Experiment 1 SIEVE-PLATE DISTILLATION COLUMN

Shrankhla Narya 09001038 AIM: To find the number of theoretical stages in a Sieve Plate Distillation and calculate the overall
efficiency in a sieve plate distillation column.

APPARATUS:
Distillation Column with reboiler Automatic digital Refractometer Two fluids with different boiling point (i.e. Isopropanol and n-isopropanol) Beaker

PROCEDURE:
1. 2. 3. 4. Fill the distillation column with the two fluids- Propan-1-ol and Propan-2-ol Switch on the heater and set the temperature to around 135 C Allow the system to reach steady state Collect a few drops of distillate in a beaker and measure its refractive index using refractometer 5. Collect a few drops of residue in a beaker and measure its refractive index using refractometer 6. Repeat steps 4 and 5 every 15 minutes

THEORY:
Distillation is a method of separating the components of a solution which depends upon the distribution of the substances between a gas and a liquid phase. It is called as the workhorse of chemical industries. The basic requirement for separation is that the vapor phase composition has to be different from that of the composition of the liquid phase. Distillation mainly involves vapor liquid equilibrium. Vapors are formed in a reboiler and rise in the column. Feed is supplied in the middle, separating the column in enriching/rectifying section and stripping/exhausting section. The vapor is condensed at the top and is converted into liquid. The purpose of distillation is to get more volatile component at the top and less volatile component at the bottom. An intimate contact between the liquid and vapor phase occurs on a tray, facilitating rapid exchange of mass between them. Transport of more volatile component occurs from liquid to vapor phase while transport of less

volatile component occurs from vapor to liquid phase. Thus, distillation column involves counterdiffusion of components (not necessarily equimolar). A typical distillation column looks like this:

1. Enriching Section:
Vapor rising in the section above the feed is washed with the liquid that is being recycled. The liquid coming from the condenser is leaner, less volatile as compared to the vapor rising. This causes mass transfer of less volatile component from the vapor to the liquid phase and vapor phase becomes richer in more volatile component.

2. Stripping Section:
In the section below the feed, the liquid is being stripped off of more volatile component by the vapor produced at the bottom. Liquid (coming from feed + condenser) has more volatile component and hence is stripped off by the vapor. Thus liquid now will contain less volatile component in more quantity.

3. Feed Entry:
Generally, it is the feed entry point that divides the column into rectifying section and stripping section. Feed should be introduced at a plate where operating line for enriching section cuts the operating line of the stripping section because this results in a minimum number of trays. Feed should be added at a point where its addition does not make large changes in the concentration. It should be added at a point where streams concentration matches with the feed concentration.

4. Reflux:
After the vapor from top section is condensed, some of it is sent back to the column and the rest is obtained a distillate. Reflux is the most important variable that is responsible for the high purity of the product. Without reflux, there will be no enrichment of vapor for top

section and of liquid for bottom section. More the reflux more is the purity of the distillate obtained.

5. Reflux Ratio:
Reflux ratio is the ratio of the amount of the condensed vapor which is recycled back to the column to the amount of distillate withdrawn. The reflux ratio decides how far or close the operating line is from the equilibrium curve. As the reflux ratio increases, the operating line moves away from the equilibrium curve and number of stages decreases. Total Reflux Ratio: At total reflux, minimum number of trays is required. This happens when the entire condensate is recycled back to the column the com lete li uid is re oiled no roduct withdrawn and the eed is com letel sto ed. inimum num er o sta es results when the o eratin line is at dia onal line. e lu ratio is in inite. istillate o tained is ure more volatile component and residue is pure less volatile component.

The total number of stages in case of total reflux can be calculated as under: 1. lot the e uili rium data on a s. ra h and draw a dia onal line. 2. Mark distillate and residue points on that curve. 3. Starting from distillate point, move vertically and cut the equilibrium curve, then move horizontally to cut the diagonal line. 4. Repeat step 3 until you reach the residue point. If the line at the end coincides with the residue point, then number of stages is equal to the number of steps plus one (for reboiler). 5. If line and residue point do not coincide, then does not match with the residue point, then calculate the fraction at the end. Rest is same as step 4.

OBSERVATIONS:
Temp of oil tank Temp of condensate = = C C

Distillate R.I

Residue R.I

Refractive Index of Distillate Refractive Index of Residue

= =

Experimental number of stages

CALCULATION:
Num er o sta es rom ra h Actual number of stages = 3 + 1 = 4 ( +1 for reboiler) Experimental number of stages = Overall Efficiency = =

RESULT:
Number of stages from the graph obtained are ____ and plate efficiency is ______.

CONCLUSION:
The efficiency of the column is high and is equal to 0.8. The overall efficiency of a single plate in a distilling column is defined as the ratio of the actual change in the composition of the liquid between plate n and plate n +1to the change that should occur if there were perfect equilibrium between the rising vapor and the liquid on the plate and if the rising vapor carried no entrained liquid. In general, neither of these ideal conditions is realized in practice. The typical value of plate efficiency is 0.5-0.7. So we can say that contact between liquid and vapor on the plate is good. The efficiency received is hi her in our case asicall ecause our assum tion rising vapor carried no entrained liquid did not follow.