An Improved Process of Solidifying Crude and Refined Petroleum and Petroleum Residues.
Year: 1898

page_text: An Improved Process of Solidifying Crude and Refined Petroleum
and Petroleum Residues.
We, JOHAN CONRAD BERNTROP, of 13, Brederodestraat, Amsterdam, Holland,
Chemist, and MARIUS LODENWYK QUIRYN VAN LEDDEN HULSEBOSCH, of 17.
Nieuwendyk, Amsterdam, Holland, Apothecary, do hereby declare the nature of
this invention to be as follows:-
It has already been proposed to solidify, petroleum in the crude or in the refined
state, and also petroleum residues, by treatment with alkali.. soap, peroxide of
hydrogen, or with ozokerite, wax, pitch, paraffin, or the like. But all such
additions have the disadvantage that the conversion of the petroleum or its
residues into the solid form is not effected in a direct manner, whilst the products
are not sufficiently firm, and the industrial utilization of the same as fuel is
prevented on account of the high price of manufacture. Now this invention has
reference to a process for solidifying crude and refined petroleum and also
petroleum residues, according to which a solution of resin or abietic acid in
petroleum or petroleum residues, or a mixture of these substances is mixed for
a prolonged period intimately by rubbing together or compounding with slaked
lime with the addition of water, whereby a tough mass is produced which, when
allowed to stand, will after a time (in some cases in a few minutes) solidify and
can then be moulded by pressure into a firm body suitable for transport.
This product constitutes an excellent fuel of great heating power.
If the petroleum residues contain sufficient quantities of resinous substances,
the addition of resin or abietic acid may be diminished or even wholly omitted.
The amount of the addition depends on the nature of the residues, and must
be determined experimentally in each case.
The tough mass which is obtained by rubbing with slaked lime in the pre-
sence of water, may be mixed. before solidifying, with more or less finely
powdered coal, coke, peat, lignite, sawdust, wood-flour, or other combustible,
or even substances that are not particularly combustible or even inert, and can
then be directly further condensed by pressure.
The herein-described process differs essentially from a former proposal which
consisted in mixing crude petroleum with dry powdered lime, and treating the
said mixture with a solution of resin, whereupon the solidification was effected
by an addition of resin oil. Experiments have shown that the mixture of petro-
leum, powdered lime, and added resin, without the addition of resin oil, does not
become solid, so that the latter constituent is essential for carrying out that
.process.
But, in the new process, the solidification of the petroleum is effected by first
dissolving resin in petroleum and then rubbing such petroleum (or also as above
stated, petroleum residues, and if necessary without special addition of resin)
intimately with slaked lime to which water has been added, until, in conse-

page_text: quence of the saponification of the resin, a more or less tough mass is produced
which solidifies of itself.
The following example illustrates the improved process:-
About 45 kilogrammes of resin (colophony, pine resin, etc.) or abietic acid,
are dissolved in about 270 kilogrammes of crude petroleum, which has prefer-
ably been first freed from its volatile constituents (boiling below 100° C.) and
the solution so produced is intimately rubbed with about 60 kilogrammes of
fresh-slaked lime, to which is added about 30 to 35 per cent. of water, until a
more or less tough sticky mass is produced. This mass is thoroughly well
rubbed or compounded with about 625 kilogrammes of powdered coal or coke,
or with a sufficient quantity of powdered peat, or with other combustible finely-
comminuted organic substances, until a dry dough-like mass is produced, which
can be pressed into moulds, or, when left to stand will solidify, and can then be
employed in the form of lumps or briquettes as 'fuel. The quantities above
given can obviously be varied within considerable limits, especially as regards
the proportion of the petroleum with the other powdered substances. The
petroleum or the petroleum residues can be produced in the solid form equally
well without an addition of pulverulent substances, and also material can be
produced which contains only about 25 per cent. of petroleum so that the
remainder consists mainly of pulverulent fuel.
As will be seen from the above example, a comparatively large quantity of
lime is required in order to produce the combination (which combination is
necessary for the solidification of the petroleum) of lime and resin, but if less
lime be used, the mass will not be sufficiently solid. It seems that the great
quantity of lime is necessary because only a comparatively small amount of
water can be added to the lime, if it is not desired to effect a special drying or
heating of the mixture after the rubbing or compounding.
Also the excess of lime may be necessary for the reason that a part of the sa ne
is enveloped by petroleum and is removed from the action of the resin. This is
shown by the fact that the addition of lime may be replaced partly and up to
about one half by cement, which. however, is not added directly, but only after
the saponification of the mass. The cement would then seem to serve only to
bind the water and to facilitate the solidification of the mass.
Dated this 9th day of April 1898
F. WISE HOWORTH,
46, Lincoln's Inn Fields, London, W.C.,
Agent for the Applicants.
An Improved Process of Solidifying Crude and Refined Petroleum
and Petroleum Residues.
We, JOHAN CONRAD BERNTROP, of 13, Brederodestraat, Amsterdam, Holland,
Chemist, and MARIUS LODENWYK QUIRYN VAN LEDDEN HULSEBOSCH, of 17.
Nieuwendyk, Amsterdam, Holland, Apothecary, 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:-
It has already been proposed to solidify petroleum in the crude or in the refined
state, and also petroleum residues, by treatment with alkali, soap, peroxide, of
hydrogen, or with ozokerite, wax, pitch, paraffin, or the like, but all such
additions have the disadvantage that the conversion of the petroleum or its
residues into the solid form is not effected in a direct manner, whilst the products

page_text: are not sufficiently firm and the industrial utilization of the same as fuel is
prevented on account of the high price of manufacture. Now this invention has
reference to a process for solidifying crude and refined petroleum and also
petroleum residues, according to which a solution of resin or abietic acid in
petroleum or petroleum residues, or a mixture of these substances is intimately
mixed for a prolonged period by rubbing together or compounding with slaked.
lime with the addition of water, whereby a tough mass is produced which, when
allowed to stand, will after a time, (in some cases in a few minutes) solidify and
can then be moulded by pressure into a firm body suitable for transport. This
product constitutes an excellent fuel of great heating power.
If the, petroleum residues contain sufficient quantities of resinous substances,
the addition of resin or abietic acid may be diminished or even wholly omitted.
The amount of the addition depends on the nature of the residues, and must
be determined experimentally in each. case.
The tough mass which is obtained by rubbing with slaked lime in the pre-
sence of water, may be mixed, before solidifying, with more or less finely
powdered coal, coke, peat, lignite, sawdust, wood-flour, or other combustible,
or even substances that are not particularly combustible or even inert, and can
then be directly further condensed by pressure.
The herein-described process differs essentially from a former proposal which
consisted in mixing crude petroleum with dry powdered lime, and treating the
said mixture with a solution of resin, whereupon the solidification was effected
by an addition of resin oil. Experiments have shown that the mixture of petro-
leum, powdered lime, and added resin, without the addition of resin oil, does not
become solid, so that the latter constituent is essential for carrying out that
process.
But, in the new process, the solidification of the petroleum is effected by first
dissolving resin in petroleum and then rubbing such petroleum (or also as above
stated, petroleum residues, and if necessary without special addition of resin)
intimately with slaked lime to which water has been added, until, in conse-
quence of the saponification of the resin, a more or less tough mass is produced
which solidifies of itself.
The following example illustrates the improved process :-
-
About 45 kilogrammes of resin (colophony, pine resin, etc.) or abietic acid,
are dissolved in about 270 kilogrammes of crude petroleum, which has prefer-
ably been first freed from its volatile constituents (boiling below 100° C), and
the solution so produced is intimately rubbed up with about 60 kilogrammes of
fresh-slaked lime, to which is added about 30 to 35 per cent. of water, until a
more or less tough sticky mass is produced. This mass is thoroughly well
rubbed or compounded with about 625 kilogrammes of powdered coal or coke,
or with a suitable quantity of powdered peat, or with other combustible finely-
comminuted organic substances, until a dry dough-like mass is produced, which
can be pressed into moulds, or, when left to stand will solidify, and can then be
employed in the form of lumps or briquettes as fuel. The quantities above
given can obviously be varied within considerable limits, especially as regards
the proportion of the petroleum with the other powdered substances.
The petroleum or the petroleum residues can be produced in the solid form
equally well without an addition of pulverulent substances, and also material
can be produced which contains only about 25 per cent. of petroleum so that the
remainder consists mainly of pulverulent fuel.
As will be seen from the above example, a comparatively large quantity of
lime is required in order to produce the combination (which combination is
necessary for the solidification of the petroleum) of lime and resin, but if less
lime be used, the mass will not be sufficiently solid. It seems that the great
quantity of lime is necessary because only a comparatively small amount of
water can be added to the lime, if it is not desired to effect a special drying or
heating of the mixture after the rubbing or compounding.

page_text: Also the excess of lime may be mecessary for the reason that a part of the same
is enveloped by petroleum and is removed from the action of the resin. This is
shown by the fact that the addition of lime may be replaced partly and up to
about one half by cement, which, however, is not added directly, but only after
the saponification of the mass. The cement would then seem to serve only to
bind the water and to facilitate the solidification of the mass.
Having now particularly described and ascertained the nature of the said in-
vention and in what manner the same is to be performed we declare that what we
claim is:.
1. The herein described process of solidifying crude and refined petroleum
and also petroleum residues, by intimately rubbing together and for a prolonged
period a mixture of the said substances and resin or abietic acid, with slaked
lime and water until there is produced a tough mass that will harden when :left
to itself, or which is intimately mixed with other substances more or less pul-
verulent, and which, in either case can be further subjected to pressure or
moulding, as set forth.
2. The process specified in the preceding claim with the modification that,
when using petroleum residues, the addition of resin or abietic acid is omitted.
3. In the process specified in 'Claims 1 and 2, the partial replacement of the
lime by cement which is added after the rubbing together of the petroleum or
petroleum residues (mixed with resin or abietic acid) with lime.
4. Briquettes of solidified material produced according to Claims 1, 2 and 3,
and consisting of lime and petroleum or petroleum residues and resinous sub-
stances, with or without cement and with or without finely granular or pul-
verulent material (especially combustible material), as set forth.
Dated this 31st day of December 1898.
F. WISE HOWORTH,
46, Lincoln's Inn Fields, London, W.C.,
Agent for the Applicants.