Process for the Solution of Celiulose for the Production of Threads and Films.
Year: 1899

page_text: PROVISIONAL SPECIFICATION.
New Process for the Solution of Celiulose for the Production of
Threads and Films.
I, JULES CHAUBET, of 13, Rue Caumartin, Paris, in the Republic of France,
Engineer, do hereby declare the nature of this invention to be as follows:-
It is a well known fact that a solution of cupric oxide otherwise termed "Schweit-
zer's liquor" will dissolve cellulose. It has been sought for some considerable
time to utilize this property for the manufacture of threads or films.
After a layer of such a solution has been allowed to dry on a smooth plate
very fine threads can be cut out in a circular manner and can be woven.
The
threads thus produced however are not sufficiently regular.
According to another method, cellulose is dissolved in Schweitzer's liquor with
the aid of a more electro-negative metal than copper or by means of an electric
current. This process has several defects:-1st, it is a very long one and it
takes eight days to dissolve cellulose in the proportions of only 45 grammes per
litre, and 2nd, this solution has the very serious defect of being very readily
decomposed even while it is being prepared, so that it became necessary to lower
the temperature in order to obtain the solution.
The process which forms the subject matter of this invention is free from all
these defects. By its means a solution of 65 grammes per litre can be prepared
without the aid of cooling means, without the use of electricity and without
incurring the risk of a decomposition.
My process consists in:-1st, in carrying on the operation by means of a
suitable apparatus in a medium or atmosphere saturated with ammonia, which
avoids the weakening of the liquor in ammonia and hence prevents its decomposi-
tion; and 2nd, in the simultaneous action of air loaded with ammonia upon the
copper and of the resulting liquor upon cellulose.
Although the above result may be obtained by the aid of a receiver of any suit-
able form wherein are introduced an ammoniacal solution of cupric oxide, copper
and cellulose whilst stirring is effected from time to time, I prefer to arrange the
apparatus used for that purpose in the following manner.
The apparatus consists of five receivers which are hermetically closed. The
first receiver is filled with ammonia. The second receiver is filled with ammonia
and copper. The third and fourth receivers are filled with an ammoniacal solu-
tion of cupric oxide, of copper and of cellulose, while the last receiver is full of
acidulated water.
In the first bottle I introduce air and control the outlet. As it passes through
the ammonia this air is saturated therewith and is subsequently conveyed through
the liquid contents of the second bottle containing the ammoniacal cupric solu-
tion. As it issues from the latter bottle this current of air is conveyed alternately
through the third and fourth bottles. After a period of about 24 hours, the solu-
tion obtained is thoroughly homogeneous and one litre of liquor contains 65
grammes or thereabouts of thoroughly dissolved cellulose. The manner in which
I obtain this homogeneity and this thorough solution will be hereinafter more

page_text: fully set forth. The last vessel is used to collect the excess of ammonia. When
the preparation is ended the third and fourth receivers are emptied while leaving
the remaining copper therein, when the contents of the second bottle are poured
therein after having previously added to this liquor the necessary quantity
of cellulose and having intimately mixed these ingredients by causing them
to pass through two granite moulds having eccentric axes; the second bottle is
filled with ammonia and copper is added if required; the apparatus being now
ready to operate anew and to produce at the same time the liquor required for
use for the next day.
To illustrate the manner in which I obtain a thoroughly homogeneous mixture,
I shall proceed to describe the operation of the third and fourth receivers which
together form but one receiver. The upper part of each bottle is provided with
two openings the first of which serves for the introduction of the raw material
while the other is alternately used for the ingress and egress of air. The lower
part is likewise provided with two openings which enable the vessels to com-
municate together and openings provided with discharge taps. Above the lower
openings and at some distance from the bottom is arranged a partition perforated
with small holes.
This being so, let us suppose that air is forced through the opening of the third
vessel which contains the ammoniacal solution of copper, the copper and cellu-
lose required to be dissolved, whereas the fourth bottle contains copper only
and its opening is open. As the third receiver is hermetically sealed, the gas
will compel the mixture to pass through the one partition through the pipe into
the receiver and finally through the other partition. As soon as all the liquid
has passed into the third bottle the air which is loaded with ammonia and
seeks an exit bubbles through the liquid and escapes through the upper opening.
If some time later this opening is allowed to communicate with the air proceeding
from the second vessel and if the opening therein is free, a reverse action takes
place and the liquid is forced towards the third receiver where the bubbling
mixture is effected. By alternating this manipulation, the cellulose is constantly
divided up, the solution is obtained in a thorough manner and the liquid becomes
absolutely homogeneous.
The alternate opening and closing of the openings is easily effected by the aid
of a four-way cock, which can be so manipulated that gas is allowed to pass into
the third vessel, conveys the gas and thereafter on a further manipulation of the
cock is conveyed into the fourth vessel; in the first instance the receiver receives
the excess of air saturated with ammonia proceeding from the fourth bottle, and
in the second case it receives that proceeding from the third bottle. The quarter
of a turn required to be given to the cock to vary the admission and the escape-
ment may be automatically obtained by any suitable mechanical means.
I prefer the cataract produced by means of a small water jet and the intensity
of which can be controlled by a more or less closed cock, whence the bubbling
motion and contact can be more or less prolonged in the same vessel.
The liquor thus produced and filtered may be spun in the shape of threads or
bands. Threads are obtained by causing the liquor to run through a more or less
small orifice according to a well known process. The material being freed from
copper and ammonia by any suitable acid, it can be wound upon a drum, dried and
bleached. I use it to imitate silk.
By means of a flat draw plate endless bands can be obtained being particularly
suitable for photographic or cinematographic purposes and the like. They have
the great advantage of being non-inflammable
Dated this 12th dox of Tul, 1900
CRUIKSHANK & FAIRWEATHER,
Chartered Patent Agents,
62, Saint Vincent Street, Glasgow,
Agents for the Applicant.

page_text: New Process for the Solution of Cellulose for the Production of
Threads and Films.
I, JULES CHAUBET, of 13, Rue Caumartin, Paris, in the Republic of France,
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:-
It is a well known fact that the solution of cupric oxide termed
liquor" will dissolve cellulose.
Schweitzer's
It has been sought for some considerable time to utilize this property for the
manufacture of threads and films.
After a layer of such a solution has been allowed to dry on a smooth plate
very fine threads can be cut out in a circular manner and can be woven. The
threads thus produced however are not sufficiently regular.
According to another method, cellulose is dissolved in Schweitzer's liquor
with the aid of a more electro-negative metal than copper or by means of an
electric current. This process has several defects: (1), it is a very long one
and it takes eight days to dissolve cellulose in the proportions of only 45 grammes
per litre; (2), this solution has the very serious defect of being very readily
ecomposed even whilst it is being prepared, so that it becomes necessary to
lower the temperature in order to obtain the solution.
The process which forms the subject of this invention is free from all these
defects. By its means a solution of 65 grammes per litre can be prepared with;
out the aid of cooling means, without the use of electricity and without incurring
the risk of a decomposition.
My process consists (1), in carrying on the operation by means of a suitable
apparatus in a medium or atmosphere saturated with ammonia, which avoids
the weakening of the liquor in ammonia and hence prevents its decomposition;
and (2) in the simultaneous action of air charged with ammonia upon the copper
and of the resulting liquor upon cellulose.
Although the above result may be obtained by the aid of a receiver of any
suitable form wherein are introduced an ammoniacal solution of cupric oxide,
copper and cellulose while stirring is effected from time to time. I prefer to
arrange the apparatus for that purpose in the manner illustrated by way of
example in the accompanying drawings wherein Fig. 1 is an elevation of the
apparatus and Figs. 2 and 3 are sections of the four-way cock.
As it
The apparatus consists of five receivers (Fig. 1) a, b, c, d, 1, which are hermeti-
cally closed, excepting that they are connected to each other by pipes and a con-
trolling cock. The receiver a contains ammonia. The receiver contains
ammonia and copper. Receivers c and d contain an ammoniacal solution of
cupric oxide, copper and cellulose, while the receiver contains acidulated water.
Into the bottle a I force air and control the delivery. As it passes through
the ammonia this air is saturated therewith, and is subsequently conveyed through
the liquid contents of the bottle b containing ammonia and copper.
issues from the bottle 6 this current of air is conveyed alternately through the
bottles and d. After a period of about 24 hours, the solution obtained is
thoroughly homogeneous and one litre of liquor contains 65 grammes or there-
abouts of thoroughly dissolved cellulose. The manner in which we obtain this
homogeneity and this thorough solution will be hereinafter more fully set forth.
The vessel is used to collect the excess of ammonia.
When the process is
finished the receivers c and d are emptied leaving the remaining copper therein.

page_text: The contents of the vessel b are drawn off and the liquid is collected in a suitable
vessel.
Then the necessary quantity of cellulose is added to this liquid. These
ingredients are thoroughly mixed, preferably by means of such an apparatus as
is shown in Fig. 4, though any other mixing apparatus may be employed.
This apparatus consists of a mill-stone M of granite in which is bedded an iron
axle M, which is driven by a pulley P, and of a second granite mill-stone N eccen-
tric to the first which drives it. These two mill-stones are enclosed in a stoneware
casing provided with an outlet orifice Q, the whole being supported by some
suitable framework.
GP
is
The material which is poured in through the opening R of the millstone
thoroughly mixed under the action of centrifugal force in the recess S between
the millstones and then passes between the stones to the outlet Q where it escapes
and is collected in a suitable vessel. This mixture is then poured into the
vessels c and d.
To illustrate the manner in which I obtain a thoroughly homogeneous solution,
I shall proceed to describe the operation of the receivers c and d which together
form but one receiver. The upper part of each bottle is provided with two
openings, the first e or e¹ of which serves for the introduction of the raw material
while the other for f¹ is alternately used for the ingress and egress of air.
The lower part is likewise provided with two openings, i.e. (1) the openings g
and g which enable the vessels c and d to communicate with each other, and (2)
the openings h and h¹ provided with discharge taps. Above the lower openings
and at some distance from the bottom is arranged a partition i, k, or i,
forated with small holes.
per-
This being so, let us suppose that, as shown in the drawings, air is forced
through the opening of the vessel which contains the ammoniacal solution
of copper, the copper and cellulose to be dissolved, whereas the bottle contains
copper only and its opening f¹ is open. As the receiver is hermetically sealed,
and communication with the others closed by the controlling cock, the gas will
compel the mixture to pass through the partition i, k, through the pipe g, 9³,
into the receiver and finally through the partition ¹, k. As soon as all the liquid
has passed into the bottled the air which is loaded with ammonia and seeks an
exit bubbles through the liquid and escapes through the opening f. If some
time later this opening f is allowed to communicate with the air proceeding
from the vessel b and if the opening f is free, a reverse action takes place and the
liquid is forced towards the receiver where the bubbling mixture is effected.
By alternating this manipulation, the cellulose is constantly divided up, the
solution is obtained in a thorough manner and the liquid becomes absolutely
homogeneous.
The alternate reversal of the current through the vessels c, d, is easily effected
by the aid of the cock shown in Figs. 2 and 3; the position in-
dicated in Fig. 2 shows that gas is allowed to pass into the vessel c;
in the position indicated in Fig. 3, the cock conveys the gas into the vessel d.
In the first instance the receiver receives the excess of air saturated with
ammonia proceeding from the bottle and in the second case it receives that pro-
ceeding from the bottle c. The quarter of a turn required to be given to the cock
to alternate the admission and the escapement may be automatically obtained by
any suitable mechanical means.
For this purpose however I prefer to employ a cataract produced by a small
water jet, the intensity of which can be regulated by a more or less closed valve
or cock, whence the bubbling mixture in the vessels c and d can be more or less
prolonged in the same vessel.
A special form of such apparatus is represented in Figs. 5, 6 and 7, and is
composed of a casing 1 of wood, sheet iron or any suitable material divided by
a partition 2 into two parts, covered in part by the top cover 3, and at the ends
by sides 4 pierced with holes.

page_text: This casing is fixed to a rock shaft 5 furnished at its extremity with a socket 6,
shown in Figs. 6 and 7, and fixed to the plug of the four way cock, already
described, so that all the motions of the box are imparted to the said plug.
A small jet of water which can be regulated by a tap 7 fills first the portion 8
of the casing lying beneath it; as soon as this compartment is full the equilibrium
of the box is disturbed, and it rocks over through a quarter of a turn imparting
a quarter turn to the four-way cock. The water will drop through the holes
pierced in the sides 4, and falls into any reservoir.
At the same time the second compartment 9 (Fig. 6) is placed under the jet
and after a like interval this compartment is filled and the four-way cock is
again turned in the opposite direction and returns to its first position.
The liquor produced in this manner, and filtered, may be formed into threads
or bands. Threads are obtained by causing the liquor to run through a more or
less small orifice according to well known processes. The material being freed
from copper and ammonia by any suitable acid it can be wound upon a drum,
dried and bleached. I use it to imitate silk.
By means of a flat draw plate, bands of any desired length can be obtained,
being particularly suitable for photographic or cinematographic purposes and the
like, they have the great advantage of being non-inflammable.
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;-
A new or improved process for the manufacture of threads and ribbons particu-
larly designed to imitate natural silk and to produce non-inflammable films,
consisting essentially in dissolving cellulose in Schweitzer's liquor while operating
in an atmosphere saturated with ammonia which prevents the liquor from becom-
ing too weak in ammonia and hence from being decomposed, and in the simul-
taneous action upon copper of air charged with ammonia and of the resulting
liquer on the cellulose, this process being carried on in any suitable apparatus
and in particular in that shown by way of example on the accompanying
drawings.
CRUIKSHANK & FAIRWEATHER,
Chartered Patent Agents,
62, Vincent Street, Glasgow,
Agents for the Applicant.