A New or Improved Process for Enriching Pitch Obtained by the Evaporation of Tars Produced from Coal and in Apparatus therefor.
Year: 1887

page_text: Date of Application, 29th Aug., 1887
Complete Specification Left, 29th June, 1888
Complete Specification Accepted, 26th Oct., 1888
A New or Improved Process for Enriching Pitch Obtained by the
Evaporation of Tars Produced from Coal and in Apparatus
therefor.
I MODESTE LÉONARD HONNAY of Fleurus in the Kingdom of Belgium Gentleman
do hereby declare the nature of this invention is to be as follows:-
The object of my process is to furnish industrial means of utilizing more profitably
the agglutinative and inflammable qualities given to the pitches which I treat eithre
when the tars which produce the said agglomerating material are subjected to
insufficient evaporation or when to the said pitches is added one of the tars pro-
duced from coal or when to the said pitches is added a product richer than the said
pitches and produced from one of the tars obtained from coal which has been subjected
to evaporation. However small or considerable the evaporation may be or when to
the said pitches is added any non volatile oil from coal tar or when to the said pitches
are added several or all the products hereinafter enumerated which give quality to the
agglomerating material under treatment when they are added to these substances
which means I obtain by combatting through a special treatment and the softness
communicated to the said pitches by the different modes of preparing them.
My said process gives the means of treating by caloric and with the aid either
of sulphuric acid or nitric acid or hydrochloric acid or of several of the said acids
or of all the said acids the substances which I subject to my process.
The said process consists either in placing in contact any one of the pitches which
I can treat and which is produced from a tar which has not lost sufficient substance
by evaporation with one or other of the acids which I employ or with several of the
said acids or with all the said acids at a temperature at which the same produces
ebullition or in mixing so as not to produce ebullition if that be possible one or
other of the pitches which I have to prepare and which are produced from fars
which have not lost sufficient substance by evaporation with one or other of the
acids which I employ or with several of the said acids or with all the said acids and
then elevating the said agglomerating material to a temperature which produces

page_text: ebullition or in placing in contact by any suitable means any one of the pitches
which I may treat and one or other of the products or several of the products or
all the products hereinbefore described as capable of giving more quality to the
said pitches when they are added to the said substances with one or other of the
acids several acids or all the acids which I use and this at a temperature producing
ebullition or in mixing with one or other of my acids or several or all of my said
acids so as not to produce ebullition if that be possible either of the pitches which
I submit to my treatment or the matter or matters hereinbefore described as
enriching the pitches which I treat when they are added to the same and then
elevating by any suitable means the substances which are required to be associated
to a temperature producing ebullition or in mixing if it be possible so as not to
produce ebullition with one or other of the said acids or several of the said acids
or all the said acids which I employ any one of the pitches I wish to enrich and
the matter or matters herein before described as increasing the quality of such
agglomerating material when they are added to the same then in elevating by any
suitable means the substances to be associated to a degree of heat which produces
ebullition or in placing in contact by any suitable means with one or other of my
acids or several of my acids or all my acids at a temperature producing ebullition one
of the pitches which I treat by my process or the product or products herein before
described as enriching the said pitches when they are added to these substances then
in placing in presence by any suitable means the products which are to be associated
at a temperature which may be those temperatures from which the pitch is simply.
melted up to all those temperatures producing ebullition whatever be the considerable
evaporation produced thereby or in placing in contact with one or other of my acids
or several of my acids or all the said acids at a temperature producing ebullition by
any suitable means one or other of the pitches which I have to treat and the material
or materials hereinbefore described as capable of enriching the said pitches when they
are added to the said substances then as before mentioned placing in contact by any
suitable means the substances which are to be associated at a degree of heat which
may be that from which the pitches liquified up to any other degree of heat which
produces ebullition whatever may be the resulting considerable amount of matters
evolved.
My invention comprises also any application upon one or several closed vessels in
which my operations may be effected of any apparatus capable of operating the
condensation of hydrocarbons which brought by heat to state of vapour resume their
liquid state in cooling the said apparatus being placed on the said vessel or vessels so
as to collect the inflammable liquifiablo products which are given off during the
use of my process. The acids which I employ by preference are sulphuric acid
marking 66° Beaumé nitric acid marking 40° Beaumé and muriatic acid marking
22° Beaumé it is evident that I can utilize any other acid taking as a basis the
proportion of real acid of the product or products which I would substitute for those
hereinbefore mentioned.
Dated this Twentyninth day of August 1887.
W. T. WHITEMAN,
Agent for the Applicant.

page_text: therefor.
I, MODESTE LEONARD HONNAY of Fleurus, Belgium, Gentleman, 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 :-
The present invention consists in the treatment of substances with caloric and the
aid of sulphuric, nitric or hydrochloric acid or several or all of these acids and this
treatment is applied to pitch which is not sufficiently hard or brittle for the use to
which it is destined, by either enriching it with products which might be extracted
from the tar, or by adding the enriching substances which I use and which are the
following: The coal-tar from gasometers, the coal-tar from coke furnaces and
enriching products extracted from these coal-tars, especially the non-volatile oils of
these tars.
The caloric which I use for the treatment of the pitch can be that with which the
substance is impregnated during its manufacture or it may be part of this heat and
partly heat produced otherwise, or it may be wholly produced otherwise for the treat-
ment of pitch which was allowed to cool after manufacture.
If the treatment is to be applied to harden pitch which has not sufficiently lost
certain substances by evaporation, I ascertain the quantity of oil. contained in the
pitch.
If the treatment is to be applied to a pitch which must be enriched, the quantity of
oil contained therein is also ascertained and then in proportion are added the enriching
substances which are to be used.
The acids which are preferably used are: sulphuric acid of 66° Beaumé, nitric acid
of 40° Beaumé, and muriatic acid of 22° Beaume, and the following are the proportions
in which these acids are preferably used.
1. If the pitch is to be enriched by means of coal-tar from coke furnaces or of a
non-volatile oil from coal-tar, 10 per cent. of sulphuric acid or 14 per cent. of nitric
acid or 20 per cent. of muriatic acid, all by weight, are added to the enriching
substance.
2. If the pitch is to be enriched by means of coal-tar from gasometers, 12 per cent.
in weight of sulphuric acid is added to this coal-tar. The proportions of the other
acids are not given here as their use is not advantageous when coal-tar from gasometers
is used as the enriching substance.
Of all my modes of treatment that is preferable which refers to pitch which need
not be re-melted.
1. If a pitch produced from tar, which has not sufficiently lost by evaporation, is to
be treated with one or other of the above acids, or several or all of these acids,
at a temperature at which the mixing will produce boiling I preferably operate as
follows:
I use a vertical boiler with agitator, such as is used for distilling coal-tar and use in.
conjunction with this several special apparatus.

page_text: Fig. 1 of the accompanying drawings represents in section a distilling apparatus as
used for my process, when only one of the above acids is employed. A is the boiler,
B the brickwork or masonry around it, C the boiler furnace, c the door of the latter,
D the ash-pit, E the conduit connecting the furnace with the chimney E¹, E is the
register or damper of the chimney, F the agitator of the boiler, F¹ special wing
mechanism which I use with the agitator, G ordinary spiral tube of the boiler, G¹ tube
connecting the worm G with the distillation vat, G2 is the valve of G, H a special or
additional worm used with the boiler, H' the tube connecting this worm H with the
boiler, Hvalve of H', I is a glass reservoir for the acid to be employed, ¿ an earthen-
ware tube with valve, communicating with the boiler, K is a graduated scale on the
reservoir indicating the quantity of the acid contained in the reservoir, L is a tube
connected with an acid pump by means of which the reservoir is charged with the
quantity of acid to be used, the valve of the tube conducting the acid into the
reservoir, M. is a boiler arranged above the distillation vat and communicating with
this by means of the tube M provided with a valve M², N is a valve arranged on the 1
boiler M, P running off tube of the distillation boiler, P¹ valve of P, S hole with lid
or plug formed in the boiler, I cooling chamber for the treated pitch and R¹ door of
chamber R.
If with this apparatus several kinds of acid are used at the same time, a separate
acid pump is used for each acid and connected with the reservoir by a tube 2
similar to L.
The boiler for distillation is charged with a quantity of gasometer tar equal to a
quarter of its contents and when the substance to be treated is introduced therein I
assure myself that the valve of the ordinary worm is open and those of the acid
reservoir and the special worm and the boiler M arranged above are closed; I then a
proceed with the distillation of the tar.
For this mode of treatment I prefer to use sulphuric acid only.
When the distillation is nearly finished 1 charge the reservoir with the necessary
quantity of acid and then shut off the valve of the acid pump, thus shutting off all
pressure and vapours from the pump.
When the distillation is finished and if the substance treated is at 320° I open the
door of the furnace and shut the damper or register of the chimney, if the
temperature is lower it must be brought to 320° and then the door is opened and
the damper closed.
The acid is then introduced as follows:
The valve of the special worm is opened, that of the ordinary worm closed, the
valve of the tube connecting the two vats or boilers A and M is also opened and then
I slowly and gradually open the valve of the tube between the boiler A and the acid
reservoir, thus introducing the acid. An effervescence will take place and the substance
being treated will increase in volume in such a manner that it will easily rise into the 4
upper vat M.
When the acid is all introduced the valve of the tube i is closed.
When the pitch ceases to rise which I ascertain through the hole S on the boiler A,
the process is finished and the fire is raked out of the furnace.
The pitch need now only be run off into the cooling chamber and from thence into 4
suitable receptacles.
The pitch thus treated is perfectly brittle when cold.
2. If it is desirable to treat one or other kind of pitch without boiling, with one,
several or all the above mentioned acids, I proceed with the same apparatus and in
the same manner as described above, with the exception that I let the substance to be
treated cool down to 150° before the introduction of the acid or acids and then bring
it up again to 320° after the introduction.
3. If it is desired to enrich any kind of pitch with one, several or all of the above
mentioned substances and if these substances are added together with one, several or
all of the above mentioned acids and that at a temperature which produces ebullition,
I preferably operate as follows:
I use the same apparatus as that used for the treatment of insufficiently evaporated

page_text: pitch to which I add another reservoir for the reception of the enriching substance
similar to those used actually in iar distilleries for greasing the latter.
Fig. 2 of the accompanying drawings represents such an apparatus.
A is the boiler, B the agitator, the upper vat, connected with A by the tube C¹
provided with a valve C, D is a valve on the top of the vat C, E is a tube connecting
the ordinary worm with the boiler A and provided with the valve E, F is a tube
connecting the special or additional worm with the boiler A and provided with a
valve F, G is the glass reservoir for the acid, H a tube connecting it with the acid
pump and provided with a valve H¹, P is a suitable tube connecting the acid reservoir
with the boiler A and provided with a valve, R is the reservoir for containing the
enriching substance, R₁ is a tube leading to the pump for charging the reservoir R,
and R is the tube and valve by means of which the enriching substances are
introduced from the reservoir R to the boiler A.
For each kind of acid used, a separate pump and tube is connected with the acid
reservoir.
A. If I employ gasometer tar to enrich the pitch I preferably proceed as follows:
I charge the boiler with a quantity of gasometer tar equal to one quarter of its
capacity and distil this as above described.
The oils of naphtaline and anthracene are removed and the door of the furnace
then opened and the register of the chimney closed. The pitch thus produced I enrich
with 80 per cent. of tar. If the reservoir R for the coal-tar does not hold a sufficient
quantity it must be charged several times with the-coal tar to be added to the
substance to he treated. The operation is continued the same as in the case of pitch
insufficiently evaporated. It is preferable to use sulphuric acid only in this mode of
treatment.
B. If I use tar from coke furnaces to enrich the pitch I preferably proceed as
follows:
I charge the boiler with a quantity of gasometer tar equal to of its capacity and
distil the pitch produced is enriched with 40 per cent. of tar from coke furnaces, the
operation is continued and the pitch obtained is brittle when cold.
;
With this mode of treatment either sulphuric, nitric or muriatic acid or several or
all of these may be used.
If several or all of the acids are used, they are mixed in the reservoir previous to
the introduction into the boiler.
C. If a non-volatile oil from coal-tar is used to enrich the pitch I preferably proceed
as described above under B, with the exception that I charge the boiler with a quantity
of gasometer tar equal to a third of its capacity and add only 20 per cent. of the non-
volatile oil to the pitch produced.
If I use for the enriching of the pitch either gasometer tar or tar from coke
furnaces which has already undergone a slight treatment I only use the oils still
contained in these tars, and let these tars undergo a fresh distillation for the purpose
of obtaining these oils."
4. If it is desirable to treat the pitch and the substance for enriching it with one,
several or all of the above mentioned acids without producing ebullition I proceed as
described under A, B or C of paragraph 3, only the pitch is allowed to cool down
to 150° before the introduction of the acid or acids and subsequently brought again
to 320°.
If the substance to which the acid or acids are to be added is the enriching substance
itself I proceed as follows:
I use a boiler similar to that represented in Fig. 2 with the exception that the acid
reservoir is arranged above the enriching reservoir and communicates with this,
instead of direct with the boiler. Fig. 3 represents this apparatus and A is the boiler,
Bis the agitator, C the upper vat communicating with A by the tube C¹ provided
with valve C, D is the valve on the top of the vat C, E the tube connecting the
boiler with the ordinary worm and provided with a valve E, F the tube connecting
the boiler with the special or additional worm and provided with a valve F, G is the
reservoir made of glass for containing the enriching substance and connected with the

page_text: boiler A by a tube K of earthenware and provided with a valve, H is the acid
reservoir arranged above and connected with the reservoir G by a tube H¹ provided
with a valve H, J is the tube connecting the acid reservoir with the acid pump and
provided with a valve J and G¹ is the tube by means of which the reservoir G is
charged with the enriching substance.
5. If it is desirable to mix the acid or acids with the pitch and the enriching
substance, without producing ebullition and bringing them afterwards to a degree of
temperature producing ebullition, I proceed in the same manner as indicated under 4,
with the exception that the acid or acids are introduced into the boiler after they have
been mixed with the enriching substance. This gives the same result and is only a
inodification of the process.
6. If it is desirable to mix one, several or all of the above mentioned acids at a
temperature which produces ebullition with a pitch which has been mixed with the
enriching substance or substances at a temperature which only melts the pitch, or any
temperature up to boiling point no matter how great the evaporation produced, I
proceed in the same manner as in the above described cases only I mix the acid or
acids and the enriching substances at a temperature of 150° and then introduce them
into the melted pitch without submitting it to a fresh ebullition as this fresh ebullition
would produce a considerable evaporation of the material.
7. If desired the acid or acids may be divided in two parts which are mixed
relatively with the pitch and the enriching substance, the whole being afterwards
mixed in the boiler and treated as described above. This gives the same result and is
only a modification of the process.
Independently of the enriching substances which may be used and are mentioned
above, if I have to treat an insufficiently evaporated pitch having the same quality as
the pitch mentioned in the above cases, for instance a pitch produced from coal-tar
which has been distilled for the production of naphtaline and anthracene and already
enriched during the distillation of the coal-tar with 8 to 10 per cent. of oil, I preferably
use for again enriching this pitch 40 per cent. of gasometer tar or 20 per cent. of tar
from coke furnaces or 10 per cent. of non-volatile oil of coal tar.
It is well understood that I do not limit myself to the precise details as given above
and represented in the accompanying drawings, as these may be modified and altered
at will without deviating from the principle of the invention, and I also do not limit
myself to the above named proportions of the different substances used, as these
depend upon and will vary according to the nature and quality of the pitch to be
treated.
It is to be understood that besides using any of the before mentioned acids, I may
use any other suitable acid.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. For enriching pitch obtained from coal-tar by evaporation the adding thereto of
tar from gasometers or from coke furnaces or of non-volatile oils obtained from coal-
tar together with either sulphuric, nitric, muriatic or any other suitable acid or a
combination of two or more of such acids and submitting the whole to the influence of
heat substantially as hereinbefore set forth.
2. In apparatus for enriching pitch the combination with an ordinary boiler A and
an ordinary worm G of a special or additional worm such as H and a reservoir I of
glass or equivalent material and a vat M arranged above the level of the boiler A
substantially as hereinbefore described and illustrated in figure 1 of the accompanying
drawings.
3. In apparatus for enriching pitch the combination with an ordinary boiler, an
ordinary worm, a special or additional worm, a 'reservoir and vat G and C of a
reservoir such as R for containing the enriching substance and arranged above the
level of the boiler substantially as hereinbefore described and illustrated at Figure 2
of the accompanying drawings.

page_text: 4. In apparatus for enriching pitch the combination with an ordinary boiler, an
ordinary worm, a special or additional worm and a vat C of a reservoir such as G for
containing the enriching substance and arranged above the level of the boiler and a
reservoir such as H for containing the acid and arranged above the level of and com-
municating with the reservoir G for the purpose of mixing the acid with the enriching
substance previous to their introduction into the boiler substantially as hereinbefore
described and illustrated at figure 3 of the accompanying drawings.
Dated this 30th day of June 1SSS
W. P. THOMPSON & BOULT,
Agents.