Improvements in the Process of Preparing Benzol and its Homo- logues, Naphthaline, and Anthracene from Petroleum, Petroleum Scales, Tar, Tar Oils, Paraffin, Vaseline, Ozokerite, and the like, and from Natural Illuminating Gas.
Year: 1890

page_text: Date of Application, 11th Feb., 1890
Complete Specification Left, 10th Nov., 1890-Accepted, 11th Feb., 1891
PROVISIONAL SPECIFICATION.
Improvements in the Process of Preparing Benzol and its Homo-
logues, Naphthaline, and Anthracene from Petroleum,
Petroleum Scales, Tar, Tar Oils, Paraffin, Vaseline, Ozokerite,
and the like, and from Natural Illuminating Gas.
We, FAUSTIN HLAWATY, of 3, Gartengasse, Vienna, Engineer, and Dr. EZECHIEL
FRIEDMANN, of 18a, Schönbrunnerstrasse, Fünfhaus, near Vienna, Lawyer, both in
the Austrian Empire, do hereby declare the nature of this invention to be as
follows:-
This invention relates to the process of making benzol and its homologues and
napthaline and anthracene from natural hydrocarbons and it has for its object so
to treat petroleum, residues of petroleum refineries, coal-tar, brown coal-tar, shale
tar, the oils of these tars, paraffine, ceresine, vaseline, ozokerite and the like, and
natural illuminating gas as to extract from these materials the greatest. possible
quantity of the said aromatic compounds.
According to this invention, any one or any mixture of the aforesaid liquid or
solid hydrocarbons is put into a closed vessel or retort, communicating with a
system of pipes and a condenser. The retort is so heated that a pressure of from
to atmosphere is maintained inside the same, and the liquid produced by
condensation taking place in the portion of the piping near the retort, is caused to
flow down through branch pipes to red hot pipes, by passing through which the
said liquid is again vapourized: The vapours coming directly from the retort and
those produced in the red-hot pipes unite on their way to the refrigerator, but
before entering the same, they are yet somewhat cooled and the liquid thus
condensed is conveyed back to the retort.
From the condensed liquid collecting in the refrigerator the benzol, its homo-
logues, the napthaline and the anthracene are separated in the well known way, and
to the residual liquid finely subdivided cellulose is added, such as saw-dust, dry
rotten wood, hay, straw, peat or the like. The whole is then brought into a retort,
which is heated to about 750° Fahrenheit and into which superheated steam of the
same temperature is caused to enter; the vapours thus enclosed are conveyed into
a suitable condenser.
The incondensible gases escaping from the condensers, in the first operation as
well as in the second one, and natural illuminating gas are converted into benzol
and homologues of benzol by passing them through red-hot pipes filled with pieces
of coke, pumice stone, or other suitable absolvent and communicating with a
condenser.
In the two first operations, distilling is carried on until the mass in the retort is
converted into coke, but in both cases, the apparatus may be worked continuously
by refilling the retort from time to time, until it becomes necessary to remove the
coke formed.
When treating the residues of the first distillate, a greater yield may be obtained
by using vapours of acetic acid, or of methyl or ethyl-alcohol instead of steam.
Dated this Eleventh day of February. 1890.

page_text: 0021 0
COMPLETE SPECIFICATION.
די
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Improvements in the Process of Preparing Benzol and its Homo-
logues, Naphthaline, and Anthracene from Petroleum,
Petroleum Scales, Tar; Tar Oils; Paraffin, Vaseline, Ozokerite,
and the like, and from Natural Illuminating Gas.
We, FAUSTIN HLAWATY, of 3, Gartengasse, Vienna, Engineer, and Dr. EZECHIEL
FRIEDMANN, of 18^, Schönbrunnerstrasse, Fünfhaus, near Vienna, Lawyer, both in
the Austrian Empire, 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 following statement :-
This invention relates to the "process of making benzol, tuluol, xylol, cumol,
naphthaline and anthracene from petroleum, residue from petroleum refineries, coal
tar, coal tar oil, shale tar, shale tar oil; brown coal tar, brown coal tar oil, paraffine,
ceresine and vaseline, ozokerite and the like and natural illuminating gas so as to
extract from these materials the greatest possible quantity of the said aromatic
compounds.
On the accompanying drawing
Figure 1 is a front view partly in section of an apparatus suitable for carrying
out the aforesaid process and
Figure 2 is a plan thereof.
According to this invention any one or any mixture of the aforesaid liquid or
solid hydrocarbons is put into a boiler 6 communicating above with a closed vessel
or retort c provided with pressure gauge c¹ and communicating with a system of
pipes d d and a condenser f. The boiler is heated quickly by means of a
furnace a in such manner that a pressure of 1 to 1 atmosphere above the ordinary
atmospheric pressure maintained inside the same.
The vapours produced are led through the aforesaid pipe system d in which the
less volatile products gradually condense and afterwards flow through red hot
pipes d' heated in any convenient manner while the more volatile products are
carried directly to the main condenser f.
By passing through the red-hot pipes d' the condensed less volatile products are
partly rendered into more volatile ones which also pass to the main condenser f
where they mix with the aforesaid volatile products which passed directly thereinto.
The so-obtained condensed liquid consists mostly of benzol tuluol xylol and cumol.
Before entering the main condenser all the vapours are subjected to a cooling
process (the means for which is not shown on the drawing) whereby all the less
volatile products are separated in order to be carried back to the retort.
By this process the apparatus may be worked continuously. For this purpose it
is only necessary to feed the retort gradually with tar or other material to be
treated. But it is necessary to interrupt the operation from time to time in order
to draw the cokes or final product out of the retort.
The not condensed gas which escape from the condenser are led through red
hot pipes filled with pieces of cokes pumice stone or other suitable neutral absorbent
material offering great surface and they thus also become converted into benzol,
tuluol, xylol and cumol and are collected in the condenser. It has not however
been thought necessary to show a separate apparatus for this purpose.
Natural illuminating gas is treated in the same manner for the purpose of
obtaining benzol, tuluol, xylol and cumol therefrom.
From the condensed liquid collecting in the condenser the benzol and other
aromatic products are separated in the well known way and to the residual liquid,
which consists of other hydrocarbons, is added about 10 to 20 per cent. of pulverized
cellulose in the form of moss, sawdust dry rotten wood, peat, broken coal, hay, straw
or the like together with some caustic alkali. The whole is enclosed in a retort g
which is heated by a furnace h and superheated steam at about 750 F. (400 C.) is..
caused to enter it by the pipe g¹ whereby a decided separation of the carbonaceous

page_text: compounds is effected.
The vapours thus evolved are passed through pipes i and
pipes i heated red hot in any convenient way and filled with small pieces of cokes or
iron filings and communicating with a condenser in. which the so-formed benzol,
tuluol, xylol and cumol are collected. In the liquid so obtained the naphthaline
and anthracene are contained in a dissolved condition, in the cooling of the liquid
these substances are thrown down. Instead of the aforesaid steam of 750° F. it is
advantageous to use vapours of acetic acid or of ethyl- or methyl- alcohol, whereby
about 40 per cent. of the liquid are converted into aromatic compounds of the kind
named.
Having now particularly described and ascertained the nature of our said inven.
tion and in what manner the same is to be performed, we declare that what we
claim is
First. The hereinbefore described process for obtaining benzol, tuluol, xylol,
cumol, naphthaline, and anthracene from petroleum, residue from petroleum
refineries, coal tar, coal tar oil, shale tar, shale tar oil, brown coal tar, brown coal
tar oil, paraffine, cèresine and vaseline, ozokerite and the like consisting in sub-
jecting such hydrocarbons to distillation while keeping a pressure of 1 to 1
atmosphere in the retort, passing the products, which condense before coming to
the condenser, through red hot pipes, passing the vapours produced in the latter
and those coming directly from the retort into the condenser, passing back to the
retort the products which condense just before coming to the condenser, and
separating the aromatic liquids from the distilled liquid substantially as set forth.
Second. The described process for obtaining benzol, tuluol, xylol, cumol
naphthaline and anthracene consisting in treating the residue remaining after
removal of the aromatic compounds produced as firstly claimed, by adding thereto
pulverized cellulose in the form of saw dust, peat, brown coal, moss, dry rotten
wood, straw hay or the like and a caustic alkali, and subjecting, the whole to
distillation steam from water being introduced or vapours of acetic acid or ethyl or
methyl-alcohol substantially as set forth.
Third. The process described for obtaining benzol, tuluol, xylol and cumol
consisting in treating the not condensed gases which escape from the condenser in
the processes firstly and secondly claimed, or treating natural lighting gas, the said
gases being passed through red hot pipes containing cokes, pumice stone or the like
and passing the products so obtained into a condenser substantially as set forth.
Dated this 10th day of November 1890,
Dated this 10th day of November 1890.
JENSEN & SON,
77, Chancery Lane, London, W.C., Patent Agents.