IMPROVEMENTS IN THE MANUFACTURE OF LIQUID HYDRO-CARBONS AND PARAFINE
Year: 1853

page_text: LETTERS PATENT to Paul Wagenmann, of Bonn, Rhenish Prussia,
for the Invention of "IMPROVEMENTS IN THE MANUFACTURE OF LIQUID
HYDRO-CARBONS AND PARAFINE."
Sealed the 18th March 1854, and dated the 20th December 1853.
PROVISIONAL SPECIFICATION left by the said Paul Wagenmann
at the Office of the Commissioners of Patents, with his Petition,
on the 20th December 1853.
I, PAUL WAGENMANN, of Bonn, Rhenish Prussia, do hereby declare
the nature of my said Invention for "IMPROVEMENTS IN THE MANUFACTURE
OF LIQUID HYDRO-CARBONS AND PARAFINE" to be as follows:-
My improvements consists in breaking the coals or bituminous slate
in pieces of about the size of a walnut, and if they are very sulphurous
1 sprinkle them with lime water. They are then taken to a drying
furnace of the following construction:-1 space, by preference of two
hundred feet in length and twenty feet in width, is intersected by walls
of two feet high; at the distance of every four feet these walls are bound

page_text: together by arches of one brick thick, and on these arches the coals or
bituminous slate are spread.
The space below the arches is filled up with the residue from the
retorts.
The coals or bituminous slate when dried is distilled in retorts, which
are in so far different from those used at the gas works that the pipes
for letting out the produce of distillation are on the opposite ends to
those where the doors are. Over each fire are two retorts, each by
preference of about eight feet long and two feet wide, with an opening
of five inches to let out the produce of distillation. The fire runs below
the retorts in a direction from front to back, the fire bars only extending
part of the
way. I prefer to arrange a stack consisting of eight fires
and sixteen retorts around one chimney, by which means I am enabled
to lead the flame from one fire to the others, and by that means to heat
the retorts by a graduated heat.
The produce of distillation of the sixteen retorts meet together in one
iron pipe about eighty feet long and two feet diameter, which is sur-
rounded by another, so that cold water can run between the two pipes
for cooling. The gases, after having passed this pipe, enter in two
cylinders about twelve feet in height and four feet in diameter. These
cylinders are filled with iron wire chips. The gases, after having passed
the cylinders, pass through another iron pipe forty feet high into the
air, which pipe to regulate the draft is furnished with a regulator.
It is important that the produce of distillation should not be con-
ducted so as to produce pressure in the retorts.
The produce of distillation runs into a general reservoir, and the
reservoir is so arranged that the condensed productions will have an
average heat of 30° centegrade. The oils separate themselves here
from the ammoniacal water. The ammoniacal water is thrown over the
cooled residue of the drying furnaces and mixed with it, which produces
a very good manure. The tar, after being separated from ammonia, is
distilled, and the product of distillation is cooled by the means of a lead
pipe standing in a cooling apparatus, the water for cooling being kept
always lukewarm. The product of distillation is divided into three
qualities:-

page_text: No. I., from the beginning of the distillation to 0.865, specific
gravity.
No. II., from 0.865-0-900, specific gravity.
No. III., 0.900 1.930, specific gravity.
"
The produce No. I. is mixed with sulphuric acid and hydrochloric
acid at a temperature of 25° centegrade. Three hours afterwards the
oil is taken off and washed with a solution of caustic soda at 60°
centegrade; it is left two hours, and then separated from the solution
and distilled. In tho still is mixed a concentrated solution of soda.
After the distillation the oils are light yellow, and give an average weight
of 0-815-0-825, specific gravity. To correct the smell I wash the oils
again with sulphuric acid and hydrochloric acid, separate them from
the solution, and wash with concentrated solution of soda.
The oil No. II. is treated the same as No. I., but with different
quantities of acids, and at a temperature of 35° centegrade. The pro-
duct after the distillation is a lighter oil.
The oil No. III. is the product for the preparation of the finest oil
and parafine candles. This oil is treated with sulphuric acid and hydro-
chloric acid at a temperature of 33° centegrade, and allowed to stand;
it is then separated from the acids and washed with a solution of soda
at a temperature of 60° centegrade, and distilled.
The oil contains parafine, and is taken to a cool cellar at an average
temperature of 12° centegrade, where it remains in iron butts for eight
days. After this time the parafine is separated from the oil by means
of a centrifugal machine, and cast in cakes, and pressed in a cold
hydraulic press; afterwards melted and mixed with sulphuric acid, then
separated and washed in water; it is then heated and cast in cakes, and
again pressed by a heated press; afterwards again melted and mixed
with sulphuric at a temperature of 70° centegrade; the acid is drawn
off, and the parafine is washed in water, after this it is melted with
stearine.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Paul Wagenmann in the Great Seal Patent Office
on the 20th June 1854.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I,
PAUL WAGENMANN, of Bonn, Rhenish Prussia, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twentieth day of December, in the
year of our Lord One thousand eight hundred and fifty-three, in
the seventeenth year of Her reign, did, for Herself, Iar heirs and
successors, give and grant unto me, the said Paul Wagenmann, Her
special licence that I, the said Paul Wagenmann, my executors, admi-
nistrators, and assigns, or such others as I, the said Paul Wagenmann,
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 MANUFACTURE OF LIQUID HYDRO-CARBONS AND
PARAFINE," upon the condition (amongst others) that I, the said Paul
Wagenmann, by an instrument in writing under my hand and scal,
should particularly describe and ascertain the nature of the said Inven-
tion, 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 Paul Wageumann, do hereby de-
clare 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 following statement thereof (that is to say):
My improvements consist in breaking the coals or bituminous slate
in pieces of about the size of a walnut, and if they are very sulphurous
I sprinkle them with lime water. They are then taken to a drying
furnace of the following construction:-A space, by preference of two
hundred feet in length and twenty feet in width, is intersected by walls

page_text: of two feet high; at the distance of every four feet these walls are
bound together by arches of one brick thick, and on these arches
the coals or bituminous slate are spread. The space below the archics is
filled up with the residue from the retorts. The coals or bituminous
slate when dried is distilled in retorts, which are in so far different from
those used at the gas works that the pipes for letting out the produce
of distillation are on the opposite ends to those where the fire doors
are. Over each fire are two retorts, each by preference of about eight
feet long and two feet wide, with an opening of five inches to let out
the produce of distillation. The fire runs below the retorts in a direċ-'
tion from front to back, the fire bars only extending part of the way. I
prefer to arrange a furnace consisting of eight fires and sixteen retorts
around one chimney, by which means I am enabled to lead the flame
from one fire to the others, and by that means to heat the retorts by a
graduated heat. The produce of distillation of the sixteen retorts meet
together in one iron pipe about eighty feet long and two feet diameter,
which is surrounded by another, so that cold water can run between
the two pipes for cooling. The gases, after having passed this pipe,
enter into two cylinders about twelve feet in height and four feet in
diameter. These cylinders are filled with iron wiro chips. The gases,
after having passed the cylinders, pass through another iron pipe forty.
feet high into the air, which pipe to regulate the draft is furnished with
a regulator.
It is important that the produce of distillation should not be
conducted so as to produce pressure in the retorts. The produce of
distillation run into a general reservoir, and the reservoir is so arranged
that the condensed productions will have an average heat of 30°
centegrade. The oils separate themselves here from the amnioniacal
water. The ammoniacal water is thrown over the cooled residue of
the drying furnaces and mixed with it, which produces a very good
manure.
'
Having thus stated the nature of my said Invention, I will proceed
to describe the manner of performing the same.
.

page_text: DESCRIPTION OF THE DRAWINGS.
Figure 1. shows an arrangement of eight fires or furnaces com-
municating with a central chimney. Each fire or furnace has two
retorts over it as indicated by dotted lines, and there are openings and
slides or dampers, by which the neighbouring fires or furnaces may be
allowed to communicate with or be shut off from each other. Figure 2
shows a vertical section; Figure 3 shows a transverse section, taken
through one of the fire-places and its two retorts; Figure 4 shows a
longitudinal section of one of the fire-places and through one of the
retorts heated thereby; Figure 5 shows an external view of part of
the elevation of the several fire-places and retorts; and Figure 6 shows
a vertical and horizontal section of the chimney in the retorts.
I would state, that although I prefer the combined arrangement of
retorts shown, and the same forms part of my Invention, I do not in
respect to that part of my Invention which relates to the collection
and treatment of the products, confine myself to the use of such an
apparatus, as products obtained from other arrangements of retorts
may be treated according to the means herein-described as forming
another part of my Invention. The arranging of a succession of
retorts around the same chimney as shewn by the Drawings, offers
considerable facility in working, as the heat of one furnace, when no
longer required to act on its own retorts with the degree of force
previously offered, may be turned into the next fire-place, and thus
gradually bring up the heat of the retorts over that fire.
The heat is conducted from one furnace to another by means of two
flues, one of which communicates directly with the chimney and the
other with the following furnaces, so that when the first is opened and
the other closed, the fire passes immediately into the next furnace. For
instance, supposing the fire to be in No. 1, when the flues Nos. 1 to 7,
leading to the chimney, are closed, and those leading to the other
furnaces are opened, and flue No. 8, leading to No. 1 furnace shut,
and flue No. 8, leading to the chimney opened, the heat passes through
the furnaces Nos. 1, 2, 3, 4, 5, 6, 7, and 8, before it reaches the
chimney. But during this process the ashpit door of No. I must

page_text: remain open, and those of Nos. 2 to 8 closed, and the grate doors of
Nos. 2 to 8 must also remain closed. The distilling process of the
bituminous matter commences at a temperature of about one hundred
degrees centegrade, and is increased during a period of from six to
eight hours to a moderate red heat, at which it ceases.
The products which are distilled off are conducted away from the
back ends of the retorts, and the several retorts are connected to one
receiving pipe of about two feet diameter, and the products of about
100 lbs. to 150 lbs. of the dried bituminous matter are distilled over
by a retort in about six or eight hours, and the receiving pipo above
mentioned is surrounded by a larger one into and through which
cold water is run. The gases passing from this pipe as beforo ex-
plained, enter two cylinders filled with wire chips; the gases then pass
through another pipe about forty feet high into the air, the draft in
which is regulated by a regulator or valve. The condensed products
of distillation collected as above explained in a common reservoir, where
they are allowed to settle and separate from the ammoniacal water,
which is removed and thrown over the ashes or spent products (for
the production of manure) from the retorts after they have given off
their heat to the materials on the arches before explained, where the
ashes when hot from the retorts are thrown and there remain till cooled
down. The tar thus obtained is mixed in iron vessels for one hour,
say in quantities of two hundred and fifty gallons with ten gallons of a
solution of sulphate of iron at a temperature of 28° to 30° centegrade,
and after three hours the oils are separated from the solution which
during that time has absorbed the hydro-sulphate of ammonia from the
tar. The tar is now placed in an iron boiler capable of containing three
hundred gallons, heated by an ordinary furnace, and connected with
another very strong steam boiler which is worked at a pressure of
eighty lbs. to the square inch, and from which a stream of steam one-
sixth of an inch in diameter is poured upon and into the tar and so
distils it.
The tar, after being separated from ammonia, is distilled, and
the product of distillation is cooled by the means of a lead pipe of
about one hundred feet long and four inches wide in a cooling appa-

page_text: ratus of seven feet high and three feet wide. On account of the hot
steam the water for cooling will become warm, and must, therefore, be
continually replaced by other cold water, but in such manner that the
water remains always lukewarm. The product of distillation is divided
into three qualities:--
No. I., from the beginning of the distillation till it comes to 0.865,
specific gravity.
No. II., from 0.865 to 0-900, specific gravity.
No. III., from 0.900 to 1-930, specific gravity.
The product No. I. is mixed up for half an hour with about seven
per cent. sulphuric acid, and two per cent. of hydrochloric acid, and in
mixing machines of lead at a temperature of twenty-five degrees cen-
tegrade. Three hours afterwards the oil is taken off and washed with
a solution of caustic soda at a temperature of sixty degrees centegrade;
it is left two hours, and then separated from the solution, and distilled
in a similar vessel to that before used in the distillation of the tar. In
the still is mixed two per cent. of concentrated solution of soda. After
the distillation the oils are light yellow, and give an average weight
of 0.815-0.825, specific gravity. These oils are known in the trade
under the name of "photogine," or "mineral oil." To correct the smell,
I wash the oils again with two per cent. of sulphuric acid of sixty
degrees Beaumé, and half per cent. of hydrochloric acid, separate them
from the above acids, and wash them with one per cent. concentrated
solution of caustic soda.
The oils No. II. are treated in the same manner as the oils No. I.,
but with the addition of one per cent. sulphuric acid and half per cent.
of hydrochloric acid, at a temperature of thirty-five degrees centegrade.
The distilled produce from the commencement of the process until it
has reached a specific gravity equal to 0-865, is added as a lighter oil
to No. I; the second part of the produce which commences with a
specific gravity of 0.865, and cease at that of 0.890, gives an oil of
from 0-870 to 0-880 specific gravity, and which comes into the trade
under the name of heavy mineral oils.
The produce, the specific gravity of which is above 0-890, is the oil
No. III., from which is prepared the finest oil and the parafine candles.

page_text: This oil is treated with six per cent. of sulphuric acid, and half per
cent. of hydrochloric acid, at a temperature of thirty-three degrees:
centegrade, and allowed to stand two or three hours. It is then
separated from the acids and washed with a solution of caustic soda
of four degrees Beaumé, at a temperature of sixty degrees centegrade,
and distilled.
The oil commences to distil at a specific gravity of 0.720, and
being quite fine at 0-780, is used for cleaning clothes and washing
gloves.
The oils ranging between 0-780-0-865, are classified under the
raw oils No. I., for another rectification with them. The oils from
0-865-0-900 are classified under the raw oils No. II., to be refined
with them. The other oil contains parafine, and is taken to a cool
cellar at an average temperature of twelve degrees centegrade, where
it remains in iron butts for about eight days. After this time the
parafine is separated from the oil by means of a centrifugal machine,
and cast in cakes and pressed in a cold hydraulic press; afterwards
melted and mixed half an hour, at a temperature of eighty degrees
centegrade, with fifty per cent. sulphuric acid; two hours afterwards the
acid is taken away, then separated, and washed in water; it is then
hented and cast in cakes. It is then taken again to a hydraulic press,
which is heated by means of steam, and pressed warm between hair
cloths; afterwards again melted and mixed with 150 per cent. of
sulphuric acid for half an hour at a temperature of seventy degrees
centegrade; two hours afterwards the acid is drawn off, and the
parafine is washed in water. After this it is melted with half per cent.
of stearine and mixed with a solution of one per cent. of caustic potash
of forty degrees Beaumé, and after two hours the remaining impurities
have mixed with the stearine and the caustic potash, and are drawn
off. It is then boiled with a strong solution of oxalic acid of five.
degrees Beaumé, with the addition of one and a half per cent. of
stearine, and when clear is cast in cold forms or candle moulds at a
temperature of ninety-five-degrees centegrade. Where acids are used,
the vessels employed are made of lead, and where alkalis are used,
they are made of iron. Except in the cases mentioned, all the

page_text: sulphuric acids used by me are mixed with half per cent. hydrochloric
acid, and possess a specific gravity of sixty-six degrees Beaumé.
In witness whereof, I, the said Paul Wagenmann, have hereunto
set my hand and seal, this Seventeenth day of June, in the year
of our Lord One thousand eight hundred and fifty-four.
PAUL WAGENMANN. (L.S.)
Witness,
GEORGE W. HODGSKIN,
of Ederschlag, in Rhenish Prussia, and
15°, St. Helen's Place, London.