An improved manufacture of Aruncial suk like Filaments from Viscous Liquids, and Apparatus for that Purpose.
Year: 1886

page_text: An improved manufacture of Aruncial suk like Filaments from
Viscous Liquids, and Apparatus for that Purpose.
I, COMTE HILAIRE DE CHARDONNET, of 20 Place de l'etat Major, Besancon
Doubs, France, do hereby declare the nature of this invention to be as follows:-
This invention relates to the manufacture of artificial filaments resembling silk
from viscous liquids.
For this purpose purified cellulose is nitrated by any suitable known process in
order to render it soluble in a mixture of alcohol and ether. Pyroxyline is
dissolved in a mixture of four parts of ether with six parts of alcohol, and a
reducing metallic protochloride such as of iron, chromium, manganese, tin, &c is
dissolved in alcohol, together with a small proportion of an organic oxydisable base,
such or quinine or aniline.
Furthermore, a suitable coloring matter soluble in alcohol is added. The two
solutions are mixed and allowed to rest until the reaction is complete. This com-
pound, which I term the mother liquid of the artificial silk, will solidify on the
evaporation of the solvent, forming a new kind of celluloid.
When the solution is allowed to flow through a small orifice into certain liquids,
such as water, it at once solidifies, forming a filament which in the first instance is
hollow, containing solution within it, and which on being withdrawn from the
water hardens in the air.
The mother liquid is for this purpose introduced into a closed receptacle in
which the requisite pressure is maintained by an air pump. This recipient has at
its lower part a tubular extension surrounded by a jacket through which cold
water is made to circulate, and within the tubular extension are situated the lower
ends of upwardly directed nozzles through the upper ends of which the mother
liquid issues. These nozzles consist of a glass tube terminating at the upper end
in a contracted orifice of from th to th millimetre in diameter, and surrounded
by a second tube rising somewhat above the orifice of the nozzle. A current of
cold water is made to flow slowly through the outer tube and to overflow its upper
end, whence it falls down into a trough below, which conducts it back to the
reservoir. Thus the filament of mother liquid issuing in an upward direction from
the nozzle is brought in contact with the current of water and at once solidifies, so
that it can be at once led upwards over a revolving reel or bobbin on which it is

page_text: wound. The outer tube slides with a water tight joint upon the nozzle, so a
can be lowered to uncover the orifice of the nozzle when no filament is issuing.
In order to replace the filament upon the reel should it break at any time, an
elbow lever carrying at its end a spring fork or clip is moved periodically so as to
embrace the nozzle so as to sieze the broken end of the filament, and then to
sweep upwards with the same in a circular arc over the reel or bobbin, and when
in its highest position the clip is brought in contact with a brush surface, which
separates the end of the filament therefrom, causing it to fall upon the bobbin
below, which continues to wind it up again.
By preference two or more of the filaments are united together before passing
on to the bobbin, for which purpose two or more of the nozzles are arranged side
by side, and the filaments issuing from these are first led through guides which
keep them apart until they are sufficiently hardened, after which they pass between
inclined guides which lead them together.
According to another arrangement the filaments as they issue from the nozzles
are fed forward by a slowly rotating cylinder with soft surface such as caoutchouc
or felt partly immersed in the water the speed of rotation being made to correspond
with the rate of issue from the nozzles.
If there be a stoppage in the flow, the bead formed at the orifice of the nozzle is
at once drawn forward, and in order to avoid entanglement of the loose end thus
produced, two or more of the filaments are united in bundles on leaving the
cylinder, this being effected by simple adhesion either in passing the filaments in
the desired groups between the teeth of a comb having a to and fro motion, or by
applying to the surface of the cylinder conical guides that collect the filaments
together, or by other suitable means. The above described apparatus is enclosed
in a casing, made air tight with the exception of an exit tube for leading the
alcoholic vapour given. off to a condenser, and of small apertures through which
the filaments issue, and whence they are led to a hot air drying apparatus, where
they are kept as long as may be necessary for them to barden completely. The
filaments are then wound in groups upon bobbins or reels having a double rotary
movement so as to impart to them a certain torsion at the same time that they are
wound up, the mechanism used for this purpose being similar to that for spinning
and winding cocoon silk.:
The drying apparatus consists of two closed vertical chambers communicating
with each other at top and bottom. The one chamber in which the filaments are
made to circulate and in which they are wound on the bobbins, is heated, while
the other one is cooled by a current of water or by refrigerating apparatus. The
air rises in the hot chamber, drying the filaments, and the vapours are condensed
therefrom in the cold chamber, the same body of air being made to circulate
continuously through the two chambers, carrying the condensible vapours from the
one to the other. The condensed water is separated from the alcohol either by
freezing or by rectification. The alcohol and ether need not be separated and can
Berve repeatedly for dissolving fresh quantities of pyroxyline.
By introducing into the drying apparatus a neutral or reducing gas instead of
air, solvents that would be too oxydisable in air, such as methylene, may be used.
Instead of uniting several filaments while still in a moist or soft condition
as described, they may sometimes be wound separately upon bobbins on passing
from which they are then united and spun directly into threads in a similar
manner to spinning cocoon silk. In this arrangement the filament is made to pass
directly from the nozzle into a separate trough through which a current of water
circulates, the water being led thence into an alembic where the alcohol is
separated therefrom, after which it is again conveyed to the troughs. On issuing
from the water bath the thread is led more or less vertically upward and is wound
upon a bobbin, the filament being supported on V-shaped guides that have a to
and fro motion, in a similar manner to ordinary spinning machinery, so that the
convolutions have time to dry before being covered over. For making good
fractures of the filaments in this arrangement there is provided a spring arm

page_text: having a pincer-like extremity that embraces the end of the nozzle this being
supported by a lever, by means of which the attendant, as soon as he observes the
fracture of a thread, moves the arm from the nozzle to the edge of the winding
bobbin, whereby the pincers of the arm are made to carry a fresh filament from the
former to the latter.
The edge of the bobbin is formed with an adhesive surface or with bristles, or of
felt, to which the filament adheres as it is presented thereto by the arm, which is
then moved back again by the attendant through a different path, so that it may
not interfere with the newly formed filament,
The above action may be rendered automatic by causing a very light lever to
rest upon the filament on its way to the bobbin, which lever in falling when the
filament breaks makes an electrical contact whereby the above described apparatus
is put in action.
The above described troughs and winding bobbins are all enclosed in the hot
chamber of the drying apparatus. The circulation of the air in the latter may be
accelerated by a pump or fan.
The threads prepared by spinning the said filaments may be treated with a
hygrometric or non-combustible preparation, and the fabric woven therefrom may
be treated with an incombustible dressing, such as a mixture of gelatine glycerine
and sugar.
In place of the water tank or trough above described, may be used a glass tube
through which water is made to circulate.
It is advisable to impart to the winding bobbin a to and fro motion in the
direction of its axis that is not synchronous with its revolutions; by this means
the filaments are wound on the bobbin in a serpentine manner, whereby the
consecutive convolutions are made to cross each other instead of lying straight
upon each other, and thus adhesion is more effectually prevented.

page_text: Viscous Liquids, and Apparatus for that Purpose.
I, COMTE HILAIRE DE CHARDONNET, of 20 Place de l'etat Major, Besancon,
Doubs, France 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:-
-
I
This invention relates to the manufacture of filaments resembling silk from
viscous liquids. For this purpose pyroxyline, produced by nitrating pure cellulose
along with 10 to 20 per cent of a reducing metallic protochloride, such as that of
iron, manganese, chromium or tin, and a small quantity, about per cent, of a
vegetable organic base, such as quinine, aniline, or rosaniline, is dissolved in
a mixture of parts of ether to 6 parts of alcohol. To this is added colouring
matter soluble in the mixture. It is of advantage to dissolve first the pyroxyline
in the greater part of the solvent, and the other ingredients in the residue of the
solvent and then to mix the two solutions. The proportions may be somewhat
varied as found by practice according to the nature of the pyroxyline used and the
strength or elasticity required in the filaments produced. When the collodion
liquid prepared as described flows through a small orifice into cold liquid such as
water, it comes out as a thread solid on its exterior which forms a sheath enclosing
a portion still 'liquid within, but the thread can be drawn out of the water and
being exposed to the air it becomes dry and solid throughout. For practically
producing filaments in this manner apparatus are employed such as are represented
in the accompanying drawings. Fig. 1 is a transverse section, and Fig. 2 is an
elevation of the end portion. Figs. 3 and 4 are respectively a section and elevation
of parts drawn to a larger scale, and Fig. 5 is a plan of the pincers. The collodion
solution well filtered is kept in a closed internally turned receptacle, under
a pressure of 2 to 3 atmospheres maintained by an air compressing pump. From
this receptacle it is led by a pipe A provided with a stop cock B, to the apparatus
along which the pipe A extends within a casing C through which cold water is
made to circulate issuing by the pipe a. On the upper face of the pipe A are
bosses into which are screwed nuts c that have fixed in them tubes d by thin
packing e of vulcanised caoutchouc or analogous material. Each of the tubes dis
connected to an upper glass tube i by a flexible impervious union f which may be.
of caoutchouc or fabric coated. with caoutchouc. The sectional area of passage
through this union can be varied by pinching it more or less by the screw g in the
clamp h of which Fig. 6 is a plan, thus adjusting the outflow of the liquid and
consequently the size of filament produced. The glass tube is drawn out at the
point so as to present a small orifice such as th of a millimetre in diameter.
Enclosing this end of the tube is an outer glass tube J supported by an arm k and
communicating by a flexible pipe with a supply of cold water, the flow of which
can be regulated by a screw clamp m worked by a button n. The arm projects
from a vertical slide o which in its lower part has rack teeth gearing with
a pinion p that can be turned by a button q. The upper end of o is connected by a
link to an arm & which is pivotted at S¹ and carries at its end a stopper t. When

page_text: the apparatus is not at work, the slide o is lowered, bringing j down below the
mouth of i, and closing that mouth by the stopper t so that the liquid in the mouth
of i does not become solidified by exposure, the stopper closing also the mouth of j.
On raising o, t and solution issues from i as a filament through the water which
overflow and finds its way to a drain D. Spring pincers (see Figs. 3, 4 and 5)
are fixed on a bar D¹ which is carried by a bell crank E jointed as shewn in Fig. 1
to two bent arms F and G. The arm G is fixed on a spindle H on which
is a crank M caused to reciprocate from M to M (Fig. 1) several times per minute.
By this action the parts E, F and G are made to move to the positions indicated
by the dotted lines E¹, F1, G¹ and the pincer springs v¹ are brought in contact with
a rapidly revolving brush I.
At first starting, the material issuing from i overflows the tube j and the
pincers adhere to it; these rising draw it out as a thread over horizontal glass
guide rods which keep several of the filaments separate at first, then over bent
guides y which collect the several filaments to be wound together on the reel K.
Should one of the threads break, the solution overflowing ; is in like manner
seized by the pincers when they descend, is drawn out as a thread by their
ascent, and led over the guides x and y to the reel K to be wound. The pinions
still ascending are cleaned by the brush I before they descend again. The reel K
besides revolving is made to move to and fro in an axial direction so that the
successive convolutions of the filament as it is wound may cross each other
obliquely. This movement is given from a crank on a pulley L linked by N to a
sleeve O between collars 2 on the spindle P of the reel. The machinery
described, of which there are a number of sets arranged in line, is enclosed in
a chamber having glass windows Q through which the action within can be
observed. Through the chamber air warmed to 85° to 90° Fahr. is passed by
supply and discharge conduits R and S. The vapours carried with the air may
be condensed by cooling, and the air may be again warmed and passed through the
chamber, while the condensed liquids may be again used for solution. The drying
of the filaments might be promoted by maintaining a partial vacuum in the
chamber, all parts communicating with the exterior being in that case arranged
with suitable packings to prevent ingress of air. The filaments produced may be
rendered incombustible by treating them either before or after weaving with an
anticombustible preparation such as a mixture of glycerine, gelatine and sugar.
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 manufacture of artificial silk like filaments by passing through fine
orifices and cold liquid covering them, a solution in ether and alcohol of pyroxyline
and metallic protochloride with a small proportion of oxidisable organic base,
substantially as described.
2. For producing filaments in the manner referred to in the preceding claim the
construction and use of apparatus substantially as described with reference to
the accompanying drawings.