IMPROVEMENTS IN THE PRE- PARATION AND TREATMENT OF SACCHARINE SUBSTANCES AND COMPOUNDS
Year: 1878

page_text: LETTERS PATENT to Astley Paston Price, of 47, Lincoln's Inn Fields, in the
County of Middlesex, for the Invention of "IMPROVEMENTS IN THE PRE-
PARATION AND TREATMENT OF SACCHARINE SUBSTANCES AND COMPOUNDS."
communication from abroad by Moriz Weinrich, of Vienna, in the Empire of
Austria.
Sealed the 24th January 1879, and dated the 17th August 1878.
PROVISIONAL SPECIFICATION left by the said Astley Paston Price at the
Office of the Commissioners of Patents on the 17th August 1878.
ASTLEY PASTON PRICE, of 47, Lincoln's Inn Fields, in the County of Middlesex,.
"IMPROVEMENTS IN THE PREPARATION AND TREATMENT OF SACCHARINE SUBSTANCES
AND COMPOUNDS." A communication from abroad by Moriz Weinrich, of Vienna,
in the Empire of Austria.
This process has for its object the preparation of saccharate of lime by lixiviating:
a combination of molasses and lime, hereafter called melassate of lime, the same
being formed by mixing directly the warm molasses or syrups with the necessary
quantity of dry slaked lime (powdered hydrate of lime) in about the proportion.
required to form tribassic saccharate of lime.
The resulting melassate of lime hardens by itself, without any further drying, to
a compact homogenous and friable mass easily reduced to a gravelly form or into
powder. In this form when brought into a mixing apparatus and mixed with
alcohol a sandish mass is obtained, that I call sandy melassate of lime, which pre-
sents in consequence of the smallness and granular condition of its molecules great
advantages for lixiviation with alcohol, even of high concentration, and preserves its.
sandish nature, without opposing any difficulty to further operations by agglom-
erating.
The sandy melassate of lime prepared by this process is capable of being com-
pletely lixiviated in the mixing apparatus, thus effecting a considerable saving of
time and plant. Further, the mixed sand can be brought in separate filter tanks or

page_text: macerating vessels (elutors) for further lixiviation, after which the purified
saccharate of lime is freed from alcohol by distillation, and thus rendered suitable
for further treatment.
In carrying out my Invention I place in suitable mixing apparatus a certain
quantity of molasses or syrups, which are then heated to about 100° centigrade
(212° Fahrenheit), and I mix the same intimately with a certain quantity of dry
slaked lime (viz., dry hydrate of lime) in the state of fine powder.
The proportion of hydrate of lime to the molasses to be treated will depend upon
the amount of sugar contained therein, and partly also upon the purity of the lime,
but generally as a rule about 1 cwt. of the sugar contained in a certain quantity of
molasses will require about one half hundredweight of lime calculated in its anhy-
The impure
drous condition, my object being to form tribasic saccharate of lime.
saccharate of lime thus resulting is placed in suitable vessels, which by preference
are removed to or are contained in a heated room.
After about 20 hours the melassate of lime will stiffen to a dry, hard, compact,
and brittle mass that can be easily removed from the moulds and reduced into
pieces. These pieces it will be found advantageous to pass through a breaking
machine, where the pieces are further reduced to about the size of a walnut.
In order further to reduce the pieces into a finer or pulverulent condition a Carr's
disintegrator may be employed.
The melassate of lime being brought to this state it cannot yet be directly sub-
mitted to lixiviation, but has to undergo a preliminary operation in order to obtain
this peculiar sandish condition, in which it is especially convenient for lixiviation,
and called by me sandy melassate of lime.
I effect this in the following manner :-I partially fill a vessel closed at the top
by a cover, and provided with a mixing mechanism with alcohol, and whilst the
mixing arms are moving I introduce the broken melassate of lime, so that it is
mixed quite uniformly with the alcoholic fluid, and receives thereby its sandish or
granular character, and which will be found to possess greater facility for lixivia-
tion than melassate of lime prepared by the ordinary processes.
I can use for the complete lixiviation of the sandy melassate of lime the same
mixing tank in which the preliminary admixture was effected of the melassate of
lime with alcohol, and for this purpose I employ by preference a mixing apparatus
herein-after described, but other apparatus may be employed.
The mixing apparatus consists of a tank with a false bottom of narrow sieves,
and an interposed filter of linen or canvas cloth, above which the finely broken
melassate of lime is introduced by means of a funnel-shaped orifice, the alcohol
having been introduced by means of a cock. At the same time the mixing mechan-.
ism is put in motion by means of bevel wheels.
After a few minutes the mixture assumes the peculiar form of my sandy mel-
lassate of lime, and can then be lixiviated in a tranquil state in any convenient
tank. But I generally prefer to carry on the process of lixiviation in the same
mixing tank by rotating the mixing arms continuously, and after some time
drawing off the alcoholic solution charged with impurities by means of a cock,
whilst a further supply of fresh alcohol is introduced. Thus beginning with a con-
centrated alcohol of about 70% and finishing the operation with a feebler alcohol
of about 40% the sandy melassate of lime will be almost completely lixiviated and
purified in about from 10 to 12 hours, after which the sandish mass is drawn off
by means of a sliding shutter into one or into several suitable vessels, from which
the alcohol flows off, and which may subsequently be distilled by means of
steam.
It is to be remarked that the alcohol used for the admixture of the melassate of
lime need not be pure; it may be slightly charged with impurities from preceding
operations, the use of such alcohol being more economical at the commencement of
lixiviation. Thus the whole process can be so arranged that only fully-charged
solutions are submitted to distillation.

page_text: The lixiviated sandy melassate of lime will be found to consist of purified
saccharate of lime, and after being freed from the remaining alcohol by distillation
is dissolved, either by means of water or steam, and the resulting solution is con-
ducted into the saturating vessels for the treatment of beetroot juice, or it may be
directly utilized for the production of sugar by the decomposition of the saccharate.
The impure alcoholic solutions being drawn from the mixing or lixiviating vessels
are submitted to distillation by steam in a suitable apparatus.
The alcohol obtained from the distillation of any of the products resulting from
any of the before-mentioned operations may, as is well understood, be re-utilized.
As a substitute for mixing tanks or elutors the lixiviation of the sandy melassate
of lime may be effected in a filter press.
Under the term of alcohol as used in this my Provisional Specification I include
both methyl alcohol and ordinary alcohol, or similar bodies or mixtures of the
same.
What I wish to be understood as sandy melassate of lime is the melassate of lime
resulting from the foregoing process, and which when in a state of division upon
being submitted to the action of alcohol assumes a granulated form or condition.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said Astley. Paston Price in the Great Seal Patent Office on the 11th
February 1879.
1
ASTLEY PASTON PRICE, of 47, Lincoln's Inn Fields, in the County of Middlesex.
"IMPROVEMENTS IN THE PREPARATION AND TREATMENT OF SACCHARINE SUBSTANCES
AND COMPOUNDS." A communication from abroad by Moriz Weinrich, of Vienna,
in the Empire of Austria.
"
:
The said Invention relates to a process having for its object the preparation of
saccharate of lime by lixiviating a combination of molasses and lime, herein-after
called "melassate of lime," the same being formed by mixing directly the warm
inolasses or syrups with the necessary quantity of dry slaked lime (powdered
hydrate of lime) in about the proportion required to form tribasic saccharate of
lime.
The resulting "melassate of lime" hardens by itself without any further drying
to a compact homogenous dry and friable mass, easily reduced to a gravelly form or
into powder. In this form, when introduced into a mixing apparatus and mixed
with alcohol, a sandish mass is obtained, herein-after termed "sandy melassate of
lime," which presents in consequence of the smallness and granular condition of its
molecules great advantages for lixiviation with alcohol even of high concentration,
and preserves its sandish nature without opposing any difficulty by agglomerating
to further operations.
The sandy melassate of lime prepared by this process is capable of being com-
pletely lixiviated in the apparatus in which the preliminary mixing with alcohol is
carried out, thus effecting a considerable saving of time and plant, or the sandy
melassate of lime may be conducted into filter tanks or macerating vessels (elutors)
for further lixiviation. In either case after having been completely lixiviated the
purified saccharate of lime is freed from alcohol by distillation, and thus rendered
suitable for further treatment.
In carrying out the said Invention there is placed in a suitable mixing apparatus
a certain quantity of molasses or syrups, which is heated to say from about 85° to
100° centigrade, and the same is intimately mixed with a certain quantity of dry
slaked lime (videlicit, dry hydrate of lime) in the state of fine powder.
The proportion of hydrate of lime to the molasses to be treated will depend upon
the amount of sugar combined therein, and partly also upon the purity of the lime,
but generally as a rule about 1 cwt. of the sugar contained in a certain quantity of
molasses will require about one-half hundredweight of lime, calculated in its
anhydrous condition, the object being to form tribasic saccharate of lime. The
impure saccharate of lime thus resulting is placed in suitable vessels, which by
preference are removed to or are contained in a room, which may be a little
warmed, by itself, without using any artificial drying.
After the lapse of, say, about 20 hours, the melassate of lime will have stiffened to
a dry, hard, compact, and brittle mass capable of being removed from the mould
and reduced into pieces with facility. These pieces it will be found advantageous to
pass through a breaking machine, in which the pieces are further reduced to say
about the size of a walnut. In order further to reduce the pieces into a finer or
pulverulent condition a Carr's disintegrator may be employed.
The melassate of lime having been brought to this state it cannot yet be directly
submitted to lixiviation, but has to undergo a preliminary operation in order to
obtain the peculiar sandish condition herein-before referred to, in which it is
especially convenient for lixiviation. This preliminary operation is carried out in
the following manner:-A vessel is employed closed at the top by a cover and
provided with a mixing mechanism. This vessel is filled with alcohol, and the
inixing mechanism being set in motion the broken melassate of lime is intro-
duced, so that it is mixed quite uniformly with the alcoholic fluid, and receives

page_text: thereby its sandish or granular character, which renders it more susceptible of
lixiviation than melassate of lime prepared by the ordinary processes.
In effecting the complete lixiviation of the sandy melassate of lime the same
mixing tank may be used in which the preliminary admixture was effected of the
melassate of lime with alcohol. This mixing apparatus may be constructed in any
suitable manner, but it is preferred to employ for the purpose an apparatus of the
construction shewn in vertical section in the accompanying Drawing, and. next
lierein-after described.
This mixing apparatus consists of a tank a with a perforated false bottom b of a
fine mesh, covered with a layer c of linen or canvas cloth; in bearings in the bottom
and the cover of this tank is mounted a vertical shaft & carrying mixing arms cand
a bevel wheel f, with which latter engages a bevel pinion g for transmitting motion
from any suitable prime mover. The tank is filled with alcohol by means of a
cock h, and the mixing mechanism having been put in motion the finely broken
melassate of lime is introduced on to the filtering layer c through a funnel-shaped
orifice i.
After the lapse of, say, a few minutes the mixture assumes the peculiar form of
the sandy melassato of lime, and can then be lixiviated in a tranquil state in any
convenient tank. It is generally preferred however to carry on the process of
lixiviation in the same mixing tank by rotating the mixing arms continuously, and
after some time drawing off the alcoholic solution charged with impurities by
means of a cock k, whilst a further supply of fresh alcohol is introduced through
the cock h; thus commencing with a concentrated alcohol of about 70% or of
slightly less strength, and finishing the operation with a feebler alcohol of about
40%, the sandy melassate of lime will be almost completely lixiviated and purified
in, say, about from 10 to 12 hours, after which the sandish mass is drawn off
through an opening at 6 (normally closed by a sliding valve) into one or more
suitable vessels, from which the alcohol flows off, to be subsequently distilled by
means of steam.
It is to be remarked that it is not necessary that the alcohol used for the
admixture of the melassate of lime should be pure, it may be slightly charged with
impurities from preceding operations, the use of such alcohol being more enonomical
at the commencement of lixiviation. Thus the whole process can be so arranged
that only fully charged solutions are submitted to distillation.
The lixiviated sandy inelassate of lime will be found to consist of purified
saccharate of lime, and after being freed from the remaining alcohol by distillation
is dissolved either by means of water or steam; and the resulting solution is con-
ducted into the saturating vessels for the treatment of beetroot juice, or it may
be directly utilized for the production of sugar by the decomposition of the
saccharato.
The impure alcoholic solutions being drawn from the mixing or lixiviating
vessels are submitted to distillation by steam in a suitable apparatus.
The alcohol obtained from the distillation of any of the products resulting from
any of the before-mentioned operations may, as is well understood, be re-utilized.
As a substitute for mixing tanks or elutors the lixiviation of the sandy melassate
of lime may be effected in a filter press or Taylor filters suitably prepared for this
process.
Under the term of alcohol, as used in this my Specification, I include both
methyl alcohol and ordinary alcohol, or similar bodies or mixtures of the same.
What I wish to be understood as sandy melassate of lime is the melassate of
lime resulting from the foregoing process, and which, when in a state of division,
upon being submitted to the action of alcohol assumes a granular form or
condition.
Having now described and particularly ascertained the nature of the said
Invention, and the manner in which the same is or may be used or carried into
effect, I would observe in conclusion that what I consider to be novel and original,
and therefore claim as the Invention secured to me by the herein-before in part

page_text: recited Letters Patent is, the preparation of saccharate of lime by first mixing
together warm molasses or syrups with dry slaked lime (powdered hydrate of lime,
so as to form a hard, solid, dry, and compact "melassate of lime," and then reducing
such melassate of lime in the manner herein-before described, and mixing it in its
reduced form with alcohol or alcoholic liquids, so as to form what I designate sandy
melassate of lime, and finally converting the latter into saccharate of lime by
lixiviating it with alcohol or alcoholic liquids, substantially as herein-before
described.
In witness whereof, I, the said Astley Paston Price, have to this my Speci-
fication set my hand and seal, this Eighth day of February, One thousand
eight hundred and seventy-nine.