CHAPTER ONE 1.0 INTRODUCTION Absorption is a mass transfer process in which a vapour solute in a gas mixture is dissolved into a liquid phase which the solute is more or less soluble. An example of absorption is absorption of the solute ammonia from an air- ammonia mixture by water. Absorption, in common with distillation, usually use special equipment for bringing gas and liquid phases into intimate contact. The gas absorption unit in this experiment is meant to demonstrate the absorption of CO2 into water in a packed column. The gas and liquid normally flow counter-currently, and the packing serve to provide the contacting and development of interfacial surface through which mass transfer takes place. The gas absorption is also designed to operate at atmospheric pressure in a continuous operation. A common apparatus used in gas absorption and certain other operations is the packed tower. The device consists of a tower, equipped with a gas inlet and distributing space at the bottom; a liquid inlet and distributor at the top; gas and liquid outlet at the top and bottom, respectively; and a supported mass of inert solid shapes, called tower packing. There are many types of random packing available, for example Ceramic Ball saddle and the most common is the Raschig ring. These packing are used to increase the surface area of contact between the gas and the liquid absorbent. In a packed tower, there is a limit to the rate of gas flow which is called as flooding velocity. The tower cannot operate if it exceeds this limit. At loading point, which is the point in which the droplets of liquid are carried up with the gas in packed column, the gas start to prevent the liquid from flowing down, and thus, pools of liquid start to appear in the packing. Fig 1.1 Diagram of a Gas Absorption Column Page | 1 1.1 AIMS & OBJECTIVES To calculate the rate of absorption of carbon dioxide into water from analysis of liquid solutions flowing down absorption column. 1.2 SIGNIFICANCE/IMPORTANCE OF GAS ABSORPTION COLUMN To remove contaminants from gas streams. It aims at separation of acidic impurities from mixed gas streams. 1.3 LIMITATIONS OF GAS ABSORPTION COLUMN We assume every other component in air is non-reactive. We assume they non-volatile (it does not evaporates quickly). Page | 2 CHAPTER TWO 2.0 BACKGROUND THEORY Gas absorption is mass transfer operation where one or more species is removed from a gaseous stream by dissolution in a liquid. The component that is extracted from the gaseous stream is known as solute and the component that extracting the solute is known as solvent. Carrier gas is the insoluble component present in the gas that is not absorbed by the solvent. The transfer is based on the preferential solubility of solutes in the solvent (Gas Absorption and Desorption, n.d.). Packed towers are used for continuous counter-current contacting of gas and liquid in absorption (Geankoplis, 1993).The mechanism in packed tower is the gas and liquid phase flows counter – currently where they interact on the packings interface. The liquid flows in downward direction, over the surface of the packing, whereas the gas flows through the space or voids of the packings in upward direction. The gas flow is driven by pressure while the liquid flow is driven by the gravity force. The gas undergoes pressure drop due to the liquid occupied some part of the open space and voids of the packing. Thus, reducing the area available for the gas to flow. If the packing is dry with no liquid feed, then maximum flow gas is available. The pressure drop increases as the liquid flow rate into the tower increases. High flux will resulting in flooding. This occurrence happen at the upper limit of the gas flow rate called flooding velocity since the liquid is blown out with the gas at the flooding point. The gas start to hinder the liquid flow at loading point where accumulation of liquid start appearing in the packing. Low flux will resulting in channelling or weeping, There are two types of packings types which is random and structured. Fig 2.1 Typical Packed Tower Packings: (a) Raschig ring, (b) Lessing ring, (c) Berl Saddle, (d) Pall Ring (Geankoplis C. J., 1993) One of the oldest specially manufactured types of random packings are Raschig rings and still in general use. (Separation Columns (Distillation, Absorption and Extraction)) They provide a large surface area within the volume of the column for the interaction between liquid and gas. They also enhance the contact time between liquid and gas. (iitb.vlab.co.in, 2011). Page | 3 Fig 2.2 Generalized Correlation for Pressure Drop in Packed Columns (Eckert, Chem. Eng. Prog., 66(3), 39 (1970) y-axis = x-axis = 𝑮𝟐𝒚 𝑭𝒑 𝑽𝟎.𝟏 𝒙 𝒈𝒄 (𝝆𝒙 −𝝆𝒚 )𝝆𝒚 𝑮𝒙 𝑮𝒚 √𝝆 𝝆𝒚 𝒙 −𝝆𝒚 Where, 2 Gy = Gas Mass Velocity, kg/m s 2 Gx = Liquid Mass Velocity, kg/m s 3 𝜌𝑦 = Density of Gas, kg/m 3 𝜌𝑥 = Density of Liquid, kg/m -1 Fp = Packing Factor, m 2 Vx = Kinematic Viscosity, m /s gC = Gravitational Constant, In the packed column, the gas and liquid streams are counter-currently run, with liquid running down between the packings and gas flowing up through the wetted packings, making contact with the liquid along the way. The gas contains the solute, the component to be absorbed by the liquid, the absorbent. One phenomena that may occur in tall towers is called channelling, in which liquid flows down closer to the walls and gas flows up through Page | 4 the centre. This reduces the efficiency of mass transfer because there is less contact between the two phases, (Seader 209). Under the assumptions that diffusion controls the mass transfer and that there is no resistance to diffusion across the liquid-gas interface, the two-resistance theory describes how mass transfer occurs in the column. The transfer of CO2 to water occurs in three steps: 1) from air to the air-water interfacial surface, 2) across the interfacial surface into the liquid phase, and finally 3) into the bulk liquid phase. As mentioned, the optimal operating conditions for the tower had to be determined before the absorption of CO2 could be studied. To do this, the loading zone had to be found. The loading zone is the region between the loading and flooding points. As water flows down a column, at a certain air flow rate, water will begin to accumulate in the packings. This is called the loading point. As air velocity is increased, more water will be accumulated. At the flooding point, the air velocity will be high enough such that entire liquid is entrained, causing the whole column to be filled with water. Column operation in the loading zone is unstable, and thus it is recommended to operate at below the loading point in the preloading region. The two critical aforementioned points can be determined both physically and graphically. Physically, the loading point can be observed when surges of air can be seen moving up the column. The flooding point can be seen when water has been pushed out of the top of the column by the air. The mass transfer flux is proportional to the concentration difference, where k is called the mass transfer coefficient, A is the area of the interface, N1 is the flux at the interface, Cli and Ci are the concentration at the interface and the bulk solution, respectively. N1=(𝐶li−𝐶1) Page | 5 CHAPTER THREE 3.0 DESCRIPTION OF APPARATUS Figure 3.1 Gas Absorption Column Machine: This is where the experiment is being carried out, It contains different parts such as the packed column, pressure gauge, valves and so on. Figure 3.2 Oilless Air Compressor: This was responsible for the pumping the CO2 from the cylinder is then pressurized within the compressor. Once the compressor completes the pressurization, it expels the gas (CO2) to the gas absorption column machine. Page | 6 Figure 3.3 Carbon dioxide Cylinder: This is responsible for storing the Carbon dioxide gas in a liquid and pressurised form in the cylinder. Figure 3.4 Stop Watch: To record the time and time interval taken during the experiment. Page | 7 Figure 3.5 Phenolphthalein: Acts as an indicator during titration. Figure 3.6 Conical Flask: This is where the titration takes place. Figure 3.7 Measuring Cylinder: This is used for measuring a certain volume of liquid. Page | 8 3.1 PROCEDURE Fill the liquid reservoir tank at the base of the column to approximately threequarter full with preferably deionized water. Note the volume added [22.5 liters]. With gas flow control valves C and C closed, start the liquid pump and adjust the water flow through the column to approx. 10 liters/minute on the flow meter F by adjusting flow control valve C. Start the compressor and adjust control valve C, to give an air flow of approx. 10% of full scale on flow meter F. Carefully open the pressure regulating valve on the carbon dioxide cylinder, and adjust valve C3 to give a valve on the flow meter F, approx. One half of the air flow F2. Ensure the liquid seal at the base of the absorption column is maintained by, if necessary adjustment of control valve C. After 5 minutes of steady operation, take samples at 5 minute intervals from S and S. Take 150ml samples at known times in each case. Analyze the samples according to the procedure detailed below. Withdraw a sample of liquid S5 from the sump tank with the sampler provided, approximate volume of 150ml, or from liquid outflow point S4. Discharge the sample at the base of a 100ml graduated cylinder, flicking the cylinder to throw off excess liquid above the 100ml mark. Add 5-10 drops of phenolphthalein indicator solution (a) above; if the sample turns red immediately, no free Co, is present. If the sample remains colourless, titrate with standard alkali solution (b) above. Stir gently with a glass rod until a definite pink colour persists for about 30 seconds. This colour change is the end point; Note the volume VB of alkali solution added. For best results, use a colour comparison standard, prepared by adding the identical volume of phenolphthalein solution (a) to 100ml of sodium bicarbonate solution (c) in a similar graduated cylinder. Page | 9 CHAPTER FOUR 4.0 EXPERIMENTAL RESULT/CALCULATION This are the data generated in a tabular form, calculation of result and discussion of result. TABLE 4.1 ParametersConcentration of NaOH = 0.0277 Volume of samples = 100ml VT (Volume of Water in System) = 22.5 litres F1 (Flow rate) = 10 litre/min Table of Raw Data Time from start (minutes) 5 10 15 From Sump Tank S5 (Corresponding to conditions at the top of the tower) VB(ml) 16.8 37.3 49.0 From liquid Outflow Point S4 (Corresponding to conditions at the bottom of the tower) VB(ml) 12.6 46.2 49.8 To obtain the different concentrations of carbon-dioxide dissolved in water from the amount of NaOH required to neutralize the water sample, the relation below is used – 𝑔𝑚𝑜𝑙𝑒 𝑉𝐵 × 0.0277 𝑜𝑓 𝑓𝑟𝑒𝑒 𝐶𝑂2 = = 𝐶𝑑 𝐿𝑖𝑡𝑟𝑒 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑖𝑛 𝑚𝑙 At 5 minutes from start, volume of base required to neutralize 100ml of water sample from the top of tower = 16.8ml, therefore 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 16.8×0.0277 100 = 4.65 × 10−3 𝑀 At 5 minutes from start, volume of base required to neutralize 100ml of water sample from the bottom of tower = 12.6ml, therefore 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 12.6×0.0277 100 = 3.49 × 10−3 𝑀 At 10 minutes from start, volume of base required to neutralize 100ml of water sample from the top of tower = 37.3ml, therefore Page | 10 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 37.3×0.0277 100 = 1.033 × 10−2 𝑀 At 10 minutes from start, volume of base required to neutralize 100ml of water sample from the bottom of tower = 46.2ml, therefore 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 46.2×0.0277 100 = 1.279 × 10−2 𝑀 At 15 minutes from start, volume of base required to neutralize 100ml of water sample from the top of tower = 49.0ml, therefore 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 49.0×0.0277 100 = 1.357 × 10−2 𝑀 At 15 minutes from start, volume of base required to neutralize 100ml of water sample from the bottom of tower = 49.8ml, therefore 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 = 49.8×0.0277 100 = 1.379 × 10−2 𝑀 TABLE 4.2 Completed Table of Results Time from start (minutes) 5 10 15 From Sump Tank S5 (Corresponding to conditions at the top of the tower) Cd in tank VB(ml) (gmol/Litre) (×10-2) 16.8 0.465 37.3 1.033 49.0 1.357 Average Rate of Absorption = Average Rate of Absorption = 𝐶𝑑𝑖 (𝑡=40)− 𝐶𝑑𝑖 (𝑡=10)×𝑉𝑇 From liquid Outflow Point S4 (Corresponding to conditions at the bottom of the tower) Cd at outlet VB(ml) (gmol/Litre) (×10-2) 12.6 0.349 46.2 1.280 49.8 1.379 𝑔. 𝑚𝑜𝑙𝑒/𝑠𝑒𝑐𝑜𝑛𝑑 30×60 0.01357(𝑡=15)− 0.00465(𝑡=5)×22.5 30×60 𝑔. 𝑚𝑜𝑙𝑒/𝑠𝑒𝑐𝑜𝑛𝑑 Average Rate of Absorption = 0.00000496 4.2 DISCUSSION OF RESULT It can also be seen from the results gotten, that the concentration of CO2 in water at the outflow point S4 increases as the volume VB increases. Also it can be seen from the results gotten the concentration of CO2 in water from the outflow point S4 is higher than the concentration of CO2 from Sump Tank S5 which is directly proportional to volume VB from Sump Tank and the absorption rate is gotten at a value of 0.00000496. Page | 11 CHAPTER FIVE 5.0 CONCLUSION Upon analysis of the experimental results it can be concluded that gotten the concentration of CO2 in water from the outflow point S4 is higher than the concentration of CO2 from Sump Tank S5 which is directly proportional to volume VB from Sump Tank. Gas absorption is a unit operation in which a soluble component is absorbed by contact with a liquid phase in which the component is soluble. In this experiment, water is used to remove carbon dioxide from air. The performance of packed gas-liquid absorption tower is evaluated to determine how the mass transfer rate is affected by gas flow rate, especially as the column approaches its loading and flooding points. From the data, it can be observed that if the volume of the standardized sodium hydroxide solution increases, the concentration increases, and also the rate of absorption increases. Also the aim of the experiment which is to calculate the rate of absorption of carbon dioxide into water from analysis of liquid solutions flowing down absorption column was achieved. 5.1 RECOMMENDATION Provision of a new and standard Gas Absorption Column as the one in the laboratory is not inline with the standard. Provision of standby generation in case of power supply failure. 5.2 REFERENCES Gas-absorption-pdf. https://pdfcoffee.com-gas-absorption-pdf.com Gas Absorption Colum-Mass Transfer Experiment. https://439341397-gas-absorption-column-mass-transfer-experiment-adocx.com POST LABORATORY ASSIGNMENT Question – Practical application(s) of Gas Absorption Column Answer(s) – Petroleum Industry Food Industries. Industrial waste treatment Metallurgical industry for extraction. Pharmaceutical industry for drug production. Page | 12