School of Life Sciences & Chemical Technology

Diploma in Chemical & Biomolecular Engineering

Distillation Column
CBE Laboratory Module 3.1

Group D Tan Weili Tan Wen Guang Benjamin Tia Esmeralda Daniel Yu Shenghe Joshua Zulkifli Ali Amdan 03/05/11

S10075769H S10076805D S10077174H S10079152B S10076705C

Summary

The aim of this experiment is to determine the pressure drop, the boil-up rate, the purity and to observe the different degrees of foaming at different three power levels; 0.4kW, 0.6kW, 0.8kW in a distillation column. Temperatures at T2, T4, T6, and T8 are also taken to show the temperature difference throughout the column for a mixture of 20 vol% pure methanol and 80 vol% water. Four relationships are also observed and explained. Generally, as the pressure drop gets bigger, the boil-up rate increases. The purity remained the same for the first two boilup rates, at 95%, but changed at the third boil-up rate, at 89%. At the first boil-up rate when pressure was 29cmH2O, the degree of forming was gentle and localised to one stage of the column. At the second boil-up rate when pressure drop was 40cmH2O, the degree of foaming was still gentle but was spread out throughout the column. At the final boil-up rate when pressure drop was 76cmH2O, the degree of foaming had changed to being violent, but back to localise to only a single stage in the column. One glaring error in this experiment is the first boilup rate reading. A reason for this error is that small amounts of liquid built-up were taken into account, resulting into a wrong reading. This error was rectified in subsequent readings.

Introduction
Distillation is defined as a process where a liquid or vapour mixture is separated into its components through the adding and removing of heat to achieve a desired purity. It is based on the differences in boiling points between the since the more volatile liquid will be boiled off first, then condensed to achieve a higher purity. Distillation columns are designed to ensure that the separation is done efficiently. However, this process requires tremendous amounts of energy on both heating and cooling, and can contribute more than 50% of the operating costs in a plant. In the chemical industry, distillation is a very common method of separation since it can separate large quantities of mixtures. There two types of distillation the industry uses; continuous distillation and batch distillation. Batch distillation is more commonly used when small quantities of liquids need to be separated, like in the experiment.

Approach
10 litres of a mixture of 20 vol% pure methanol and 80 vol% water was prepared. This is transferred into the reboiler. There is a heating element in the reboiler that was used to heat up the mixture at three different powers; 0.4kW, 0.6kW and 0.8kW. The reboiler was set to the highest power setting first to allow the system to get heated up quickly, and then reduced to 0.4kW. The system is then allowed to achieve steady-state before readings are taken. For each power setting, four sets of temperature readings, the degree of foaming, pressure drop, boil-up rate and purity was taken.

Results and Analysis

Power(kW)

Temperature (oC) T2 T4 T6 T8

0.4 0.6 0.8

66 72 79

68 75 82

73 81 86

79 84 87

Degree of Foaming (Gentle/Violent; Spread out/ Localised) Gentle; Localised Gentle; Spread out Violent; Localised

Pressure Drop (cmH2O) 29 40 76

Boil-Up Rate (ml/s) 0.627 0.138 0.225

Purity (%) 95 95 89

From the results obtained, it is clear that the power supplied has affected, directly or indirectly, every result. As power increases, the temperature readings throughout the column get higher since more hot vapour rise through the column. Power also has a direct effect on boil-up rate since the more power supplied, the faster the liquid will reach boiling temperature for the methanol and the faster methanol and water will be boiled off. There is a slight error in the first boil-up rate. 5.50ml of liquid is collected in 8.77s when power was at 0.4kW, in contrast with the other readings when the powers of 0.6kW and 0.8kW collected 2.75ml and 4.50ml of liquid in 20.0s respectively. A possible reason for this error is that a small amount of liquid built-up was collected as well as the sample, leading to the inaccuracy. Theoretically, the boil-up rate is proportional to the pressure drop. When the boil-up rate is low, the pressure drop is small and the same is applied when both parameters are big. This is because as more liquid is boiled off, more vapour is formed and travels up the column. However, due to trays preventing the vapour from moving up except via small holes in the trays, the pressure below increases greatly while the pressure in the upper part of the column stays the same or increases slightly. Foaming refers to when the liquid, usually reflux liquid, expands due to vapour or gas passing through it. It occurs when agitation is caused by the pressure difference in the column as fast, pressurised vapour is trying to get through the orifices. The bigger the pressure drop, the more violent the foaming. Also, whether foaming is localised or spread out depends on the density of the vapour.

Discussion
From the results, ignoring the error for the first value, the trend observed is that as the difference in pressure increases, the boil-up rate increases. Pressure can be defined as the amount of air molecules pushing down on the liquid and it suggests that the boil-up rate would slow down as the more energy is given to the mixture. When there is no liquid in the column, the trays of the column already provide intrinsic pressure and can be related to the equation:

hd=0.186Co2vlvhole2
The equation shows that the pressure difference depends on the differences in density between the vapour and liquid phases as well as velocity of vapour at the orifices.

From the graph, it can be seen that purity is affected by boil-up rate. Although purity is only affected by temperature, the graph shows differently. Methanol vaporizes at 650C and water at 1000C. Therefore, if the temperature of the distillation column is below the boiling point of water and above 650C, methanol will be able to vaporise and water will stay at liquid state, thus pure methanol will be obtained. However, from the graph, it is evident that purity is affected by boil-up rate. Some reasons for this difference in results may be: Water evaporates below boiling point therefore some water may have evaporated, affecting the concentration of methanol in top product receiver, thus explaining the differences in levels of purity. Some mixtures have boiling points that are really close, therefore increasing the difficulty for the mixture to me separated. Methanol and water have a difference of 350C in boiling points so as heat in the reboiler increases, so does the boil-up rate and this will definitely affect the purity of methanol in the top product receiver as some water might have vaporized and affected the purity. As the power supplied was increased to 0.8kW, it had been some time since the start of the experiment and therefore most the methanol in the reboiler might have been vaporized already causing the concentration to decrease. From the results, (ignoring the error of the first reading) as the boil up rate increases, the foaming will spread out and eventually become localize again. Foaming happens when there is expansion in the liquid which is due to the passage of the vapour. At 0.4 kW, the boil-up rate is assumed to be much lower than 0.627ml/s had gentle, localised foaming. At 0.6 kW, the boil-up was 0.138ml/s, and the foaming was still gentle but spread out. This is due to the decreasing density of the vapour that allows the vapour to flow faster hence forming a spread out formation. Eventually the density of the vapour will increase the vapour settles down and becomes denser which causes the foaming to be localised again. From the results, as pressure drop increases, the foaming gets more violent. Foaming occurs when there is agitation which is caused by the difference in pressure which also will increase the vapour velocity, forcing the vapour through the orifice trays. Therefore, the increment in the pressure drop foaming will become more violent. A variety of experimental errors occurred during this experiment. An inconsistent flow rate and error in determining when the system has reached steady-state as well as previous fluid built-up were the errors encountered. An inconsistent flow is troublesome in that it makes it harder to determine when steady-state has been reached. To solve this problem, adjust the valve controlling the tank or inlet pipe accordingly. Determining steady-state in this experiment is a problem because in is a batch process, and thus cannot perfectly be in steady state. To overcome this problem, when most parameters stabilise for about a minute, that is when readings should be taken. Previous fluid built-up from previous experiments as well as just before taking samples is a problem since it affects the purity of the sample taken. To overcome this problem, ensure that before running the experiment and before taking a sample, make sure the sample collection area is has been drained.

Conclusion

In conclusion, the higher the pressure drop, the more the boil-up rate as seen in the experiment. This is due to the differences in densities between the vapour and liquid phases and velocities of the of the vapour as it passes through the orifices of the trays. Although purity should only be affected by temperature, it is affected by boil-up rate. It could happen due to a variety of reasons, such as water evaporating and contaminating the sample. Boil-up rate affects foaming because of the passage of condensate liquid through vapour and their respective densities. A gentle and localised foaming suggests a low boil-up rate, while a violent, spread out foaming suggests a high boil-up rate.

References

http://lorien.ncl.ac.uk/ming/distil/distil0.htm http://en.wikipedia.org/wiki/Continuous_distillation http://ocw.korea.edu/ocw/college-of-engineering/process-control/lecture-notes-1/l7-dynrespii.pdf http://www.cheresources.com/invision/topic/3137-foaming-vs-pressure-drop/ http://www.cbu.edu/~rprice/lectures/distill7.html