Year: 1886

page_text: Date of Application, 6th Mar., 1886.
Complete Left, 6th Dec., 1886.
Complete Accepted, 7th Jan., 1887.
We RUDOLF ENGLERT and Dr. FRANZ BECKER both of Prague (Bohemia) Austria,
Proprietors of Chemical Works do hereby declare the nature of this invention to be
as follows:-
-
This invention relates to the purification of beet-root-juice, cane juice and other
saccharine juices of vegetable origin.
According to the invention the saccharine juices extracted by the diffusion process
are first repeatedly defecated by treating the same as usual with lime and carbonic acid
and separating the lime-scum by means of filter-presses; sulphite of alumina or of
iron or hydro-sulphurous acid or a hydro-sulphite or a mixture of this acid and its
salts is then added to the juices whereupon the same are again saturated and boiled
up and separated from the scum by means of filter-presses. By this treatment the juices
become so thoroughly defecated and decolorized that they do not need to be treated
with charcoal; after having been concentrated, the juices may again be treated with
the above named substances, lime and carbonic acid and freed from the scum by
means of filter-presses. Finally, the thick purified juice is filled into moulds.
The sulphites of alumina or of iron, necessary for carrying out the described
process may best be prepared by conducting sulphurous acid into closed vessels,
which either contain hydrate of alumina and water, or hydrate of protoxide of iron.
Hydro-sulphurous acid can easily be prepared by dissolving iron or zinc in an
aqueous solution of sulphurous acid, addition of lime-milk, filtration of the mixture,
and addition of oxalic acid to the filtrate, which is again filtered; for obtaining
hydro-sulphites which are less liable to decomposition than the free acid, the desired
bases are added to the prepared acid. The following bases may be used with
advantage-Ammonia, baryta, strontia, lime, magnesia, alumina, oxide of zinc,
protoxide of iron, oxide of manganese.
Although we have stated that the purifying substances are added to the thin and
the thick juices and that the juices are afterwards saturated with carbonic acid, we do
not limit ourselves to this process, but sometimes treat the thin juice only or add the
purifying substances without subsequent saturation.
G. F. REDFERN,
4, South Street, Finsbury, London,
Agent for the Applicants.

page_text: Improvements in the Process of Purifying Saccharine Juices.
We, RUDOLF ENGLERT and Dr. FRANZ BECKER, both of Prague (Bohemia) in
the Empire of Austria, Proprietors of Chemical Works, 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 a new or improved process of purifying saccharine
juices such as are produced in sugar-mills and sugar refineries whereby the juices are
so perfectly defecated that they do not need to be treated with charcoal, and a mere
mechanical filtering by means of good filter-presses suffices for producing saccharine
juices which can with advantage be directly converted into filling mass.
This process consists in the addition to the juices under treatment of sulphite of
alumina (whether the acid, neutral or basic salt), or sulphite of iron, or hydro-
sulphurous acid (SO, H₂), or (as this acid in its free state is too liable to
decomposition) by preference, a hydro-sulphite.
In carrying out this invention, the saccharine juices are first defecated in the usual
manner by treating the same with lime and carbonic acid and separating the lime-
scum by means of filter-presses; the saturation with carbonic acid being preferably
continued until the alkalinity of the juice is reduced to from 0.03 to 0.04 per 100.
After this, the juices are boiled, and a sufficient quantity of sulphite of alumina
or of sulphite of iron (by preference an aqueous solution of sulphite of alumina,
saturated with sulphurous acid) is added to them in order to lower the alkalinity
of the juices to about 0:01 per 100. When thin juice is subjected to the herein
described process, a smaller quantity of sulphite of alumina or of sulphite of iron may
be added to the juice, and the alkalinity lowered to the required degree by subsequent
saturation with carbonic acid. The juice with the before named substance added to
it, is boiled for some minutes more, and then the precipitate formed is separated from
the juice by thoroughly filtering the latter by means of a good filter-press, while it is
as hot as possible.
The thin juice defecated in the manner described is concentrated, and the thick
juice produced is advantageously treated again with sulphite of alumina or sulphite
of iron and carbonic acid in the same manner as the thin juice; after which the
thick juice may be converted into filling-mass.
In consequence of the addition of sulphite of alumina to the alkaline saccharine
juice, sulphite of lime and hydrate of alumina are formed. The sulphite of lime acts
as a decolorizer and at the same time its sinking down in the liquid, concurrently
with the precipitation of the hydrate of alumina effects a thorough defecation of the
juice the precipitate formed is so dense that it can be easily and perfectly separated
from the juice.
It is advantageous to eliminate the sulphate of lime formed in the saccharine juices
under the action of the sulphurous acid. For this purpose carbonate of strontia or
carbonate of baryta, in a quantity equivalent to that of the sulphate of lime, is added
to the thick juice, and then the whole is boiled.
As hereinbefore stated, hydro-sulphurous acid, or preferably, hydro sulphite may be
used instead of the sulphites of alumina or iron. In this case from 2 to 5 parts by

page_text: eight of one or the other of these salts are added to 1,000 parts by weight of the
ice. After thoroughly stirring together, the mass is boiled, when the freed acid will
the one hand combine with the lime, and on the other hand energetically decolorise
e liquid, while the remaining oxide sinks down, carrying with it the organic matter
spended in the juice and thereby mechanically purifying the same.
The decloration produced is nearly complete, as one part of a hydro-sulphite has
he same effect as five parts of the sulphites referred to. It is therefore possible in
his manner to obtain nearly colorless juices without the use of animal charcoal.
The following salts may to advantage be employed for the hereinbefore described
urpose, namely,
e successively treated in the following manner namely,
1st defecation: The raw juice is heated with from 2 to 3 per cent of lime, and
saturated with carbonic acid to an alkalinity of 0.10 per cent and the scum is
separated by means of a filter-press.
2nd defecation The juice is mixed with per cent of lime, and saturated with
carbonic acid to an alkalinity of 0.04 per cent and the scum is separated by
means of a filter-press.
3rd defecation: The juice is mixed with 1 per mille of a hydro-sulphite, saturated
with carbonic acid to an alkalinity of 0.02 per cent, and boiled; the scum is
separated by means of a filter-press provided with double cotton cloths, and
under the pressure of a head of juice of from 10 to 15 feet.
CONCENTRATION OF THE THIN JUICE TO THICK JUICE.
4th defecation From 2 to 4 per mille of a hydro-sulphite and from 1 to 2 per mille
of milk of lime are added to the thick juice, then the same is saturated with
carbonic acid to an alkalinity of 0.03 per cent and boiled; the scum is then
separated in the same manner as described after the 3rd defecation.
CONVERSION OF THE THICK JUICE INTO FILLING-MASS.
Filling-masses prepared in the manner hereinbefore described are very pure and of
great density and can easily be freed from the syrup or mother-liquor by means of a
centrifugal machine.
The following processes are employed to prepare the above named purifying
nedia:
To prepare sulphite of alumina or of protoxide of iron sulphurous acid-under
ressure if possible is carried through a series of closed vessels communicating with
one another and preferably provided with an agitator, and containing water and
ydrate of alumina or water and hydrate of protoxide of iron, the said acid being fed
nto the vessels until the liquid is saturated.
When hydro-sulphurous acid or salts of this acid are to be obtained, filings of iron
or zine dust are brought in excess into an aqueous solution of sulphurous acid. In
order to obtain a highly concentrated solution, more sulphurous acid is placed in the
iquid, but only in such quantity that the solution shall not smell of the acid.
When zinc dust has been employed, the reaction which takes place is expressed by
he following chemical equation:

page_text: consequently sulphite of zinc and hydro sulphite of zinc are formed. To eliminate the
former from the solution, milk of lime is added to the liquid, when insoluble sulphite
of lime and soluble hydro-sulphite of lime is formed; the solution of the latter salt is
separated by means of filtration.
To separate from this solution of hydro-sulphite of lime free hydro-sulphuric acid,
the lime is precipitated by means of sulphuric, oxalic or phosphoric acid, whereupon
the liquid is filtered. During this operation as well as during all other operations for
the purpose of preparing hydro-sulphurous acid, the contact of the liquid with the
atmospheric air is to be avoided as far as possible.
If salts of the hydro-sulphurous acid are to be prepared, the mixture of the solutions
of sulphito and hydro-sulphite of zinc, obtained as hereinbefore stated, is agitated with
the base employed which, in consequence of this treatment becomes substituted for
the oxide of zinc.
According to whether the salt formed by the combination of the new base with the
sulphurous acid is soluble or insoluble, there will result from the described operation a
mixture of the solutions of the sulphite and hydro-sulphite of the base, or a pure
solution of the hydro-sulphite.
The two following chemical equations illustrate examples of the first kind with the
use of alumina, and of the second kind with the use of lime :
3 (Zn SO3 + Zn 80,) + 2 Al, (HO)₁ = Al, (SO3)3 + Al₂ (SO2)3 + 6 Zn O.
Zn SO3 + Zn SO, + 2 CaO = Ca SO, + Ca SO₂ + 2 Zn 0.
-
We are aware that heretofore the use of the soluble acid sulphites as defecators of
sugar has been proposed, but to the best of our knowledge and belief neither neutral
and basic sulphites have been used for this purpose, nor has the addition of sulphites
to the juices been combined with a subsequent saturation with carbonic acid.
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 :-
1st. The herein described means for defecating and decolorising saccharine juices in
sugar mills and sugar refineries by the addition to the said juices of neutral or basic
sulphite of alumina, neutral or basic sulphite of protoxide of iron, hydro-sulphurous
acid or hydro-sulphites.
2nd. The herein described process of purifying and decolorising thin as well as thick
saccharine juices, by the addition of sulphite of alumina or sulphite of protoxide of iron,
or hydro-sulphurous acid, or a hydro-sulphite, and subsequent saturation with carbonic
acid.
3rd. The herein described process of defecating and decolorising saccharine juices,
the said process consisting in the addition to the boiling juice which has becu previously
saturated to an alkalinity of from 0:03 to 0.04 per cent, of a quantity of sulphite of
alumina or of protoxide of iron sufficient to decrease the alkalinity of the juice to 001
per cent, and in the subsequent separation of the deposit by means of a filter-press,
while the juice is kept as hot as possible, or, when hydro-sulphites are used, in the
addition to the juice, previously saturated to an alkalinity of 0.04 per cent, of 1 per
mille of a hydro-sulphite, decreasing the alkalinity to 002 per cent by subsequent
carbonating, separating the scum by means of filter presses, concentrating the juice,
adding to the thick juice from 2 to 4 per mille of the hydro-sulphite and from 1 to 2
per mille of milk of lime, saturating the juice to an alkalinity of 0.03 per cent, boiling
the same and separating the scum by means of filter-presses.
G. F. REDFERN,
4, South Street, Finsbury, London,
Agent for the Applicants.