Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
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1
r:FTgpDS OF MAKING DISPERSIBLE ADDITIVES
FOR POLYMERIC MATERIALS
c-'ttOS S-REFERENCE
This application is a division of application n°
2,191,990 filed on December 3, 1996.
FTFr.D OF INVENTION
The present invention generally relates to thermo-
plastic polymeric materials containing one or more additives.
More specifically, the invention as broadly
disclosed, relates to synthetic filament additives (e. g.,
colorants) and to methods for incorporating such additives in
melt flows of filament-forming thermoplastic polymeric
materials prior to melt-spinning to form synthetic filaments
theref rom .
However, the invention as claimed is restricted to a
method of making an additive for polymeric materials.
BACKGROUND AND SUMMARY OF THE INVENTION
Th,e incorporation of additives in so-called "neat"
thermoplastic polymeric host materials (that is, polymeric
materials containing no additives) so as to achieve desired
physical properties is well known. Thus, the art has
conventionally incorporated colorants, stabilizers,
delusterants, flame retardants, fillers, antimicrobial agents,
antistatic agents, optical brighteners, extenders, processing
aids and other functional additives into polymeric host
materials in an effort to "engineer" desired properties of the
resulting additive-containing polymeric host material. Such
additives are typically added any time prior to shaping of the
polymeric material, for example, by spinning or molding (e. g.,
extrusion, injection, or blow-molding) operations.
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The incorporation of colorant additives in filaments
formed by melt-spinning a polymeric material has presented
unique challenges. For example, the amount of particulate
pigment dispersed in a concentrate which is added to the
polymeric material must be sufficiently high to impart
satisfactory color density, but must not be so high as to
interrupt the spinning process. One prior proposal for
incorporating colorant additives in thermoplastic polymeric
materials is disclosed in U.S. Patent No. 5,236,645 to Frank R.
Jones on August 17, 1993.
According to the Jones '645 patent, additives are
introduced into a thermoplastic melt by feeding at least one
additive in an aqueous vehicle containing a dispersant to form
an aqueous additive stream to a vented extruder which is
extruding a thermoplastic. The aqueous portion of the aqueous
additive stream is thereby volatilized within the extruder and
is removed therefrom via an extruder vent. As a result, a
substantially homogeneous system containing the thermoplastic,
dispersant and the additive is obtained which may thereafter be
spun into a filament by melt-extrusion through filament-forming
orifices in a spinneret associated with a spin pack assembly.
Although the techniques disclosed in the Jones '645
patent are entirely satisfactory, some further improvements to
incorporating additives in a melt flow of thermoplastic
polymeric materials would be desirable. For example, it would
especially be desirable if the additive stream was non-aqueous
as this would obviate the need for a vented extruder (i.e.;
since a volatilized aqueous portion of the additive stream
would not then need to escape prior to melt-spinning).
Furthermore, it is entirely possible that a non-aqueous
additive stream could be introduced physically near or into the
spin pack assembly where it can be mixed with a melt flow of
the polymeric material immediately upstream of the spinneret
orifices (and preferably downstream of the polymer filter
section of the spin pack assembly) thereby bypassing the
extruder. Such a possibility would then allow additive
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concentration and/or types to be changed on a continuous basis
to produce sequential lengths of melt-spun filaments having
desired, but different, properties and/or characteristics.
That is, the upstream processing equipment, for example, the
extruders and process piping, which supply the polymeric host
material to the spin pack assembly would not necessarily need
to be shut down for purposes of cleaning. Furthermore, by
introducing a non-aqueous additive stream directly into the
spin pack assembly, the flushing time would be relatively short
thereby allowing, for example, quick color changes to occur
from one filament production batch to another. It is towards
providing such improvements that the invention as broadly
disclosed hereinafter is directed.
The present invention as it is claimed hereinafter is
directed to a method of making an additive from concentrate
system for introduction into a thermoplastic polymeric
material, comprising the steps of:
(i) coating a pigment with a dispersant by forming
an aqueous dispersion containing solid pigment
particles and a dispersant, and spray drying the
aqueous dispersion so as to obtain solid
dispersant-coated pigment particles;
(ii) dispersing the solid dispersant-coated pigment
obtained according to step (i) in a liquid
nonaqueous polymeric carrier.
The additive concentrate system that is so made, may
be added directly to a melt flow of the polymeric material in
metered amounts.
The additive concentrate system that is so made
includes a filament additive which is dispersed in a liquid or
liquefied nonaqueous carrier. The filament additive may,
during use, be in the form of a solid particulate or a liquid.
When a solid particulate is used, the additive system of this
invention most preferably also includes a dispersant which
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coats the particulate additive. The additive concentrate
system according to this invention is most preferably in the
form of a flowable paste which can be added in metered amounts
(dosed) to a melt flow of the polymeric material prior to being
spun into filaments, for example near or into the spin pack
assembly upstream of the assembly's filament-forming spinneret
orifices.
In such a manner, therefore, synthetic filament
batches having different additives may be produced sequentially
on a continuous basis without costly equipment downtime. That
is, the same spin pack assembly may be used to produce a first
batch of filaments containing one type of additive during one
production interval, and then used to produce a second batch of
filaments containing a second type of additive during a
succeeding production interval by changing the additive which
is introduced into the filament-forming melt. Moreover, the
time interval needed to change between different additives is
relatively short since the additive system is most preferably
introduced into the melt flow near or into the spin pack
assembly which in turn reduces significantly the time needed to
flush residual additive incorporated into the first batch of
filaments. Production of different additive-containing
filaments (e.g., filaments containing different colorants) is
now possible in a relatively short period of time without
stopping filament winding.
Thusy another aspect of the invention as broadly
disclosed involves a method of continuously producing
sequential lengths of different additive-containing filaments
by continuously supplying a melt-spinnable polymeric host
material to orifices of a spinneret and, during a first time
interval, controllably dosing a concentrate system having one
additive into the polymeric material to form a first polymeric
mixture which is extruded through the spinneret orifices.
Subsequently, during a second time interval, another
concentrate system containing a different additive is
controllably dosed into the polymeric material without
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disrupting the continuous supply of polymeric material to the
spinneret orifices to form a second polymeric mixture which is
extruded through the spinneret orifices.
During the change of additive concentrate, an
intermediate time interval will be needed in order to flush the
spinneret of residual amounts of the first additive
concentrate. Thus, during the intermediate time intervals, an
intermediate length of filaments will be produced which will
change over the filament length from containing all of the
first additive concentrate to containing all of the second
additive concentrate. This intermediate length of filaments
produced according to the present invention will be handled
separately from the first and second lengths of production
filaments. However, the amount of such intermediate length of
filaments will be relatively small since, as noted above, the
time interval needed to flush the spinneret of residual amounts
of the first additive concentrate is relatively short.
Other advantages ensue from introducing the additive
concentrate system to the polymeric host material within the
spin pack assembly. For example, the spin pack assembly and
its associated spinneret orifices may be so designed to form
melt-spun multicomponent filaments (e. g., filaments having
multiple domains of different polymer blends, colorants and/or
other additives) such as those filaments disclosed in U.S.
Patent No. 5,162,074 to Hills by splitting a melt-flow of
polymeric host, material into two or more subflows within the
spin pack assembly. According to the present invention,
therefore, the additive concentrate system may be introduced
into the spin pack assembly and mixed with one or more of such
subflows of polymeric host material without being mixed with
other subflows so as to form multicomponent filaments.
Therefore, while the discussion which follows emphasizes the
production of filaments in which the additive concentrate
system is substantially homogeneously mixed through the
filament cross-section, it will be understood that the present
invention is likewise applicable to the formation of
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multicomponent filaments whereby the additive concentrate
system is substantially homogeneously mixed throughout one or
more multiple polymeric domains in the filament cross-section
without being present in the other domains) (e. g., as in core-
sheath filaments, pie wedge filaments, side-by-side filaments
and the like).
As noted above, significant processing flexibility
ensues according to the present invention. Processing
flexibility is the result of at least two features of the
present invention. First, additive concentrate systems can be
mixed above the spinneret with either the entire host polymer
or only a portion of the host polymer. For example, a
functional additive (e. g., an antistatic agent) concentrate
system might be mixed with only a third of the host polymer
such that a third of the filaments spun contain the antistatic
agent and the remaining two-thirds do not.
Second, two or more additive concentrate systems can
be mixed with the host polymer above the spinneret to achieve
a single attribute in the fiber that is spun. For example, a
yellow additive concentrate system and a blue additive
concentrate system can be concurrently mixed with host polymer
above the spinneret to provide a green fiber when the mixture
is spun. There is no theoretical limit for the number of
additive concentrate systems that can be mixed with the host
polymer above the spinneret. The number of additive
concentrate systems is limited only by the space available to
inject the systems into the line. It is contemplated that the
host polymer might also contain some additive prior to mixing
above the spinneret.
These two features of .the present invention are not
mutually exclusive and great flexibility ensues from combining
them. Using color as an example, either single color or
multicolor yarn can be spun using the present invention.
Single color yarn may be spun by mixing one or more color
additive concentrate systems (e. g., a yellow system and blue
system as exemplified above) with the entire host polymer such
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that a one color yarn (e. g., a multifilamentary yarn containing
only green filaments) results.
Multicolor yarn (e.g., heather yarn) may be spun by
selectively coloring separated portions of the host polymer and
keeping each separated portion segregated until spun. For
example, a portion of the host polymer might be colored with
both the yellow and the blue additive systems to produce green
filaments. Another portion of the host polymer might be
colored with a red additive system to produce red filaments
which are spun concurrently with the green filaments. The
resulting multifilamentary yarn will therefore exhibit a
heathered color due to the combination of individual red and
green filaments present in the yarn.
The concepts above apply also to the spinning of
filaments having multiple cross-sectional domains, such as
core-sheath filaments, pie wedge filaments, side-by-side
filaments and the like. Thus, for multidomain filaments, the
additive concentrate system may be mixed with one or more split
flows of the host polymer and then recombined with the
remainder of the host polymer flow to achieve filaments having
the additive present only in one or more of the cross-sectional
domains.
When the additive is a colorant, therefore, a
virtually unlimited number of multicolored, multidomain
filaments can be produced. For example, only the core of a
core-sheath filament may include one or more colorant additives
which imparts to the fiber a color attribute that is visibly
perceptible through the uncolored sheath. In this regard, it
has been found that colorant additives) contained only in the
core of a core-sheath multidomain filament results in a color
intensity that is achieved with reduced colorant loading levels
(e.g., between about 5 to about l0% less) as compared to
filaments having the same colorant additives) homogeneously
dispersed throughout the entire filament cross-section to
achieve comparable color intensity.
Alternatively or additionally, the colorant additive
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may be present in the sheath of a core-sheath filament so as to
achieve a color effect that is a combination of the core and
sheath colors. Thus, by selectively choosing and incorporating
colorants into the core and/or sheath, virtually any color
attribute can be achieved for the resulting filament. Some
particular combinations of colorants in both the core and
sheath of a core-sheath filament may not necessarily result in
a "pure" color combination of such colorants being realized for
the filament. That is, the additive/subtractive effects of
colorants in the core and sheath of core-sheath filaments are
relatively complex and sometimes cannot be predicted with
absolute certainty. However, routine experimentation with
colorants in the core and/or sheath of core-sheath filaments
will result in virtually an unlimited number of desired
filament color attributes being obtained.
Other multiple domain filament combinations are
envisioned, such as side-by-side domain filaments having
different color attributes in each of the sides or pie wedge
filaments whereby one or more of the wedges have the same or
different color attributes. Such multiple domain filaments may
be usefully employed to form heather yarns since the color
additive-containing domains will visually present themselves at
different locations along the length of the filaments when
twisted (e. g., as may occur during yarn processing).
Furthermore, the colorants and domains in which such colorants
are present can be selected to achieve filaments which
macroscopically appear to be uniformly colored.
Furthermore, although the additive concentrate
systems of this invention may be metered (dosed) into the host
polymer (whether in its entirety or in one or more of its split
flows) at a substantially constant rate, periodic or continual
variance of the dose rate is also envisioned. Thus, as noted
briefly above, when changing from one filament recipe to
another, one or more of the additive concentrates will need to
be varied in order to switch filament production from a former
recipe to the then current recipe. A random or constant dosage
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rate variance can also be practiced, however, in which case the
resulting filaments will have more or less of the additive
distributed along its length. When the additive is a colorant,
such a technique allows filaments to be formed having a
slub-like color appearance along its axial length which may be
employed, for example, to produce yarns having a striated or
marbled impression.
These and other aspects and advantages of this
invention will become more clear after careful consideration is
given to the following detailed description of the preferred
exemplary embodiments thereof.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
Reference will hereinafter be made to the
accompanying drawing wherein FIGURE 1 is a schematic view of a
filament melt-spinning apparatus in which the additive system
of this invention may be added to a melt flow of polymeric
material prior to spinning.
DETAILED DESCRIPTION OF THE PREFERRED
EXEMPLARY EMBODIMENTS
To promote an understanding of the principles of the
present invention, descriptions of specific embodiments of the
invention follow and specific language describes the same. It
will nevertheless be understood that no limitation of the scope
of the invention is thereby intended, and that such alterations
and further modifications, and such further applications of the
principles of the invention as discussed are contemplated as
would normally occur to one ordinarily skilled in the art to
which the invention pertains.
Thus, for example, while reference has been, and will
hereinafter be, made to melt-spinning of filaments, it will be
understood that other operations which serve to shape a melt of
a polymeric material to a final form (e.g., extrusion or
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. injection molding, blow-molding or the like) are contemplated.
Furthermore, for ease of reference, the discussion which
follows will emphasize the presently preferred embodiment of
the invention in terms of incorporating colorants into
polymeric materials, but the present invention can likewise be
employed to incorporate virtually any other conventional
additive as may be desired. In this regard, the term "pigment"
as used herein and in the accompanying claims is meant to refer
10 to virtually any material that may be added physically to a
polymer melt flow, and thus generically encompasses colorant
pigments which will be emphasized in the discussion which
follows. Thus, suitable pigments which may be employed in the
practice of this invention include solid and liquid colorants,
stabilizers, delusterants, flame retardants, fillers,
antimicrobial agents, antistatic agents, optical brighteners,
extenders, processing aids and other functional additives.
As used herein and in the accompanying claims, the
term "color" includes Munsell Values between about 2.5/ to
about 8.5/ and Munsell Chromas greater than about /0.5. (Kelly
et al, The ISCC-NBS Method of Designating Colors and a
Dictionary of Color Names, National Bureau of Standards
Circular 553, pp. 1-5 and 16 (1955)).
The host polymer in which the additive concentrate
system of this invention may be incorporated includes any
synthetic thermoplastic polymer which is melt-spinnable.
Exemplary polymers are polyamides such as poly(hexamethylene
adipamide), polycaprolactam and polyamides of bis(4-amino-
cyclohexyl) methane and linear aliphatic dicarboxylic acids
containing 9, 10 and 12 carbon atoms; copolyamides; polyester
such as poly(ethylene)terephthalic acid and copolymers thereof;
polyolefins such as polyethylene and polypropylene; and
polyurethanes. Both heterogeneous and homogeneous mixtures of
such polymers may also be used.
I. Additive Concentrate Preparation
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As noted above, the additive concentrate system
employed in the practice of the present invention is a
dispersion or solution of pigment in a nonaqueous liquid or
liquefied polymeric carrier. The pigment may be a solid
particulate (e.g., a colorant) which is coated with a
dispersant for physical dispersion in the carrier material.
Alternatively, the pigment may be in a form which is soluble
with the carrier, in which case the dispersant is not
necessarily employed. Thus, the pigment may homogeneously be
suspended and/or solubilized in the carrier.
Although a variety of pigments may be employed in the
practice of the present invention, it is presently preferred
that the pigment is a particulate colorant pigment having a
mean particle size of less than 10 um, preferably less than
about 5 um, and most preferably between 0.1 ~m to about 2 Vim.
If present, the preferred dispersants which may be
employed in the practice of this invention are the water
soluble/dispersible polymers as described in U.S. Patent No.
3,846,507. One particularly useful dispersant in this class is
a copolymer of caprolactam/ hexamethylene-diamine/isophthalic
acid/sodium salt of sulfo-isophthalic acid having a molecular
weight of about 7,000, a specific gravity (H20=1) of about 1.1,
a solubility in water of about 25o at 20°C. This preferred
water soluble/dispersible polyamide copolymer dispersant is
manufactured by BASF Corporation and will hereinafter be
referenced as "C-68".
Other useful dispersants that may be employed in the
practice of this invention are water soluble/dispersible
polyesters. One particularly preferred polyester which is
completely dispersible in water is commercially available from
Eastman Chemical Products, Inc., Kingsport, Tennessee, under
the product name "LB-100". This preferred water soluble/
dispersible polyester has a specific gravity (H20=1) of about
1.08, and is available commercially as a 30o solution of the
polyester in water.
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Other water soluble/dispersible polymers that may be
useful in the practice of the present invention include, but
are not limited to other water soluble/dispersible polyamides
and copolymers thereof, water soluble/dispersible polyesters
and copolymers thereof, water soluble/dispersible vinyl
polymers and copolymers thereof, water soluble/ dispersible
alkylene oxide polymers and copolymers thereof and water
soluble/dispersible polyolefins and copolymers thereof, as well
as mixtures of the same. other dispersants, like monomeric
dispersants, may be suitable for use with the present
invention.
One presently preferred technique for producing the
additive dispersion of this invention uses as a starting
material the aqueous dispersion formed according to the above
referenced Jones '645 patent. The aqueous dispersion may then
be bead-milled and subjected to a spray drying operation so as
to remove the aqueous component. The resulting dispersant
coated pigment granules (hereinafter more simply referred to as
the "dispersible pigment granules") in powder form are then
mixed with a nonaqueous liquid polymeric carrier material.
The carrier material can be virtually any material
that is liquid at or below melt-spinning temperatures of the
polymeric host material. Preferably, the carrier material is
a polyamide or a polyester. The carrier material must also be
compatible with the thermoplastic polymeric host material. For
example, when; providing an additive concentrate system for
incorporation into a nylon-6 polymeric host material, the
presently preferred carrier is polycaprolactone since it is
liquid at room temperatures (20°C). However, carriers that may
be liquefied at elevated temperatures (e. g., less than about
200°C) are also useable in the practice of this invention. For
example, when providing an additive concentrate system for
incorporation into a nylon-6 polymeric host material, it is
also possible to use copolyamides having a melting point of
less than about 200°C. One particularly preferred class of such
copolyamides is commercially available under the trade name
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Vestamelt* copolyamides from Huls America Inc. of Piscataway,
New Jersey, with Vestamelt 722*being particularly preferred.
One alterative technique to make the additive
concentrate system according to this invention involves mixing
the pigment, carrier and, if present, dispersant to form a
nonaqueous paste in a one-step process thereby eliminating the
need to prepare an aqueous dispersion which is subsequently
spray dried. It is preferred that the dispersant, if present,
and the carrier be premixed prior to addition of the pigment.
The mixture may then be milled so as to obtain a paste which
can be introduced directly into a melt flow of the polymeric
host material.
The additive concentrate system of this invention may
also be prepared by combining the pigment and the dispersant in
a high-intensity mixer (e. g., a Henschel FM series mixer
available commercially from Henschel Mixers America, Inc. of
Houston, Texas) until they are intimately mixed. Thereafter,
the shear imparted by the mixer is reduced, and the required
mass of carrier is added to yield the additive concentrate of
this invention in paste form.
The dispersants that may be employed in the one-step
technique, in addition to those described above, include
polyethylene glycol p-octyl phenyl ether (Triton X-100),
polyoxypropylene/ethylene block copolymers (Pluronic 25R2),
alkoxylated diamines (Tetronic 150R1), sodium lauryl sulfate
and cationic dispersants (VariQuat). The dispersant (i.e., the
non-carrier material), if present, is present in the additive
concentrate system in an amount between about 5 to about 100
wt.% based on the weight of the pigment, and more preferably,
between about 40 to about 100 wt. o.
However formed, the additive concentrate system is
most preferably in the form of a flowable paste having a
viscosity during introduction into the polymeric host material
ranging between about 500 cP to about 500,000 cP, and most
preferably between about 1,500 cP to about 100,000 cP, at a
temperature between about 20°C to about 200°C. The dispersible
* (trademarks)
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additive may be maintained to within an acceptable viscosity
range by application of heat (e. g., by keeping the dispersible
additive in a suitable storage vessel which is jacketed with
electrical resistance heaters and/or a heat transfer medium).
The additive concentrate system preferably contains
pigment in an amount between about 5 to about 75 wt.%, more
preferably between about 10 to about 65 wt.o based on the
weight of the additive concentrate system. The additive
concentrate system (the dispersible additive) itself is
incorporated into the polymeric host material at levels between
about 0.01 to about 15 wt. o, more preferably between about
0.05 and 10.0 wt.o based on the total weight of the polymeric
host material and additive concentrate system.
II. FILAMENT PRODUCTION
Accompanying FIGURE 1 schematically depicts a
filament spinning operation 10 by which additive concentrate
systems may selectively be mixed with a melt flow of polymeric
host material discharged from a conventional screw extruder 12
and supplied to an inlet of the spin pack assembly 14. More
specifically, the polymeric host material is introduced into
the upstream polymer filter section 14a of the spin pack
assembly before being extruded through orifices in the
spinneret 14b to form additive-containing filaments 16. Prior
to reaching the spinneret 14b, the polymeric host material may
be distributed by a plurality of thin distribution plates 14c
in accordance with the above-noted U.S. Patent No. 5,162,074 to
William H. Hills, which may or may not have one or more static
mixing plates, for example, as disclosed in U.S. Patent No.
5,137,369 to John A. Hodan.
Batches of the additive concentrate systems in paste
form are respectively held within portable tanks 18a-18d. In
the accompanying FIGURE 1, tanks 18a-18d are shown supported on
wheeled carts 20a-20d, respectively, so as to permit each of
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IS
the tanks 18a-18d to be replaced easily with stand-by tanks
containing a fresh supply of the same or different additive
concentrate system. However, other means can be employed which
allow the tanks 18a-18d to be portable, such as in-ground or
overhead conveyance systems, cranes and the like. Preferably,
the additive concentrate system contained in each of the tanks
18a-18d is different -- that is, tanks 18a-18d may each contain
a different pigment or pigment mixture so that selective
incorporation of each will result in the desired properties
being achieved for the filaments 16.
Specifically, the tanks 18a-18c may each respec-
tively contain dispersible colorant pigments corresponding to
selected colors such as aqua, magenta and yellow, while tank
18d may have a specially formulated tint color (e. g., white,
black or the like) to achieve the desired color hue, chroma
and/or intensity. The differently colored additive concen-
trates held within the tanks 18a-18d may thus be volumetri-
cally dosed or mixed with the polymeric host material so as to
achieve a virtually unlimited number of resulting colors of the
melt-spun filaments 16. In a like manner, other filament
properties may be "engineered" by selective incorporation of
other non-colorant pigments.
The carts 20a-20d also support a primary pump 22a-22d
and a metering pump 24a-24d, respectively. The pumps 22a-22d
and 24a-24d are most preferably gear-type pumps which serve to
force the additive concentrate system paste through respective
supply lines 26a-26d to the spin pack assembly 14. More
specifically, the primary pumps 22a-22d serve to maintain a
relatively constant input pressure to the immediately
downstream respective metering pump 24a-24d. The primary pumps
22a-22d are therefore relatively larger capacity as compared to
their respective downstream metering pump 24a-24d.
The additive concentrate system paste within each of
the tanks 18a-18d is maintained under constant agitation in
order to prevent sedimentation of the pigment therein. Such
agitation may be accomplished by a motor-driven mixer 26a-26d
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1G
and/or via recycle lines 28a-28d (and/or lines 3oa-3od). of
course, if the pigment is in solution with the carrier, then
such agitation may not be needed.
The metering pumps 24a-24d are variable speed so as
to achieve variable volumetric outputs within their respective
capacity range stated previously. The speed of the metering
pumps 24a-24d is most preferably controlled by a logic
programmable controller LPC. Specifically, for a given "recipe"
(for example, a desired color for the pigmented filaments 16)
input into the controller LPC, appropriate outputs will be
issued to one or more of the metering pumps 24a-24d to cause
them to operate at a speed to achieve a desired volumetric
output for their particular dispersible additive. Thus, it
will be recognized that for certain desired colors, some but
not all of the metering pumps 24a-24d will be supplying paste
from their respective tanks 18a-18d to the spin pack assembly
14 and/or may be operated at different speeds to achieve
different volumetric outputs. Suffice it to say, that by
selectively controlling the operation of the metering pumps
24a-24d and, when operated, their respective speed (and hence
their respective volumetric outputs), selective volumetric
paste doses can be continuously supplied to the spin pack
assembly 14 where the respective additive concentrate systems
will be homogeneously mixed with the melt flow of polymeric
host material being fed by the extruder 12 via line 32.
The ,respective speed of one or more of the metering
pumps 24a-24d may also be varied continually to thereby
respectively vary the volumetric dose of one or more of the
colorant systems over time. Such speed (dose) variance will
thereby cause more or less additive concentrate system being
incorporated into the filament per unit time where results in
a filament having varying amounts of the additive per unit
length. In the context of color additives, such speed variance
may be employed so as to form filaments having a randomly
striated or marbled color appearance.
The additive concentrate pastes from lines 26a-26d
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17
are most preferably introduced directly into the spin pack
assembly 14 at a location corresponding to the distribution/
mixing section 14c -- that is, at a location downstream of the
polymer filter 14a, but upstream of the spinneret 14b. In this
manner, a relatively quick additive change between successive
batches of filaments 16 is possible (i.e., to allow for changes
in additive recipe to be realized from one filament batch to
another). In addition, such an inlet location for the additive
concentrates also allows for a wide range of processing
flexibility to be achieved. For example, the additive pastes
from tanks 18a, 18b, 18c and/or 18d may be mixed with the
entirety of polymeric host material supplied via line 32 so
that all of the filaments 16 have the same color.
Alternatively, the distribution/mixing section 14c of the spin
pack assembly 14 may be so provided to split the flow of
polymeric host material with one or more of the additive
concentrate pastes being mixed with one or more of such split
flows to achieve, for example, multiple differently colored
filament groups which may remain segregated to form single
color yarns or may be combined to form multicolor yarns, such
as in a heather yarn. In addition, several additives may be
mixed with the host polymer so that, for example, single color
yarns having multiple additive concentrations therein may be
produced from the same spinning equipment. Similarly, one or
more additive concentrate pastes may be mixed with split flows
of polymeric ,host material within the distribution/mixing
section 14c of the spin pack assembly 14 to achieve
multifilamentary yarns having differently colored filaments
(e. g., as may be desired to produce yarns having a heathered
appearance).
Although accompanying FIGURE 1 (and the description
above) shows the additive concentrate system pastes being
preferably introduced into the melt flow of polymeric host
material directly into the spin pack assembly 14 at a location
between the polymer filter section 14a and the spinneret 14b,
it will be understood that the pastes may be incorporated into
CA 02208225 1997-06-03
18
the melt flow of polymeric host material at any location
upstream of the spinneret 14b. Thus, for example, the additive
system pastes may be incorporated into the melt flow of
polymeric host material by feeding through an injection port
associated with the extruder 12 and/or through a port in line
32. Thus, for example, the additive system pastes may be
introduced to the polymeric host material at or downstream of
the extruder throat, but upstream of the spinneret 14b.
Different batches of colored filaments 16 may thus be
produced continuously by simply changing the recipe in the
controller LPC and allowing a sufficient time interval to
elapse to ensure that any residual amounts of the additive
concentrate system pastes associated with the prior recipe have
been purged from the spin pack assembly 14. While some off
specification filament will ensue during the change-over to the
new recipe, its economic impact is small by comparison to
complete shut-down of the spinning operation. Furthermore,
since relatively small amounts of the additive concentrate
system pastes will residually be present in the spin pack
assembly 14 at the time of recipe change-over, only a
relatively short time interval is needed to purge the spin pack
assembly of the prior additive recipe and begin producing
filaments pigmented with the new recipe.
III. Examples
The following nonlimiting examples will provide a
further understanding of this invention.
In this regard, carpet samples formed of filaments
colored in accordance with the present invention and filaments
colored in accordance with conventional extruder melt-blending
techniques were tested according to the following procedures
and, where applicable, a subjective rating scale of between 1
to 5 was utilized (5 being the best rating):
Yarn Degradation: Data representative of yarn strength/
CA 02208225 1997-06-03
19
elongation before and after 100, 200 and 30o hours ultraviolet
radiation exposure according to AATCC Test Method 16-1993,
Option E.
~olorfastness: Yarn color/visual data after 100, 20o and
30o hours ultraviolet radiation exposure according to A.ATCC
Test Method 16-1993, Option E.
Taber Abrasion Test: ASTM D3884-92.
Crocking: AATCC Test Method 8-1989.
Exposure to 50% Bleach: Carpet samples were cut into two
4.5" x 9" squares. 25 ml of a bleach solution containing about
2.6~ sodium hypochlorite (50~ Clorox~ brand bleach and water)
was poured into the center of one sample to form a test region
approximately 2" in diameter. The sample was allowed to air dry
for 24 hours after which it was rinsed with a hot
detergent/water solution containing 12 parts water and 1 part
detergent. The rinsed sample was air dried for 24 hours after
which it was visually rated on a scale of 1 to 5 against the
untreated sample using AATCC Gray Scale in a Macbeth light
booth (daylight setting).
~Iisual Grades After Exposure to Ozone: AATCC Test Method
129-1990.
Visual Grades After Exposure to N02: AATCC Test Method
164-1992.
'
ply Heat Exposure: Samples are heated in a laboratory
oven (1600 Watts, Model No. 0V-490, Blue M. Electric Co., Blue
Island, Illinois) at 280°F and 320°F and removed after ten
minutes. The samples are allowed to cool and visually rated on
a scale of 1 to 5 using AATCC Gray Scale.
i i
CA 02208225 2002-05-15
Tetra~od Wear: ASTM D5251-92.
Examglt~ 1
Dispersant-coated pigment particles were prepared
using the components noted in Table A below. The components
were blended using a high shear dissolver type mixer. A water
soluble polyamide dispersant polymer (C-68 manufactured by BASF
Corporation in accordance with U.S. Patent No. 3,846,507 except
10 that poly(E-caprolactam) was used as a starting material
instead of e-caprolactam) was first dissolved in water to
prepare a 25 percent stock solution. Pigment dispersions were
then bead-milled with 2 mm glass beads for three passes through
the mill and were thereafter spray-dried. The dispersions were
spray-dried using a Niro FSD-Pilot* unit, which had a 1.5 meter
diameter, 0.8 meters cylinder height, 40° cone, and a fluidized
bed collector at the bottom of the chamber. Dispersions were
fed into the dryer with a two-fluid, externally-mixed nozzle.
The spray-dryer was run with 253-263°C inlet and 67-103°C
outlet
20 temperatures. The spray-dried powder tended to be dusty, and
thus a fluidized bed collector was used to increase agglomerate
size and thereby reduce the dust.
* (trademark)
CA 02208225 1997-06-03
21
% Pigment in % Dispersant
Aqueous in Aqueous
Pigment Dispersion Dispersion
Inorganic 32.5 13.0
Yellow
Organic Blue 20.0 15.0
Organic Red 20.0 15.0
Inorganic Tan 30.o 12.0
Organic Green 25.0 12.5
Organic Black 20.0 15.0
White/Stabili 32.5 13.0
zer
Example 1 was repeated except that a water-
dispersible polyester (LB-100 from Eastman Chemical Products,
Inc.) was used as the dispersant polymer in the amounts noted
in Table B below. Unlike Example 1 above, all dispersions
according to this Example 2 contained 5.0% of a polyoxy-
propylene-polydxyethylene block copolymer surfactant (Pluronic~
2582 surfactant from BASF Corporation). Spray-dried
dispersions using LB-100 as the dispersant were not dusty, and
were prepared using the Niro spray-dryer which was not
equipped with a fluidized bed collector. The Niro spray dryer
was run with 220°C inlet and 80-95°C outlet temperatures. These
dispersions were fed into a rotary wheel type atomizer running
at 18,500 rpm.
CA 02208225 1997-06-03
22
% Pigment in % Dispersal
~aueous in Aqueous
Pigment Dispersion Dispersion
Organic Blue 27.5 20.6
Organic Red 27.5 20.6
Inorganic Tan 32.5 13.0
Organic Green 32.5 24.7
Organic Black 25.0 18.7
White 40.0 16.0
White/Stabili 40.0 16.0
zer
Example 3
The additive concentrate pastes in Table C below were
prepared by first melting at 150°C 50-60~ of the required
copolyamide carrier polymer (Vestamelt 722 from Huls America
Inc.). The spray-dried powders obtained according to Example
1 above were then bag-blended in desired ratios to achieve
desired final colors and stirred into the molten carrier
polymer. The balance of the carrier polymer needed was then
added and stirred into the concentrate blend formulation. The
spray-dried powders tended to form large agglomerates which did
not disperse without extended agitation. Thus, the blends were
stirred overnight (approximately 10 to 12 hours) prior to yarn
extrusion.
The white/stabilizer pigments used in the blended
pigment ratios for all final colors, except Gray and Light
Gray, were not the spray dried coated pigments obtained
according to Example 1. Instead, the white/stabilizer pigments
were compounded with Vestamelt 722 polymer using a vented twin
screw compounding extruder to obtain chip concentrates having
CA 02208225 1997-06-03
23
25 wt.~ of white pigment and 25 wt.~ stabilizer. The chip
concentrates of such white/stabilizer pigments were then
blended in desired ratios with certain of the spray-dried
pigments obtained in Example 1 to achieve the final colors
noted below in Table C.
TABLE C
Total % Pigment
final Color in Paste
Light Gray 13.9
Gray 9.3
Black 20.4
Light Green 20.0
Purple 25.3
Blue 19.0
Light Tan 19.8
Mauve 18.7
Green 19.0
Brown 19.7
EXAMPLE 4
The additive concentrate pastes in Table D below were
prepared following the procedures of Example 3 above, except
that the spray-dried powders obtained from Example 2 were used,
and the carrier was polycaprol~ctone. Unlike Example 3, no
compounded chips of white/stabilizer pigments were used.
i i
CA 02208225 2002-05-15
24
Total $ Pigx~ent
Final Color in Paste
Light Gray 37.0
Gray 37.8
Black 34.0
Light Green 39.0
Purple 35.5
Blue 34.8
Light Tan 35.0
Mauve 30.5
Green 34.9
Brown 37.7
Example 5
A Barmag 6E* extruder was used for filament yarn
extrusion with the additive concentrate pastes in Table C being
fed downstream of the extruder at around 150°C in desired
ratios to achieve the filament color noted below in Table E.
The resulting melt-spun filament yarns were 6-hole pentagonal
cross-section, 715 +/- 15 denier, and 14 filaments/ end. Eight
ends of these undrawn yarns were combined during draw texturing
to prepare 2250/112 denier yarns which were then two-ply cable-
twisted to make 4500/224 denier carpet yarns. The carpet yarns
were then tufted into 1/10 gauge, 26 ounces/square yard, 3/16"
pile height level loop carpets.
The carpets were then tested to determine various
physical properties using the testing methods and techniques
described previously. The results of such testing are tabulated
below in Tables 1-4 and are presented in comparison to carpets
formed of "control" filaments of matching color. The "control"
* (trademark]
CA 02208225 1997-06-03
filaments were made using conventional compounded pigment chips
which were melt-blended with the polymeric host chip in an
extruder, with the melt-blend then being fed to the spinneret.
Table E
A dditive % Additive
t t
t
Conce ntrate as Concen
P e ra
e
Final Compo nents ther haste in
O
10 ~o~ Than Stab s Filament
Light black, white, 1.4
Gray green, blue
Gray black, white, 2.6
blue, red
Black black, white 3.8
Light black, white, 1.4
Green green, tan
Purple black, white, 2.6
blue, red
Blue black, white, 2.8
blue, red
Light black, green, tan 1.7
20 Tan
Mauve black, blue, red 2.8
Green black, green, blue 4.2
Brown black, white, red, 6.5
tan
CA 02208225 1997-06-03
26
0
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a
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CA 02208225 1997-06-03
27
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CA 02208225 1997-06-03
28
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CA 02208225 1997-06-03
29
U
0
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m m m m m m m m
o w a~ ~ ~ a~-~a~a~ m a~ a~ ~ ~
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a
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CA 02208225 1997-06-03
EXAMPLE 6
Example 5 was repeated except that the additive
concentrate pastes of Table D were fed at the extruder throat
at ambient temperature (about 20°C). The paste components and
the amount of paste in the filaments are noted below in Table
F. The resulting filaments were formed into carpets and tested
similar to Example 5. The results appear in Tables 5-8 below.
10 Table F
A dditive % Additive
t t t
t
Soncen e P as ra
tra e e
concen
Final Compo nents ther Paste in
O
Color Than Stabilizer Filament
Light black, white, 0.6
Gray green, blue
Gray black, white, 0.7
blue, red
Black black, white 2.2
20 Light black, white, 0.8
Green green, tan
Purple black, white, 2.0
blue, red
Blue black, white, 1.6
blue, red
Light black, green, tan 1.0
Tan
Mauve black, blue, red 1.9
Green black, green, blue 2.2
Brown black, white, red, 3.6
tan
CA 02208225 1997-06-03
31
0
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o . . , . . . . , .
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° ~ cf c~ c~ ~ c~i ~n ,--~ c~i co ~ o ~ c~i ~ ~
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CA 02208225 1997-06-03
32
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CA 02208225 1997-06-03
33
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CA 02208225 1997-06-03
34
Table 8. Carpet visual ratings after exposure to dry heat and Tetrapod wear.
Test Samples made wit~i LB-100
Dr~Heat Exposure500 K
" in Tetra
od
2,80 B 3?U S Lair End
B
TAN CTRL B 4-5 4 3 3
TAN PCL 4-5 4 3 3
LT GRAY CTRL B 4-5 3 3 3
LT GRAY PCL 4-5 3 3 3
LT GREEN CTRL 4-5 3-4 3 3
B
LT GREEN PCL 4-5 4 3 3
GRAY CTRL B 4-5 4 3 3
GRAY PCL 4-5 4 3 3
BLACK CTRL B 5 5 3-4 4
BLACK PCL 5 5 3-4 3-4
GREEN CTRL B 5 4-5 Z-3 3-4
GREEN PCL 5 4-5 3-4 3-4
BLUE CTRL B 5 4-5 3-4 3-4
BLUE PCL 4-5 4 3-4 3-4
PURPLE CTRL B 4-5 4 3-4 3-4
PURPLE PCL 4-5 4 3-4 3-4
CA 02208225 1997-06-03
The data in Tables 1-8 above demonstrate that the
performance properties of carpet yarns made from pigmented
filaments of this invention are comparable to carpet yarns
which are colored according to the conventional practice of
melt-blending pigmented chips with base polymer chips. It is
surprising that the incorporation of the low molecular-weight
polymer as the carrier in the dispersible additive did not
affect either the breaking strength or elongation of the
pigmented filaments of this invention when compared to
10 conventional melt-colored filaments.
EXAMPLE 7
A tan additive concentrate paste was formed by direct
blending of 40 wt.o tan pigment particles, 8 wt.% of
polyethylene glycol p-octyl phenyl ether (Triton X-loo)
dispersant, and 52 wt.~ polycaprolactone. The resulting
additive concentrate paste was preheated to approximately 140°C
and exhibited a viscosity of between 2000 to 4000 cP. The
20 paste was pumped directly into a spin pack assembly at a
location downstream of the polymer filter but upstream of the
spinneret orifices (58 hole asymmetrical trilobal). The
additive concentrate paste was mixed with the nylon-6 polymeric
host material within the spin pack assembly at a rate of
between about 6.0 g/min (to obtain about 0.8-1.1 wt.% pigment
in the result~.ng melt-spun filaments) to about 7.3 g/min (to
obtain about 1.1-1.5 wt.o pigment in the resulting melt-spun
filaments). The resulting melt-spun filaments had a uniformly
colored appearance along the lengthwise extent as viewed with
30 an unaided eye. Microscopic views of filament cross-sections
revealed that substantially homogenous to somewhat striated
mixing had occurred in dependence upon the injection rate of
the additive paste.
