CERTAIN IMPROVEMENTS IN TREATING FATTY AND OILY MATTERS
Year: 1860

page_text: LETTERS PATENT to Jules Léonard Louis Cambacérès, of Paris, in the
French Empire, Chief Engineer of Bridges and Roads, for the Invention
of "CERTAIN IMPROVEMENTS IN TREATING FATTY AND OILY MATTERS."
PROVISIONAL SPECIFICATION left by the said Jules Léonard Louis
Cambacérès at the Office of the Commissioners of Patents, with his
Petition, on the 25th July 1860.
I, JULES LÉONARD LOUIS CAMBACÉRÈS, of Paris, in the French Empire,
Chief Engineer of Bridges and Roads, do hereby declare the nature of the
said Invention for "CERTAIN IMPROVEMENTS IN TREATING FATTY AND OILY
MATTERS," to be as follows:-
Attempts have heretofore been made to employ nitrous and nitric acid
advantageously for solidifying the liquid portion of fatty matters in order to
render them suitable for the manufacture of candles. This solidification is in
a great measure resisted by a too energetic reaction of these concentrated
acids, especially when aided by heat. Now, by acidulating water with nitric
acid, and subjecting the fatty and oily matters to the action of the same for
several hours, I produce the necessary solidification. Nitric acid diluted in
water has been before employed, but a metal, such as finely powdered zinc, has
been added to produce the nitrous acid; while according to my process, the

page_text: single action of nitric acid, diluted with water, suffices for neutral bodies. It
is the same for oleic acid, but the action then only takes place when this fatty
acid retains a small portion of iron produced by its contact with the press
plates used to extract saponified matters. This iron, however, being in such
a small quantity is not free, but is combined with the fatty matters. If it
were free the action would be too energetic, and the inconvenience would
arise which has hitherto rendered it necessary to abandon every process in
which nitric acid diluted with water, in combination with powdered metal, has
been employed in order to produce nitrous acid. It is sometimes necessary to
place the oleic acid produced by pressure in contact with iron a second time
to increase the quantity of the metal with which it is combined. Also for
fatty saponified matters which have not been submitted to pressure, it is indis-
pensible to effect this contact with powdered iron, for example, before sub-
mitting it to the action of water acidulated with nitric acid. The acid need
not be pure, it can be mixed with other acids, or with salts, such as nitrates,
nitrites, and other combinations, but it is absolutely necessary that it be
diluted with a considerable quantity of water, without the addition of any metal
in a free form in the acid solution. The fatty matters thus solidified are
treated with sulphuric acid and distilled. The solidified oleic acid is distilled
to deprive it of its colour.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Jules Léonard Louis Cambacérès in the Great Seal
Patent Office on the 25th January 1861.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JULES
LEONARD LOUIS CAMBACERES, of Paris, in the French Empire, Chief Engineer
of Bridges and Roads, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-fifth day of July, in the year of our Lord
One thousand eight hundred and sixty, in the twenty-fourth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said Jules Leonard Louis Cambacérès, Her special licence that I, the
said Jules Leonard Louis Cambacérès, my executors, administrators, and
assigns, or such others as I, the said Jules Leonard Louis Cambacérès,
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

page_text: vend, within the United Kingdom of Great Britain and Ireland, the Channel
Islands, and Isle of Man, an Invention for "CERTAIN IMPROVEMENTS IN
TREATING FATTY AND OILY MATTERS," upon the condition (amongst others) that
1, the said Jules Leonard Louis Cambacérès, 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 Inven-
tion, 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 Jules Leonard Louis Cambacérès,
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 thereof, that is to say :-
Attempts have heretofore been made to employ nitrous and nitric acid for
solidifying the liquid portion of fatty matters in order to render them suitable
for the manufacture of candles. The solidification has in a great measure been
resisted by a too energetic action of these acids, especially when aided by heat
to liquify the fatty matter. Now instead of employing a weak dose of concen-
trated nitric acid I acidulate water with nitric acid, and subject the fatty and
oily matters to the action of the same for several hours, and so produce the
necessary solidification. Nitric acid well diluted in water has been before
employed but not alone; a metal, such as finely powdered zinc, has been added
to produce the nitrous acid, while according to my process the single action of
nitric acid, diluted with water, produces the necessary solidification. The
quantity of water acidulated with this nitric acid is about half by weight of
the fatty matters under operation. For tallow the liquid marks about five
degrees Beaumé. For palm oil, three degrees.
The other fatty and oily substances which nitrous acid solidifies are also
solidified by this water. The quantity of nitric acid varies according to the
material. The operation is carried on at nearly boiling point. Tallow requires
from two to three hours; palm oil, from an hour and half to two hours. If
the operation is continued beyond this point opposite results are obtained. The
point of fusion of these two substances is augmented at least ten degrees by
this treatment. The nitric acid need not be pure; it may be impregnated in a
slight degree with other acids. Water acidulated with nitric acid may in some
cases be replaced by water acidulated with sulphuric acid and a soluble nitrate.
If an ammoniacal salt is added to the liquid acid in a large quantity the
hardened tallow does not take a sufficient tint to prevent candles being made
directly from it; the tint disappears in sunlight, an effect which does not

page_text: take place when the nitric water is free from all kinds of salts. The solidifi-
cation is effected in a stoneware pan, or in a vat made of oak, heated by steam
through a stoneware coil. The mixing is effected by a wooden stirrer, or by
forcing air in a finely divided stream into the liquid mass. As soon as the
operation is finished the mass is allowed to rest, when the fatty body separated
from the liquid acid is withdrawn. It is washed in pure water, if necessary,
before submitting it to the action of sulphuric acid and to distillation. If con-
centrated sulphuric acid is employed, it is necessary to submit the fatty matter
for some hours to a temperature of from 302° to 309° Fahr., to deprive it of
water, and of the water absorbed by the coloring matter, which always formis
an action secondary to that of the nitric acid, and distinct from that which
produces solidification. But, if with a view to avoid the great loss of fatty
matter resulting from the action of the concentrated sulphuric acid, and a
certain quantity of water is added, it will not be necessary to expose the fatty
matter to a high temperature previous to solidification. The time for the last
acidification will only be longer, and it will be regulated in such manner as to
compensate for the loss produced by the concentrated sulphuric acid with the
increased expense occasioned by the operation required when the acid is more
or less diluted with water. This generally marks about from 86° to 104° Fahr.
This acid does not become incorporated with the fatty matter as the con-
centrated acid does, and it can be used for another acidification. After the
saponified fatty matters have been washed in boiling water, they are submitted
to an operation differing somewhat from ordinary desiccation usually followed
before distillation. For this purpose the matter is placed in a boiler under a
chimney, and provided with a stirrer. In this boiler there is a leaden coil, and
by means of which the temperature is raised to from 302° to 356° Fahr. At
this high temperature the free water is evaporated, and the water combined
with the coloring matter is driven off from it. The operation generally lasts
from ten to twelve hours, destroys in a great measure the coloring matter, and
it is followed chiefly with a view to obtain by distillation more crystallised and
whiter acids. It is an operation altogether distinct from ordinary desiccation,
and which has not been hitherto adopted. Its duration depends upon the
nature of the fatty body acidified. At the end of the operation last described,
distillation takes place in the ordinary manner. The distilled matter shews
different degrees of fusion, but the lowest for hard tallow is from 115° to
118° Fahr., and this is more than sufficient to make a candle which will not
run or gutter. Thus all the labor of pressing and of dividing the products
according to the different degrees of fusion in order to make candles of dif
ferent qualities is dispensed with. But in order without resorting to pressure

page_text: to make a white candle having only a slight green tint, which disappears in
sunlight, it is necessary to submit the distilled material to a purification and
clarification by a new process.
That which I now follow consists in treating the fatty body with sulphuric
acid diluted to mark 8° Beaumé, in washing it in boiling water to remove all
trace of the acid; then in pure water, and afterwards in clarifying it with
white of egg. The small quantity of oleic acid which the fatty acids always
retain, even when they are submitted to a strong pressure, colors in a very
sensible manner by this treatment. This effect is increased when the oleic
acid is obtained by distillation after sulphuric saponification. It is owing to
the action of the wash waters assisted by heat.
To avoid this defect, by moderating the heat, I make use of a water
acidulated by any acid, but chiefly by hydrochloric acid, in which a mineral or
vegetable salt is dissolved in such manner as to obtain a solution sufficiently
concentrated to prevent the yellow tint produced by pure hot acidulated or
albuminized water. The mixture is well stirred, and the fatty liquid is
allowed to settle, and is washed as required in saline water. With the same
purpose and for the same reason, I add a mineral or vegetable salt to the
albuminized water before using it. This albuminized water alone is used, if
the substance is free of all oxide, adding to it a little oxalic acid; ammoniacal
salts, and especially the sulphate of ammonia are by preference used, in order
that if the coloring element retains any trace of the saline substance, this sub-
stance shall not injuriously affect combustion, but on the contrary favour it by
the decomposition of the sulphate on the wicks of the candles.
Oleic acid of commerce is also solidified under my process by means of
water acidulated with nitric acid; but then the action although the same in
appearance, differs in so far that it can only be produced so long as the oleic
acid retains, as is generally the case, a small quantity of iron, arising from its
contact with the plates of the press used to extract it from saponified fatty
matters. This iron is not free; if it was not combined with the fatty matter,
or the organic matter which colors the fatty matter, and if it was mixed at the
time of the operation with nitric acid, the action would be too energetic; the
solid acid formed, which is no other than elaidic (elaidique) acid, would be
partly destroyed, the more so under heat, and the inconvenience would arise
which has led to the abandonment of every process in which powdered metal
with nitric acid in order to produce nitrous acid has been employed. Some-
times the plates of the press are tinned or galvanised. Oleic acid placed in
contact with tin or zinc does not solidify as well as if in contact with iron, but
the principle is the same. Prolonged contact of oleic acid with a metal

page_text: attackable by nitric acid, is sufficient to cause this mode of combination to
produce solidification, when the oleic acid is afterwards submitted to the action
of water acidulated with nitric acid. Solidification takes place in the manner
before described for neutral bodies. It is only necessary to heat to a lower
temperature to that of a water bath at the most, and to prolong the action to
at least four hours, replacing water as it becomes evaporated. I have some-
times found it necessary in order to arrive at complete solidification, to put
oleic acid, extracted by pressure, again in contact with a metal, and by pre-
ference with iron, to increase the quantity of the metal combined. So also it
is often necessary to add a fresh supply of nitric acid.
Oleic acid solidified in manner before explained is washed, if required, and
is submitted to the action of heat at a high temperature for several hours, as
before described with reference to the fatty bodies treated by sulphuric saponi-
fication. It is afterwards distilled in the ordinary manner to obtain elaidic
(elaidique) acid. If it is required to be obtained in such a state of purity as
to shew the crystallization of the elaidic (elaidique) acid, that solidification
must be adopted which takes place by treating the oleic acid of commerce with
nitric water, without any fresh contact with iron, and the matter must be
pressed before distillation. The acid resulting from this pressure, and which
has not been distilled, is afterwards treated with the acidulated water, the
pressure having brought it again in contact with the iron; it is solidified in
the same manner. I submit to an analogous treatment fatty bodies saponified
either by lime or by sulphuric acid, but which have not been previously
hardened by water acidulated with nitric acid. If it is not desired to extract
by pressure the oleic acid which forms part of them, and if it is desired to
solidify this acid, leaving it mixed with the other fatty solid acids, such as
stearic and margaric, the fatty matters are slightly warmed, and are run in a
liquid state on to iron or other metal plates, or they are passed into a filter
through powdered metal, such as iron filings. The filtration must be per-
formed with great care to prevent the filtered fatty matter carrying away any
particles of iron in suspension. The operation is then continued in a similar
manner to that before described for free oleic acid.
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 as my improve-
ments in treating fatty and oily matters,-
First, the employment of water acidulated with nitric acid, either in
a pure state or mixed with very small portions of other acids or with salts, for
solidifying fatty and oily matters which are known to be capable of being
solidified by nitric acid, substantially as herein-before described.

page_text: Second, the employment of lime or concentrated sulphuric acid, or diluted
sulphuric acid, for producing saponification in fatty and oily matters produced
in manner herein-before described.
Third, bringing oleic acids and fatty saponified matters containing oleic acid
in contact with iron or other metal on which nitric acid acts, and treating
them afterwards with the same acidulated water to distil them, in order to
remove the foreign mineral substances and the colored matter resulting from
these operations, all as herein-before described.
In witness whereof, I, the said Jules Leonard Louis Cambacérès have
hereunto set my hand and seal this Nineteenth day of January, One
thousand eight hundred and sixty-one.
Witness,
CH. ARMENGAUD, J.. Ing. Civil,
J. L. L. CAMBACÉRES. (L.s.)
Boulev. de Strasbourg, No. 23,
à Paris.