Improvements in the Manufacture of Compositions having as a Basis Oxidized Oil or Oxidized Oil and Fibrous Material.
Year: 1898

page_text: Date of Application, 30th Nov., 1898
Complete Specification Left, 30th Sept., 1899-Accepted, 25th Nov., 1899
Improvements in the Manufacture of Compositions having as a Basis
Oxidized Oil or Oxidized Oil and Fibrous Material.
I, CHARLES JAMES GRIST, of 20, Gracechurch Street, in the City of London,
Electrical Engineer, do hereby declare the nature of this invention to be as
follows:-
This invention relates to improvements in the manufacture of compositions, for
waterproofing, engine and other packings, acid tank linings, electrical insulating
compositions, paints, anti corrosive composition and compositions for like uses,
golf balls, blocks for paving roads and ways, carriage brake blocks, tyres and tyre
covers for wheels of vehicles and for other uses, and has reference to certain
modifications of such compositions as are described in the Specification of Letters.
Patent No. 21,742, 15th November 1895.
I take seed or other arying out and partially oxidize it by applying heat to
the vessel in which it is contained, having previously added litharge or other
suitable oxidizing agent, to a temperature of say 400° F. or upwards taking care
that it does not boil for more than say about 24 hours furthermore attention
should be given that the oil is kept stirred for about 48 hours being continually
kept in motion by suitable apparatus which may be conveniently arranged on or
adjacent to the vessel for the purpose.
The oil is then allowed to cool until it reaches about its normal temperature.
I now take a suitable fibrous substance such for instance as jute, hemp, cotton,
animal fibre or other suitable fibre, in which the separate fibres composing the
mass are or can be made to be distinct and separable but at the same time of
uniform or substantially uniform character and taking care that the fibres shall
be clean and free from any deleterious foreign substance in mixture or adhering
to them. These I free from the fibres by means of carding or other suitable
cleansing method.
I then spread and loosen the fibres subjecting them to the action of heated air
in order to remove as far as possible traces of aqueous moisture because any
moisture present militates against the success of the process.
The partially oxidized oil being now at about its normal temperature and the
fibres in a clean and dry condition; I immerse such fibres in a loosened and
graduated condition into the oil; the fibres are then immersed in the oil but imme-
diately taken out again and I attach great importance to these precautions.
The fibres thus dipped are placed in a hydro extractor of the usual or con-
venient pattern for the purpose of extracting the superfluous oil not actually
adhering to the fibres.
When this has been effected and the free oil has been thoroughly removed I
take the fibres out of the extractor and each fibre is found to be covered at
intervals with small particles of oil which adhere to it. I now spread these
fibres as loosely as possible on wire gauze or other suitable netting or reticulate
or openwork surface and pass a current of heated air for suitable periods through

page_text: them by means of a revolving fan or other suitable air supplying means turning
every hour or so and redistributing the fibres on the netting by suitable lifting
and turning means till each particle of oil is oxidized and dried.
Then I again immerse the fibres in the oil and throw off or remove the super-
fluous oil by means of the hydro extractor or its equivalent and more globules of
oil will be found to be adhering to portions of the fibres not covered after the
first dipping; then I repeat the drying process explained above and when dry I
immerse the fibres again and again removing surplus oil drying between each
dipping for say 12 to 14 repetitions of the operations already described, but I
find it necessary to employ a much higher velocity of revolution to the hydro
extractor so as to effect the application at each successive dipping of a more
attenuated distribution of the oil over the surfaces of the fibres.
The number of the successive operations of dipping and drying with removal
of surplusage of oil will vary slightly according to the use the product is designed
to be put to.
If at each dip coarser or thicker applications of the oil were made the fibres
would be liable to become over charged with oil so that the moving heated air
would be unable to oxidize the whole sufficiently and the resulting product would
be useless for my purposes.
I now grind up the fibres treated as described above, until they become of a
homogeneous character.
This masticating or grinding I prefer to accomplish by means of rolls, (running
at different surface speeds so as to obtain the desired effect) running at a high
speed.
The material is now placed in crushing rolls which I employ cold and I add
about 5% to 10% of powdered sulphur to it while the crushing is progressing
taking care that the fibrous treated material is not allowed to become so heated
as to injure it.
This I prevent by occasionally stripping it off the rolls by means of a knife
or gauge suitable for the purpose. When the sulphur is thoroughly mixed I
allow the material to cool to about normal and I then again place it in the crush-
ing rolls and add whatever colouring or hardening material is desired such as
French chalk, ochre, asbestos or other suitable material adapted to the particular
purpose in view.
The new waterproofing composition or material as now delivered from the rolls
is in sheets and ready for use and it can when cool be stored away until required
for use.
For waterproofing and for other purposes such as bed sheeting, clothing, double
texture and other goods I may proceed as follows; the material in sheets is again
put through the rolls and then it is immersed in naptha, ketone, turpentine or other
suitable solvent till it assumes the proper consistency required for any particular
purpose the superfluous spirit being carefully removed and in the case of naptha
and turpentine I place the material again in the crushing rolls, and working it
until it is in such a soft pliable condition that it will readily adhere to a material
or fabric under pressure or can be spread on with a knife or gauge.
It can be run on to the fabric in any convenient thickness by passing the
materials to be combined through heavy callenders or rolls and within a few
hours afterwards it will be ready for use, or it can be spread on fabric in very
thin layers by the ordinary spreading machines, such as are in use in rubber
factories by means of a knife or gauge.
Or I may take the material after the drying operation is finished, and without
putting it through a grinding and crushing process, place it in a vessel contain-
ing a ketone or other suitable spirit which will soften or dissolve the oil so that
I shall be able to remove it from the fibres by means of a wringing or other suit-
able arrangement. I then remove the surplus spirit by evaporation or otherwise
till the oil assumes a suitable consistency for the purpose I have in view.
For insulating compositions for electrical purposes I may proceed as follows

page_text: during the process of grinding and crushing the material I add a larger percentage
of sulphur-between 15% and 20%-and when this is thoroughly worked into
the material I add from 5% to 25% of gutta percha or other suitable compounds
for the purpose of giving enhanced tenacity to the compound, subjecting the
whole to the action of crushing rolls as before and rolling it into sheets by means
of heavy callenders or rolls. When cool it may be stored away for use till
required and is ready to be applied to practical use. It may if desired be sub-
jected to a vulcanizing process of any ordinary or convenient kind such as heating
it in a steam jacketted vessel, without or with the gutta percha.
then
When it is necessary to soften the material for coating wire or other purposes
I crush the sheets of material again in the rolls which are warm and
transfer it immediately to the feeding rolls of a wire covering machine the
machine being heated all round by steam likewise the nozzle and die through
which the material passes on to the wire.
Or I may take the sheets of material and soften them by means of a spirit
solvent such as naptha or turpentine or other suitable method in the manner
above described for waterproofing and other purposes.
The material can now be
placed in a wire coating machine of usual or convenient pattern for electrical pur-
poses but when the wire appears to be satisfactorily coated with the material it
is run through a hot air chamber in order that any solvent spirit still retained in
it may be evaporated and the material may be afterwards subjected to a vul-
canizing process.
Or again I may take the sheets of material and after crushing them in the
rolls run them into thin sheets by means of heavy callenders which be then cut
into strips and tape the material onto the wire by means of any of the known
taping machines.
By this means a material is produced which will withstand climatic influences
and will resist wear and not crack or perish. and also be pliable, while the saving
in labour required to be expended is great and the goods require less time in
manufacture.
Improvements in the Manufacture of Compositions having as a Basis
Oxidized Oil or Oxidized Oil and Fibrous Material.
I, CHARLES JAMES GRIST, of 20. Gracechurch Street, in the City of London,
Electrical Engineer, 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 :-
This invention relates to improvements in the manufacture of compositions, for
waterproofing, engine and other packings, acid tank linings, electrical insulating
compositions, paints, anti corrosive composition and compositions for like uses,
golf balls, blocks for paving roads and ways, carriage brake blocks, tyres and tyre
covers for wheels of vehicles, mats and for other uses, and has reference to certain
modifications of such compositions as are described in the Specifications of Letters
Patent No. 21742, 15th November 1895 and No. 22574, 26th November 1895.
I take linseed or other drying oil and partially oxidize it by applying heat to
the vessel in which it is contained, having previously added litharge or other
suitable oxidizing agent, to a temperature of say 400° F. or upwards taking care

page_text: that it does not boil for more than say about 24 hours furthermore attention
should be given that the oil is kept stirred for about 48 hours, being continually
kept in motion by suitable apparatus which may be conveniently arranged on or
adjacent to the vessel for the purpose.
The oil is preferably then allowed to cool until it reaches about its normal tem-
perature.
I now take a suitable fibrous substance such for instance as jute, hemp, cotton,
animal fibre or other suitable fibre, in which the separate fibres composing the
mass are or can be made to be distinct and separable but at the same time of
uniform or substantially uniform character and taking care that the fibres shall
be clean and free from any deleterious foreign substance in mixture or adhereing
to them. These I free from the fibres by means of carding or other suitable
cleansing method.
I then spread and loosen the fibres subjecting them to the action of heated air
in order to remove as far as possible traces of aqueous moisture because any
moisture present militates against the success of the process.
The partially oxidized oil being now at about its normal temperature and the
fibres in a clean and dry condition, I immerse such fibres in a loosened and
graduated condition into the oil; the fibres are then immersed in the oil but imme-
diately taken out again and I attach great importance to these precautions.
The fibres thus dipped are placed in a hydro extractor of the usual or con-
venient pattern for the purpose of extracting the superfluous oil not actually
adhering to the fibres. Or the fibres in a loosened and evenly arranged or gradu-
ated condition may be placed in the hydro extractor and the oil poured directly
upon them by means of a tube with a rose attached, leading from the tank or
vessel containing the oil situated above the hydro extractor; or other suitable
method..
When this has been effected and the free oil has been thoroughly removed I
fake the fibres out of the extractor and each fibre is found to be covered at
intervals with small particles of oil which adhere to it. I now spread these
fibres as loosely as possible on wire gauze or other suitable netting or reticulate
or openwork surface and pass a current of heated air for suitable periods through
them by means of a revolving fan or other suitable air supplying means turning
every hour or so and redistributing the the fibres on the netting by suitable lifting
and turning means till each particle of oil is oxidized and dried.
Then I again immerse the fibres in the oil and throw off or remove the super-
fluous oil by means of the hydro extractor or its equivalent and more globules of
oil will be found to be adhering to portions of the fibres not covered after the
first dinning; then I repeat the drving process explained above and when dry I
immerse the fibres again and again removing surplus oil drying between each
dipping for sav 6 to 10 or even more repetitions of the operations already
described. but I find it necessary to employ a much higher velocity of revolution
to the hydro-extractor in order to effect the application at each successive dip-
pino with a more attenuated distribution of the oil over the surfaces of the fibres.
The number of the successive operations of dipping and drying with removal
of surplusage of oil will vary slightly according to the use the product is designed
to be put to.
If at each dip coarser or thicker applications of the oil were made the fibres
would be liable to become over charged with oil so that the moving heated air
would be unable to oxidize the whole sufficiently and the resulting product would
be useless for my purposes.
I now grind up the fibres treated as described above, until they become of a
homogeneous character.
This masticating or grinding I prefer to accomplish by means of rolls (running
at different surface speeds so as to obtain the desired effect) running at a high
speed.
cold and I add
The material is now placed in crushing rolls which I employ co

page_text: to it while the crushing is progressing whatever colouring or hardening matter is
desired such as French chalk, ochre, asbestos, or other suitable material adapted
to the particular purpose I have in view taking care that the fibrous treated
material is not allowed to become so heated as to injure it This I prevent by
occasionally stripping it off the rolls by means of a knife, gauge or the like suit-
able for the purpose.
When these materials are thoroughly mixed I allow the mixture to cool to about
the normal temperature and I then again place it in the crushing rolls and I
add 5% to 10% of powdered sulphur mixing it thoroughly in the same manner
as the coloring or hardening material.
My improved material as now delivered from the mixing rolls is passed through
heavy callenders and rolled into sheets ready for use and it can when cool be
stored away until required.
For mats, acid tank linings, carriage brake blocks, paving, cold packings and
other uses I proceed as follows:-
I roll the material into sheets of the required thickness and place them in
moulds of the required pattern (for mats) in a heated press. When properly
pressed I allow to cool before taking out, they can then if required be punched
to any pattern. In the case of cold packing. after running the material through
the callenders into sheets of the required thickness it can be then cut into the
required shape. For acid tank linings I place the sheets of material in which
no adulterant material has been mixed that the acid is likely readily to attack,
between smooth sheets of metal or other suitable substance in a hydraulic or vul-
canizing press where I can obtain sufficient pressure and heat to give the material
a close and smooth surface.
For brake blocks I take the sheets and work them again in the mixers adding
from 5% to 15% of hot resin or other suitable substance. I then roll into sheets
through warm callenders and place the sheets one upon another in a vulcanizing
press till the required thickness is obtained. I press these and take out when
cold then the material can be cut into the required shape. Or I may mould the.
material into the required shape when hot. For paving blocks I may add such
hardening matter as slate dust or other suitable material. The mixture can then
be placed in moulds and subjected to heat and pressure in a press or it can be
run into sheets and used in that form.
For paints, I make two solutions, the first containing a mixing of the material
of the required colour which has been reduced by the addition of about 33½%
of ketone or other suitable spirit as afterwards described under the head of water-
proofing.
The second solution is composed of shellac, resin. kowrie gum or other suitable
substance mixed in about equal proportions and reduced by the addition of about
20% of methylated spirits. I then mix the two solutions in proportion of about
5 narts of the first to one part of the second solution.
For anti corrosive and adhesive solutions I take the raw material as herein
afterwards described for waterproofing only I may add a little resin if necessary
(adhesive solution). I then add a larger proportion of spirit in order to reduce
it to a thinner consistency.
For waterproofing and like purposes such as bed sheeting, clothing, double
texture and other goods I may proceed as follows:-the material in sheets is again
put through the mixing rolls and then immersed in naptha, turpentine. ketone or
other suitable solvent till it assumes the proper consistency required for the pur-
pose. the superfluous spirit being carefully removed.
If ketone or similar spirit is used I find that a convenient method to employ is
as follows: break up the material and place it in a steam jacketted and closed
vessel containing the spirit, the vessel being provided with an arrangement of
revolving blunt knives fitted inside. The parts can be set in motion by steam
or other power and the material will be reduced to the proper consistency within
a short space of time and with small loss of spirit.

page_text: When operating with the use of turpentine or naptha I work the material again
and again through the crushing rolls then adding the spirit and working it until
it is in such a soft pliable condition that it will readily adhere to a material or
fabric under pressure or can be spread on with a knife or gauge.
It can be run on to the fabric in any convenient thickness by passing the
materials to be combined through heavy callenders or rolls and within a few
hours afterwards it will be ready for use, or it can be spread on fabric in very
thin layers by the ordinary spreading machines such as are in use in rubber
factories by means of a knife or gauge. Or I take the material after the drying
operation is finished, and without putting it through a grinding and crushing
process, place it in a vessel containing a ketone or other suitable spirit which will
soften or dissolve the oil so that I shall be able to remove it from the fibres by
means of a wringing or other suitable arrangement; (or use boiling water instead
of a spirit but in such case after the oil is removed from the fibres great care
must be taken that all moisture is thoroughly removed). I then remove the
surplus spirit by evaporation or otherwise till the oil assumes a suitable consis-
tency for the purpose I have in view.
For insulating compositions for electrical purposes I proceed as follows:-
during the process of grinding and crushing the material I add a large percentage
of sulphur between 15% and 20%-and when this is thoroughly worked into
the material I add from 5% to 25% of gutta percha or other, suitable material or
compounds of materials for the purpose of giving enhanced tenacity to the com-
pound, subjecting the whole to the action of crushing rolls as before and rolling
it into sheets by means of heavy callenders or rolls.
When cool it may be stored away for use till required and is ready to be
applied to practical use. It may if desired be subjected to a vulcanizing process
of any ordinary or convenient kind such as heating it in a steam jacketted vessel,
without or with the gutta percha.
then
When it is necessary to soften the material for coating wire or other purposes
I crush the sheets of material again in the rolls which are warm and
transfer it immediately to the feeding rolls of a wire covering machine the
machine being heated all round by steam likewise the nozzle and die through
which the material passes on to the wire.
Or I take the sheets of material and soften them by means of a spirit
solvent such as naptha or turpentine or other suitable method in the manner
above described for waterproofing and other purposes.
The material can now be placed in a wire coating machine of usual or con-
venient pattern for electrical purposes but when the wire appears to be satis-
factorily coated with the material it is run through a hot air chamber in order
that any solvent spirit still retained in it may be evaporated and the material
may be afterwards subjected to a vulcanizing process. Or again, I may take the
sheets of material and after crushing them in the rolls run them into thin sheets
by means of heavy callenders which be then cut into strips and tape the material
onto the wire by means of any of the known taping machines. For any of the
above methods for insulating wire I may use the oxidized oil which has been
removed from the fibres in the manner before mentioned.
For tyres, shoe soles, valves, golf balls, engine packing, some kinds of mats
and other uses I proceed as follows:-I work the material after the oxidizing
process is completed thoroughly in the mixing rolls adding 10% to 20% of
flowers of sulphur
I then place the material in a steam jacketted vessel heated with steam which
may be of a temperature of 270° F. for a period of say 10 hours. Care must be
taken that the material is not so overheated that it is charred. I then take the
material and again place it in the rolls and I sometimes add adulterant matter
such as whitening plumbago, waste vulcanized rubber, rubber, gutta percha or
other suitable material or materials for the purpose either of cheapening the

page_text: resulting product or of giving it increased resiliency and tenacity according to
the purpose
I have in view.
The proportions in which the materials are used varies greatly according to the
quality required. When these are thoroughly mixed I add from 5% to 10%
of flowers of sulphur and thoroughly mix in the rolls. For solid tyres I take
the mixing without the addition of gutta percha or waste vulcanized rubber, and
place it in a squirting machine and force it by that means through a die which
gives to it the required shape. I then place it in moulds and run these into a
vulcanizing press heating it up to about 270° F. for a period of say 3 hours.
The tyres are then when cold ready for use.
For valves, shoesoles, engine packings, mats and other uses I take the mixing,
without gutta percha and place it in moulds of the required shape then transfer
the moulds into a vulcanizing press heated up to about 260° F. for varying lengths
of time-from 10 minutes upwards according to the purpose for which it is to
be used and the quality required. For golf balls I take the oxidized oil and fibre
after it has been treated in the steam jacketted vessel and work it thoroughly in
the mixers. I then sometimes add from 10% to 50% of gutta percha or other
suitable material or materials and thoroughly mix. I take the resulting mixture
and place it when warm in moulds of the required shape, which are placed in a
press. The balls can afterwards be taken out and painted in the ordinary manner.
For steam packings I sometimes take the oxidized oil and fibre, treated as
described, in the steam heated vessel and add colouring or hardening matters or
other suitable materials and work it thoroughly in the mixers. I then run it
through the callenders into sheets afterwards placing it in a hydraulic vulcan-
izing press between smooth sheets of metal or other suitable substance to obtain a
good surface. For electrical insulation in a hard form or in the form of a vul-
canite or for like uses I submit the mixing to a greater degree of heat and
pressure.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is
1. The herein before described method of manufacturing compositions having as
a basis oxidized oil and fibrous material whereby a greater percentage of oil to
fibre is attainable without detriment to the utility of the composition by applica-
tion to the fibre of the oil in more attenuated or finer particles by the use of
an increased number of repetitions of the applications of oil and a greatly
increased speed of revolution of the extractor used to remove the surplus oil, as
set forth.
2. In the manufacture of compositions having as a basis oxidized oil, the method
of obtaining oxidized oil in bulk by the oxidation of the oil in attenuated particles
whilst supported on fibres and then the removal of the oxidized oil from such
fibres, by a process of solution, or softening and mechanical separation, as set
forth.
3. The various compositions of matters having as a basis oxidized oil or oxidized
oil and fibrous material and their manufacture as herein before set forth.
Dated the 27th day of September 1899
WM: BROOKES & SON,
55 & 56, Chancery Lane, London, Agents for the Applicant.