Improvements relating to the Purification of Molasses and other Saccharine Solutions.
Year: 1887

page_text: Date of Application, 9th July, 1887
Complete Left, 7th Apr., 1888
Complete Accepted, 1st June, 1888
TROYDDIONAL SPECIFICATION.
Improvements relating to the Purification of Molasses and other
Saccharine Solutions.
We, CARL LEUCHTENBERGER, of Berlin, Derflingerstrasse 5. and BERNHARD MOISKE,
of Frankfort-on-the-Oder, Kingdom of Prussia, and German Empire Manufacturers
do hereby declare the nature of this invention to be as follows:-
This invention relates to the purification of molasses and other saccharine solutions
by separating therefrom the salts and acids therein contained. It has been tried
repeatedly before already to purify molasses by means of precipitating its salts, and
more particularly experiments and propositions in this respect have been made by the
chemists Vivien" and "Trobach all of which employ sulphuric acid to decompose
the salts of the molasses and to precipitate said salts by means of alcohol, then to
remove the salts precipitated by means of filtration, and to crystallize the sugar from
the alcoholic saccharine solution partly purified in consequence of the preceding
treatment. To obtain the sugar or syrup in a direct manner by means of boiling,
has not been possible by the use of the methods hitherto known and employed, for
the reason that a considerable percentage of the salts of molasses being sulphates will
not allow of being precipitated in sacchariferous alcohol. This hears reference more
particularly to the salts of ammonia and soda, and also to such salts as will originate
during the inevitable neutralizing treatment of the volatile organic acids by means of
carbonate or hydrate of calcium.
Now, the method constituting the subject matter of our present invention has for
its purpose to free molasses and other impure saccharine solutions in so perfect a
manner from all their noxious matter, such as salts, acids, colouring matter, that
a pure treacle is obtained.
This said novel method is based upon the following experiment that is to say :-
Saliferous molasses being mixed with sulphuric acid will produce the respective
sulphates of potash, soda and aminonia, organic acids being disengaged. The acid
syrup thus obtained being mixed with alcohol will produce mucous secretions consisting
almost entirely of sulphate of potash. But as experiments have shewn, neither
ammonia nor soda has been precipitated, because sulphate of ammonia and sulphate
'

page_text: of soda are more readily soluble in alcoholic syrup than in pure alcohol. But hy
transferring the said salts into alum, by means of adding sulphate of alumina, then
the entire amount of salt contained in the molasses will be precipitated without fail in
the shape of potassium-alum, sodium-alum and ammonia-alum shewing a decidedly
crystalline configuration. Further, the sugary solution freed from its salts, but still
somewhat acid because of the organic acids produced by the decomposition of the
salts of molasses, and because of the small excess of sulphate of alumina, will produce
only with carbonate or hydrate of barium combinations with the non-volatile organic
acids insoluble in alcoholic syrup.
By reason of these discoveries we have invented the following method, that is
to say;
We mix the molasses to be purified with a suitable quantity of sulphuric acid in
ratio with the amount of salt contained in the said molasses, care being taken that the
sulphuric acid is not added in excess because it is intended that the molasses should
only enter into an acid reaction under the action of the organic acids liberated. Now,
under the action of the said organic acids liberated the entire sugar of the molasses is
inverted within a suitable boiling vessel placed under vacuo, while, at the same time,
the volatile acids of the molasses are evaporated.
The inversion process being completed, a concentrated solution of sulphate of
alumina is added to the mass while the latter is being stirred and cooled, the said
solution being employed in such a ratio as to have for one part by weight of salt
fully two parts by weight of sulphate of alumina. After the mass has cooled down,
alcohol of about 90 per cent. is added to the same until a complete precipitation of the
salts, in the shape of alum, has taken place. After this, the precipitated mass is
separated from the liquid and used for the production of pure aluin.
The alcoholic syrup now entirely freed of salt will contain, besides colouring
matter, volatile organic acids and a small excess of sulphate of alumina. In order
to remove these acids and to decompose the surplus of sulphate of alumina so as
to form hydrate of alumina, the syrup is transferred into a closed vessel provided
with means for condensation. The said syrup is then heated, and, when it has
attained boiling temperature, neutralized by adding carbonate of barium while, at
the same time, the alcohol is continually condensed. It is a peculiarity of the
acid alcoholic syrup that while cold, carbonate in very considerable excess may be
added to the same without causing the least neutralizing effect, while, when at
the boiling temperature, the neutralization will take place without any material
difficulty.
The syrup being thus neutralized is now cooled and freed of the precipitated
substances by means of a filtering press. The treacle or syrup which in this
manner is now completely purified, is freed of the spirits in any convenient and
well-known manner, in order to recover the alcohol, whereupon it is refined by
means of bone-black and boiled for the market.
Dal..... 1007
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicants.

page_text: We, CARL LEUCHTENBERGER, of Berlin, Derfingerstrasse 5, and BERNHARD
MOISKE, of Frankfort-on-the-Oder, Kingdom of Prussia and German Empire, Manu-
facturers, 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 :-
This invention relates to the purification of molasses and other saccharine solutions
by separating therefrom the salts and acids therein contained. It has been tried
repeatedly already to purify molasses by means of precipitating its salts. and more
particularly experiments and propositions in this respect, have been made by the
chemists Nugues, Marguerite, Vivien, and Trobach all of which employ sulphuric
acid in order to decompose the salts of the molasses and to precipitate said salts by
means of alcohol, then to remove the salts precipitated, by means of filtration, and to
crystalize the sugar from the alcoholic saccharine solution partly purified in con-
sequence of the preceding treatment. To obtain the sugar or syrup in a direct
manner by means of boiling, has not been possible by the use of the methods hitherto
known and employed for the reason that a considerable percentage of the salts of
molasses being sulphates, will not allow of being precipitated in sacchariferous alcohol.
This bears reference more particularly to the salts of ammonia and soda, and also to
such salts as will originate during the inevitable neutralizing treatment of the volatile
organic acids, by means of carbonate or hydrate of calcium."
Now, the method constituting the subject matter of our present invention, has for
its purpose to free molasses and other impure saccharine solutions in so perfect a
manner from all their noxious matter, such as salts, acids and colouring matter, that a
pure treacle is obtained.
This said novel method is based upon the following experiment, that is to say :-
Saliferous molasses being mixed with sulphuric acid will produce the respective
sulphates of potash, soda, and ammonia, organic acids being disongaged. The acid
syrup thus obtained being mixed with alcohol will produce mucous secretions con-
sisting almost entirely of sulphate of potash. But as experiments have shown,
neither ammonia nor soda have been precipitated, because sulphate of ammonia and
sulphate of soda. are more readily soluble in alcoholic syrup than in pure alcohol.
But by transferring the said salts into alum, by adding sulphate of alumina, then the
entire amount of salt contained in the molasses, will be precipitated without fail in
the shape of potassium-alum, sodium-alum and ammonia-alum showing a decidedly
crystaline configuration. Further the sugary solution freed from its salts, but still
somewhat acid because of the organic acids produced by the decomposition of the

page_text: '
salts of molasses, and hecause of the small excess of sulphate of alumina, will produce
only with carbonato or hydrate of barium combinations with the non-volatile organic
acids insoluble in alcoholic syrup.
By reason of these discoveries we have invented the following method, that is to
say:
We mix the molasses to be purified with a suitable quantity of sulphuric acid in
ratio with the amount of salt contained in the said molasses, care being taken that
the said sulphuric acid is not added in excess because it is intended that the molasses
should only enter into an neid reaction under the action of the organic acids liberated.
Now, under the action of the said organic acids liberated, the entire sugar of the 1
molasses is inverted within a suitable boiling vessel placed under vacuo while, at the
same time, the volatile acids of the molasses are evaporated.
The inversion-process being completed a concentrated solution of sulphate of
alumina is added to the mass while the latter is being stirred and cooled, the said
solution being employed in such a ratio as to have for one part by weight of salt 1
fully two parts by weight of sulphate of alumina. After the inass has cooled down,
alcohol of about 90 per cent. is added to the same until a complete precipitation of
the salts, in the shape of alum, has taken place. After this, the precipitated mass is
separated from the liquid and used for the production of aluin powder.
In
The alcoholic syrup now entirely freed of salt, will contain besides colouring
matter, non-volatile organic acids and a small excess of sulphate of alumina.
order to remove these acids and to decompose the surplus of sulphate of alumina so
as to form hydrate of alumina, the syrup is transferred into a closed vessel provided
with means for condensation. The said syrup is then heated and, when it has
attained the boiling temperature, neutralized by adding carbonate of barium while,
at the same time, the alcohol is continually condensed. It is a peculiarity of the acid
alcoholic syrup that, while cold, carbonate in very considerable excess may be added
to the same without causing the least neutralizing effect, while, when at the boiling
temperature the neutralization will take place without any material difficulty.
The syrup thus being neutralized, is now cooled and freed of the precipitated
substances by means of a filtering press. The treacle or syrup which in this manner
is now completely purified, is freed of the spirits in any convenient and well known
manner, in order to recover the alcohol, whereupon it is refined by means of bone-
black and boiled for the market.
In order to remove the organic acids and the greater part of colouring matter we
have found that good results may be obtained by subjecting the molasses to a
preliminary treatment so as to reduce before proceeding as hereintofore described,
the said acids and colouring matter by means of powder of zine and ammonia in
the form of an alcoholic solution, experiments having proved that the organic acids
of the molasses, and particularly those of a sebacic nature, allow of being reduced to
aldehyd by means of powder of zinc, in the presence of ammonia or another uncom-
bined alkali. We have, further, found that the said reduction will take place more
energetically in the presence of alcohol, than in the presence of water, and that
by means of borings or filings of zine the said reaction is not effected. We have,
moreover, found that the treatment of the molasses just referred to, will have a most
detrimental effect upon the colouring matter therein contained.
Dark-coloured, nearly black and undiaphanous molasses diluted by an addition of
alcoholic water and ammonia, will show the same auburn condition after being thus
diluted. Adding to the said solution a small quantity of powder of zine (say 1 or
2 per cent. of the weight of the molasses) will cause the colouring matter to vanish
almost instantaneously within certain limits. Removing the alcohol and the ammonia
by means of distillation from the solution of molasses thus treated, will not cause
the said solution to re-assume an auburn colour. By passing carbonic acid through
the solution freed of the alcohol, a liquid will be obtained which will allow of being
filtered readily and which will then contain neither zinc, nor organic salts. The
molasses thus preliminarily purified, will be better fit for being thoroughly purified
after our method hereintofore described in accordance with the purposes of this
5

page_text: invention, whilst at the same time this mode of procedure will offer a means for
producing out of the molasses lime-sugarates in a very pure state.
The said preliminary treatment is as follows:-
The molasses contained in a closed receptacle of wrought iron, is diluted by adding
to it liquid ammonia containing preferably 35 per cent. alcohol, and is then well
stirred. While being stirred a quantity of powder of zine (1 to 2 per cent. as above
stated) is added to the mixture through a suitable opening in the containing
receptacle and the compound raised for 15 to 20 minutes to a temperature of about
105 degrees and remains unstirred during this time. After the lapse of the said
space of time, the temperature of the mixture is raised so as to expel all volatile
matter, the latter being condensed for renewed use. Carbonic acid is passed through
the solution thus freed from its alcohol, and the said solution then forced through a
filtering press. The residuary mass of filtration will contain metallic, and carbonate
of zine as well as lime and other residues from the molasses, whilst the filtered liquid
will constitute a saccharine solution of a deep-yellow colour and an agreeable taste,
but still containing all of the salts of soda and potassa in the form of carbonates which
are now to be precipitated to form alum in accordance with the motives of the present
invention and as hereinbefore described.
In some cases, the molasses themselves contain much ammonia in the shape of
carbonate of ammonia, and in such case we propose to add to the molasses 1 to 2 per
cent., by weight, of lime in the form of lime-milk, then to heat the solution while being
stirred and to mix with it alcohol so that the mixture will contain about 35 per cent.
of the latter.
Having now particularly described and ascertained the nature of our said
invention, and in what manner the same is to be performed, we declare that what
we claim is :-
First. The method, substantially as herein described, consisting in removing the
alkalies from molasses or other impure sugary compounds by means of transforining
the said alkalies into sulphates and combining the same with sulphate of alumina to
form alum, and precipitating, by adding alcohol, the aluminates thus formed.
Second. The method, substantially as herein described, consisting in inverting the
molasses freed of its salts, by exposing the same to the action of the organic acids
liberated while within a receptacle placed under vacuo and while the volatile organic
acids therein contained are evaporated.
Third. The method, substantially as herein described, consisting in neutralizing
and precipitating the non-volatile organic acids in alcoholic saccharine solution by
means of carbonate of barium added while the said solution is at the boiling
temperature and while the alcohol is being continually condensed.
Fourth. The method, substantially as herein described, consisting in preliminarily
purifying the molasses by reducing the organic acids and the colouring matter by
ineans of treating the same with powder of zinc, ammonia and alcohol or, by making
use of the ammonia and uncombined alkali already contained in the molasses, with
powder of zinc and alcohol.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicants.