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Патент USA US2107668

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‘ Patented Feb. 8,‘ 1938
: _,2,l07,6.68
I
UNITEDQS’AI‘ATES‘ ‘PATENT OFFICE.
' 2.1mm
lemon or mnucmc. ARTIFICIAL
'
wimmnnysen, Kenmore, u'ia John s. rm;
‘
51 meme a-ignmen‘ts,
.
to E. I. dn-Pont de Nemours ieompannwil
'
mingtoa,
, a corporationofnehware
No
.'
mead July as, res..
SerialNo. m.aiz
(CI. 18-54)
‘
invention relates to threads, ‘sheets, films,
and other .materials produced by extruding
(spinning or casting‘) cellulosic solutions, such as
viscose, cellulose acetate and other, cellulosic
i derivatives. More particularly, it relates to La
'
.
1
.,
reducing the tensile strength of the product.
‘Speci?cally, we have found that by introducing
into the viscose certain substances which disap
pear or are eliminated ‘automatically at ‘some.
stage in the usual production or ?nishing'of the
\ method of producing materials of thcr'type men-' thread,_ an arti?cial
is produced which
' _tioned having a diminished luster.
has a crinkled‘, channeled or porous exterior and
it relates to: a method of producing rayon' having is composed of a substantially solid‘ cellulose mass
sbecmcauy.
a diminished luster and preferably equal to or .'
10 lower than that possessed by natural silk.
Arti?cial thread produced, by theusualviscose 1
process is characterized by a' high brilliant luster. .'
~For many purposes brilliant arti?cial .threadis
u unsuitable and a product of lower luster is de
free ‘from foreign material. Due-to the struc
ture of the exterior surface, it - -
-
r- a luster
10
'equalto 'or lower than that of arti?cial Isilk.‘
It is therefore an object of
invention to
provide a method of producing arti?cial thread
by the viscose process having a luster lower than
sired. ‘Several methods have already been {dei-v ordinary viscose silk and preferably ‘equal to or ll
jvised‘to produce viscose arti?cial
lower than that of natural silk.
Y
'
‘thread having
a substantially diminished luster.
, Another object of this invention is to provide
One of the methods used prior to this invention a method of prodiicing'a mat appearing~ ar
consisted in depositing or precipitating a"luster
'20 duilingmat rial on previously formed thread.
According to ne speci?c procedure of thatproc
ess, a ‘skein of arti?cial thread was alternately‘
‘treated with a solution containing a soluble bar;
ti?cialthread consisting of solid cellulose free
from foreign materialsand having a crinkled,
porous or channeledsurface.
'
_
A further object of this invention is to provide
a method of producing arti?cial thread which
ium ‘salt and a solution containing a sulphate - comprises the addition of a certain ‘substance to
. g5 radical.‘ frhe insoluble barium salt resulting from viscose which automatically disappears in they
the reaction was produced on the surface of the
thread and, though it reduced the luster, ‘it did
.-not give permanent effects. Frequently, in use
"
the precipitated material was removed and as a
usual process of producing or ?nishing the
thread.
.
s
_
,
'
Other objects will appear from the following
description‘ and appended claims. -
'_
7' .
*3) consequence an unattractive material resulted.’ . According to this invention‘, ‘arti?cial thread
‘In addition, the running 'qualities and the having a mat appearance and a luster similar to
physical properties of the thread were seriously ..or lower than natural silk is produced by spin
a?ected. Moreover, the appearance and particus ning in the usual manner a viscose solution con
, larly the luster did not simulate natural silk.
,5 ' Another proposed procedure for producing
tain’ing‘a?certain substance, which substance is
‘distilled or.- otherwise removed at one or more
. arti?cial thread having a mat appearance'con
stages in the process of producing the
sisted in incorporating into the viscose various _ No special steps are necessary to .remove the
materials, suchv as pigments, oils, fats and the . added substance. The removal is automatically
like. The threadv prgduced by this process con
“ sisted of a mass of cellulose having liquid’or pig;
'ment particles incorporated therein. Though
this method produced/a product of low luster,-the "
type of luster was not comparable or similar to
that of natural silk. Also, in view of the con
45 stitution of the mass, there ‘was a loss of tensile.
strength.
_
-
/
.
accomplished in the usual operations of ?nishing
the thread. The product'of this process is sub 40
stantially solid‘ cellulose free from foreign‘ or
added
materials.
It is ' characterized
by
a
- ,
crinkled, ‘porous or channeled exterior surface
and
vstrength.
substantially " its normal. tensile
‘
'
.
‘
_
'
'
The substance added'to the viscose may be
Hollow arti?cial threads produced from'viscose , kerosene, turpentine or other comparatively high
possessed a. reduced luster. These hollow ?la
ments because of their structure had a very low
so tensile strength and thus were therefore not
suitable for ’a great number, of uses.
_ .Wehave found that we can produce an arti
?cial thread by the viscose process, which is char
acterized by a luster equal toor lower‘ than that
1- possessed by natural silk without sacri?cing or
)
boiling‘ volatile ‘hydrocarbons or similar com
;pounds or substances, solids or‘ liquids which, due _
to lack of suitable terminology, is designated by 50
the term “vaporizable substance”. By theuterm
“vaporizable substance” is meant a substance or
compound which is insoluble in a spinning solu
tion, or, if soluble in ‘the spinning solution, in-~~"'
soluble in the ‘answering bath liquid, suwsi'ib- u
aioaeea
2
stance possessing a su?ciently low vapor pres
sure so that it will not be removed from the
spinning solution prior tospinning, particularly
ing the usual ?nishing operations, the kerosene
is automatically substantially eliminated.
Any of the well-knowngcoagulating baths may
be used.
when the spinning solution is evacuated to remove
the air, nor is it removed during spinning except
_ in some instances a relatively small per cent may
sulphuric acid, ‘24% sodium sulphate and 0.8%
be removed,‘ depending upon the substance
‘chosen, said vapor pressure being sufficiently high
zinc sulphate.
.
.
'
The product resulting from the method pre
so that thesubstance may be removed from the
10 thread (as by steam distillation or otherwise) in
viously described consists‘ of substantially pure 10
cellulose. When examined under the microscope
washing, desulphuring, bleaching, drying or other
steps in the usual spinning and ?nishing opera
,
We prefer, however, to use one con
taining zinc or analogous metals. A bath which
has given satisfactory results consists of 11%
at a magni?cation not exceeding 440 diameters,
it appears as a substantially solid thread showing
no liquid, gas or solid particles. Magni?cation
of 440 diameters is used as a standard because a
It. is to be observed that this de?nition
tions.
does not include such materials as ligroin, ben
15 zene, carbontetrachloride, carbon disulphide and
regular viscose thread, if inspected at a su?ie
ciently great magni?cation, may show the pres
similar materials of comparatively low boiling
point and high vapor pressure which, though
they result in the production of materials hBN'. ence of foreign liquid or solid particles or even
ing a reduced luster, do not resist evacuation of 'of air which may not have been cempletely re
the spinning solution ‘and/or are removed for ‘moved from- the viscose. The cross-section of 20
' the most part during spinning, so that no control the product is similar to that of an undelustered
v thread, except that the surface structure'and
of the resulting luster is possible.
I
contour are crinkled, porous or channeled. This"
In accordance with this process, one or a plu
rality of the vaporizable compounds is introduced a feature permits greater scattering of light than
is possible in the ordinary undelustered thread.
25 into the viscose prior to the spinning thereof and
, Although this invention has been described
is eliminated automatically in the process of pro
ducing the ?nished, thread without the aid of any
special operations. It may be incorporated in the
viscose at any time between dissolving the cel
speci?cally in connection with arti?cial thread
produced from viscose, it is not limited thereto.
The principles of this invention are equally ap
30
30 lulose xanthate in caustic soda and the time the ' plicable to other cellulose spinning solutions, as,
viscose is ready to be spun. It may aiso be added for instance, those containing cellulose deriva
to the steeping caustic, to the alkali cellulom or tives such as celiulose acetate, cellulose ethers,
to the carbon disulphide. Preferably, it is added or the, like.» Furthermore, the invention is not,
to‘ the mixture of caustic soda, water and .cel
. restricted to the production of arti?cial thread.
lulose xanthate as‘ these are being mixed. The ,It is likewise suitable in the manufacture of sheets I
substance may be added directly to the caustic or films from cellulosic solutions of the type’
solution ,or may be ?rst mixed with a- small previously mentioned and including viscose, cel
amount of caustic and then added to the main lulose acetate, and cellulose ethers.
The term “extruding” used in the claims is in
tended to‘ cover genericaily the extrusion of the 40
cellulosic solution from the spinnerets in the
production of threads or the casting of the solu
to the batch. If desired, to aid the emulsifica
tion any of the commoniy _known emulsifying tions to produce sheets or ?lms.
Since it is obvious that various changes may be
agents for this purpose, including soaps, gums,
sulphonated vegetable oils, alkylated naphthalene ' made in the speci?c details of operation above 45.
and anthraquinone sulphonic acids (such as the set forth without departing from the nature ‘or
‘spirit of this invention, this invention is not re8
Nekals) may be employed.
a , .
The amount of vaporizable substance added stricted thereto except as set ‘forth in the ap
pended claims.
'
i
: depends on the desired luster. Satisfactory re
We claim: '.
‘
sults have been obtained by inccrporating ap
cherge.-- Preferably, an emulsion of the vapor
(0 izable compound in water is separately prepared
in any suitable manner and this emulsion added
.
proximately from 0.05% to 3.0% of the vaporiza
'
5o
1. A method ef-producing solid arti?cial thread
ble compound in aviscose solution of the usual
having a luster equal to or lower than natural
following speci?c examples indicate the preferred
quantities of the various materials added:
high b-oiling'hydrocarbon in .a viscose solution,
type, the proportions being based on weight. ‘The ' silk which comprises introducing a vaporizable
Kerosene__'__ 0.5% emulsi?ed with Monopole oil
Turpentine" 0.6
emulsi?ed with Nekal A. E. M.
The process may be carried out as previously
explained, but in order to more clearly illustrate
one precise mode of operation, the following de
scription of one procedure is given: 1;‘
/',
To a ‘spinning charge of ‘100 pounds slit-viscose
produce-:1 in the usual manner, .there is'added a
thick, creamy emulsion containing 14 cos. of a
spinning said solution and ?nishing the thread in 55
the usual manner whereby- the hydrocarbon is
i substantially eliminated.
2. A method of producing solid arti?cial thread
having a luster‘ equal to or lower than natural'
silk which comprises introducing a vaporizable 60
. high vboiling ‘hydrocarbon in a viscose solution at
some stage in the manufacture thereof, spinning-X
said solution- and ?nishing‘ the thread in the
usual way whereby the hydrocarbon is substan
tially eliminated.‘ '
‘
65
> .3. A, method of producing solid arti?cial thread.
227 grams of kerosene and 280 cc. of ‘water. The having a luster equal to or iower than natural
emulsion is preferably made, by dissolving the 1 silk which comprises introducing an emulsion of
suitable emulsifying agent, such as M'onepole oil, '
emulsifying agent in'the kerosene andthen add- ‘ a vaporizable high boiling hydrocarbon in a _
viscose solution,‘ spinning said ‘solution and?n 70,
70 ing the water witln'constant agitation. Upon the ' ishing
the thread in the usual manner whereby
introduction of the emulsion in the viscose, the
mass, is agitated“ until the distribution of the the hydrocarbon is substantially'eliminated.
4; A method of producing‘ solid arti?cial thread
emulsion is'coinplete. ' The viscose thus produced
’ ‘.is allowed to ripen and is spun and the thread
‘produced processed in the usual manner. Dur
having .a luster equal‘ to .or less'_-than natural silk
which comprises introducing-0.05% to 3.0%. by
3
2, 107,668
weight of a vaporizable high boiling hydrocar
cellulosic solution containing 0.05% to 3.0% by
bon in a. viscose solution at some stage in ‘the
weight of kerosene in an aqueous bath and ?n
ishing the material in the usual manner whereby
said kerosene is substantially eliminated.
15. A method of preparing solid threads, ?lms.
sheets and the like which comprises extruding a
manufacture thereof, spinning said solution and
?nishing the thread in the usual manner, whereby
the hydrocarbon is substantially eliminated.
5.. A method of producing solid arti?cial thread
having a reduced luster which comprises incor
porating kerosene in a viscose solution at some
solution containing 0.05% to 3.0% by weight of
turpentine and ?nishing the material in the usual
stage in the manufacture thereof, spinning said
manner whereby said turpentine is substantially
solution and ?nishing the thread in the usual
manner whereby said kerosene is substantially
eliminated.
-.
'
eliminated.
10
'
sheets and the like which comprises extruding a
cellulosic solution containing a vaporizable high
boiling hydrocarbon in an aqueous bath and ?n
ishing the material in the usual manner whereby
said hydrocarbon is substantially eliminated.
17. A method of preparing solid threads, ?lms,
sheets and the like which comprises extruding a
-
6. A method of producing solid arti?cial thread
having a reduced luster which comprises incor-v
16 porating 0.05% to 3.0% by'weight of kerosene
in a viscose solution at some stage in the manu
facture thereof, spinning said solution and ?n
ishing the thread in the usual manner whereby
said kerosene is substantially eliminated. “
solution containing a member of a terpene group
and ?nishing the material in the usual manner
"7. A method of producing solid arti?cial thread
having a reduced luster which comprises incor
porating 0.5% by weight ,of kerosene in a viscose
solution at some stage in the manufacture there
of, spinning said solution and ?nishing the thread
25 in the usual manner. whereby said kerosene is
20
substantially eliminated.
'
16. A method of preparing solid threads, ?lms,
whereby the terpene is substantially eliminated.
18. A method of preparing solid threads, ?lms,
20
sheets and the like which comprises extruding a
cellulosic solution containing 0.5% by weight of
kerosene in an aqueous bath and ?nishing 'the
material in the usual manner whereby said kero
sene is substantially eliminated.
19. A method of preparing solid threads, ?lms.
sheets and the like which comprises extruding a
.
8. A method of producing solid arti?cial thread
having a reduced luster which comprises incor
porating an‘ emulsion containing kerosene in a
viscose solution in such quantities that from 0.05%
to 3.0% by weight of kerosene is present, spinning
said solution’ and ?nishing the thread in the usual
manner, whereby said kerosene is substantially
solution containing 0.6% by weight of turpentine
and ?nishing the material in the usual manner
whereby said turpentine is substantially elim
inated.
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_
-
eliminated.
35
.
40
45
J
20. A method of preparing solidthreads, ?lms,
9. A method of/producing solid arti?cial thread ‘ sheets and the like which comprises extruding a
having a reduced luster’which comprises incor
viscose solution containing 0.05% to' 3.0% by
porating a member of the terpene group in a vis— weight of kerosene and ?nishing the material in
cose solution at some stage in the manufacture
the usual manner whereby said kerosene is sub
thereof, spinning said solution and ?nishing the stantially eliminated. thread in the usual manner whereby said mem
21. A method of preparing solid threads, ?lms, 40
ber is substantially eliminated.
7
~/
,.
sheets and the like which comprises extruding a
10. A method of producing solid arti?cial viscose solution containing 0.05% to 3.0% by
thread having a'reduced luster which comprises weight of turpentine and ?nishing the material
incorporating turpentine in a viscose solution at in the usual manner whereby said turpentine is
some stage in the manufacture thereof, spinning substantially eliminated.
‘
said solution and ?nishing the thread in the usual
22. A method of preparing solid threads, ?lms,
manner, whereby said turpentine is substantially sheets and the like which comprises extruding a
eliminated.
'
‘
viscose solution containing a vaporizable high‘
'11. A method of producing solid, arti?cial boiling hydrocarbon and ?nishing the material in
thread having a redu'ced‘luster which comprises the usual manner whereby said hydrocarbon is
50
incorporating 0.05% to 3.0%, by‘ weight of ‘tur
substantially eliminated.
=
pentine in a viscose solution at some stage in the '
23.v A method of preparing solid threads, ?lms,
manufacture thereof, spinning said solution and
?nishing the thread in the usual manner, whereby
55 said turpentine is substantially eliminated. N
~12. A method of producing solid arti?cial
sheets-and the like which comprises extruding a
viscose solution containing a member of a 'ter
penegroup and ?nishing the material in the usual
manner whereby the terpene is substantially elim
55
thread having a reduced-luster which comprises . inated.
incorporating 0.6% by weight of turpentine in a ‘
24. A method of preparing solid threads, ?lms,
viscose solution at some stage in ~the manuiac-’ 3, sheets and the like which comprises extruding a
l
ture thereof, spinning said solution and ?nishing
viscose solution containing 0.5% by weight of
the " thread in the usual manner, whereby-said kerosene and ?nishing the material in the usual 60
turpentine is substantially eliminated. ,
tmanner whereby said kerosene is substantially
13. A‘ method of. producing solid arti?cialv
thread having a subdued luster which comprises
eliminated.
.
_
25. A method of preparing solid threads, ?lms,
incorporating'an emulsion containing turpentine
.65 in a viscose solution in such‘quantities ,that from ' sheets and the like which comprises extruding a 65
viscose solution containing 0.6% by, weight of tub
0.05% .to 3.0% by weight of ‘turpentine is pres .pentine and ?nishing the material 'in the usual‘
ent, spinning said solution and. ?nishing the manner whereby said
‘ , thread in the usual manner, whereby said turpen
eliminated.
.
z
_
.
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70 tineis
14. Asubstantial”
method of preparing solid. threads, ?lms,
sheets and the like which comprises extruding a
somea'roms.
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