Uninflammable Nitro-cellulose Products.
Year: 1898

page_text: PROVISIONAL SPECIFICATION.
Uninflammable Nitro-cellulose Products.
I, LUCIEN LOUIS BÉTHISY, of 71, Boulevard Voltaire, Paris, France, Chemist,
do hereby declare the nature of this invention to be as follows:-
My invention consists of a new compound or product having a base of cellulose
(such as flax, hemp, cotton, etc.,) the said compound being produced either in the
solid and plastic, or in the liquid, state. The said product has the quality of
being uninflammable in the solid or plastic state while in the liquid condition
it is adapted to form a coating or varnish for celluloid and the like whereby
to diminish or altogether destroy their inflammability.
The manufacture of the plastic or solid product comprises a series of stages
as hereinafter described, of which the first the conversion of vegetable cellulose
into pyroxilin. For this purpose 6 lbs. of cellulose are steeped for about two
hours in a mixture of:-
Sulphuric acid at 66° Beaumé about 132 lbs.
Nitric acid at 132 (sp. gr.) about 44 lbs.
the said mixture being maintained at a temperature of 85° Fahrenheit in the
usual way.
The nitro-cellulose is then centrifugated until it contains only
about half its weight of acid, after which it is steeped in fuming sulphuric acid.
The second operation is pulping and bleaching.
The nitro-cellulose or
pyroxilin is reduced in a paper-pulping machine and is then washed with
carbonate of soda and afterwards in water; it is then transferred to the bleaching
vats and about three times its volume of water is added of which three-fourths
is run off in order to remove the carbonate of soda; about 2% of permanganate
of potash solution is added to destroy the organic colouring matters, and after
standing an hour the tank is filled up with water and stirred; the pulp is then
washed in abundance of water after which an aqueous solution of sulphurous acid
is added; it is then drained and let rest for about twenty-four hours and then centri-
fugated until the pulp contains no more than about 50% of water.
The third operation is partial desiccation and grinding.
effected in three stages in cone mills.
The grinding is
At the first grinding, from 10% to 15%
of camphor or naphthaline only is added. At the second grinding is added from
about 10% to 15% of desiccated albumen (egg or blood) as well as from
10% to 15% of mica in powder, if it is required to produce a transparent incom-
bustible composition, or from 10% to 15% of alum and powdered asbestos, if an
opaque composition is desired. At the third grinding, suitable colouring matters
are added according to the desired colour of the product.
The fourth operation is the conversion into collodion. The above described
mixture is first pressed under hydraulic pressure of about 2000 lbs. per square
inch into thin cakes which are then broken up and moistened with about 20%
of alcohol at 96° Gay Lussac, after which there is added 10% of the pasty
mixture undermentioned. Essential oil of lavender, cedar, birch, rosewood
generally any essential oil having a camphorated base and vaseline oil
or

page_text: dissolved in acetic ether with the addition of from 20% to 50%
(according to the desired degree of flexibility or rigidity of the product) of liquid
chloride of zinc at 45° Beaumé, and from 5% to 10% white gelatine.
paste is allowed to rest for twenty-four hours in a closed vessel before use.
The
The fifth operation is that of solidification and baking. The collodion thus
obtained is cut up into pieces of from ten to twenty pounds, which are kneaded
beween a pair of rolls heated to 60° C. until the paste has acquired a suitable
consistency, formed into sheets of about three-eighths of an inch thick which are
placed in a tightly closed receptacle for about twelve hours.
The material is then condensed into a compact homogeneous condition, for
which purpose the block pressers ordinarily used for condensing celluloid are
used.
The material is then sliced into sheets of required thickness by the same
means as are employed for celluloid.
The essential property of the plastic celluloid composition thus produced is
its uninflammability, a property due to the novel composition of the product
and more especially to the introduction therein of chloride of zinc. The celluloid
composition also possesses all the other properties of known products, having a
base of cellulose, such as celluloid, xylonite, etc., which are however highly
inflammable. By varying the proportions, this celluloid composition may be
rendered permanently flexible or as rigid as required and hence it can be used
like celluloid for making collars, cuffs, and other imitation linen goods, and
also for making waterproof fabrics, toys, and fancy goods, artificial leaves and
flowers, and for electrical purposes, etc., as well as for many other uses for which
celluloid and the like is unsuitable on account of its inflammability.
The composition in the liquid form is the collodion obtained at the fourth
operation as herein described. It is an incombustible varnish suitable as a
coating for celluloid and the like, whereby to render the same uninflammable.
The celluloid may in certain cases be exposed to the action of the vapours of
glacial acetic acid and afterwards dipped into the liquid incombustible composition
for the purpose of being rendered uninflammable.
Dated this 25th day of Nov 1808
A. M. & WM. CLARK,
Chartered Patent Agents,
53, Chancery Lane, London.
Uninflammable Nitro-cellulose Products.
I, LUCIEN LOUIS BÉTHISY, of 71, Boulevard Voltaire, Paris, France, Chemist,
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 consists of a new compound or product having a base of cellulose
(such as flax hemp, cotton, etc.,) the said compound being produced either in the
solid and plastic, or in the liquid state. The said product has the quality of
being uninflammable in the solid or plastic state while in the liquid condition
it is adapted to form a coating or varnish for celluloid and the like products
whereby to diminish or altogether destroy their inflammability.
The manufacture of the plastic or solid product comprises a series of stages
as hereinafter described, of which the first is the conversion of vegetable cellulose

page_text: into pyroxilin. For this purpose 6½ lbs. of cellulose are steeped for about two
hours in a mixture of: -
Sulphuric acid at 66° Beaumé about 132 lbs. ;
Nitric acid at 132 (sp. gr.) about 44 lbs.
the said mixture being maintained at a temperature of 85° Fahrenheit in the
usual way. The nitro-cellulose is then centrifugated until it contains only
about half its weight of acid, after which it is steeped in fuming sulphuric acid.
The second operation is pulping and bleaching. The nitro-cellulose or
pyroxilin is reduced in a paper-pulping machine and is then washed with
carbonate of soda and afterwards in water; it is then transferred to the bleaching
vats and about three times its volume of water is added of which three-fourths
is run off in order to remove the carbonate of soda; about 2% of permanganate
of potash solution (containing 50% permanganate, and 50% water) is added to
destroy the organic colouring matters, and after standing an hour the tank is
filled up with water and stirred; the pulp is then washed in abundance of water
after which an aqueous solution of sulphurous acid is added; it is then drained
and let rest for about twenty-four hours and then centrifugated until the pulp
contains no more than about 50% of water.
The third operation is partial desiccation and grinding. The grinding is
effected in three stages in cone mills. At the first grinding, from 10% to 15%
of camphor or naphthaline only is added. At the second grinding is added from
about 10% to 15% of desiccated albumen (egg or blood) as well as from
10% to 15% of mica in powder, if it is required to produce a transparent incom-
bustible composition, or from 10% to 15% of alum and powdered asbestos in
equal parts, if an opaque composition is desired. At the third grinding suitable
colouring matters are added according to the desired colour of the product.
The fourth operation is the conversion into collodion. The above described
mixture is first pressed under hydraulic pressure of about 2000 lbs. per square
inch into thin cakes which are then broken up and moistened with about 20%
of alcohol at 96° Gay-Lussac, after which there is added 10% of the pasty
mixture undermentioned. Essential oil of lavender, cedar, birch, rosewood, or
generally any essential oil having a camphorated base, and vaseline oil in
equal proportions, dissolved in acetic ether with the addition of from 20% to 50%
(according to the desired degree of flexibility or rigidity of the product) of liquid
chloride of zinc at 45° Beaumé, and from 5% to 10% of white gelatine. The
paste is allowed to rest for twenty-four hours in a closed vessel before use.
The fifth operation is that of solidification and baking. The collodion thus
obtained is cut up into pieces of from ten to twenty pounds which are kneaded
between a pair of rolls heated to 60° C, until the paste has acquired a suitable
consistency, and formed into sheets of about three-eighths of an inch in thickness
which are placed in a tightly closed receptacle for about twelve hours.
The material is then condensed into a compact homogeneous condition, for
which purpose the block pressers ordinarily used for condensing celluloid are
used.
The material is then sliced into sheets of the required thickness by the same
means as are employed for celluloid.
The essential property of the plastic celluloid composition thus produced is
its uninflammability, a property due to the novel composition of the product
and more especially to the introduction therein of chloride of zinc. The celluloid
composition also possesses all the other properties of known products, having a
base of cellulose, such as celluloid, xylonite, etc., which are however highly
inflammable. By varying the proportions this celluloid composition may be
rendered permanently flexible or as rigid as required and hence it can be used
like celluloid for making collars, cuffs, and other imitation linen goods, and
also for making waterproof fabrics, toys, and fancy goods, artificial leaves and
flowers, and for electrical purposes, etc., as well as for many other uses for which
celluloid and the like is unsuitable on account of its inflammability.

page_text: .The composition in the liquid form is the collodion obtained at the fourth
operation as herein described. It is an incombustible varnish suitable as a
coating for celluloid and the like, whereby to render the same uninflammable.
The celluloid may in certain cases be exposed to the action of the vapours of
giacial acetic acid and afterwards dipped into the liquid incombustible composition
for the purpose of being rendered uninflammable.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed I declare that what
I claim is: -
1. A new article of manufacture composed of nitro-cellulose, camphor, or
naphthaline, albumen, powdered mica, or alum, and powdered asbestos, colouring
matter (if desired) alcohol, essential oil, vaseline oil, acetic ether, zinc chloride,
and white gelatine, said matters being incorporated and treated in the manner
herein before described in the proportions specified for producing a liquid collodion,
then dried and solidified if necessary by the usual means of drying and solidifying
celluloid for the production of an uninflammable plastic solid substance having
a base of nitro-cellulose for use as a substitute for ordinary celluloid for all
purposes for which celluloid is used.
2. A new article of manufacture resulting from the preparation apart of a
paste containing essential oil, vaseline oil dissolved in acetic ether, zinc chloride,
and white gelatine; the incorporation of said paste in a previously prepared
mixture of nitro-cellulose, camphor, albumen, powdered mica (or powdered alum
and powdered asbestos) and alcohol and the treatment of the whole in the manner
herein before specified for producing a new liquid collodion which is then dried
and solidified if desired by the processes ordinarily employed for celluloid for
producing a new solid composition which is plastic and uninflammable and
adapted for use as a substitute for ordinary celluloid for all purposes for which
the latter is used.
Dated this 91at da...
T1
1000
A. M. & WM. CLARK,
Chartered Patent Agents,
53, Chancery Lane, London.