Im- PROVEMENTS IN THE DISTILLATION AND SEPARATION OF HYDROCARBURETS AND THEIR DERIVATIVES, AND IN APPARATUS FOR THE SAME
Year: 1863

page_text: LETTERS PATENT to William Clark, of 53, Chancery Lane, in the County
of Middlesex, Engineer and Patent Agent, for the Invention of "Im-
PROVEMENTS IN THE DISTILLATION AND SEPARATION OF HYDROCARBURETS AND
THEIR DERIVATIVES, AND IN APPARATUS FOR THE SAME."-A communication
from abroad by Jean Théodore Coupier, of .29, Boulevart St. Martin,
Paris, Manufacturer.
Sealed the 18th November 1863, and dated the 5th June 1863.
PROVISIONAL SPECIFICATION left by the said William Clark at the
Office of the Commissioners of Patents, with his Petition, on the
5th June 1863.
I, WILLIAM CLARK, of 53, Chancery Lane, in the County of Middlesex,
Engineer and Patent Agent; do hereby declare the nature of the said
Invention for IMPROVEMENTS IN THE DISTILLATION AND SEPARATION OF HYDRO-
CARBURETS AND THEIR DERIVATIVES, AND IN APPARATUS FOR THE SAME," to be as
follows:-
In the various methods of treating hydrocarburets for obtaining coloring
matters therefrom, I have remarked that the result differs according as they
contain a greater or less quantity of heavy oils, also that the amount of
coloring matter greatly varies, while the latter does not always furnish the

page_text: same tinctorial products. I have also found when operating with pure
products, obtained at great expense in a laboratory, that each of the
hydrocarburets contained in these oils possesses peculiar properties, and
should, in order to obtain good results, be treated separately and in a different
manner.
The object of this Invention is thus to find a practical means of separating
the hydrocarburets, so as to obtain manufacturing products containing 95 per
cent. of pure matters. For this purpose I employ the apparatus represented
in the accompanying Drawing, Fig. 1 of which shows an elevation of the
rectifying column, partly in section, while Figs. 2 and 3 show a plan and
central section of one of the plates.
a; rectifying column, composed of a series of plates b, mounted on a lower
reservoir c, which is heated by means of a worm tube d. Each plate bis
divided into compartments, which forces the liquid to make a lengthened
traverse throughout the plate, so as to afford time for the products of distil-
lation to be given up before falling on the lower plate, and so as to become
completely separated from the hydrocarburet during its distillation; d', steam
passages in the lower plate for uniformly heating all the channels in each
plate in which the liquid passes, for which purpose the steam passages extend
throughout the extent of each channel; e, exit for the liquid to pass from the
upper to the lower plate; f, emptying cock; 9, man-hole; h, thermometer,
placed on the upper plate of the rectifying column; i, syphon, for conducting
the vapours in course of distillation to the separating worm pipe j. The pipe
is contained in a bath k, which regulates the temperature by the super-eleva-
tion of the temperature of the liquid it contains. The worm pipe j is furnished
with two pipes l, for returning all the distilled products to the column in a
greater state of purity than those in course of distillation; m, thermometer of
the bath; n, refrigerating condenser; o, worm tube, for heating the liquid in
bath k.
This apparatus is based on the same principle as ordinary distilling appa-
ratus, but differs from it, 1st, in the arrangement of the plates for the purpose
of obtaining the same result with a considerably less number of them, the
object being to maintain the temperature at a certain point in a certain
number of superposed plates heated one by the other, which is necessary in
order to effect the distillation of hydrocarburets the boiling point of which is
above 212 degrees Fahrenheit; 2ndly, in this case the apparatus is furnished
with a bath containing a separating worm pipe and also a heating worm pipe,
the bath being also filled with a liquid the boiling point of which is above

page_text: that of water, and consisting either of a solution of chloride of calcium or of
oil, according as the boiling point of the hydrocarburets to be separated is
more or less elevated, so as to maintain the bath at the necessary temperature
by means of a heated worm tube contained in said bath. I use steam for
heating the hydrocarburets the boiling point of which is below 275 degrees
Fahrenheit, while for those requiring higher temperatures I superheat the
steam.
Supposing, for example, without limiting myself in any way to the mixed
hydrocarburets herein menționed, I wish to obtain the separation of the
hydrocarburets contained in benzine, viz., 1st, an oil lighter than benzine;
2ndly, benzine; 3rdly, toluine; 4thly, xyline; and 5thly, cumine. The dis-
tillation should be effected in the following manner :-For all the parts which
may be distilled below 76 degrees Fahrenheit steam under two atmospheres
may be used, and the temperature of the liquid contained in the bath main-
tained at 140 degrees Fahrenheit at the maximum. For benzine, which may
be distilled at from 176 to 180 degrees Fahrenheit, I use steam at two
atmospheres, and heat the bath to a temperature of from 150 to 158 degrees
Fahrenheit as a maximum. For toluine, which distils at from 230 to 235
degrees Fahrenheit. I use steam at 3 atmospheres, and the bath at a
temperature of from 212 to 221 degrees Fahrenheit at the maximum. For
xyline, which distils at from 257 to 266 degrees Fahrenheit, I use steam at
six atmospheres, the bath being at a temperature of from 248 to 257 degrees
Fahrenheit as a maximum. For cumine, which distils at from 300 to 305
degrees Fahrenheit, I use steam at 6 atmospheres superheated, the tempera-
ture of the bath being from 286 to 293 degrees Fahrenheit, and so on for
those hydrocarburets the boiling points of which are higher than those above
mentioned. The result obtained from 20 gallons may be seen by reference to
the Diagram Fig. 4, plus 1 quart of phenic acid and two per cent. loss. It will
be seen by this Diagram that every time the temperature rises suddenly the
distilling action produces an impure product, composed (generally of two
sorts), viz., that distilled immediately, and that afterwards produced. The
impure products are placed on one side to be re-distilled, each separately,
in the same manner as before, the pure products being ready for use.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said William Clark in the Great Seal Patent Office on the
3rd December 1863.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, WILLIAM
CLARK, of 53, Chancery Lane, in the County of Middlesex, Engineer and
Patent Agent, send greeting.
WHEREAS Iler most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Fifth day of June, in the year of our Lord
One thousand eight hundred and sixty-three, in the twenty-sixth year of
Her reign, did, for Herself, Her heirs and successors, give and grant unto
me, the said William Clark, Her special licence that I, the said William
Clark, my executors, administrators, and assigns, or such others as I, the
said William Clark, 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 DISTILLATION AND SEPARATION OF HYDROCARBURETS AND THEIR DERIVATIVES,
AND IN APPARATUS FOR THE SAME," a com". to me from abroad by Jean
Théodore Coupier; of 29, Boulevart St. Martin, Paris, Manufacturer, upon
the condition (amongst others) that I, the said William Clark, 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 William Clark, do hereby declare the
nature of the said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, reference being had to the Sheet of Drawings hereunto annexed,
and to the letters and figures marked thereon (that is to say):-
In the various methods of treating mixed bydrocarburets for obtaining
coloring matters therefrom, I have remarked that the result differs according
as they contain a greater or less quantity of heavy oils, also that the amount
of coloring matter greatly varies, while the latter does not always furnish the
same tinctorial products. I have also found, when operating with pure

page_text: products obtained at great expense in a laboratory, that each of the hydro-
carburets contained in these oils possesses peculiar properties, and should,
in order to obtain good results, be treated separately and in a different
manner.
The object of this Invention is thus to find a practical means of separating
the hydrocarburet so as to obtain manufacturing products containing 95 per
cent. of pure matters. For this purpose I employ the apparatus represented
in the accompanying Drawing, Fig. 1 of which shows an elevation of the
rectifying column, partly in section, while Figs. 2 and 3 show a plan and
central vertical section of one of the plates.
a, rectifying column, composed of a series of plates b, mounted on a lower
reservoir c, which is heated by means of a worm tube d¹. Each plate 6 is
divided into compartments, which forces the liquid to make a lengthened
traverse throughout the plate, so as to afford time for the products of distil-
lation to be given up before falling on the lower plate, and so as to become
completely separated from the hydrocarburet during the distillation; d, steam
passages in the lower plate for uniformly heating all the channels in each
plate in which the liquid passes, for which purpose the steam passages extend
throughout the extent of each channel; e, exit for the liquid to pass from the
upper to the lower plate; f, emptying cock; 9, man-hole; h, thermometer,
placed on the upper plate of the rectifying column; i, syphon, for conducting
the vapours in course of distillation to the separating worm pipe j. This pipe is
contained in a bath k, which regulates the temperature by the super-elevation of
the temperature of the liquid it contains. The worm pipe j is furnished with
two pipes 1, for returning all the distilled products to the column in a greater
state of purity than those in course of distillation; m, thermometer of the
bath; n, refrigerating condenser; o, worm tube for heating the liquid in
bath k.
This apparatus is based on the same principle as ordinary distilling
apparatus, but differs from it, 1st, in the arrangement of the plates for the
purpose of obtaining the same result with a considerably less number of them,
the object being to maintain the temperature at a certain point in a certain
number of superposed plates heated one by the other, which is necessary in
order to effect the distillation of hydrocarburets the boiling point of which is
5 above 212 degrees Fahrenheit; 2ndly, in this case the apparatus is furnished
with a bath containing a separating worm pipe and also a heating worm
pipe, the bath being also filled with a liquid the boiling point of which is
above that of water, consisting either of a solution of chloride of calcium or of

page_text: oil, according as the boiling point of the hydrocarburets to be separated is
more or less elevated, so as to maintain the bath at the necessary temperature
by means of a heated worm. tube contained in said bath. I use steam for
heating the hydrocarburets the boiling point of which is below 275 degrees
Fahrenheit, while for those requiring higher temperatures I superheat the
steam.
Supposing, for example, without limiting myself in any way to the mixed
hydrocarburets herein mentioned, I wish to obtain the separation of the
hydrocarburets contained in. benzine, viz., 1st, an oil lighter than benzine;
2ndly, benzine; 3rdly, toluine; 4thly, xyline; and 5thly, cumine. The distillation
should be effected in the following manner :-For all the parts which may be
distilled below 76 degrees Fahrenheit steam under two atmospheres may be
used, and the temperature of the liquid contained in the bath at 140 degrees
Fahrenheit at the maximum. For benzine, which may be distilled at from 176
to 180 degrees Fahrenheit, I use steam at two atmospheres, and heat the bath
to a temperature of from 150 to 158 degrees Fahrenheit at. the maximum.
For toluine, which distils at from 230 to 235 degrees Fahrenheit, I use steam
at three and a half atmospheres, the bath being at a temperature of from
212 to 221 degrees Fahrenheit at the maximum. For xyline, which distils at
from 256 to 267 degrees Fahrenheit, I use steam at six atmospheres, the bath
being at a temperature of from 248 to 257 degrees Fahrenheit at a maximum.
For cumine, which distils at from 300 to 305 degrees Fahrenheit, I use steam
at six and a half or seven atmospheres superheated, the temperature of the
bath being from 286 to 293 degrees Fahrenheit, and so on for those hydro-
carburets. the boiling points of which are higher than those above mentioned.
The results obtained from twenty gallons may be seen by reference to the
Diagram Fig. 4, plus one quart of phenic acid and two per cent. loss: It
will be seen by this Diagram that every time the temperature rises suddenly
the distilling action produces an impure product, composed generally of two
sorts, viz., that distilled immediately, and that afterwards produced. The
impure products are placed on one side to be re-distilled, each separately, in
the same manner as before, the pure products being ready for use.
Having described the nature of this Invention, and the manner of perform-
ing the same, I declare that what I claim as the Invention to be protected by
the herein-before in part recited Letters Patent is,-
First, the improved method of separating all kinds of mixed hydrocarburets
and their derivatives as herein-before described, whereby all the units con-
tained in the most complex hydrocarburets, such as petroleum, schist, and

page_text: others are separated in a single operation, so as to obtain direct, without
increase of cost, either pure hydrocarburets or pure derivatives therefrom,
aniline being derived from benzine and toluidine from toluine, which are
pure products hitherto unknown in commerce.
Secondly, I claim the application of a rectifying column, such as that
herein-before described, or any analogous thereto, for effecting the separation
of hydrocarburets, as herein described.
In witness whereof, I, the said William Clark, have hereunto set
my hand and seal, this First day of December, in the year of our
Lord One thousand eight hundred and sixty-three.
Witness,
W. G. E. SWINNOCK,
53, Chancery Lane,
London.
W. CLARK. (L.S.)