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. 17, 1946.
2,412,832
E. c. PFEFFER, JR., ETAL
TEXTILE MATERIAL AND METHOD OF PREPARING IT
Filed Oct .
30 ,
1945
STABILIZATION DATA
shrinkage 1n 5 washes Artnr stabilizing Process:
Fonnulae on Percent by Weight Buis
(A)
Fabric Construction
(B)
(1)
$5 1Z1-5
(2)
$5 l<1-5
$5 $1-5
75% Vincolo Staple l:
2% Acetato Stnplhßlendod 1.28"/yd
Ylnin louve
111.9 2.11
6.9
11.8
8.9 1.1
12.11 2.2
1.2
.B
5.3
15.5 1.1
6.1
0
5.5
11.7 1.9
5-9
.5' 5.5
11.0 11.5
5.1
.8 2.8
.6
6.9
855i Vincolo Simple t
1.5i Arlhcßlondsd
Pllín leus
5.0
21/1
‘á 2K..
59 55 Count
'arp an
n3
x
la .7 gyjd
50i vincola :emph t
501 Annen suplhmandnd 1,76*/yd
Clvllry 11111101"
18/1
1
1
19 T-S 'up
'r-z funn;
à s117Count
äh y”
80S Viaocn suple a:
20# Anstatt 8tlp1s,B1ond¢d 2.52714
2x1 T1111. lun
21;/1
19 T-S In'
1 9 1~-z ruïne
1
116166 Count
6.5 ç_llbd
60‘ Vinson Staple t
hof Aunt. suphßnndu 2.25"/ya
Plain 'un
50/2 19 T-Z singles
nr
65
15 T-S P11.
Ind filling
5-5
701 Vincolo Selpln à
50% Aut-u suplhßlendsu
2x2 '1*'111 ll‘vn
lâ T-Z singlet
20/ 2
T'S P17»
'lr
and filling
COBRE
SSXEel ç_x/ïd
1oo$4m1mer§z my»
(Vil‘uola)
98 dlniar 'up '
152 deninx‘ filling
92x70 Count.
9.a
1.5
1.9
0
2.2
2.7 oflyd
t
Mezza/’072;
.Zi/¿mm1 £177.27; J7:
¿hay
~-¢
"
i
Patented Dee. 17, 1946
_UNÉTED lSTATES -l'nßlrlaN'r ori-'lcs
2,412,832
TEXTILE MATERIAL AND METHOD OF
PREPARING IT
'
Edward C. Pfeffer, Jr., and Jack Epelberg, Troy,
.
~l
N. Y., assignors to Cluett, Peabody & Co., Inc.,
Troy, N. Y., a corporation of New York
Application Gctober 30, 1943, Sei-_iai No. 508,368
8 Claims.
This invention pertains to textiles and relates
more particularly to a novel textile material, for
example a woven fabric permanently stable with
respect to laundry shrinkage and resistant to
Wrinkling, crushing and creasing, and if desired
of a soft hand and good draping quality, and to
'
2
when used alone possess many disadvantages
whichI substantially lessen their field of useful
ness. For example, some of them have or emit
during curing an exceedingly disagreeable odor
or irritating or toxic fumes necessitating special
and extensive precautions in their use; in some
instances the disagreeable odor is persistent in
or develops in the fabric after finishing; some of
these resinous type materials cause permanent
10 discoloration or browning of the fabric so that
ì they are not `applicable to white material; some
of them make the constituent flbers of the fab
a novel method of preparing such a material,
the present invention representing a further de
velopment of an improvement upon the invention
disclosed in the copending application of Pfeffer
and Epelberg, Serial No. 495,620, vfiled July 21,
1943.
The term “textile material” as herein employed
ric tender thereby reducing the tensile strength
ls intended to include filaments, ñbers, staple or
of the fabric; and some of them are unduly ex
yarns, whether in the finished state or at some 15 pensive, particularly when employed in the large
intermediate stage in the production thereof.
amounts sufficient effectively to provide crease
'I'he term also includes fabrics whether knitted,
resistance as well as dimensional stability.
Woven or felted, as Well as garments or other
The aforesaid application further disclosed, as
articles made from such fabrics.
a wholly novel concept, the employment of a dial
A principal object of the present invention is 20 dehyde, glyoxal
to provide textile material, for instance of any
of the classes just above enumerated-for more
speciñc example a woven fabric-_which possesses
CHO
HO
even better stability with respect to dimensional
also known as oxalic aldehyde, or ethanedial as
shrinkage, together with equal or better-resist 25 a, stabilizing and crushprooñng medium in sub
ance to crushing than the material disclosed in
stitution for the formaldehyde theretofore em
' the aforesaid application as well as other advan
ployed, and pointed out substantial advantages
tages of the latter material and which, if de
for the glyoxal as compared with the -materials
sired, may have a very soft hand and ñne drap
which had previously been employed, for example
30
ing qualities. A further object is to provide a
the fact that the glyoxal may be or in fact must
novel method of preparing textile material of this
be used in low concentrations, for example from
improved character. Other and further objects
0.6% to 4.65% by weight in the treating bath,
and advantages of the invention will be pointed
whereas such prior materials as urea formalde
out in the following more detaileddescription
hyde condensation products must be use-d in con
and by reference to the annexed drawing which 35 centrations of from 6% to 8% for stabilization
consists of a, table showing the characteristics
and from 14% to 16% for creaseprooñng.
of the fabric of the present invention as com
Further, it was noted that glyoxal does not
pared with those of untreated fabric and of fab
emit disagreeable fumes during curing; it does
ric which has been treated in accordance with
not substantially tender the textile material or
the procedure of the aforesaid application.
40 make it brittle, when used in the concentrations
In'the above application it was pointed out
requisite for stabilization or l crushprooñng; it
that customary previous modes of stabilizing and
does not discolor or brown the textile material to
crushprooñng textile materials had involved the
any harmful degree; it may readily be applied
use of solutions or suspensions of intermediate
without necessitating special equipment, and it
45
condensation products of synthetic resins or resin
has little odor in solution of a strength suit
components either with or without a plasticizer,
able for its intended use.
i
and forming and` curing the resin in situ, and
It was also noted that thë glyoxal is applied
that such resinous substances as had commonly
to the fabric in water solution but it does not
been employed (phenol formaldehyde, urea form
exist as the above compound when in water solu
aldehyde, and melamine formaldehyde, etc.) 50 tion since it hvdrates to form a compound known
2,419,832
3
.
As illustrative. without limitation of the scope
of the invention, the following suggestions as to
reagent strengths .and conditions of treatment
are cited, it beingnoted that in accordance with
the present invention substantially the same
as tetrahydroxydioxane, which has the following
structural formula:
110110
-
/
amount of glyoxal and catalyst are employed as
110110
disclosed in the above application, the resinous
o
material being in addition thereto.
When the water in which this material is dis-A
1.
Amount of glyoxal:
solved is evaporated and further heat is applied, l0
15 to 120 cubic cms. of 30% glyoxal solu
the material readily dehydrates yielding glyoxal
tion per liter of treating bath, or ap
as shown by the following formula:
proximately .6 to 4.65% glyoxal by
O
weight in the treating bath.
nonc/ \cnor1
11011
‘H011
2. Type of catalyst:
'
<
Acid-reacting, such as organic acids or
salts of inorganic acids or organic acids `
15
which produce an acid effect.
While we do not definitely know the exact ac
3. Amount of catalyst:
tion which occurs when cellulose in association
1/8 to 4 gms. per liter of treating bath, or
with glyoxal is heated. we believe that a reaction 20
approximately .0125 to .40% by weight
takes place in consequence of which the cellulose
of treating bath.
of the individual fibers of the fabric is at least
4. Amount of resin:
partially converted into a reaction product which
12 to 50 gms. of 100% condensation prod
uct per liter of treating bath or approxi
mately 1 to 5% by Weight of the treat
ing bath.
may be termed “dicellulose diacetal” or “cellu
lose glyoxal,” as may be preferred, such prod
uct being of the long-chain, high molecular
weight type, but with cross-linkages making it
more stable than the formaldehyde resins.
We have now discovered that whereas glyoxal
5. Amount of softener, if used:
tor) in these low concentrations provides a de
bath.
6. Baking temperature:
212° F. to 350° F.
gree of stabilization and crushprooflng compar
7. Baking time:
alone (or in association with a catalyzer accelera
-
Approximately 1% by weight of treating
able with the results obtained by the use of
.
2 minutes to 40 minutes.
larger amounts of the formaldehyde condensa
tion products previously employed, unexpectedly
Obviously the baking temperature and the bak
better results are _obtainable by associating with
Certain condensation products (now obtain
able from the Reichhold Chemicals, Inc., and
from the American Cyanamid Company, respec
tively) which are useful in the practice of the
the glyoxal one or more amino-aldehyde water
dispersible resinous condensation products, for y
example urea or melamine formaldehyde, but
ing time are inversely related.
'
employing such resinous condensation products 40 present invention but which as yet have no estab
in amounts far too small (except in association
lished chemical names, are herein for conven
with the glyoxal) to accomplish either stabiliza
ience referred to as “Beckamine P-364” and
tion or crushproofing. Further, Wholly unex
“Aerotex M-3,” and are herein identified and de
pectedly it has -been discovered that when thus
fined respectively as follows:
used in association*y the stabilizing effect of the 45
Beckamine P-364 is a water-dispersible con
combined resin and glyoxal is even greater than
densation product of urea formaldehyde. Its
that of the equivalent amount of either material
preparation is fully described in copending ap
alone and that damage to the fabric is less than
plication Serial No. 540,883, filed June 17, 1944.
might result from an equivalent amount of either
and assigned to Reichhold Chemicals, Inc., Bos
the glyoxal or the resin condensation product by
ton, Massachusetts, from which this reagent may
itself.
be obtained.
For certain purposes, for instance in the man
Aerotex M-3 is a methylated methylol-mel
ufacture of men’s sport shirts, it is desirable that
the fabric be very soft and possess» excellent drap
ing qualities or in other words that it should
have a very “soft hand,” although this charac
teristic is not normally possessed by most fabrics
1amine and may be prepared substantially as fol
ows:
Formula-960 parts by Weight of formalin
(37% by Weight CHzO) and 252 parts by Weight
of melamine are charged into a reaction vessel
made from synthetic fibers. 'It has further been
fitted with an agitator, thermometer, and reflux
discoveredthat when the glyoxal and resin are
condenser and arranged so that it can be placed
thus used in association,- as above suggested, a 60 under a vacuum and heated. The contents of
very soft -hand or feel may be imparted to the
the reaction vessel are heated for one-half hour
fabric by including in the treating bath a cation
to a temperature of 62° C. and the pH adjusted
active softener, for example one of the quater
to 7.5 with 2 normal NaOH. After heating for
nary ammonium compounds.
another one-half hour, a vacuum of 28 inches
As described in the aforesaid application, it is
of mercury is applied and the mixture concen
found desirable, in order to hasten the action
trated by removal of water. After 40 minutes’
and to avoid overheating of certain types of
heating at approximately 54° C. the heat and
fabric, to employ an acid catalyst to facilitate
vacuum are removed and there is added 1000
the reaction between the glyoxal and the ce1
-parts by weight of methyl alcohol containing
lulose of the fiber. «Among such catalysts may 70 enough 2 normal HaPO4 to neutralize the 2 nor- y
be mentioned oxalic acid, ammonium chloride,
mal NaOH added previously. The mixture at a
ammonium sulphate, and ammonium nitrate.
pH of 6.4 is then heated to distill off an azeo
Oxalic acid is highly satisfactory since vits use
tropic mixture of methanol and water, anhydrous
avoids the development of any substantial color
methanol being continuously added to replace
during heat treatment.
75 the distillate. After heating in this way for
i
'
,
'
5
9,419,888
'
_
about 8 to 'I hours, one part~ of the distillate will
tolerate 100 partsof toluol and the resin is, con
6‘.
--
_
.
Exmru 2
-
p
.A plain weave, 60% spun viscose rayon and 40%
acetate rayon fabric in the greige made oi' blended
sidered dried. It is then concentrated under a
vacuum of 28 inches oi' mercury to a solids' con
30/2-19 Z turns in the singles and 13 8 turns in
tent of approximately 50%- The methylated 5 the ply in both warp and filling yarns is desized,
methylol-melamine thus prepared may be dis'
scoured, and dried on the tenter frame. The loss
persed in water to a concentration of 10% resin
on the above operation if, 2.25 inches per yard
solids.
_
corresponding to 6.2%. The white. pure finished
Hereinafter, when Beckamine P-364 and Aero-fabric has a count of 65 x 4g, and a Weight of 6,5
'18X M-3 are referred t0» it 1S understood that 10 oz. per yard. This fabric is then passed through
these terms designate the products above de'
an impregnating Solution containing
cc. of
scribed respectively, or the equivalents thereof.
glycxal solution (at 30.2% glyoxal content by
The IOUOWIDE Special examples are given as u“
weight), 3 grams of oxalic acid, and 45 .grams of
lustrßtive 0f the application 0f the Present novel
a water-dispersible condensation product of urea
process as a practical matter in materials 0f dif- 16 formaldehyde (producedby Reichhold- chemicals
ferent types.
‘
‘
‘
Inc. and designated as P-364 Beckamine) per
EXAMPLE ’1
liter of solution. This urea formaldehyde prod
uct is condensed to a molecular weight such that
A plain weave, 100% spun viscose rayon fabric
it is completely dispersible in` water in a very
in the greige, made of 28/1 warp and 14/1 iilling 20 finely divided state, but is not sufficiently soluble
yarns of spun viscose rayon staple fiber is de-
to produce a clear solution.
On a weight per
sized, scoured and dried on the tenter frame.
centage basis this solution contains 2.25% gly
The white, pure finished fabric has a count of
oxal, 0.296% oxalic acid, and 3.36% urea formal
66 x 41 and a weight of 4 oz. per yard. This
dehyde reaction product by weight. After the
fabric is then passed through an impregnating 25 fabric is passed through this solution and is well
solution containing 60 cubic centimeters of glywetted out, it is squeezed to remove excess solu
oxal solution (0f 30.2% . glyOXal @Ontent by
weight) , 3 grams of oxalic acid, and 45 grams of
a water dispersible condensation product of urea
tion and is then dried on a tenter frame in air
at around 180° F. to' dimensions before impreg
' nating. The dried fabric is then cured in a tenter
formaldehyde (produced by Reichhold Chemicals 30 frame oven or loop dryer oven in circulating
Inc. and designated as P-364 Beckamine) per
air at '280° F. for 8 minutes, after which it is
liter of solution. This urea formaldehyde product
soaped, rinsed and dried t'o the original pure
is condensed to a molecular weight such that it is
finish fabric dimensions on a tenter frame. The
-completely dispersible in water in a very finely
resulting fabric is white, free from any odor, firm
divided state, but is not sufficiently soluble to 35 and resilient, with greatly improved resistance to
produce a clear solution. On a weight percentage
shrinkage on washing, which effect is permanent
basis this solution contains 2.25% glyoxal, 0.296%
to washing, and hasv improved resistance to creas
oxalic acid, and 3.36% urea formaldehyde reacing and crushing. A comparison of these proper
tion product by weight. After the fabric is passed
ties of the untreated pure finish fabric and of
through this solution and is well wetted out, it is 40 the treated fabric is shown below. 'I'he .table
squeezed to remove excess solution and is then
shows only the warp shrinkage. The ñllingv
dried on a, tenter frame in air at around 180° F.
shrinkage is always much lower in the untreated
to dimensions. before impregnating. The dried
fabric and is also satisfactorily controlled. The
'fabric is then cured in a tenter oven or loop dryer
tensile strength and abrasion resistance of the
oven in circulating air at 280° F. for 8 minutes, 45 fabric are not appreciably affected by the process.
after which it is soaped, rinsed, and dried to the
original pure finish fabric dimensions on a tenter
shrinkage 0n washing. inches per 216ml
frame. The resulting fabric is white, free from
any odor, ñrm and resilient’ with greatly improved l
o o
[5 modified rayon washes-mildnsiga?i solution at 100 -120 F. for 30
resistance to shrinkage on washing, which effect 50
is permanent to washing, and has improved re
sistance to creasing and crushing. A comparison
washes _______________ __ Wim) wrm Wârp Wîrp Wgm
of these properties of the untreated pure finish
fabric and of the treated fabric is shown below.
untreated _____________ __
The tensile strength and abrasion resistance of 55 Treated --------------- --
3.5
0
3.9
-1
4,43
-1
4.25
«2
4.20
‘~1
the fabric are not appreciably affected by the
process_
l
l Denotes a gain.
Shrink-age on washing, inches per yard
[5 modified rayon washes-mild soap solution at 100°-l20° F. for 30 min.]
Warp Filling Warp Filling Warp Filling Warp Filling Warp Filling
Washes .............. _.
untreated _________
Treated ............. -..
1
2
a
4
5
6.10
1.27
ara
1.50
7.13
1.47
7.03
1.30
7.2;
1.27
0
.1
0.2
.1
.1
.2
.1
.2
.1
.2
The process loss is 1.3 inches per yard in the
warp, none in the filling.
'I'he process loss is .9 inch per yard in the warp.
Creuse resistance
Crease resistance
[Percentage recovery in one min. from a 180° fold formed
under standard conditions]
[Percentage recovery in one min. from a 180° fold formed under
Untreated
Treated
,
Per cent
45
Untreated
85 75 Treated
standard conditions]
Per cent
70
I
80
9,412,882
7
oxal, 2.98% voxalic acidv and 3.0% Aerotex M3 by
weight. After the fabric is passed through this
solution and is well wetted out. it is squeezed to
_Exmrns 3
A 2 x 2 twill, 70% spun viscose rayon and 30%
spun acetate rayon fabric in the greige, made of
blended 20/2-15 Z turns in the singles and 8 8
turns in the ply in both warp and filling yarns is
desized, scoured and dried on the tenter frame.
The loss on the above operation is 0.98 inch per
yard corresponding to 2.7%. The white, pure
remove excess solution and is then dried on a
tenter frame in air at` around 180° F. to dimen
sions before impregnating. The dried fabric is
then cured in a tenter oven or loop dryer oven in
circulating air at 280° F. for 8 minutes, after
which it is soaped, rinsed and dried to the origi
finished fabric has a count of 56 x 47, and a
weight of 8.8 oz. per yard. . This fabric is then
nal pure -finish fabric dimensions on a tenter
frame. The resulting fabric is white, free from
odor, firm and resilient, with greatly improved re
sistance -to shrinkage on washing, which effect is
passed through an impregnating solution con
taining 60 cubic centimeters of glyoxal solution
(of 30.2% glyoxal content by weight) , 3 grams of
oxalic acid and 40 cubic centimeters of a water
soluble. thermosetting alkyl urea formaldehyde
` permanent to washing, and has improved resist
ance to creasing and crushing. A comparison of
these properties of the untreated. Dure finish
condensation product (manufactured by Sharples
fabric and of the treated fabric is shown below. -
Chemicals Company) per liter of solution. On a
The table shows only the warp shrinkage. The
filling shrinkage is always much lower in the un
weight percentage basis this solution contains
2.25% glyoxal, .296% oxalic acid and 1.95% alkyl 20 treated fabric, and is also satisfactorily con
urea formaldehyde reaction product by weight.
trolled. The tensile strength and abrasion resist
After the fabric is passed through this solution
ance of the fabric are not appreciably aHected by
and is well wetted out, it is squeezed to remove ex
cess solution and is then dried on a tenter frame
the process.
«
Shrinkage on washing, inches per yard
in air at around 180° F. to dimensions before'im 25 [5 modified rayon washes-mili?) soâi’pl solution at 100°-lm° F. for
pregnating. The dried fabric is then cured in a
m
.
ì
tenter oven or loop dryer oven in circulating air
at 280° F. for 8 minutes, after which itis soaped,
rinsed and dried to the original pure finish fabric
Warp
Warp
Washes ............... ..
`
`
l
2
dimensions on a tenter frame. The resulting 30
fabric is white, free from any odor, firm and re
Untreated _____________ ._
2.83
Treated ............... ._
0
'
Wer
War
W
3 p
4 p
grp
3.06
3.1
3.2
3.a
.3
. l
.3
.2
silient, with greatly improved resistance to
shrinkage on washing, which effect is permanent
The process loss is .6 inch per yard in the warp.
to washing, and has improved resistance to creas
ing and crushing, A comparison of these proper 35
ties of the untreated pure finish fabric and of the'
treated fabric is shown below. The tensile
strength and abrasion resistance of the fabric are
notappreciably affected by the process.
.
Grease resistance
[Percentage recovery in one minute from a 180° fold formed under
standard conditions]
Per cent
Untreated __Treated _
____
..-__
45
60
shrinkage on washing, inches per yard
[5 modiilcd rayon washes-mild soap solution at l00°-120° F. for 30 min.]
Warp Filling Warp Filling Warp Filling Warp Filling Warp Filling
washes .............. _.
1
Untreated ........... _. 4
Treated ............. ._
2.25
.1
2
.a
`1
2.11
.1
3
.26
0
3.55
O
Í4
.4s
0
The process loss is .8 inch per yard in the warp,
I and .5 inch per yard in the filling.
Crease resistance
[Percentage recovery in one min. from a 180° fold formed under
standard conditions]
Per cent
Untreated ______________________________ _..
80
Treated _______________________________ __
90
3.6
.2
5
.se
.l
3.91
.2
.es
0
EXAMPLE 5
A plain weave, 85% spun viscose rayon and
15% Aralac (casein'flber) fabric in the greige
made of blended 21/1-16 Z turns in the singles
55 in both warp and filling yarns, is desized, scoured
and dried on a tenter frame.
The loss in the
above operation is 0.56 inch per yard corrcspond-`
ing to 1.6%. The white, pure finished fabric has
a count of 69 x 55 and a weight of 4.7 oz. per
EXAMPLE 4
60 yard. This fabric is then passed through anim
pregnating solution containing 60 cubic centi
A 100% plain woven filament viscose rayon
Y meters of glyoxal solution (of 30.2% glyoxal con
fabric made of 98 denier warp and 152 denier fill
tent by weight), 3 grams of oxalic acid, 30 grams
ing yarns, with a count of 92 x 70 and weighing
of the water-dispersible urea formaldehyde con
2.7 oz, per yard is desized, scoured and dried on
the tenter frame. The loss in the above operation 65 densation product designated as P--364 Beck
is .1 inch per yard correspondingto .3%. 'I'he
amine and 20 grams of the water-soluble mela
white. pure finished fabric is passed through an „
impregnating-solution containing 60 cubic centi
mine formaldehyde reaction product known as
Aerotex M3, per liter of solution. _On a weight
meters of glyoxal solution (of 30.2% glyoxal con
percentage basis this solution contains 2.25% gly
tent by weight). 3 grams of oxalic acid, and 38 70 oxal, .296% oxalic acid, 2.24% P-364 Beckamine
and 1.56% Aerotex M3 by weight. After the
grams of a water-soluble condensation product
of melamine formaldehyde (produced by Ameri
fabric is passed through this solution and is well
can Cyanamid Company and designated as Aero
wetted out, it is squeezed to remove excess solu
tex M3) per liter of solution. On a weight per
tion and is then dried on a tenter frame in air at
centage basis this solution contains 2.25% gly 75 around 180° F. to dimensions before impregnat
2,412,832
»
10
lower in the untreated fabric, and is also satis
factorily controlled. The tensile strength and
abrasion resistance of the fabric are not appre
ciably affected by the process.
shrinkage on washing, inches per yard
ing. The dried fabric is then cured in a tenter
oven or loop dryer oven in circulating air at 280°
F. for 8 minutes, after which it is soaped, rinsed,
and dried to the original pure finish fabric di
mensions on a tenter frame. The resulting
fabric is white, free from odor, firm and resilient,
[5 modified rayon washes-mild soa solution at 100°-120° F. for 30
with greatly improved resistance to shrinkage on
washing, which effect is permanent to washing,
and has improved resistance to creasing and
`
Warp Warp Warp Warp Warp
Washes _______________ _ _
1
2
3
. 4
ñ
crushing. A comparison of these properties of
the untreated pure finish fabric and of the treat
Untreated _____________ __
6. 10
6. 53
7. 13
7. O3
7. 2i
ed fabric is shown below. The table shows only
Treated_..`: ........... ._
0
.1
D
.l
.1
the warp shrinkage. The filling shrinkage is al
ways much lower in the untreated fabric, and
is also satisfactorily controlled. 'I'he tensile 15 4The process loss is 1.3inches per yard in th
warp.
_
strength and abrasion resistance of the fabric
Crease resistance
are not appreciably affected by the process.
[Percentage recovery in one min. from l80° fold formed under
Shrinkage on washing, inches per yard
'
standard conditions]
.
,
[5 modified rayon washes-mild soa solution at 100°-l20° F.
for 30 min.
Warp Warp Warp Warp
20
Warp
min.
'
Per cent
45
Untreated ___
Treated
..-__
EXAMPLE 7
A plain weave, 100% spun viscose rayon fabric
Una-eared _____________ __
3.9
4.06
aoc
4.03
AL23 25 in the greige, made of 28/1 warp and 14/1 ñll
Treated ............... __
i
0
.1
.3
_
.3
.3
ing yarns of spun viscose rayon staple fiber is
desized, scoured and dried on a tenter frame.
The process loss is 1.3 inches per yard in the
The white, pure finished fabric has a count of
Warp.
66 x 41 and a weight of 4 oz. per yard. 'I‘his
C'rease resistance
30 fabric is then passed through an impregnating
[Percentage recovery in one min. from a 180° fold formed under
solution containing 60 cubic centimeters of gly
Washes.-.
1
2
3
4
5
standard conditions]
oxal solution (of 30.2% glyoxal content by
Per cent
Untreated _____________________________ __
50
Treated
80
________________________________ __
weight) , 3 grams of oxalic acid, 45 grams of wa
ter-dispersible urea formaldehyde condensation
product known as P-364 Beckamine, and 6 grams
of the quaternary ammonium salt, octa decyl
oxymethyl pyridiniumv chloride per liter of solu
tion. On a weight percentage basis this solution
EXAMPLE 6
A plain weave, 100% spun viscose rayon fabric
in the greige, made of 28/1 warp and 14/1 filling
contains 2.25% glyoxal, 0.296% oxalic acid, 3.36%
yarns of spun rayon viscose rayon staple fiber is 40 urea formaldehyde reaction product and 0.56%
desized, scoured, and dried on the tenter frame.
quartemary compound by weight. After the
The white,«pure finished fabric has a count of
fabric is passed through this solution and is
66 X 41 and a weight of 4 oz. per yard. This
well wetted out, it is squeezed to remove excess
fabric is then passed through an impregnating
solution and is then dried on a tenter frame in
solution containing 60 cubic centimeters of gly
air at around 180° F. to dimensions before im
oxal solution (of 30.2% glyoxal content -by
pregnating. The dried fabric is then cured in a
weight), 3 grams of oxalic acid, 45 grams of a
tenter oven or loop dryer oven in circulating air
water-dispersible condensation product of urea
at 280° F. for 8 minutes, after which it is soaped.
formaldehyde (produced by Reichhold Chemicals
rinsed and dried to the original pure finish fabric
Inc., and designated as P-364 Beckamine), and
dimensions on a tenter frame. The resulting
10 grams of NOPCO 1322-X neutralized with .5
fabric is white, free from any odor, soft and re
gram oxaiic acid. NOPCO 1322-X belongs to the
silient, with greatly improved resistance to
class of quaternary ammonium compounds re
shrinkage on washing. which effect is perma
ferred to as cation-active softeners. On a
nent to washing, and has improved resistance
weight percentage basis this solution contains ' to creasing and crushing. The fabric is found
2.25% glyoxal, 0.346% oxalic acid, 3.36% urea
to be water-repellent and retains most of its wa.
formaldehyde reaction product, and 0.976%
NOPCO 1322-X by weight. After the fabric is
passed through this solution and is well wetted
out, it is squeezed to remove excess solution and
is then dried on a tenter frame in air at around
180° F. to dimensions before impregnating. The
dried fabric is then cured in a tenter oven or
loop dryer oven in circulating air at 280° F. for 8
minutes after which it is soaped, rinsed and dried
to the original pure ñnish fabric dimensions on
a tenter frame. The resulting fabric is white,
free from odor, soft and resilient, with greatly
improved resistance to shrinkage on washing,
which effect is permanent to washing, and has
improved resistance to creasing and crushing.
A comparison of these properties of the untreated
pure ñnish fabric and of the treated fabric is
shown below. The table shows only the warp
shrinkage. The ?lling shrinkage is always much .CA
ter repellency through at least five launderings.
A comparison of these properties of the untreated
pure ñnish fabric and of the treated fabric is
shown below. The table shows only the 'warp
shrinkage. The filling shrinkage is always much
lower in the untreated fabric, and is also satis
factorily controlled. The tensile strength and
abrasion resistance of the fabric are not appre
ciably affected by the process.
Shrinkage on washing, inches per yard
l', modified rayon washes-mild soa solution at l00°-120° F. for 30
.
min.
W'ashes _______________ ._
War
1 p
War
2 p
War
3 p
W
4am
untreated _____________ _ .
e. lo
e. 53
7.13
7.03
7. 2i
Treated _______________ _-
. 1
0
0
0
. 1
Wgr!)
9,412,l82
12
' The process loss is 1.5 inches per yard in the
warp.
The mixed process in which both glyoxal and
resinous material are employed not only pro
‘
Crease resistance
l duces dimensional -stability but also crushre
sistance. However, it is important to note -that
[Percentage recovery in one min. from a 180° fold formed under
the crush resistance is apparentlyproduced sole
ly by the glyoxal since there is not sumcient resin
to have any appreciable effect on crush resistance.
standard conditions]
\
Untreated
___--
Per cent
45
It will be -observed that in no case is the
Treated
95
quantity of resin employed in association with
As more particularly pointed out `in the afore 10 .the glyoxal even as much as 50%> of the resin re
said application, it appears that the glyoxal treat
quired when resin alone is used for stabilization.
ment affects the individual fiber throughout its
It is also to be emphasized, as indicated by the
entire structure, causing a partial but incomplete
-conversion of the cellulose. Apparently the same
- above specific examples, that the resin in associa
tion with the glyoxal not only produces dimen
actiontakes place when the glyoxal is employed 15 sional stability but also crush resistance. How
in association with a resin.
«
ever, the crush resistance must be attributed> to
It is our belief that when cellulose ñbers are
the glyoxal since there is not. suiiicient resin to
treated with a thermosetting resinous compound
produce crush resistance, it being notedthat for
there is a ydefinite reaction between the cellulose
effective crush resistance it is necessary when
and the resinous material and that some further 20 using resin alone to employ even more than the
condensation of the resinous material with itself
8% shown in column 6, in fact to employ 14%
also takes place during the curing operation.
or more of the resin.
We base our belief (with reference to the auto
To illustrate .the neutral effect of the resin upon
condensation of the resinous material) upon the
crease resistance, when used in the small per
fact that an increase inV wet strength of the 25 centages of the present invention, a fabric like
fabric is observed when compared with the re
that of Example 1 above described was stabilized
sults produced by reacting the cellulose material
using two different formulae as follows:
wtih glyoxal alone. Apparently the combined
1. 60 cc. of glyoxal (30.2%) per liter, 3 grams
treatment of cellulose fibers with glyoxal and a
resinous material is to produce a fiber consisting
in part of a reaction product of cellulose and
glyoxal and in part of a reaction product of
of oxalic acid per liter.
2. 60 cc. of glyoxal (30.2%) per liter, 45 grams
of P-364 Beckamine (75% resin content) per
cellulose and the resinous material, with the
The following table shows the wash stability re
sults obtained with these two treatments, with
liter, 3 grams of oxalic acid per liter.
resinous material in a more highly condensed
state after curing than it was originally. What
ever actually takes place in the cellulose fiber
when subjected to the combined treatment-with
glyoxal and the thermosetting resin, it is cer
tain that the physical characteristics of the fiber
are thereby modified. ,
.
a working loss >of 1.4 inches.
'
' .
Warp shrinkage-5 modified washes
washes ..... .............
1
Untreated fabric ........... __
I
2
s
4
5
6. l
6. 5
7. l
7. 0
7. 2
1.1
1.2
1.3
1.4
1.4
40
For ready comparison ofthe results obtained
by the present invention with those obtained by
Treated [abrio:
1 ....................... ._
2 ____________________ _ _ l _ _
0
0
0
. 1
. l
prior usual methods of stabilization by the em
ployment of resins alone, or bythe use of glyoxal
alone as described in the aforementioned appli
The following table shows the results with these
cation, reference may be had to the table shown
same two >treatments regarding tensile strength,
in the drawing. In this table. column A indicates
crease resistance and abrasion resistance.
usual losses in scouring; columnB the shrink
age of normal ~(untreated) fabric during five
Tensile strength
standard laundry washings; column 1 indicates 50
the shrinkage losses in fabrics which have been
Dry
treated with glyoxal alone; column 3 shows the
losses in >fabric treated with resin alone: and co1
vumn 2 indicates losses in fabric treated with gly
oxal together with a small mount of resinous con
densation product.`
et
Untroated____ Warp
5l 121g“
59 Warp
Grease
resist-
Abrssion
resistance
ance
(Taber)
29
45 135 turns.
.
In each of the columns B and 1 'to 3 inclusive,
:there is a subcolumn headed “%5” and a second
Treated:
1___
'
____
37
40
23
2l
85
2 _______ _ _
46
60
26
28
85
Satisfactory.
Do.
subcolumn headed “%1-5.” The column headed
"%5” represents the total shrinkage of the treat (Si)
Thus while the addition of the small quantity
ed fabric in iive’modiiied washes without any
of resin in accordance with the present invention
process or working loss allowed. The column
does'improve shrinkage control or dimensional
headed “%1-5" _represents the difference in the
stability and in some cases may improve the
measurements of the abrio between the first and
finish of the fabric, it apparently contributes
ñfth wash, or in ther words, the progressive
nothing substantial to the crush resistance of
shrinkage between the first wash and the fifth
.the fabric.
i.
.
wash. For example, if a fabric shows 3% shrink
As indicated in the above specific examples,
ase in the first wash and it still shows 3% shrink
-various types of resinous condensation product
age after the fifth Wash, the %1-5 shrinkage is 0.
maybe used, among them the reaction product of
The table shows that the addition of a small 70 urea and formaldehyde, known as dimethylol
quantity of resin to the glyoxal produces better
urea. Among the other resinous materials which
stabilization than results from the use of glyoxal
are useful for the purpose is P-364 Beckamine.
alone. For instance, the results obtained in col
This is a reaction product of urea and formalde
umn 2 are in most instances considerably better
hyde in which the reaction or condensation is car
than those obtained in column l.
75 ried to the point where the material no longer
13
2,412,232
forms a clear solution in water but actually
. forms an extremely fine dispersion. In fact, this
material is film forming from water dispersion
14
Reaction proceeds according to the following
equation:
R-CONH-ClIzOH + H-N-X
which is not the case with a dimethylol urea
solution. The P-364 Beckamine is also very
stable on storage for this type of material. A
dimethylol urea solution is not stable on storage.
The alkyl urea resinous condensation product is
formed by the reaction of _an alkyl substituted
urea and formaldehyde simultaneously with the 10
reaction of urea and formaldehyde so that the
The above synthesis does not apply where the
final material might be called a co-condensation
acid radical selected for X is the radical of a weak
~ product of urea and substituted urea with formal
acid, for instance-_acetic or formic. For wealr
dehyde. The material is deflnitely film forming
acid as acetic
'
and produces a stable solution in water.
Another useful resin is Aerotex M3, a water
soluble reaction product of low molecular weight
of melamine and formaldehyde. It is water-sol
uble and the solution is quite stable on storage.
It appears to be i'llm forming from water solution 20
R-CONH-CHr-O-COCH: + N -4
to a certain degree.
It is also to be observed as indicated vin the
above specific examples, that more than one resin
may be used in association with the glyoxal in the
treating bath, but in any event the total quan 25
tity of resinous material is quite low, in fact
substantiallyless than one-half the amount of
resinous material which `would be lrequired for
R-CONH-CHa-’ _iD-COOH:
While certain examples have hereinabove been
given as illustrative of the utility of this inven
stabilization if no glyoxal were employed. For
best results it appears that substantially the same 30 tion, we consider it to be applicable to a wide
limiting quantities of glyoxal should- be used as
when glyoxal is employed alone, while the quan
tity of resinous material would appear to be with
variety of textile materials including fibers, yarns
and fabric of
weight.
(1) Regenerated cellulose
a-Viscose
to the fabric a cation-active softener is added to
the treating bath in an amount approximately
(2) Cotton cellulose
in a range of from 1% to 5% of the solution by
35
When it is desired to impart a. soft hand or feel ~
1% by weight of the bath.
The term “cation-active” as used in the pres 40
ent sense, simply means that the active part of
.
b-Cuprammonium
c-Saponified acetate
(3) Mixtures-Major part cellulose
a-Viscose-acetate
b-Viscose-aralac (casein)
c-Viscose-soya bean protein
the molecule in these compounds is the cation
d-Viscose-peanut protein
rather than the anion, as is usual with many of
e-Viscose-Wool
i
the present finishing agents and dyes. Most cat
f-Viscose-cotton
ion-active compounds may be considered as de 45
(4) Spun and iilament yarns.
rived from ammonium hydroxide NH4OH where
one or more of the H’s are replaced by complex
It is to be understood that the above are merely
organic radicals. One type includes the quater
by way of example and not by Way of limitation,
nary ammonium compounds. Some are relative
and that the invention is inclusive of all modifi
ly simple while others are extremely complex 50 cations and equivalents falling within the ‘terms
products containing nitrogenous bases, such as
of the appended claims.
pyridine, quinoline, acridine replacing the H’s in
the NH4 group.
The possibilities in new com
1. The method of stabilizing regenerated cellu
lose textile material which comprises as steps
55 impregnating the material with an aqueous
glyoxal solution containing between 0.6% and
4.65% by weight of glyoxal, an acid catalyst and
an amino-formaldehyde thermosetting resinous
condensation product in amount between 1% and
wherein
60 5% of the solution by weight, removing the mate
rial from the solution, and baking the material
R stands for an alkyl radical containing not less
at a temperature between 212° F. and 350° F.
than 8 C atoms.
2. The method of stabilizing textile fabric pre
The group N(tert)„Í represents the molecule of a
dominantly of yarns of regenerated cellulose
tertiary base such as trimethylamine or pyri
bo which comprises as steps immersing the fabric in
dine.
an aqueous solution containing glyoxal. approxi
X represents the acidic radical, preferably of a
mately in the amount of 0.6% to 4.65% by weight
weak acid as typified by acetic or formic.
in the treating solution, an amino-formaldehyde
thermosetting resinous condensation product in
Mode of synthesis
total amount between 1% and 5% by vweight of
Heat together an acylamidomethylol compound,
the solution, and oxalic'acid, expressing excess>
for instance stearoamidomethanol with a salt of
fluid, drying the fabric under tension and bak
pyridine corresponding to the iinal salt desired,
ing the fabric at a temperature between `212" F.
for instance pyridine hydrochloride in an’excess
and 350° F. for a period of between two minutes
75 andfortyminutes.
’
of the free base.
pounds of this type seem unlimited.
'I'he empirical formula of the pyridinium com
pounds can be represented by
R-coNH-cHz-Ndem-‘x
¿nasse _
3. The method of stabilizing textile fabric pre
and an acid catalyst, until it is thoroughly wet,
drying the fabric,~> baking it at a temperature be
dominantly of yarns of viscose rayon Iwhich com
prises as steps immersing `said fabric in a water
tween 212° F. and 350° F. for a period of from
solution `containing between 0.6% and 4.65% by
two minutes to forty minutes, thereby to react the
weight of glyoxal, between 1% and 5% by weight 5 cellulose of the yarns with the glyoxal, and wash
of an amino-formaldehyde thermosetting resin
ing, rinsing and drying the fabric. `
.
ous water-dispersible condensation product,A and
5. As a new article of manufacture, the product
between 0.0125% and 0.40% acid catalyst by . producedvaccording tothe method set forth in
weight, until it is thoroughly wet, extracting ex
claim 1.
»
cess liquid, drying the fabric, and baking the l0. ,6. As a new article of-manufacture, the prod- fabric to react the glyoxal with the cellulose of
uct produced according to the method set forth
the yarn.
L
`
in-claim 2.
4. 'I'he method of stabilizing textile fabric pre
dominantly of yarns of. regenerated cellulose
which comprises a‘s steps immersing said fabric in
an aqueous treating medium containing from 15
to 120 cc. of an approximately 30% glyoxal solu
tion (30.2% glyoxal by weight) and from 20 to
50 grams of a Water-dispersible urea-formalde
hyde condensation product per liter of solution 20g
7. As a new article of manufacture, the prod
uct produced according to _the method set forth
in claim 3.
8. As a new article of manufacture. the prod
uct produced according to the method set forth
in claim 4.
‘
`
.,
‘
EDWARD C.. PFEFFER, Jn.
JACK EPELBERG.
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