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Патент USA US2406408

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. Patented Aug._ 27, 1946
2,406,408 '
UNITED STATES PATENT OFFICE
TREATMENT OF TEXTILE MATERIALS
George W. Seymour and Walter Brooks, Cumber
land, Md., assignors to Celanese Corporation of
America, a corporation of Delaware
.
-
No Drawing. Application December 30, 1942,
Serial N0. 470,662
8 Claims. (01. 252-835)‘
1
2
,
This invention relates to the treatment of tex- '
tile materials and relates more particularly to
the conditioning of ?bers and ?laments‘ made
of organic derivatives of cellulose whereby the
upon the ?bers or ?laments treated or presented
other difficulties of applications.
Particularly in the case of conditioning of rela
tively short length or staple ?bers formed of or
same are rendered more amenable to textile op 5 ganic derivatives of cellulose do the prior lubri
erations such as carding, drafting,- spinning and,
cating compositions fall short of what‘ was de-,
- also weaving or knitting, and to the formed yarns
sired.
While some such compositions were ca
and fabrics made from or containing said or
ganic derivatives of cellulose ?bers or ?laments.
pable of conditioning the ?bers to withstand the
numerous bendings and twistings imparted there
An object of the present invention is thepro 10' to during processing, they did not impart the
vision of an improved method of preparing a sta- .
desired degree vof friction between the fibers to I '
ble liquid for conditioning ?bers‘ and ?laments
comprising organic derivatives of cellulose to im
enable them to be drawn or drafted to ?ne yarns.
On the other hand, some compositions are satis
prove their amenability to textile operations such ~> factory with respect to their friction character
as carding, drafting, spinning, twisting, coning, 15 istic but do not properly condition the ?bers for
pirning, hanking, weaving, knitting and the like.
weaving, knitting or other textile operations. ‘
A further object of our invention is to provide
a treatment for textile ?bers or ?laments con
We have found that these and other disad
vantages arising' out of the use of known condi-r
taining organic derivatives of cellulose with a
tioning ?uids can be avoided by the use of the
novel conditioning ?uid whereby they are ren 20 conditioning ?uid of the present invention com
dered more anti-static and have the proper
amount of friction between the ?bers to give a
control to carding and drafting.
prising a mixture of several ingredients, some
of which react with each other. Fibers treated
with our novel composition behave much more.
A further object of the present invention isvto
satisfactorily in carding and drafting operations
provide a process for the treatment of organic 25 and in subsequent winding, twisting, warping,
derivatives of cellulose textile materials with a
weaving, knitting and like operations than do
conditioning ?uid containing different types of
untreated ?bers and ?laments, or ?bers and ?la
lubricants, softeners and other ingredients where
by fabrics made from such materials have a softer
hand and present a uniform appearance.
7
Another object of the invention is the provision
ments treated with known conditioning ?uids.
Moreover, we have found that ?bers treated with
30 our conditioning ?uids are not deleteriously af
fected upon storage and in some case may even
of an improved textile material made of or con
be improved after being stored for a time. Fur
taining organic derivative of cellulose ?bers or
thermore, the conditioning ?uid of our inven
?laments having applied thereto a conditioning
tion does not alter its effects on the fibers stored
?uid of the present invention.
'
.
35 for long periods of time but retains the same
Other objects of our invention will appear from
balance of friction for carding and drafting op
the following detailed description and the ap
pended claims.
_
.
erations, lubricative properties for other textile
operations and conditioning properties to with
stand the rigors of processing. Other advan
Many substances such as vegetable, animal and
mineral oils, both normal and specially treated, 40 tages are also imparted to the yarn by our con
have been employed for lubricating or condition
ditioning ?uid as will appear hereinafter.
_
ing textile materials in order to render them
In accordance with our invention we treat ?bers
more suitable for processing a fabric. While
or ?laments containing organic derivative of cel
these substances have resulted in some improve
- lulose with a conditioning agent formed by re
ments in processing, they‘ still left much to be 45 acting a mineral oil, a fatty acid and sulphuric
desired and in addition presented problems of . acid and to this reaction product adding a vege->
their own. Thus, the oils tend to gum or poly
*tabl'e ‘oil, an alkali, an alkyloiamine and water.
merize with time so that lubricated ?bers and
This conditioning agent‘ is stabilized, preserved
?laments cannot be processed uniformly due’to ., against oxidation and given an enhanced cover
the hardening of the oil. ‘Moreover, such gum 50 ing power by the addition of an alkylated phenol
ming or polymerization makes it diiiicult for the
or other spreading and penetrating agent.
conditioning agent to beremoved from the fabrics
The ?bers or ?laments to be treated in ac
made with such textile materials. Also lubri
.. cordance 'withv this invention may have as a basis
cating or conditioning compositions heretofore
any suitable organic derivative of cellulose such
used did not penetrate or spreadevenly into or
as organic esters of cellulose and cellulose ethers.
2,406,408
4 .
' lose acetate, cellulose propionate and cellulose
acid, palmitic acid, etc. The preferred fatty acid,
butyrate or mixed esters such as cellulose acetate
butyrate or cellulose acetate-propionate, while
I
1
,
1
.
step of ourinvention may be any suitable fatty
acid, examples of which are oleic acid, recinoleic
. ‘ Examples of organic esters of cellulose are. cellu-'
‘however, is oleic acid of at least 'technical grade
examplesof cellulose 'ethers are ethyl cellulose 5 or better. The sulphuric acid employed is fuming
sulphuric acid containing about 20% SO: and is
and‘benzyl cellulose.- However, the conditioning
commonly termed “Oleum 20%”.
"
'
agent of the instant-ginventionis particularly ad
; - A preferredimethod of preparing the condition;
vantageous in connection with the 'usefof cellulose‘
; acetate as the basis for the ?bers or ?laments, . - ing ?uid of our invention is as follows:
, especially acetone-soluble cellulose acetate hav 10 ._ About 29 parts of a white mineral oil of 50 vis
1, cosity, 21.5 parts of oleic acid or its equivalent of
other fatty acids and 10.5 parts of raw vegetable
oil such as olive oil, rice oil or peanut oil are
f ing an acetyl value of 521/2% to 56%, preferably
._ Silt/2%, calculated as acetic acid. However,'par- '
‘ tially saponi?ed organic estersof cellulose-may be
mixed and "cooled to about 10° C. in a; jacketed ‘
also employed as the basis of the ?bers or ?la
,
;
,
‘
1
l5 mixer through the jacket of which circulates a
cooling medium having a temperature of --10° to
This invention is applicable to the treatment
of ?ne ?laments,,or a plurality of such ?ne ?la-h v —20° C. With constant stirring about 6.5 parts
of fumingsulphuric acid are slowly added, say in
ments associated together in the form of yarn, or ‘
a 30 minute period. The temperature rises to
larger ?laments such as arti?cial bristles, horse- '
hair, straw and the like; and also to fabrics or 20 about 20° C. du'ring'the reaction time of about 75
other articles formed therefrom. It, is, particu
ments.
,
minutes.
h
..
-
To the above reaction product is-adde'd about
: larly applicable to the treatment of relatively
.parts. of diamyl phenol and then "a mixture of
short lengths of ?bers, say from 1/4 inch to 6 or
about 11.6 parts of triethanolamine or its equiv
1 more inches in length that are known in the trade
‘ as staple ?bers. The conditioning liquid may be 25 alent of other alkylolamine, 1.6 parts of: sodium
‘ , applied to the staple ?bers or to the continuous ’ hydroxide or its equivalent of potassium hydroxide
‘ , ?laments from which the staple ?bers are cut or
and 14 parts of water. The whole batch is stirredv
j to the ?laments as they are-being cut. The ?bers
j' or'?laments need not consist wholly of ?bers or
" ‘until all reaction ceasesand a clear oil'is formed.
~
Some of the raw vegetable oil may be added with
‘ ?laments of organic derivative of ‘cellulose but '30~ the alkali, if so desired. This conditioning liquid
may contain ?bers of other materials such as - may be‘ mixed with water and applied as an emul
sion to the ?bers, filaments, yarns. etc.
,
= natural silk; arti?cial ?bers of. reconstituted
In the resulting product substantially 40% of
the original oleic or equivalent fatty acid is sul
j on arti?cial ?bers that contain ?nely divided pig 35 fated and/or sulfonated; substantially 9% of the
original raw vegetable oil is sulfated and/or sul
‘ ment-like materials that alter the lustre and/or
fonated; the mineral oil remains substantially un
‘ color of the ?ber without deleterious effect. '
affected chemically; none of the vegetable oil is
As stated above, our novel- conditioning ?uid
saponi?ed- ‘by the alkali and triethanolamine
1 comprises the reaction product of mineral oil,
cellulose, wool, cotton, etc.
The conditioning
' . liquid of the present invention may be employed
‘ fatty acid and sulphuric acid, which reaction 40 which has been added in amounts to neutralize
all the sulfuric acid present and most but not all
of the oleic or other fatty acid used. The product
is slightly acid due to the‘ presence of about 10%
1 resulting compound stabilized and otherwise’ im
of umieutralized oleic acid.
‘ proved by the addition of an alkylated phenol,
1 or where the ?bers to be treated contain an ester ‘45. a; The product is an oily compound which readily
of cellulose with an alkylated phenol and/or’ . forms a stable, white emulsion in water, 2% emul
‘ product is reacted with a raw ‘vegetable oil, an‘
_j alkali, an alkylolamine and water and the whole'
sian'thereof having a pH of 6.8.
esteri?ed vegetable oil. In a preferred form of’
'
.
" . In place of all or a part of the diamyl pheno
our invention all or a part of the raw vegetable;
employed in the above formula there may be sub
oil is added with the fatty acid and takes part in‘
the ?rst reaction. Other materials may also be 50' stituted other alkyl derivatives of phenols; The
alkylated phenol not only acts as an anti-oxident
added, such as, for example, softeners for particu
but also enhances the penetrative and spreading
lar ?bers being treated; substances which aid in
.e?ects of the. conditioning liquid in and on the
emulsifying the com-position and also facilitate
‘?bers and yarns and stabilizes the conditioning
‘ the removal of the same by scouring; preserva
‘ tives'lsuch as Dowicide A (sodium ortho phenyl 55 ‘liquid whereby it does not separate into its com- _
ponents upon standing. Examples of other alkyl
‘ phenate), etc. Fugitive dyes or tints may also be
derivatives of. phenols or alkylated phenols are
added to identify the materials in processing also ‘
dibutyl
and 'diamyl derivatives of\cresols and
permanent dyes, etc. may be added.
,
xylenols, the dibutyl and diamyl derivatives of
The mineral oil employed in forming the con
ditioning liquid of our invention may be, one hav- ~ 60 any of thei‘mono-chlorophenols, etc. The diamyl
phenol may also be‘replacedain whole. or in part by '
. ing a. para?inic or naphthenic base and a viscosity
tricresyl phosphate or- triphenyl ' phosphate or
of ‘ 50 to 75 seconds. The viscosity referred, to I‘
similar compounds. ‘ When the ?ber or yarn being
herein is Saybolt Universal at 100° F. However, '
the viscosity of the mineral oilemployed is deter; " Y, treated, contains organic esters ,of cellulose, the
' mined by the over-all viscosity desired in the ‘65' addition ‘of an acetylated vegetable oil, such as
acetylated castoror oilve oil, ‘may be employed ad
conditioningvliquid or, in other words, the limit
of viscosity of the mineral oil is set by the~over-.
all viscosity of the conditioning liquid which dried ‘
on the ?bers gives desirable textile character-_
vantageously. . These-agents although having sev
eral functions are‘ called, for the purpose of sim- _ '
plifying’the description of the ‘invention, spread
" istics thereto. ' This over-all viscosity may be‘ on _70 ing and penetrating agents.
_
,_
,
" the order of 80 to 200 seconds and preferably 4
about 150 seconds. ‘Optimum results are obtained ,
'“theremay be substituted otherjhydroxylated
using a white mineral oil having a paraiilnic base
amines such as_'monoethanolamine, diethanol
i . and a viscosity of 50seconds. '
‘In. place of all or a partof the'triethanolamine
- ,llamine, viliethylamino ethanol,‘ .ethyl ldiethanol- ‘
The ‘fatty acid employed in'the ‘?rst reaction '75 amine, amethyl-zv-amino'propanol, etc.
"
5
The proportions of the several ingredients may
reacting a mixture comprising a mineral oil, a
. be varied to some degree, depending somewhat
on the use to which the treated ?bers are to be
put‘ and the properties which it is desired to em- .
phas'ize. Thus; where it is desired to increase the
spreading, and wetting properties the amount of
vegetable oil, ahigher fatty acid and fuming sul
phuric acidat a temperature no greater than
about 20° C. whereby sulphonation of at least
part of the fatty acid and vegetable oil occurs
and then adding diamyl phenol and an amount
of alkali-metal hydroxide and an alkylolamine
diamyl phenol may be increased from 5 parts to
to‘ neutralize all of the sulfuric acid and the
10 or more parts. Also the amount of mineral oil
may be varied from 20 parts to 35 parts depending a major portion of the higher fatty acid.
on the lubricity desired. Also the amount of 10 _4. Process for the preparation of a conditioning ’
alkali and alkylolamines may be varied. In this
liquid for textile materials whicncomprises re
acting a mixture comprising, a mineral oil, a,
respect we have found that the preferred condi
vegetable oil, a higher-fatty acid and fuming sul
tioning liquid should be one that a 2% emulsion
phuric acid at a temperature no greater than
of same in water has ‘a pH of from 6.6 to '7.
The conditioning liquid obtained in accordance 15 about 20° C. whereby sulphonation of at least with our invention may be applied to ?bers and
?laments in the concentrated form or it may be
applied as an emulsion, or dissolved or suspended
in a carrier. The amount of conditioning liquid
part of the fatty acid and vegetable oil occurs
and then adding an acetylated castor oil and an
amount
applied may vary from 1 to 10 or more per cent 20
based on the weight of the untreated ?bers. The
' ning yarns and ?laments by wicks, rollers or other
furnishing devices. However, it may also be ap
plied to ?bers by dipping bales ‘thereof in a bath
C. whereby sulphonation of at least part of ‘the
fatty acid and vegetable oil occurs and then
adding a spreading and penetrating agent and
.
-'I'he term “sulfonation" as used in the appended
claims designates not only the phenomenon of
sulfonation proper (that is the formation of prod
ucts wherein sulfur atoms are linked directly to
carbon atoms) but also sulfati'on (thatis the for
an amount of alkali-metal hydroxide and an‘
so
6. Process for the preparation of a condition- ‘
linked to oxygen atoms that are in turn linked to
It is to be understood that the foregoing de
tailed description is given merely by way-of illus
alkylolamine to neutralize all of the sulfuric acid
and the major portion of the higher fatty acid.
ing liquid for textile materials which comprises
mation of products wherein the sulfur atoms are '
' carbon atoms).
hydroxide‘ and , an
‘acid at a temperature no greater than about 20°
of the conditioning liquid or by. spraying the same
_
alkali-metal
,5. Process for the preparation of a condition
ing liquid for textile materials which comprises
reacting a mixture comprising a mineral oil, a
vegetable .oil, oleic acid and fuming sulphuric
conditioning liquid is preferably applied to run-4
with a mistof some.
of
alkylolamine to neutralize all of thesulfuric acid
and the major portion of the higher fatty acid.
reacting a mixture comprising a mineral oil, a
35 vegetable oil, oleic acid and fuming sulphuric acid
‘ at a temperature no greater than about 20° C.
whereby sulphonation of- at least'part of the fatty
tration and that many variations maybe made
acid and vegetable oil occurs and then adding
therein without departing from the spirit of our
diamyl phenol and an amount of alkali-metal
invention.
40 hydroxide and an alkylolamine to neutralize all
Having described our invention, what we desire
of the sulfuric acid and the major portion of the
higher fatty acid.
"
’ '
to secure by Letters Patent is:
7. Process for the preparation of a condition
.1.,Process for the preparation of a‘ condition
ing liquid for textile materials which comprises
ing liquid for textile materials which comprises
reacting a mixture comprising a mineral oil, a‘ 45. reacting a mixture comprising a mineral oil, a
vegetable oil, ‘a higher fatty-acid and fuming
vegetable oil, oleic acid and fuming sulphuric acid
sulphuric acid at a temperature no greater than
at a temperature no greater than about 20° 0.
about ‘20° C. whereby sulphonation of at least
whereby sulphonation of at least part of the fatty
part of the fatty acid and vegetable oil occurs
acid and vegetable oil occurs and then adding
and then adding a spreading and penetrating 60 an acetylated castor oil and an amount of alkali
metal hydroxide and an alkylolamine to neu
agent and an amount of alkali-metal hydroxide
and an alkylolamine to neutralize all of the sul
tralize all of the sulphuric acid and the major
furic acid and the major portion of the higher
fatty acid.
'
portion'of the higher fatty'acid.
. ',
8. Process for the preparation of a condition
.
2._Process for the preparation of a condition 6,5 ing liquid for, textile materials which comprises
ing liquid for textile materials which comprises ' reacting a mixture comprising a mineral oil. raw
reacting a mixture comprising a mineral \oil, a
peanut oil, oleic acid and fuming sulphuric acid
vegetable oil, a higher fatty acid and fuming sul
at a temperature no greater than about 20° C.
phuric acid at‘ a temperature no greater than
whereby sulphonation of at least part of the
about 20° 0. whereby sulphonation of at least part 60 fatty acid and vegetable oil occurs- and then
adding a spreading and penetrating agent and
_ of the fatty acid and vegetable oil occurs and
then adding an alkylated phenoland an amount
an amount of alkali-metal hydroxide and an
of alkali-metal hydroxide and an alkylolamine
alkylolamine to neutralize all of the sulphuric
acid and the maior portion'of the higher fatty
' to neutralize all of the sulfuric acid and the major
portion of the higher fatty acid.
a
‘ 8. Process for the preparation of a condition
ing liquid for textile materials which comprises
65
acid.
*
~
GEORGE W. SEYMOUR.
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