CHE435 Week 5 Lab

Chemical Engineering Laboratory
Liquid-Liquid Extraction
Lab Session Summary
• Theory of Liquid-Liquid Extraction
• Liquid-Liquid Extraction applications
• Important factors in solvent selection
• Continuous vs batch Extraction
• Experiment manual and process diagram
Extraction Process & Equipment
Extraction: one or more solutes are removed from a liq by transferring the
solute(s) into a second liq phase (solvent).
• The solvent is a mass separating agent that must be recovered later.

• The two liq phases must be immiscible (insoluble in each other) or partially
immiscible.
• Separation is based on different solubilities of the solute in the two phases.

• Although extraction is fairly common, the ratio of distillation to extraction units in
industry is about 20 to 1.
• Extraction can be done at low temperature (since vaporization is not required).

• Extraction is a gentle process suitable for unstable molecules such as
proteins or DNA.
 Extraction is a common laboratory and commercial unit operation;
• In commercial penicillin manufacturing, after the fermentation broth is

sent to a centrifuge to remove cell particles, the penicillin is extracted
from the broth. Then the solvent and the penicillin are separated from
each other by one of several techniques
• In petroleum processing, aromatic hydrocarbons such as benzene,

toluene, and xylenes are separated from the paraffins by extraction
with a solvent such as sulfolane. The mixture of sulfolane and
aromatics is sent to a distillation column, where the sulfolane is the
bottoms product, and is recycled back to the extractor.
• The simplest extraction operation is single-contact batch extraction in which the
initial feed solution is agitated with a suitable solvent, allowed to separate into two
phases after which the solvent containing the extracted solute is decanted. This is
analogous to the laboratory procedure employing a separating funnel. It has an
advantage of achieving better separation and, hence, increased efficiency. However,
the separation rate is low.
• On an industrial scale, the extraction operation more usually involves more than one
extraction stage and is normally carried out on a continuous basis. The equipment
may be comprised of either discrete mixers and settlers or some form of column
contactor in which the feed and solvent phases flow counter currently by virtue of the
density difference between the phases. It has an advantage of achieving higher
separation rate on the expense of separation efficiency.
Illustration of the extraction mechanism in batch mode
Batch vs Continuous
Batch process
Continuous process
Mass balance
In order to find the quantity of the solute remaining in the
feed (at the end of the batch process) or in the raffinate (at
the end of a continuous process), mass balance law can
be applied.
For Batch operation:
Original amount of solute in the feed = Amount of solute

remaining in Feed + Amount of solute in Solvent
For Continuous operation:
Flow rate of solute in the feed = Flow rate of solute in

Raffinate + Flow rate of solute in Extract
Batch process mass balance
𝑚𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 = 𝑚𝑠𝑜𝑙𝑢𝑡𝑒 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔 𝑖𝑛 𝑓𝑒𝑒𝑑 + 𝑚𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
The amount of solute in the solvent can be found by taking a sample of the solvent mixture at
the end and testing it to find the mass fraction of solute in the mixture (see next slide).
Knowing the original amount of solute in the feed, the amount of solute remaining in the feed
can be easily found.
Finding mass fraction of solute in solvent
In the L-L extraction unit that is used in the lab, water is used as a solvent to remove ethanol
(solute) from sunflower oil. Check the Experiment Manual for more details.
In order to find the mass fraction of ethanol in the water, you may use density tables which
provides the fraction of ethanol (solute) in water (solvent) as function of Temperature and
Density of a water-ethanol sample.
Finding mass fraction of solute in solvent
Sampling steps:
1- take a sample of 100 mL of solvent-solute mixture from the solvent tank during or at the end
of the operation.
2- check the temperature and density of the sample.
3- use the density tables to find mass fraction of ethanol in the solvent (𝑤𝐸 ).
At the end, you will be able to identify the remaining mass of ethanol in the feed by applying
mass balance law.
𝑚𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑖𝑛 𝑓𝑒𝑒𝑑 = 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔 𝑖𝑛 𝑓𝑒𝑒𝑑 + 𝑤𝐸 ∗ 𝑚𝑠𝑜𝑙𝑣𝑒𝑛𝑡−𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑚𝑖𝑥𝑡𝑢𝑟𝑒
Where 𝑤𝐸 is the mass fraction of ethanol in the solvent

Density Tables
Density in kg/m³ as a function of mass fraction of ethanol wE and temperature T, 0% < wE < 50%, 10°C < T < 20°C
Density Tables
Density in kg/m³ as a function of mass fraction of ethanol wE and temperature T, 0% < wE < 50%, 20°C < T < 30°C
Batch Extraction Video
Link: https://www.youtube.com/watch?v=8bZl7mcG0Ew
Solvent Properties
1. Easy to separate from the diluent (immiscible or partially miscible system
where separation by distillation is easy).
2. Highly selective for the desired solute and not very selective for
contaminants.
3. Non-Toxic
4. Non- Corrosive
5. Readily Available
6. Chemically Stable
7. Environmentally Friendly
8. Inexpensive
Solvent Properties
Solubility parameter (δ) is simple approach to selecting a solvent with large
selectivity: latent energy of vaporization
The solubility parameter has the advantage of being a property of only the pure
components, it is easily calculated from parameters that are easy to measure and
are often readily available, and tables of δ are available
δ value is useful for quick estimation of the miscibility of two liqs:

The closer the values of δA and δB the more likely the liqs are miscible:
For example, δ values in (cal/ml)1/2 are:
Water = 23.4 Water and ethanol are miscible.

Ethanol = 12.7 Water and benzene are immiscible.
Benzene = 9.2
Ethanol and benzene are miscible.
Experiment Manual

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Chemical Engineering Laboratory

• The solvent is a mass separating agent that must be recovered later.

• Separation is based on different solubilities of the solute in the two phases.

• Extraction can be done at low temperature (since vaporization is not required).

• In commercial penicillin manufacturing, after the fermentation broth is

• In petroleum processing, aromatic hydrocarbons such as benzene,

For Batch operation:

Original amount of solute in the feed = Amount of solute

For Continuous operation:

Flow rate of solute in the feed = Flow rate of solute in

𝑚𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 = 𝑚𝑠𝑜𝑙𝑢𝑡𝑒 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔 𝑖𝑛 𝑓𝑒𝑒𝑑 + 𝑚𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑠𝑜𝑙𝑣𝑒𝑛𝑡

𝑚𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑖𝑛 𝑓𝑒𝑒𝑑 = 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔 𝑖𝑛 𝑓𝑒𝑒𝑑 + 𝑤𝐸 ∗ 𝑚𝑠𝑜𝑙𝑣𝑒𝑛𝑡−𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑚𝑖𝑥𝑡𝑢𝑟𝑒

Where 𝑤𝐸 is the mass fraction of ethanol in the solvent

δ value is useful for quick estimation of the miscibility of two liqs:

For example, δ values in (cal/ml)1/2 are:

Water = 23.4 Water and ethanol are miscible.

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