IMPROVEMENTS IN THE PURIFICATION OF SUGAR, MOLASSES, AND SACCHARINE JUICES, AND IN, THE REGENERATION OF PART: or THE SUBSTANCES EMPLOYED, AND ALSO IN THE PREPARATION OF MANURE FROM THE RESIDUES THEREOF.”
Year: 1873

page_text: "
LETTERS PATENT to Jean Marie Onésime Tamin, of the City, County,
and State of New York, United States of America, and at present
of Chancery Lane, in the County of Middlesex, Doctor of Medicine,
for the Invention of "IMPROVEMENTS IN THE PURIFICATION OF SUGAR,
MOLASSES, AND SACCHARINE JUICES, AND IN, THE REGENERATION OF PART: or
THE SUBSTANCES EMPLOYED, AND ALSO IN THE PREPARATION OF MANURE FROM
THE RESIDUES THEREOF.”
"
Sealed 'the 20th March 1874, and dated the 26th September 1873.
I
PROVISIONAL SPECIFICATION left by the said Jean Marie Onésime
Tamin at the Office of the Commissioners of Patents, with his
· Petition, on the 26th September 1873.
I, JEAN MARIE ONÉSIME TAMIN, of the City, County, and State of
New York, United States of America, and at present of Chancery Lane,
in the County of Middlesex, Doctor of Medicine, do hereby declare the
nature of the said Invention for "IMPROVEMENTS IN THE PURIFICATION
OF SUGAR, MOLASSES, AND SACCHARINE JUICES, AND IN THE REGENEration of Part
[Price Sd.]

page_text: OF THE SUBSTANCES EMPLOYED, AND ALSO IN THE PREPARATION OF MANURE FROM
THE RESIDUES THEREOF," to be as follows:-
My Invention consists in the use of soluble metallic silico fluorides,
especially the silico fluoride of calcium or of magnesium, or of aluminium,
or of lead, or of manganese, or of nickel, or other soluble metallic silico
fluorides, either separately or combined in any suitable proportion.
•
In carrying out my Invention I proceed as follows:-After having
ascertained the weight of the saline matters contained in the sugar or
saccharine juice to be treated, I add a proportionate quantity of the
silico fluoride to be used (about one part by weight of the silico fluoride
to one of the sulphuric ashes of the saccharine matter) in order to
separate by precipitation the alkaline bases and at the same time more
or less of the organic matters. The silico fluoride may be employed
either in the state of a solid salt or in solution, and added to the juice at
any stage, but generally during or after the dissolution of the sugar in
refining or after (or instead of) defecation, or in lieu of the second car-
bonatation in the manufacture of raw sugar. The process may be carried
on without necessarily increasing the temperature usually employed in
these operations, as coagulation is unnecessary, owing to albumen, blood,
or fine bone black being dispensed with.
After the silico fluoride and the sugar or juice have been commingled
for about five minutes, the temperature may however be raised as usual
during a few moments, and at the same time I neutralize the juice by
means of an oxide, for instance, oxide of lead, of calcium of baryta, of
manganese, of aluminium, of magnesium, or others, either separately or
mixed, or by adding soluble sulphate, phosphate, carbonate, chromate,
or manganate of potassa, or lime. After this operation, if the juice
has become too alkaline, more particularly after the addition of the
oxides, I may introduce into the saccharine juce (especially when the
oxide of lead is used) bi-phosphate of lime, or carbonic acid gas, as.it
is now used in the manufacture of 'sugar in order to Deutralize the
excess of alkalinity. If too much sulphate, or other salt 'of" potassa
has been used, I may remove it by adding a little more of the silico
fluoride. It will therefore be readily understood that little or no incon-
venience results from using an excess of the silico fluoride or of the
neutralizing substances.
After.neutralization the juice may be decanted, if it is not too thick
(about 18° Beaumè), or.if the areometric degree is too high, (say 29° to

page_text: 31° Beaumé,) it is filtered, and after this decantation or filtration the
subsequent treatment of the sugar, molasses, or saccharine juices is con-
ducted in the usual manner.
--
The residuum on the filters or on the bottom of the vessel after decan-
tation is carefully pressed, and then washed or not, as the case may be, and
more or less dried; then mixed with more or less ammoniacal, water, or
other ammoniacal matter, and with any suitable sulphates, phosphates, or
carbonates, those of lime for example, for use as manure. This manure will
therefore consist for the most part of the organic and inorganic matters
contained in the sugar itself, or the juice treated, together with nearly
an exact proportion of the elements of the silico fluoride and the neutra-
lizing substances used. It will thus be seen that the composition of
this manure will vary in the same degree as the juice or sugar treated,
but its chief characteristic is that it always contains fluorides or
silico fluorides (the amount of which may readily be ascertained by
anlysis) so that it is therefore possible before completing the preparation
of the manure to add sulphuric acid, or the residuam may be merely
calcined and decomposed by steam in order to produce in either case
fluoride of silicium, and consequently hydrofluosilicic acid by means of
which a certain amount of the primitive silico fluoride may be regenerated
by adding a suitable base. The exact proportion of sulphuric acid, as
also of the hydrofluosilicic acid, and the base are calculated by the
equivalents after analysing the residuum.
2
3
The silico fluorides to be employed for the purification of sugar as
above described are generally prepared by dissolving to saturation a
carbonate of the metal to be used in hydrofluosilicic acid. The exact
proportion of acid and carbonate must be calculated by the equivalents,
but they are generally three equivalents of carbonate (the general
formula of silico fluorides being admitted as [Mƒl] ³ [Sift] * and
that of the acid 3 H F 1 [Sif 13] * [according to the annotation of
Berzelius]) to one equivalent of anhydrous acid contained in the
hydrated acid. 'In certain cases, as for the silico fluoride of aluminium
for instance, I may prepare it by dissolving (until saturation of the
hydrofluoric acid [3 H F 7] takes place) gelatinous alumina in hydro-
fluosilicic acid (one equivalent of anhydrous alumina, calculated in the
gelatinous state, is generally sufficient for one equivalent of hydro-.
fluosilicic acid, and the same for all the oxides of the same group as
that of alumina). If the silico fluoride obtained is used in solution the

page_text: areometric degree may be readily ascertained in order to calculate the
quantity of anhydrous salt contained in the said solution, which may
therefore be employed as conveniently as the salt in the solid state.
When it is desired to obtain solid silico fluorides the solution should
be slowly and carefully evaporated, otherwise the silico fluoride becomes
quickly decomposed. In practice I prefer a solution prepared imme-
diately before use, and in preparing said solution it is important not to.
exceed the degree of saturation, because if an excess of lime is added,
silica will be precipitated, and the silico fluoride already formed will be
decomposed.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Jean Marie Onésime Tamin in the Great Seal
Patent Office on the 26th March 1874.
I,
JEAN
TO ALL TO WHOM THESE PRESENTS SHALL COME,
MARIE ONÉSIME TAMIN, of the City, County, and State of New York,.
United States of America, and at present of Chancery Lane, in the
County of Middlesex, Doctor of Medicine, send greeting:
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-sixth day of September, in the year of
our Lord One thousand eight hundred and seventy-three, in the thirty-
seventh year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said Jean Marie Onésime Tamin, Her special
licence that I, the said Jean Marie Onésime Tamin, my executors, ad-
ministrators, and assigns, or such others as I, the said Jean Marie
Onésime Tamin, my executors, administrators, and assigns, should at any
time agree with, and no others, from time to time and at all times
thereafter during the term therein expressed, should and lawfully might
make, use, exercise, and vend, within the United Kingdom of Great
Britain and Ireland, the Channel Islands, and Isle of Man, an
Invention for "IMPROVEMENTS IN THE PURIFICATION OF SUGAR, MOLASSES, AND
SACCHARINE JUICES, AND IN THE REGENERATION OF PART OF THE SUBSTANCES
EMPLOYED, AND ALSO IN THE PREPARATION OF MANURE FROM THE RESIDUES
THEREOF," upon the condition (amongst others) that I, the said Jean
Marie Onésime Tamin, my executors or administrators, by an instru-
.
"

page_text: ment in writing under my, or their, or one of their hands and seals,
should particularly describe and ascertain the nature of the said In-
vention, and in what manner the same was to be performed, and
cause the same to be filed in the Great Seal Patent Office within six
calendar months next and immediately after the date of the said.Letters
Patent.
NOW KNOW YE, that I, the said Jean Marie Onésime Tamin, do
hereby declare the nature of my said Invention, and in what manner
the same is to be performed, to be particularly described and ascertained
in and by the following statement, that is to say :-
•
My Invention consists in the methodical use for the purification of
sugar or saccharine juices, of soluble silico fluorides, or hydro-
fluosilicates, or soluble double flourides of silicium, and almost all
the metals, more especially the hydrofluosilicates of ammonia, magnesia,
iron, lead, calcium, alumina, and manganese, but preferably those of
ammonia and alumina. I also employ the hydrated fluoride derived
from the hydrofluosilicates and belonging to the same chemical group
as alumina, as will be hereinafter described when treating of the
manufacture of said hydrofluosilicates. I may further employ fluosilicic
jellies, as will also be herein-after described. I may employ these
substances either separately or in combination with the object, "either
of varying (during the purification) their mode of action on the
impurities to be eliminated from the crystallizable sugar or· saccharine
juices, or of obtaining by such combination a product of average
quality and less cost.
The proportion of the simple or compound salt to be added to the
saccharine matters is dependent on the quality and on the quantity of
ash contained in said matter, and can only be exactly determined after
analysis of the ash and by calculation of the equivalents. It is however
sufficient in practice to add for a given weight of ash an equal weight
of the reagent, calculated in the anhydrous state.
The reagent may be employed either in the state of a solid salt or
in solution, and it may also be dissolved in the water used for washing
the filters and residues. ("petites eaux"), care being taken to increase
the dose of the reagent by an amount corresponding to the proportion
of ash contained in said water.
"
•

page_text: The action of the reagent is chiefly to clarify and separate the
greater part of the saline matters contained in the saccharine matters,
and at same time more or less of the foreign organic matters..
The reagent may be added at any stage of the ordinary manufacture,
but generally during or after the melting of raw sugars, or the
remelting of second, third, or fourth products in refineries or after
defecation or second carbonation (or even in lieu of these two latter
operations) in the manufacture of raw sugar.
By my Invention the use of blood, albumen, and fine bone black is
not indispensably necessary for clarifying.
1st. Supposing the reagent employed to consist of hydrofluosilicate
of alumina I proceed, for example, as follows:-After the hydro-
fluosilicate has been mixed in suitable proportion with the saccharine
juice the latter is neutralized by adding lime, baryta, lead, or ammonia,
or by the addition of another oxide, carbonate, or other salt of volatile
acid, united to a base such as magnesia, lime, or other base, whether
simple or compound. The temperature is then raised, as in the ordinary
process.
2ndly. If the reagent employed consists of metallic fluosilicates,:
contrary to the method above described,, and to the various methods
employed,. the neutralizing agent may be added before the reagent and
the alkaline juices be operated on.. To 100 parts of: ash, for example,
I add about 12. to 15 hundredths of base, and then mix the reagent
with the saccharine juices thus alkalized, raising the temperature until
ebullition takes place in order to coagulate the precipitates. The dose
is correct if juices of varying composition are found to be neutral
after being 'heated. If the contrary is the case the exact proportion of
base to be added may be quickly found by a few preliminary experi-
ments, or by calculating the equivalents after analysis of the salts of
the sugar. The object of this neutralization is to obviate the in-
conveniences to which the use of metallic fluosilicates, properly so
called, that of lead for example, might lead. As these fluosilicates
contain but one. equivalent of base, while two or three are required, in
order that a double decomposition may be completely effected in the
juice, equivalent for equivalent, it is therefore preferable to add to the
juice one or two equivalents of base (according to the composition of the

page_text: fluosilicate used) before the reagent to avoid displacing a base whose
acid would remain.free.
3rdly. When the juices are neutral the reagent alone may be added,
heating to about from 120 to 140 degrees Fahrenheit, and filtering
before adding the neutralizing substance, after which which a second
filtering is effected. This neutralizing body may also be added to each
of the subsequent products ("jets") in order to obtain by successive
precipitations a series of clarifications at but small cost. This method
will also facilitate filtration and the passage of the fine liquors when
clarifying sugar in the moulds. The first precipitate resulting from
the reagent alone would be composed of fluosilicates in an almost pure
condition.
The addition of the reagent, and the neutralization previous and
subsequent to such addition, may be effected at the ordinary temperature
at which sugar is melted in manufactories or refineries.
If the reagent
employed be the fluosilicate of ammonia, lime or its carbonate would
be added so long as ammonia is disengaged, for if the addition of the
reagent serves to precipitate the bases the addition of the lime or of
other insoluble bases, or of their carbonates, is intended to pre-
cipitate the acid and any excess of the reagent if the dose has not been
exact.
If an excess of base (lime for example) be added, a current of carbonic
acid may be introduced in the juice (as now practised in sugar manu-
factories) until it becomes neutralized. Or instead of carbonic acid the
acid or neuter phosphates of lime may be used for neutralizing the
excess of base. A phosphate of magnesia added with the same object
would also have the advantage of enriching the residues with a certain
proportion of ammoniaco-magnesian phosphates if the reagent employed
was fluosilicate of ammonia.
When the juice is more or less clarified it is decanted, that is,
supposing the areometric degree not to be too high (17 to 18 degrees
-Baumé), but if it marks 29 to 30° it is filtered as in ordinary, after
which the sugar molasses or saccharine juices are passed through the
ordinary operations. The residues of this decantation or filtration are
washed, pressed, and dried more or less, and may if desired be mixed
with ammoniacal liquor from any source, after which the mixture is more
or less solidified by the addition of sulphates, phosphates, or carbonates of

page_text: lime or potassa, and in this condition forms an excellent manure. 'The
residues of the several clarifications may also be utilized separately. as
well as the fluosilicates precipitated as above described (under the 3rd
head), but in this case without any mixture.
.It will be evident however that it is neither the addition of the
ammoniacal liquor nor even of the phosphates, sulphates, or carbonates
that constitutes the essential feature of the manure, whose composition
is as varied as that of the saline or foreign organic matters contained in
the different sacharine matters treated. Hence it is impossible to give
any fixed formula for the manure, but it may be stated that it contains,
as its: essential chemical feature, nearly the whole of the fluorine and
silica in the reagents employed in addition to the greater part of the
saline or, organic matters contained. in the saccharine matter treated, and
the greater or less richness of the ammoniacal. liquor and of the
phosphates, sulphates, or carbonates if thought desirable to employ
them.
⚫ Owing to the variable proportion of fluorine and silica contained in
the residues (which analysis only can exactly determine), said residues
may. before being finally converted into manure be. treated with sulphuric
acid or be heated to a red heat, and decomposed by steam with a
view to produce fluoride of silicium and hydrofluosilicic acid, and
consequently by dissolving either a carbonate or an oxide in the latter
acid to recover or regenerate a certain proportion of the reagent
originally employed in the purification. The exact proportion of
sulphuric acid to be added is calculated by the equivalents after analysis
of the residues, but in practice the same amount by weight of sulphuric
acid as of the reagent used for purifying is sufficiently exact.
"
When. fluosilicate of ammonia is employed the fluosilicates separated
by the first filtration as described under the 3rd head may be mixed
with a salt of ammonia, and the mixture sublimated in order to directly
regenerate more or less of the hydrofluosilicate of ammonia originally
employed. The proportions of the mixture are as in all cases calculated
by the equivalents after analysis of the residues of the purification of
the saccharine matters. The residue of this sublimation, with sal
ammoniac for example, furnishes a manure containing chlorides instead &
of fluorine and silica. The manure will thus be found richer in
sulphates than fluorine if the regeneration of the hydrofluosilicic acid is
.I

page_text: obtained by the addition of sulphuric acid, and richer in fluorine than
in sulphates if heat and steam alone are employed; or it will contain a
maximum of fluorine and silicium if there be no regeneration effected.
The manure will have a maximum amount of richness if phosphate
of magnesia is employed to saturate the excess of base, thus preserving
more or less of the ammonia of the reagent. This manure restores to
the soil on which are grown sugar-producing plants (cane, beet, &c.) a
large portion of the mineral matters which are necessary to prevent its.
rapid exhaustion.
The method of preparing the reagents in question forms no part of
this Invention, which applies only to their application, but it would
however be perhaps useful to give more complete details on a subject
which has not been sufficiently developed in published works.
For alkaline earthy oxides, the relation between the metal and the
oxygen of which is ::1:1, three equivalents of oxide are necessary to
saturate one equivalent of hydrofluosilicic acid, and at same time that
this reaction is effected one equivalent of metallic fluoride is precipitated
from the solution. The same applies to calcium and all the metals of
this series.
For metals properly so called, such as lead for example, two equiva-
lents of insoluble fluoride precipitate on the three equivalents of base
employed. These several precipitates of insoluble fluorides and a small
portion of the silica are recovered, and may if mixed with the residues
of the purification serve to increase the quantity of hydrofluosilicic acid
reproduced as previously explained. In every case where a carbonate
may be dissolved in hydrofluosilicic acid the reaction is effected at the
ordinary temperature. If more than three equivalents of base or of
carbonate be added the hydrofluosilicate formed is decomposed, and a
proportion of silica equivalent to the excess of base added is precipitated
as well as an insoluble fluoride.
In order to prepare hydrofluosilicate of ammonia either ammonia or
its carbonate is mixed with the hydrofluosilicic acid, the proportions
being determined by a calculation of equivalents.
For oxides whose relation between the metal and the oxygen is :: 2 : 3;
one equivalent added to three of the acid constitutes an acid salt, two
equivalents a neutral salt, and three equivalents a hydrated fluoride,

page_text: When however an excess of base is added, instead of precipitating
fluorides as in the case of alkaline oxides, silica alone is precipitated in
proportion equivalent to the excess of oxide added exceeding one
equivalent, and instead of being precipitated the fluoride remains
dissolved. The same is the case with aluminium and all the tetratomic
oxides. The silica is recovered and mixed with the residues of the
purification, the same as in the case of the precipitated fluorides. This
second class of reagents is prepared by dissolving either at the ordinary
temperature or at from 80° to 100° Fahrenheit, a gelatinous oxide of
alumina, for example in hydrofluosilicic acid, the oxide being calculated
in the anhydrous state. This gelatinous oxide is prepared by precipi-
tating alum or the sulphate or other salt of alumina with the aid of
ammonia or carbonate of ammonia, and then washing the gelatinous
precipitate.
It will be seen from what has been stated concerning the manufacture
of the hydrofluosilicates that they may be obtained such that their
solution presents a more or less neutral or even alkaline reaction,
according to the quantity of base in excess added to the solution of acid
salt, and proportionately to this excess of base, chiefly ammonia. The
ordinary hydrofluosilicates have all an acid reaction. Whatever may
be the reagent employed the rule is invariable that the exact proportion
to be added to the saccharine matters is always equivalent to the ash
contained in said matters, and the weight of salt should always be
calculated in the anhydrous state whatever may be the water of crystalli-
zation of the solid salt or the water of its solution. In practice however
one part by weight of the salt will be sufficient for one of ash as before.
In order to ensure greater accuracy in the dosing the ash of the water
used for washing the filters and residues and the ash of the sugar may
both be analysed, the mean equivalent taken, and an equivalent propor-
tion of the reagent in a dry state dissolved in the said water, which is
then put in the dissolving pan instead of blood.
When employing reagents with a base of alumina the neutralization
of the juices may be dispensed with, especially when before the addition
they are neutral or even slightly alkaline, and do not require to be. again
passed through the bone black filters. It is however preferable to
'operate on the juices when in a neutral or even slightly alkaline
condition. The other purifying operations are the same as when the
juices are neutralized. By the employment of an alkaline reagent the

page_text: subsequent neutralization of the juices may be sometimes dispensed
with.
This Invention also includes the use of hydrated fluorides and
fluosilicic jellies, inasmuch as said substances are derivable only from
fluosilicates.
Whether a volatile base, such as ammonia, or whether an alkaline
earthy oxide, or an earthy or a metallic oxide be added, these jellies will
be more or less thick, neutral, or alkaline, according to the amount of
silica precipitated. The exact composition is determined by the equiva-
lent between the excess of base, the silica precipitated, and the equivalent
of the hydrcfluosilicate, which is thus more or less decomposed. These
jellies may even present a very free alkaline reaction, that of ammonia
or lime for example.
These auxiliary reagents, hydrated fluorides, and fluosilicic jellies are
employed similarly to and in the same proportions as the hydrofluosili-
cates, and are calculated by the equivalents after a complete analysis of
the saccharine matters to be purified, one part of the reagent in a dry
state to one of ash being the proportion usually adopted.
Assuming that it is the molecular condition and the quantity of
mineral and organic matters contained which retards the crystallization
of sugar, I have found after many experiments that the method which
best effects the desired purification is to employ hydrofluosilicate of
ammonia with the view of substituting salts with a volatile base for
nearly the whole of the salts with fixed bases of the sugar, afterwards
employing insoluble carbonates (the proportioning of which is in some
sort self-regulating) which permits the major part of the acids to be in
turn precipitated by disengaging the volatile base, whilst the volatile
acid is disengaged also. Viewed economically the employment of the
residues for regenerating the reagent by sublimation constitutes a very
important advantage.
Instead of employing the residues of the sublimation as manure they
may be used to regenerate the sal ammoniac. The ammoniacal liquor
from gas works is filtered through plaster (sulphate of lime or gypsum)
and forms sulphate of ammonia, which on being treated by the chlorides
resulting from the sublimation (consisting for the most part of chloride
of potassium) reproduces sulphate of potassa and hydrochlorate of
i

page_text: ammonia. These two salts are separated by taking advantage of the
difference of time required for their sublimation or crystallization. In
this manner sal ammoniac is obtained.
The sulphate of ammonia may also be used to regenerate the fluosili-
cate of ammonia by mixing it with the residues, but the sublimation is
much slower.
In order to compensate for the waste which is inevitable at each
regeneration of the reagent hydrofluosilicic acid is saturated by the
residues of the sublimation, and insoluble fluosilicates of potassa and
soda are formed, the hydrochloric acid remaining in the solution. The
solution is then saturated with ammonia and concentrated, and the
sal ammoniac crystallizes.
The above constitutes a series of economical regenerating operations,
which may be almost as conveniently effected as is the revivification of
bone black.
•
The mixing of the fluosilicate of potassa and sal ammoniac should
be very carefully calculated and effected, the fluosilicate of potassa and
soda being slightly in excess, for example, about one part by weight of
fluosilicate to of sal ammoniac.
The sublimation may be effected in the furnaces ordinarily employed
for this purpose, while the sublimated substance may be purified by
crystallizing it in water, and then sublimating a second time. After
having thus examined in detail all that relates to the use of hydro-
fluosilicates or of their direct derivatives I will proceed to describe the
method to which I give the preference.
In addition to the special application of the reagent my process is based
on the law of " malaguti,'
""that when two molecular systems act the
one on the other their elements ever tend to compose new systems of
more stable equilibrium;" and this law has led me to deduce the
following:- "That in presence of water, more especially when in
ebullition, the insoluble carbonates decompose the soluble, and even the
insoluble salts in suspension in a liquid, and form with the base of car-
bonate insoluble salts, while the carbonic acid is disengaged."
Supposing the reagent einployed for purifying sugars to be the fluosili-
cate of ammonia, I proceed as follows:-Observing the general
directions given in this Specification as well as those relating to. the

page_text: proportions, I mix the reagent with the juices, in lieu of blood, and fine
bone black, and as they then become slightly acid I simply. add the
proportion of base (lime, ammonia, or other), necessary to give a very
slight alkalinity to the said juices. Then without raising the tem-
perature the precipitate, consisting chiefly of insoluble fluosilicates, may
be separated, but ebullition facilitates both the coagulation of the .
precipitate and a prompt filtration. I may also neutralize or alkalize
the juices before adding the reagent, so as to render them either neutral
or slightly alkaline. The ordinary crystallizing operations are then
proceeded with as regards this first product, and if the syrups resulting,
from this or the following products should become slightly acid there is
added it may be even an excess of insoluble carbonate, for example, of
lime, baryta, lead, or bismuth. This subsequent addition of a carbonate
produces a fresh clarification and precipitation. The presence of an
excess of carbonate will be shown when all effervescence or disengage-
ment of gas ceases after boiling; generally from two to three parts of
carbonate are added for one of the reagent. If the insoluble carbonates
were added before separating the first precipitates there would be a risk
of re-decomposing a great part of the insoluble fluosilicates already
formed, but remaining in suspension in the juices for the action of, the
insoluble carbonate (which is added to the juices so long as there is any
effervescence or gaseous disengagement, or even any considerable
shrivelling when in ebullition, usually in the proportion of three parts of
carbonate to one of the reagent), is precisely to precipitate and
decompose the excess of reagent the soluble fluorides, and consequently
more or less of the insoluble fluosilicates in suspension.
"
The carbonate may be added to the juices either in a dry state or in
the form of a milk in small quantities at a time to avoid too great an
effervescence, but little or no carbonate of ammonia being formed.
Supposing carbonate of ammonia to be formed, the ordinary addition of
lime to the washing water (petites eaux) in the turbines and apparatus
for boiling down the residues and low products would be sufficient to
decompose the said carbonate and expel the ammonia, which condenses
in the apparatus, and serves to keep the same clean, or fit remains in the
low products and residues and prevents their fermentation. It is
however preferable to effect a complete clarification of the third or fourth
products (jets) by adding from 15 to 20 hundredths of lime to one of the
original ash dosed. The ammonia in the juices remains free and entirely
disappears after the several products have been boiled.

page_text: The third principle on which my process is based is that only the
quantity of carbonate is decomposed which is necessary :-1st, for
neutralizing the juices; 2ndly, for decomposing and precipitating a
possible excess of reagent or the soluble fluorides which might be
formed; and 3rdly, for saturating the acids of the volatile bases which
the juices contain, the excess of carbonate remaining inert at the
bottom of the apparatus. All these reactions may be readily followed
with the assistance of a glass tube placed in communication with the
mass of juice such as used with the ordinary vacuum pan. The supply
of milk of carbonate or of lime may be thus regulated by a continuous
examination of the reaction until the clarification becomes suddenly
evident. In this manner the introduction into the juices of only that
proportion of base which is strictly necessary is ensured, this being with
difficulty avoided when lime or other bases are employed. The employ-
ment of carbonates with poisonous bases such as those of baryta or
lead is thus rendered possible without incurring danger, the more so as
the presence of the free ammonia in the juices ensures the entire
precipitation of such bases or of their carbonates, or their various salts
formed with the acids of the juices. The whole of these salts pass into
the residues.
I would remark that the carbonate of lead will precipitate the whole
of the chloride of lead contained in a solution, and as under the influence
of the carbonate of lead all the soluble chlorides become chloride of
lead, the chlorides of the juices will thus be almost entirely eliminated
at same time that the metal of the soluble chloride, sodium for example,
will become a base capable of forming with carbonate of lead a
precipitate of double carbonate of lead and soda in this example..
The general advantages of salts of lead are in this manner utilized for
the decolorization and the separation of the organic and inorganic
matters contained in sugar.
"The foregoing method applies whether one or other fluosilicate be
employed for precipitating the bases and one or other carbonate for
effecting the purification.
Instead of a fluosilicate with a volatile hase other fluosilicates may
be employed, as for instance those of magnesia or alumina. The mode
of operation remains the same, but less carbonic acid is disengaged, it
forming insoluble carbonates by the double decomposition of, the
.

page_text: carbonate of magnesia for example, which during the ebullition rises in
the form of scum, and so favors the purification.
With regard to the salt of alumina which was precipitated when
neutralizing the first product the subsequent addition of insolubie
carbonate has the effect especially of precipitating the soluble fluorides
and the excess of reagent, while the carbonic acid is disengaged by
removing from the juice the excess of lime which may have remained in
it after the first neutralization. It also permits of purifying or treating
sugars or saccharine juices in a constantly alkaline medium without the
liability of forming definite combinations of the bases with the sugar,
which would lead to a considerable loss of crystallizable sugar. It
further prevents through the alkalinity of the operation all fermentation
in sugar manufactories or refineries.
Instead of adding the neutralizing substance after the reagent I may,
as before mentioned, neutralize or even alkalize the solutions of the re-
agent before using the same.
Finally, I would recommend the employment of hydrofluosilicate of
of ammonia and carbonate of lime, or in order to obtain a more perfect
purification the employment of the said reagent, followed by that of
carbonate of lead or of baryta.
The use of hydrofluosilicate of ammonia permits of the direct regene-
ration of the reagent with the aid of the precipitate from the first
product. The first precipitate will thus be composed principally of
fluosilicates of potassa and soda, in addition to aluminates, if the re-
agent employed were alumina. The second precipitate will be composed
of insoluble fluorides of silica or of silicates, and of the excess of
insoluble carbonate added, and of the several insoluble salts formed by
the double decomposition of the soluble salts remaining in the juices
and of the insoluble carbonate added. The third precipitate if obtained
As all these precipitates
will contain but insoluble carbonates only.
contain more or less organic matters separated therewith they should be
carefully pressed and washed.
Having described the nature of the Invention and the manner of
performing the same, I declare that what I claim as the Invention to be
5 protected by the herein-before in part recited Letters Patent is,―
1st. The process of purifying sugars, molasses, aud saccharine juices
by the methodical employment, as herein specified, of soluble siliço-

page_text: fluorides, or hydrofluosilicates, or of the hydrated fluorides or fluosilicic
jellies derived therefrom, substantially in the manner described.
2nd. The utilization of the residues of this purification as manure, as
set forth.
3rd.. The regeneration of the hydrofluosilicates by means of the
residues, as herein described.
4th. The utilization of the residues of this regeneration as manure, as
described.
5th. The purification of sugars and saccharine juices generally without
the necessity of neutralizing the same, as herein described.
6th. The employment of fluosilicates in solution whether nentralized
or alkalized, as specified.
In witness whereof, I, the said Jean Marie Onésimé Tamin, have
hereunto set my hand and seal, this Twenty-fifth day of March,
in the year of our Lord One thousand eight hundred and seventy-
four.
J. M. O. TAMIN. (L.S.)