Manufacture of Saponaceous Products from Petroleum.
Year: 1894

page_text: Manufacture of Saponaceous Products from Petroleum.
I, CHARLES WEYGANG, of No. 3 Hermitage Villas, Childs Hill, in the County
of Middlesex, Gentleman, do hereby declare the nature of this invention to be as
follows:-
My invention relates to the treatment of petroleum in such a manner as to obtain
therefrom saponaceous products, applicable to various purposes, as hereinafter set
forth.
I combine with petroleum, resinous substances or fatty matters capable of
being saponified, and treat the compound with alkali, thus obtaining a saponaceous
product, which may be also obtained by first saponifying or dissolving the resinous
or fatty matter by alkali or by fusing these substances together and then mixing
the product with petroleum; in both cases the incorporation of the substances is
promoted by heating. When the product settles, a clear liquid may be decanted
This
which is applicable as a polish or for treating fibres, yarns and the like.
liquid may be rendered colourless or nearly so by the addition of alkaline silicate
or a further proportion of alkali. It may also be rendered more or less inodorous
by adding a small proportion of naphthaline to the ingredients first employed, or
lime may be added either fused with the resinous matter or combined with the
caustic soda and water, sometimes with a little acid. When the product is to be
used as soap, I add a little soap, sometimes with a little starch and alkaline silicate,
boiling the whole to the desired consistence. The solid petroleum soap thus
obtained may be dissolved in water, boiled, seponated and again boiled, or it may
be remelted with other soaps and suitable soap ingredients.
A jelly consistence may be obtained by saponifying the petroleum mixed with
resinous materials by addition of caustic lime and solution of caustic soda, and
subsequently adding a little dilute acid.
Or, instead of resinous material, I incorporate a little soap with the petroleum,
add a solution of calcium chloride and wash with water.
The material thus produced is applicable for medicinal, waterproofing, lubricating
and other purposes.
The petroleum with about half its weight of the resinous material, with a little
naphthaline and vegetable oil boiled with solution of caustic soda, furnishes an oily
material suitable as a vehicle for pigments, and may be made siccative by addition
of some oxidising salt dissolved in sulphuric acid, boiling in water and decanting
the oil.
.
The saponaceous petroleum product obtained as above described by saponifying
the mixture of petroleum and resinous or fatty matter with or without bituminous
matter, alkaline silicate or lime, may be mixed with calcium chloride or with
calcined gypsum or with lime or mixtures of these producing a paste which can be
moulded into solid blocks of artificial fuel. The paste may also be made up, before
moulding, with peat or coal dust or other carbonaceous substances.
In most of the applications above set forth, the saponifying of the petroleum
mixture may be effected at various stages of the process.
Thus, for instance, in producing the fuel blocks, resinous ingredients with or

page_text: without bituminous matters may be first saponified, then mixed with calcined
gypsum or its equivalent and incorporated with the petroleum.
Dated this 12th day of February 1894.
ABEL & IMRAY,
Agents for the Applicant.
I, CHARLES WEYGANG, of No. 3 Hermitage Villas, Childs Hill, in the County
of Middlesex, 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 :-
My invention relates to the treatment of petroleum in such a manner as to
obtain therefrom saponaceous products applicable to various purposes hereinafter
set forth.
I combine with petroleum a resinous substance or fatty matter capable of being
saponified, dissolving such substance in the petroleum preferably by means of heat
and in a manner according to the nature of the article to be produced, and I treat
the mixture with alkalies and other agents consistent with the use to which the
product is to be put.
The resulting saponaceous product I treat further in accordance with the article
to be made, proceeding for the different purposes substantially as follows:-
I produce an oil which is more or less soluble or miscible in water by first
combining petroleum with a resiuous or equivalent matter; for instance: I melt
50 lbs. rosin in 100 lbs. petroleum. While the mixture is still hot I add by drops
or otherwise very slowly and intermittently under active stirring about 1 pints of
a saturated solution of strong caustic soda for every 50 lbs. of rosin employed:
After the mixture has cooled I decant the clear oil and add to the same a further
proportion of the aforesaid caustic solution, equal to 2 to 2 quarts for every 50 lbs.
of rosin employed. I add the alkali as before by drops or otherwise very slowly
and intermittently under active stirring. I allow the mixture to settle and then
decant the clear oil for the different purposes for which it is intended.
The black gummy residue precipitated after the addition of the first portion of
alkali, and also any residue or solid precipitate after the second addition, can be
used in the manufacture of common soap, or for other purposes.
With the object of increasing the viscosity of the oil or its solubility I may
sometimes repeat the operation of adding the aforesaid caustic solution in the same
manner to the decanted oil and then decanting again.
Instead of proceeding as hereinbefore just described I treat the mixture of
petroleum and resinous or fatty matter first with ammonia and subsequently with
another alkali, for instance: I take 100 lbs. of petroleum and dissolve therein 50 lbs.
rosin. I allow the mixture to cool and then add liquor ammonia, preferably of highest
strength, very slowly and intermittently under active stirring, until the mixture
becomes solid. This mixture I prefer to leave for 24 hours or longer. I then
re-heat it until it becomes fluid and clear, and after cooling again I add in the
same manner as herein before described, that is, very slowly and intermittently,
under active stirring, a saturated solution of strong caustic soda, until a solid
sediment begins to form. I allow the liquid to settle and decant the clear oil.
Although I prefer to use caustic soda in conjunction with the ammonia 1 do not
confine myself to the same; other alkalies employed in the same manner would
produce similar results.
For some purposes I produce a more or less scluble or miscible oleaginous matter
by fusing the primary ingredients with an alkaline carbonate and an alkaline

page_text: borate; for instance: I melt 50 lbs. rosin in 100 lbs. petroleum. I continue the
heating and add in small quantities and at intervals about 20 lbs. of finely
broken ordinary crystal soda, and about 10 lbs. borax. I then add about 10 lbs. of
water by dropping the same in at intervals and stirring energetically.
For the purpose of producing a more or less inodorous oil I take one of the
soluble or miscible oleaginous preparations hereinbefore described, and for this
particular purpose I prefer to employ the preparation produced by means of
ammonia, or that produced by means of carbonate of soda and borax. I agitate
the oleaginous mixture with about an equal bulk of water and the resulting milky
emulsion I heat to boiling point. After resting a short time the petroleum separates
with a pale yellow colour. This separated oil I agitate with an alkaline liquor,
such as caustic soda, ammonia, silicate of soda, or with caustic lime, when the oil
separates in an almost, colorless and odourless condition. I find that ammonia
produces the best results; and in order to avoid any trace of a petroleum smell I
may combine with the original mixture about 1 or 2% of naphthaline or an equal
quantity of turpentine or the like.
For the purpose of producing a soap I take about 120 lbs. of petroleum and melt
therein about 20 lbs. rosin (more or less may be employed, but this is a good
average proportion). When the rosin is dissolved I add to the heated mixture a
solution of caustic soda in a proportion of one half pint for every 10 lbs. of rosin
employed adding the caustic solution very gradually and intermittently under active
stirring. I allow the mixture to settle and decant the clear oil which I re-heat
with about 30 lbs. of ordinary fat soap. This is a good average proportion, but
more or less may be used. When the soap is melted I add gradually and inter-
mittently under active stirring a further proportion of the caustic solution,
generally equivalent to about 4 quarts, and I keep the mixture on the boil during
the operation. The exact proportion of alkali depends on the character of the
petroleum and is determined by testing a little of the mixture under operation by
solution in some distilled water, and if an appreciable quantity of free oil globules
rise to the surface, more alkali is required. Towards the end of the saponification
I add a small quantity of water, dropping the same in slowly and intermittently up
to a proportion of about 25% of the whole and I continue the boiling and active
stirring for about 1 hour or longer, after which I may add more water with the
soap if desirable and separate the lye on cooling.
:
In the place of the ordinary fat soap I may combine with the petroleum mixture
an equivalent proportion of a fat but this is not so generally applicable as the
soap. However, the employment of a fat, such as palm oil, or cocoa nut oil, in
addition to the soap, is generally an advantage. Such fat is added to the mixture
after the other ingredients are thoroughly combined, additional alkali being added,
if necessary, and in proportion to the quantity of fat employed.
When fat is employed in the place of soap it is generally advantageous to render
the petroleum more soluble or miscible in the first instance, that is before mixing
it with the fatty matter. In this case the more or less soluble or miscible oleaginous
compounds described in the early part hereof will serve for examples.
By treating the soap herein before described, or equivalent mixture, with a
soluble salt of an alkaline earth, such as calcium chloride, I obtain a substance. of
jelly or grease like consistence, according to the detailed procedure; thus: I obtain
a soft or jelly consistence by taking the soap with its minimum proportion of alkali
and combining therewith slowly and in small proportions at a time calcium chloride,
previously dissolved in as little water as possible. The addition of the calcium
chloride is continued until the mass is neutral or almost. so, and I then gradually
add water, commencing with small proportions and working the same into the
composition by energetic beating mixing or kneading, and gradually increasing the
quantity until it distinctly separates from the greasy mass. I then add more water
for the purpose of washing, and allow it to separate and run off, and I repeat the
operation until the greasy substance is more or less neutral and tasteless, after
which I heat it when the remaining excess of water separates on cooling.

page_text: By combining larger proportions of caustic alkali with the soap in the first
instance a proportionately larger amount of the mineral salt is absorbed and the
product becomes harder and more resembling solid grease.
.
Instead of employing the petroleum soap for the purpose of producing the
grease like substances, I obtain similar results by employing the more or less
soluble oils herein before described, but with a minimum proportion of rosin and
the addition of a fatty matter, such as palm oil or cocoa nut oil. For instance:
I melt about 20 lbs. of rosin in about 120 lbs. petroleum. To the heated mixture
I add about pint of a saturated solution of strong caustic soda. I allow the
mixture to cool and decant the clear liquid to which I then add very slowly and
intermittently a further proportion of the caustic solution until the mixture begins
to solidify. I then reheat the mass and melt in about 25 lbs. or upwards of a fatty
matter, such as-palm oil or cocoa nut oil. I then work in very slowly and in small
quantities at a time, calcium chloride previously dissolved in as little water as
possible, and I otherwise proceed as hereinbefore described. It being also
understood that the proportion of the alkali determines the hardness of the
product.
Such grease like substances are more particularly applicable as lubricants for
machinery.
For the purpose of producing a substance applicable as varnishes and vehicles
for paints. I proceed somewhat in the following manner: I take the hereinbefore
described more or less soluble or miscible oil and combine with the same an agent
which will impart siccative properties and at the same time neutralize the alkali.
I take for instance the decanted more or less soluble or miscible oil prepared by
melting petroleum with rosin and then treating the mixture with caustic soda
substantially as hereinbefore described. I prefer to employ a mixture consisting
of rather a large proportion of rosin, say from 50 to 75 parts to 100 parts of
petroleum. The resulting more or less soluble oil I combine with sulphate of zinc,
which I prefer to add in a dry powdered condition, in small quantities at intervals,
under constant agitation, until the mixture is neutral, and I may boil the mixture to
promote the action.
When thoroughly neutral I allow it to settle and then decant the clear oil for
use as a varnish or for allied purposes.
Instead of employing for the purpose just described an oil prepared in the first
instance with caustic soda, I may employ a similar mixture prepared with other
alkalies, more particularly the more or less soluble or miscible oil consisting of
petroleum and rosin treated with ammonia and then with caustic soda, substantially
as hereinbefore described; otherwise proceeding in the same manner as in the
preceding instance.
By mixing with the more or less soluble or miscible oil in the first instance other
oils, such as linseed oil, cotton seed oil, castor oil, or the like, and then treating the
mixture with an agent imparting siccative properties and which at, the same time
neutralizes the alkali, as herein before set forth, I obtain more elastic products,
particularly suitable as vehicles for paints. I generally employ for this purpose
raw linseed oil, or sometimes cotton seed oil, and 1 mix such oils with the miscible
petroleum oil in various proportions, according to the quality or toughness desired,
it being understood that the larger the proportion of linseed or cotton seed oil the
tougher the final product will be. I then treat the more or less soluble or miscible
oleaginous mixture with a siccative and neutralizing agent, more particularly
sulphate of zinc, and otherwise proceed substantially in the manner as hereinbefore
described.
In order to produce a dry solid material, I first make a more or less soluble or
miscible oleaginous mixture as hereinbefore described, but also combining with the
same an alkaline silicate. The resulting product I treat with a soluble salt of an
alkaline earth somewhat in the manner as hereinbefore described, proceeding in
detail substantially as follows:-In about 120 parts petroleum I melt about 20 parts
or more of rosin. I cool the mixture and add very slowly at intervals a composition

page_text: consisting of about 20 parts of a strong solution of silicate of soda and 10 parts
of a saturated solution of strong caustic soda, thoroughly mixed together. I stir
the oleaginous mixture energetically and gently heat it up to boiling point, con-
tinuing this until thorough combination takes place and the mass begins to thicken
and to more or less solidify. I then work in gradually and in small proportions
at a time 15 parts or thereabouts (:calculating dry weight:) of calcium chloride,
dissolved in as little water as possible. I mix, knead or grind the mass together
for a short time until it becomes a uniform pasty substance, and if I do not readily
obtain this condition I gradually add a little water in small quantities at intervals.
I may wash the product with the addition of further water, and then expose it to
dry after mechanically eliminating as much water as possible. Such a product
answers the purpose of an excellent fuel where an intense heat is required in a
small space.
For some purposes the product may be used without drying.
I also produce a solid applicable as fuel by first saponifying rosin and mixing the
resulting soap with petroleum in conjunction with calcined gypsum, proceeding in
detail substantially as follows:-I saponify about 3 parts by weight of rosin with
an alkali, using soda almost without exception, and practically proceeding in the
same manner as in making rosin soap for sizing paper. I prefer to allow the lye
to separate and to employ the solid soap only. I mix the aforesaid soap with
about 12 parts by weight of petroleum and about 6 parts by weight of gypsum,
preferably freshly calcined. I thoroughly mix the ingredients and continue
stirring until the mixture is sufficiently viscid to prevent settling, and 1 then leave
it alone when it sets in a few hours to a solid substance. With this mixture, and
almost at any stage, but preferably after it has set to the aforesaid solid consistence,
I more generally combine a certain proportion of carbonaceous matter, in the form
of fine coal, or charcoal, or the like, for the purpose of assisting the hardening of
the mixture. I can employ such carbonaceous matter in almost any proportion,
usually from 50 to 100 parts of a material like coal dust to 100 parts of the
petroleum mixture.
It has already been proposed to compound mineral oils with resinous and fatty
matters and alkalies for various purposes. I therefore make no general claim to
the compounding of these substances but
Having now particularly described and ascertained the nature of this inven
tion and in what manner the same is to be performed 1 declare that what I
claim is:-
1. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum, saponifying by gradual
addition of alkali, decanting the clear liquor produced; again gradually adding
alkali and decanting, thus obtaining a petroleum oil or oleaginous liquid more or
less soluble or miscible in water.
2. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum, treating the mixture with
ammonia, reliquifying and again adding alkali, thus obtaining a petroleum oil or
oleaginous liquid more or less soluble or miscible in water.
3. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum, fusing a gradually added
alkaline carbonate in combination with an alkaline borate in the heated mixture,
and then gradually dropping in a small proportion of water, thus obtaining an
oleaginous substance more or less soluble or miscible in water.
4. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum, treating the mixture with
alkalies and thus obtaining a more or less soluble or miscible oleaginous matter;
mixing the same with water; separating the oil from the water by the application
of heat, and agitating the separated oil with alkaline solutions, thus obtaining an
oil with little or no odour.
5. The herein described manufacture of saponaceous products from petroleum

page_text: by melting rosin and an already saponified substance in petroleum; saponifying the
mixture by the gradual addition of alkali and a minimum of water, thus obtaining
a soap.
6. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum; adding alkali to the mixture;
decanting the resulting clear oil; melting the same with a fatty matter and then
saponifying by the gradual addition of alkali, thus obtaining a soap.
7. The herein described manufacture of saponaceous products from petroleum
by rendering petroleum more or less soluble or miscible; adding a fatty matter and
then saponifying the mixture and thus obtaining a soap.
8. The herein described manufacture of grease like substances or viscid oils
suitable as lubricants by treating the saponaceous products of petroleum herein
described with a soluble salt of an alkaline earth more particularly calcium
chloride.
9. The herein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum, treating the mixture with
alkalies, thus obtaining a more or less soluble or miscible oleaginous matter; mixing
the same with an agent which neutralises the alkali and imparts siccative properties,
thus obtaining an oil applicable for varnishes and for vehicles for paints.
10. In combination with the process referred to in the preceding claim, the
admixture therewith of an elastic oil as herein described, thus obtaining a superior
oil applicable for varnishes and vehicles for paints.
11. The berein described manufacture of saponaceous products from petroleum
by melting rosin or equivalent material in petroleum and adding alkali in combina-
tion with an alkaline silicate; then treating the mixture with a soluble salt of an
alkaline earth more particularly calcium chloride, thus obtaining a greasy or solid
product applicable as a fuel.
12. The herein described manufacture of saponaceous products from petroleum
by mixing therewith a soap made from rosin in conjunction with calcium sulphate,
thus obtaining a solid applicable as a fuel.
13. In combination with the substance described in the preceding claim the use
of carbonaceous matters for the purpose of hardening the compound as herein
described.
Dated this 12th day of December 1894.
CHARLES WEYGANG,
"Edneys," West Wellow, near Romsey, Hampshire.