A PROCESS OF EXTRACTING SUGAR FROM MOLASSES SYRUPS AND THE JUICE OF PLANTS
Year: 1883

page_text: LETTERS PATENT to CARL STEFFEN, of the City of Vienna in the Empire of
Austria. for an Invention of "A PROCESS OF EXTRACTING SUGAR FROM
MOLASSES SYRUPS AND THE JUICE OF PLANTS
"
PROVISIONAL SPECIFICATION left by the said Carl Steffen at the Office of
the Commissioners of Patents on the 12th May 1883.
CARL STEFFEN of the City of Vienna in the Empire of Austria "A PROCESS OF
EXTRACTING SUGAR FROM MOLASSES SYRUPS AND THE JUICE OF PLANTS."
My said invention relates to improvements in processes for extracting sugar
from molasses, syrups and the juice of plants as secured to me by letters patent
N° 967 dated February 22nd 1883.
According to my process as described in my original patent on a process for
extracting sugar from molasses, syrups and the juice of plants (called by me
separation) the sugar was separated from the aqueous saccharine solution by
forming a calcareous saccharine solution saturated with lime and carrying out the
said operation at a temperature under 35° Centigrade and then introducing a fresh
quantity of lime into the calcareous saccharine solution so as to convert the
soluble calcareous saccharate into an insoluble combination and precipitate or
separate the same from the solution but always taking care that the temperature
never exceeds 35° Centigrade.
The object of this present specification is to introduce certain improvements on
my said process which consist chiefly.
1) of a method of saturating saccharine solutions with lime in a rational
efficatious manner at any desirous temperature under 35° Centigrade and also a
practical method of introducing the lime into the aqueous calcareous saccharine
solution saturated with lime at such said temperatures, which said method can
be employed in separating out or precipitating calcareous sugar according to the
separation process and all other such separating methods for calcareous sugar the
object of which is to precipitate the sugar out of aqueous saccharine solutions at
the ordinary or a low temperature with the assistance of lime and without
employing warınth or alcohol.

page_text: 2) of the method of facilitating the rapid formation of calcareous saccharine
solutions in introducing lime into aqueous saccharine fluids or liquids as well as
the precipitation of the calcareous saccharate by introducing lime into such said
solution of calcareous saccharate in such manner that the period of the formation
of saturated calcareous saccharate and the precipitation of the calcareous saccharate
follow each other with such rapidity that the introduction of the requisite quantity
of lime for both operations can be simultaneously introduced without producing
unfavorable results.
3) of the circumstance that when a calcareous saccharine compound containing
more lime per 100 parts sugar than will form a single basic compound is introduced
into an aqueous saccharine fluid in such quantity that the entire sugar in the
mass or mixture contains more than 15 parts by weight of calcium oxyd to
100 parts sugar in solution, the sugar can be precipitated or separated out of this
said calcareous saccharine solution by introducing free lime at a temperature
under 35° Centigrade and without employing alcohol or artificial warmth.
The same result can be attained by introducing so much sugar to a precipitated
calcareous saccharine compound or admixture above the one basic proportions that
the mixture contains more than 15 parts by weight of calcum oxyd in solution to
100 parts sugar and then adding a sufficient quantity of free lime.
4) of the circumstance, that a higher calcareous saccharine compound derived
from an earlier precipitating operation is added to a calcareous saccharine solution
it being immaterial how the same was formed so that nearly all the sugar in the
mixture is precipitated as an insoluble calcareous saccharine compound when the
calcareous saccharine compound so introduced; contains so much lime that 20 parts
calcium oxyd to 100 parts sugar is dissolved in the mixture and the temperature
maintained under 35° Centigrade.
5) of the method of separating the solid calcareous saccharine compound
precipitated according to the process patented to me and the method given in this
said specification, into soluble calcareous saccharine compounds and free bydrate
of lime.
In respect to the first case, the best and most efficacious manner of attaining a
calcareous saturation of saccharine liquids or fluids is, when the lime is introduced
into an aqueous saccharine solution at a temperature under 35° Centigrade and the
mixture continuously cooled in such manner that an increase in warmth or a
raising of the temperature through the lime introduced and the warmth hereby
generated during the saturation or lime introduction period is as far as possible
prevented.
If the aqueous with lime saturated calcareous saccharine solution is formed, the
precipitation of the calcareous saccharate can be immediately proceed with without
removing any excess of lime that may have remained from the saturating period
by introducing the requisite quantity of lime at a temperature below 35° Centigrade
for precipitating or separating out the sugar, care being taken that the temperature
of the liquid is raised as little as possible by the lime introduced and the warmth
generated by the same.
This can be attained, in practice, by arranging cooling devices in such apparatus
wherein the mixture of the saccharine solution with the lime is carried out, or in
placing such said cooling devices on the exterior of the said mixing apparatus,
vessels or receptacles so that the requisite cooling of the fluid during the lime
introducing period can be effected and the warmth generated by the lime prevented
from exercising any injurious or deleterious action on the formation of the
calcareous saccharate.
Water pipes or tubes for cooling can be arranged in the mixing apparatus or
the stirring apparatus can be made from such cooling pipes or tubes, or other
suitable devices can be employed so that physical or chemical methods are applied
to absorb the heat emitted through the introduction of the lime as aforesaid.
The lime is introduced into the fluid or liquid in such quantities and at such
times that the cooling device can absorb the warmth generated.

page_text: In order to be able to judge the correct size it must be taken into account that
for each 100 Kilogrammes sugar operated upon 15,000 to 20,000 units of heat are
set free by the application of the lime.
In respect to case II it must be mentioned that in my patented separation
process for producing calcareous sugar from saccharine fluids stress is laid on the
circumstance that the spontaneous precipitation of calcareous sugar without the aid
of artificial warmth or alcohol does not take place when the precipitation of
calcareous sugar has been preceeded by the formation of a soluble with lime
saturated calcareous saccharine compound.
Calcareous saccharate is never precipated from aqueous saccharine solutions
without the employment of alcohol or artificial heat in such manner that the lime
introduced forms an insoluble and precipitating calcareous saccharine compound
direct with the sugar it being immaterial how and under what circumstances the
said lime was introduced but on the contrary. the lime and the sugar must always
first form a soluble with lime saturated calcareous saccharine compound and only
then when all these requirements have been fulfilled can a precipitation of
calcareous saccharate take place in the presence of a profficient quantity of lime.
That this is correct is proven by the facts firstly that one never attains a
precipitating of calcareous saccharate from an acqueous saccharine solution if the
same has not been previously fully saturated with lime, secondly, that when only
a part of the sugar has been precipitated by the introduction of lime into a
saccharine solution saturated with lime the remaining lye is a saccharine solution
fully saturated with lime out of which the entire sugar contained in the same can
be precipitated by introducing a fresh quantity or quantities of lime and carefully
observing that the temperature does not exceed 35° Centigrade.so that at last
when a pure saccharine solution was employed lime water remains as lye in which
no more lime is to be found than corresponds with the suitability of lime in
water.
This is further corroborated by the fact that a lime saturated calcareous
saccharine solution will convert solid calcareous saccharate until a perfectly with
lime saturated calcareous saccharine solution has been formed.
If now care is taken to produce the rapid formation of lime saturated calcareous
saccharine solutions under given conditions and the requirements for the
precipitation of calcareous saccharate out of such said solutions by introducing
lime are fulfilled both operations can follow each other with such rapidity that the
quantity of lime required for the first and second operation can be introduced at
one time into the saccharine solution. These conditions which must be fulfilled
consist therein that the commencing temperature of the aqueous saccharine fluid
or liquid must be so low and the quantity of sugar in the liquid so limited that the
quantity of lime for forming a lime saturated saccharine solution and for
precipitating the calcareous saccharate (whether such lime be introduced at one
time or successively) and consequently the heat emitted will not create a
temperature in the fluid equal to 35° C.
The lower the temperature can be held under 35° C. the better will be the result
obtained and the less lime is required.
As mentioned above 15,000 units of heat are set free for every 100 kilo sugar
which must be carefully observed.
The most important consideration is to prevent the injurious or deleterious effect
of the warmth set free by the lime which can be attained when the temperature of
the fluid is sufficiently low at the commencement of the operation.
As the quantity of lime depends on that of the sugar and the first ie the lime
determines the quantity of warmth set free it is evident that the injurious
influence or action of the warmth set free can be decreased by limiting the
quantity of sugar in the fluid so that a less quantity of lime is required for the
operation.
If on the other hand mechanical, chemical or physical means or devices are
employed which absorb the heat produced on introducing the lime as soon as the

page_text: same is emitted or remove the same it is possible to commence the operation
without regard to a specially low temperature or limitation of the sugar in the
liquid and to precipitate the calcareous saccharate from the aqueous saccharine
solution by introducing the entire quantity of lime necessary to precipitate the
sugar so long as attention is paid to keeping the temperature below 35° C.
In respect to the cases 3 and 4 firm calcareous saccharate [zuckerkalk]
precipitated by the foregoing method is mixed with the saccharine solution and
the further precipitation of insoluble calcareous saccharate by adding free lime
(ad 3) to the saccharine solution or by adding a further quantity of firm calcareous
saccharate (ad 4) proceeded with.
The calcareous saccharate so precipitated is separated from the lye in suitable
filter presses, one part of the same is not washed but employed for new
precipitating purposes whereas the other part is washed and converted into sugar
in the well known manner.
The process mentioned ad 5 is based on the property of the calcareous saccharate
precipitated according to my separation or precipitating process and the four
precipitating methods mentioned above, to decompose in aqueous more or less strong
saccharine liquids in such manner that a soluble calcareous saccharine compound
is created and free hydrate of lime precipitated.
This property is in this case made use of to convert the finished purified
calcareous saccharate into a calcareous saccharine solution which is poor in lime
through the action of a free saccharine liquid the separating out the superfluous
lime before the calcareous saccharate is acted on by acids to decompose the same.
For this purpose the hard calcareous saccharate is mixed with a saccharine
liquid and the resulting calcareous saccharine solution separated from the hydrate
of lime in a filter press or other suitable apparatus.
The calcareous saccharine solution is subjected to saturation whereas the hydrate
of lime is waste.
The hard calcareous saccharine compounds precipitated according to the methods
described ad 1, 2, 3, 4 which is best carried out by employing quick lime ground
in a suitable lime mill and in one of the known mashing apparatus with cooling
devices are separated from the lye in filter presses, suctions bags, centrifugal
machines or other apparatus, suited to separate solid from fluid matters and are
then ground in one of the well known saccharate mills.
'
According to case 5 the said compounds are converted into a soluble calcareous
saccharine compound, then saturated and worked up into sugar in the well known
manner.
The saccharate was washed with pure water of ordinary temperature in the
filter presses etc. which said water is employed for dissolving molasses syrups etc. or
for the extraction or diffusion of saccharine bodies:

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Carl Steffen in the Great Seal Patent Office on the 10th November
1883.
CARL STEFFEN of the City of Vienna in the Empire of Austria. "A PROCESS OF
EXTRACTING SUGAR FROM MOLASSES SYRUPS AND THE JUICE OF PLANTS
"
My said invention relates to improvements in processes for extracting sugar from
molasses, syrups and the juice of plants as secured to me by letters patent dated
the twenty second day of February one thousand eight hundred and eighty three
and numbered 967.
According to my process as described in my original patent on a process for
extracting sugar from molasses, syrups and the juice of plants (called by me
separation) the sugar was separated from the acqueous saccharine solution by
forming a calcareous saccharine solution saturated with lime and carrying out the
said operation at a temperature under 35° Centigrade and then introducing a fresh
quantity of lime into the calcareous saccharine solution so as to convert the soluble
calcareous saccharate into an insoluble combination and precipitate or separate the
same from the solution but always taking care that the temperature never exceeds
35° Centigrade. The object of this present specification is to introduce certain
improvements on my said process which consist chiefly,
1) Of a method of saturating saccharine solutions with lime in a rational
efficacious manner at any desirous temperature under 35° Centigrade and also a
practical method of introducing the lime into the aqueous calcareous saccharine
solution saturated with lime at such said temperatures which said method can be
employed in separating out or precipitating calcareous sugar according to the
separation process and all other such separating methods for calcareous sugar the
object of Which is to precipitate the sugar out of aqueous saccharine solutions at the
ordinary or a low temperature with the assistance of lime and without employing
warmth or alcohol.
2.) of the method of facilitating the rapid formation of calcareous saccharine
solutions in introducing lime into aqueous saccharine fluids or liquids as well as
the precipitation of the calcareous saccharate by introducing lime into such said
solution of calcareous saccharate in such manner that the period of the formation
of saturated calcareous saccharate and the precipitation of the calcareous saccharate
follow each other with such rapidity that the introduction of the requisite quantity
of lime for both operations can be simultaneously introduced without producing
unfavorable results.
3) of the circumstance that when a calcareous saccharine compound containing
more lime per 100 parts sugar than will form a single basic compound is intro-
duced into an aqueous saccharine fluid in such quantity that the entire sugar in
the mass or mixture contains more than 15 parts, by weight of calcium oxyd
to 100 parts sugar in solution, the sugar can be precipitated or separated out of
this said calcareous saccharine solution by introducing free lime at a temperature
under 35° Centigrade and without employing alcohol or artificial warmth.
The same result can be attained by introducing so much sugar to a precipitated
calcareous saccharine compound or admixture above the one basic proportion that
the mixture contains more than 15 parts by weight of calcium oxyd in solution to
100 parts sugar and then adding a sufficient quantity of free lime.
4) of the circumstance, that a higher calcareous saccharine compound derived
from an earlier precipitating operation is added to a calcareous saccharine solution
(it being immaterial how the same was formed) so that nearly all the sugar in the

page_text: mixture is precipitated as an insoluble calcareous saccharine compound when the
calcareous saccharine compound so introduced contains so much lime that 20 parts
calcium oxyd to 100 parts sugar is dissolved in the mixture and the temperature
maintained under 35° Centigrade.
5) of the method of separating the solid calcareous saccharine compound
precipitated according to the process patented to me and the method given in this
said specification into soluble calcareous saccharine compounds' and free bydrate of
lime.
In respect to the first case; the best and most efficacious manner of attaining a
calcareous saturation of saccharine liquid or fluid is, when the lime is introduced
into an aqueous saccharine solution at a temperature under 35° Centigrade and
the mixture continuously cooled in such manner that an increase in warmth or a
raising of the temperature through the lime introduced and the warmth hereby
generated during the saturation or lime introduction period is as far as possible
prevented.
If the aqueous with lime saturated calcareous saccharine solution is formed, the
precipitation of the calcareous saccharate can, be immediately proceeded with
without removing any excess of lime that may have remained from the saturating
period by introducing the requisite quantity of lime at temperatures below
35° Centigrade for precipitating or separating out the sugar, care being taken
that the temperature of the liquid is raised as little as possible by the lime
introduced and the warmth generated by the same.
This can be attained in practice by arranging cooling devices in such apparatus
wherein the mixture of the saccharine solution with the lime is carried out, or
placing such said cooling devices on the exterior of the said mixing apparatus
vessels or receptacles so that the requisite cooling of the fluid or liquid during the
lime introducing period can be effected and the warmth generated by the lime,
prevented from exercising any injurious or deleterious action on the formation of
the calcareous saccharate.
Water pipes or tubes for cooling can be arranged in the mixing apparatus or the
stirring apparatus can be made from such cooling pipes or tubes, or other suitable
devices can be employed so that physical or chemical methods are
applied, to absorb
the heat emitted through the introduction of the lime as aforesaid.
The lime is introduced into the fluid or liquid in such quantities and at such
times that the cooling device can absorb the warmth generated.
•
In order to be able to judge the correct size it must be taken into account that
for each 100 Kilogrammes sugar operated upon 15,000 to 20,000 units of heat
are set free by the application of the lime.
In respect to case 2 it must be mentioned that in my patented separation
process for producing calcareous sugar from saccharine fluids stress is laid on the
circumstance that the spontaneous precipitation of calcareous sugar without the
aid of artificial warmth or alcohol does not take place when the precipitation of
calcareous sugar has been preceeded by the formation of a. soluble with lime
saturated calcareous saccharine compound.
-
Calcareous saccharate is never precipitated from aqueous saccharine solutions
without the employment of alcohol or artificial heat in such manner that the lime
introduced forms an insoluble and precipitating calcareous saccharine compound
direct with the sugar, it being immaterial bow and under what circumstances the
said lime was introduced, but on the contrary the lime and the sugar must always
first form a soluble, with lime saturated calcareous saccharine compound and only
then when all these requirements have been fulfilled can a precipitation of
calcareous saccharate take place in the presence of a sufficient quantity of lime.
That this is correct is proven by the facts, firstly, that one never attains a
precipitation of calcareous saccharate from an aqueous saccharine solution if the
same has not been previously fully saturated with lime, secondly, that when only
a part of the sugar has been precipitated by the introduction of lime into a
saccharine solution saturated with lime the remaining lye is a saccharine solution

page_text: fully saturated with lime out of which the entire sugar contained in the same
can be precipitated by introducing a fresh quantity or quantities of lime and
carefully observing that the temperature does not exceed 35° Centigrade so that
at last when a pure saccharine solution was employed lime water remains as lye
in which no more lime is to be found than corresponds with the solubility of lime
in water.
This is further corroborated by the fact, that a lime saturated calcareous
saccharine solution will convert solid calcareous saccharate until a perfectly with
lime saturated calcareous saccharine solution has been formed.
If now care is taken to produce the rapid formation of lime saturated calcareous
saccharine, solutions under given conditions and the requirements for the pre-
cipitation of calcareous saccharate out of such said solutions by introducing lime.
are fulfilled both operations can follow each other with such rapidity that the quantity
of lime required for the first and second operations can be introduced at one time.
into the saccharine solution.. These conditions, which must be fulfilled consist
therein, that the commencing temperature of the aqueous saccharine fluid or liquid
must be so low and the quantity of sugar in the liquid so limited that the
quantity of lime for forming a lime saturated saccharine solution and for pre-
cipitating the calcareous saccharate (whether such lime be introduced at one time
or successively) and consequently the heat emitted will not create a temperature
in the fluid equal to 35° Centigrade.
The lower the temperature can be held under 35° Centigrade the better will be
the results obtained and the less lime is required. As mentioned above 15,000
units of heat are set free for every 100 Kilo sugar which must be carefully
observed.
The most important consideration is to prevent the injurious or deleterious
effect of the warmth set free by the lime which can be attained when the tempe-
rature of the fluid is sufficiently low at the commencement of the operation.
As the quantity of lime depends on that of the sugar and the first i.e. the lime
determines the quantity of warmth set free, it is evident that the injurious
influence or action of the warmth set free can be decreased by limiting the
quantity of sugar in the fluid so that a less quantity of lime is required for the
operation.
If on the other hand mechanical, chemical or physical means or devices are
employed which absorb the heat produced on introducing the lime as soon as the
same is emitted or remove the same it is possible to commence the operation
without regard to a specially low temperature or limitation of the sugar in the
liquid and to precipitate the calcareous saccharate from the aqueous saccharine
solution by introducing the entire quantity of lime necessary to precipitate the
sugar so long as attention is paid to keep.the temperature below 35° Centigrade.
In respect to the cases 3 and 4, firm calcareous saccharate (Zuckerkalk) pre-
cipitated by the foregoing methods is mixed with the saccharine solution and the
further precipitation of insoluble calcareous saccharate by adding free lime (ad 3)
to the saccharine solution or by adding a further quantity of firm calcareous
saccharate (ad 4) proceeded with.
The calcareous saccharate so precipitated is separated from the lye in suitable
filter presses, one part of the same is not washed but employed for new precipitating
purposes, whereas the other part is washed and converted into sugar in the well
known manner.
The process mentioned (ad 5) is based on the property of the calcareous saccharate
precipitated according to my separation or precipitating process and the four
precipitating methods mentioned above, to decompose in aqueous more or less
strong saccharine liquids in such manner that a soluble calcareous saccharine
compound is created and free hydrate of lime precipitated. This property is in
this case made use of to convert the finished purified calcareous saccharate into a
calcareous saccharine solution which is poor in lime through the action of a free

page_text: saccharine liquid thus separating out the superfluous lime before the calcareous
saccharate is acted on by acids to decompose the same.
For this purpose the hard calcareous saccharate is mixed with a saccharine liquid
and the resulting calcareous saccharine solution separated from the hydrate of lime
in a filter press or other suitable apparatus.
The calcareous saccharine solution is subjected to saturation whereas the
hydrate of lime is waste. The hard calcareous saccharine compound precipitated
according to the methods described ad 1, 2, 3, 4 which is best carried out by
employing quick lime ground in a suitable lime mill and in one of the known
mashing apparatus with cooling devices, are separated from the lye in filter presses,
suction bags, centrifugal machines or other apparatus suited to separate solid from
fluid matters and are then ground in one of the well known saccharate inills..
According to case 5 the said compounds are converted into a soluble calcareous
saccharine compound, then saturated and worked up into sugar in the well known
manner. The saccharate was washed with pure water of ordinary temperature in
the filter presses etc which said water is employed for dissolving molasses, syrups etc
or for the extraction or diffusion of saccharine bodies.
Having now described my said invention for improvements in processes for
extracting sugar from molasses, syrups and the juice of plants I wish it to be
understood that what I claim and desire to secure by Letters Patent is :-
By the precipitation or separation of calcareous saccharate out of aqueous
saccharine liquids by introducing lime without employing alcohol or artificial
warmth at any desirable temperature under 35° Centigrade.
1 The cooling of the aqueous saccharine solution by the operation of introducing
lime into the said solution, or saturating the same with lime and during the period
of the lime introduction and saturating period and also the cooling of the calcareous
saccharine solution by the operation of separating out or precipitating calcareous
saccharate and during the lime introduction period and the precipitation of the
calcareous saccharate period substantially as and for the purpose set forth in the
foregoing specification.
2. The precipitation of calcareous saccharate out of aqueous saccharine fluids
or solutions at any desired temperature under 35° Centigrade without the employ-
ment of alcohol or artificial warmth in such manner that the temperature of the
fluid liquid or solution on commencing the operation is so low and the sugar
contained in the fluid or liquid so limited that the introduction of a sufficient
quantity of lime to precipitate the said sugar in the fluid, liquid or saccharine
solution will not evolve or create sufficient warmth to raise the temperature of the
said fluid liquid or saccharine solution under treatment to 35° Centigrade
substantially as and for the purpose set forth in the foregoing specification.
3. The employment of mechanical means or devices or chemical or physical
processes by the above mentioned process of precipitating calcareous saccharate;
the object of which said devices or processes are to absorb, transmit or carry off
the heat evolved or generated through the introduction of lime in the aforenamed
saccharine solution substantially as and for the purpose set forth in the foregoing
specification.
4. The production of an aqueous calcareous saccharine solution by saturating
aqueous saccharine fluids liquids or solutions with a calcareous saccharine compound
containing more lime than a one basic compound or in other words a more than
single basic compound for the purpose of precipitating calcareous saccharate by
introducing lime at a temperature under 35° Centigrade substantially as and for
the purpose set forth in the foregoing specification.
5. The precipitation of calcareous saccharate out of aqueous saccharine solutions
fluids or liquids by introducing a sufficient quantity of calcareous saccharate rich
in lime at temperatures under 35° Centigrade and without the employment of
alcohol or artificial warmth substantially as and for the purpose set forth and
described in the foregoing specification.

page_text: 6. The employment and application of my said invention as specified in the
foregoing 5 claims to the waste or spent fluids or liquids resulting from the
precipitating operations in order to obtain the entire amount of sugar contained
in the same substantially as and for the purpose set forth in the foregoing
specification.
7. The convertion of such precipitated firm calcareous saccharate produced from
aqueous saccharine solutions at a temperature under 35° Centigrade without the
employment of alcohol or artificial heat into soluble calcareous saccharine compounds
and the separating out of the superfluous lime through the action of aqueous
saccharine solutions or aqueous calcareous saccharine solutions which are poor in
lime substantially as and for the purpose set forth in the foregoing specification.
In witness whereof I the said Carl Steffen have hereunto set my hand and
seal this twenty fifth day of. June in the year of Our Lord One thousand eight
hundred and eighty three
Witnesses
FERDINAND BLUM.
HERM. KOHLSTOCK.
CARL STEFFEN (L.S.)