Improvements in the Manufacture of Acetone.
Year: 1898

page_text: PROVIDIONAL DIECIFICATION.
Improvements in the Manufacture of Acetone.
I, JOSEF LUDWIG HAWLICZEK, of 34, Linnet Lane, Liverpool, in the County
of Lancaster, Manufacturing Chemist, do hereby declare the nature of this inven-
tion to be as follows:-
-
This invention has reference to the manufacture of acetone; and has mainly
for its object to produce it at a cost considerably below that at which it is at
present produced, and, at the same time, to improve the yield of acetone, and its
manufacture generally.
According to the method by which acetone is now generally produced, acetate
salts of an alkaline earth, or metal acetates, are subjected to dry or destructive
distillation. In common practice, however, it is the brown or grey acetate of
lime of commerce which is used for that purpose, owing to its being relatively
cheap, and easily obtained. This acetate of lime is a secondary or by-product
in wood-charcoal making, but, nevertheless, in consequence of the small yield,
and the tedious mode of its manufacture, it commands a high market value.
It has also been attempted to produce acetone by the direct conversion of liquid
acetic acid; but this method of manufacture is not commercially worked.
"
By the present invention, the employment of the expensive materials, referred to,
are obviated, and thus the saving above referred to, is attained; together with
improvements, generally, in the eficiency in the process, or method of manufacture.
According to my invention, I employ as the primary raw material for the
production of acetone, wood, sawdust peat, turf," or any organic substance,
which yields acetic acid on being subjected to destructive distillation: and this
material is treated and subjected to dry or destructive distillation in the manner
hereafter described, with the effect that the acetic acid so obtained is converted
direct at its formation into acetone.
In the manufacture of acetone from substances, as above named, they are
impregnated or conglomerated, as the case may be, with the oxide, hydrated
oxide, or carbonate of an alkaline earth, or similar compounds of certain heavy
metals, or the acetate salts of the same, or such salts of the same groups, which,
on heating, leave behind their respective oxide or carbonate; and the organic
substance, so impregnated or conglomerated, is subjected to the process of dry
or destructive distillation. By this method or process, I find the acetic acid
formed is directly and wholly or nearly wholly converted into acetone, which passes
over as vapour mixed with the other volatile products, such as wood-tar and
methyl-alcohol; these products being all recovered by ordinary condensation.
The liquid products of condensation so obtained are separated from the tar by
decantation, the acetone being separated from the methyl-alcohol by rectification.
The wood charcoal produced by this process is quite suitable for any ordinary
use, and is not inferior in quality to the charcoal made in the ordinary way,
inasmuch as it only contains a slightly higher amount of mineral matter than the
latter one. If, however, charcoal of a very high standard is required, it may

page_text: easily be freed from nearly all mineral contaminations, by merely washing it with
acidified water.
In practice, when lime salts are used, I prefer to make use of them for the
purpose of mixing or impregnating the organic substances; but I do not confine
myself to the use only of lime salts, as the other aforenamed mineral substances
may also be suitable. If wood, peat, or other similar materials be treated, I
would, for example, impregnate them with a strong solution of acetate of lime,
and perform this operation in vacuum; so as to facilitate a perfect admixture of
the fibre of the material with the mineral matter. If sawdust, or a physically
like organic substance is to be treated, I prefer to conglomerate it with hydrated
lime, and form the compound or mass into blocks of convenient size, previous to
being subjected to destructive distillation. However, the employment or applica-
tion of the one mode, or the other, will vary, as the case may individually demand.
Acetone may also be directly produced from wood, or like sustances, by allowing
the combined vapours of the products of dry distillation-as obtained in the
ordinary way to pass over the mineral matters above specified or referred to,
at an elevated temperature; but I prefer (unless to meet special cases) to employ
the process or method first described as being the simpler, and more economical
and satisfactory in every respect.
CHEESBROUGH & ROYSTON,
Applicant's Patent Agents, 15, Water Street, Liverpool.
I, JOSEF LUDWIG HAWLICZEK, of 34, Linnit Lane, Liverpool, in the County
of Lancaster, Manufacturing Chemist, do hereby declare the nature of this inven-
tion and in what manner the same is to be performed, to be particularly described
and ascertained in and by the following statement:--
This invention has reference to the manufacture of acetone; and has mainly
for its object to produce it at a cost considerably below that at which it is at
present produced, and, at the same time, to improve the yield of acetone, and its
manufacture generally.
According to the method by which acetone is now generally produced, acetate
salts of an alkaline earth, or metal acetates, are subjected to dry or destructive
distillation. In common practice, however, it is the brown or grey acetate of
lime of commerce which is used for that purpose, owing to its being relatively
cheap, and easily obtained. This acetate of lime is a secondary or by-product
in wood-charcoal making, but, nevertheless, in consequence of the small yield,
and the tedious mode of its manufacture, it commands a high market value.
It has also been attempted to produce acetone by the direct conversion of liquid
acetic acid; but this method of manufacture is not practicable.
By the present invention, the employment of the expensive materials, referred to,
are obviated, and thus the saving above referred to, is attained; together with
improvements, generally, in the efficiency in the process, or method of manufacture.
According to my invention, I employ as the primary raw material for the
production of acetone, wood, sawdust, peat, turf," or any organic substance
which yields acetic acid on being subjected to destructive distillation; and this,
material is treated and subjected to dry or destructive distillation in the manner

page_text: hereafter described, with the effect that the acetic acid so obtained is directly
converted into acctone.
In the manufacture of acetone from substances, as above named, they are
impregnated, coated, or conglomerated, as the case may be, with the oxide, hydrated
oxide, or carbonate, of an alkaline earth, or similar compounds of certain heavy
metals, or the acetate salts of the same, or such salts of the same groups, which,
on heating, leave behind their respective oxide or carbonate; and the organic
substance, so impregnated, coated, or conglomerated, is subjected to the process
of dry or destructive distillation. By this method or process, I find the acetic
acid formed is directly and wholly, or nearly whoily, converted into acetone. This
actone passes over as vapour mixed with the other volatile products, such as
wood-tar, and methyl-alcohol; these products being all recovered by suitable
condensing apparatus, and collected.
The liquid products of condensation so obtained are separated from the tar
by decantation; the acetone being separated from the methyl-alcohol by rectifica-
tion.
With regard to the alkaline earths referred to, I find that lime, for several
reasons, is one which may be used with advantage; and as regards the metals,
their oxides, or salts of same referred to, lead, zinc, or copper, or their oxides,
or salts, are very suitable, and may be successfully employed.
When wood is employed as the organic substance, the charcoal produced by
this process is quite suitable for any ordinary use, and is not inferior in quality
to the charcoal made in the ordinary way, inasmuch as it only contains a slightly
higher amount of mineral matter than it. If, however, charcoal of a very high
standard is required, it may easily be freed from nearly all mineral contaminations
by merely washing it with acidified water.
In practice, when lime or lime salts are used, I prefer to make use of them for
the purpose of mixing with, coating, or impregnating the organic substance;
but I do not confine myself to the use only of lime or lime salts, as the other
aforenamed mineral substances may also be suitable. If wood, peat, or other
similar material be treated, I may impregnate, mix, or coat it with lime (which
includes hydrated lime) or lime salts; and in some cases where impregnation is
resorted to, I perform this operation in vacuum, so as to facilitate a perfect
impregnation of the fibro of the material with the mineral matter. If sawdust,
or a physically like organic substance is to be treated, prefer to conglomerate
it with hydrated lime, and form the compound or mass into blocks of convenient
size, previous to being subjected to destructive distillation. However, the employ-
ment or application of the one mode, or the other, will vary, as the case may
individually demand.
As a modified method, under this invention, of the method above described,
acetone may also be directly produced from wood, or like substances, by passing
the combined vapours of the products of dry distillation (such as those obtained
in the ordinary way) over or through the mineral matters above specified or
referred to, at an elevated temperature; but I prefer (unless to meet special cases)
to employ the process or method first described as being the simpler, and more
economical and satisfactory in every respect.
A suitable form or construction of distilling apparatus is shewn in the annexed
drawing, in which Figure 1 is a cross section, and Figure 2 a longitudinal section
shewing the inside of the retort chamber, with the outside cover of this chamber
removed, and the lower part in section through A. A Figure 1.
Referring to the drawings, a a are pairs of inclined retorts, is a vertical
bifurcated neck, common to the ends of these pair of retorts, through which the
material to be subjected to destructive distillation is introduced; and are the
charging doors or covers thereon. care furnaces on which the heating fuel is
burned, and d are flame or gas flues communicating with e by the openings c¹; and
with the chambers e above, in which the retorts a are disposed and set.
These chambers e are comprised of the hollow floor of brickwork f having

page_text: checkered openings, and the space f¹ below it, through which the gases pass to
the chamber space e; an outer cover wall g; and end or, division walls h. The
chamber walls of e overhang the base work of the structure, as shewn by the
drawing, and are largely supported from below by the columns i and brackets
or girders, the upper plates of which extend from one support to another.
Through these plates, j', the ends of the retort a project, they being largely
supported by these plates by means of projecting ledges a¹ on their back sides,
which rest on the inside of the plates. The outer cover walls g rest at one end
on the outer edges of the plates g'; and at the other, upon a girder & above; and
they have linings of iron, which rest on these supports. By this construction,
these outer cover walls g' can be readily taken down and put in place.
Above the girders there is a dome or roof l, enclosing the upper bifurcated
branches of the retorts.
In action, fire gases pass from the furnace e up into the space f¹ below the
floor f, and thus through these spaces in the said floor into the chamber e; and
they pass from this chamber by an opening m in the upper part of the walls m¹.
By this wall m', and its upper outlet opening, and the distributing floor f, the
flow of gases into the chamber e, and the heating action upon the retorts a, is
well distributed and fairly equalized; and the uniform distillation of the materials
in the retort accomplished.
The heating gases, in passing into the upper part of the apparatus pass away
into the downtake flues to the flues s below, by which they are conducted away
from the apparatus to the chimney.
As regards the distilling action, volatile matters are driven off from the
materials with which the retorts are charged, and the vapours or gases of distilla-
tion pass up from the charge into the neck b, and away by pipes o into the main p
to the condensers--which will be of any known suitable kind. The material to be
distilled is charged into the retorts through the charging doors or covers 61, and
neck ; and after the volatile constituents of the materials are distilled, the
charcoal or carbon remaining is discharged from the retorts by opening the lower
retort doors, whereupon the discharge of this charcoal or carbon will be
automatic, by reason of their angle of inclination being greater than the angle of
repose of this material.
In the case of the modified method of manufacture of acetone, wherein the
wood is first subjected to distillation, and the vapours of distillation are then
passed over the mineral matters at an elevated temperature, the apparatus sub-
stantially as shewn and described, may be employed in carrying it out. In one
case the alkaline earth or heavy metal, in any suitable physical form may be
placed directly on top of, or mixed in amongst the wood or organic substance in
the retorts. Or there may be employed in the brickwork setting of the plant,
other retorts or chambers heated by the heating gases, for, and containing the
mineral substance, through which substance, while in a highly heated state, the
products of distillation are passed directly from the distilling portion of the
apparatus.
Having now particularly described and ascertained the nature of this
invention and in what manner the same is to be performed, I declare that what
I claim is:
1. The manufacture of acetone substantially as herein described, namely, the
manufacture direct from an organic substance yielding acetic acid on being
heated, by subjecting such substance to distillation in closed chambers or vessels,
and bringing the products of distillation directly into contact with an alkaline
earth, as the oxide, hydrated oxide, or carbonate of such earth, or, with the
compounds of heavy metals, such as referred to, which on heating leave behind
their oxide or carbonate.
2. In the manufacture of acetone, the herein described process consisting in
incorporating or combining an organic substance as described with an alkaline

page_text: earth, as the oxide, hydrated oxide, or carbonate of such earth, or, with the
compounds of heavy metals, such as referred to, which on heating, leave behind
their oxide or carbonate; subjecting these combined substances to heat in a
closed externally heated vessel: and subsequently artificially cooling the said
resultant vapours and gases of distillation.
3. The manufacture of acetone direct from wood, or woody substances, and lime,
by subjecting such substances to heat in closed vessels, and bringing the products
of distillation of the wood or woody substance directly into contact with the lime ;
substantially as set forth.
Dated his 20th love of A 1900
CHEESBROUGH & ROYSTON,
Applicant's Patent Agents, 15, Water Street, Liverpool.