Note: Descriptions are shown in the official language in which they were submitted.
-` lO~V940
The invention pertains to curing catalyst combinations for textile
resins.
Various catalysts and accelerators have been employed in the curing
of thermosetting aminoplast resins in the finishing of cellulosic textile
materials. Such catalysts include metal salts of the strong inorganic acid
salts of such metals as zinc, magnesium, and the like. Van Loo et al in U.S.
Patent 3,084,071 teach the use of water-soluble aluminum salts of aluminum
chloride, aluminum nitrate, and aluminum sulfate as accelerators for water-
soluble thermosetting aminoplast resins on 80 x 80 cotton percale. Such
finishes normally produce wrinkle recovery values of about 250F. to about
300F. as measured on a Monsanto Wrinkle Recovery Tester. However, the total
tensile strength ~warp ~ fill) of the materials so finished is lower than
; normally desired, usually being 20 to 60 pounds as measured on a Scott
Tester, where an untreated value of 80-100 or more is desired. It has been
recognized that as wrinkle recovery values increase, tensile strength losses
also increase, therefore textile finishers are required to balance wrinkle
recovery and tensile strength requirements. My invention shows improved
tensile strengths while maintaining wrinkle recovery properties over the
sluminum sulfate of the art.
Accordingly, the present invention provides in a process for curing
` a watcr-soluble thermosetting aminoplast resin treated textile material, the -
improvement which comprises treating a textile material by applying to said
material about 1% to 10% of a water-soluble thermosetting aminoplast resin,
based on the weight of the textile material, and from about 1% to 25% of a
mixture of aluminum sulfate and magnesium sulfate based on the weight of
said resin, said mixture of salts comprising from between 0.5 and 2.0 parts
of magnesium sulfate per part of aluminum sulfate and curing said resin to
' a water-insoluble state by heating the so treated textile material to a
temperature of from about 3QQ to 40QF.
,...................................... ..
The invention is the use of mixtures of aluminum
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sulfate and magnesium sulfate as curing catalysts or accel-
erators for thermosetting aminoplast textile finishing resins.
Finished cellulosic textile materials cured with thermosetting
aminoplast resins and the curing catalyst mixture of the in-
vention have high wrinkle recovery with reduced losses intensile strength.
In the process of the invention about 1 to 10% pre-
ferably about 3 to 5%, of a water-soluble thermosetting amino-
plast resin is applied to a textile material, based on the
weight of the textile material, and from about 1% to 25%, pre-
ferably about 10 to 15% of curing catalyst solids, based on
the weight of resin, and thereafter the resin is dried and
cured to react the resin with the material.
.
The cellulosic textile material to which the in-
i 15 vention is applicable are formed textile fabrics whether
knitted, woven, felted or otherwise formed, composed of at
least 20% cellulose fibers, such as cotton, viscose rayon, jute, ~-
ramie, hemp and the like. Preferably, the cellulosic textile
materials are completely of cellulosic fibers and more speci- ~
fically cotton fibers. However, blends of cellulosic fibers -
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with non-cellulose materials for example wool, various syn-
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thetic fibers, for example, polyester fibers, such as that
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sold under the trademark Dacron~ acrylic fibers such as those
l sold under the trademarks Creslan~, Acrilan~, Orlon~, ~abrics
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;~ 25 and polyamide fibers such as nylon and the like are within the
scope of the invention.
The thermosetting aminoplast resins useful in the
invention are resins which impart wrinkle resistance to cellu-
losic textile materials. These materials may be employed
singly or in combination. For example, the urea-formaldehyde
resins including the methylol ureas and the alkyl ethers
thereof, particularly the methyl ethers, the cyclic ureas, for
example, 2-imidazolidinone, 1,2- and 1,3-propylene urea, and
- 2 -
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4,5-dihydroxy-2-imidazolidinone, their formaldehyde conden-
sates and alkylated (particularly methylated) derivatives,
and the like, are within the scope of the invention. Poly-
methylol melamines and their alkylated derivatives, and more
particularly their methylated derivatives wherein from 1-6
moles of formaldehyde are combined with the melamine and from
1-6 moles of an alcohol are useful resins within the scope of
the invention. For example, dimethoxymethylmelamine, tri-
methoxymethylmelamine, tetramethoxymethylmelamine, hexa-
10 methoxymethylmelamine, and the like are useful. Methylol
derivatives of 4,5-dihydroxy-2-imidazolidinone and the methy-
lated derivatives thereof and mixtures of the methylol and
alkoxymethyl derivatives of 4,5-dihydroxy-2-imidazolidinone
with alkylated urea-formaldehyde resins and alkylated poly-
15 methylol melamines are useful resins in the invention. These
aminoplast resins are water-soluble and essentially monomeric -
in form. Minor amounts of polymer may be present in these
.. .
resins in the form of dimers, trimers, tetramers. The amino-
plast resins may also be used in combination wlth other tex- ~ ~
20 tile finishing materials such as, for example, water and oil -
repellents. Water repellents such as methylolated fiber re-
active nitrogenous compounds containing long-chain (C6-Cl~)
alkyl or alkoxyl groups, such as N-methylol stearamide, are
~ useful. Oil repellents such as polycarbon fluorocarbons, for
t 25 example, are also useful in the invention. Curing catalysts
are usually applied as aqueous solutions containing 20 to 100
' - by weight of catalyst solids. The catalyst mixture of the in-
vention comprise aqueous solutions containing about 20~ total
catalyst solids comprising a mixture of from about 0.50 part
30 to about 2.0 parts, preferably from about 0.75 part to about
J 1.5 parts, magnesium sulfate per part of aluminum sulfate.
The curing catalysts may be applied to textile materials with
the resinous composition. The catalyst and resinous composi-
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11)4~9~0
tion may be applied by any conventional technique, such as
immersion, padding, spraying and the like and followed, where
necessary, by squeezing, hydroextraction or similar processes,
in order to affix the desired amount of catalyst solids onto
the fabric. For fibrous cellulosic materials, concentrations
of total catalyst solids of from about O.01 to 2.5% and more,
particularly from 0.15 to 0.75~, based on the dry weight of
the fabric may be used. In the examples below the concentra-
tion of the catalyst is reported on the weight of the pad
bath employed.
Following the application of the resin and curing
catalyst to the textile fabric, the material is subject to
drying and curing operations to effect the properties of
shrinkage control and wrinkle resistance. The drying and
curing operation may be carried out in a single step or in
separate steps. The temperatures at which the drying and - - -
curing operations are effective vary widely and are influ-
i enced to some extent by the fabric and type of resin employed.
Normally, the range of temperature extends from about 180F.
to about 400F. or even higher. Generally, the time of the
drying or curing operation is inversely proportional to the
temperature employed, and iis influenced by whether or not
separate or combined drying and curing steps are employed.
Generally, when drying and curing are carried out in a com-
bined operation, at time of from about 1 minute to about 10
~ minutes may be employed at temperatures from about 225F. to
$ - 400F. respectively. When the fabric has been dried prelim-
inary to curing, curing times of 5 minutes to about 0.5 minute
at a temperature of from 300 and 400F., respectively, are
successfully employed.
In the examples below, the wrinkle recovery of the ~ ~
treated fabric is measured in degrees on a Monsanto Wrinkle ~ - -
Recovery Tester following the American Association of Textile
- 4 -
1(~4~)940
Chemists and Colorists (AATCC) Test Method 66-1972. The tensile strength of
the fabric is measured in pounds on a Scott Tester by the Grab Method, accord-
ing to the A.S.T~M. standards.
The following examples are illustrative of the invention and are
not to be construed as limitative. Parts and percentages are by weight unless
otherwise designated.
Example 1
An aqueous pad bath is prepared conta;ning 4.5% by weight solids of
1,3-bis(hydroxymethyl)-4,5-dihydroxy-2-imidazolidinone, 0.6% by weight of
magnesium sulfate and 0.05% by weight of aluminum sulfate, an application is
made to 80 x 80 cotton percale by padding, an 82% wet pickup on the weight of
the untreated fabric being obtained. The fabric is dried at 225 F. and cured
at 325 F. for 1.5 minutes. The results obtained are as follows: -
pH of Total (Warp ~ Fill) Tensile Strength
bath Wrinkle Recovery Warp (lbs.) Fill (lbs.)
.--. -~ ......................................................................... ................. .."-;
4.1 251 43 31 ;
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xamples 2-8
Six aqueous pad baths are prepared each containing 4.5% by weight
resin solids of 1,3-bis(hydroxymethyl)-4,5-dihydroxy_2_;m;dazolidinone, 0.1%
of a commercial non-ionic surfactant, Deceresol Surfactant NI* conc., and
various amounts of either a~ ;num sulfate or magnesium sulfàte as the
accelerator. Application is made to 80 x 80 cotton percale by padding, and
82% wet pickup on the weight of the untreated fabrics being obtained. The
fabrics are then dried at 225 F. and cured at 325 F. for 1.5 minutes. The
results are reported in Table I.
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Examples 9 -13
Five aqueous pad baths are prepared, each con-
taining 4.5% by weight resin solids of 1,3-bis(hydroxymethyl)-
4,5-dihydroxy-2-imidazolidinone, 0.1% of a commercial non-
ionic surfactant (Deceresol Surfactant NI Conc.) and 0.29%
~` by weight of aluminum sulfate plus varying amounts of magne-
sium sulfate as the accelerator. Application is made to 80 x
80 cotton percale by padding, an 80~ wet pickup on the weight
of the untreated fabric being obtained. The fabrics are then
dried at 225F. and cured at 325F. for 1.5 minutes. The
results are reported in Table II. Example 11 shows that a
higher total tensile strength is obtained with the accelerator
of this invention for 305F. wrinkle recovery than obtained
in Examples 5 and 6 of Table I with aluminum sulfate alone.
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Examples 14-l9
Five aqueous pad baths are prepared with the same
ingredients as in Examples 9-13 except that the amount of
aluminum sulfate used in each bath is 0.23% by weight. The
application, drying, and curing are carried out as in Ex-
amples 9-13. The results obtained are reported in Table III.
These results show again the higher total tensile strength
obtained with the accelerator of this invention than that
obtained with aluminum sulfate in Table I for comparable
wrinkle recovery values.
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Examples 20-23
An aqueous solution containing 11.5~ by weight of
aluminum sulfate and 9.8% by weight of magnesium sulfate was
prepared by dissolving the required amounts of the respective
salts in water. This composition was then evaluated on dif-
ferent textile materials as an accelerator for pre-cure pro-
cesses versus a commercial accelerator.
Four aqueous pad baths were prepared having the
following compositions in percentage amounts as shown below
10 in Table IV.
TABLE IV
Example No. 20 21 22 23
Commercial Resin (1) 10 10 25 25
Commercial Accelerator (2) 2 -- 5 --
15 Accelerator of this Invention-- 2 -- 5 -
Deceresol Surfactant N.I. Conc. (3~ 0.1 0.1 0.1 0.1
~ Pad Bath pH 5.4 3.8 4.0 3.6
t~ (1) The commercial resin is a 45~ aqueous solution of
'! 1,3-bis(hYdroxymethyl)-4,5~dihydroxy-2-imidazoli-
dinone.
(2) The commercial accelerator is an aqueous solution
of 30% by weight magnesium chloride.
(3) A non-ionic surfactant comprising an ethylene
oxide addition product of nonylphenol. - -
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The pad baths containing 2% by weight of the ac- ;
celerator solution were applied to 80 x 80 cotton percale and
the baths containing 5% by weight of the activator solutions
- - were applied to 65/35 polyester/cotton, and viscose rayon -~
challis. Application was by padding to obtain a wet pickup
of 70% on 80 x 80 cotton, 55~ on 65/35 polyester/cotton and
110% on viscose challis, respectively. All samples were dried
i. at225F. for 1.5 minutes and cured at 350F. for 1.5 minutes
except for the viscose challis which was cured for 2.0 minutes
,~ at 320F. The results obtained are reported in Tables V and VI.
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(1) All washes reported in Table V consisted of a normal
cycle at 110F. using a 4 lb. load, a high setting and 90
grams of AATCC Standard Detergent No. 124, followed by tumble
drying after the last wash.
(2) AATCC Test Method 114-1971
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~3) Discoloration of fabric, both 80 x 80 cotton and 65/35 -
polyester/cotton shirting, after heating with AATCC Scorch
Tester for 60 seconds at 400F., initially and after
treatment with chlorine as per (2) above. The higher the
rating, the less the discoloration; a rating of 5 equals no
discoloration. ~ -
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(4) AATCC Test Method 124-1971 was used. The higher the
rating, the better the durable press appearance; a rating of
5 is the maximum value attainable. ;~
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(5) AATCC Test Method 112-1972 (Modified) was used on fabric
having 5-10% residual moisture. The results, in parts per
million, are averages of four sepàrate tests.
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Examples 24-25
Two pad baths are prepared each containing 4.5%
real of 1,3-bis(hydroxymethyl)-4,5-dihydroxy-2-imidazolidi-
none, 5% by weight of a commercial water repellent (Aerotex
Water Repellent 96) and 3% by weight of a commercial fluoro-
carbon oil repellent (Pentel~ G-26, from Pennwalt Corp.).
One pad bath contains 2% by weight of a commercial accelera- "
tor, while the other contains 2~ by weight of an aqueous
solution of the catalyst of this invention. The pad baths
are applied to 80 x 80 cotton percale to obtain a wet pickup
of 80%, and the treated fabrics are then dried for 1.5 minutes
at 225F. and cured for 1.5 minutes at 350F. The water and
oil repellencies of the treated fabrics are measured initi-
ally, after one dry cleaning, and five washings. The results
obtained are shown in Table VII.
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