MT-304 Gas-Liquid Absorption

Batch-A2 Rig 2.
09002058 Rohit Geesa 09011045 Shivi Jain 09D02032 Vivek Pandey

Date of Experiment: 14-02-2011 Date of Submission: 17-02-2011

AIM:
To study the reaction of carbon dioxide with the hydroxide solution in the Absorption Column.

MOTIVATION:
The absorption of a gas into a liquid is one of the fundamental processes of industrial chemistry. It makes it possible to separate one or more components of a gaseous mixture and to produce a liquid containing a desired quantity of a gas. Absorption is a powerful tool for the gas separation and purification. The chemical reaction brings two benefits for absorption. One is the increase of carrying capacity for gas components. Another is the reduction of mass transfer resistance or increase of mass transfer coefficient. Both factors contribute to the increase of absorption rate.

THEORY:
The following reaction takes place in the set up: Gas containing and air, is passed through the packed column from the bottom. The packed column is packed with Raschig rings. A solution of known concentration (1.43N) of NaOH is passed from the top. As it trickles down the column, it comes in contact with the rising gas mixture, and is absorbed into the liquid with the above reaction. NaOH is passed in excess of the theoretical requirement for the column. The gas is then passed through a column of standing liquid in the bubbling pot. As it bubbles through the liquid, more is absorbed into the liquid. When samples are titrated with 0.1N HCl solution prepared, two end points are obtained, one with Phenolphthalein, and another with Methyl Orange. Phenolphthalein gives the first end point, with the following reactions taking place: Methyl Orange gives the second end point which is due to an additional reaction: Using reverse titration technique, amount of dissolved in the solution can be calculated and a comparison can be made between the packed column and the Bubbling Column Yields.

Experimental procedure :

Add 1500gm of solid NaOH to 25 Litres of water and prepare a 1.5N solution of NaOH.

Flow rate of NaOH solution is set to 10lph in the adsorption tower. Fill bubbling pot with the same solution of NaOH.

Set flow rate of air to 30 lph and 2 to 70lph for first set of readings and then 90lph for the second set of readings.

NaOH solution prepared is first titrated with the HCl solution to check its normality.

Samples required for the two endpoint titrations are withdrawn from the bubbling pot outlet and the packed column outlet. This is done at regular intervals of 10,20 and 30 minutes for both the flow rates of 2.

Observations :
normality of NaoH from titration = 1.48 N HCl conc. = 0.1 N liquid flow rate (NaoH) = 10 l/hr air flow rate = 30 l/hr CO2 flow rate = 70 l/hr Absorption Column Time (min.) NaOH 1st end point (ml) NaOH 2nd end point (ml) Deviation (ml) Bubble Column Time (min.) 10 20 30 NaOH 1st end point (ml) 14.6 14.8 14.1 NaOH 2nd end point (ml) 0.9 0.6 0.5 Deviation (ml) -13.7 -14.2 -13.6 Table 1 : Table shows the calculated values for the Absorption column and the Bubble Column for 70 L/hr flow rate Absorption Column Time (min.) N2 (mol/l) NaOH Reacted (mol/hr) CO2 fed (mol/hr) CO2 reacted (mol/hr) Yield of CO2 (%) 10 1.32 1.8 3.125 0.9 25.60 20 1.2 3 3.125 1.5 44.80 30 1.28 2.2 3.125 1.1 32.00 Bubble Column Time (min.) 10 20 30 Table 2. .In this table, the amount of CO2 which reacted was calculated based on the titrations done, and the amount of CO2 present instantaneously and over a cumulative timeframe was calculated. Shown below is a table which highlights the values of instantaneous and cumulative yield for the absorption column. For the bubble column, a similar analysis was carried out. For cumulative calculations, an average value between the two data points was used to give us a more realistic picture of the true nature of the yield. The table below shows the data obtained for the bubble column for the given flow rate. N2 (mol/l) 1.37 1.42 1.36 NaOH Reacted (mol) 0.39 0.24 0.42 CO2 fed (mol/hr) 2.225 1.625 2.025 CO2 reacted (mol/hr) 1.17 0.72 1.26 Yield of CO2 (%) 42.58 31.31 50.82 10 14.3 1.1 -13.2 20 13.7 1.7 -12 30 14.4 1.6 -12.8

Co2 flow rate = 90 lph Absorption Column Time (min.) NaOH 1st end point (ml) NaOH 2nd end point (ml) Deviation (ml) Bubble Column Time (min.) 10 20 30 NaOH 1st end point (ml) 13.2 13.2 14.5 NaOH 2nd end point (ml) 0.4 0.6 0.8 Deviation (ml) -12.8 12.6 13.7 Table 3 : Table shows the calculated values for the Absorption column and the Bubble Column for 90 L/hr flow rate. Absorption Column Time (min.) NaOH 1st end point (ml) NaOH 2nd end point (ml) Deviation (ml) Bubble Column Time (min.) NaOH 1st end point (ml) NaOH 2nd end point (ml) Deviation (ml) 10 13.2 13.6 0.4 20 13.2 13.8 0.6 30 14.5 15.3 0.8 10 14.5 16 1.5 20 14.6 16.2 1.6 30 14.7 16.3 1.6 10 14.5 1.5 -13 20 14.6 1.6 -13 30 14.7 1.5 -13.2

Time (min.)

Absorption Column N2 (mol/l) NaOH Reacted (mol/hr) CO2 fed (mol/hr) CO2 reacted (mol/hr) Yield of CO2 (%) 10 1.3 2.00 4.02 1 22.5 20 1.3 2.00 4.02 1 22.5 30 1.31 1.90 4.02 0.95 20.0

Bubble Column Time (min.) 10 20 30 N2 (mol/l) 1.28 1.26 1.37 NaOH Reacted (mol) 0.66 0.72 0.39 CO2 fed (mol/hr) 3.02 3.02 3.07 CO2 reacted (mol/hr) 1.98 1.08 0.39 Yield of CO2 (%) 56.25 76.15 33

In order to better understand the trends observed both with respect to the behaviour of the two columns with time, and the behaviour of the two columns with respect to increasing flow rate, a graph was plotted and the graph plotted is shown below. A) Absorption Column A graph showing Instantaneous yield for both flow rate.
60.00 50.00 40.00 30.00 20.00 10.00 0.00 10min 20 min 30 min absorption column 90 lit absorption column 70lit

A graph showing cumulative yield for both flow rate from table 3 [appendix]
45.00 40.00 35.00 30.00 25.00 20.00 15.00 10.00 5.00 0.00 10min 20 min 30 min

absorption column 90 lit absorption column 70 lit

B) Bubble Column A graph showing Instantaneous yield for both flow rate.

70.00 60.00 50.00 40.00 30.00 20.00 10.00 0.00 10min 20 min 30 min bubble column 90 lit bubble column 70lit

A graph of instantaneous yield versus time was also plotted and the variations seen are shown in the figure given above. A graph showing cumulative yield for both flow rate from table 3 [appendix] .
70.00 60.00 50.00 40.00 30.00 20.00 10.00 0.00 10min 20 min 30 min bubble column 90 lit bubble column 70lit

A graph of cumulative yield versus time was plotted and the variations seen are shown in the figure given above.

SAMPLE CALCULATIONS
Flow rate of Carbon Dioxide = 70 L /Hr

For sample collected from absorption column after 10 mins: Volume of HCl (V1) = Burette Reading of phenolphthalein Deviation = 14.3 1.1 = 13.2 ml NaOH concentration used in titration (N2)= N1 * V1/V2*10 =0.1*13.2*10/10 = 1.32 mol/lit Balance on hydroxide solution Moles of NaOH reacted = (nNaOH Inlet nNaOH outlet) x flow rate of NaOH = (1.5-1.32)*10 = 1.6 mol/hr As per the reaction one mole of CO2 reacts with two mole of NaOH. So, Moles of CO2 absorbed in the column = nNaOH/2 = 0.8 mol/hr Molar flow rate of CO2 = 70Lit/hr/22.4 = 3.125 mol/hr Yield of reaction: Yield = moles of CO2 absorbed / moles of CO2 fed*100 = (0.80/3.125)*100 = 25.60 %

For sample collected from bubbling pot After 10 mins: Volume of HCl (V1) = Burette Reading of phenolphthalein Deviation = 14.6 0.9 = 13.7 ml NaOH concentration used in titration=N1 * V1/V2 = 0.1*13.7*10/10 = 1.37 mol/lit Balance on hydroxide solution (Moles of NaOH t=0 moles of NaOH t) x volume = nNaOH reacted = (1.48-1.37)*3 = 0.33 moles Moles of CO2 reacted = (moles of NaOH reacted*60/10)/2 = 0.33/2 = 0.99 moles/HR Final balance on CO2 Moles of CO2 fed to bubbling pot = moles of CO2 in column outlet. = moles of CO2 in column inlet moles of CO2 reacted in column = 3.125 0.8 = 2.325 mol/hr Yield of reaction: Yield = moles of CO2 absorbed / moles of CO2 fed = (0.99/2.325)*100 = 42.58 %

CONCLUSION AND DISCUSSIONS :

SOURCES OF ERROR:
1) Error in preparing 0.1N HCl can lead to erroneous results because all calculations are done with concentration of HCl as 0.1N. In our experiment, the normality of HCl was found out to be less than 0.1N, so we adjusted it taking concentration of NaOH to be 1.48N rather than 1.5N. 2) Least count of the beakers used for making the titre solutions were 10 ml, thereby introducing significant errors in making samples of the appropriate concentration. 3) Flow rate of the gas was constantly fluctuating, leading to irregular absorption 4) NaOH is measured using a simple analytical balance and there is a source of error in the measurement in its weight during preparation of 1.5N NaOH solution. 5) We may have stopped the titration at different colour density occurred during the titration.