SUMMARY

The main objective of the experiment is to study the extraction of potassium bicarbonate
(soluble components) which is coated on ceramic balls ( the solid). The extraction of
potassium bicarbonate is carried out in a 3-stage Rotocell –type extractor using water.

The pure solvent (water) is first supplied to a nozzle from a tank using a feed pump
in a continuous 3-stage mode. When the enriched solvent passed through the third stage,
the solvent is collected in the extract tank. The solvent and extraction material travel in
counter-current flow, with the depleted extraction residue dropping into a tank after one
rotation of the extractor.

Firstly, the experiment is carried out by weighing the weight of the balls and the
coated potassium bicarbonate which are divided into equal halves. The first half of the
coated ceramic balls is divided into three segments and filled up in the extractor. The other
half is divided into 6 equal portions and weighed. Each of the six equal portions was further
divided into 3 to make sure an equal number of ceramic balls were added into the Rotocell
extractor. The mass balance was used to determine the weight of the ceramic balls.

The solvent tank is filled up with 7 liter of water. The temperature and pump
controllers are set at given values. The conductivity of solvent 1 is recorded. Solvent pump 1
is switched on and for every 15 minutes interval, the extractor is filled up with the remaining
balls until all of them are used up. The conductivity of solvent tank 2 is recorded, once the
solvent tank 1 is empty. Again ,the conductivity of solvent tank 3 is recorded , once the
solvent tank 2 is empty. Finally ,when the solvent tank 3 is almost empty, the conductivity of
product tank is recorded and the volume of the tank is measured.

The observed trend was : The conductivity of each successive solvent tank increased,
when the extraction of Potassium Bicarbonate from the ceramic balls into the solution
increases. This can be observed clearly from the graph on the next page which is marked as
Figure 1.
 RESULTS

TABLE 1

Solvent flow rate 10 L/h

Conductivity (µs) Conductivity (µs) (KCHO3
basis i.e conductivity – initial
conductivity of tank 1 )

Solvent tank 1 1 -
Solvent tank 2 499 498
Solvent tank 3 575 574
Product tank 695 694
*Conductivity of the initial feed in tank 1 is set as reference.

Volume of product tank water : 5450 ml

Writing up :

12)

Conductivity (µs)
800

700

600

500

400
Conductivity (µs)
300

200

100

0
Solvent tank 1 Solvent tank 2 Solvent tank 3 Solvent tank 4

Figure 1 : Conductivity (µs) versus solvent tank 1 ,2 ,3 and 4.

13) Initial mass fraction of potassium bicarbonate in the ceramic balls :

0.657 wt%

14) Mass fraction of potassium bicarbonate in the final extract stream :

0.0466 wt%

15) Ways to improve the yield of the final extract is elaborated in the DISCUSSION.

DISCUSSION

Solid liquid extraction is a type of leaching which involves the removal of a soluble material
through dissolution in a dissolving solvent. (1)

The differences in conductivity of the pure water and the water which contains dissolved
impurities gives the extent of reaction. The conductivity of solvent tank 1 containing pure
water was measured at 1 µs, and then the conductivity of the remaining tanks was
measured respectively in order for the extraction process to be measured.

Figure 1 is not a linear graph because the ceramic balls were not distributed into the tank at
a constant rate which does not allow the water to be evenly distributed over them. The
extraction process is said to be reaching its limit, when there is no more potassium
bicarbonate being extracted into the water. The initial and final mass fractions are obtained
by performing a series of calculations to get the required results using the conductivity of
solutions.

There were a few minor discrepancies such as human errors in handling the stop watch, the
parallax error in reading the exact volume of the product tank. The heat pump of solvent
tank 1 was not functioning properly and this may have made the final result to be not quite
accurate. The results would have been more accurate if the solvent tanks were completely
empty, when taking down the conductivity reading for the respective tank as there was
always some solution left in each of the tank as this can alter the experimental values for
conductivity. This leads to a reduction in the volume of water collected at the end of the
experiment which is 5450 ml given the initial amount of water used is 7000ml.

The yield of the final extraction can be improved by altering certain extraction conditions.
The extraction rate is affected by surface area of ceramic balls. A larger surface area is
provided for the solvent by reducing the size of ceramic balls. This will enable an increase in
the rate of diffusion of solute into solvent. Agitation will further increase the rate of
diffusion of potassium bicarbonate from the ceramic balls into the solvent. An increase in
temperature will also help the extraction rate to proceed at a faster rate as it decreases the
viscosity of solvent which improves the extraction of potassium bicarbonate into the
solution. Pure solvent can be introduced for each stage of extraction process as it increases
the rate of extraction of potassium bicarbonate rather than using back the same recycled
solvent for each stage. A higher number of stages will increase the overall efficiency of
extraction. Higher concentration of potassium bicarbonate provides more potassium
bicarbonate molecules per volume. Thus ,it increases the rate of mass transfer.

CONCLUSION

The main aim of the experiment is achieved successfully , provided the minor discrepancies
are ignored. The initial mass fraction of potassium bicarbonate in the ceramic balls is
0.657wt %. The final mass fraction of potassium bicarbonate in the ceramic balls is 0.0466
wt %. The yield of the final extraction can be improved by increasing the surface area of
ceramic balls, agitation ,increasing number of stages in extraction ,concentration of
potassium bicarbonate and also the temperature for the extraction process being carried
out ( operating temperature).
 REFERENCE

 (1)http://wiki.answers.com/Q/What is solid liquid extraction

 Lab Manual
 Richardson, J.F. et al (2002) Coulson & Richardson’s Chemical Engineering Volume
2 Fifth Edition Particle Technology and Separation Processes. Great Britain,
Butterworth-Heinemann.
 Separation Process Notes by Dr. Gan Su Yin

APENDIX

Sample calculations

13) Initial mass fraction of the Potassium Bicarbonate in the ceramic balls

Mass of potassium bicarbonate coated ceramic balls : 1522g

Mass of pure ceramic balls : 1512g

Mass of potassium bicarbonate : 1522 -1512 =100g

Initial mass fraction = ( 100/1522) = 0.657 wt %

14) Mass fraction of Potassium Bicarbonate in the ceramic balls in the Final Extract Stream.

Refer to the graph in the Appendix (1) in the lab manual which is the Conductivity versus the
Molarity of Potassium Bicarbonate.

Given graph is linear till Molarity = 0.06

Using the equation of graph ,y =mx + C

Gradient of graph =( 9000 -2000) / (0.06 -0.013) = 148936.1702

Therefore ,equation of graph : y = 148936.1702x

Using the results obtained for the final extract ,

When y = 694 µs , therefore x= 4.66 X 10-3 which is the concentration.

No. of moles = Concentration X Volume = 4.66 X 10-3 X 5.450L = 0.0254 moles

No. of moles = Mass / Molar mass

Molar weight of Potassium Bicarbonate = 100.115 g/mol

Mass of Potassium Bicarbonate = 0.0254 X 100.115 = 2.54 kg

Assumption made : The solution in product tank has the same density to that of water
which is 1000 kg/L

Mass of solution = 5.45 X 1000 =5450 kg

Mass fraction of potassium bicarbonate in the Ceramic Balls in the Final Extract Stream

= 2.54 /5450 =0.0466 wt%

Appendix 1

Initial mass of potassium bicarbonate coated ceramic balls 1522g

1 st portion of ceramic balls 127g
2 nd portion of ceramic balls 128g
3 rd portion of ceramic balls 127g
4th portion of ceramic balls 129g
5th portion of ceramic balls 128g
6th portion of ceramic balls 127g
Experiment : Solid-Liquid Extraction of Potassium
Bicarbonate coated Ceramic Balls ( SLE )

Group number 20
Name Kuknesvary Puniamurthy
(007973)
Group members 1)Lim Chew Shean
2)Foong Hua Yeang Anthony
3)Lohashenpahan
Shanmuganathan
4)Loh Xuejing
Date of experiment 31.10.2011
Date of handling - in 07.11.2011