STEPS OF FRACTIONAL DISTILLATION?
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The various components of crude oil have different sizes, weights and boiling temperatures; so, the first step is to separate these components. Because they have different boiling temperatures, they can be separated easily by a process called fractional distillation. The steps of fractional distillation are as follows:
You heat the mixture of two or more substances (liquids) with different boiling points to a high temperature. Heating is usually done with high pressure steam to temperatures of about 1112 degrees Fahrenheit / 600 degrees Celsius.
The mixture boils, forming vapor (gases); most substances go into the vapor phase.
The vapor enters the bottom of a long column (fractional distillation column) that is filled with trays or plates. The trays have many holes or bubble caps (like a loosened cap on a soda bottle) in them to allow the vapor to pass through. They increase the contact time between the vapor and the liquids in the column and help to collect liquids that form at various heights in the column. There is a temperature difference across the column (hot at the bottom, cool at the top).
The vapor rises in the column.
As the vapor rises through the trays in the column, it cools.
When a substance in the vapor reaches a height where the temperature of the column is equal to that substance's boiling point, it will condense to form a liquid. (The substance with the lowest boiling point will condense at the highest point in the column; substances with higher boiling points will condense lower in the column.).
The trays collect the various liquid fractions.
The collected liquid fractions may pass to condensers, which cool them further, and then go to storage tanks, or they may go to other areas for further chemical processing
Fractional distillation is useful for separating a mixture of substances with narrow differences in boiling points, and is the most important step in the refining process.
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If a beaded fractionating column is used, sometimes a wad of glass wool is inserted into the top so that the beads do not spill out. Before using the column, remove this wad as it may interfere with the passage of vapors (Figure 5.44a). If using a Vigreux column, check for broken glass indentations (which would case a leak in the column).
The distilling pot will need to be heated much more vigorously than with a simple distillation, as there is a greater distance for the vapors to travel before reaching the condenser. The vapors will tend to reflux in the column (condense and drip back into the distilling pot) unless stronger heating is applied.
A rule of thumb is that the distilling pot needs to be 30oC hotter than the top of the column in order for material to ascend the column. If it is difficult to achieve more than a reflux, the column can be insulated by wrapping it with glass wool then aluminum foil . This allows the column to maintain heat and the sample to remain in the gas phase longer. A small gap can be left in the foil or glass wool if desired to "peek in" on the activity in the column.
Ideally both liquid and gas should be seen in the fractionating column, as the sample needs to undergo many vaporization-condensation events . Droplets of liquid should be seen on the surfaces of the packing material, but there should never by a large pool of liquid. A "river" of liquid traveling up the column is called flooding (Figure 5.45). If a column floods, remove the heat until the liquid drains back into the distilling flask, then resume heating at a gentler rate.
Cleaning of a fractionating column:
Vigreux column: rinse with acetone. Don't use a scrub brush or the glass indentations may break.
Steel wool column. rinse with large amounts of acetone. Don't rinse with water as wet steel will rust over time.
Glass bead column: rinse with acetone, then replace the glass wool wad to prevent the beads from pouring out when horizontal. Alternatively, pour out the glass beads to be cleaned separately. Be delicate when using a scrub brush on the fractionating column as there are fragile indentations near the bottom joint which can break.