Year: 1898

page_text: Date of Application, 3rd Feb., 1898
Complete Specification Left, 2nd Nov., 1898-Accepted, 17th Dec., 1898
For the success of this process it is necessary that the vapours of the acetic acid
be brought into intimate contact with the carbonate employed. As the said
carbonate crumbles and becomes reduced to a fine powder, this powder must be
brought into intimate contact with the vapours by means of mechanical agitators.or
stirrers, which involves the use of numerous stuffing boxes or of trunnions, which are a
source of leakage in the apparatus; either vapours of acetic acid or of acetone
escaping outwards, or atmospheric air leaking into the apparatus, according to the
pressure within and without the apparatus, and causing serious losses.
According to this invention we obviate these objections by passing the vapours
of acetic acid in air tight vessels over fragments of porous substances such for
example as pumice stone, bricks, or the like, the pores of which have been filled with
the carbonate of an alkaline earth (carbonate of lime or of baryta for instance).
Such fragments of pumice stone, or the like, we immerse in a strong solution of the.
acetate of the base, the carbonate of which we wish to produce in the pores of the
pumice stone, or the like, say in a solution of acetate of lime. We then dry
the fragments of pumice stone, or the like, and, if we find they are not sufficiently
rich in acetate, we repeat the operation, or boil a portion of the solution down to
dryness with the fragments of punice stone, or the like. The dry fragments are
then placed in the apparatus serving for the conversion of acetic acid into acetone,
and are there heated to about 500 degrees centigrade, when the acetate is
decomposed yielding acetoue, and leaving within the pores of the pumice stone, or
the like, the desired carbonate.
The apparatus for the conversion of the vapours of acetic acid into acetone (which
we term the "decomposer") consists of an oven capable of being heated to a
temperature approaching a red heat, within which is or are disposed a tubular retort

page_text: one to the other.
or tubular retorts, preferably in an inclined or vertical position. They may be made
of cast iron and are each provided with an inlet for the admission of acetic acid
vapours with an outlet for the exit of the acetone vapours, and with apertures
capable of being closed for charging and discharging the fragments of pumice stone
or the like.
Several retorts may be so joined together that the vapours pass from
When the retorts have been filled with the fragments of pumice stone or the like
prepared as herein before described, the decomposer is heated to a temperature of
about 500 degrees Centigrade and is then ready for the passage through it of the
heated acetic acid vapour which may be generated in an ordinary still from ordinary
acetic acid and the waste heat from the decomposer may be used to heat the still
and the vapours. The vapours are passed through the retorts at such a speed that
most of the acetic acid is split up into acetone, water, and carbonic acid, as indicated
by the equation hereinbefore given.
The gases issuing from the decomposer consist of vapours of undecomposed acid
of acetone, of water, and of carbonic acid. We cause these vapours to pass through
an ordinary cooling worm wherein the water, the acetic acid, and much of the
acetone condense. The carbonic acid together with the remainder of the acetone
vapours, are led to a scrubber, or washing apparatus, where the gas is freed from
acetone by washing with water. We prefer to cause the gas to bubble through the
water.
The two solutions of acetone thus obtained are mixed, the acetic acid is neutralised
with a suitable base (soda or lime) the acetone is distilled off, and then purified by
redistilling and fractionating.
The acetate in the residual solution can be recovered by evaporation.
Improvements in the Manufacture of Acetone and in Apparatus
therefor.
We, HANNAH HURTER, of Holly Lodge, Cressington Park, near Liverpool, in the
County of Lancaster, Widow, Executrix and Legal Representative of Ferdinand
Hurter, Ph.D., deceased, late of G 11, Exchange Buildings, Liverpool aforesaid,
Chemist, and THE UNITED ALKALI COMPANY, LIMITED, of G 11, Exchange Buildings
aforesaid, do hereby declare the nature of this invention and in what manner the
same is to be performed, to be particularly described and ascertained in and by
the following statement:-
Acetone has been manufactured by submitting an acetate to a process of dry
distillation, vapours of acetone mixed with steam being obtained, these vapours
being condensed and a carbonate remaining in the retort.
It has been proposed to manufacture acetone by passing the vapours of acetic
acid over a carbonate of the alkaline earths at an elevated temperature (see
"Journal of Society of Chemical Industry" Vol. XV (1896) p. 612) the acetic acid
vapours being decomposed and yielding a mixture of vapours of acetone, of water,
and of carbonic acid according to the following equation:

page_text: For the success of this process it is necessary that the vapours of the acetic acid
be brought into intimate contact with the carbonate employed. As the said
carbonate crumbles and becomes reduced to a fine powder, this powder must be
brought into intimate contact with the vapours by means of mechanical agitators
or stirrers, which involves the use of numerous stuffing boxes or of trunnions which
are a source of leakage in the apparatus; either vapours of acetic acid or of acetone
escaping outwards, or atmospheric air leaking into the apparatus, according to the
pressure within and without the apparatus, and causing serious losses.
According to this invention we obviate these objections by passing the vapours
of acetic acid in air tight vessels over fragments of porous-substances such, for
example, as pumice stone, bricks, or the like, the pores of which have been filled
with the carbonate of an alkaline earth (carbonate of lime or of baryta for instance).
Such fragments of pumice stone or the like we immerse in a strong solution of the
acetate of the base, the carbonate of which we wish to produce in the pores of the
pumice stone or the like, say in a solution of acetate of lime. We then dry the
fragments of pumice stone or the like and, if we find they are not sufficiently rich
in acetate, we repeat the operation, or boil a portion of the solution down to dryness
with the fragments of pumice stone or the like. The dry fragments are then
placed in the apparatus serving for the conversion of acetic acid into acetone, and
are there heated to about 500 degrees Centigrade, when the acetate is decomposed
yielding acetone, and leaving within the pores of the pumice stone or the like the
desired carbonate.
The apparatus for the conversion of the vapours of acetic acid into acetone
(which we term the "decomposer") consists of an oven capable of being heated to
a temperature approaching a red heat, within which is or are disposed a tubular
retort or tubular retorts; preferably in an inclined or vertical position. They may
be made of cast iron and are each provided with an inlet for the admission of
acetic acid vapours with an outlet for the exit of the acetone vapours, and with
apertures capable of being closed for charging and discharging the fragments of
pumice stone or the like. Several retorts may be so joined together that the vapours
pass from one to the other.
When the retorts have been filled with the fragments of pumice stone or the like
prepared as hereinbefore described, the decomposer is heated to a temperature of
about 500 degrees Centigrade and is then ready for the passage through it of the
heated acetic acid vapour which may be generated in an ordinary still from ordinary
acetic acid and the waste heat from the decomposer may be used to heat the still
and the vapours. The vapours are passed through the retorts at such a speed, that
most of the acetic acid is split up into acetone, water, and carbonic acid, as indicated
by the equation hereinbefore given.
The gases issuing from the decomposer consist of vapours of undecomposed
acetic acid, of acetone, of water, and of carbonic acid. We cause these vapours to
pass through an ordinary cooling worm wherein the water, the acetic acid, and
much of the acetone condense. The carbonic acid, together with the remainder
of the acetone vapours are led to a scrubber, or washing apparatus, where the gas
is freed from acetone by washing with water. We prefer to cause the gas to
bubble through the water.
The two solutions of acetone thus obtained are mixed, the acetic acid is
neutralized with a suitable base (soda or lime) the acetone is distilled off, and then
purified by redistilling and fractionating.
The acetate in the residual solution can be recovered by evaporation.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, we declare that what we
claim is
1. In the manufacture of acetone, passing the vapours of acetic acid over, or in
contact, with fragments of porous substance, such as pumice stone, bricks or the

page_text: like, the pores of which have been filled with the carbonate of an alkaline earth
substantially as herein before described.
2. For use in the manufacture of acetone, porous substances such for example as
pumice stone, bricks or the like, having the pores thereof filled with an alkaline
earth by immersing the said porous substances in a strong solution of the acetate
of the base of the carbonate with which it is desired to fill the pores substantially as
herein before described.
3. In the manufacture of acetone, passing the vapours of acetic acid through a
vessel or chamber containing porous substances having the pores thereof filled with
the carbonate of an alkaline earth and heated to a temperature of say about 500
degrees Centigrade substantially as herein before described.
Dated this 2nd day of November 1898.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.