IMPROVEMENTS IN TREATING COAL TAR, DEAD OILS, AND FOR PRODUCING PHENIC OR CARBOLIC PROVISIONAL SPECIFICATION
Year: 1863

page_text: LETTERS PATENT to Jules Albert Schlumberger, of Golden Square, in
the County of Middlesex, Chemist, for the Invention of "IMPROVEMENTS
IN TREATING COAL TAR, DEAD OILS, AND FOR PRODUCING PHENIC OR CARBOLIC
PROVISIONAL SPECIFICATION left by the said Jules Albert Schlum-
berger at the Office of the Commissioners of Patents, with his Petition,
on the 18th February 1863.
I, JULES ALBERT SCHLUMBERGER, of Golden Square, in the County of
Middlesex, Chemist, do hereby declare the nature of the said Invention for
"IMPROVEMENTS IN TREATING COAL TAR, DEAD OILS, AND FOR PRODUCING PHENIC
OR CARBOLIC ACID," to be as follows:-
This Invention of "Improvements in Treating Coal Tar, Dead Oils, and for
Producing Phenic or Carbolic Acid," relates to a process of treating the heavy
oils obtained from coal tar with lime. There is great difficulty in obtaining
a satisfactory result from this process, unless the right proportions are taken to
produce a homogeneous compound of phenate of lime. It has, in fact, been
considered practically impossible to treat the heavy oils with lime in the same
that they are treated with caustic potash or soda, and for that reason it is
considered that the present Invention offers great economy over the old
process.

page_text: In carrying out the Invention I take the heavy oils afterthe naphthaline
has been settled, the specific gravity of which should be from 12° to 4° Cartier,
it being of great importance that it should be lighter than water. Arrange-
ments should also be made to deprive the benzine of all the heavier oils,
which would possess a density of from 12° to 14° Cartier after the deposition
of the naphthaline.
The proportions requisite would vary according to the quality of the heavy
oils, which differ enormously: These oils, which when freed from naphtha-
line indicate from 12° to 14° Cartier, contain the largest proportions of phenic
acid, the average proportions of phenic acid contained in these oils being from
to of its weight, as may be ascertained by a previous analysis. For the
sake of example, let us suppose a certain hydrocarbon to contain 25 per
cent. of phenic acid. The oils are transferred to an earthenware or iron
vessel or even wooden vessel provided with a tap in the lower part. For
each 100lbs. weight of oil take 6 to 7 lbs. of thoroughly slacked lime as
pure as possible. For each 2 lbs. of lime take 4 lbs. of water. This milk
of lime is poured into the oil, which is kept briskly stirred until the lime
is completely dissolved; it is then allowed to stand for from 2 to 3 days. The
phenate of lime separates as a heavy layer at the bottom of the vessel.
The oils become lighter still on account of the elimination of the phenic
acid, and remain in the upper part of the vessel. When the solution of
phenate of lime is perfectly liquid, which may be ascertained by drawing
samples from time to time from the lower cock, it is drawn off, and will
be found to contain no longer any trace of naphthaline or any other foreign
hydrocarbon. It is then transferred into another vessel, and saturated with
an acid by previously well-known methods. In distilling a second time,
crystallised phenic acid is certain to be the result after submitting the product
to simple refrigeration.
The novelty of this process, which constitutes the merit of the Invention,
consists in the separation of the greatest portion of the naphthaline from the oils,
and in producing after this elimination an oil lighter than water, which can
then be completely separated by difference of density from the resulting phenate
of lime. It is equally essential to employ a thin milk of lime, without which
the phenate of lime would thicken, and retain consequently certain portions of
naphthaline which had escaped crystallization.

page_text: SPECIFICATION in pursuance
of the conditions of the Letters Patent, filed
by the said. Jules Albert Schlumberger in the Great Seal Patent Office
on the 11th August. 1863.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JULES
ALBERT SCHLUMBERGER, of Golden Square, in the County of Middlesex, Chemist,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Thirteenth day of February, 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. Jules Albert Schlumberger, Her special licence that I,
the said Jules Albert Schlumberger, my executors, administrators,. and
assigns, or such others as I, the said Jules Albert Schlumberger, 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 TREATING COAL
TAB, DEAD OILS, AND FOR PRODUCING PHENIC OR CARBOLIC ACID," a communication
to me.from abroad by Jean Jaques Müller, of Bâle, Switzerland, upon the
condition (amongst others) that I, the said Jules Albert Schlumberger, 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 Jules Albert Schlumberger, do hereby
declare the nature of the said Invention, and in what manner the same is to
be performed, to be particularly described and ascertained in and by the fol-
lowing statement (that is to say):-
The object of this Invention, as communicated to me by my foreign corres-
pondent, is to effect an economy in the manufacture of phenic or carbolic acid
from dead oils or thick heavy oils obtained from coal tar. To this end it is
proposed to substitute lime for the potash or caustic soda, which has been
generally used for separating the said phenic acid from dead oils. The improved
mode of treating the dead oils for producing phenic acid is as follows:-The
dead oil is allowed to stand for a few weeks until the napthaline has become
separated by crystallisation. Of the oil thus prepared take one hundred kilo-

page_text: grammes, and mix therewith in a suitable vessel from about six to seven kilo-
grammes of milk of lime, the milk of lime being made in the proportion of two
kilogrammes of lime to fifteen kilogrammes of water. This mixture is to be kept
well stirred until the lime is quite dissolved, and it is then allowed to rest for
from two or three days. A phenate of lime is thus obtained, which, by reason
of its specific gravity settles at the bottom of the vessel, is then to be decanted
from the light oils. The solution of phenate of lime being clear is now placed
in a suitable vessel, and saturated by an acid in the way that is now generally
practised. It is preferred to use 'muriatic acid, which combines with the lime,
forming therewith a soluble salt. The phenic acid thus obtained, which is
easily separated from the muriate of lime by decantation, is distilled over for
purification. A second distillation will produce crystallized phenic acid. It
should be remarked that it is very important to use the dead oils as free as
possible from napthaline, and that for this reason the napthaline is removed, as
above explained, before applying the milk of lime.
Having now set forth the nature of the Invention of improvements in
treating coal tar dead oils, and for producing phenic or carbolic acid therefrom,
and explained the manner of carrying the same into effect, I wish it to be
understood that under the above in part recited Letters Patent, I claim manu-
facturing phenic or carbolic acid in the manner above described.
In witness whereof, I, the said Jules Albert Schlumberger, have hereunto
set my hand and seal, the Eighth day of August, in the year of
our Lord One thousand eight hundred and sixty-three.
JULES ALBERT SCHLUMBERGER. (L.8.)