Note: Descriptions are shown in the official language in which they were submitted.
CA 02208213 1997-06-03
1
DISPERSIBLE ADDITIVE SYSTEMS FOR POLYMERIC MATERIALS
CROSS-REFERENCE
This application is a division of application n°
2,191,990 filed on December 3, 1996.
FIELD OF INVENTION
to 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
therefrom. However, the invention as claimed is restricted to
disposable additive systems for polymeric materials.
20 BACKGROUND AND SUMMARY OF THE INVENTION
The 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
30 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.
The incorporation of colorant additives in filaments
formed by melt-spinning a polymeric material has presented
CA 02208213 2002-05-17
2
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 '545 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
30 filter section of the spin pack assembly) thereby bypassing
the extruder. Such a possibility would then allow additive
CA 02208213 2003-08-O1
3
concentration and/or 'types to be changed on a continuous basis
to produce :cequentia:L lengths of melt-spun filaments having
desired, but: different, properties and/or characteristics.
That is, the upstream :processing equipment, for example, the
extruders anct process piping, which supply the polymeric host
material to t:he 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 allowixig, for example, quick color changes to
occur from one filament production batch to another. It is
towards prov.idinc~ such. improvements that the present invention
is directed.
ThE: present invention is concerned with a nonaqueous
additive concentrate system for thermoplastic polymeric host
materials which may be added directly to a melt flow of the
polymeric material in metered amounts.
More particularly, tr:e invention as claimed is
concerned with a dispersible system for polymeric material
comprising dispersan~-coated pigments in a liquid non
aqueous polymeric carrier, wherein the dispersant is
selected from the grc_>up consisting of polyethylene glycol
2~~ p-octyl phenyl etrue:r, polyoxypropylene/polyoxyethylene
block copolymers, alkoxylated diamines, sodium lauryl
sulfate, cationic, dispersants and mixtures thereof.
This addit:ivEe system is most preferably in the
form of a particulate paste which can be added in metered
amounts (dc:~ed) to a melt flow o:f the po-lymeric host
material prior to being spun ir-:tc filaments. By providing a
number of additive ~>y~tems having a number of different
additive attributes, and controllably dosing one or more
into the melt flour of polymeric material, melt-spun
30 filaments having d.lf:ferent additive attributes may be
produced on a contim:cous bass ( ~_ . a . , ~a.ithout shutting down
CA 02208213 2002-05-17
3a
the spinning operation). The present invention is
particularly advantageous to produce on a continuous basis
sequential lengths of filaments having different color
attributes.
The additive concentrate system according to the
present invention includes a filaments 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,
CA 02208213 1997-06-03
4
the additive system of this invention most preferably also
includes a dispersant which 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 shArt period of time without stopping filament
winding.
Thus, another aspect of this invention 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
CA 02208213 1997-06-03
a different additive is controllably dosed into the polymeric
material without 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. 5,1'62,074 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
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6
invention is likewise applicable to the formation of
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
CA 02208213 1997-06-03
7
system as exemplified above) with the entire host polymer such
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
to 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
2o 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
30 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 10~ less) as
compared to filaments having the same colorant additives)
homogeneously dispersed throughout the entire filament
cross-section to achieve comparable color intensity.
CA 02208213 1997-06-03
8
Alternatively or additionally, the colorant additive
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
CA 02208213 1997-06-03
9
to be varied in order to switch filament production from a
former recipe to the then current recipe. A random or
constant dosage 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
CA 02208213 2002-05-17
will be understood that other operations which serve to shape
a melt of a polymeric material to a final form (e. g.,
extrusion or 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 to virtually any
10 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
30 thereof; polyolefins such as polyethylene and polypropylene;
and polyurethanes. Both heterogeneous and homogeneous mixtures
CA 02208213 2002-05-17
11
of such polymers may also be used.
I. A~Slditive Concentrate Preparation
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 ~.m, and most preferably between 0.1 um to
about 2 um.
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 sulfoisophthalic 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
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11a
soluble/dispersible polyesters. One particularly preferred
polyester which is completely dispersible in water is
commercially available from
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12
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.
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 thermopladtic 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 ( a . g . , less than
about 200°C) are also useable in the practice of this
CA 02208213 2002-05-17
13
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 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 loo wt.%.
* (trademarks)
CA 02208213 1997-06-03
14
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
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.~, more preferably between
about 0.05 and 10.0 wt.~ 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
CA 02208213 2004-06-21
No. 5,137,369 to John A. Hodan.
Batches of the additive concentrate systems in paste
form are respectively held within portable tanks 18a-isd. In
the accompanying FIGURE 1, tanks 18a-18d are shown supported
on wheeled carts 20a-20d, respectively, so as to permit each
of 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.
10 preferably, the additive concentrate system contained in each
of the tanks l8a-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-
Crates 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 2oa-2od 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
CA 02208213 1997-06-03
16
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 and/or via recycle lines 28a-28d (and/or lines 30a-
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
CA 02208213 1997-06-03
17
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
are most preferably introduced directly into the spin pack
assembly 14 at a location corresponding to the distribution/
l0 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
20 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
30 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
CA 02208213 1997-06-03
18
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
the melt flow of polymeric host material at any location
upstream of the spinneret 14b. Thus, for example, the additive
l0 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
20 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
30 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
CA 02208213 1997-06-03
19
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/
elongation before and after 100, 200 and 300 hours ultraviolet
radiation exposure according to AATCC Test Method 16-1993,
l0 option E.
Colorfastness: Yarn color/visual data after 100, 200 and
300 hours ultraviolet radiation exposure according to AATCC
Test Method 16-1993, Option E.
Taber Abrasion Test: ASTM D3884-92.
Crocking: AATCC Test Method 8-1989.
20 ~posure 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~ Cloroxn 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 riilsed with a hot
detergent/wate~ 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
30 booth (daylight setting).
y,isual Grades After F~mosure to Ozone: AATCC Test Method
129-1990.
Visual Grades After Exposure to N02: AATCC Test Method
164-1992.
CA 02208213 2002-05-17
Qry Heat ~~X_posure: 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.
Tetra.~oc~ Wear: ASTM D5251-92.
~xamDle 1
to
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 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
20 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 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 02208213 1997-06-03
21
TABLE A
% 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 30.0 12.0
Organic Green 25.0 12.5
Organic Black 20.0 15.0
White/Stabili 32.5 13.0
zer
Example 2
2o Example 1 was repeated except that a water-
dispersible polyester (LB-1o0 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-polyoxyethylene 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
30 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 02208213 1997-06-03
22
TABLE B
% Pigment in % Dispersant
AS~ueous 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 l0 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 02208213 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 % Pia~ment
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
20 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 polycaprolactone. Unlike
Example 3, no compounded chips of white/stabilizer pigments
30 were used.
CA 02208213 2002-05-17
24
Total % Pigment
Final Color in Paste
Light Gray 37.0
Gray 37.8
lack ~' ~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
* (trademark)
CA 02208213 1997-06-03
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" 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
Concen trate aste Concentrate
P
Final Compo nents ther Paste in
O
C Th Stabilizer filament
olor an white, 1.4
Light black,
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
Tan
Mauve black, blue, red 2.8
Green black, green, blue 4.2
Brown black, white, red, 6.5
tan
CA 02208213 1997-06-03
26
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CA 02208213 1997-06-03
27
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CA 02208213 1997-06-03
28
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CA 02208213 1997-06-03
29
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CA 02208213 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
Additive ~ Additive
Concentrate Paste Concentrate
Final Components Paste in
Other
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
I
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 02208213 1997-06-03
31
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CA 02208213 1997-06-03
32
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CA 02208213 1997-06-03
33
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CA 02208213 1997-06-03
34
Table 8. Carpet visual ratings after exposure to cry lueat anc~ Tetrapod wear.
Test Samples mace wit~1 LB-100
D Heat Ex osure500_x_
in Tetra
od
Z80 F 320 S fair EIlCI
F
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 2-3 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 02208213 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
l0 conventional melt-colored filaments.
EXAMPLE 7
A tan additive concentrate paste was formed by
direct blending of 40 wt.~ tan pigment particles, 8 wt.~ of
polyethylene glycol p-octyl phenyl ether (Triton X-1o0)
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.
20 The 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 thg resulting melt-spun filaments) to about 7.3
g/min (to obtain about 1.1-1.5 wt.~ pigment in the resulting
melt-spun filaments). The resulting melt-spun filaments had
a uniformly colored appearance along the lengthwise extent as
30 viewed with 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.
