Chemical Extraction Techniques Explained
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ScribdTranslationsChemical Extraction Techniques Explained
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ScribdTranslationsExtraction
chemical extraction
Separation technique of a compound from a solid mixture or
liquid, taking advantage of the differences in solubility of the components
from the mixture in a suitable solvent.
Being one of the most used separation techniques for compounds
in the chemical laboratory.
In the chemical laboratory, the separation and purification of
desired products are as important as optimization
from its synthesis, which, in addition to improving the
reaction conditions aiming for a high yield
to form the desired product, it is necessary to propose
efficient separation processes that allow for a
maximum recovery of the product from the mixture of
reaction. Extraction is one of the most useful techniques.
to do it.
What does it consist of?
This technique separates an organic product from a reaction mixture or isolates it from its
natural sources. It can be defined as the separation of a component from a mixture
through a solvent.
It is widely used in practice to separate organic compounds from the
aqueous solutions or suspensions in which they are found.
The procedure consists of shaking them with an organic solvent that is immiscible with water and
let both layers separate. The different solutes present are distributed among
the aqueous and organic phases, according to their relative solubilities.
Thus, inorganic salts are practically insoluble in most organic solvents.
common, will remain in the aqueous phase, while the organic compounds that
they do not form hydrogen bonds, insoluble in water, will be found in the organic phase.
Types of extraction
Liquid-liquid extraction
Simple liquid-liquid extraction
Continuous liquid-liquid extraction
Solid-liquid extraction
Batch solid-liquid extraction
Continuous solid-liquid extraction
Examples: Simple liquid-liquid extraction
The mixing, agitation, and separation of the two immiscible phases involved in a
simple liquid-liquid extraction operation is carried out in a funnel.
decantation. This funnel should be 30 to 50% larger than the
total volume of the solvents to be used at each moment, so that it is
space for the agitation of the solvents.
After separating both phases, the lower one is removed by the key and the upper one by
the mouth; this is how possible contaminations are prevented. The number of extractions
necessary in each particular case depends on the distribution coefficient and the
relative volumes of water and solvent
Characteristics of the extraction solvent
That it is not miscible with the other solvent (Water or an aqueous solution is usually
one of the solvents involved and the other solvent is an organic solvent.
That the desired component be much more soluble in the extraction solvent.
than in the original solvent.
That the rest of the components are not soluble in the extraction solvent.
It should be sufficiently volatile, so that it can be easily removed from
product extracted by distillation or evaporation.
That it is not toxic or flammable, although, unfortunately, there are few solvents that
They meet both criteria: there are relatively non-toxic but flammable solvents.
like hexane, others are not flammable but are toxic such as dichloromethane or the
chloroform, and others are toxic and flammable like benzene.
Immiscible solvents with water: Solvents
used more frequently
The more polar the organic solvent, the more miscible (soluble) it is.
it's with the water.
For example, polar solvents like methanol, ethanol, or the
acetone is miscible with water, and therefore, is not suitable
for liquid-liquid extractions.
Organic solvents with low polarity such as the
dichloromethane, diethyl ether, ethyl acetate, hexane or the
Toluene is commonly used as an organic solvent for
extraction.
Emulsions
Often, especially when working with alkaline solutions, one
form emulsions during the extraction process. These can
to break, usually by:
a smooth rotating movement to the liquid in the separation funnel,
maintained in its normal position;
2) vigorous stirring of the emulsified layer with a glass rod;
3) saturation of the aqueous layer with common salt;
4) centrifugation.
Method 3, salt saturation, has a double advantage: it reduces
the solubility in water of most solutes and solvents
Organic. Its name is salinity effect.
Once the extraction operation is completed, it is necessary to recover the
product extracted from the combined organic phases. For this, it is
You need to dry the resulting organic phase with a drying agent.
filter the resulting suspension and finally remove the solvent
organic from the dry solution containing the extracted product by
distillation or evaporation.
Although extraction is usually used to separate the product
selectively desired from a mixture, sometimes what is intended with
Extraction is the process of removing unwanted impurities from a solution.
Desiccant. Compound used to extract moisture from the air or from
liquids and solutions in organic solvents. It is important to know the
chemical nature of the substance to be dried.
The desiccant must be insoluble, not produce reactions even with it.
solvent I with the solute should not be a catalyst for reactions of
condensation polymerization and must have a high capacity
desiccant in relation to the dissolution. A liquid is said to be dry
when at the end of the process there is something left of the solid desiccant
Typical desiccant agents form hydrated and anhydrous salts.
Anhydrous sodium sulfate
(Na2SO4), calcium chloride
anhydrous (CaCl2) and the sulfate of
anhydrous magnesium (MgSO4)
they are the most desiccants
used to dehydrate
solutions, whether due to their
accessibility and low cost
speed and nature of the
reactants.
In the extraction processes, where an aqueous solution and another is used
organic, the order of the phases depends on their relative densities. The
halogenated solvents, denser than water, remain below it,
while the rest, being less dense, remain above.
Most of the aqueous solutions used in processes of
extraction contains 5-10% solute. Therefore, the density of these
solutions are very close to that of water (1.0 g/mL). Exceptionally it can
presenting the case of a dissolution in a less dense organic solvent
that the water, which, having a very high solute concentration, increases its
considerably denser and resulting greater than that of the aqueous phase.
Continuous liquid-liquid extraction
When the solubility of the compound to be extracted in the extraction solvents
is not very high, another procedure is usually used that involves a
continuous extraction of the initial phase (normally an aqueous phase) with portions
news from the organic extraction solvent. To avoid using large volumes
of the extraction solvent, the process is carried out in a closed system in which the
extraction solvent is heated in a flask and the solvent vapors are
they condense in a refrigerant placed on a tube or extraction chamber
what the aqueous solution to be extracted contains. The hot condensed solvent is
passes through the aqueous solution, to finally reach, with part of the
extracted product, to the initial flask, where the organic solvent is vaporized again,
repeating a new extraction cycle, while the extracted product, non-volatile,
it is concentrating in the flask.
Soxhlet
Discontinuous solid-liquid extraction
In the favorable case of a mixture of solids in which one of the
compound is soluble in a certain solvent (usually a
organic solvent), while the others are insoluble, we can
perform an extraction consisting of adding this solvent to the mixture
contained in a beaker, a flask or a capsule of
porcelain, cold or hot, shake or crush with the help of a
glass rod and separate by filtration the solution that contains the
extracted product and the insoluble fraction that contains the impurities. Yes,
On the contrary, the intention is to dissolve the impurities of the mixture.
solid, leaving the desired product as an insoluble fraction, the process,
instead of extraction, it is called washing.
Extracción sólido-líquido continua
Solid-liquid extraction is usually much more efficient when it
does continuously with the hot extraction solvent in
a closed system, using a methodology similar to the
commented for continuous liquid-liquid extraction, based on the
maceration with organic solvent, previously vaporized in a
flask and condenser in a refrigerant, from solid mixture to
extract contained within a cartridge or cellulose bag that is
Put it in the extraction chamber. The passage of the organic solvent.
with part of the product extracted to the initial flask, it allows for the
same organic solvent is vaporized again, repeating a
new extraction cycle, while the extracted product does not
volatile, it is concentrating in the flask.
Materials:
a) Decantation funnel
cork
German-shaped funnel
Erlenmeyer flasks for collecting the phases
e) Support, nut, and metal ring
Procedure
[Link]
Some equipment used in the industry to
extraction
Stage extraction: Contact extraction
differential continuum
Mixer - Settler
Spray towers
Pierced plates towers
Fill towers
Tray columns
Pulsed columns
Centrifugal Extractors
RISKS AND SAFETY REGULATIONS
Hot extractions
Solid-liquid or liquid-liquid extraction in
hot is a relatively routine operation
in chemistry laboratories. The most common case
it is extraction with the Soxhlet system. Given that
volatile liquids are usually used for her
flammable materials, the regulations will need to be applied
general recommendations for the use of
this type of compounds that have already been discussed
(overpressure, presence of flammable vapors).
It is recommended:
Heat the extraction system using a water bath or an oil bath to a
temperatura suficiente, pero no más alta, para asegurar la ebullición del disolvente.
When the extraction is of long duration, it is advisable to have a system for
control of cooling water in the face of possible water supply interruptions.
Have an appropriate action system (manual fire extinguisher, etc.) close to the location.
of the operation.
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The solid or liquid waste generated in these operations will be deposited in the
corresponding waste containers.
Extrusions at room temperature
As mentioned, in most liquid-liquid extraction processes or
solid-liquid at room temperature, a volatile organic compound is used,
usually a flammable solvent, with which any overpressure in the assembly or
a steam leak can cause a fire. It should be taken into account that whenever there
Handling substances of these characteristics presents a risk of fire and explosion.
The systems for controlling these risks are:
Carry out the operation at the showcase.
Have a fire protection system (extinguisher, appropriate manual, etc.) close to the location.
of the operation.
If a decanting funnel is used with manual agitation, there is also the problem of
direct contact with products and the possibility of inhaling high concentrations
of vapors when relieving the pressure of the funnel (generated by vaporization during stirring)
through the valve of the shut-off valve. In this operation, it is advisable to wear gloves.
waterproofs, protective clothing and, as mentioned earlier, carry out the operation in
the showcase, although this may be uncomfortable, especially if the substances involved in
the process has high hazard characteristics.