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Technical Report 1_ Liquid-liquid Extraction
Technical Report 1_ Liquid-liquid Extraction
Technical Report 1_ Liquid-liquid Extraction
LIQUID-LIQUID EXTRACTION
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I.INTRODUCTION
Liquid-liquid extraction (LLE), also known as solvent extraction or partitioning, is a
method that can be used for separating compounds based on their relative solubilities in two
different immiscible liquids. One of the liquids in question is usually water (or a solution thereof)
and here, one may describe it as aqueous solvent for better differentiation with respect to an
organic liquid. It is based on the principles of differential solubility and selective partitioning and
hence an inevitable process for isolating, purifying or concentrating some specific substances
from complex mixtures.In the basic approach of LLE, two immiscible liquids are mixed leading
to transfer of a solute (the substance whose mobile species) between phases.. Liquid-liquid
extraction has been improved by the development of advanced techniques and equipment,
including mixer-settlers, spray column, packed column, and plate column.
In the food industry itself, Liquid Liquid Extraction is applied to a number of critical
purposes associated with enhancing the quality, safety, and efficiency of food production and
processing. One of the major objectives is the isolation and purification of essential nutrients like
vitamins, minerals, and fatty acids that may be utilized as supplements or additives. It is also a
major tool in the extraction and concentration of natural flavors and aromas from plants, fruits,
and herbs; LLE improves sensory qualities of food products. Besides that, it removes unwanted
substances and off-flavors—bitter compounds, for example—to enhance taste and safety.
III. CONTENT
Liquid-liquid extraction (LLE) is an operation in which a solute dissolved in one liquid phase is
transferred to a second liquid phase. Sometimes called extraction, solvent extraction, or simply liquid
extraction, this process involves bringing two immiscible or partly miscible liquids into contact with each
other. During this contact, soluble substances in one liquid phase diffuse into the other liquid phase.
LLE is widely used in various fields such as chemistry, biology, and engineering. In chemistry, it
is employed to separate and purify compounds, especially in organic synthesis and analytical procedures.
In biology, LLE is used to isolate and purify biomolecules, such as proteins and nucleic acids, from
complex mixtures. In engineering, LLE plays a crucial role in the extraction and purification of valuable
materials, such as in the petroleum industry for refining hydrocarbons and removing impurities. Overall,
the versatility and efficiency of liquid-liquid extraction make it an indispensable technique for isolating,
purifying, and recovering a wide range of substances across different scientific and industrial applications.
Solute (B): The solute is the material that needs to be extracted. It is the specific substance or
compound that is present in the feed solvent and is the target of the extraction process. The
solute's properties, such as its solubility and chemical stability, are important factors that
influence the choice of extraction solvent and the overall efficiency of the extraction.
Solvent (S): The solvent, also known as the extraction solvent, is the immiscible liquid added to
the process to extract the solute from the feed. This solvent must have a high affinity for the
solute but remain immiscible with the feed solvent to facilitate phase separation. The extraction
solvent's properties, including its selectivity for the solute and its ease of recovery, are critical to
the success of the extraction process.
Extract: The extract is the exit phase that is rich in solute. It is the phase that results after the
solute has been transferred from the feed solvent to the extraction solvent. The extract contains a
higher concentration of the solute and can undergo further processing to isolate and purify the
desired compound.
Raffinate: The raffinate is the exit phase that is lean in solute. It is the remaining phase from
which the solute has been largely removed during the extraction process. The raffinate typically
contains the feed solvent and any residual solute that was not transferred to the extraction solvent.
2. Partition Ratio: The partition ratio, or distribution coefficient, defines the ratio of solute
concentrations between the two immiscible phases at equilibrium. A higher partition ratio
indicates that the solute preferentially partitions into one phase over the other, facilitating
effective separation. This property is crucial in designing extraction processes to ensure that the
desired solute is efficiently transferred to the extracting solvent, leading to higher yields and
purities in the extracted product.
3. Solute Selectivity: Solute selectivity refers to a solvent's ability to selectively extract a specific
solute from a mixture containing multiple components. High selectivity ensures that the target
solute is efficiently separated from other substances present in the feed mixture. This
characteristic is particularly important in applications requiring the isolation of pure compounds,
such as pharmaceuticals and fine chemicals production. Solvents with high selectivity contribute
to the overall purity and quality of the extracted product by minimizing contamination and
co-extraction of unwanted components.
4. Mutual Solubility: Mutual solubility describes the degree to which two immiscible solvents
dissolve in each other when brought into contact. In liquid-liquid extraction, maintaining low
mutual solubility is advantageous as it helps in preserving distinct phases. This property prevents
the formation of emulsions and ensures clear phase separation, which is essential for efficient
recovery of the solvent-rich phase (extract) and the feed-rich phase (raffinate). Effective phase
separation simplifies downstream processing steps and reduces the complexity of solvent
recovery and recycling processes.
5. Stability: The stability of a solvent, both chemically and thermally, is critical for maintaining its
effectiveness throughout the extraction process. Chemically stable solvents do not undergo
undesirable reactions that could alter the solute or degrade the solvent itself, ensuring the integrity
of the extracted product. Thermally stable solvents withstand variations in temperature during
extraction without compromising their performance or physical properties. Stability ensures
consistent extraction efficiency and product quality, making solvent selection a crucial
consideration in designing robust and reliable extraction processes.
6. Density Difference: The density difference between the two liquid phases involved in extraction
facilitates phase separation after the solute transfer process. A significant density contrast enables
easy gravitational settling or centrifugation, ensuring efficient recovery of the solvent-rich phase
(extract) and the feed-rich phase (raffinate). This property simplifies the separation process,
reduces solvent losses, and enhances overall extraction efficiency, contributing to the economic
viability and sustainability of liquid-liquid extraction processes.
7. Viscosity – low viscosity (water-like) is preferred because higher viscosity generally increases
mass transfer resistance and makes liquid-liquid phase separation more difficult.
Viscosity refers to the measure of a fluid's resistance to flow. In the context of
liquid-liquid extraction, low viscosity is preferred, ideally resembling that of water. This
preference arises because higher viscosity tends to increase the resistance to mass transfer,
making it more difficult for the solute molecules to move between the two liquid phases. When
the viscosity of the solvent is high, it creates additional barriers to the movement of solute
molecules, slowing down the extraction process. This increased resistance can hinder the efficient
transfer of the desired components from one phase to another, reducing the overall effectiveness
of the extraction. Moreover, higher viscosity can also complicate the liquid-liquid phase
separation process. It can lead to slower settling of phases or emulsification, where the two phases
mix to form a stable emulsion, making it challenging to separate them.
8. Interfacial tension – preferred values for interfacial tension between the feed phase and the
extraction solvent phase generally are in the range of 5−25 𝑑𝑦𝑛𝑒/𝑐𝑚. Systems with lower values
easily emulsify while higher values result to low interfacial area and poor mass transfer
performance.
Interfacial tension refers to the force per unit length acting at the interface between two
immiscible liquids, such as the feed phase and the extraction solvent phase in liquid-liquid
extraction. In this process, it's important to consider the interfacial tension between these two
phases.
9. Recoverability – solvent physical properties should facilitate low-cost options for solvent
recovery, recycling, and storage and enable low-cost methods for purging from the overall
process impurities that may accumulate over time.
Recoverability in the context of solvent selection for a process refers to the ease and
cost-effectiveness of recovering, recycling, and storing the solvent, as well as purging any
accumulated impurities from the overall process. To ensure recoverability, it's essential to
consider the physical properties of the solvent. Solvents that are easily separable from the desired
product, either through simple physical methods like distillation or filtration, are preferred.
Additionally, solvents that have low volatility, meaning they don't readily evaporate at normal
operating temperatures, are advantageous as they can be recovered more efficiently.
10. Availability and cost – the solvent should be readily available at a reasonable cost.
Availability and cost are critical considerations when selecting a solvent for any process.
a. Readily Available: A solvent should be easily accessible in the required quantity
and quality. Availability ensures that there are no disruptions in the production
process due to shortages or delays in obtaining the solvent. It's advantageous to
choose solvents that are commonly produced or readily sourced from suppliers to
maintain a steady supply chain.
b. Reasonable Cost: Cost-effectiveness is essential for maintaining the economic
viability of a process. The solvent should be affordable and not significantly
inflate the overall production expenses. Opting for solvents that are cost-effective
helps in keeping the operational costs low and maximizes the profitability of the
process.
Types of Extraction
1. Solid-liquid extraction - A solute is transferred from a solid phase to a liquid phase.
This process typically involves extracting desired compounds or substances from
solid materials, such as plant material, ores, or biomass, using a liquid solvent. The solute
dissolves in the liquid solvent, forming a solution, which can then be separated from the
solid residue through filtration or other separation techniques. Solid-liquid extraction is
widely used in various industries, including pharmaceuticals, food processing, and
environmental remediation, for extracting valuable compounds or removing contaminants
from solid materials.
Examples of Extraction
1. Brewing Coffee - During the brewing process, soluble compounds such as caffeine, oils,
and flavor compounds are extracted from the coffee grounds into the liquid (usually
water) to produce the beverage. This extraction occurs as hot water comes into contact
with the coffee grounds, dissolving and suspending these compounds in the water. While
the mechanism of coffee brewing differs from some traditional extraction processes (such
as liquid-liquid extraction), the fundamental principle of extracting soluble compounds
from a solid material using a liquid solvent is the same. Therefore, brewing coffee is
commonly categorized as a form of extraction.
2. Making Tea - When tea leaves (or tea bags containing tea leaves) are steeped in hot
water, soluble compounds such as flavonoids, catechins, and caffeine are extracted from
the leaves into the water. This process occurs due to the dissolution of these compounds
in the hot water, resulting in the formation of the tea beverage. Similar to coffee brewing,
making tea involves the extraction of soluble compounds from a solid material (tea
leaves) using a liquid solvent (hot water). Therefore, making tea is considered a form of
extraction.
This basic setup can be modified and adapted for different extraction processes and
scales, depending on the specific requirements of the application. Additional equipment, such as
heating mantles, reflux condensers, or filtration setups, may be incorporated as needed to
optimize the extraction process.
Common Equipment
1. Mixer-Settlers
The mixer and settler are essentially two separate components that are integrated to act as
one system. Mixer-settlers are widely used for liquid/liquid solvent extraction applications where
they generally operate in a continuous mode of operation. The name comes from the two steps
involved in phase-splitting: one is a first mixed for mass-transfer of liquid phases and another step
employs gravity to naturally divide, settling down components.
It consists of vertical vessels incorporating a turbine or propeller agitator. It is provided
with charging nozzles at the top and a discharge connection provided with a sight glass at the
bottom. The feed solution to be extracted is taken into the agitated vessel, required amount of the
solvent is added and the whole mass is agitated for a predetermined time. At the mixing cycle,
agitation is stopped and settling is applied for the phase separation.Afterwards, the raffinate and
extract phases are withdrawn from the bottom discharge connection into separate receivers.
2. Spray Column
3. Plate Column
substances. Overall, plate columns are indispensable tools in liquid-liquid extraction, providing
efficient and customizable solutions for a variety of industrial applications.
4. Packed Column
Application In Industry
Liquid-liquid extraction, also known as solvent extraction, is widely used in various industrial
applications for separating components from liquid mixtures
1. Pharmaceutical Industry
Liquid-liquid extraction (LLE) plays a crucial role in the pharmaceutical industry for the
separation, purification, and isolation of various compounds. This technique is employed in
several stages of drug development and production, including the extraction of active
pharmaceutical ingredients (APIs) from complex mixtures, purification of reaction products,
removal of impurities, and isolation of natural products.
Pharmaceutical LLE Process:
1. Purification of Synthetic Drug Compounds: After chemical synthesis, crude reaction
mixtures often contain impurities or by-products. LLE can be employed to purify the target drug
compound by selectively extracting it into a suitable organic solvent phase, leaving behind
unwanted impurities in the aqueous phase.
2. Isolation of Natural Products: Many pharmaceuticals are derived from natural sources like
plants or marine organisms. LLE is used to isolate and concentrate bioactive compounds from
these natural extracts. For instance, extracting alkaloids from plant material using organic
solvents.
2. Chemical Industry
Liquid-liquid extraction (LLE) is extensively utilized in the chemical industry for the
separation, purification, and recovery of various compounds from liquid mixtures. This technique
is applied in processes involving the extraction of valuable chemicals, removal of impurities,
purification of intermediates, and recovery of metals from solutions.
Application of LLE in the Chemical Industry:
1. Metal Extraction and Recovery: LLE is employed in hydrometallurgical processes for
extracting and recovering metals from ores or solutions. For instance, in copper mining, LLE is
used to extract copper ions from leach solutions containing copper sulfate or copper oxide.
Organic extractants like hydroxyoximes or dialkylphosphoric acids are often used as selective
extractants for specific metals, allowing the separation and recovery of target metals from
complex solutions.
2. Purification of Chemicals: LLE is used to purify chemical compounds by selectively
removing impurities or separating desired components from reaction mixtures. For example, in
the production of organic acids like acetic acid, LLE can be employed to separate and purify
acetic acid from fermentation broths or reaction mixtures.
3. Aromatics Extraction in Refining: In the petroleum refining industry, LLE is utilized for the
extraction of aromatics (e.g., benzene, toluene, xylene - BTX) from hydrocarbon mixtures.
Aromatic extraction is crucial for producing high-purity benzene and toluene used as feedstock’s
in the petrochemical industry.
4. Removal of Contaminants in Chemical Processes: LLE is employed for the removal of
unwanted contaminants or impurities from process streams. For instance, in biodiesel production,
LLE can be used to remove glycerol and soap contaminants from biodiesel to improve its quality.
3. Food and Beverage Industry
Liquid-liquid extraction (LLE) plays a significant role in the food and beverage industry
for various applications, including the extraction and purification of natural flavors, removal of
undesirable components, and separation of valuable compounds from food matrices. This
technique enables the isolation and concentration of specific compounds that contribute to the
sensory characteristics, quality, and functionality of food products. Below are examples
illustrating how LLE is employed in the food and beverage industry:
Application of LLE in Food and Beverage Industry:
1. Extraction of Natural Flavors and Fragrances: LLE is used to extract essential oils, flavors,
and fragrances from natural sources such as fruits, herbs, spices, and flowers. Organic solvents
like hexane, ethanol, or supercritical carbon dioxide are utilized to selectively extract volatile
aromatic compounds, resulting in concentrated flavor extracts.
2. Debittering and Decolorization of Food Oils: LLE is employed for the removal of bitter
compounds, pigments, or impurities from food oils. For example, in the production of olive oil,
LLE can be used to remove bitter phenolic compounds or chlorophyll pigments from olive oil
extracts, improving the sensory attributes and quality of the final product.
4. Reduced Environmental Impact: This is achieved through LLE applied in the biofuels
industry and which works to reduce impacts on the environment due to production processes. Due
to LLE, there is reduced waste production and lesser energy use; this makes the process of
producing bio fuel, green and preserving the environment.
5. Optimization of Production Processes: LLE is very essential in enhancement of optimized
numerous separative steps in the biofuel production process since it offers easy means for
separation of the components. It is an optimization that enhances not only the performance of
processes and products, but it is also beneficial in the management of resources for better yields
and costs.
6. Sustainable Biofuel Technology: The advantages of LLE facilitate cost and energy-efficient
process technology required for polygeneration and the commercial viability of sustainable
biofuels. This technology is very useful in the development of other renewable energy sources
such as the biofuels to help in cutting down effects on the lives of citizens.
Summary
● Liquid-liquid extraction is a process where a solute is transferred from one liquid phase to
another, separating components of a mixture by treating them with a solvent that preferentially
solubles the desired components. This separation occurs when substances from one solution are
transferred to another.
● The selection of a solvent for a process involves several factors, including loading capacity,
partition ratio, solute selectivity, mutual solubility, stability, density difference, viscosity,
interfacial tension, and recoverability.
● Solid-liquid extraction, liquid-liquid extraction, and acid-base extraction are methods used in
industries like pharmaceuticals, food processing, and environmental remediation to remove
contaminants, purify, separate, and concentrate solutes.
● Brewing coffee and tea involves extracting soluble compounds from coffee grounds and leaves
using hot water, using a liquid solvent to dissolve and suspend these compounds.
● A liquid-liquid extraction setup involves a separatory funnel with a stopcock, holding two
immiscible liquid phases. The organic phase contains the solute, while the aqueous phase contains
the extracting agent. The denser phase settles, while the lighter phase remains.
● Some mechanisms and equipment include mixer-settlers, spray columns, plate columns, and
packed columns are mineral process equipment used in solvent extraction, chemical
manufacturing, wastewater treatment, purification, petrochemical, oil refining, and chemical
processing.
● Liquid-liquid extraction (LLE) is a crucial technique in various industries, including
pharmaceuticals, chemicals, food and beverage, and environmental remediation. It is used for the
separation, purification, and isolation of compounds, metal extraction, and aromatics. In the food
and beverage industry, it is used for extracting natural flavors and removing undesirable
components. LLE also aids in environmental remediation by selectively transferring target
compounds into an immiscible organic phase. It is also used for radioactive waste treatment.
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