AN IMPROVED PROCESS OF PHRIRVING AND CLADIEVING Sicomadiun INTORS AND Senzas OF PURIFYING AND CLARIFYING SACCHARINE JUICES AND SYRUPS
Year: 1871

page_text: LETTERS PATENT to Jean Vincent Prosper Lagrange, of Rue de la
Banque, No. 19, Paris, Chemist, for the Invention of "AN IMPROVED
PROCESS OF PHRIRVING AND CLADIEVING Sicomadiun INTORS AND Senzas 11
Sealed the 26th January 1872, and dated the 23rd November 1871.
PROVISIONAL SPECIFICATION left by the said Jean Vincent Prosper
Lagrange at the Office of the Commissioners of Patents, with
his Petition, on the 23rd November 1871.
I, JEAN VINCENT PROSPER LAGRANGE, of Rue de la Banque, No. 19,
Paris, Chemist, do hereby declare the nature of the said Invention for
"AN IMPROVED PROCESS OF PURIFYING AND CLARIFYING SACCHARINE JUICES AND
SYRUPS," to be as follows:-
:—
The organic matters which are found in abundance in juice and
syrups, and which are very injurious to the manufacture and refining of
sugar, are very imperfectly eliminated by the processes at present
employed.

page_text: niacal salts to lime juices, and of ammonia alone to non-limed juice
intended to be run through conduits, prevents deposits in these conduits,
avoids alterations, and during the whole of the work described up to the
end the juice and syrup preserve a perfect alkalinity.
Second. The Refining.-The object of the process is by the employment
of ammoniacal salts and phosphate of ammonia to purify the juice and
syrup by eliminating organic matters and the salts of lime from them,
and to dispense with the animal black and blood ordinarily used for the
purpose of clarification. In order to clarify the process consists in intro-
ducing into. the boiler at about 70 degrees Centigrade from one to two
thousandth parts of slaked lime. After the lime is dissolved I introduce
a proportional quantity of phosphate of ammonia, and I carry the liquid
to the boiling point. The lime and the organic matters are thus pre-
cipitated at the same time that the clarification is effected. I proceed
then to the filtration of the clarified juice; I can dispense with the lime,
and clarify by the introduction of phosphate of ammonia alone. In the
purification of juices, as the lime can be found combined with the
sugar, I prefer to use the phosphate of ammonia alone, without the
previous addition of lime.
Thirdly. I employ ammoniacal water after hydration of the lime in
milks of lime at all densities. I also employ ammoniacal water for the
cleansing of the filters containing animal black in grains, used in the
processes above described. The ammonia prevents acidity, and renders
the formation of pectates and lactates of lime and other organic matters
in the saccharine juices and syrups impossible; I make in short an
advantageous employment of ammoniacal water in doses varying
according to the nature of the juice in all temperatures, and in all the
different stages of the manufacture and refining of sugar, such as during
the rasping of the beetroot at the discharge of the presses of cane mills
used in the colonies, during, before, or after the evaporation, the concen-
tration, and the heating down of saccharine juices and syrups, and lastly
for the cleansing of filters and in milks of lime.
The treatment above described with phosphate of ammonia is appli-
cable to all the series of syrups, and permits them to be conducted by
underground conduits or otherwise, without any alteration. The sulphites.
and byposulphites of ammonia and the bydro-fluosilicate of ammonia
fulfil the same conditions and purposes as the phosphate of ammonia,
and in addition thereto possess greater colouring properties.

page_text: The principal advantages derived from my new process are:-
Augmentation of quantity, and superior richness of product, dispensa-
tion with animal black and blood in the heating, and economy and
rapidity in manufacture.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Jean Vincent Prosper Lagrange in the Great Seal
Patent Office on the 23rd May 1872.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JEAN
VINCENT PROSPER LAGRANGE, of Rue de la Banque, No. 19, Paris,
Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-third day of November, in the
year of our Lord One thousand eight hundred and seventy-one, in the
thirty-fifth year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said Jean Vincent Prosper Lagrange, Her
special licence that I, the said Jean Vincent Prosper Lagrange, my
executors, administrators, and assigns, or such others as I, the said
Jean Vincent Prosper Lagrange, 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 "AN IMPROVED PROCESS OF PURIFYING
AND CLARIFYING SACCHARINE JUICES AND SYRUPS," upon the condition
(amongst others) that I, the said Jean Vincent Prosper Lagrange,
my executors or administrators, by an instrument in writing under
my, or their, or one of their hands and seals, should particularly
describe and ascertain the nature of the said Invention, 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 Vincent Prosper Lagrange, do
hereby declare the nature of my said Invention, and in what manner

page_text: the same is to be performed, to be particularly described and ascertained
in and by the following statement thereof, that is to say :—
The organic matters which are found in abundance in juices and
syrups, and which are very injurious to the manufacture and refining of
sugar, are very imperfectly eliminated by the processes at present
employed.
The object of my Invention is a process for purifying and clarifying
saccharine juices and syrups and other fluid or semi-fluid saccharine
matters of whatever origin by means of ammonia and ammoniacal salts,
such as the phosphates, sulphites, and hyposulphites of ammonia, and
the hydro-fluorosilicate of ammonia.
The chief novelty of my process consists on the one hand in the
property possessed by ammonia of precipitating organic matters, and on
the other hand in the property of phosphate of ammonia of precipitating
salts of lime indecomposable by carbonic acid.
Saccharine juices and syrups treated by ammonia (the volatilized
portion of which is revivified) remain without alteration under the most
varying temperatures throughout all the course of the manufacture and
refining.
I proceed to describe my process in detail :-
1st. The Manufacture.—In treating the beetroot or other saccharine
plant I cause ammoniacal water, preferably heated, to flow over the
rasping or breaking machine. To the juices proceeding from the presses
or mills ammonia may likewise be added. After tempering with lime,
preferably under heat, I introduce into the juice a quantity of phosphate
of ammonia in proportion to the amount of lime combined either with
the sugar or with the organic substances to be eliminated; thus, for
example, 84 parts of real lime correspond to 135 parts of phosphate of
ammonia. I obtain immediately a double precipitate, composed on the
one hand of phosphate of lime, and on the other of organic matters
which the ammonia set at liberty completely precipitates. The liquor
is then cleared by decantation or by filtration under pressure, and the
work terminated by the ordinary concentrating evaporation.
I have mentioned in the above example the work by calcic tempering,
and by dispensing with the carbonic acid gas while preserving as an
economical means the usual processes of carbonation, I obtain an equal

page_text: purification with a complete elimination of the salts of lime by adding
phosphate of ammonia after the saturation or carbonation. I can equally
well cause the phosphate of ammonia to act before, during, or after these
different operations.
The operation before the calcic treatment is as follows:-The juice
proceeding from the presses alkalized with ammonia is treated in a
deficating boiler or vessel with a solution of phosphate of ammonia at
10° Beaumé (for instance, 6 decilitres per hectolitre of juice at 5°
Beaumé) ebullition is produced, then about one kilogramme of hydrated
lime is added to each hectolitre (proportions which vary according to the
quality of the juice), and the liquid is well stirred, when a deposit of
insoluble phosphate of lime is formed, and ammonia given off which
precipitates the organic matters. The liquor is then cleared, or the
mixture passed through filters under pressure, when the juice will be
found to be limpid, well deficated, and free from salts of lime. After
filtration the juice is sent, without passing over animal charcoal, to the
concentrating apparatus, and thus perfect defication and saturation are
obtained by the same means.
The process, however, which I prefer is the following :-To employ the
ammonia at the breaking machine under heat, to add likewise ammonia
to the juices proceeding from the presses or mills in order to saturate
the organic acids which are developed during the breaking and pressing
operation. To heat the juice saturated with ammonia to a temperature
of from 70° to 75° Centigrade, to then add the lime necessary for the
tempering, which is done under heat in order the better to eliminate the
organic matters, to carry the temperature up to the first ebullition, to
clear the juice and send it to the saturating boilers. The juice having
become clear, a fresh quantity of lime is added before the saturation,
and the mixture is brought to the boiling point, and this I call the calcic
ebullition; it destroys not only the glucose pre-existing in the juice, but
it also decomposes by transformation into ammonia the principal azotes,
which are active sources of the fermentation and transformation of sugar.
After the calcic boiling the temperature is maintained at about 90°
Centigrade, and I cause carbonic acid gas to arrive. This saturation,
which I call the hydratod saturation, at high temperature causes the
formation of hydrated carbonate of lime, which is rapidly and abundantly
precipitated in the form of flakes, and completely purifies the juices.
The juice thus saturated is treated with a small quantity of phosphate

page_text: tion, the concentration, and the heating down of saccharine juices and
syrups, and lastly during the cleaning of filters and in milks of lime.
The treatment above described is applicable to all the series of syrups,
and permits them to be run through underground conduits or pipes or
otherwise without any alteration in their constitution. The sulphites
and hyposulphites of ammonia and the hydro-fluosilicate of ammonia
fulfil the same conditions and purposes as the phosphate of ammonia,
and in addition thereto possess greater discolouring properties.
The principal advantages derived from this my new process in which
the reagent has the essentially alkaline property are, preservation of
juices and syrups, augmentation of quantity and superior richness of
product, dispensation with animal black and blood in the treatment,
and economy and rapidity of manufacture.
And having now described the nature of my said Invention, and in
what manner the same is to be performed, I declare that I claim, the
process of purifying and clarifying saccharine juices and syrups and other
fluid or semi-fluid saccharine matters of whatever origin, characterized,—―
1st. By the employment of ammoniacal water and the salts of
ammonia.
2ndly. By calcic ebullition.
And, 3rdly. By the hydrated saturation at a high température, sub-
stantially as herein-before explained.
In witness whereof, I, the said Jean Vincent Prosper Lagrange,
have hereunto set my hand and seal, this Eighth day of May
One thousand eight hundred and seventy-two.
Witness,
CH. ARMENGAUD,
Civil Engineer,
Boulevard de Strasbourg, 23,
Paris.
J. V. P. LAGRANGE. (L.s.)