shows the breakdown of the manufacturing capital costs. From this, it can be seen that the largest contribution to the manufacturing cost is the column condenser and the TSA purification system. Actual values can be found in Table 3. The column condenser is so large because of the low temperature driving force. Because the cost of the condenser could be reduced significantly if this driving force was increased, one area for further investigation is the further cooling stream that serves as the heat exchanger working (cold) fluid.

Ma nuf actu ng Ca l ri pita

CO LUMN CON DENSER TSA TURBIN E MA I HEAT EXCHANG ER N CO LUMN CO MPR ESSO R

Figure 2: Manufacturing capital breakdown The total manufacturing capital is the sum of the costs of the equipment plus a 25% contingency. The offsite utility investment is set at 40% of the manufacturing capital. The sum of these two values is the total fixed capital. The working capital necessary to run the plant is .194 times the fixed investment. Figure 3 compares these up-front costs.
Tota C apita vestment l lIn

Ma nufa in cturg Capit al Off it nve ent s e I stm Workin Capi g t al

Figure 3: Total capital investment breakdown

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Next the manufacturing costs were calculated. The only utility needed is the electricity to run the compressor. The electricity generated by the turbine leads to a utilities credit. The values can be found in Table 4. Only one worker is needed to run the plant, and her wages were given in the problem description. The problem description also gave the base cost of supervision, payroll maintenance, supplies and materials, taxes and insurance, SARE, and depreciation. Figure 4 compares these costs. From this chart, it can be seen that the major contributors to the annual manufacturing costs are wages and SARE costs. If one compares the credit given for energy recovered by the turbine, one sees that it is only about $3000/yr, one-tenth the electricity cost for the compressor, while the cost of the turbine is almost twice that of the compressor. Further analysis is warranted to investigate the effect of the removal of the turbine on the remaining equipment in the process, especially the main heat exchanger, and the economics of the design.

Tot AnnualMa nufa ur g Cost al ct in

W ages SARE Depre t n ciaio Payro ll Ut tie min ili ( us s cr s) edit Taxes, ns nce I ura O ns e Mainenance it t O th uppli a er S es nd M ate l ria s O ffs Mainenance it e t

Figure 4: Breakdown of annual manufacturing cost From all of these calculations the net present value, rate of return, and annual earnings of the project can be calculated. Straight line depreciation to zero salvage value was used. The project life and tax life were set at 12 years each. The minimum discounted cash flow (DCF) rate of return was given as 15%. The income tax rate was 32%. Table 1 summarizes these calculations. Details of the actual calculations can be found in Table 5. Table 1: Economic indicators for cryogenic process Indicator Value NPV $ 2.201 * 106 Rate of return 75.7 % Annual earnings $ 3.544 * 105 / yr

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Sensitivity analysis
A sensitivity analysis, shown in Figure 5, was performed to determine how several factors will affect the net present value of the process.

Sensiti An sis vity aly

10% i ease n D r e of etu ncr i CF at r rn 10% decr ease n DCF rae of et n i t r ur 10% icr e i I me Tax n eas n nco

Change

10% decre inIn ase come Tax 10% i ase in pic ofN2 ncre re 10% decr e i prce o N2 eas n i f 10% ncr e i wages i eas n 10% dec ase i wages re n no change

0. 00E+00

5. 00E+05

1. 00E+06

1.5 0E+06

2.0 0E+06

2. 50E+0 6

3. 00E+06

NetPre sentValu e

Figure 5: Sensitivity Analysis The bottom row of the chart reflects the net present value of the process described thus far. Wages are the most significant factor of the annual manufacturing costs besides SARE expenses which are dependent upon the price of N2. Compared to other factors considered, the cost of wages seem to have little overall effect on the net present value. The selling price of N2 appears to have the most significant impact on the net present value. This makes sense as the selling price is the only contributing factor to the overall revenues, whereas the wages are only a part of the total expenses. This would lead to the selling price having a greater overall impact over the cost of wages. Factors such as the DCF rate of return and the income tax rate seem to have relatively small effects on the net present value. It is interesting to note that the factors (rate of return, income tax, and wage rates) that will probably stay fairly constant when yearly inflation is taken into account have little effect on the net present value, while the price of N2, which is subject to the whims of supply and demand in the industrial chemicals market, may have a large effect.

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Process Design

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Table 2: Stream Data Table

Stream Name Stream Description Phase Vapor Mole Fraction Temperature Pressure Flowrate Composition NITROGEN OXYGEN AR WATER CO2 Stream Name Stream Description Phase Vapor Mole Fraction Temperature Pressure Flowrate Composition NITROGEN OXYGEN AR WATER CO2 Stream Name Stream Description Phase Vapor Mole Fraction Temperature Pressure Flowrate Composition NITROGEN OXYGEN AR WATER CO2 K KPA KG-MOL/HR K KPA KG-MOL/HR K KPA KG-MOL/HR S1 Feed Vapor S2 S3 S4 S5 TSA Feed Clean Feed T1 Feed Bottoms Mixed Vapor Vapor Liquid 1.000 0.999 1.000 1.000 0.000 319.261 1200.000 64.600 0.780 0.201 0.009 0.010 3.49E-04 319.261 1200.000 64.000 0.788 0.203 0.009 0.000 0.000 112.000 1190.000 64.000 0.788 0.203 0.009 0.000 0.000 110.474 1190.000 40.607 0.671 0.315 0.014 0.000 0.000

310.928 101.325 64.600 0.780 0.201 0.009 0.010 3.49E-04

S6 S7 S8 S9 S10 Cond feed Cond out Turb Feed Turb Out Waste Out Mixed Vapor Vapor Vapor Vapor 0.228 1.000 1.000 1.000 1.000 91.095 290.000 40.607 0.671 0.315 0.014 0.000 0.000 S11 Tops Vapor 101.317 280.000 40.607 0.671 0.315 0.014 0.000 0.000 130.000 270.000 40.607 0.671 0.315 0.014 0.000 0.000 103.819 101.325 40.607 0.671 0.315 0.014 0.000 0.000 304.290 91.325 40.607 0.671 0.315 0.014 0.000 0.000

S12 S13 HiP Product Product Vapor Vapor 1.000 1.000 1.000 298.000 1180.000 23.393 0.990 0.008 0.002 0.000 0.000 297.013 790.801 23.393 0.990 0.008 0.002 0.000 0.000

106.811 1190.000 23.393 0.990 0.008 0.002 0.000 0.000

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Equipment specifications
Unit C1 Description Oil-filled screw type compressor Specifications - Atlas Copco unit model GA90 - Power requirement 100 kW - Unit cost $33,500 - Outlet temperature is 10 F above ambient temperature - Introduces 2-4 ppm oil into air stream - Uses F-1 alumina to remove water, volume: 106.537 ft3 - Uses 13X zeolite sieve to remove carbon dioxide, volume: .958 ft3 - Vessel height: 9.75 ft - Vessel diameter: 3.747 ft - 4 cell heat exchanger - 1 hot cell, 3 cold cells - Outlet temperature set on three cells to appropriate values - Pressure drop of 10 kPa over each cell - Total volume: 2.334 m3 - Height: 14.4 m - Diameter: 0.227 m - Vessel is stainless steel - Contains 15 stainless steel sieve trays with 24 spacing between trays - Operating pressure: 1190 kPa - Floating head condenser (stainless steel) with heat exchange area of 24.1 m2 - Pressure drop of 10 kPa across exchanger - Pressure drop of 900 kPa - Design type: centrifugal/turbine - 80% efficiency for turbine and brake motor - Outlet pressure: 101.325 kPa - Brake horsepower: 13.561 hp - Drops pressure of product outlet to desired value of 100 psig

TSA

Temperature swing adsorber

E1

Main multi-cell heat exchanger

T1

Cryogenic distillation column

E2

Column condenser

V1 EX1

Waste valve Waste expansion turbine

V2

Product valve

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Economic Analysis
Table 3: Equipment capital cost Equipment Cost ($) Column condenser 74210 TSA 72330 Turbine 56000 Multi-cell heat exchanger 52450 Column 46308 Compressor 34358.97 Total 335657 Table 4: Utilities summary Equipment Cost ($) Compressor 39600 Turbine - credit 3203 credit Table 5: Manufacturing cost Item Cost ($) Wages 190100 SARE 118800 Depreciation 46990 Payroll 38010 Utilities (minus credits) 36397 Taxes, Insurance 17620 Onsite Maintenance 16784 Other Supplies and Materials 8391 Offsite Maintenance 3356 Table 6: Economic indicators Indicator Value NPV $ 2.201 * 106 Rate of return 75.7 % Annual earnings $ 3.544 * 105 / yr

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Conclusions and Recommendations

The proposed design is profitable and produces the amount of nitrogen required. The profit of the process is sensitive to the price of nitrogen, which should be monitored. The cost of the turbine vs. the energy credit of the expansion process should be investigated. Ways to increase the temperature driving force in the column condenser should be investigated to reduce costs. Other types of compressors that do not utilize oil should be investigated to eliminate hydrocarbon contaminants in the system.

Acknowledgements
We would like to thank Bud Kuhn of for all of the help he gave us with the oil-filled screw-type compressors. He helped us determine the specific model to use for our cryogenic system. Over the phone he answered many questions about installation and shipping. He also gave some insight to what actual cryogenic plants are using in industry today. We would also like to thank our fellow classmates for the assistance they provided in clearing up some facts about the project and giving pointers about Pro/II.

References
1. Acharya, D. , F. Fitch, and R. Jain, Some Issues in Operating Adsorption Prepurification Systems for Cryogenic Air Separation, Separation Science and Technology, v 31, n 16, pp. 2171-2182 (Sept. 1996). - Prepurification is discussed in this article. It also talks about the possible reasons for molecular sieve degradation. It helps the reader understand the importance of eliminating these degradations before the process is finalized. Agrawal, R., D. W. Woodward, W. T. Kleinberg, and K. B. Wilson, Efficient Processes to Produce Nitrogen by Cryogenic Air Separation, Proceedings of the Low Temperature Engineering and Cryogenics Conference 1990, pp. 338-343 (1990). - This design process involves a single cryogenic column, which includes a waste expander cycle. Some advantages and disadvantages are talked about and solutions to the disadvantages are also discussed. Alcoa, Choosing an Alcoa Activated Alumina Dessiccant Basics of Dehydration Design Barron, R., Cryogenic Systems, McGraw Hill, Inc., New York, pp. 230-239 (1966). - Two different column designs are discussed. Both were invented by Linde in the early 1900s. The first is the first cryogenic design ever put into effect, which is a single-column design. Biegler, L. T., I. E. Grossman, and A. W. Westerberg, Systematic Methods of Chemical Process Design, Prentice Hall, Inc., Upper Saddle River, New Jersey (1997). - This text was used for virtually every aspect of the project, including sizing and costing of equipment, mass and energy balances, and economic evaluation of process. Clarke, M. E. and J. B. Gardner, Refrigeration with Expansion Turbines, Contemporary Physics, v 17, n 6 , pp. 507-528 (Nov. 1976).

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- This article talks about expansion turbines used in refrigeration. It can be used to gain a better understanding of what a turbine is and how it works. 7. Compostion of Atmosphere Relative Abundance, available via http://www.c-fc.com/charts/atmosph.htm on the WWW. - This page was used to obtain the flow rates of water and carbon dioxide while sizing the TSA. Espie, D. M., J. A. Mandler, D. Miller, and D. OConnor, Dynamics and Control of Chemical Reactors, Distillation Columns, and Batch Process, v 2, Pergamon Press, Tarrytown, New York, pp. 193-199 (1993). - A brief description of a double-column. which produces pure nitrogen at less than 0.1 percent oxygen and impure nitrogen at less than 1 percent oxygen. A simplified flowsheet that explains the unique challenges of cryogenic distillation column control. GA90-315: Introduction Page, available via www.atlascopcocompressors.com/html/products/industry/oil_lubr/90_315/ga90_315.htm on the WWW. - This page introduced the advantages of the screw-type compressors and gave links to other pages that contained information helpful in determining what model number compressor to use.

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10. GA90-315: Rotary Screw Elements Design, available via http://www.atlascopcocompressors.com/html/products/industry/oil_lubr/90_315/rotary/rotary.htm on the WWW. - The main operations of the rotary compressors were shown here so that the mechanics behind it were apparent and understandable. 11. Glossary Wet-bulb temperature, available via http://www.bom.gov.au/climate/glossary/wetbulb.shtml on the WWW. - The definition of wet-bulb temperature was obtained from this page. It was needed for the TSA calculations. 12. Gottzman, C. F., and R. J. Selines, Industrial Gases for Process Metallurgy : Present and Future, 1990 Elliott Symposium Proceedings,, p. 497 (1990). - The basic design for a single-column with waste expander cycle is discussed. The possible recoveries of products are given in the article. - Used to determine the operating pressure of the distillation column and the recovery percentage of nitrogen product from the system. 13. Guthrie, K. M., Capital Cost Estimating, Chemical Engineering, pp. 122-129 (Mar. 24, 1969). - This article was used in conjunction with the section on Guthries method of sizing and costing in the course textbook. It provided detailed graphs for each component of the process and added information that was not part of the textbook. 14. Hardenburger, T., Producing Nitrogen at the Point of Use, Chemical Engineering, pp. 136-146 (Oct. 1992). - A discussion of the importance of nitrogen production and some uses for the gas are included in this article. It also talks about how onsite production is important. Some safety factors are discussed, which include a list of how high certain levels can become before an explosion will occur. 15. KOM-Plant (Oxygen/Nitrogen Gas Generating Plant) System Configuration, available via http://www.kobelco.co.jp/eneka/p11/gkome.htm on the WWW. - This web site consists of a current plant design that is in use. The company that designed this process offers it for sale to other industries. It consists of a double column design. 16. Kuhn, Bud, Atlas Copco, Saltsbug Rd., Pittsburgh, PA 15239, 412-795-6088.

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- Bud was able to give the data needed for the screw-type compressor, which included the unit cost, installation, power requirement, and shipping costs. He sent this information through email, fax and telephone conversations. 17. Michael, K. P., Industrial Gas : Surveying Onsite Supply Options, Chemical Engineering, p. 72 (Jan. 1997). - Cryogenic air separation is broken down into the basic parts. Therefore it makes it easier to understand when this type of system is looked at for the first time. It also talks about the requirements of common processes that are possible for cryogenic systems. - Used to determine the cryogenic temperature of air and the pressure of the initial compressor. 18. Perry, R. H., D. W. Green, and J. O. Maloney, Eds., Heat-transfer Equipment, Chapter 11, in Perrys Chemical Engineers Handbook, 7th ed., McGraw-Hill, New York, pp. 11-102-11-104 (1997). - It gives a general introduction of cryogenic air separation, which includes both of Lindes early designs. Air purification before it enters the system is also talked about. This includes a discussion of molecular sieves and the possible choices for the solid adsorbent. 19. U.S. Patent 4453957 Pahade, R. F., J. H. Ziemer, and H. Cheung, Double Column Multiple Condenser-Reboiler High Pressure Nitrogen Process. - The design of a plant that produces large quantities of nitrogen at high pressures. This is done with a double column design and several condenser-reboilers. The patent write up includes a detailed flowsheet of the process. 20. U.S. Patent 4464188 Agrawal, R. and T. E. Cormier, Process and Apparatus for the Separation of Air. - This includes the patent for a rectification column for cryogenic air separation, which has two nitrogen recycle streams and an additional air stream. All of these streams are used to reboil the column and save on energy costs. The nitrogen is also used for refrigeration. 21. U.S. Patent 5385024 Roberts, M.J. and H. Cheung, Cryogenic Rectification System with Improved Recovery. - This also includes the patent for a rectification system involving cryogenic separation. However, this plant design uses nonproduct streams, which are compressed and added to incoming feed. Then the mixture is passed through the system where it is used to allow for greater recovery of product. 22. Valenzuela, D. P., A. L. Myers, Chapter 2: Adsorption of Pure Gases, Adsorption Equilibrium Data Handbook, Prentice Hall, pp. 6-12,55-56 (1989). - This chapter was used in finding the amount of adsorbent needed in the TSA for the carbon dioxide and hydrocarbons in the system. 23. Wet Bulb Depression Table, available via http://nesen.unl.edu/stedii/Wetbulb.html on the WWW. - The wet-bulb depression table was used to determine relative humidity. This data was then used in the TSA calculations.