IMPROVEMENTS IN THE METHOD OF REFINING SACCHARINE VEGETABLE JUICE, MUSCOVY SUGAR, AND SYRUPS
Year: 1880

page_text: LETTERS PATENT to William Spence, of 8, Quality Court, Chancery Lane, in
the County of Middlesex, Patent Agent, for an Invention of "IMPROVEMENTS
IN THE METHOD OF REFINING SACCHARINE VEGETABLE JUICE, MUSCOVY
SUGAR, AND SYRUPS." A communication from abroad by Anton Gawalowski,
of Trebitsch, Moravia, Austria, and Franz Teichmann, of Wagstadt, Silesia,
Austria.
PROVISIONAL SPECIFICATION left by the said William Spence at the Office
of the Commissioners of Patents on the 27th February 1880.
WILLIAM SPENCE, of 8, Quality Court, Chancery Lane, in the County of
Middlesex, Patent Agent. "IMPROVEMENTS IN THE METHOD OF REFINING
SACCHARINE VEGETABLE JUICE, MUSCOVY SUGAR, AND SYRUPS." (A communi-
cation from abroad by Anton Gawalowski, of Trebitsch, Moravia, Austria, and
Franz Teichmann, of Wagstadt, Silesia, Austria.)
This Invention relates to improvements in the method of refining saccharine
vegetable juice, muscovy sugar, and syrups of any kind without submitting the
juice, molasses, or the clear to the usual filtration of spodium.
This improved method is modified according to its application; 1, with pure
vegetable juice (beet root or cane juice), and with beet root juice to which sub-
products are added; 2, with solutions of raw sugar or syrups (in refining);
3, with molasses and little sub-product syrups.
With reference to the first process it takes place at the separation or saturation
of the vegetable juice (beet root or cane juice.) The juice is first properly heated,
and then is added, either at once or after the addition of lime, as hereinafter
described, 02 to 0-5 per cent. of phospite of alumina (upon ten tons of beet root.)
This phosphite of alumina or a solution of phosphate of alumina in phosphoric
acid is a new agent.
Another agent employed is a residual powder obtained in the production of red
or yellow prussiate of potash. The said powder or raw spodium dust is freed from
all potash compounds, and is stirred with raw muriatic acid or nitric acid and left
to settle. The black pulp of this mixture is then diluted with water and the

page_text: salts of iron and lime and other waste stuffs of this solution eliminated by lixiviation.
The residual powder and the spodium dust essentially contain decolouring animal
charcoal, and besides some sand and insoluble salts of lime. Other kinds of
nitric charcoal may be used for the purpose, but they must be refined, lixivated,
and treated with acids in the manner before stated.
The residual product or spodium dust may be revivified as required by
lixiviating and boiling with etching lye of soda treated with muriatic acid and
dried; and if after frequent use its decolouring powder has been lost it may be
heated in air tight retorts and cooled down. The juice after complete saturation,
and if necessary in a heated state, is now separated from the pulp by means of a
suitable press or filter.
The juice after being refined is brought to the boiler to be condensed into
molasses by evaporation. The second modification of the process is that of refining
in application with solutions of raw sugar or syrups.
The raw sugar or syrups is dissolved in or diluted with pure water in boilers
und thereby brought to the required consistency.
Then to this solution in a heated state is added one quarter to two and a half
per cent. of lime to the quantity of raw sugar or dry substance. The clear obtained
after well mixing the milk of lime (by preference specially prepared) with the said
solution is heated and skimmed; and there is further added 0-2 to 0.5 per cent. of
phosphite of alumina and residual powder or spodiumi dust.
The third modification of the Invention consists in applying the improved
method of refining with molasses or little sub-product syrups. The syrups of the
third, fourth, or further production, as well as the juices recovered from the osmosis
process, or from the various molasses saturations, and further the molasses diluted
below 60 per cent. Balling, are put into a boiler and mixed either at once or after the
addition of lime with phosphite of alumina, and the mixture is then saturated and
pressed through suitable filters. The refined juice may be either directly con-
centrated by evaporation, or it may previously be treated in a heated state with
refined residual powder or spodium dust, whereby it will be further decoloured.
This is separated by suitable filters from the residual powder or spodium dust, and
concentrated by evaporation till it may be filled in moulds for crystallization.
Instead of using the carbonic acid produced during the working process for the
gas of saturation, this gas is taken from a generator which supplies a gas of the
highest percentage. The generator is similar to those ordinarily used in the
preparation of mineral waters, but is a novelty as applied to the manufacture of
sugar.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said William Spence in the Great Seal Patent Office on the 26th August
1880.
WILLIAM SPENCE, of 8, Quality Court, Chancery Lane, in the County of
Middlesex, Patent Agent. "IMPROVEMENTS IN THE METHOD OF REFINING
SACCHARINE VEGETABLE JUICE, MUSCOVY SUGAR, AND SYRUPS." (A communi-
cation from abroad by Anton Gawalowski, of Trebitsch, Moravia, Austria, and
Franz Teichmann, of Wagstadt, Silesia, Austria.)
This Invention relates to improvements in the method of refining saccharine
vegetable juice, muscovy sugar, and syrups of any kind without submitting the
juice, molasses, or the clear to the usual filtration of spodium.
This improved method is modified according to its application; first, with pure
vegetable juice (beet root or cane juice) and with beet root juice, to which sub-
products are added; secondly, with solutions of raw sugar or syrups (in refining);
thirdly, with molasses and little sub-product syrups.
These special modifications of the improved method of refining are hereinafter
described.
With reference to the first process it takes place at the separation or saturation
of the vegetable juice (beet root or cane juice). The juice is first properly heated,
and then is added, either at once (according to the quality required) or after the
addition of lime, as hereinafter described, 0-2 to 0.5 per cent. of phosphite of
alumina "A" (upon ten tons of beet roots), and this addition to the juice is properly
mixed.
"A," the said phosphite of alumina, is prepared as follows:-
In one process the raw material used consists of spodium powder, sulphuric acid,
and sulphate of alumina, and by the alternative action of the spodium and the
sulphuric acid there is first obtained free phosphoric acid containing lime; the said
phosphoric acid with the sulphate of alumina, gypsum, sludge, and other sweepings,
form a pulp from which the sulphite of alumina is lixiviated by water, and the
result is a clear watery fluid which is applied in the improved method as a
separating agent under the denomination of "A.”
Or phosphoric acid and hydrate of alumina in the state in which they are sold
are directly mixed together with water, then this solution is either diluted or
concentrated, as required, and the same is applied in the manner stated. This
agent "A," phosphite of alumina, or a solution of alumina in phosphoric acid is a
new one.
"C," another agent which is applied, and is hereinafter called "C," is prepared
in the following manner :-
In the production of red or yellow prussiate of potash a residual powder ensues,
which is used as a manure (though of little value) and for decolouring glycerine,
potato syrup, vegetable oils, okerite, and other substances. This residual powder
or raw spodium dust is taken and stirred in a vat with hot water, and then
lixiviated until the run off water contains little or no trace of incombustible
residues of distillation. By this process, applied by preference, the said raw
residual powder or the spodium dust is freed from all potash compounds, and this
is the first degree of refining.
Then the residual powder or spodium dust which has been thus prepared is
stirred in a wooden vat with raw muriatic acid or nitric acid, and left at rest.
The black pulp of this mixture is then diluted with water, and the salts of iron
and lime, as well as the waste stuffs of this solution, are lixiviated until they are
thoroughly eliminated. By this second refining are washed away the metallic iron,
carbonate of iron, the lime, and the compounds of iron which are generally contained
in the raw residue of prussiate of potash and sometimes in the spodium dust. The

page_text: residual powder thus obtained is dark grey or black, and the spodium dust is velvet
black; it essentially contains decolouring animal charcoal, and, besides, some sand
and insoluble salts of lime.
In case the residues, which are by preference used as described, should not be at
hand in sufficient quantities as required, they may be also supplied directly from
the waste blood of town butcheries. The caked or more fluid blood, the wastes of
flesh, of glue, of wool, or of tannery, are heated in the ordinary spodium pots or
retorts, and there is obtained the same raw material as the raw residual powder
above described. Also the charcoal which remains in the retorts in the production
of gas from waste wool may be used as a raw material for the purpose. All these
kinds of nitric charcoal must be refined, lixiviated, and treated with acids, as before
described.
The agent "C," which is thus prepared, may also be obtained from cokes resulting
from the production of gas out of the press cakes of greasy fulling sludge. The
said cokes contain nitric charcoal, and may be applied for decolouring sugar.
The residual powder or spodium dust may be revivified after its use for
decolouring sugar. For this purpose it is lixiviated until the sugar is fully
eliminated, and it is boiled in a wooden vat with etching lye of soda, whereby it is
freed from all organic substances. Then the said powder, if necessary, is boiled
once more with soda or etching lye of soda and washed with soda, which may be
done upon filtering cloth or in a filter press, after which the powder is put once
more into a wooden vat and treated with muriatic acid. After boiling the mixture
is again washed out upon a filter cloth or in a filter press, upon which the residual
powder or spodium dust thus thoroughly cleansed is dried in a suitable drying stove
or upon drying plates, and can then be used again as before. If after frequent use
the said residual powder or spodium dust has lost its decolouring power it is
heated to a glow in air tight retorts, and after cooling down may be used again as
before.
In the foregoing statement the two agents "A" and "C" have been described,
which are often referred to in the description of the method of refining.
After heating the juice there is added to the same, if not done before (as
mentioned), one half to five per cent. of lime and refined residual powder or
spodium dust, the latter being either raw or refined. The quantities of the agent
added may be varied, and it is to be understood that all further indications of
quantities or weights are variable according to circumstances. Wherever the
addition of lime, phosphate of alumina, residual powder ("C"), or spodium powder
is expressed in per cents., the latter are always to be understood in reference to the
quantity of beets. The juice then after complete saturation, and, if necessary,
in a heated state, is now separated from the pulp by means of a suitable press or
filter.
When the fluid juice requires to be twice saturated the refined residual powder
or spodium dust may either be added at the beginning of the second saturation or
after the same. The said addition may be recovered then, as it will be contained
in the cakes of the pulp, and may be revivified, as before described under "C."
If the said addition of refined residual powder or spodium dust is not required
to be recovered the saune may by preference be added during the first saturation
or separation. The juice thus refined is now brought to the boiler to be condensed
into molasses by evaporation.
After henting the boiler residual powder or spodium dust is added, and if a
higher degree of refining be desired there is further added 1/200 to 2/100 per cent.
of phosphite of alumina, as described under " A," whereupon the saturation is
continued up to the required degree. The molasses is then placed on a press covered
with linen, Hannel, fustian, or other suitable fabric, and the juice obtained therefrom
is finally condensed in a vacuum until it can be filled in moulds, as usual.
The molasses thus refined may if preferred be further refined by the usual
spodium filtration, but this will still include the improved method of refining
described above. The said residual powder or spodium dust then will act on the

page_text: juice of a highly refined condition, and the agent may easily be revivified, as
described under "C."
The second modification of the improved method of refining, or that in application
with solutions of raw sugar or syrups, will now be described.
The raw sugar or syrup is dissolved or diluted with pure water in ordinary
boilers, and brought to a suitable consistency, on which there is added to this
solution in a heated state one quarter to two-and-a-half per cent. of lime (per cents.
of the quantity of raw sugar or dry substance). The milk of lime "B," which is
used by preference in this application, as also in that described before, may, if
preferred, be prepared in the following manner :-
"B." Well burned lime is thrown into pure water, and stirred into the state of
milk, and when the pulp has set the water is let off and mixed again with water.
This is repeated three or four times, whereby the alkaline salts which may be
contained in the water, as well as in the limestone, are washed off. The use of
milk of lime prepared in this manner is preferred, although not absolutely necessary
to produce a good refining. The clear obtained after adding (and well mixing) the
milk of lime, as described, to the solution of sugar is heated and skimmed.
There is further added 0-2 to 0.5 per cent. of phosphite of alumina, as described
under "A," and residual powder or spodium dust as stated.
After skimining the clear is saturated with alkaline matter, as usual. If it is
desired to recover the addition of residual powder or spodium dust the saturation
must be done at once after adding the phosphite of alumina. The pulp then must
be separated from the clear juice, and the latter submitted to the operation with
residual powder or spodium dust. These agents may be recovered and revivified
for repeated use, as described under "C."
All the pulpy matters, as well as the residual powder and the spodium dust which
are recovered from the filters, may be lixiviated by water in order to recover the
sugar they still contain. The said lye water may either be used for diluting raw
sugar, or they may be condensed in the evaporators. After the application of the
improved method there is no need of additional refining.
The third modification of the said Invention consists in applying the improved
method of refining with molasses or little sub-product syrups. The syrups of the
third, fourth, or further production, as well as the juices recovered from the osmosis
process, or from the various molasses saturations, and further the molasses diluted
below sixty per cent. Balling, are put into a boiler and mixed together either at
once, or after the addition of lime with phosphite of alumina "A." "If the addition
of lime is made after that of the phosphite the contents of the boiler are slightly
heated, and the skimming takes place before the feeding of lime or milk of lime.
The mixture is then saturated and pressed through suitable filters. The refined
juice may be either directly concentrated by evaporation, or it may previously be
treated in a heated state with refined residual powder or spodium dust, and thereby
further decoloured. It is then separated by suitable filters from the residual powder
or spodium dust and concentrated by evaporation until it can be filled in moulds
for crystallization.
The saturation by carbonic acid is usually effected by the ordinary carbonic
acid produced during the working process, but it may also be taken from the
generator hereinafter described, and which is new as applied to the manufacture of
sugar.
In the said generator the carbonic acid is obtained from carbonic compounds, such
as limestone, witherite, strontianite, marble, marlstone, chalk, magnesite, dolomite,
or the like, acted upon by dissolving acids, such as sulphuric or muriatic acid, and
the carbonic acid thus obtained is from four to nine times more effective than all
the kinds of carbonic acid hitherto used in the manufacture of sugar, such as that
derived from a lime kiln or burning cokes and the like. The gas from the said
generator may likewise be washed to such a degree as to become pure. The con-
struction of the generator is, as usual, for the production of mineral waters, and the
Invention only applies to its use in manufacturing sugar, but expensive pumps

page_text: and blowers for compressing and injecting the carbonic acid are thereby dispensed
with.
The following are some of the advantages resulting from the use of the
Invention :-
There is no need of a spodium house with all its accessories, as usual, owing to
which the working expenses are considerably reduced.
There is also a considerable saving of time, fuel, steam, water, and labor, together
with the prevention of waste connected with the filtration over granulated spodium,
and the quality of the sugar produced is improved.
Having thus described the nature of the said Invention, and the manner in which
the same is to be performed (communicated to me from abroad as aforesaid), I hereby
declare that what I claim ns of the said Invention is,-
First. The method of refining and decolouring saccharine juices, as described,
without the use of spodium filtration.
Secondly. The use of phosphite of alumina, as described, as an additional agent
during the process of separation and saturation.
Thirdly. The use of a new and original agent "C," as described, consisting of
refined residual powder and of refining spodium dust.
And, lastly. The application to the manufacture of sugar of a generator, as
described, for the production of carbonic acid gas to be used therein.
In witness whercof, I, the said William Spence, have hereunto set my hand
and seal, the Twenty sixth day of August, in the year of our Lord One
thousand eight hundred and eighty.
Witness,
FRANK REDMAN,
8, Quality Court,
Chancery Lano.
WILLIAM SPENCE. (L.S.)