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Патент USA US2404665

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Patented July 23, 1946
2,404,665
UNITED STATES PATENT OFFICE”
METHODS OF HARDENING AND TANNING OF
ARTIFICIAL FIBERS MADE OF PROTEIN
Rudolf ‘Signer, Berne, Switzerland
No Drawing. Application March '13, 1943, Serial
No. 479,142. In Germany January 15, 1942
5 Claims.
1
This invention relates to methods ‘of hardening
(C1. 18-475)
2
the second chemical condensing can be carried
and tanning arti?cial ?bers made of protein sub
out at different temperatures. Particularly, ‘it is
stance.
advisable to carry out the elongating at elevated
temperature in connection with which the work
,Arti?cial ?bers made of protein substance, for
‘example of casein, have moderate physical proper
ties such as for example a very small strength in
ing can be considerably expedited and conse
quently also be rendered continual.
wet condition, due to swelling in water.
Numerous methods for minimizing this draw
back have already been proposed. Some of these
operations can be chosen at will. The ?rst opera
tion may consist in a treatment with organic sub
The succession of the chemical condensing
are based on chemical effects such as hardening 10 stances, such as aldehydes, chinone etc., the
‘with formaline and tanning with aluminium,
second operation may consist in tanning with
metal salts or vice versa.
chromium, or other metal salts. Further methods
are of physical nature such as stretching and
Example 1
elongating methods which result in bringing about
Fibers dry-spun from slightly alkaline caseinate
a higher order of conditioning of the particles of 15
are exhaustively hardened with formaldehyde
the ?ber.
vapor. For eliminating the alkali the ?bers are
It has also already been proposed to combine
dipped in diluted acid for a short time at room
chemical and physical effects by, for example,
temperature. Thereupon the acid is washed out.
?rst stretching the spun ?ber and hardening same
in elongated condition with formaline or sub 20 The ?bers are gathered into bundles in parallel
. relation and the latter are then slowly elongated
jecting the ?ber to an elongating process between
in wet condition into double length at room
a preliminary and a subsequent hardening with '
temperature. The elongated bundles are sub
formaline.
mersed during four days, at a temperature of 20°,
It has now been discovered that extraordinarily
great improvements on the strengths in wet and 25 in a bath containing 100 g. of chrome alum and
10.6 g. of calcined soda per litre. The bundles
dry condition of the ?ber can be obtained if a
are then washed and dried.
previous chemical effect is followed by a vigorous
mechanical elongation and the elongated ?ber
Example 2
is then subjected to a second but different chem
30
A
cord
of
long
?bres having been hardened
ical condensation. ,
with formaldehyde is continuously unwound from
The changing of the chemical condensing
a spool at a velocity of 1 in. per min. and simul
agent between the preliminary and the later
elongation has a determinative in?uence as will
taneously wound on a second spool at a velocity
of 2 in. per min. The cord of long ?bers is thus
A casein ?ber which has been preliminarily 35 elongated into double length between the two
spools. During the elongating the ?bre is passed
treated with formaldehyde has in wet condition
through a bath of water of 40° and subsequently
an elasticity similar to rubber. If this ?ber is
introduced in a bath consisting in a chrome alum
elongated to double length and exhaustively hard
and calcined soda solution of the same composi
ened with formaline in elongated condition at
tion as speci?ed in Example 1. This bath moistens
room or elevated temperature the ?ber shrinks
the ?ber prior to being rolled up by the second
on the cessation of the tension almost back into
spool, whereby the penetration of the chrome bath
the length which it has had prior to the elon
into the ?ber is facilitated when the full spool
gating.
is submersed in said bath.
Therefore, this treatment produces only a very
The chrome solution is maintained at a temper
small permanent elongation and a correspond 45
ature of 40°. The elongation is effected by the
ingly small increase of the strength in wet and in
two spools along a path of travel of about 6 m.
dry condition. The same ?ber, having been pree
The full spools are submersed in said chrome bath
liminarily hardened with formaldehyde and elon
for two days, whereupon the threads are washed
gated in wet state into double length and then
tanned with chromium salt in elongated condi 50 and dried.
All temperatures are indicated in centigrades
tion, shrinks on the cessation of the tension
throughout the speci?cation.
hardly any, while the strength in wet and in dry
I claim:
state is almost twice as great as before.
1. The method of increasing the strength of
The three method steps, namely, the ?rst chem
ical condensing, the mechanical elongation, and 55 arti?cial ?bers made from casein, which com-'
be readily seen from the following comment.
2,404,665
T
~~
3
prises dry-spinning arti?cial ?bers from an alka
line casein mass, hardening the dry ?bers while
- they are in alkaline condition by treating them
with gaseous formaldehyde, freeing said ?bers of
alkali by treating them with dilute acid, stretch
ing the ?bers while they are wet, treating the
?bers while in‘wet stretched condition with a
chromium salt solution, and then washing" and
salt to render the solution basic, said solution
serving to maintain therthreads stretched, and
then washing and drying the permanently
stretched threads.
4. The method of increasing the wet and dry
strength of arti?cial threads made from casein ,
,which ‘comprises dry-spinning arti?cial ?bers
from an alkaline casein mass, hardening the
fibers by treatment with gaseous formaldehyde
2. The method of increasing the wet and dry 10 while the ?bers are ‘alkaline, freeing said ?bers
strength of arti?cial threads made from casein "
of alkali by treating them with dilute acid,
which comprises dry-spinning ‘threads from an‘
stretching the threads while they are in wet con
alkaline casein mass, hardening the dry threads ' ' dition to approximately double their length, treat
drying the ?bers.
while they are still in alkaline condition by treat-_ ,
ing them while in stretched condition with a chro
ing them with formaldehyde in gaseous form, re 15 mium salt bath at a temperature of approximately
moving the alkali from the threads by treating
40° C., to substantially maintain the elongation,
them with dilute acid, stretching the threads
vand then washing and drying the fibers.
While they are wet, and while they are still ‘in wet
5. The method of increasing the wet and dry
stretched condition treating them with a solu-'
strength of arti?cial threads made from casein
tion of chrome alum to maintain them elongated,
which comprises dry-spinning arti?cial ?bers
and then washing and drying the threads.
from an alkaline casein mass, hardening, the
3. The method of increasing the wet and dry
?bers by treatment with gaseous formaldehyde
strength of arti?cial threads made from casein
while} the ?bers are. alkaline, freeing said ?bers
which comprises dry-spinning threads from an
of alkali lby treating them withv dilute‘ acid,
alkaline casein mass,_hardening the dry threads
stretching the threads while they are in wet'con
while they are‘ in alkaline'condition by treating
them with gaseous formaldehyde, freeing said
threads of alkali by the action of an acid, stretch
ing the wet threads to approximately double their
length and while they are in stretched condition
‘passing them through a chromium salt solution
containing chrome alum and su?‘icient alkaline
dition to approximately double their length, treat
ing them while in stretched condition with a chro
mium salt bath at atemperature of approxie
mately 40° C., and for a period of at least two
days to substantially maintain the elongation,
and then washing and drying the elongated ?bers.
RUDOLF ,SIGNEEt.
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