IMPROVEMENTS IN TREATING PRODUCTS ARISING FROM THE DISTILLATION OF A CERTAIN TAR OR NAPTHA, TO RENDER THE SAME SUITABLE FOR DISSOLVING OR REMOVING FATTY OR RESINOUS SUBSTANCES
Year: 1854

page_text: LETTERS PATENT to Warren De la Rue, of Bunhill Row, in the County
of Middlesex, Manufacturer, for the Invention of "IMPROVEMENTS IN
TREATING PRODUCTS ARISING FROM THE DISTILLATION OF A CERTAIN TAR OR
NAPTHA, TO RENDER THE SAME SUITABLE FOR DISSOLVING OR REMOVING FATTY
OR RESINOUS SUBSTANCES."
Scaled the 17th April 1855, and dated the 23rd December 1854.
PROVISIONAL SPECIFICATION left by the said Warren De la Rue al
the Office of the Commissiouers of Patents, with his Petition, on the
23rd December 1854.
1, WARREN DE LA RUE, of Bunhill Row, in the County of Middlesex,
Manufacturer, do hereby declare the nature of the Invention for "IMPROVE.
MENTS IN TREATING PRODUCTS ARISING FROM THE DISTILLATION OF A CERTAIN TAR
OR NAPTHA. TO RENDER THE SAME SUITABLE FOR DISSOLVING OR REMOVING FATTY OR
RESINOUS SUBSTANCES," to be as follows:-
The object of my Invention is the preparation of certain very volatile and
nearly odourless products from Rangoon tar, otherwise called Burmese naptha,
or petroleum, in order to render them applicable to the purposes of dissolving
resinous or fatty bodies, or removing greasy or resinous stains from leather,
woollen, silk, cotton, or linen fabrics, household furniture, gloves, and other
habiliments.
For this object, I first submit the native tar, called Rangoon tar, Burmese
naptha, or petroleum, to processes of distillation, as described by me in former
Patents; 1 then take those distillates, boiling below two hundred and twelve

page_text: degrees, and up to four hundred and fifty degrees Fahrenheit, and then sepa-
rately mix them very gradually with either one-fourth of their bulk of fuming
nitric acid, of specific gravity 15, or with one-third of their bulk of a mixture
of nitric and strong sulphuric acids. After the whole of the acid has been
added, and well mixed therewithin glass or stone vessels, cooled by the external
application of cold water, I leave the fluids in contact for some days, and then
separate the acid and the nitro compounds, formed from the supernatent
hydro-carbons, which, however, still contain acid vapours.
The supernatent hydro-carbons are now washed with a weak solution of
carbonate of soda, or other alkaline ley, and submitted to fractional distillation,
and the washing repeated on the separate distillates. Lastly, the distillates
are dried by contact with dry chloride of calcium (muriate of lime), or other
suitable water-absorbing substances, and kept according to the range of tem-
perature between which they boil. The liquid thus obtained boil from one
hundred and forty degrees Fahrenheit upwards.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Warren De la Rue in the Great Seal Patent Office on
the 22nd June 1855.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, WARREN
DE LA RUE, of Bunhill Row, in the County of Middlesex, Manufacturer,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Pateut, bearing date the Twenty-third day of December, in the year of our
Lord One thousand eight hundred and fifty-four, in the eighteenth year of
Her reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said Warren De la Rue, Her special license that I, the said Warren
De la Rue, my executors, administrators, and assigns, or such others as
1, the said Warren De la Rue, 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 "IM-
PROVEMENTS IN TREATING PRODUCTS ARISING FROM THE DISTILLATION OF A CERTAIN
TAR OR NAPTHA, TO RENDER THE SAME SUITABLE FOR DISSOLVING OR REMOVING
FATTY OR RESINOUS SUBSTANCES," upon the condition (amongst others) that
I, the said Warren De la Rue, by an instrument in writing under my

page_text: 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 Warren De la Rue, do hereby declare
the nature of the said Invention, and in what inanner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement thereof (that is to say):-
The object of my Invention is the preparation of certain very volatile and
nearly odourless products from Rangoon tar, otherwise called Burmese naptha,
or petroleum, in order to render them applicable to the purposes of dissolving
resinous or fatty bodies, or removing greasy or resinous stains from leather
woollen, silk, cotton, or linen fabrics.
In a former Patent I mentioned the difficulty of separating by distillation
the various hydro-carbons which are obtained from Burmese naptha,and I also
mentioned that they might be further purified by treatment withsulphuric acid,
by washing, and by re-distillation; in that case, however, the portion of the
hydro-carbon dissolved by the sulphuric acid was not again made usefully
available; on the other hand, by the substitution of nitric, or a mixture
of nitric and sulphuric acids, for sulphuric acid alone, compounds are ob-
tained which may be employed in perfumery; and it is on this account that I
give preference to the employment of nitric acid, or a mixture of nitric and
sulphuric acids, to sulphuric acid alone.
Nitric acid or nitro-sulphuric acid is not of the same value in the puri-
fication of those hydro-carbons obtained from Burmese naptha which boil
much above 400° Fahrenheit, as the nitro compounds obtained from such have
not an agreeable odour, and are, moreover, with difficulty purified, on account
of their resinous consistence, and their liability to change, whereas nitro com-
pounds, obtained from the hydro-carbons boiling below 400° Fahrenheit, are
fluid or crystalline, and less liable to decomposition. Rangoon tar, Burmesc
naptha, or petroleum, is extensively obtained in the Burmese territory, and is
well known in commerce in India, and when submitted to distillation it yields
fluid and solid products, varying in their volatility. By preference I choose
those hydro-carbons obtained according to the processes described by me in
the Specification of my first Patent, by rectification by means of steam, which
may be distilled without leaving any considerable residue, boiling above 400°
Fahrenheit, for example, not more than a fourth of such high boiling residne.
The varous hydro-carbons from Burmese naptha consist essentially of two
distinct classes, the one class,constituting the chief part, not being acted upon;

page_text: or only with great difficulty acted upon, by strong sulphuric, strong uitric, or
strong nitro-sulphuricacids, and another class readily acted upon by these acids.
The object of this Patent is to separate these two classes, and to render them
or their products usefully available.
Having selected the various products of distillation, and classed them in
groups, not varying more than about 20° Fahrenheit in the volatility of their
chief portion, I carefully mix them separately with, by preference, one-fourth
of their bulk of nitric acid, specific gravity 15, in stoneware or glass vessels,
cooled by the external application of cold water. These vessels should expose
a very large cooling surface, in proportion to their cubical contents. After
agitating the mixture for about six or eight hours, I allow it to remain at rest
for about four hours, and then separate by decantation the supernatant hydro.
carbons from the nitro compounds and the acid.
Having transferred the hydro-carbons, into a suitable closed vessel, I agitate
them with a fourth of their bulk, of a solution of carbonate of soda, consisting
of one part of a cold saturated solution of carbonate of soda and eight parts of
cold water, and thus I remove any free nitric or nitrous acids; the hydro-carbons
still retain nitrous compounds, which I remove after the hydro-carbons have
been decanted from the alkaline carbonate, by agitating them with a saturated
cold solution of copperas (proto-sulphate of iron). The hydro-carbons are next
well washed by agitation with cold water, and carefully distilled several times
by means of a slow current of steam of about 212° Fahrenheit passing through
them; or, by preference, by their being placed in a still with water, and dis-
tilled from its surface by the external application of heat. By repeating this,
operation as often as may be necessary, generally two or three times, the
hydro-carbons are obtained nearly free from a portion of nitro compounds, which
they hold in solution, and which usually fall to the bottom of the water in the
still, when the hydro carbons are carefully driven off by heat from the surface
of water. The distillates are lastly dried, and still further purified, by being
allowed to stand for several days in well-closed vessels, with about a quarter of
their weight of quick lime, or other suitable dryer, in lumps of about the size
of a hazel nut, and after dessication, and removal from the lime by distillation
in retorts or stills, furnished with thermometers, by means of which the
distillates, as they are distilled over, are to be classified according to their
volatility. I have ascertained by analysis that the per-centage composit on of
the various hydro-carbons thus purified is nearly the same, that is to say, thev
are composed of nearly the same relative weights of carbon and hydrogen
throughout along range of boiling points; but for the purposes of dissolving or
removing fatty and resinous substances, I prefer to take such as boil from 1409

page_text: to 300° Fahrenheit, and I am careful to collect the distillates between limits
of not more than 10° Fahrenheit. To render the nitro compounds obtained
by the action of nitric acid sufficiently pure to be used in perfumery, I add
that portion just described, which has been left as a residue in distilling the
hydro-carbon from the surface of water to the nitric acid, and thesupernatant
nitro compounds from which the hydro-carbon was originally decanted; Itheu
separate the nitric acid from the nitro compounds by means of a glass vessel,
furnished with a glass stop-cock, and then mix the nitric acid with three or
four times its bulk of water, by which means a considerable portion more of
the nitro compounds are separated, and fall to the bottom of the liquid. The
nitro compounds still retain some of the hydro-carbons, from which I separate
them by distilling off the hydro-carbons in a retort containing water; the nitro
compounds when nearly free from hydro-carbons sink to the bottom of the
water in the retort. These nitro compounds I further purify by washing them
with water, and separate the fluid portion, by the external application of ice
and filtration,from any crystals ofnitro compounds resulting from the prolonged
action of nitric acid.
Having described the nature of my Invention, and the best means of
carrying it out, I would remark that I do not confine myself strictly to the
details or the proportions given, as both may be varied; nor do I claim the
processes, except as applied to the oils or hydro-carbons obtained from
the substance known as Rangoon tar, Burmese naptha, or petroleum; but
what I do claim is, the preparation from Rangoon tar, Burmese naptha, or
petroleum, by means of nitric acid, or a mixture of nitric and sulphuric
acids, and the processes described, firstly, useful solvent or detergent fluids;
and, secondly, of nitro compounds useful in perfumery.
In witness whereof, 1, the said Warren De la Rue, have hereunto set
my hand and seal, this Twenty-first day of June, in the year of our
Lord One thousand eight hundred and fifty-five.
Witness,
JONAH NATHAN,
110, Bunhill Row, London.
WARREN DE LA RUE. (L.S.)