Process and Apparatus for the Production of Fuming Sulphuric Acid, or of Sulphuric Anhydride from the Acid Waste or Residual Matter Obtained in the Petroleum, Paraffin, and Tar Industry.
Year: 1889

page_text: Date of Application, 29th July, 1889
Complete Specification Left, 28th Apr., 1890-Accepted, 31st May, 1890
PROVISIONAL SPECIFICATION.
Process and Apparatus for the Production of Fuming Sulphuric
Acid, or of Sulphuric Anhydride from the Acid Waste or
Residual Matter Obtained in the Petroleum, Paraffin, and Tar
Industry.
I, JOHANN DAVID STARCK, Manufacturing Chemist, of Tschemin, Bohemia, in the
Austro-Hungarian Empire, do hereby declare the nature of this invention to be as
follows:-
:
My process for obtaining fuming sulphuric acid or sulphuric anhydride from the
dark-coloured and impure sulphuric acid which constitutes a bye-product in the
refining of petroleum, paraffin and similar bodies, comprises the following
steps:-
The acid waste is heated to a temperature of from 125° to 250° C., thereby forming
sulphurous acid and water. The sulphurous acid thus obtained is converted into
sulphuric acid by means of the atmospheric oxygen and by the aid of a suitable
catalytic or .contact substance.
For the uniform development of sulphurous acid, I employ a specially constructed
apparatus. It chiefly consists of a cast-iron, tube or retort of about 30% diameter,
and 125 % length, mounted in a furnace in such a manner that the discharge end
of the tube is about 20% higher than the inlet and that the flames may circulate
freely around the retort.
The liquid is admitted through an iron funnel situated at such a height that the
column of liquid in the feed pipe will approximately balance the pressure in the
retort.
The acid waste admitted through the feed pipe is decomposed, and leaves a coke-
like residue which is constantly removed by an endless screw, and falls at the
discharge end into a closed tank of sheet metal, from which it is removed at regular
intervals of time.
The quantity of waste acid admitted through the feed pipe is regulated by means
of a valve and depends on the nature or origin of the acid. As an average, it amounts
to about 30 kilogrammes per hour.
The gases developed in the retort are conducted by lead pipes through a cooler
into a tank in which the products of condensation (water and hydrocarbon) accumulate
This tank is provided with a water gauge and two discharge cocks, one of which is
situated near the bottom and serves for the water of condensation, while the other,
situated at about two thirds of the height of the tank, serves for drawing off the
hydrocarbon floating on the water.
Air
The sulphurous acid thus separated, is now completely relieved of water in a tower
similar to a Glover's tower, and by means of sulphuric acid of about 60° Beaumé.
In a second tower. similar to the first, the air necessary for the reaction is dried.
and sulphurous acid are now forced by pumps into a mixing cylinder after which the
mixed gases are conducted over the contact substance. The pumps are so constructed.
as to maintain the necessary ratio between the quantity of air and the quantity of
sulphurous acid gas; (about 36 parts of gas to 100 parts of air).
The contact substance, situated in a cast-iron pipe or a canal, is heated to incipient
red heat, and maintained at this temperature by means of a furnace.
The contact substance consists preferably of platinised asbestos or platinised pumice-
stone, or of metallic oxides precipitated upon porous bodies.
The gases coming out of the contact canal consist of sulphuric anhydride, the
nitrogen of the consumed air, besides atmospheric air and sulphurous acid which
have not taken part in the reaction, and a small quantity of carbonic acid.

page_text: The vapours of anhydride are condensed in suitable receivers, either by themselves
or in concentrated English sulphuric acid, and the gases containing sulphurous
acid are conducted into lead-chambers for their conversion into English sulphuric
acid.
000
FAIRFAX & WETTER,
433, Strand, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Process and Apparatus for the Production of Fuming Sulphuric
Acid, or of Sulphuric Anhydride from the Acid Waste or
Residual Matter Obtained in the Petroleum, Paraffin, and Tar
Industry.
I, JOHANN DAVID STARCK, Manufacturing Chemist, of Tschemin, Bohemia, in the
'Austro-Hungarian Empire, do hereby declare the nature of this invention and in what
manner the same is to be performed to be particularly described and ascertained in
and by the following statement:-.
My process for obtaining fuming sulphuric acid or sulphuric anhydride from the
dark coloured and impure sulphuric acid which constitutes a bye-product in the
refining of petroleum, paraffin and similar bodies, comprises the following steps:-
The acid waste is heated to a temperature of from 125° to 250° C. thereby forming
sulphurous acid and water. The sulphurous acid thus obtained is converted into
sulphuric acid by means of atmospheric oxygen and by the aid of a suitable contact
substance (also called catalytic body).
For the uniform development of sulphurous acid, I employ a specially constructed
apparatus illustrated by the accompanying drawings. It chiefly consists of a cast-
iron tube or retort r of about 30 diameter, and 125% length, mounted in a
furnace o in such a manner, that the discharge end of the tube is about 20 % higher
that the inlet and that the flames may circulate freely around the retort.
The liquid is admitted through an iron funnel t, situated at such a height, that
the column of liquid in the feed pipe will approximately balance the pressure in the
retort.
The acid waste admitted through the feed pipe undergoes decomposition and
leaves a coke-like residue which is constantly removed by an endless screw and falls
at the discharge end into a closed tank b of sheet-metal, from which it is removed at
regular intervals of time.
The quantity of waste acid admitted through the feed pipe is regulated by means of
a valve and depends on the nature or origin of the acid. As an average, it amounts
to about 30 kilogrammes per hour.
The gases developed in the retort are conducted by lead pipes through a cooler k
into a tanka, in which the products of condensation (water and hydrocarbon)
accumulate. This tank is provided with a water gauge and two discharge cocks,
one of which, h, is situated near the bottom and serves for the water of condensation,
while the other, h¹, situated at about two thirds of the height of the tank, serves for
drawing off the hydrocarbon floating on the water.
Air
The sulphurous acid thus separated, is now completely relieved of water in a tower g
similar to a Glover's tower, and by means of sulphuric acid of about 60° Beaumé. In
a second tower, similar to the first, the air necessary for the reaction is dried.
and sulphurous acid are now forced by pumps into a mixing cylinder, after which
the mixed gases are conducted over the contact substance. The pumps are so
constructed, as to maintain the necessary ratio between the quantity of air and the
quantity of sulphurous acid gas; (about 36 parts of gas to 100 parts of air.
The contact substance, situated in a cast-iron pipe d or in a canal, is heated to
incipient red heat, and maintained at this temperature by means of a furnace o¹, in
which the temperature can be exactly regulated.

page_text: The contact substance consists preferably of platinised asbestos or platinised pumice-
stone, or of metallic oxides precipitated upon porous bodies.
The gases coming out of the contact canal consists of sulphuric anhydride, the
nitrogen of the consumed air, besides atmospheric air and sulphurous acid which have
not taken part in the reaction, and a small quantity of carbonic acid.
The vapours of anhydride are condensed in suitable receivers a', either by
themselves or in concentrated English sulphuric acid, and the gases containing
sulphurous acid are conducted into leaden chambers for their conversion into English
sulphuric acid.
The quantity of sulphuric anhydride obtained depends on the nature or origin of the
raw material and reaches in the average about 40
per cent.
Having now particularly described and ascertained the nature of my said
invention, and in what manner the same is to be performed I declare that what
I claim is:-
1. The process for obtaining sulphuric anhydride or fuming sulphuric acid from
the acid waste or residual matter produced in the petroleum, paraffin, and tar
industry, which consists in decomposing the said raw material by heat (at a
temperature of 125 to 250°) relieving the sulphurous acid thus generated, from
condensable vapours, by cooling, mixing the said acid with air in the ratio of
36 to 100, conducting the mixture of these gases over a catalytic substance (con-
sisting of finely divided platinum or metallic oxides) and condensing the sulphuric
anhydride formed by the operation, substantially as described.
2. The apparatus for the generation of sulphurous acid, comprising in its
construction, an inclined piper provided with a screw conveyor and heating
apparatus,a feeding appliance te for supplying a controllable quantity of raw material
under pressure, a closed trough b, a cooler and a receiver a, substantially as
described.
3. The apparatus for producing sulphuric anhydride comprising in its construction
a pair of towers g, pumps p. mixing cylinders c, contact canal d provided with heating
apparatus, and receiver a, substantially as described.
Dotad this 28th day of April 1890
JOHANN DAVID STARCK.
By Fairfax & Wetter,
433, Strand, London, Agents.