New Manufacture of Compound for Mixing with Caoutchouc.
Year: 1899

page_text: New Manufacture of Compound for Mixing with Caoutchouc.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention (as communicated to me from abroad by William V. McManus, of Kings-
bridge Avenue, New York City, U.S.A., Contractor) to be as follows:-
The invention relates to the manufacture of a compound useful for mixing with
caoutchouc for increasing its bulk while retaining its useful properties
In carrying out this invention two kinds of materials are intimately mixed and
heated. These materials include an oil such for instance as rape-seed oil and a solid
comminuted mineral which makes a vulcanizable compound with certain oils
Minerals such as graphite, white lead or oxide of zinc may be used for this purpose.
These mixed materials while hot are sprinkled with certain reagents-sulphuric
acid and chloride of sulphur being best-whereby a modification and union of the
materials takes place producing granules of a somewhat caoutchone-like material
These may be ground in a stream of water to prevent mere crushing and
to promote true comminution. After the impurities are wasbed out with alkalı
and water the fine material 18 ready for incorporation in a well known way with
rubber.
The best mode of carrying out this invention involves the use of an electric
current around or near the mass for producing an electric influence simultaneously
with the heating thereof. It is advantageous to supply this influence by the use of
the well known resistance conductors whereby electric current itself produces the
requisite high temperature.
By use of the electric and thermal influences concurrently, numerous advantages
are obtained in practice, such as saving in time, labor and chemicals, as well as
improvement in product.
New Manufacture of Compound for Mixing with Caoutchouc.
I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
[Price 8d.]

page_text: invention (as communicated to me from abroad by William V. McManus, of Kingsbridge
Avenue, New York City, US A., Contractor) and in what manner the same 18 to be
performed to be particularly described and ascertained in and by the following
statement:—
This invention relates to the manufacture of a compound useful for mixing with
caoutchouc for increasing its bulk while retaining its useful properties.
In carrying out this invention, two kinds of materials are intimately mixed and
heated. These materials include a non drying vegetable oil such for instance as rape-
beed or colza oil and a comminuted solid material which makes a vulcanizable
compound with certain oils Minerals such as graphite, white lead-or nine-oxide
may be used for this purpose.
These mixed materials while hot are sprinkled with sulphuric acid and sulphur
chloude, whereby a compounding of the substances takes place producing granules
of a some-what caoutchouc-like material.
These may-be granules are preferably soaked and then ground in water to prevent
mere crushing and to promote true comminution. After the impurities are washed
out with alkali and water the fine material is ready for incorporation in a well known
way with rubber.
The best mode of heating the mixed material involves the use of an electric current
around or near the mass for producing an electric influence simultaneously with the
beating thereof
It is advantageous to supply this influence by the use of the well known resistance
conductors whereby the electric current itself produces the requisite high temperature.
By use of the electic and thermal influences concurrently, numerous advantages
are obtained in practice, such as saving in time, labour and chemicals, as well as
improvement in product.
The proportions of the materials may be varied, the following is found to be a good
composition.
About 5 lbs. of rape seed oil are mixed with 5 lbs. of powdered graphite, and the
mixture is heated to about 110° F. in a vessel of material not liable to corrosion.
The heated material is then sprinkled with about 8 fluid ounces of sulphuric acid
about 66% and 6 fluid ounces of sulphur chloride, these being either separately
spinkled, or being first mixed and the mixture sprinkled. During the sprinkling
which may occupy about one to two minutes the whole should be actively agitated, by
any suitable mixer.
The product is of a granular, and somewhat elastic character which is finely
ground in water as above described and is then washed with a weak solution of
caustic soda.
Instead of plumbago or other forms of almost pure graphite, graphite of cheap
kinds such as commercial graphite containing little silver silica may be employed.
When electricity is applied I provide a vessel surrounded by insulated electric
resisting conductors, the whole being surrounded by an outer shell or casing.
In practice I prefer to use the conductors for developing the necessary heat for
bunging the materials to the temperature necessary for sprinkling. These materials
are charged in this vessel and there heated.
I prefer to employ sufficient current to raise the initial temperature of the vessel
to about 300° Fahr. For this purpose the electric mains may be supplied with
current at a potential sufficient to produce the higher temperature required, a switch
being used, whereby resistances can be introduced for afterwards lowering the
temperature of the vessel to 110º.
With this apparatus, I first throw the full potential of the mains upon the
conductors, maintaining this connection for a short time
I have found that this sets up an influence within the vessel which is maintained
when, after a short time, the resistances are introduced and the temperature of the
vessel is held at 110° Fabr
These changes may be accomplished before introduction of the mass within the

page_text: vessel, since the high initial potential is intended to simply start an electric condi-
tion, and not to establish a certain thermal condition.
I have found that by use of these expedients, the compounding of the materials is
greatly promoted, the sulphuric acid and sulphur chloride are prevented from in-
corporating themselves inextricably with the mass, and in consequence the cost in
labour, materials and time of eliminating these reagents is greatly lessened.
Where the electrio influence is omitted, the treatment with caustic soda should be
continued for a number of days: and even when at last the litmus paper shewa no
acid reaction, I have found that time developed such a reaction afterwards.
When electric influence is employed, I am able to thoroughly eliminate all
impurities after grinding, by one brief washing with cold dilute caustic soda, followed
by washing with clear water, and the preparation of my new material can be
completed within a few hours.
The use of two different degrees of electric influence is not essential to my process,
but I have found it to give the best results.
I have found that my compound can be advantageously used in a mixture
containing four parts of the compound to six parts of pure rubber, but I do not limit
myself to these proportions.
Having now particularly described and ascertained the nature of this invention
and in what manner the same is to be performed, I declare that what I claim is :—
:-
1. The herein described manufacture of a compound for mixing with caoutchouc by
mingling a non drying vegetable oil such as rape seed or colza oil with comminuted
solid material such as graphite white lead or zine oxide, heating grinding the mixture,
sprinkling it with sulphuric acid and sulphur chloride grinding the resulting granules
in water, and finally washing the product with alkaline solution.
2. The modification of the process above set forth by subjecting the mixture of
oil and solid to electrical influence as herein described.
3. The compound manufactured as above set forth.