OBJECTIVES :

To provide practical method to separating water from

aqueous methanol mixtures.
To produce refined product uncontaminated.
To yield a significant economic advantage in the
lower cost of equipment and energy.
To invent efficient method by lowering amount of
methanol in residue water.
To obey environmental regulations in chemical
industry.
 THEORY :
According to this invention, water is removed from an initial
mixture comprising methanol and water by subjecting said
mixture to azeotropic fractional distillation in the presence of
sufficient by adding any hydrocarbon compound to form an
azeotrope.
Azeotropic distillation usually refers to the specific technique
of adding another component to generate a new lower-boiling
azeotrope that is heterogeneous by producing two immiscible
liquid phases.
Methanol in free water mixture in vapor form is contacted with
a water-insoluble, normally liquid, hydrocarbon, having a
boiling point substantially not higher than the boiling point of
the alcohol in the mixture, to form an azeotrope.
 The free water which azeotrope has a boiling point differing
from the boiling point of the alcohol thus by a difference
sufficient to allow separation from the alcohol to produce an
essentially anhydrous alcohol.

The water-insoluble hydrocarbon employed in the process of

the present invention may be any which will form with the
water in admixture with alcohol by a difference sufficient to
allow separation of the azeotrope.

Methanol, for instance a difference. Among the suitable water

insoluble hydrocarbons are those generally containing from
about 3 to 8 or 10 carbon atoms, for instance minoring
aromatics, for example benzene, cycloalkanes, cyclopentane,
and alkanes, for example pentane.
 The hydrocarbons can have substituents other than hydrogen and
carbon as long as the substituent does not deleteriously affect the
operation of the water-insoluble hydrocarbon in the present
invention.

The water-insoluble hydrocarbon is contacted with a vaporous

methanol-water mixture in amounts sufficient to remove water
from the mixture. These amounts will depend upon the water-
removing efficiency of the particular water-insoluble
hydrocarbon.

The amount used will depend upon the amount of water in the
vaporous methanol-water mixture at the height of column where
the water-insoluble hydrocarbon is introduced.
 METHODOLOGY:
In a process for separating water from methanol mixture to
produce a methanol product with a reduced water content :

1. The crude aqueous methanol mixture is fed into a distillation

column.
2. Distilling the aqueous methanol mixture in distillation column
to provide a methanol-water vapor, introducing into column a
water-insoluble normally liquid hydrocarbon which forms an
azeotrope.
3. Introducing the aqueous methanol mixture in the presence of
hydrocarbon compound into a distillation tower having a top
portion, an intermediate portion and a bottom portion.
4. At the intermediate portion of the tower maintained at a
temperature of about 90 C to about 95 C to form an
azeotrope comprised of methanol and hydrocarbon compound
and a residue comprised of water.

5. Removing the azeotrope as overhead vapors from the top

portion of the tower at temperature of about 60 C to about
65C.

6. Removing the water residue from the bottom portion of the

tower at a temperature of about 95 C to about 100C.
 DISCUSSION :
A common form of purification for removal of water from
aqueous methanol is fractional distillation.
However, disadvantages of this treatment are that the
equipment for carrying out this treatment has a relatively high
capital cost and the wastewater produced as a residue cannot
have more than a certain proportion of methanol in order to
meet environmental regulations.
Thus, any expedient which can serve to keep the equipment
and therefore its cost as small as possible, and the content of
methanol in the separated water of the residue as low as
possible, is very desirable.
 This is a process in which a methanol-water mixture in vapor
form is contacted with a water-insoluble, normally liquid
hydrocarbon having a boiling point substantially no higher
than the boiling point of methanol, to form an azeotrope
The azeotrope has a boiling point sufficiently different from
that of methanol to accomplish the separation of enough water
from the methanol to produce an essentially anhydrous
alcohol.
It can thus be seen that the process of the invention can yield a
significant economic advantage in the lower cost of
equipment, energy and an environmental advantage due to a
lower amount of methanol in the residue water if such water is
to be discarded.