of Saccharine Solutions with the Alkaline Earths.
Year: 1885

page_text: of Saccharine Solutions with the Alkaline Earths.
2
I, CHARLES DENTON ABEL of No 28 Southampton Buildings, Chancery Lane, in
the county of Middlesex Consulting Engineer and Patent Agent, do hereby
declare the nature of my invention for "IMPROVEMENTS IN THE PRODUCTION OF
SUGAR BY THE TREATMENT OF SACCHARINE SOLUTIONS WITH THE ALKALINE
EARTHS (a communication from Marc Maurice Rotten of N° 97 Koniggratzer-
strasse, Berlin in the Empire of Germany, Engineer) to be as follows:-
"
The present invention relates to improvements in a method for the extraction or
the separation of sugar from strongly concentrated, impure solutions by means of.
alkaline earths.
All methods of extracting or separating sugar as yet known and based on the
formation of saccharates of alkaline earths render the separation of sugar only
possible from diluted solutions, it being necessary that either the solution of sugar
from which the extraction or separation is to be effected shall shall have only a
low degree of concentration, or that the reagent shall be used in the shape of hot
aqueous-lye (baryta and strontia-lye) or mixed with water (milk-of-lime or line-
paste). Every method for extracting or separating sugar that requires the use of
diluted solutions has naturally the one disadvantage that the quantity of non-
saccharine lye. is very great and thus, even if the quantity of sugar contained in
it be small, the loss of sugar is considerable and the working up and utilisation of
the dilute non-saccharine lye (residuum) combined with great expense.
These defects, as also a series of other disadvantages common to all the methods
just mentioned, and more evident in some than in others, are avoided by the
present invention, which allows of the extraction or separation of sugar with the
employment of the smallest possible quantity of water, and which thus.constitutes
a method of extraction or separation of sugar from strongly concentrated solutions.
This method is based on an observation made in a series of experiments, that
sugar in strongly concentrated solutions, in which its nolecules are comparatively
close together, has a far greater affinity for the hydrates of the alkaline earths and
a much greater inclination to form saccharates than when in diluted solutions.

page_text: The following method in which the application of strontia is described, requires
only a simple mixture of the sugar in a strongly concentrated solution, such as is
found in molasses or the "filling mass," with the base in a solid or compact formi.
It has been ascertained that the contact of the dry-strontia with the strongly
concentrated sugar solution effects even at the ordinary temperature a very
rapid formation of saccharates, which is not be be attained when solutions are
employed.
Among the forms in which strontia can possibly be applied (pulverised oxide of
strontia, hydrate of strontia and crystallised strontia) the product which arises
from the slaking of calcined strontia, the dihydrate of strontia, deserves the
preference.
This dihydrate of strontia is produced in the following manner. Caustic strontia
in lumps as it comes from the furnace is exposed to a fine spray of water or of
aqueous vapor; the porous calcined mass sucks up the water eagerly, turns white,
and developing a quantity of steam, crumbles into a white crystalline powder..
All excess of water that has been added evaporates and, if too great an abundance
of water has been avoided, there remains only so much water in the strontia as
corresponds with the formula Sr O, 2 H, O.
The hydrate of Strontia (Sr O, H, O) obtained in the well known manner or
the crystals of the nine times hydrated strontia Sr O, 9 H, O. can likewise be used
advantageously, whereas with pulverised non-hydrated caustic strontia or with hot
concentrated lye of caustic strontia quite apart from the fact that the production
of the last named is much more complicated than that of the dihydrate), a
corresponding reaction according to the present method can only be produced with
difficulty and after a long time, as heating ensues in this case and the complete
formation of the saccharates is consequently retarded. Owing to the considerable
quantity of water contained in the strontia lye and to the heating produced by the
high temperature of the concentrated lye, or by the hydration of the caustic
strontia, the mass also becomes so watery, that it fails to have that consistency
which is requisite for a quick and complete formation of saccharates.
A certain paste-like consistency of the mixture as also an energetic stirring up
thereof is very material for the complete success of the process of making strontia-
sugar according to this method, otherwise the strontia, owing to its greater specific
gravity, would fall to the bottom and thus be removed from the reaction.
Under
the conditions just stated the strontia saccharate is formed by the method herein-
after described in a time of such short duration (to hour) as could not be
attained if solutions and the same small quantities of strontia were used.
The practical carrying out of this method would be, according to what has just
been said, as follows:-The thick semi-liquid or tacky solution of sugar (molasses,
filling mass etc.) containing from 40 to 60 per cent of sugar, is well mixed up with
pulverised strontia for the purpose of forming the saccharates.
Apparatus are used for this similar to those employed in the manufacture of
sugar for cutting up firm or compact filling masses in general, that is to say
strongly constructed stirring machines with strong arms for cutting and mixing up
the thick semi-liquid, viscous matter. However, any apparatus that causes a
strong stirring motion and incorporation can be used for this purpose. The amount
of strontia that is added is regulated by the amount of sugar contained so that, for
each 100 lbs of sugar, 40 lbs of hydrate of strontia are added, or for each
equivalent of sugar, one equivalent of oxide of strontium (Sr O) is employed.
According to the concentration of the sugar solution and to the energy of the
stirring, the formation of the saccharate ensues within the limits stated more or
less quickly, but it is mostly completed, (especially if dihydrate is applied), within
a quarter of an hour, which is manifested by the clear almost white color and
homogeneous thick paste-like condition of the inass. When this appearance shews
itself, the mass is mixed in the same apparatus with as much water or as much of
the fluid gained from the washing out of the saccharate, as will render it sufficiently
liquid to be forced by means of a pump into the strongly constructed filter-presses

page_text: into which the mass is admitted from the mixing apparatus in this state. The
impure saccharate that remains on the sides of the filter-press, after the expressing,
is clarified with pure water or the water containing strontia of the remainder of
the non-saccharine parts. The wash-water thus obtained can always be used for
washing fresh quantities of the saccharate.
The first non-saccharine lye that runs off can, if it is not concentrated enough,
be used in a similar manner; but after being used a second time, and when the
strontia is removed, it has generally a specific weight of from 40° to 45° Brix and
therefore represents a highly concentrated residuum.
The washed-out saccharate, obtained in the manner just described, and which
contains about one equivalent of sugar to one equivalent of strontia, is easily
soluble in hot water and even more so in hot saccharine water, and this solubility
is taken advantage of to separate the insoluble impurities (particles of slag,
carbonate sulphate and phosphate of strontia). The best way of doing this is to
let the hot solutions of saccharate settle in high vessels and after decantation of
the clear solution, to boil the insoluble parts lying at the bottom once more in
water and separate them from the liquid by means of filter-presses, suction-
filters etc. The clear solution of saccharate thus obtained is disengaged from the
strontia by introducing carbonic acid, and the carbonate of strontia thus detached
is worked up again into caustic strontia according to the well known methods. By
this means, and especially if solutions of sugar are used for dissolving the
saccharate, a tolerably concentrated liquor is obtained, which contains from
20% to 30% of sugar of excellent purity.
According to this method more than 90% of the sugar contained in the
molasses, filling mass etc, are extracted if the impure lye (residuum) is only used
once over again for mashing saccharates.
The lye that remains after the extraction of the saccharate contains, in addition
to all the so-called non-saccharine parts a greater or smaller quantity of sugar,
glucose, strontia, lime and a little free ammonia, according to the material used.
These substances can according to circumstances, be neglected and these lyes
(residuum) may be worked up direct in the well known way into raw potashes or
manure. But in most cases it will be advantageous to separate and extract the
one or the other of the substances just named. The most advisable way of doing
this is to add a quantity of spirits to the cold residuum and in such proportion
that a spirit solution of at least 50% is formed. By this means, if there is a
sufficient quantity of strontia or lime the saccharates and glucose parts which do
not dissolve easily in spirits are precipitated. Any superfluous or additional
strontia is likewise in so far separated by the addition of spirits that, at the
most, th toth per cent of Sr O remains in the solution. The precipitate can be
separated by decantation, filter-presses and suction filters from the fluid, and in so
far as it consists of sugar or strontia it is used again in the way described in the
process of extraction. If the precipitate contains large quantity of glucose (which
will shew itself regularly whenever molasses containing glucose, particularly
osmosed molasses, refined or cane sugar inolasses are used) the glucose is extracted
separately by decomposing the gluensate by the introduction of carbonic acid.
The residuum containing spirits is freed from spirits and ammonia by distillation
in the well known manner and is then used for making fuel manure etc.
When strontia containing lime or molasses rich in lime-compounds are used, the
whole amount of lime contained in them is found again in the residuum lye. If
these lyes have taken up so much lime that the carbonate of strontia extracted
from them by saturation or the saccharate precipitated by spirits are rendered too
impure by lime and accordingly furnish a strontia preparation mixed with excess
of lime (which, owing to the great solubility of sugar-lime, would lessen the
extract of sugar) it is advisable to proceed to a separation of the lime from the
strontia. This can be effected by amalgamating with alkaline hydrate (caustic
solution of residuum carbon) either the non-saccharine lye containing lime before
its treatment with spirits, or the hydrated solution of the precipitate produced by

page_text: spirits, whereby hydrate of strontia alone is crystallised; or again, the two solutions
just mentioned can be subjected to a treatment with insufficient quantities of
carbonic acid, which gives rise to a precipitate consisting chiefly of carbonate of
lime with very little strontia, whereas in the further saturation that follows, a
carbonate of strontia, tolerably free from lime is precipitated.
The following advantages may be claimed for the method just described :-
1. The simplicity of the method of proceeding combined with the short
duration of the operation till the pure solution of sugar is obtained.
.
2. The perfect manner in which the strontia employed is turned to account,
which substance when mixed with sugar, dissolves easier and more perfectly than
it does with water alone.
3. The avoidance of lixiviation apparatus and crystallisation vessels for the
.production of strontia crystals.
4. The avoidance of all heating and artificial cooling.
5. The extraction of refuse lye in a highly concentrated form.
6. The extraction of all valuable substances otherwise remaining in the
-residuum, especially of strontia in the shape of caustic strontia.

page_text: Saccharine Solutions with the Alkaline Earths.
I, CHARLES DENTON ABEL of No 28 Southampton Buildings Chancery Lane in
the County of Middlesex, Consulting Engineer and Patent Agent 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:-
The present invention relates to improvements in a method for the extraction or
the separation of sugar from strongly concentrated impure solutions by means of
alkaline earths.
All methods of extracting or separating sugar as yet known and based on the
formation of saccharates of alkaline earths render the separation of sugar only
possible from diluted solutions it being necessary that either, the solution of sugar
from which the extraction or separation is to be effected shall have only a low
degree of concentration or that the reagent shall be used in the shape of hot
aqueous lye (baryta and strontia lye) or mixed with water (milk of lime or lime
paste). Every method for extracting or preparing sugar that requires the use of
diluted solutions has naturally the one disadvantage that the quantity of non-
saccharine lye is very great and thus even if the quantity of sugar contained in it
be small the loss of sugar is considerable and the working up and utilisation of the
dilute non-saccharine lye (residuum) combined with great expense.
These defects, common to all the methods just mentioned, as also a series of
other disadvantages which are more evident in some than in others, are avoided by
the present invention which allows of the extraction or separation of sugar with
the employment of the smallest possible quantity of water, and which thus
constitutes a method of extraction or separation of sugar from strongly concentrated
solutions.
This method is based on an observation made in a series of experiments that
sugar in strongly concentrated solutions in which its molecules are comparatively
close together has a far greater affinity for the hydrates of the alkaline earths and
a much greater inclination to form saccharates than when in diluted solutions.
The following method, in which the application of strontia is described requires
only a simple mixture of the sugar in a strongly concentrated solution, such as is
found in molasses or the filling-mass, with the base in a solid or compact form. It
has been ascertained that the contact of the dry strontia with the strongly con-
centrated sugar solution effects even at the ordinary temperature a very rapid
formation of saccharates which is not to be attained when solutions are employed.
Among the forms in which strontia can possibly be applied (pulverised oxide of
strontia, hydrate of strontia and crystallised strontia) the product which arises
from the slaking of calcined strontia, the dihydrate of strontia, deserves the
preference.
This dihydrate of strontia is produced in the following manner. Caustic strontia
in lumps as it comes from the furnace is exposed to a fine spray of water or of
aqueous vapour; the porous calcined mass sucks up the water eagerly turns white

page_text: and, developing a quantity of steam, crumbles into a white crystalline powder.
All excess of water that has been added evaporates and if too great an abundance
of water has been avoided there remains only so much water in the strontia as
corresponds with the formula Sr O, 2 H, O.
The hydrate of strontia Sr O, H. O, obtained in the well known manner or the
crystals of the nine times hydrated strontia (Sr O, 9 H, O) can likewise be used
advantageously, whereas with pulverised non-hydrated caustic strontia or with hot
concentrated lye of caustic strontia (quite apart from the fact that the production
last named is much more complicated than that of the dihydrate) a corresponding
reaction according to the present method can only be produced with difficulty and
after a long time, as heating ensues in this case, and the complete formation of the
saccharates is consequently retarded.
Owing to the considerable quantity of water contained in the strontia lye and
to the heating produced by the high temperature of the concentrated lye, or by the
hydration of the caustic strontia, the mass also becomes so liquid that it fails to
have that consistency which is requisite for a quick and complete formation of
saccharates.
A certain paste-like consistency of the mixture, as also an energetic stirring up
thereof is absolutely necessary for the complete success of the process of making
strontia sugar according to this method, otherwise the strontia, owing to its greater
specific gravity, would fall to the bottom and thus be removed from the reaction.
Under the conditions just stated the strontia saccharate is formed by the method
hereinafter described in a time of such short duration (to hour) as could not
be attained if solutions and the same small quantities of strontia were used.
The practical carrying out of this method would be, according to what has just
been said, as follows:-The thick scni-liquid or viscous solution of sugar (molasses,
filling mass, &c) containing from 40 to 60 per cent of sugar is well mixed up with
pulverised strontia for the purpose of forming the saccharates.
Apparatus are used for this similar to those employed in the manufacture of
sugar for cutting up firm or compact filling-masses in general, that is to say
strongly constructed stirring machines with strong arms for cutting and mixing up
the thick semi-liquid viscous mass. However, any apparatus that causes a strong
stirring motion and incorporation can be used for this purpose. The amount of
strontia that is added is regulated by the amount of sugar contained in the
molasses & so that for each 100 lbs of sugar 40 lbs of dihydrate of strontia are
added, or for each equivalent of sugar, one equivalent of oxide of strontium (Sr O)
is employed.
According to the concentration of the sugar solution and to the energy of the
stirring the formation of the saccharate ensues within the limits stated more or less
quickly, but it is mostly completed (especially if dihydrate is applied) within a
quarter of an hour, which is manifested by the clear almost white color and homo-
genous thick paste-like condition of the mass. When this appearance shews itself,
the mass is mixed in the same apparatus with as much water or as much of the
fluid gained from the washing out of the saccharate as will render it sufficiently
liquid to be forced by means of a pump into the strongly constructed filter presses
into which the mass is admitted from the mixing apparatus in this state.
The impure saccharate that remains on the partitions of the filter press, after the
expressing, is purified with pure water, or the water containing strontia, of the
remainder of the non-saccharine parts. The wash-water thus obtained can be used
for diluting fresh quantities of the mixed mass. The first non-saccharine lye that
runs off has generally a specific weight of from 40° to 45° Brix. and therefore
represents a highly concentrated residium.
The washed out saccharate obtained in the manner just described, and which
contains about one equivalent of sugar to one equivalent of strontia is easily
soluble in hot water and even more so in hot saccharine water, and this solubility
is taken advantage of to separate the insoluble impurities (particles of slag,
carbonate, sulphate and phosphate of strontia. The best way of doing this is to

page_text: let the hot solutions of saccharate settle in high vessels and after decantation of
the clear solution to boil the insoluble parts lying at the bottom once more in
water and separate them from the liquid by means of filter presses, suction
filters &c. The clear solution of saccharate thus obtained is disengaged from the
strontia by introducing carbonic acid and the carbonate of strontia thus detached
is worked up again into caustic strontia according to the well known methods.
By this means, and especially if solutions of sugar are used for dissolving the
saccharate, a tolerably concentrated liquor is obtained which contains from 20°
to 30% of sugar of excellent purity.
°
According to this method more than 90% of the sugar contained in the molasses,
filling mass, etc. are extracted if the impure lye (residuum) is only used onco over
again for the dilution of the mixed mass.
The following principal advantages may be claimed for the method just
described..
1. The simplicity of the method of proceeding combined with the short duration
of the operation till the pure solution of sugar is obtained.
2. The perfect manner in which the strontia employed is turned to account
which substance when mixed with sugar dissolves easier and more perfectly than it
does with water alone.
3. The avoidance of lixiviation apparatus and crystallisation vessels for the
production of strontia crystals.
4. The avoidance of all heating and artificial cooling.
5. The extraction of refuse lye in a highly concentrated form:
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what
I claim is
The herein described process for extracting sugar from strongly concentrated
impure solutions, such as filling-mass or inolasses, by thoroughly mixing therewith
hydrate of strontia in solid form and maintaining for a time energetic agitation of
the pasty mass, separating the strontia saccharate from the mother lye and dis-
solving it in hot or saccharine water for separation of insoluble inipurities and for
subsequent treatment with carbonic acid.