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Diethyl ether is prepared from ethanol (a.k.a grain alcohol, ethyl alcohol,
drinking alcohol) by heating it with concentrated. The reaction proceeds thru
an intermediary, "Ethyl sulfuric acid", as do most reactions of this type.
Preparation 1
by Zaphraud
Dry (anhydrous) or nearly dry ethyl alcohol is allowed to flow into a mixture of
alcohol and sulfuric acid heated to 130 c-140 c. The vapors are collected, and
ether and some alcohol and water condense out. The sulfuric acid is a
catalyst, but since it becomes more and more dilluted as a consequence of
the water produced by the reaction, the process becomes inefficient (which is
why anhydrous ethanol is the best!)
95% ethanol may be recovered from water + CH3CH2OH pulled from the
bottom of the fractioning column (marked 'out')... by connecting it to another
column and distilling it...
This may be converted to 100% ethanol by mixing the 95% with calcium
oxide and distilling - the water is used up to make Calcium hydroxide! This in
turn can be re-fed to the "FEED TANK" after cooling.
Preparation 2
by Eleusis
Though this is not the most pleasant process, Diethyl Ether may be produced
by the condensation of ethanol. To do this, assemble a typical fractional
distillation setup with a vigreux column and a three neck flask. Don't forget to
drop a stirrer magnet into the flask before clamping everthing up, and you
will be heating this on an oil bath (no flames allowed when Ether is around,
you know). The vigreux column goes in the central neck, an addition funnel in
one side beck, and a thermometer goes in the other side neck.
Dump the receiver flask contents into a large beaker or bowl and swirl with
10% Sodium Hydroxide solution until the pH is neutral. Pour this mixture into
a separatory funnel to separate the Ether from the aqueous hydroxide and
wash twice more with equal volumes of half-saturated Sodium Chloride
solution (~18g/100mL of water @ room temp). Let the last wash solution +
Ether rest in the flask until everything has settled, then carefully drain off the
wash, and pour the Ether out of the top into a round bottom flask. Add 15g of
Calcium Chloride (Damp-Rid) for every mole of Ether, drop in stirrer magnet
and stir for 2 hours.
Distill the Ether from the Calcium Chloride by heating on a bath (oil or water)
at no higher than 45C! Collect distillate that comes over in the range of 31-36
C.
Preparation 3
Diethyl Ether
This is also called ethyl ether or ether and must not be confused with
petroleum ether. If, for example, you see a formula calling for ether, then it
refers to diethyl ether, if it does not specify petroleum ether, then do not use
petroleum ether. 100g of ethanol (dry ethanol is best) is placed in a 1/2 liter
distilling flask, and with good cooling, 180g of concentrated sulfuric acid
(98% H2SO4 is added slowly. This flask needs a thermometer fitted, so that
the bulb dips down below the liquid surface. The addition funnel should
extend below the surface, so that the ethanol can be added below the
surface of the acid. Heat and maintain the mixture's temp at 140-145 c by
heating on a sand bath. Ethanol is run in from the addition funnel at the same
rate as the liquid distills over (about 2 drops per second). Mark the flask
before distilling, so that you can be sure of the addition rate. After about
150g of alcohol (ethanol) has been added, stop heating. The distillate will
require the following purification steps: Shake twice with 50 cc of 10% sodium
hydroxide solution, to free from sulfuric acid. Shake twice with 50 cc of
saturated sodium chloride solution, to free from ethanol. The ether is then
dried over anhydrous calcium chloride for 24 hours and distilled on a water
bath, collecting the fraction boiling at 35 C. Yield: 100g.
Anhydrous Ethyl Ether. This is for those formulas calling for dry, pure, or
anhydrous ether. The ether product from above is dried over thin slices of
metallic sodium (metallic sodium wire works well also) for 24 hours. Then the
ether is distilled on a water bath, over fresh (fresh means a different batch
than what you used to dry with) metallic sodium. Note: Ether develops
explosive peroxides upon sitting for any length of time, even if just purchased
from a supply house. Therefore, before handling ether, which has been
stored, shake with ferrous sulphate or with lead peroxide. To keep peroxides
from forming in fresh ether; add several sections of copper or iron wire to the
dark container and store in a cool place.
Ethanol in a tightly closed glass container as it will pick up water from the air
rapidly.