U.S. patent number 3,849,158 [Application Number 05/386,037] was granted by the patent office on 1974-11-19 for carpet embossing in register with print.
This patent grant is currently assigned to Congoleum Industries, Inc.. Invention is credited to Robert P. Conger, Leon B. Palmer.
United States Patent |
3,849,158 |
Palmer , et al. |
November 19, 1974 |
CARPET EMBOSSING IN REGISTER WITH PRINT
Abstract
Pile fabrics prepared from nylon carpet fibers having a textured
or embossed surface and a process of developing the textured effect
which comprises selectively contacting the surface of said carpet
with a chemical fiber shrinking agent therefore, allowing the
shrinking action to occur and, thereafter, effectively removing the
shrinking agent from the surface, said shrinking serving to reduce
the height of the pile in the treated areas and creating said
textured surface.
Inventors: |
Palmer; Leon B. (Little Falls,
NJ), Conger; Robert P. (Park Ridge, NJ) |
Assignee: |
Congoleum Industries, Inc.
(Kearny, NJ)
|
Family
ID: |
23523894 |
Appl.
No.: |
05/386,037 |
Filed: |
August 6, 1973 |
Current U.S.
Class: |
8/497; 8/598;
8/574; 8/601; 8/929; 28/160; 8/570; 8/575; 8/599; 8/924; 26/69B;
156/277 |
Current CPC
Class: |
D06Q
1/06 (20130101); Y10S 8/929 (20130101); Y10S
8/924 (20130101) |
Current International
Class: |
D06Q
1/06 (20060101); D06Q 1/00 (20060101); B44d
001/02 (); B44d 005/02 (); D03d 027/00 () |
Field of
Search: |
;161/63 ;156/277
;117/8.5,9,11 ;26/69B ;28/76P |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Van Balen; William J.
Attorney, Agent or Firm: Laughlin; Richard T.
Claims
What is claimed is:
1. A process for producing an embossed effect on nylon pile fabric
having a surface of nylon fibers which comprises,
applying to defined areas of the pile surface of said fabric a
chemical embossing agent for said fibers,
said agent being an azole having a five membered heterocyclic
aromatic ring or fused aromatic ring containing two or more
heteroatoms, in the five membered ring, at least one of which is
always nitrogen, blended into a liquid base vehicle, said liquid
base vehicle also including an acid,
allowing said embossing agent in its vehicle to remain in contact
with said fibers for a period of time and at a temperature
sufficient to reduce the height of said pile, without deterioration
of said fibers,
and, thereafter, effectively removing the embossing agent from the
fabric,
said reduction in height of the fibers being in the area contacted
by said embossing agent only and being a reduction sufficient to
display a significant embossed effect in the overall fabric.
2. A process of claim 1 wherein said embossing agent is
benzotriazole with acetic acid in concentrations of 5% to 50%
benzotriazole and 15% to 60% glacial acetic acid by weight, of
total embossing composition.
3. A process of claim 2 wherein said embossing agent is
incorporated in a transparent vehicle therefor.
4. A process of claim 2 wherein said embossed effect is made in
register with a printed color design on said fabric and
said vehicle is a dye printing paste carrying said embossing
agent.
5. The process of claim 2 wherein said embossing action occurs
within approximately 15 minutes at a temperature above
50.degree.C.
6. A process in accordance with claim 5 wherein said embossing
action occurs in a steam environment.
7. A process of claim 6 wherein said embossing composition is
present in a concentration of about 45 to 65% in the vehicle
therefor.
8. A process of claim 7 wherein said embossing agent is
benzotriazole and hydroxyacetic acid.
9. A process of claim 7 wherein said embossing agent is
benzotriazole and formic acid.
10. A process of claim 7 wherein said embossing agent is
benzotriazole and phosphoric acid.
11. A process of claim 7 wherein said embossing agent is
benzotriazole and oxalic acid.
12. A process of claim 7 wherein said embossing agent is
benzotriazole and hydrochloric acid.
13. A process of claim 7 wherein said embossing agent is
benzotriazole and propionic acid.
14. A process of claim 7 wherein said embossing agent is
benzotriazole and citric acid.
15. A process of claim 7 wherein said embossing agent is
benzotriazole and sulfuric acid.
16. A process of claim 7 wherein said embossing agent is
benzotriazole and maleic acid.
17. A process of claim 7 wherein said embossing agent is
benzotriazole and monochloroacetic acid.
18. A process of claim 7 wherein said embossing agent is
benzotriazole and acrylic acid.
19. A process of claim 7 wherein said embossing agent is pyrrole
and acetic acid.
20. A process of claim 7 wherein said embossing agent is indole and
acetic acid.
21. A process of claim 7 wherein said embossing agent is
2-methylindole and acetic acid.
22. A process of claim 7 wherein said embossing agent is pyrazole
and acetic acid.
23. A process of claim 7 wherein said embossing agent is
5-chloroindazole and acetic acid.
24. A process of claim 7 wherein said embossing agent is
5-chlorobenzotriazole and acetic acid.
25. A process of claim 7 wherein said embossing agent is
1-hydroxylbenzotriazole monohydrate and acetic acid.
26. A process of claim 7 wherein said embossing agent is
5-aminotetrazole monohydrate, and acetic acid.
27. A process of claim 7 wherein said embossing agent is
benzothiazole and acetic acid.
Description
BACKGROUND OF THE INVENTION
In the production of nylon pile fabrics, it is often desirable to
emboss the surface thereof in order to provide added decorative
appeal. In some instances, the embossed areas are printed with dyes
to further embellish the surface design.
Embossing the pile fabrics is conventionally accomplished with a
heating embossing roll or plate which has been engraved or
otherwise treated to create the design desired in raised relief on
the surface. A method which eliminates the use of embossing rolls
has been disclosed in U.S. Pat. Nos. 2,790,255 and 2,875,504. In
accordance with these patents, the pile fabric is formed from a
combination of shrinkable and non-shrinkable yarns. Upon subjecting
the fabric to the influence of heat, the pile formed from the
shrinkable yarns contracts while the base and the non-shrinkable
yarns remain intact thereby yielding a pile made up of high and low
areas to give the appearance of an embossed or carved product.
A chemical embossing method is disclosed in U.S. Pat. No.
2,020,698. According to this patent, fabric having a pile of
organic ester of cellulose yarn is locally treated with an alkali
or alkaline salt saponifying agent in order to obtain ornamental
differential effects in the treated areas. Furthermore, since the
organic ester of cellulose pile yarns that have not been saponified
are more difficult to change from their position, after they are
once set than are the saponified organic ester of cellulose yarn,
it is possible to obtain a differential lay between the saponified
and unsaponified organic ester of cellulose pile yarn. Thus, the
fabric, after the application of the saponifying agent, may be
washed, finished and dried with the pile erect, after which the
fabric may be run through water and brushed across the piece to lay
the pile towards the selvage and it is then dried. This causes the
saponified pile yarn to lie flat while the unsaponified yarn
remains substantially erect. Upon subsequent steaming and brushing
the fabric in the opposite direction, any unsaponified yarn which
may have been slightly bent from the vertical by the previous
brushing toward the selvage is caused to stand erect without
disturbing the position of the laid or crushed saponified organic
ester of cellulose pile yarn.
SUMMARY OF THE INVENTION
It is the primary object of this invention to provide a simple
process for producing a nylon pile having a textured or embossed
surface.
Another object is to provide such a process which is readily
adaptable to standard printing equipment.
Another object is to provide a process which allows the production
of pile fabric having embossed areas in register with a printed
design.
A further object is to provide an embossing process which is
readily adaptable to curved and irregular surfaces.
Various other objects and advantages of this invention will be
apparent from the following detailed description thereof.
It has now been discovered that it is possible to produce superior
nylon pile fabrics having embossed surfaces by contacting selected
portions of the surfaces with a chemical embossing agent for the
fibers of said pile fabric causing dimensional change by linear
contraction of the treated fibers and, thereafter, effectively
removing the embossing agent. The resulting product is thus
depressed at the treated areas.
The embossing composition can be transparent so that the appearance
of the product is not altered other than in being embossed.
Alternatively, the embossing agent can be part of a dye or pigment
composition used in printing the fabric so that the color appears
in perfect register in the areas of embossing agent
application.
The depth of the depressed areas can be controlled by varying the
concentration and/or type of embossing agent. This variation in
concentration can be effected by the amount of vehicle applied as
well as by the strength of the embossing reagent.
Furthermore, the embossed depth can be controlled to some degree by
the depth of penetration of the print paste carrying the embossing
agent as well as the steamer time and steamer temperatures to which
the pile fabric is subjected in order to activate the chemical
embossing agents which provide the desired effect.
This discovery makes possible the production of a product having
embossed surfaces which can be in complete register with a printed
design. Additionally, the discovery makes possible the utilization
of many types of printing apparatus for purposes of effecting
embossing, thereby eliminating the need for expensive embossing
equipment. Further, it allows the embossing of a surface without
exerting sufficient pressure to permanently deform the pile fabric.
A great number of products can be produced by the process. They can
be used for floor, wall and ceiling coverings, drapery, upholstery
and the like, and, in fact wherever pile fabrics are utilized. They
are readily adaptable to decorating any surface on which pile
fabrics can be applied. Many additional applications will occur to
those skilled in the art.
This invention will be better understood from the following
detailed description thereof together with the accompanying
self-explanatory drawings in which:
FIG. 1 is an enlarged top view of a section of an embossed product
of this invention; and,
FIG. 2 is an enlarged cross-sectional view of the same product
taken through line 2--2.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the production of the pile fabrics of this invention, the pile
yarn employed is nylon. Synthetic fibers prepared from polyamides
such as nylon are well known to those skilled in the art.
Likewise, the embossing agents which are applied to the nylon
fibers in order to produce the desired effect are also known
chemical compounds. For purposes of this invention, the term
"embossing agent" is defined as any active chemical composition
which when applied to the pile fabric produces a measurable
reduction of pile height, but without significant deterioration of
the nylon fibers. The exact chemical/physical mechanism by which
this result is achieved is not completely understood. However, it
is believed that the embossing agent may owe its effectiveness
largely to its capability to function as a hydrogen bond breaker.
Initially, the fibers are in a stretched and crystalline state.
When the hydrogen bond is broken between the polymer chains, the
fibers relax and shrink. Regardless of the mechanism, the overall
effect produced is one of dimensional change, the most desirable
effect, involving linear contraction of the fiber.
In order to be applicable for the novel process of this invention,
the embossing agent should provide a reduction of the pile height
through a shrinkage reaction, should not adversely affect the
printing means, e.g., print screens, and should be capable of being
substantially removed or inactivated subsequent to the embossing
action. Other characteristics of the embossing agent which are
desirable, though not essential, include compatibility with dye
print pastes, capability of being regulated by factors of time,
temperature and concentration, i.e., susceptibility to activation
by a conventional steaming operation and exhibiting no residual
embossing activity. Needless to say, minor adjustments in the
nature of the components and process conditions, and/or the
embossing apparatus can be employed to overcome the absence of
certain of these desired characteristics.
The embossing agent for the nylon fibers is applied to one surface
of the pile fabric in any desired design, whether it be random or
predetermined. One of the easiest methods of applying the agent is
by utilizing conventional printing technique such as silk screen or
block printing. The embossing agent can be applied as a
concentrate, as part of a transparent vehicle, or as part of a dye
composition utilized for pile fabric printing. The nature of the
embossing agent dictates the nature of the vehicle to be utilized.
Among such applicable vehicles are included: water, and alcohols
such as methanol and isopropanol. Often thickeners, e.g., gums, and
cellulose derivatives, are included in order to obtain viscosity
characteristics demanded in print technology and to enable the
embossing agent to adhere to and operate on the synthetic fiber and
to hold the printed pattern.
In those instances where it is desired to achieve a single- or
multi-colored printed decoration with a distinct color for the
embossed areas, the embossing agent can be incorporated into a
particular dye or pigment composition. The dye or pigment will
generally be in the form of a print paste ink to which the
appropriate amount of agent is added. It is to be noted that in
preparing these modified dye compositions, the pH levels,
viscosities, and dye concentrations which are essential to an
effficient dyeing operation must also be controlled. The resultant
effect is an embossed design in register with the printed pattern.
If different depths of embossing are sought, they are achieved by
use of different concentrations of agent in the areas calling for
such different depths.
Generally, it is desirable that the embossing agent be soluble or
in solution in the solvent medium from which it is applied to the
selected areas of the fabric. However, if the agent is not soluble
it should be in the composition in a form at least sufficiently
finely divided to pass through the print screen, that is, it should
be present in a micro pulverized form which indicates particle
diameter of the order of 100 microns or smaller. That is, it must
not only pass through a screen but it must pass through freely,
dispersed through the dye paste throughout the printing operation.
The purpose of this, of course, is to make sure that the agent
becomes uniformly dispersed over the fiber in the print process so
that the shrinking effect will be uniformly developed in the
fiber.
As previously indicated, the preferred embossing agent is one which
is dormant during the successive printing operations but then is
activated by the elevated temperature of a steam chamber usually
utilized to fix the dye onto the fibers. The embossing agents of
this invention which can function in this manner on nylon and
produce shrinkage of the nylon fibers without physical
deterioration comprise an azole such as benzotriazole in
combination with an acid such as acetic acid. When this combination
of chemicals is added to the dye print paste in the proper
concentrations and proportions, nylon carpet pile can be embossed
deeply without significant fiber deterioration exactly in register
with a printed design by shrinking the nylon fibers. While the
preferred azole is benzotriazole, other azoles containing one to
four nitrogens in the aromatic, heterocyclic, 5-membered ring may
be used. Examples are pyrrole, 5-chloroindazole,
5-chlorobenzotriazole, 5-amino tetrazole monohydrate and
benzothiazole. While acetic acid is preferred, other acids may be
used such as formic, phosphoric, citric, hydroxyacetic, oxalic,
propionic, maleic, hydrochloric and sulfuric. At the individual
concentrations employed in this process benzotriazole or its
substituted products and analogues alone, or the acid alone, are
not generally useful because of such factors as insolubility at
room temperature, ineffectiveness, volatility, toxicity,
destructiveness, cost.
The advantages of this type of chemical embossing agent are that
there is no need for rigid time control in the process and there is
minimal concern regarding excessive uncontrollable embossing
because other factors can be changed. Thus, the degree of
diminution of the pile height can be controlled by adjusting the
amount of dye paste applied, the concentration of embossing agent
in the dye paste and the temperature and time of exposure in the
steam chamber. All these factors can be adjusted according to
properties of the nylon fiber comprising the pile fabric. While the
depth of embossings will be determined by the practitioner in
accordance with the type of embossed product being prepared,
reduction in pile height will generally not exceed more than about
50%, this value being indicative of excellent embossing without
exposing the backing materials.
Embossing can be achieved, if desired, by subjecting the treated
fibers to heat for short periods of time. Thus, the treated
surfaces may be subjected to the radiation from the bank of
infrared lamps, particularly where the embossing agent is not part
of a dye print paste. Additionally, even where the steaming
operation is not essential to activate the embossing agent, such
steaming may have the effect of increasing the penetration of the
embossing agent and increasing the speed of its action on the
fibers.
A critical step of the novel process of this invention involves
terminating the embossing action and/or effective substantial
removal of the embossing agent from the pile fabric. It may be
necessary to achieve complete elimination of all residues of the
embossing process which may contribute undesirable properties to
the finished fabric, such as odor, toxicity and color and texture
change. Needless to say, any termination or quenching technique
resorted to will depend on the particular embossing composition
employed. The most useful technique for removing residues of the
embossing process is by thoroughly washing the fabric with water
and detergents. In those instances where the embossing agent is
part of a dye or pigment composition, the washing cycle is utilized
to remove excess dye of pigment serves also to remove traces of the
agent. Where an acidic embossing agent is utilized, e.g., formic
acid on nylon, it is possible to halt the embossing action more
rapidly by rinsing with an aqueous ammonia or mildly alkaline
solution. This neutralization of the acid serves to insure the
total removal thereof.
Other techniques for terminating the embossing action and/or
removing the embossing agent include evaporation and dry cleaning.
Thus, if the agent is volatile, steaming of the treated pile fabric
will serve to evaporate a large portion of the embossing agent
content. Where rinsing techniques are not effective, it may be
necessary to resort to a dry cleaning procedure to remove the
embossing residues.
The invention has particular application to tufted carpet which are
to have a printed decoration applied thereon. Unusual design
effects can also be obtained when the pile fabric is printed with a
multi-colored design wherein one or more of the dye compositions
contain the appropriate embossing agent. The process of printing
such carpets includes the steps of passing carpets, tufted or
unpigmented or colored fibers, into a screen printing apparatus
whereby a design is printed on the surface of the carpet. Each
screen applies a separate color to make up the final design. The
embossing agent can be added to one or more of these printing
stations by addition to the dye composition, or it can be applied
by a separate station in a transparent vehicle. The fabric is then
passed into a steaming chamber to set the dyes and cause embossing
and then to a washing cycle which serves to remove excess dye as
well as to terminate the embossing action and/or remove the
embossing components.
Accordingly, in the embossing of carpet or textured pile fabric,
and for all practical purposes we are discussing the embossing of
carpeting, it is important that any color design on the surface of
the carpet which is related to the embossing be in accurate
register with the embossing. Since we are concerned only with
chemical embossing the problem is then one of inducing the
differential fiber length between the embossed colored areas and
unembossed areas and, while it is possible to induce shrinkage of
synthetic nylon fibers, it is necessary for preparation of the
carpet that the film shrinkage be induced with no significant
deterioration of what is left. Thus, if the operation of embossing
involves true shrinkage the shrunk fabric fiber should have a
texture approximating that of the original.
Many azoles are largely insoluble in water at room temperature.
Some become solubilized, however, at room temperature in an acid
solution such as acetic acid. Thus, for example, while the
preferred benzotriazole is only slightly soluble in water at room
temperature (about 2% at 77.degree.F), up to at least 50%
benzotriazole goes into solution in a 40% solution of glacial
acetic acid in water at room temperature (77.degree.F) and remains
in solution. Because of this, we are able to meet an important
practical requirement that the embossing agent be preferably
soluble or at least finely dispersable in the dye print paste at
room temperature. Complete solubility or dispersability to an
extremely finely divided condition is required so that the
individual particles contained in the printing paste can pass
through the carpet printing screen and reach a maximum area of the
nylon fiber to develop the desired effect. Preferably the
solubilizing medium should be water although other solvents may be
employed. However, the partial or total replacement of water by
another solvent may cause a reduction in the extent of carpet
embossment by the benzotriazole/acid embossing agent.
A number of factors appear to influence the effectiveness of azoles
as embossing agents for nylon carpet. These include the location
and number of nitrogen atoms in the azole ring, the presence of the
active hydrogen atom on the azole ring nitrogen, the type and
location of substituent groups, the presence of heteroatoms such as
oxygen and sulfur in the azole ring, the type and concentration of
acid employed, the ratio of azole to acid and the extent of
solubility of the azole in acid solution at room temperature.
As noted before, benzotriazole is the preferred azole. In addition
to its ready solubility in acid solution at room temperature,
benzotriazole is preferred because of its manageability (safe
margin between fiber shrinkage and fiber destruction),
effectiveness as an embossing agent, nonoffensive odor, lack of
volatility, ease of handling and relative nontoxicity.
Suitable combinations of benzotriazole and acetic acid are selected
from within approximately the following broad range of
concentrations for each component as to obtain nylon carpet
embossment to the desired depth. These ranges represent parts per
hundred of the total print paste.
Benzotriazole 5-50
Galcial Acetic Acid 60-15
Preferably, however, the proportions of benzotriazole and acetic
acid will be selected from within approximately the following
narrower ranges.
Benzotriazole 15-30
Glacial Acetic Acid 45-25
Within these concentration ranges, the individual components used
alone are unsuitable for nylon carpet embossment. At the
concentration needed for carpet embossment, benzotriazole is
insoluble in water at room temperature and the destructive effect
of benzotriazole on nylon fibers is difficult to control, while the
concentration of acetic acid alone needed to emboss carpet will
generally exceed 60%. The combination of benzotriazole and acetic
acid provides an easily manageable and effective embossing
agent.
A procedure of trial and error is required in order to arrive at
the best proportions of benzotriazole and acetic acid or other
azoles and other acids needed to achieve a desired depth of
embossment without deterioration of the nylon carpet pile. It is,
of course, important that the nylon fibers remain physically fibers
and that the shrunk carpet pile retain its original physical
character as well as acceptable appearance and feel. Generally,
however, it will be found that the sum of the concentration of
benzotriazole and the concentration of acetic acid in the print
paste will fall within the limits of 45-65%. Whenever maximum
carpet embossment is obtained (that depth just short of fiber
deterioration, unacceptable hardness or the like) any reformulation
which calls for increasing either component should be accompanied
by a reduction in the concentration of the other component,
otherwise fiber deterioration will occur.
The concentration range within which benzotriazole and acetic acid
may be selected does not necessarily hold true for other acids and
other azoles. Suitable concentrations and proportions must be
determined by trial and error.
Depth of embossment as well as the deteriorating effect of the
embossing agent upon the nylon carpet fibers is not only related to
the strength of the embossing agent, but is also related to the
distribution and penetration of the embossing agent into the nylon
carpet pile. Therefore, print paste viscosity is important in
influencing the depth of embossing as well as the embossed pile
character since it regulates the penetration of the dye print paste
containing the embossing agent into the carpet pile as well as the
quantity of embossing agent deposited. Both penetration and amount
of embossing agent applied can also be regulated by the number of
squeegee roller strokes. Other factors effecting both shrinkage and
attack of nylon fibers are steamer time and temperature. Too long a
steamer time or too high a temperature generally aggravate nylon
fiber deterioration. Generally, it appears that the maximum
reduction in nylon carpet pile height will not exceed much more
than about 50% without fiber deterioration reflected in
unacceptable pile hardness, harshness, weakness, fusion, and the
like. Lesser embossed depths are of course obtained by altering the
proportions and/or concentrations of the components of the
embossing agent.
In order to practically evaluate the utility of a particular
chemical or combination of chemicals as an embossing agent for
nylon carpet, the chemical system is incorporated in the dye
printing paste and applied to a section of the nylon carpet by
means of a screen printing technique so as to simulate plant
production procedure as closely as possible. The treated carpet
sample is steamed about 15 minutes at 215.degree.-200.degree.F,
thoroughly rinsed with water and dried at 180.degree.F. Then the
embossed area is rubbed briskly with the finger tips or for example
by means of a wooden knife handle to loosen and separate tufts. In
the plant, this is accomplished by brushing. The depth of
embossment is then measured and observations made regarding the
character of the embossed nylon, e.g., strength, brittleness,
softness, definition, color. Measurement of the pile height at the
embossed and unembossed areas is made by means of a thin, half-inch
wide steel ruler marked off in 1/64 inch intervals. But any method
of measurement is useful so long as it is standardized from
operation to operation and is reproducible to about 1/64 inch.
However, for the preliminary determination of whether or not a
chemical composition is capable of shrinking nylon fibers and for
thus determining its potential suitability as a chemical embossing
agent for nylon carpet, we have devised a simpler, less time
consuming beaker test procedure. Using this test, the percent
shrinkage and the percent weight loss experienced by a 50
centimeter loop of nylon carpet filament or carpet yarn is
determined by immersing the yarn loop in an aqueous solution or
dispersion of the test chemical for 15 minutes at 215.degree.F
(102.degree.C). This test affords a simple way of determining what
effect a selected chemical will have on the nylon fibers and
provides a means of predicting whether or not a chemical will
function as an embossing agent for nylon carpet. Also, the test
provides a method for determining such effects as chemical
concentration, temperature, time, print paste additives, solvents
other than water, nylon type and construction and the like. Details
of the test procedure are outlined as follows in Table I.
TABLE I
BEAKER TEST PROCEDURE
1. prepare a solution or dispersion of the chemicals to be tested
in water.* If heated, cool to room temperature. Weigh 30 grams into
a 32 .times. 200 mm test tube.
2. Place test tube in preheated Silicone bath and heat contents of
test tube to the desired temperature (usually 215.degree.F
(102.degree.C)).
3. cut approximately 1 meter length of nylon yarn or filament which
has been held at 73.degree.F and 50% relative humidity for 24 hours
and tie in a single loop.
4. Hang the loop under 50 gram load for 30 seconds and measure the
length of the loop to 0.1 cm.
5. Weigh loop to nearest 1/10 mg.
6. Immerse nylon loop in hot chemical solution, agitate gently and
observe any change in character of the nylon fibers. Generally hold
for 15 minutes or less.
7. Remove the nylon loop and wash thoroughly in copious amounts of
water. Blot and dry to constant weight at 73.degree.F and 50%
relative humidity.
8. Measure length of nylon loop as in 4.**
9. Determine weight of nylon loop as in 5.
10. Calculate % shrinkage and % weight loss.
With the information thus obtained concerning the extent of
shrinkage, deterioration or destruction of the nylon fibers, it
then becomes possible to predict whether or not the chemical
composition has any potential as an embossing agent, and eventually
proceed to the formulation of a printing paste which includes the
shrinking material. Experience has shown, however, that while such
test results prove that the chemical agent will shrink nylon fiber
and thus has an embossing capability for nylon carpet, these
results tell us only roughly what concentration of the chemical
agent is required to emboss nylon carpet. Nor do we know the exact
extent of fiber deterioration that will be experienced on the nylon
carpet. Generally, the following relationship seems to exist
between beaker test results and screen printing test results on
nylon carpet. Beaker test shrinkage results must reach at least
about 50% shrinkage in 15 minutes at 215.degree.F in order for an
embossing agent to produce even trace to very weak carpet
embossment. But beyond about 50% shrinkage via the beaker test, the
nylon filament begins to deteriorate rapidly (test loop weakening
and fragmentation). On the other hand, if appears that deeply
embossed carpet can only be anticipated if the chemical shrinkage
agent causes fiber destruction in the beaker within about 60
seconds. Generally, the maximum depth of embossment obtainable
without causing unacceptable nylon carpet fiber deterioration is
usually about 50%.
Apparently, the difference between beaker test shrinkage results
obtained on a loop of nylon filament on yarn, and screen printing
test results obtained on nylon carpet, occurs because the chemical
is utilized much less effectively on the carpet pile than in the
beaker test. Screen printing does not supply sufficient print paste
(containing embossing agent) to the nylon carpet pile to provide a
completely uniform coating of the nylon fibers. Furthermore, the
depth of penetration into the carpet pile is often of the order of
only about 50%. Also, during steaming, the concentration of the
embossing agent may be reduced, and chemical which may be consumed
is not replaced. However, in the beaker test, the nylon loop is
surrounded constantly and uniformly by a surplus of hot chemical
solution of practically the same concentration throughout the
duration of the test thus allowing the chemical to function more
effectively.
The following examples will further illustrate the embodiment of
this invention. In these examples, all parts given are by weight
unless otherwise noted.
EXAMPLE I
The shrinkage and weight loss experienced by a test loop of DuPont
type 846 bulk continuous filament nylon 6/6 (1,300 denier, 68
filaments, o twist, semi-dull, regular acid dyeable) was determined
by means of the beaker test procedure described in Table I using
benzotriazole in conjunction with glacial acetic acid in water.
Test results in Table II show that, for example, an embossing
system comprising benzotriazole 20% and acetic acid 15% and water
65% causes the nylon loop to shrink 52% accompanied by a weight
loss of 2.3% in the shrunk fibers without deterioration of the
fiber properties in 15 minutes at 215.degree.F (Run No. 676).
However, the concentration of embossing agent which produces this
degree of nylon shrinkage in the beaker test generally produces
little or no shrinkage when screen printed on nylon carpet face
pile. Therefore, the beaker test procedure was further utilized to
determine the concentrations and proportions of benzotriazole and
acetic acid that would cause the nylon test loop to disintegrate
within 60 seconds. As indicated previously, this degree of attack
of the nylon filament in the beaker test is indicative of the
substantial embossment that can be expected to develop when nylon
carpet is treated with the embossing agent using a screen printing
technique. The test temperature was 215.degree.F.
Test results are shown on Table 11 for various benzotriazole/acetic
acid systems as well as for those combinations having small
portions of acetic acid replaced by other acids such as sulfuric
acid, formic acid, phosphoric acid, and toluenesulfuric acid. It is
understood that percentages shown represent the percent contained
in an aqueous solution. Also shown are shrinkage and weight loss
values for individual components at intermediate and maximum
concentrations used. A variety of concentrations and porportions of
benzotriazole and acetic acid were found to disintegrate the nylon
test loop fibers within less than 60 seconds, e.g., 35/25, 35/20,
30/25, 25/30, 27.3/27.3, 15/45, 15/47.3, 10/50, 12.5/47.5, as well
as benzotriazole 15%/acetic acid 45%/85% phosphoric acid 2.7%.
Thus, these data show that the combination of benzotriazole and
acetic acid has the capability to cause nylon fibers to shrink
strongly and therefore is a potentially good embossing agent for
nylon carpet. The replacement of small portions of acetic acid by
other acids offered no particular advantage.
TABLE II
__________________________________________________________________________
Nylon Filament Weight Run Shrinkage Loss Loop No. Chemicals* (%)
(%) Character
__________________________________________________________________________
** Water 10.5 1.27 Good 673 Benzotriazole (BTA)***, 10% 43.0 +6.83
Good 672 Benzotriazole***, 20% Gummy mass 3 minutes 671
Benzotriazole***, 30% Gummy mass 20 seconds 681 Benzotriazole***,
35% **** Disintegrate 12 seconds 682 Benzotriazole***, 40% ****
Disintegrate 10 seconds 680 Benzotriazole***, 50% **** Disintegrate
10 seconds 357 Acetic Acid, 30% 13.5 1.06 Good 659 Acetic Acid, 45%
27.0 3.92 Good 668 Acetic Acid, 50% 35.5 6.73 Good 669 Acetic Acid,
55% Broken loop 15 minutes 670 Acetic Acid, 60% Fragmented 15
minutes 337 Acetic Acid, 45%/85% Phosphoric Acid, 2.7% 29.7 3.89
Good 342 Acetic Acid, 59.3%/85% Phosphoric Acid, 3.7% Start
disintegrate 10 minutes 258 BTA, 35%/Cellosolve Solvent, 25% 38.2
4.45 Good 405 BTA, 20%/Isopropyl Alcohol, 40% 18.2 0.19 Good 676
BTA, 20%/Acetic Acid, 15% 52.2 2.32 Good 675 BTA, 25%/Acetic Acid,
15% Broken loop 15 minutes 679 BTA, 40%/Acetic Acid, 15% ****
Disintegrated 12 seconds 674 BTA, 50%/Acetic Acid, 15% ****
Disintegrated 8 seconds 254 BTA, 35%/Acetic Acid, 25% ****
Disintegrated 10 seconds 265 BTA, 35%/Acetic Acid, 20% ****
Disintegrated 10 seconds 267 BTA, 35%/Acetic Acid, 15% Fragmented
15 minutes 264 BTA, 30%/Acetic Acid, 25% Disintegrated 15 seconds
257 BTA, 30%/Acetic Acid, 20% Fragmented 15 minutes 266 BTA,
25%/Acetic Acid, 25% Fragmented 15 minutes 274 BTA, 25%/Acetic
Acid, 30% **** Disintegrated 30 seconds 318 BTA, 27.3%/Acetic Acid,
27.3% **** Disintegrated 30 seconds 324 BTA, 20%/Acetic Acid, 35%
Mostly disintegrated 15 minutes 338 BTA, 15%/Acetic Acid, 47.3%
**** Disintegrated 10 seconds 391 BTA, 15%/Acetic Acid, 45% ****
Disintegrated 25 seconds 392 BTA, 10%/Acetic Acid, 50% ****
Disintegrated 25 seconds 393 BTA, 10%/Acetic Acid, 45% Fragmented
15 minutes 394 BTA, 5%/Acetic Acid, 55% Fragmented 15 minutes 398
BTA, 25%/Acetic Acid 27.5% Fragmented 6 minutes 402 BTA,
12.5%/Acetic Acid, 47.5% **** Disintegrated 60 seconds 263 BTA,
35%/Acetic Acid 12.5%/ Cellosolve Sol. 12.5% Fragmented 15 minutes
292 BTA, 25%/Acetic Acid 22.5%/ Sulfuric Acid, 2.5% Friable 15
minutes 293 BTA, 25%/Acetic Acid 22.5%/90% Formic Acid 2.8% 72.4
21.6 Friable 295 BTA, 25%/Acetic Acid 22.5%/85% Phosphoric Acid
3.3% Fragmented 15 minutes 327 BTA, 25% Acetic Acid 20%/85%
Phosphoric Acid 6% 79.7 25.0 Friable 335 BTA, 15%/Acetic Acid
45%/85% Phosphoric Acid 2.7% **** Disintegrated 20 seconds 300 BTA,
25%/Acetic Acid 22.5%/95% Toluenesulfonic Acid 2.6% Fragmented 15
minutes
__________________________________________________________________________
*BTA = Benzotriazole. The benzotriazole is added to the acid
solution to facilitate room temperature solubility. **Avg. of 13
runs water alone at 212.degree.F. ***Approx. 200.degree.F required
to solubilize BTA in water. ****Deeply embossed carpet can be
anticipated in those instances where th beaker test shows the test
loop disintegrating within about 60 seconds. However, it may occur
that such beaker disintegrating times are too destructive for
carpet embossment. Then, the chemical concentration must be
regulated to produce a longer time to test loop disintegration.
EXAMPLE II
The shrinkage and weight loss experienced by a test loop of DuPont
type 846 bulk continuous filament nylon 6/6 (1,300) denier, 68
filament, O-twist, semi-dull, regular acid dyeable) was determined
by means of the beaker test procedure described in Table I using
the following aqueous recipes shown in Table III containing a
combination of benzotriazole and an acid other than acetic acid.
The test temperature and maximum duration of test was 215.degree.F
and 15 minutes respectively.
While the preferred acid is acetic acid as described in Example 1,
other acids such as formic, phosphoric, citric, hydroxyacetic,
oxalic, propionic, maleic, acrylic, hydrochloric, monochloroacetic
and sulfuric will also function in combination with benzotriazole
to produce shrinkage of nylon fibers. Test results are recorded in
Table III. It is understood that the percentages of components
shown represent the percent of each contained in an aqueous
solution. These data shown that by properly selecting the
concentrations and proportions of benzotriazole and any one or more
of these acids, the resulting chemical system can be expected to
emboss nylon carpet via shrinkage of the fibers. As indicated,
previously, it is generally necessary to obtain nylon fiber
disintegration within 60 seconds in the beaker test in order to
provide a benzotriazole/acid combination that will substantially
emboss nylon carpet. Usually, little or no carpet embossment can be
expected until beaker test shrinkage values exceed 50%. Whenever
beaker test results show a disintegration time of more than 60
seconds, the concentration of one or both components of the
benzotriazole/acid embossing system should be increased in order to
realize a system that will deeply emboss nylon carpet. Lesser
depths of embossment can be obtained, of course, by employing
benzotriazole/acid combinations which increase disintegration
times.
TABLE III
__________________________________________________________________________
Nylon Filament Shrink- Weight Run age Loss Loop No. Chemicals* (%)
(%) Character
__________________________________________________________________________
** Water 10.5 1.27 Good 672 Benzotriazole, 20%*** Gummy mass 3
minutes 681 Benzotriazole, 35%*** Disintegrated 12 seconds 150 90%
Formic Acid, 33.3% 16.6 0.67 Good 688 Maleic Acid, 25% 13.8 0.71
Good 687 Propionic Acid, 25% 19.2 2.28 Good 348 Acrylic Acid, 25%
16.0 1.05 Good 686 Sulfuric Acid, 10% 8.2 0.19 Good 92 Citric Acid,
50% 23.8 +4.03 Good 685 37% Hydrochloric Acid, 26.7% 43.5 16.3 V.
Weak 684 70% Hydroxyacetic Acid 35.7% 8.43 0.58 Good 683**** Oxalic
acid 2H.sub.2 O, 35% 19.6 1.80 Good 70 Monochloroacetic Acid, 25%
29.3 2.71 Good 151 85% Phosphoric Acid, 29.3% 16.5 +2.36 Good 283
BTA, 35%/Monochloracetic Acid, 25% Disintegrated 10 seconds 296
BTA, 25%/Monochloroacetic Acid, 25% Disintegrated 20 seconds 286
BTA, 25%/Monochloroacetic Acid, 20% Mostly disintegrated 15 minutes
316 BTA, 25%/Acetic Acid, 13%/Mono- chloroacetic Acid, 12% Partial
disintegrated 7 minutes 284 BTA, 35%/Propionic Acid, 25%
Disintegrated 10 seconds 303 BTA, 25%/Maleic Acid, 25% Fragmented
15 minutes 304**** BTA, 25%/85% Phosphoric Acid, 25% 61.8 1.80
Friable 315**** BTA, 25%/85% Phosphoric Acid, 29.3% 62.0 3.16
Friable 317 BTA, 25%/Oxalic Acid-2H.sub.2 O, 35% Friable 15 minutes
325 BTA, 25%/70% Hydroxyacetic Acid, 35.7% 57.1 2.10 Good 326 BTA,
25%/37% Hydrochloric Acid, 13.3% 38.6 1.17 Good 328 BTA, 25%/Citric
Acid.H.sub.2 O, 25% 65.6 +2.1 Brittle 329 BTA, 25%/37% Hydrochloric
Acid, 26.7 55.8 16.4 Fragile 330 BTA, 25%/Sulfuric Acid, 10% 36.3
0.35 Good 349 BTA, 25%/Acrylic Acid, 25% Fragmented 15 minutes 678
BTA, 15%/88% Formic Acid, 17% 49.3 0.97 Good 677 BTA, 20%/88%
Formic Acid, 17% Broken loop 15 minutes
__________________________________________________________________________
** Avg. 13 runs water alone at 212.degree.F. * BTA = Benzotriazole.
The BTA is added to the acid solution to facilitat room temperature
solubility. *** Soluble about 200.degree.F. **** Soluble above
170.degree.F.
EXAMPLE III
The shrinkage and weight loss experienced by a test loop of DuPont
type 846 bulk continuous filament nylon 6/6 (1,300 denier, 68
filaments, O-twist, semi-dull, regular acid dyeable) was determined
by means of the beaker test procedure described in Table I using
the aqueous recipes shown in Table IV containing azoles other than
benzotriazole and glacial acetic acid. The test temperature and
maximum duration of testing was 215.degree.F and 15 minutes
respectively. Test results are recorded in Table IV.
These data show that there are a number of substituted products and
analogues of benzotriazole, representative of the mono, di, tri,
and tetra azoles, which can function as shrinking agents for nylon
fibers. Depending upon the azole employed and the ratio and
concentrations of acid and azole used, the extent of shrinkage can
range from very weak after 15 minutes at 215.degree.F to total
disintegration of the nylon filament within 60 seconds.
Combinations which produce this latter effect can be anticipated to
produce strong carpet embossment.
While the preferred acid is acetic acid, other acids should be just
as effective with other azoles as with benzotriazole (See Example
II).
TABLE IV
__________________________________________________________________________
Nylon Filament ** Acetic Sol.* Shrink- Wt. Run Azole Acid at age
Loss Loop No. Type (%) (%) RT. (%) (%) Char.
__________________________________________________________________________
788) 778) Tap Water 0 0 -- 7.03 0.68 Good 804) 357 Acetic Acid 0 30
Y 13.5 1.06 Good 659 Acetic Acid 0 45 Y 27.0 3.92 Good AZOLE
__________________________________________________________________________
826 Pyrrole 25 30 Y Disintegrate 5 secs. 856 Pyrrole 20 25 Y 80.2
15.6 Friable 850 Pyrrole 15 45 Y Disintegrate 8 secs. 846 Pyrrole
35 -- N Disintegrate 3 secs. 827 Indole 25 30 N Disintegrate 5
secs. 829 2-Methylindole 25 30 N Disintegrate 10 secs. 828
N-Methylpyrrole 25 30 N 32.5 2.22 Good DIAZOLE
__________________________________________________________________________
822 Pyrazole 25 30 Y 44.5 11.4 Good 847 Pyrazole 35 0 130 27.1 3.9
Good 815 3,5-Dimethylpyrazole 25 30 Y 24.2 4.1 Good 813
5-Aminoindazole 25 30 Y 19.0 0.5 Maroon 814 5-Chloroindazole 25 30
210 Disintegrate 45 secs. 851 5-Chloroindazole 15 45 170
Disintegrate 10 secs. 276 Imidazole 25 30 Y 9.5 0.6 Good 207
Imidazole 50 0 Y 27.3 7.2 Good 275 Benzimidazole 25 30 Y 18.6 +0.6
Good 812 1-Methylimidazole 25 30 Y 8.1 0.6 Good TRIAZOLE
__________________________________________________________________________
735 Benzotriazole 25 30 Y Disintegrate 35 secs. 857 Benzotriazole
20 25 Y 61.3 8.1 Good 391 Benzotriazole 15 45 Y Disintegrate 25
secs. 681 Benzotriazole 35 0 200 Disintegrate 12 secs. 825
1-Methylbenzotriazole .H2O 25 30 Y 32.9 6.1 Good 741
1-Hydroxybenzotriazole 25 30 180 65.7 7.8 Fragile 746
5-Chlorobenzotriazole 25 30 190 Disintegrate 40 secs. 832
1-Hydroxybenzotriazole .H2O 28.3 30 180 Fragmented 15 mins. 737
1,2,4 - Triazole 25 30 Y 20.5 2.9 Good 738 3-Amino-1,2,4-Triazole
25 30 150 13.0 1.5 Good 830 Urazole 25 30 215 20.9 1.7 Good
TETRAZOLE
__________________________________________________________________________
820 5-Aminotetrazole.H2O 25 30 200 33.2 4.9 Good 831
5-Aminotetrazole.H2O 30.5 30 200 40.1 7.0 Good 852
5-Aminotetrazole.H2O 15 45 190 62.8 28.8 Fragile 849
5-Aminotetrazole.H2O 35 0 215 7.8 +0.3 Good 883
1,5-Pentamethylenet- etrazole 25 30 Y 22.5 4.67 Good OXAZOLE
__________________________________________________________________________
821 2-Methylbenzoxazole 25 30 Y 41.3 2.7 Brown ISOOXAZOLE
__________________________________________________________________________
809 5-Methylisoxazole 25 30 Y 30.8 6.7 Good 808
3,5-Dimethylisoxazole 25 30 Y 26.2 5.9 Good THIAZOLE
__________________________________________________________________________
833 Benzothiazole 25 30 N Fragmented 15 mins. 853 Benzothiazole 15
45 Y 82.3 36.7 Fragile 818 Aminothiazole 25 30 Y 13.8 0.7 Brown 823
2-Amino-6-Methoxy- benzothiazole 25 30 Y 24.6 +0.5 Good 816
2-Methylbenzothiazole 25 30 N 34.8 +19.2 Wk. spot 844
2-Chlorobenzothiazole 25 30 N 26.0 +3.1 Good OXADIAZOLE
__________________________________________________________________________
855 3,4 Dimethylfurazan 25 30 Y 34.4 7.7 Good THIADIAZOLE
__________________________________________________________________________
825 2,1,3-Benzothiaziazole 25 30 N 23.0 2.3 Good
__________________________________________________________________________
* RT = room temperature. Y=Yes N=insoluble or immicible even at
215.degree.F. Other figures indicate temperature .degree.F at which
solubility occurs. ** 15 minutes at 215.degree.F unless otherwise
indicated.
EXAMPLE IV
This example illustrates the preparation of an embossed pile fabric
typical of the products of this invention.
A 4 inch by 7 1/2 inch rectangular area of nylon carpet was treated
by means of a screen printing technique with a dye print paste
containing 27.5% benzotriazole and 25% glacial acetic acid by
weight as the embossing agent.
Carpet construction was as follows:
Type --100% nylon 6/6, spun yarn, non heat set
Face Weight -- 28 oz./yd. sq. (950 grams/sq. meter)
Machine Gauge -- 5/32 inch (3.96 millimeters)
Machine Stitch Rate --9.6 stitches/inch (3.8
stitches/centimeter)
Pile Height -- 17/32 inch, (1.35 centimeters) singles
The dye print paste was formulated as follows:
SAMPLE NO. 278SP Material * Grams
______________________________________ 1. Water 24.2 2. Cibaphasol
AS 0.5 3. Antifoam 73 0.8 4. Kelzan (1%) (0.2% Dowicide A) 22.0 5.
Acetic Acid, Glacial 25.0 6. Benzotriazole 27.5 7. Dye 0.1
______________________________________ *2 = Sulfuric acid ester,
Levelling and pentrating agent 3 = Alcohol ether, antifoaming agent
4 = Xanthan gum thickner plus preservative in water to provide a
Brookfield viscosity of 760 cps. at 78.degree.F (No. 3 Spindle,
21/2 rpm.
There was no evidence of embossing while the nylon carpet was held
at room temperature for several minutes. Upon subjecting the carpet
to steaming for 15 minutes at about 218.degree.F, significant
embossing due to fiber shrinkage was observed. Thereafter, the
embossed carpet was throughly rinsed with water and dried. The
rinsing removed residual chemicals. The embossed nylon pile was
rubbed briskly.
The resulting carpet exhibited excellent embossing with a 44%
reduction in pile height in the treated area in perfect register
with the printed rectangle. Despite this degree of shrinkage, the
nylon tufts retained their individuality and, while increasing in
firmness remained acceptably soft. There was no evidence of
deterioration of fiber physical properties.
EXAMPLE V
The nylon carpet construction cited in Example IV was again treated
by means of a screen printing technique. However, in this case the
concentration and proportion of benzotriazole and acetic acid were
changed substantially so that the dye print paste contained 15%
benzotriazole and 45% glacial acetic acid by weight as the
embossing agent.
The dye print paste used was as follows:
SAMPLE NO. 411SP Material * Grams
______________________________________ 1. Water 17.2 2. Cibaphasol
AS 1.0 3. Antifoam 73 0.8 4. Polygum 260 (5%) 21.0 5. Acetic Acid,
Glacial 45.0 6. Benzotriazole 15.0 7. Dye 0.05
______________________________________ *4 -- Locust bean gum
thickener providing a Brookfield viscosity of 1,200 cps. at
78.degree.F (No. 3 spindle, 21/2 rpm)
Once again there was little evidence of embossing while the nylon
carpet was held at room temperature. Upon subjecting the carpet to
steaming at about 215.degree.F for a period of 15 minutes,
significant embossing due to shrinkage of the nylon carpet pile was
noted. Thereafter, the embossed carpet was rinsed and dried. The
embossed nylon pile was rubbed briskly.
The resulting carpet exhibited an area with a 41% reduction in pile
height in register with the printed area. The shrunk tufts were
well defined, strong and while somewhat firmer, were acceptable
soft.
While it is obvious that a number of concentrations and proportions
of benzotriazole and acetic acid serve very effectively as
embossing agents for nylon carpet (see Example VI, Table V),
generally that combination of benzotriazole and acid will be
selected so as to provide the desired embossment most economically.
Thus, since benzotriazole is by far the more expensive component,
the most economical combination will comprise a low concentration
of benzotriazole and a high concentration of acetic acid such as
shown by the subject example.
EXAMPLE VI
Additional embossed nylon carpets were prepared by means of the
embossing procedure described in Example IV, hereinabove, utilizing
various concentrations and proportions of benzotriazole and acetic
acid contained in the dye print paste as shown in Table IV.
Corresponding depths of embossment and embossed pile character are
indicated in Table V.
TABLE V
__________________________________________________________________________
Carpet Embossment Sample BTA/Acetic Acid* Paste** Depth No. (% in
Paste) Visc. (cps.) (%) Pile Character
__________________________________________________________________________
262SP 35/25 360 53 Hard, Harsh 271SP 25/25 480 31 Soft, Good 279SP
30/25 760 50 V. Firm, Harsh 299SP 35/20 720 50 V. Firm, Harsh 301SP
28/25 520 44 Firm, Good 320SP 25/30 960 41 Firm, Good 328SP
27.3/27.3 760 44 Firm, Good 371SP 25/30 1160 47 Firm, Good 372SP
15/45 1480 47 Firm, Good 392SP 10/50 1320 35 Soft, Good 399SP 3/60
1200 35 Soft, Good 418SP 15/45 1000 41 Firm, Good
__________________________________________________________________________
* BTA = Benzotriazole ** Brookfield 78.degree.F, No. 3 spindle,
21/2 rpm. Xanthan gum thickener all samples.
In recapitulation, it is to be understood that the process of
embossed carpet involves manipulation corresponding to that of
printing a pattern on the carpet. Where mere embossment is sought
the printed composition is colorless. Where the design combines
color with the embossment a dye paste is the vehicle generally,
whether the operation be a mere embossment or an embossment
combined with dyeing. It is preferred that there be no shrinkage of
the nylon fibers at ambient temperatures, even up to 50.degree.C.
In plant operations the delay from printing to steaming may be as
such as 8-10 minutes. Hence, if there is no significant effect on
the material at temperatures below 50.degree. C for 15-20 minutes
there is ample time for operations. That is, activation of the
shrinkage is reserved for the stage where the printed material
enters the steaming operation. In standard carpet handling the
steaming is a 10-20 minute operation to fix the dye and in this
stage the embossing is completed in the first few minutes.
For effective embossment there should be at least perceptible
shrinkage in the tufts. Generally penetration of the embossing
print paste will be of the order of 50%. Where it is desired to
have full depth coloration of the printed area uniformly to the
back of the fabric, this can be accomplished by predying the carpet
completely to the back by means of an operation such as pad dyeing.
Where it is desired to have full coloration of the area uniformly
to the back of the fabric it is desirable to predye the carpet
completely to the back by means of an operation such as pad dyeing.
It should be apparent that in operations where mere embossment is
sought there is no significant problem in the placement of the
design on the fabric. Where embossment is combined with a
multi-colored print there is the register problem and the color
area will be in perfect register with the embossed design when the
shrinking agent is combined with the color paste as set forth in
detail in the examples.
It is thus seen from this data, that a variety of concentrations
and proportions of benzotriazole and acetic acid are readily
applicable to the novel process of this invention.
In the production of the pile fabrics of this invention, the pile
yarn employed is prepared from fiber-forming synthetic linear
polyamides. Examples of these fiber-forming synthetic linear
polyamides are those obtainable from polymerizable
monoaminomonocarboxylic acids and their amide-forming derivatives
including caprolactam and those obtainable from the reaction of
suitable diamines with suitable dibasic carboxylic acids or their
amide-forming derivatives. Such synthetic linear polyamides are
referred to as nylon.
Nylon or polyamide polymers, filaments and fibers are well known to
those skilled in the art and extensive discussion is, therefore,
unnecessary. Thus the term "polyamide" or "nylon" is known to
include any long chain synthetic polymeric amide which has
recurring amide groups as an integral part of the main polymer
chain and which is capable of being formed into a filament in which
the structural elements are oriented in the direction of the axis
of that chain.
Polyamide resins coming within this definition and contemplated in
the practice of the present invention are formed generally by
reaction of a diacarboxylic acid with a diamine or by a
self-condensation of an aminocarboxylic acid. Illustrative of these
polyamide resins are nylon -6,6, prepared by the condensation of
hexamethylenediamine and adipic acid; nylon -6,10, prepared from
hexamethylenediamine and sebacic acid, both of the foregoing
having, as prepared, molecular weights exceeding 10,000: nylon-6
produced by thermal polymerization of epsilon-aminocaproic acid of
caprolactam; nylon-11, the self-condensation products of
11-aminoundecanoic acid; as well as a variety of polymers prepared
from polymerized, unsaturated fatty acids and polyamine
compounds.
The practice of the present invention has, however, particular
application to solid melt-extrudable and orientable fiber-forming
polyamides and more particularly to fibers and filaments prepared
therefrom which have a denier and tenacity appropriate, and well
known to those skilled in the art, for use in carpet, rugs,
tapestry and the like. Illustrative of these polyamides are those
having a filament denier of 2-30 or higher or nylon yarns in the
denier range of 15-15,000 or higher. The tenacities of nylon yarn
for use herein are within the range of 3-10 grams per denier. The
elongation of commercial fibers can range between 15 and 65%. The
undrawn filament is capable of being stretched as much as 5 times.
It is understood additionally that encompassed within the
polyamides that can be employed in the practice of this invention
are high molecular weight synthetic linear polyamides, in addition
to those described hereinabove, that have been modified, for
example, to enhance their usefulness for particular
applications.
An extended discussion of polyamides of sufficiently high molecular
weight to be capable of being melt spun into filaments and coming
within the contemplation of this invention appears in D. E. Floyd,
Polyamide Resins, Reinhold Plastics Application Series, Reinhold
Publishing Corporation, New York, N.Y. (2d printing, 1961), and H.
R. Mauersberger, Matthews' Textile Chemical Properties, John Wiley
and Sons, Inc., New York, N.Y., pp. 933-971, 1034., (6th ed. 1954),
Mary E. Carter, Essential Fiber Chemistry, Marcel Dekker, Inc., New
York, N.Y. 1971 pp. 91-109, H. F. Mark, S. M. Atlas, E. Cernis
(Edited by), Man-Made Fibers, Science and Technology, Volume 2,
Interscience Publishers 1968, pp. 181-295, Tech.-Talk from Monsanto
Textiles Division Bulletin TT-35 August 1969.
Summarizing, it is thus seen that this invention provides a novel
and effective method for embossing nylon pile fabrics.
Variations may be made in procedures, proportions, and materials
without departing from the scope of the invention as defined in the
following claims.
* * * * *