IMPROVEMENTS IN THE TREATMENT OF PARAFFINE FATTY AND RESINOUS MATTERS
Year: 1867

page_text: LETTERS PATENT to Leo de la Peyrouse, of Somerset Street,. Portman
Square, in the County of Middlesex, for the Invention of "IMPROVEMENTS
IN THE TREATMENT OF PARAFFINE FATTY AND RESINOUS MATTERS." -A
communication from abroad by Leon Krafft, Chemist, Rue de l'Eglise a
Neuilly, pres Paris.
Sealed the 24th March 1868, and dated the 27th September 1867.
PROVISIONAL SPECIFICATION left by the said Leo de la Peyrouse at
the Office of the Commissioners of Patents, with his Petition, on the
27th September 1867.
I,.LBO DE LA PEYROUSE, of Somerset Street, Portman Square, in the County
5 of Middlesex, do hereby declare the nature of my said Invention: for
"IMPROVEMENTS IN THE TREATMENT OF PARAFFINE FATTY AND RESINOUS
MATTERS," to be as follows:-
Raw or crude paraffine of commerce is, as is well known, a mixture of
paraffine, tar, carbonaceous matters, heavy mineral:oils, and coloring, matters,
and the purification or refining of such paraffine as well as its decoloration
'consists in the separation of the before-mentioned substances.
In order to effect the separation of the tarry and carbonaceous matters I
employ such chemical agents as possess the property of removing the before-
mentioned impurities, and of concreting a portion of the heavy oils contained
in the paraffine. I also employ such. chemical agents as will effect the pre-

page_text: cipitation of the tarry matters contained in the crude paraffine, as well as the
precipitation of the coloring matters, so as to yield paraffine entirely free
from tarry matters, and both limpid and transparent, and of a white, or grey, or
pale yellow color. I also adopt as a method of separating the tarry matters
from the crude paraffine by maintaining the same in a state of fusion for a
given time at a temperature of about 60° Centigrade. The tarry matters and
other impurities being denser than the paraffine sink, and the paraffine is
withdrawn in a purified condition. Before proceeding to effect by means of
pressure the separation of a portion of the mineral oils contained in impure
paraffine, I cause to act on the dissolved paraffine such chemical agents as
possess the property of combining with a portion of the heavy mineral oil,
clarifying the liquid paraffine, and abstracting from it the greater portion of
the coloring matters. I also employ natural and artificial cold so as to obtain
and retain the paraffine in a solid form, such as cake, or otherwise, at a
temperature of from about 6° to 10° Centigrade below zero, for the purpose
of separating the mineral oils therefrom. I also employ saponifiable liquid
fatty bodies as well as such liquid bodies which have a boiling point of about
100° Centigrades, such as chloroform, naptha, bydruret of amylene, for the
purpose of effecting the separation of mineral oils by solution from impure
paraffine.
I shall now proceed to describe the substances which I employ for the
precipitation of the tarry and carbonaceous matters, and for effecting the
decoloration and clarification of paraffine and the separation therefrom of
the mineral oils.
In order to separate the tarry and carbonaceous matters contained in crude
paraffine it is first melted or fused by heating it to a temperature of from 120°
to 180° Centigrade; the water and the earthy matters which are contained in
the crude paraffine are thereby separated, and the paraffine. is then agitated
either mechanically or otherwise, and to it is added during such agitation such
quantities of sulphuric acid containing. in solution either nitrous acid or
sulphurous acid, or mixtures of the same, as may be requisite for effecting the
separation of the coloring matter, and to concrete. the tarry and oily com-
pounds contained therein; these concreted products are allowed to settle and
the clear paraffine is decanted. Or I employ a solution of chloride of zinc,
and by preference such a solution of the same in water as shall have a boiling
point of about 120° Centigrade. I raise this solution to about its boiling point
and place the crude paraffine therein, and after submitting it to the action of
such a solution of chloride of zino for such time as shall be necessary to
destroy the coloring and other matters and to concrete the tarry products, 1

page_text: anow the impurities to Substat, an
processes the concretion of the tarry matters and of a portion of the heavy
mineral oils will be effected, and the paraffine will become purified:
Similar results may be obtained by employing nitrous acid, azoto amidon,
obtained mixing nitric acid and starch, or obtained by other means; sulphu-
retted hydrogen and its compounds may also advantageously be employed for
like purposes.
I also employ as a bleaching agent sulphurous acid, which I introduce
either into the melted paraffine as a gas, or I generate the same in the vessel
containing the paraffine.
In order to effect. the precipitation of the tarry and carbonaceous matters I
employ alkaline or earthy sulphurets, hydro-sulphurets, hypo-sulphites, or
sulphites, and after effecting the separation of such tarry and carbonaceous
matters by any of the processes herein-before mentioned the paraffine is
allowed to deposit any insoluble impurities it may contain, during which time
it is maintained in a liquid state, and after subsidence it is drawn off through
cocks provided for that purpose, but the discharge cock placed at or about the
bottom of the vessel is by preference not opened until the purified paraffine
has been drawn off.
I prefer to wash the paraffine after having been thus treated with hot or
tepid water before commencing the decoloring process. The decolorisation I
effect by means of oxygen, which may be produced either in the melted
paraffine, or be introduced therein in a gaseous form at or about the bottom
of the vessel containing the paraffine. And I further employ as decolorising
agents such other substances as sulphurous acid, which I have found to give
good results. I further employ alumina, and in such case employ it either in
a hydrated condition, or in the form of refractory clay, pipe-clay, kaolin clay,
or otherwise. The salts of alumina, such as alum, may be advantageously
employed for the decoloration and clarification of paraffine, and for the pre-
cipitation of the coloring matters contained therein. The pulverulent matters
herein-before described may be employed either in solution in water, or they
may be treated with the paraffine, the same being kept stirred or agitated; a
jet of steam may advantageously be introduced into the paraffine during such
operation. After this process it is subjected to a process of filtration, and to
it is added from 10 to 20 per cent: of a saponifiable oil, or some volatile spirits
extracted from solid or liquid bituminous. matters or resin, obtained from the
distillation of seaweeds rich in paraffine and tar, chloroform, ether, hydruret
of amylene. The liquid paraffine is then run into moulds, where it is allowed
to crystallize slowly; the moulds are cooled, to a low temperature so as to

page_text: effect perfect solidification; this solidification is obtained at a temperature
varying from 5 to 8 degrees Centigrade below zero, it is then pressed at a low
temperature, as I have before described. The heavy mineral oils which
discolor the crude paraffine are thus separated, and on the examination of
the cakes it will be seen whether it be necessary to repeat the operation, or
whether the bleaching and purification can be proceeded with at once, either
by simply filtering it when in a heated state through animal charcoal in the
ordinary way, or otherwise.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Leo de la Peyrouse in the Great Seal Patent Office on the
27th March 1868.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, LEO DE LA
PEYROUSE, of 10, Somerset Street, Portman Square, in the County of
Middlesex, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-seventh day of September, in the year of our
Lord One thousand eight hundred and sixty-seven, in the thirty-first year of
Her reign, did, for Herself, Her heirs and successors, give and grant unto
me, the said Leo de la Peyrouse, Her special license that I, the said Leo de
la Peyrouse, my executors, administrators, and assigns, or such others as I,
the said Leo de la Peyrouse, my executors, administrators, or 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
aud Ireland, the Channel Islands, and Isle of Man, an Invention for
"IMPROVEMENTS IN THE TREATMENT OF PARAFFINE FATTY AND RESINOUS
MATTERS," a communication to me from abroad by Leon Krafft, Chemist,
Rue de la Eglise, á Neuilly, pres Paris, upon the condition (amongst others)
that I, the said Leo de la Peyrouse, my executors or administrators, by an
instrument in writing under my hand and seal, 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 Leo de la Peyrouse, do hereby
declare the nature of the said Invention, and in what manner the same is to

page_text: be performed, to be particularly described and ascertained in and by the
following statement, that is to say :-
Raw or crude paraffine of commerce is as is well known a mixture of
paraffine, tar, carbonaceous matters, heavy mineral oils, and colouring matters,
and the purification or refining of such paraffine, as well as its decolouration,
consists in the separation of the before-mentioned substances.
In order to effect the separation of the tarry and carbonaceous matters I
employ such chemical agents as possess the property of removing the before-
mentioned impurities, and of concreting a portion of the heavy oils contained
in the paraffin. I also employ such chemical agents as will effect the precipi-
tation of the tarry matters contained in the crude paraffin, as well as the
precipitation of the coloring matters, so as to yield paraffin entirely free from
tarry matters and both limpid and transparent, and of a white, or grey, or pale
yellow color. I also adopt as a method of separating the tarry matters from
the crude paraffin by maintaining the same in a state of fusion for a given time at
a temperature of about sixty degrees Centigrade. The tarry matters and other
impurities being denser than the paraffin sink, and the paraffin is withdrawn
in a purified condition. Before proceeding to effect by means of pressure the
separation of a portion of the mineral oils contained in impure paraffin I
cause to act on the dissolved parathin such chemical agents as possess the
property of combining with a portion of the heavy mineral oil clarifying the
liquid paraffin and abstracting from it the greater portion of the coloring
matters. I also employ natural and artificial cold, so as to obtain and retain
the paraffia in a solid form, such as cake or otherwise at a temperature of
from about 6 degrees to ten degrees Centigrade below zero for the purpose
of separating the mineral oils therefrom. I also employ saponifiable liquid,
fatty bodies as well as such liquid bodies which have a boiling point of about
100 degrees Centigrades, such as chloroform, naptha, hydruret of amylene for
the purpose of effecting the separation of mineral oils by solution from impure
paraffin.
I shall now proceed to describe the substances which I employ for the
precipitation of the tarry and carbonaceous matters, and for effecting the
decoloration and clarification of paraffin, and the separation therefrom of
the mineral oils.
In order to separate the tarry and carbonaceous matters contained in crude
paraffin, it is first melted or fused by heating it to a temperature of from 120
degrees to 130 degrees Centigrade; the water and the earthy matter which are
contained in the crude paraffin are thereby separated and the paraffin is then
agitated, either mechanically or otherwise, and to it is added during such

page_text: agitation such quantities of sulphuric acid containing in solution either nitrous
acid or sulphurous acid, or mixtures of the same as may be requisite for
effecting the separation of the coloring matter, and to concrete the tarry and
oily compounds contained therein these concreted products are allowed to
settle and the clear paraffin is decanted or drawn off. I employ a solution of
chloride of zinc, and by preference such a solution of the same in water as
shall have a boiling point of about 120 degrees Centigrade. I raise this
solution to about its boiling point, and place the crude paraffin therein, and
after submitting it to the action of such a solution of chloride of zinc for such
time as shall be necessary to destroy the coloring and other matters, and to
concrete the tarry products, I allow the impurities to subside and then remove
the paraffin. By these processes the concretion of the tarry matters and of a
portion of the heavy mineral oils will be effected, and the paraffin will become
purified.
Similar results may be obtained by employing nitrous acid, azoto amidon,
obtained by mixing nitric acid and starch, or obtained by other means;
sulphurretted hydrogen and its compounds may also advantageously be
employed for like purposes.
I also employ as a bleaching agent sulphurous acid, which I introduce either
into the melted paraffin as a gas, or I generate the same in the vessel con-
taining the paraffin.
In order to effect the precipitation of the tarry and carbonaceous matters
I employ alkaline or earthy sulphurets, bydro-sulphurets, hypo-sulphites, or
sulphites, and after effecting the separation of such tarry and carbonaceous
matters by any of the processes herein-before mentioned the paraffin is
allowed to deposit any insoluble impurities it may contain, during which
time it is maintained in a liquid state, and after subsidence it is drawn off
through cocks provided for that purpose, but the discharge cock placed at or
about the bottoin of the vessel is by preference not opened until the purified
paraffin has been drawn off.
I prefer to wash the paraffin after having been thus treated with hot or
tepid water before commencing the decoloring process. The decolorization I
effect by means of oxygen which may be. produced either in the melted
paraffin or be introduced therein in a gaseous form at or about the bottom of
the vessel containing the paraffin. And I further employ as decolorising
agents such other substances, as sulphurous acid, which I have found to give
good results. I further employ alumina, and in such case employ it either in
a hydrated condition or in the form of refractory clay, pipe clay, kaolin clay,
or otherwise. The salts of alumina, such as alum, may be advantageously

page_text: employed for the decoloration and clarification of paraffin, and for the
precipitation of the coloring matters contained therein. The pulverulent
matters herein-before described may be employed, either in solution in water
or they may be treated with the paraffin, the same being kept stirred or
agitated; a jet of steam may advantageously be introduced into the paraffin
during such operation. After this process it is subjected to a process of
filtration, and to it is added from ten to twenty per cent. of a saponifiable oil
or some volatile spirits extracted from solid or liquid bituminous matters or
resin obtained from the distillation of seaweeds rich in paraffin and tar,
chloroform, ether, hydruret of amylene. The liquid paraffin is then run into
moulds, where it is allowed to crystallize slowly; the moulds are cooled to a
low temperature so, as to effect perfect solidification. This solidification is
obtained at a temperature varying from five to eight degrees centigrade below,
zero, it is then pressed at a low temperature as I have before described. The
heavy mineral oils which discolor the crude paraffin are thus separated, and on
the examination of the cakes it will be seen whether it be necessary to repeat
the operation, or whether the bleaching and purification can be proceeded
with at once either by simply filtering it when in a heated state through
animal charcoal in the ordinary way or otherwise.
What has been previously stated respecting the treatment of the hydro-
carbons called paraffin is equally applicable to the treatment of the animal
and vegetable fats and oils, such as grease, lard, suet, tallow, palm oil, cocoa-nut
oil, vegetable suet, Japan wax, and resinous matters, and more particularly to the
treatment of suets and tallow, the purification of which may be advantageously
effected as follows:-If suet is required to be treated it should be melted in a
wooden vat lined with lead, and containing a quantity of water equal to at
least twenty-five per cent. of the suet to be operated upon. Placed in this
vat is a leaden worm intended to admit of the circulation of the steam, or an
open steam pipe may be placed therein in order to raise the temperature of
the contents of the vat, so as to expedite the melting of the suet. With a
view to disintegrate the cellular portion of the suet for the purpose of
extracting the whole or nearly the whole of the tallow therein contained,
about two and a half per cent. by weight of vitriol or commercial sulphuric
acid is added to the contents of the vat previously diluted with from three to
four parts of water. In melting the suet with the acid and when the melting
is in part effected the developement of the nascent oxygen takes place, which
produces a whiteness and solidity such as no other method of treatment
bitherto adopted has effected. In order to obtain this nascent oxygen any
matter suitable for the development of oxygen may be used, but I prefer

page_text: mineral peroxides, to which are added a sufficient quantity of vitriol or com-
mercial sulphuric acid at 45° B., such as the peroxides of manganese or
permanganates which should be employed in the proportion of from one to
five per cent. of the quantity of suet to be treated according to the degree of
whiteness and firmness required. By continuing the operation for about five
hours the glycerine will be set free and may be separated by pressure or
otherwise. The chlorides and perchlorides of zinc and of tin which are
employed by preference at from 40 degrees to 45 degrees Baumé, give
similar results, producing especially great firmness, which may be carried to
the utmost limits without the fatty body losing any of its illuminating
qualities.
The treatment with nascent sulphurous acid above described is also
advantageous. What has been stated in reference to the treatment of suet
equally applies to the treatment of tallow. The mixture and union of certain
bydrocarbons with suet or tallow imparts to them new and hitherto unknown
properties; thus by adding to melted suet from two to five per cent. of bodies
boiling between 75 degrees and 100 degrees Centigrade, such as volatile
spirits extracted from solid or liquid bituminous matters from resin, from the
distillation of seaweeds, and other sources, and by mixing them well together
there will be obtained either with or without pressure a new product both dry
and brilliant, and particularly suitable for the purpose of illumination, even
with a plaited or woven wick, and capable of being economically substituted
for composites and other candles. The suet or tallow after having been treated
as before mentioned is then submitted to pressure or otherwise, and is mixed
with either palmitic acid, paraffine, Japan wax, refined Canabar wax, or
mixtures of the same in the proportion of about 15 to 20 per cent. of the
weight of tallow or suet employed, the resulting material will be found to be
well adapted for the manufacture of candles, and it will be evident that the
proportions in which the before-mentioned ingredients are to be employed will
be dependant on the hardness and quality of the candle required. By treating
suet and the fatty bodies with those compounds which have a boiling point
between 75° and 100° Centigrades, increased whiteness and brilliancy are
produced. The decomposition, by means of acids or otherwise of the suets
may be effected either before or after they have been submitted to the before-
mentioned process.
Having now described and particularly ascertained the the nature of the said
Invention, and the manner in which the same is or may be used or carried
into effect, I would observe in conclusion that what I consider to be novel
and original, and therefore claim as the Invention secured to me by the herein-

page_text: before in part recited Letters Patent is, the treatment of paraffine fatty
and resinous matters in the manner and for the purpose herein-before
described.
In witness whereof, I, the said Leo de la Peyrouse, have to this my
Specification set my hand and seal, this Twenty-sixth day of March
One thousand eight hundred and sixty-eight.
L. DE LA PEYROUSE. (L.S.)