Year: 1887

page_text: Date of Application, 12th May, 1887
Complete Left, 3rd Mar., 1888
Complete Accepted, 6th Apr., 1888
I, PRIMUS JUSTUS EMIL HEFFTER of Altjaner, near Janer, Schl, Germany,
Director of Sugar Refinery, do hereby declare the nature of this invention to be as
follows:-
The clarifying of sugar solutions by means of tannin has already been tried, but the
suggestions hitherto made have not led to anything beyond laboratory experiments,
as it was not possible by means of tannin to obtain filterable precipitants nor to
accomplish a complete clarification of the juices.
This result is due according to the experiments of the applicant, to the fact that the
juices have not been concentrated to the correct degree, were not made alkaline by
lime, and that the precipitation was not produced in the right way.
To obtain a coarse flaked precipitate easily separated from the liquid, it is
absolutely necessary that the juices should have a certain alkalinity due to lime, that
they should be in a concentrated state, that they should be cooled before or during
the addition of tannin, and that they should afterwards again be heated to finish the
clarification.
Without these four conditions the clarification with tannin of the juices cannot be
practically accomplished.
The degree of concentration of the juices, to act properly should be equal to that of
the rob. The minimum alkalinity should then be 0.05. The quantity of tannin
required to be added to the solution or the juices depends on the alkalinity; it is so
proportioned that after the clearing there remains yet an alkalinity of about 0.02
to 0.04. By the cooling of the juice to about 25 to 40 degrees Centigrade, a gray
coarse flaked precipitate is separated in consequence of the action of the tannin,
which probably partly consists in tannate of lime, and contains the nitrogeneous
bodies of the juices.
This precipitate only forms when the alkaline solution is cooled sufficiently. In
order to complete the clarification the juice or the solution, "along with" the

page_text: precipitate, is heated up to from 80 to 95 degrees Centigrade. Consequently the
precipitate absorbs the coloring matter possibly present in the juice, without changing
its constitution in such a way that the precipitate which can easily be separated from
the liquid, (by filtering, for instance) now shows a reddish color.
By this method one part of the tannin is used to separate lime from the juice, so that
the alkalinity of the juice is forced down to 0.05, the other part of the tannin serves
to throw out the nitrogeneous dirt from the juices.
The batch of tannin required toneutralise the great alkalinity of the juice (of at
least 0.05) is very considerable, and as the price of the tannin is rather high, it seems
desirable under these circumstances, to measure out the tannin to be added, as
sparingly as possible.
The foregoing described method may therefore be modified, and for this purpose
the following facts are given.
It has been found that that part of the tannin which combines with the lime of the
juice, and thus lowers its alkalinity, can be replaced entirely, or almost entirely by
other lime precipitants. Such precipitants may be for instance, carbonic acid,
sulphurous acid, sulphuric acid, phosphoric acid, oxalic acid. The lime precipitate
obtained through the means of such precipitants, effects through its weight also an
easy complete deposit of the slimy flaked tannic acid precipitate by being, so to say,
enveloped in it. It enables thus the tannic acid to have a more intense effect. upon
the nitrogeneous substances in the juice.
Through the reduction of the quantity of tannin thus made possible, the color of
the sugar product is lightened.
It must further be pointed out that such kinds of raw sugar as are produced by, for
instance, the eliminating process of the Steffen-osmose-diffusion process first described
in German Patent No. 31486 and since then elaborated in numerous English patents,
by the bistrontian precipitation process contain more or less Melitriose (or its
equivalent Raffinose, Melitose, Gossypose) whereby these kinds easily fall 1 to 2
shillings per hundred weight lower, because in the refining the very weakly sweetened
Melitriose is lost through its being more easily soluble in water than the raw sugar.
In applying the present method the raw sugar is obtained free from Melitriose and a
partial disappreciation is prevented.
According to this the above described method may be modified as follows:-
To the juices brought to the consistence of the rob with an alkalinity of at least 0.05
is added as much precipitant, for instance, carbonic acid, sulphurous acid, sulphuric
acid, phosphoric acid, or oxalic acid, as shall cause the alkalinity to fall to 0.01-0.05,
during which time the whole mass cools to from 25 to 40 degrees Centigrade. Now
tannic acid (tannin) is added until a flaky precipitate is formed, the precipitate is
allowed to deposit and is separated from the clear juice, which is heated up to
98 degrees Centigrade, whereby a secondary precipitation of tannin is effected, the
juice is separated from this after-precipitate by means of presses, and may then be
boiled directly. The juice purified in this way goes directly to the boiling process
without carbon filtration.
The expression "tannin" of this description means any material containing tannin
or tannic acid or its equivalent.
T1: 111 1

page_text: Improvements in the Method of Clarifying and Saturating Sugar
Solutions, Especially Beet-root Rob, by the Means of Tannic Acid
or Tannin.
I, PRIMUS JUSTUS EMIL HEFFTER, Altjaner, near Janer, Schl, Germany, 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 :-
The clarifying of sugar solutions by means of tannin has already been tried, but
the suggestions hitherto made have not led to anything beyond laboratory experi-
ments, as it was not possible by means of tannin to obtain filterable precipitates, nor
to accomplish a complete clarification of the juices.
This result is due, according to the experiments of the applicant, to the fact that
the juices have not been concentrated to the correct degree, were not made alkaline
by lime, and that the precipitation was not produced in the right way.
To obtain a coarse flaked precipitate easily separated from the liquid, it is
absolutely necessary that the juices should have a certain alkalinity due to lime, that
they should be in a concentrated state, that they should be cooled before or during the
addition of tannin, and that they should afterwards again be heated to finish the
clarification.
Without these four conditions the clarification with tannin of the juices cannot be
practically accomplished.
The degree of concentration of the juices, to act properly, should be equal to that
of the rob. The minimum alkalinity should then be 0.05. The quantity of tannin
required to be added to the solution or the juices, depends on the alkalinity; it is so
proportioned that after the clearing there remains yet an alkalinity of about 0.03
to 0.04. By the cooling of the juice to about 25 to 40 degrees Centigrade, a gray
coarse flaked precipitate is separated in consequence of the action of the tannin, which
probably partly consists in tannate of lime, and contains the nitrogenous bodies
of the juices.
This precipitate only forms when the alkaline solution is cooled sufficiently. In order
to complete the clarification, the juice or the solution "along with" the precipitate,
is heated up to from 80 to 95 degrees Centigrade. Consequently the precipitate
absorbs the colouring matter possibly present in the juice without changing its
constitution, in such a way that the precipitate, which can easily be separated from
the liquid (by filtering for instance), now shows a reddish colour.
By this method, one part of the tannin is used to separate lime from the juice, so
that the alkalinity of the juice is forced down to 0.05, the other part of the tannin
serves to throw out the nitrogenous dirt from the juices.
The batch of tannin required to neutralize the great alkalinity of the juice (of at
least 0.05) is very considerable, and as the price of the tannin is rather high, it seems
desirable under these circumstances, to measure out the tannin to be added as
sparingly as possible.
απ τα

page_text: The foregoing described method may, therefore, be modified, and for this purpose
the following facts are given. It has been found that that part of the tannin, which
combines with the lime of the juice, and thus lowers its alkalinity, can be replaced
entirely or almost entirely by other lime precipitants. Such precipitants may be for
instance, carbonic acid, sulphurous acid, sulphuric acid, phosphoric acid, oxalic acid.
The lime precipitate obtained through the means of such precipitants, effects through
its weight also an easy complete deposit of the slimy flaked tannic acid precipitate
by being so to say, enveloped in it. It enables thus, the tannic acid to have a more
intense effect upon the nitrogenous substances in the juice.
Through the reduction of the quantity of tannin thus made possible, the colour of
the sugar product is lightened.
It must further be pointed out that such kinds of raw sugar as are produced by,
for instance the eliminating process of the Steffins-osmose-diffusion-bistrontian
precipitation process, contains more or less, Melitriose (or its equivalent, Raffinose,
Melitose, Gossypose), whereby these kinds easily fall 1 to 2 shillings per hundred-
weight lower, because in the refining, the very weakly sweetened Melitriose is lost
through its being more easily soluble in water than the raw sugar. In applying the
present method, the raw sugar is obtained free from Melitriose, and a partial
disappreciation is prevented.
According to this the above described method may be modified as follows:-
To the juices brought to the consistence of the rob with an alkalinity of at least 0.05
is added as much precipitant, for instance, carbonic acid, sulphurous acid, sulphuric
acid, phosphoric acid, or oxalic acid, as shall cause the alkalinity to fall to 0.01-0.05,
during which time the whole mass cools from 25 to 40 degrees Centigrade. Now
tannic acid (tannin) is added until a flaky precipitate is formed, the precipitate is
allowed to deposit, and is separated from the clear juice, which is heated up to
98 degrees Centigrade, whereby a secondary precipitation of tannin is effected, the
juice is separated from this after-precipitate by means of presses, and may then be
boiled directly. The juice purified in this way goes directly to the boiling process
without carbon filtration.
The expression "tannin" of this description means any material containing tannin
or tannic acid, or its equivalent.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
1. In the clarification of sugar by means of tannic acid (tannin) concentrating the
juices or solutions to the consistency of the rob, and to an alkalinity of at least 0.05,
adding the requisite tannic acid when cooling the juices or solutions down to from
25 degrees to 40 degrees Centigrade adding as much tannic acid (tannin) as will bring
the alkalinity to from 0.02 to 0.04 and give a coarse grained precipitate, and then
heating both liquor and precipitate to from 80 degrees to 90 degrees Centigrade.
2. The partial replacing of the tannic acid in the above process by other precipitant
of lime, so as to reduce the alkalinity to at least 0.05, whereby all or nearly all the
tannic acid can be employed in precipitating the nitrogenous matters, instead of
being used to neutralise the mineral alkali.
Dated this 2nd day of March 1888