IMPROVEMENTS IN THE EXTRACTION OF SUGAR FROM MOLASSES AND OTHER SACCHARINE PRODUCTS AND IN THE QUALITY OF ALKALINE SALTS RESULTING THEREFROM
Year: 1884

page_text: We VICTOR DAIX of No 25 Rue d'Achery, St Quentin, in the Department of the
Aisne, Engineer, and ANTOINE LOUIS Possoz of N° 69 Avenue des Ternes, Paris,
Chemist, both in the Republic of France do hereby declare the nature of the said
Invention for IMPROVEMENTS IN THE EXTRACTION OF SUGAR FROM MOLASSES AND
OTHER SACCHARINE PRODUCTS AND IN THE QUALITY OF ALKALINE SALTS RESULTING
THEREFROM, to be as follows:-
Our system permits of effecting an important economy in the extraction of
sugar from molasses and other saccharine products.
We give to this new system of working the name of ". osmo-sucrate " because it
consists first in osmosing molasses, and manufactory and refinery syrups, and then
in precipitating the sugar contained in the exosmose waters, molasses and other
residues of the osmose, in the state of sucrate of lime, of baryta, of strontium or
other sucrate.
Then we employ these earthy sucrates to purify the syrups leaving the
osmogenes; so that the costs of treatment and of decomposition of the said
sucrates by carbonic acid, are utilized at the same time to purify osmosed or
other syrups.
The osmo-sucrate is therefore a process which by the collective combination of
economic means and of new processes, permits of obtaining first a portion more or
less large of the sugar contained in molasses and other low products by osmotic
processes which are the most economic with respect to costs of installation and
working but which until now had the grave defect of yielding only about 30 to 40
per cent of the sugar for one osmose, and which in order to yield more required a
multiplicity of very long and troublesome osmose and reosmose operations, chiefly
because the exosmose waters were badly utilized as residues suitable for making
alcohol and blacking whilst we obtain from the said exosinose waters and osmose
residues, sucrates of lime, of baryta and of strontium which are employed by us in
purifying osmosed syrups.
The osmo-sucrate offers also a well marked advantage over the processes which
consist in treating the entire of the molasses, syrups and saccharine juices by

page_text: strontium, baryta or lime to convert the entire of the sugar into sucrates, whilst
we employ these expensive chemical nieans only for extracting the sugar which the
osmose has allowed to escape into the exosmose waters and into the osmose
residues.
We obtain a particular sucrate which we call "super-calcic osmotic sucrate," in
order to distinguish it from others from which it differs essentially, and we apply
this new "
super-calcic osmotic sucrate" in the purification of beet root juices scums,
drainage liquors, molasses and osmosed syrups.
Further we increase the value of the alkaline salts and facilitate their extraction
by the formation of potassic salts easily crystallizable, such as the sulphate and
the nitrate of potash.

page_text: We VICTOR DAIX of N° 25 Rue d'Achery, St Quentin, in the Department of the
Aisne, Engineer, and' ANTOINE LOUIS Possoz of No 69 Avenue des Ternes, Paris,
Chemist, both in the Republic of France do hereby declare the nature of the said
Invention for IMPROVEMENTS IN THE EXTRACTION OF SUGAR FROM MOLASSES
AND OTHER SACCHARINE PRODUCTS AND IN THE QUALITY OF ALKALINE SALTS
RESULTING THEREFROM, and in what manner the same is to be performed, to be
particularly described and ascertained in and by the following statement :-
According to our invention we employ not only new combinations of means
which enable us to obtain new industrial results, but also new processes, for
obtaining these economic industrial results.
According to the quality of the molasses and other saccharine matters upon
which we desire to operate, we claim the right to vary the details of the treatments,
but the principles which control our invention are always based upon those given
below.
1. On the one hand, it is known that the operation of osmose, if it offers the
advantages of a first installation of slight cost and of small expenses of manu-
facture, it has the grave inconvenience of permitting only a limited extraction of
sugar, and that all the advantages which this simple method presents are greatly
diminished by the small amount of value of the sugar which is found carried away
and soiled by the salts and the non-sugar in the exosmose waters, as also in the
molasses, residues of the crystallizations of the osmosed sugar; a part of sugar
thus soiled is only extracted by repeated operations of osmose and reosmose, which
involve much time and expense, and at the final analysis, there remains in the form
of very impure molasses sugar which is badly utilised in the production of alcohol
and blacking.
2. On the other hand it is known that the processes of extraction of sugar by the
sucrates of lime, of baryta, of strontium if they have the advantage of permitting
the extraction of much larger proportions of sugar than by the osmose process
present the inconvenience of requiring very expensive installations of plant and of
heavier costs of operation.
Nevertheless, hitherto molasses and other low saccharine products have been
treated, either by osmose, or by the sucrates separately, that is to say that the two
processes have not been combined so as to utilise the management of both to the
profit of the final industrial product.
We have remarked that molasses and other saccharine products which have been
previously osmosed are particularly suitable to be purified by the earthy sucrates
(of baryta and of strontium) and particularly by the sucrates of lime, in place
of milk of lime (which hitherto had been exclusively employed for this purpose)
and especially we have searched for and found the means of extracting the sugar

page_text: '
carried away and soiled in the exosmose waters and in the osmose and re-osmose
residues. Our invention therefore in the first place consists in the mode of
treatment of molasses by the simultaneous employment of the process of osmose
and of sucrates, whilst hitherto the process of osmose or the sucrates had only
been employed separately, but never together.
1. Mode of operation when use is made of lime as precipitant of the sugar in the
low products of osmose.
Having encountered unforseen difficulties in precipitating from the waters of
exosmose, the sugar in the condition of sucrate of lime, by processes recently
approved and patented, we had to search for other processes, and we have succeeded
in operating under different conditions and which give rise to a particular sucrate
which we call "super-calcic osmotic sucrate."
We will now describe the essential.differences which we have observed between
the treatment of ordinary molasses (non-osmosed) to which the processes of other's
apply and between the treatment (by our process) of the molasses of exosmose
or concentrated waters of exosmose the contents of sugar being comparatively
the same.
A. If there is mixed cold (temperature from 0° to +15° centigrade) saccharine
solutions of molasses of beet or of cane, juices of beet and all saccharine solutions
other than waters of exosmose, in such conditions that the contents of sugar shall
be between 8 and 20 of sugar for 100 of water, and that there is mixed with them
lime (anhydrous or hydrated in powder or in milk, but by, preference anhydrous
and in fine powder) in various proportions from 100 to 120 of lime (Ca O) for
every hundred of sugar, the mixture made cold is not gelatinous; it preserves the
fluid state and can be passed to the filter press.
B. But if we mix in the same conditions of temperature, of dilution and of
proportion of the same pulverised anhydrous lime for example with solutions of
molasses of concentrated exosmose to the said sugar containing liquors and also to
sugar containing liquors of higher proportions, this mixture cannot filter through
the cloths of the filter press, it solidifies into a kind of consistent jelly; it is not
fluid. We have observed. that in raising the temperature beyond 40 degrees
centigrade, this gelatinous magma commences to fluidify and especially by heating
between 60 and 120 degrees centigrade, the gelatinous state is destroyed: there is
produced an abundant pulverulent precipitate of a sucrate of lime entirely distinct,
for this combination differs from other known sucrates by 'this solidified condition
when cold and by its other properties.
This precipitate allows itself to be very well filtered, compressed and washed by
the filter press by hot water and steam.
The mother and wash waters (weak or concentrated) being thus treated by one
or several successive additions of lime are exhausted of the sugar economically
extractible.
"
This same phenomenon (of gelatinous state when cold) is also obtained when we
add to the exosmose waters, molasses of reosmose or the last molasses of osmose, in
the ordinary proportions of work.
11
.
In order to distinguish this sucrate of lime from others from which it essentially
differs we designate it under the name of "Super-calcic osmotic sucrate" considering
that it contains generally much more lime than theory admits, even in 'admitting
that a sucrate of 5 equivalents of lime can be produced. But this excess of lime is
necessary to us for the maximum precipitation of the sugar, which is the industrial
'object of this process. Also our invention consists in producing the said 'sucrate,
in order to extract from the waters of 'exosmose and other residues of osmose, the
greatest possible quantity of sugar and in applying this new super-calcic osmotic
sucrate, to the purification of beet juices, drainage liquors; molasses and osmosed
syrups, an economic and new application which enables us to convert into sucrate
only the waters of exosmose and other residues of osmotic working.
(Nevertheless our invention also consists in extracting from exosmose waters
and other osmose residues a tri-calcic 'osulotic sucrato; by beating between 100 and
1.
1710

page_text: -
130 degrees centigrade, solutions of lime in the said osmotic residues, mixed with
the proportion of limé necessary to combine the sugar with three equivalents
of lime.
2.
'
1
But whilst considering the above as part of our invention we prefer to this
process, that producing the' super-calcic osmotic sucrate, because it enables us to
extract about a third more sugar for equal volumes of osmotic liquid of like
saccharine strength, which is due to the large proportions of lime which
characterise our super-calcic osmotic sucrate, and which by their presence pre-
vent the possibility of a part of the precipitated sugar being redissolved in sugar
deprived of lime, thanks to the excess of lime in presence at these temperatures.
We intend to reserve to ourselves, every latitude respecting the proportions of
sugar and of lime to be employed; for the formation of our super-calcic osmotic
sucrate according to the qualities which are very variable, of the products of osmose,
of exosmose and of lime; however in the most ordinary cases we employ between 5
and 8 equivalents of lime for one of sugar to be precipitated.'
2. Mode of operation when baryta is used;
There is added to the solution of impure sugar, whatever may be its saccharine
strength, a saturated and boiling solution of baryta, employing one equivalent of
baryta for one equivalent of sugar.
Use can be made of sulphuret of barium alone or of sulphuret of barium and of
soda; in these two latter cases, an excess of precipitant should be employed.
The sucrate thus produced is separated either hot or cold, by means of filter
presses and washed with ordinary, water either hot or nearly cold.
This sucrate being thus obtained and purified, is added to the osmosed molasses
and the entire submitted to carbonation.
The baryta is regenerated by the ordinary processes (calcination in a reverberatory
furnace with coal.)
3. Mode of operation, when strontium is used.
In this case the impure saccharine solutions, residues of osmose, being brought to
a saccharine strength comprised between 10 and 20% of sugar, according to their
nature and their composition are brought to the boiling temperature and crystals of
hydrate of strontium added so as to introduce from 3 to 4 molecules of strontium
for one of sugar. The entire is then passed to the washing filter press where the
separation of the sucrate from the desucrated mother waters is made, and the
washing is effected by making use of a hot solution of hydrate of strontium.
The wash waters serve to dilute the osmose molasses.
With respect to the sucrate it is added to the osmosed molasses and the entire
carbonated.
The impure carbonate of strontium resulting from this operation, charged
as it is with organic matters which have been separated from the osmosed
molasses by the act of carbonation is agglomerated into the form of bricks of
small dimensions and placed in reverberatory furnace where the strontium is
regenerated.
To again obtain hydrate of strontium, it is only necessary to submit the product
of the calcination to a methodical washing in boiling water, there are deposited on
cooling crystals of hydrate of strontium, which are ready to be employed for a new
operation.
We have moreover made an important remark of which we claim the appli-
cation.
We have succeeded in submitting to certain exosmose waters and other osmose
residues a preliminary purification, especially when these products are much charged
with organic matters. For that we add to these osmotic residues (before treating
them for sucrates) small quantities of lime insufficient to produce the gelatinous
condition, nor any precipitate of sucrate, but which determines the formation of a
highly colored deposit of impurities, easy to be eliminated by decantation or by
filtration, and particularly by carbonation.

page_text: These residues thus purified, produce osmotic sucrates much purer than if we
had not practised this preliminary purification and we claim to apply it, when
required to all the osmotic sucrates.
The mother and wash waters of the osmotic sucrates, being exhausted of sugar
as much as possible, are concentrated to about 40 degrees Baumé, then put to
crystallize in order to obtain from them the crystallizable salts. But before their
final concentration, we dissolve in it, nitrate of soda, in sufficient proportion to
transform into nitrate of potash, the chlorides and other potassic salts, which
crystallize with difficulty and confusedly in the said mother waters.
In all cases before concentrating the mother and wash waters, we can purify
them, by treating them with carbonic acid, to carbonate and eliminate the lime,
the baryta or the strontium which they contain ; and after decantation and filtration,
they are concentrated to about 40 degrees Baumé by adding to them nitrate of
soda as just described.
The saline. mother waters having been recovered, concentrated and exhausted
of nitrate of potash, are then employed as manure or for any other industrial
use, but by this manner of operating we have been able to extract from them,
in the form of nitrate, the major part of the potash and to avoid the depreciation
which the latter undergoes, when it is left in the state of chloride of potassium.
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
1. The extraction of the sugar from the waters of exosmose and other osmose
residues by the transformation of this sugar into osmotic sucrate of lime, of
baryta, of strontium and particularly into super-calcic sucrate and to utilise the
purifying power of these sucrates (in place of milk of lime) in the carbonic
purifycation of juices, syrups, drainage liquors and more particularly impure
syrups arising from osmogones, whilst hitherto the exosmose waters and other
osmose residues final drainings or osmose and reosmose molasses were only utilized
in the production of alcohols, salts, or blackings and sold at a low price.
2. The mode of treatment of the mother waters by nitrate of soda and the
concentration in order to obtain salts of potash and manures.
3. The new method of working both in its combination and in its details as
above described.
·
VICTOR DAIX.
ANTOINE LOUIS POSSOZ.
By Harris & Mills,
23, Southampton Buildings,
Agents.