IMPROVEMENTS IN THE MODES OF DISTILLING AND TREATING ORGANIC SUBSTANCES AND BITUMINOUS MATTERS, AND IN THE TREATMENT OF THEIR PRODUCTS, TOGETHER WITH THE APPARATUS USED FOR THE SAID PURPOSES
Year: 1851

page_text: WHEREAS Her present most Excellent Majesty Queen Victoria, by Her
Royal Letters Patent under the Great Seal of the United Kingdom of Great
Britain and Ireland, bearing date at Westminster, the Tenth day of December,
One thousand eight hundred and fifty-one, in the fifteenth year of Her reign,
did, for Herself, Her heirs and successors, give and grant unto me, the said
Etienne Alexander Armand, my exors, adûiors, and assigns, Her especial
license, full power, sole privilege and authority, that I, the said Etienne
Alexander Armand, my exors, adñiors, and assigns, or such others as I, the
said Etienne Alexander Armand, my exors, adñiors, or assigns, should at any
time agree with, and no others, from time to time and at all times during the
term of years therein expressed, should and lawfully might make, use,
exercise, and vend, within England, Wales, and the Town of Berwick-upon-
Tweed, and in the Islands of Guernsey, Jersey, Alderney, Sark, and Man,
and also in all Her said Majesty's Colonies and Plantations abroad, my
Invention of "IMPROVEMENTS IN THE MODES OF DISTILLING AND TREATING ORGANIC
SUBSTANCES AND BITUMINOUS MATTERS, AND IN THE TREATMENT OF THEIR PRODUCTS,
TOGETHER WITH THE APPARATUS USED FOR THE SAID PURPOSES;" in which said
Letters Patent is contained a proviso that I, the said Etienne Alexander
Armand, shall cause a particular description of the nature of my said Inven-
tion, and in what manner the same is to be performed, by an instrument in

page_text: writing under my hand and seal, to be enrolled in Her said Majesty's High
Court of Chancery within six calendar months next and immediately after
the date of the said in part recited Letters Patent, as in and by the same,
reference being thereunto had, will more fully and at large appear.
NOW KNOW YE, that in compliance with the said proviso, I, the said
Etienne Alexander Armand, do hereby declare that the nature of my said
Invention, and in what manner the same is to be performed, are fully
described and ascertained in and by the following statement thereof, reference
being had to the Drawing hereunto annexed, and to the figures and letters
marked thereon (that is to say) :-
It is well known that when organic substances, such as wood, coal, vegetable
or animal fat, gum, resin, horns, hides, and animal waste of all sorts, are
heated in a closed vessel, there takes place a decomposition of the said
substances, and a production of volatile bodies which are sublimed, and of a
solid residuum which remains in the vessel. The same thing happens when,
instead of organic substances, bituminous ore is used; only in the former case
the solid residuum is charcoal more or less pure, in the latter it is the sandy
or earthy substance which serves as a basis in the ore. The volatile products
of this destructive distillation are of various kinds, namely, gas fit for burning
or unfit for it, and vapours which are condensed when out of the distillation
vessel into water, vinegar, essence, coal tar, oil, &c. The proportion of these
different products varies according to the nature of the substance employed,
and to the degree of heat applied to the distillation. Attention has been for a
long time given to the best mode of producing and collecting these various
products by increasing the proportion of some of them at the expense of all the
others, either by using substances which give out the required product in the
greatest abundance, or by placing the said substances in the best oircumstances
in regard to the production of the required article. So are the vinegar
manufacturers using wood, which they distil at a low temperature, while the
gas makers distil coal at a high temperature, and try to reduce as much as
possible the quantity of ammonia and coal tar produced in order to get the
greatest proportion of gas. There are also some inanufacturers whose object
is to produce oil and bituminous matter, but hitherto most of them have given
the preference to the bituminous ores, and to the resinous substances, which
give the best product. Théy, however, use also the tar from the distillation of
coal or of wood for making oils of an inferior kind. There are two distinct
sorts of products obtained from this working:-1°, oils, which are lighter
than water, and are used for dissolving caoutchouc, for preparing varnish, or
may be sold for burning under the name of liquid gas. 20, bituminous matter,

page_text: which, according to its degree of liquidity, may be used for greasing, for
making preservative paint or bituminous cement; but on the one hand the
color and smell of the oils make them unfit to a great number of uses, and on
the other hand the dry residuum is brittle, and the substances made with it are
very imperfect. I have found the means of improving considerably the working
of the above-mentioned substances in respect to the economy as well as to the
perfection of the products. I have observed that, the elements of the gas and of
the tar being the same, it is possible to obtain the one out of the other, such
as gas from tar heated to a high degree, and from gas placed in contact with
tar, a liquid product, very rich in hydrogen, which dissolves in the tar, and
modifies its properties. I have thus been brought to the discovery of an
entirely new and complete system of working the aforesaid substances, which
is founded on the principle that, instead of condensing the volatile products of
the calcination or distillation of the said substances, as has been done hitherto,
the said volatile products should be made to pass through a closed vessel
containing a certain quantity of tar or tar oil, or of a liquid hydrocarbon
in a state of ebullition, in order to reduce considerably the quantity of gas
obtained, and to change the properties of the tar or tar oil or hydrocarbon
used in the same process.
To that effect I have invented a new kind of
apparatus, in which the gas is made at once to pass through the boiling
substance, and the oils are immediately separated, according to the degree of
volatilisation, the light ones being conveyed into a cooling vessel, while the
heavy oils are driven into a separate recipient. I have also invented several
processes by which the said oils are brought to a degree of perfection hitherto
unknown, the effect of which is to separate the most volatile parts, which I
call white or yellow naptha, and to give to this substance a color, smell, and
clearness such as to make it fit for being used instead of the natural naptha
or of turpentine, while the less volatile parts acquire the property of the fixed
oils by being mixed with a certain proportion of vegetable or animal oil, so as
to be used for common lamps, and to burn steadily, without volatilisation or
smell, and with a great saving. The distillation of the said oils I make by
means of a new apparatus, which allows a continuous flow of the oil into the
distilling vessel, and offers various advantages over other known contrivances.
It will be observed, that although the said Invention depends upon a new
system of distilling organic substances, several parts, as well of the apparatus
as of the processes, may be used separately and independently from each other.
I shall now describe the entire process of working as pursued by me, and
explain to that effect the annexed Drawing. The substance to be distilled is
introduced into two or more cast-iron retorts A, A, which are placed at the

page_text: side of each other in the same furnace, being opened at both ends, and of a
shape nearly similar to that of gas retorts. At both ends of each set of retorts
are placed the apparatus for condensing a part of the escaping gas, by causing
it to pass through beated pyrogenic oil, which apparatus is used as follows:-
Before lighting the fire I pour into the spheres c through the opening e,
which I afterwards close by means of a screw or of a cock, pyrogenic oil of
any kind provided its specific gravity be about 0.90 to 0.96, or its boiling
point about 892 or 482 degrees Fahrenheit. The level of the said oil rises
inside the spheres until it has reached the upper part of the small tubes a, a,
when it runs off into the pan D through the large pipe G. The said cast-iron
pan is joined to the sphere c at its upper part by means of a middle conic
piece E, and placed above a flue which allows a free admission of the flame
from the furnace. Inside the said pan is placed a copper cylinder F, opened
at both ends, being fastened by its upper edge between the joint of the picce
E and of the pan. It remains thus suspended at some distance from the
bottom of the pan. In the upper part of the space left between the said
cylinder and the sphere is placed an exit pipe I, that keeps to a constant
level the liquid contained in the pan. The spheres and the pans being pro-
vided with oil as far as the escaping points, I place into the apparatus the
substance that I am about to distil. This might be done by throwing it into
the retorts, as is practised commonly in gasworks. I prefer, however, placing
it into several iron cases B, which I then place in the inside of the retort at
the side of each other. This arrangement makes it a great deal casier to charge
and discharge the retort, and to give an equal degree of heat to the substances
which are acted upon, it makes it also easier to keep everything clean and
save the retort. It might be with great advantage applied to gas works; the
same principle may be applied to the distillation of liquid substances with some
alteration, which I shall describe hereafter. The retort which now holds the
matter to be distilled is carefully closed and luted. The furnace is lighted and
the retort is heated to redness, the said degree of heat is maintained during
the whole time of the calcination. The gas and vapours formed and emitted
during the calcination are driven through the pipe P into the pan D, passing
through a distributing contrivance H that is formed by a copper cover, under
which are placed a great number of small pipes, so that the said volatile
bodies being admitted in small bubbles into the oil contained in the pan are
more divided and better acted upon. A similar distributing contrivance II is
placed inside the sphere at the top of the large pipe, and above the two small
pipes a, a, herein-before described, so as to have about two or three inches
of its lower part dipping in the oil. The volatile bodies after having gone

page_text: through the hot oil contained in the pan, mix with the vapours formed in the
said pans, and rise together into the spheres through the pipe G and the dis-
tributing contrivance that is placed at the top of it. In the sphere they meet
with a new supply of hot oil in which they are partly condensed, the said oil
becoming more and more heated, the most volatile parts escape with the non-
condensed vapours,
the steam, and the other volatile substances into the con-
densers M, where they are partly liquified, the uncondensible gas being made
to pass over into a gasometer, or may be burnt for heating the furnaces; the
less volatile parts remain in the sphere, where they raise the level of the
liquid and cause it to run off through a, a, and fall into the pan. When the
pan itself becomes full its contents run off through I into receiver K. It will
thus be understood, that the cylinder F is used for allowing the outflow of
the liquid, without any escape of the vapours that are introduced inside by
means of the contrivance H. It may be also easily understood that the pan,
the sphere, and the condenser, being every one of them at a different degree
of temperature, contain liquids of various density and volatility, the lighter
and most volatile being in the condenser and the heaviest in the pan. The
above-described apparatus is, as aforesaid, applied at both ends of each set of
retorts, and in order that the level of the oil may be always' equal in the spheres
of both apparatus I connect them by a pipe N. When the distillation is com-
plete, which is known by experience and may be ascertained by opening the
cock of the pipe c that is placed in the retort's mouthpiece, the stopper of the
retort is taken off, the cases are quickly drawn away, and others full of
fresh materials are placed inside, the retort is closed again, and the working
continues as before. It should be observed, that although the above-described
apparatus has been invented by me as being the best actually to my know-
ledge for producing the desired result, it might be differently contrived by
giving to its parts other shapes, or connecting them differently with each other,
or using other materials. The number of the retorts used to each apparatus
is also not material, and may be varied so long as the size of the apparatus
is proportioned to the quantity of substance to be distilled; and I wish it to
be well understood that what I claim respecting this part of my Invention
is,-
First, a mode of calcining or distilling solid organic substances or bitumi-
nous matters, by placing the said substances or matters in metal or earthen-
ware cases of any suitable shape, and introducing the said cases into the
retorts, instead of placing the substances directly into the retorts as heretofore
practised.
Second, a mode of collecting the volatile products from the calcination, as

page_text: herein-before described, by which the said products being made to pass
through hot pyrogenic oil, a part of the uncondensable gas is transformed
into condensable vapour, and those vapours are condensed into liquids of
different density by passing through gases differently heated. When the
vapours to be condensed are to be collected from processes, such as in the
manufacture of coke, and therefore does not allow of using the above-described
contrivance, the passing vapours may be caused to meet the warm oil, falling
along a vertical column full of pebbles, or running in a very thin and wide
stream in a shallow flue. These contrivances are so well known that they
need not be described. In this case the uncondensed vapours escape into
the chimney, and the oil containing the condensed vapours may be divided
into bituminous matter and heavy oil, by the distilling processes, hereafter
described.
I shall now explain how I work the above-named products, in order to
make them particularly adapted for consumption. The light oils obtained in
the condenser are of a dark yellowish colour, they have a strong disagreeable
smell, their specific gravity is about 0.84 to 0.85. I have found that their
colour and smell is completely modified adding to them about one per cent.
of nitrous sulphuric acid obtained by passing nitrous vapours through con-
centrated sulphuric acid. The acid is poured gradually in order to prevent
the heating of the mixture, which should be continually agitated during that
time. After a short time's rest the oil clears itself, the colouring matter being
combined with the acid and gradually deposited. During the time this
separation takes place, the liquid becomes of a red vinous colour, if it is of a
dark green the mixture must be again agitated until it has come to the said
red vinous tinge. It should then be carefully decanted, and washed first with
lime water, which saturates the acid, and afterwards with clear water. The oil
is then placed in a reservoir S. A similar reservoir receives an equal quantity
of a concentrated saline solution made of equal weights of an alkaline chloride
and an alkaline nitrate, such as sea salt and nitrate of potash. The oil may
be distilled in the presence of this saline solution in order to absorb the
sulphurous acid that may have been left, and also to keep the distilling
apparatus provided with steam, which makes easier the working of the
distillation. I can use the above-described self-acting apparatus with a few
alterations or additions, which I shall now describe. In this part of the
working I prefer using the apparatus such as shewn in Figure 7, that is to
say, by placing an apparatus at each end of the retorts and connecting it more
closely with the retort. Instead of the open cases, I place into the retort a
closed case R having a large opening at each side, the said case is connected

page_text: at each side by a pipe f with the reservoirs S that are placed on the top of
the furnace, and heated by the escaping smoke. On the course of the pipe f
in the part that is inside the retort is placed a ball V, in which the liquids
running from the reservoir become still more heated before running into the
case R. The spheres being provided with rectified oil and the furnace heated,
the oil on one side and the saline solution on the other are allowed to run at
the same time from the reservoirs S through the connecting pipe f into the
case R. The vapours that are formed in the case go away by the openings T
into the retort, and from thence through G into the spheres, where they force
their way through the rectified oil which the spheres have been provided with.
There they get condensed, and soon heat the liquid placed in the spheres up
to the boiling point. Then the lighter parts only go away into the condensers
M, where they are condensed into an oil perfectly clear and colourless. The
heavier parts remain in the spheres C. The quantity of liquid contained in the
spheres being increased, a portion of it is syphoned off, as before described,
into the pans D, and the working goes on as already explained, having in the
different parts of the apparatus products of various densities. In respect to
the above described processes, it should be observed that, although I prefer
using nitrous sulphuric acid for rectifying the light oils, I might also uso
instead of it concentrated sulphuric acid with peroxide of manganese, or add
with chromate of potash or permanganate of potash or in general any suitable
oxidysing body. It should be observed respecting the saline solution that the
above-mentioned salts might be replaced by a melted mixture of anhydrous
lime and potash placed on three metallic sieves arranged the one above the
other inside the case R, which said substances I find to be very well adapted
for taking away the sulphurous acid and clearing the oil. The distillation
should be stopped now and then in order to renew the supply of the said
mixture or to draw out the deposited salt. I would observe that the use of
the oxydising body might be dispensed with; in that case the oil keeps a
citrous colour instead of becoming quite clear and colourless. The heavy oils
obtained in both the above-described operations I treat in the following
way: I first mix them with about one per cent. in weight of nitrous sulphuric
acid or any of the above suitable oxydising matters, and allow it to rest a
moment, then I decant the liquor and wash it repeatedly with a tepid solution
of lime. I then mix the oil with about 3/4ths in weight of fixed oil like oleine,
rape seed oil, &c., and I again add to the mixture about two per cent. of the
above oxidysing matter. I then agitate the whole mixture until it is of a fine
violet colour. I now use again a weak lime solution or merely steam, which

page_text: precipitates the sulphuric acid that may be in suspension. I filter the liquid,
and find that the oil has passed from the violet colour to the yellow, being
perfectly transparent. The separation of the acid is very slow, it is necessary
to wash repeatedly and to allow the liquid to rest one or two days after each
washing. I find that I may also proceed in the following manner-I only
make the mixture with the fixed oils after having used the second addition of
oxydising matter, decanted the liquor, and washed it with slightly alkalised
water. I then place the mixture on a sand bath warmed to about 392 degrees
Fahrenheit for about six hours. As to the heaviest oil or matter which is
found in the pans D, it may according to its degree of concentration be used
as a grease for machinery or for carriages, as common bitumen, or even as
native asphaltum. My new mode of producing the said matter gives it some
particular properties. I now only concentrate it more or less according to
the use I wish to make of it, and for that purpose I use the above-described
distilling apparatus. With the heaviest oil collected during the said distillation
I make a solid grease by mixing the solid oil with about ten per cent. in
weight of resin or of a fixed oily or fatty substance, and treating the said
mixture by a solution of lime and potash or lime and soda at a heat of 212°
Fahrenheit, and agitate continually until the substance becomes viscid.
When cooled the said substance is of a brown colour, very unctious, and may
be used for greasing carts or railway carriages.
In this second part of my Invention I wish it to be understood that what I
claim is,
First, the several described modes of treating the light oils, heavy oils, and
bituminous matters by means of the defined chemical processes when working
the apparatus herein described.
Second, a mode of distilling any kind of liquid organic substance and
bituminous matter similar to that claimed for dry substances in the former
part of this Specification, with this difference, that instead of placing inside
the retort opened cases containing the solid substances, I place inside the retort
a closed case with suitable openings, the said case being connected by any
suitable providing contrivance such as described with the vessel containing the
liquid substances, which I prefer placing outside the retort, and further a
particular contrivance, as herein described, for heating the liquid substance
on its way from the reservoir into the case. The above-mentioned case, the
form of which I have described, such as I use it can, of course, be made of
any suitable shape or material according to the convenience of the manu-
facturer, to the shape of the retort, and to the position of the other part of

page_text: the apparatus. Fixed fat bodies, for instance, when distilled by means of the
apparatus, instead of falling directly on the bottom of the case, should be made
to run inside by a fan-shaped opening through several fine metallic sieves
placed inside the case in order to divide the fall and hasten the working. It
should be mentioned that the use of a closed case V with side openings may
be preferable to open cases for the working of bituminous or asphaltic solid
ore, which I prefer treating by means of an addition of about ten per cent.
of light oil, the retort being heated to about 392°. The oil dissolves the
bituminous matter, vapours are formed, and the liquid is forced through the
openings into the pans D, where it is concentrated. After the flow from
the case has ceased, the case is pulled out of the retort, and is found to contain
nothing but the earthy matter of the ore.
Now in order to make the annexed Drawings better understood I shall sum
up the explanation of all their different parts, although I only intend claiming
as my Invention the parts which I have described as such in the above
Specification.
The Fig. 1 represents a side view of the calcining and distilling apparatus.
Fig. 2, a front view of the same. Fig. 3, a section through the axis of the
sphere and pan. Fig. 4, a section through the axis of the retort. Fig. 5, a
transverse section through the axis of the sphere and pan. Fig. 6, a trans-
verse section through the middle of the furnace. Fig. 7, a section through the
axis of the distilling apparatus, applied to the distillation of oils and other liquid
substances. Fig. 8, a transverse section of the same, through the middle of
the furnace. Fig. 9, a section of the apparatus used for working asphaltic or
bituminous ore. A, the retort. B, the open cases, filled with the matter
to be distilled. C, the spheres. D, the pans. E, conic picces, joining the
sphere and the pan. F, copper cylinder. G, copper tube, through which
the vapours are introduced into the spheres. H, distributing apparatus. a, a,
tubes for the escape of the oils from the spheres into the pans. b, b, b, small
tubes for the distribution of the vapours, being part of the distributing contri-
vance H. I, pipe for the escape of the oil from the pans. K, vessel for
collecting the liquid coming out of the pans. L, exit pipe for the vapours and
gas escaping from the spheres. c, pipe for watching the working in the retort.
d, pipe and cock for emptying the spheres. e, opening for introducing the oil
into the condensing apparatus. M, condensing apparatus. N, tube, joining
the two spheres. O, safety pipe. P', pipe, leading from the retorts into the
pans. R, closed case, for distilling liquid substances. S, reservoirs. T,
opening for the exit of vapours out of the case R. U, case for the working

page_text: of asphaltic or bituminous solid ore. f, tubes leading from the reservoirs
to the case R. V, balls for heating the liquid coming into the case R. X,
dampers.
In witness whercof, I, the said Etienne Alexander Armand, have here-
unto set my hand and seal, this Twenty-seventh day of December,
One thousand eight hundred and fifty-one.

page_text: AND BE IT REMEMBERED, that on the oath of Samuel Carpmael, the
Specification aforesaid was enrolled, word for word, as above written.
And
also the Specification aforesaid was stamped according to the tenor of the
Statute made for that purpose.
Enrolled the Fifth day of February, in the year of our Lord One
thousand eight hundred and fifty-two.