A New Composition, Forming a Sort of Artificial Silk for the Produc- tion of Threads or Filaments and Films and for Coating Threads, Fabrics, or Objects, and Apparatus Employed in the Manufacture of said Composition.
Year: 1889

page_text: Date of Application, 13th Feb., 1889
Complete Specification Left, 11th Nov., 1889-Accepted, 14th Dec., 1889
PROVISIONAL SPECIFICATION.
A New Composition, Forming a Sort of Artificial Silk for the Produc-
tion of Threads or Filaments and Films and for Coating Threads,
Fabrics, or Objects, and Apparatus Employed in the Manufacture
of said Composition.
01
i
I JULES HERRI DU VIVIER, of 61 Rue Blanche, Paris, France, Manufacturer do
hereby déclare the nature of this invention to be as follows:-
My Invention relates to a new composition, and to the preparation therefroin of
threads or filaments presenting the appearance and properties of silk obtained 'from
the cocoon.
The basis of my invention, is the combination formed by dissolving tri-nitro-cellu-
lose or tri-nitrated cotton in glacial acetic acid and the treatment of the matter so
obtained with various re-agents whereby it acquires the appearance and properties of
natural silk.
The processes of manufacturing the composition comprise the preparation of the
tri-nitro cellulose; and its mixture with the other constituent elements, and the
subsequent treatment of the composition for the purpose of converting it into artificial
silk.
4
These several operations are herein described with reference to the accompanying
drawings, figures 1 and 2 of which shew front and rear elevations of an apparatus
in two positions for the preparation of the tri-nitro cellulose or tri-nitrated gun cotton.
Figures 3 and 4 shew views of opposite sides of the, apparatus. Figure 5 shews an
elevation, figure 6 a section, and figure 7 a plan, of a machine for mixing the con-
stitutive ingredients of the artificial silk. Figure 8 shews a diagram of the method
of filtering the composition. "The same letters of reference indicate like parts in all
the figures.
17.
The preparation of the tri-nitrated cotton comprises two operations-alkalization
and nitrification. To alkalize the cotton, dissolve 4 kilogrammes of caustic soda
in 20 litres of water, let cool and add 80 litres of ammonia of commerce at 220 B. The
cotton is steeped in this bath, in the proportion of about 1 kilogramme of cotton to
10 litres of the solution, for three days and nights, stirring once a day, after which
time the cotton is removed from the bath, pressed, and washed in abundance of
water until completely neutral. The bath may serve again for another operation. but
less rapidly, and if to be used again it is preferably to mix it with a fresh bath.
The cotton, when dry, is carded in order to well open the fibres and is then ready
for nitrification which is performed by means of the apparatus represented in
figures 1 to 4. This apparatus consists of a stone ware vessel a, capable of resisting
the necessary temperature and pressure, provided with a hinged cover b of the same
material carefully ground and fixed by a cotter c passing through lugs on a hoop d
and engaging in the catch c on the locking bar fto which the cover b is attached.
The vessel a is clamped, in a ring and mounted upon a spindle g supported in a
bearing i carried by a fraine mounted to revolve about a horizontal axis in. bearings
on framing m by means of the worm gear n o. The vessel a receives rotary
motion about a horizontal axis at same time that it is rotated about its own axis by
means of the. bevel and spur gear pq8. The gearing is so proportioned that the
apparatus performs one and a half revolutions about the horizontal axis in about 5 to 6
minutes and makes about 20 revolutions about its own axis in the same time. To
charge the apparatus, about 20 kilogrammes of refined saltpetre pounded and heated
to about 45 is first introduced upon which is then poured in three or four portions,
about 30 kilogrammes of pure sulphuric acid at 66° B. and the mass is then stirred
until the liquid is clear and free from lumps. The temperature of. the mixture
should be about 85° C, and if below this it should be heated by steam or if above

page_text: this temperature it should be cooled down to this point. One kilogramme of cotton
is then introduced into the vessel in small tufts, the lid closed, and the apparatus is
revolved as above described for about 5 or 6 minutes, and the motion then arrested
with the vessel a inverted, when on removing the pin c the lid will open, as shewn in
dotted lines.in figure 1 and the contents will be discharged into a water tank t placed
beneath it. The interior of vessel a is then washed out with a jet of water under
pressure. The cotton is then thoroughly washed with 10 to 12 changes of water,
after which, the nitrated cotton is dried in a stove and is then ready for use. In
order to assist the mixing action in the vessel, lumps of stoneware or other solid
matters are introduced therein together with the cotton or a chain may be used for
the purpose each link being made zufficiently heavy and of a material not acted on
by the substances present. The proportions above indicated are suitable for a vessel
of 120 litres capacity, and would vary accordingly.
The tri-nitrated cotton having been thus obtained, the artificial silk is next prepared
as follows: The three following solutions are first prepared - (a) a solution of
gutta percha in sulphide of carbon in the proportions of 25 grammes of gutta-percha
to 200 cubic centimetres of solvent (b) a solution of isinglass in glacial acetic acid
in the proportion of 10. grammes of the former to 200 cubic centimetres of the
latter (c) a solution of tri-nitrated cotton in glacial acetic acid in the proportion of
7.grammes of cotton per 100 cubic centimetres of solvent. These three solutions are
mixed in such quantities that the mixture will contain the following relative
proportions:-
Gutta percha
0.5 gramme
0.01 gramme of glycerine and one drop of castor oil are added and the whole
kneaded together in any suitable mixing apparatus, but preferably in that represented
in figures 5, 6, and 7, consisting of a cylinder 1 confiued between top and bottom
plates 2 and 3 united by bolts 4, and cotters 5. Within the cylinder is mounted a
shaft 6 provided with stirrers 7 and driven by bevel gear 89 from a shaft 10 (turning
in bearings 12 on the top plate 2) to which a variable speed is imparted by the speed
pulleys 11. When an intimate mixture is effected the viscous liquid is subjected to
à double filtration first through a coarse, and then through a more closely woven,
fabric, the filtration being aided by a vacuum or pressure. In the latter case, the
apparatus may be simply arranged, as shewn in figure 8, in which the matter to be
filtered is placed in a receiver 13 covered at bottom with filtering fabric 14,and
resting in a funnel 15 inserted in the mouth of a bottle 16. The mouth of receiver 13
communicates by a pipe 17 with the top of a receiver 18 whose lower end commu-
nicates at 19, by a pipe 20, with the lower part of an open receiver 22, at a higher
level, filled with liquid. On opening cock 21 the liquid passes from 22 to 18, com-
pressing the air contained therein which presses upon the matter contained in
receiver 13 and forces it through the filtering surface 14 into the flask 16.
The viscous or semi-fluid matter thus obtained constitutes the basis of the new
artificial silk and from it threads may be obtained by ejecting it through a small
orifice under water, the thread thus obtained being then subjected to the action of
certain chemical agents, as hereinafter described, in order to impart to it the.
resistance and aspect of real silk as well as to render it more or less incombustible.
For this purpose, the thread is caused to pass through a series of baths, while suitably
guided by any mechanical means, viz. (1) a soda bath, for removing the acetic
acid in excess (2) an albumen bath at 3 per 1000 for animalizing the matter (3) a
bichloride of mercury bath at 54 per 1000 which coagulates the thread, the coagula-
tion being completed by passing the thread from this bath into an atmosphere of
carbonic acid gas. In order to lessen the combustibility of the thread, it is- first
passed through a 10% bath of ammonia and then through a bath of, sulphate of
alumina which precipitates in the pores of the material a deposit of alumina. The.
;

page_text: thread is then passed through a second bath of albuinen at 3 per 1000 for the purpose
of lubricating it and rendering it suitable for winding or reeling, etc.
It will be understood that the proportions hereinbefore indicated for the several
constituent elements of the artificial silk, and also of the baths for treating the same,
may be varied, without departing from the invention, and that the elements may be
replaced by others which are chemically equivalent as regards the effect produced.
For example, to obtain a lustrous thread instead of a matt thread, the gutta percha,
isinglass and glycerine may be omitted, the material being constituted by the following
elements only
Tri-nitrated cotton
Acetic acid
Castor oil
360 grammes
6 litres
. 90 grammes.
In this case, the thread is passed as before through a bath of albumen for the
purpose of animalizing it and coagulation is effected by means of a 3 per 1000
solution of phenic acid in dilute alcohol. Or the thread may be first passed through
a 5% bath of bisulphite of soda, then through a 3 per 1000 bath of albumen, and
lastly through a per 1000 coagulating bath of phenic acid. The bisulphate of soda
possesses the advantage of bleaching the material.
·
My Invention is quite independent of the apparatus for forming the material into
threads or for passing it through the baths, and is based solely upon the composition
of the artificial silk, and the mode of preparing, and methods of treating, the same
as described.
The artificial silk may be applied not only to the production of threads but also
for making films or sheets in imitation of silk, or the material inay be deposited and
applied as a coating upon ordinary textile threads, tissues, or other goods, for the
purpose of imparting to them a silky appearance.
Dated this 15th day of February food.
J. H. DU VIVIER.
By A. M. & Win. Clark,
53, Chancery Lane, London, Patent Agents.,
A New Composition Forming a Sort of Artificial Silk, for the Produc-
tion of Threads or Filaments and Films, and for Coating Threads,
Fabrics, or Objects, and Apparatus Employed in the Manufacture
of said Composition,
I JULES HENRI DU VIVIER of 61 Rue Blanche, Paris, France, Manufacturer,
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 a new composition and to the preparation therefrom of
threads or filaments presenting the appearance and properties of silk obtained from
the cocoon.
The basis of my invention is the combination formed by dissolving tri-nitro-
cellulose or tri-nitrated cotton in glacial acetic acid and the treatment of the matter
so obtained with various re-agents whereby it acquires the appearance and properties
of natural silk:
The processes of manufacturing the composition comprise the preparation of the
tri-nitro cellulose, and its mixture with the other constituent elements, and the
subsequent treatment of the composition for the purpose of converting it into artificial
silk.
The several operations are herein described with reference to the drawings left
with my provisional Specification figures 1 and 2 of which shew front and rear elevations
of an apparatus in two positions for the preparation of the tri-nitro cellulose or tri-
nitrated gun cotton. Figures 3 and 4 shew views of opposite sides of the framing

page_text: of the apparatus. Figure 5 shews an elevation, figure 6 a section, and figure 7 a
plan, of a machine for mixing the constitutive ingredients of the artificial silk.
Figure 8 is a diagram showing the method of filtering the composition. The same
letters of reference indicate like parts in all the figures.
The preparation of the tri-nitrated cotton comprises two operations-alkalization
and nitrification. To alkalize the cotton, dissolve 4 kilogramines of caustic soda in
20 litres of water, let cool and add 80 litres of aminonia of commerce at 22° B.
The cotton is steeped in this bath, in the proportion of about 1 kilogramme of cotton
to 10 litres of the solution, for three days and nights, stirring once a day, after which
time the cotton is removed from the bath, pressed, and washed in abundance of water
until completely neutral. The bath may serve again for another operation but less
rapidly, and if to be used again it is preferable to mix it with a fresh bath. The
cotton, when dry, is carded in order to well open the fibres and is then ready for
nitrification which is performed by means of the apparatus represented in figures 1
to 4. This apparatus consists of a stone ware vessel a, capable of resisting the
necessary temperature and pressure, provided with a hinged cover b.of the same
material carefully ground and fixed by a cotter c passing through lugs on a hoop d
and engaging in the catch e on the locking bar f to which the cover b is attached.
The vessel a is clamped in a ring h mounted upon a spindle g supported in a bearing i
carried by a frame k, mounted to revolve about a horizontal axis in bearings on
framing m by means of the worm gear n v. The vessel a receives rotary motion
about a horizontal axis at same time that it is rotated about its own axis by means of
the bevel and spur gear p q r s The gearing is so proportioned that the apparatus
performs one and a half revolutions about the horizontal axis in about 5 to 6 minutes
and makes about 20 revolutions about its own axis in the same time.
To charge the apparatus, about 20 kilogrammes of refined saltpetre pounded and
beated to about 45° is first introduced, upon which is then poured, in three or four
portions, about 30 kilogrammes of pure sulphuric acid at 66° B. and the mass is then
stirred until the liquid is clear and free from lumps. The temperature of the mixture
should be about 85° C. and if below this it should be heated by steam or if above this
temperature it should be cooled down to this point. One kilogramme of cotton is
then introduced into the vessel a in small tufts, the lid closed, and the apparatus is
revolved as above described for about 5.or 6.minutes, and the motion then arrested
with the vessel a inverted when on removing the pin c the lid will fall open, as shewn
in dotted lines in figure 1 and the contents will be discharged into a water tank t
placed beneath it. The interior of vessel a is then washed out with a jet of water
under pressure. The cotton is then thoroughly washed with 10 to 12 changes of
water, after which the nitrated cotton is dried in a stove and is then ready for use.
In order to assist the mixing action in the vessel, lumps of stone-ware or other
solid matters are introduced therein together with the cotton or a chain may be used
for the purpose each link being made sufficiently heavy and of a material not acted
on by the substances present.
The proportions above indicated are suitable for a vessel of 120 litres capacity, and
would vary accordingly.
The tri-nitrated cotton having been thus obtained, the artificial silk is next prepared
as follows:-The three following solutions' are first prepared-(a) solution of gutta
percha in sulphide of carbon in the proportions of 25 grammes of gutta-percha
to 200 cubic centimetres of solvent (6) a solution of isinglass in glacial acetic acid in
the proportion of 10 grammes of the former to 200 cubic centimetres of the latter (c)
a solution of tri-nitrated cotton in glacial acetic acid in the proportion of 7 gramines
of cotton per 100 cubic centimetres of solvent. These three solutions are mixed in a
cold state in such quantities that the mixture will contain the following relative
proportions:-

page_text: To this mixture are then added 0.01 gramme of glycerine and one drop of castor
oil and the whole kneaded together in any suitable mixing apparatus, but preferably
in that represented in figures 5, 6, and 7, consisting of a cylinder 1 confined between
top and bottom plates 2 and 3 united by bolts 4 and cotters 5. Within the cylinder
is mounted a shaft 6 provided with stirrers 7 and driven by bevel gear 89 from
a shaft 10 (turning in bearings 12 on the top plate 2) to which a variable speed is
imparted by the speed pulleys 11. When an intimate mixture is effected the viscous liquid
is subjected to a double filtration first through a coarse, and then through a' more
closely woven, fabric, the filtration being aided by a vacuum or pressure. In the
latter case, the apparatus may be simply arranged, as shewn in figure 8, in which the
matter to be filtered is placed in a receiver 13 covered at bottom with filtering
fabric 14 and resting in a funnel 15 inserted in the mouth of a bottle 16. The
mouth of receiver 13 communicates by a pipe 17 with the top of a receiver 18 whose
lower end communicates at 19, by a pipe 20, with the lower part of an open
receiver 22, at a higher level, filled with liquid. On opening cock 21 on pipe 20 the
liquid passes from 22 to 18, compressing the air contained therein which presses
upon the matter contained in receiver 13 and forces it through the filtering surface 14
into the flask 16.
The viscous or semi-fluid matter thus obtained constitutes the basis of the new
artificial silk and from it threads may be obtained by ejecting it through a small
orifice under water, the thread thus obtained being then subjected to the action of
certain chemical agents, as hereinafter described in order to impart to it the
resistance and aspect of real silk as well as to render it more or less incombustible.
For this purpose, the thread is caused to pass through a series of baths, while suitably
guided by any mechanical means, viz. :-(1) a soda bath, for removing the acetic acid
in excess (2), an albumen bath at 3 per 1000 for animalizing the matter (3) a
bichloride of mercury bath at 54 per 1000 which coagulates the thread, the coagula-
tion being completed by passing the thread from this bath into an atmosphere of
carbonic acid gas. In order to lessen the combustibility of the thread, it is first
passed through a 10% bath of ammonia and then through a bath of sulphate of
alumina which precipitates in the pores of the material a deposit of alumina. The
thread is then passed through a second bath of albumen at 3 per 1000 for the
purpose of lubricating it and rendering it suitable for winding or reeling, etc.
It will be understood that the proportions hereinbefore indicated for the several
constitutent elements of the artificial silk, and also of the baths for treating the same,
may be varied, without departing from the invention, and that the elements may be
replaced by others which are chemically equivalent as regards the effect produced.
For example, to obtain a lustrous thread instead of a matt thread, the gutta percha,
isinglass and glycerine may be omitted, the material being constituted by the following
elements only :-

page_text: applied as a coating upon ordinary textile threads, tissues, or other goods, for the
purpose of imparting to them a silky appearance.
Having now particularly described and ascertained the nature of my said Inven-
tion, and in what manner the same is to be performed, I declare that what. I
claim is-
1st. As a new article of manufacture, artificial silk obtained by the processes and
methods herein described.
.
2nd. The apparatus for preparing the trinitrated cellulose or cotton, substantially;
as herein described with reference to figures 1, 2, 3, and 4.
3rd. The mode of preparing, mixing, and filtering, the viscous matter forming
the basis of the artificial silk, substantially as described with reference to figures 5
to 8.
4th. The herein described combination of baths for producing artificial silk from a
composition consisting essentially of tri-nitrated cotton in solution in glacial acetic
acid or from one or other of the compositions before specified.
A
5th. The application of the matters and means hereinbefore specified for the
production of threads and films of artificial silk as well as for coating all kinds
of textile threads, fabrics, or objects, with artificial silk, substantially as described.
Dated this 11th day of November 1889.
J. H. DU VIVIER.
By A. M. & Wm. Clark,
53, Chancery Lane, London, Patent Agents.