US 2016.

0017144A1
(19) United States
(12) Patent Application Publication (10) Pub. No.: US 2016/0017144 A1
Harris et al. (43) Pub. Date: Jan. 21, 2016
(54) PROCESS AND COMPOSITION FOR WELL COSL 69/00 (2006.01)
DISPERSED, HIGHLY LOADED COLOR COSL 25/06 (2006.01)
MASTERBATCH COSL 2.3/4 (2006.01)
COSL 55/02 (2006.01)
(71) Applicant: Carolina Color Corporation, Salisbury, (52) U.S. Cl.
NC (US) CPC ................. C08L 77/00 (2013.01); C08L 23/14
(2013.01); C08L 61/02 (2013.01); C08L 67/02
(72) Inventors: Ronald M. Harris, Cumming, GA (US); (2013.01): COSL 33/12 (2013.01); COSL 8L/06
Jeffrey S. Smink, Rockwell, NC (US) (2013.01); C08L 55/02 (2013.01); C08L 23/12
(2013.01); C08L 23/08 (2013.01); C08L 23/06
(21) Appl. No.: 14/334,710 (2013.01); C08L 71/00 (2013.01); C08L 69/00
1-1. (2013.01); C08L 25/06 (2013.01); C08L 25/08
(22) Filed: Jul.18, 2014 (2013.01)
Publication Classification (57) ABSTRACT
(51) Int. Cl. A highly loaded and well-dispersed masterbatch composition
COSL 77/00 (2006.01) and process for making thereof from a split stream process.
C08L 6/02 (2006.01) The masterbatch composition includes a colorant, a thermo
COL 67/02 (2006.01) plastic carrier, a metallocene polymer processing aid, and
COSL 33/12 (2006.01) optionally an additive. The split stream may be formed of a
COSL 8L/06 (2006.01) primary feed and a secondary feed. The primary and second
COSL 25/08 (2006.01) feeds are combined by at least one of the following: Supplying
COSL23/2 (2006.01) the secondary feed in either the same feed port as the primary
COSL23/08 (2006.01) feed, in a stream located upstream the primary feed, in a
COSL23/06 (2006.01) stream located downstream the primary feed, or a combina
COSL 7L/00 (2006.01) tion thereof.
Patent Application Publication Jan. 21, 2016 US 2016/0017144 A1

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US 2016/0017144 A1 Jan. 21, 2016

PROCESS AND COMPOSITION FOR WELL losses, such as described in U.S. Pat. No. 4,759,939, Kelleret
DISPERSED, HIGHLY LOADED COLOR al., July 1988, U.S. Pat. No. 4,880,653, Keller et al., and U.S.
MASTERBATCH Pat. No. 4,949,628 van Lengerich, August 1990. In U.S. Pat.
No. 4,965,082, Chawanet al., October 1990, describes down
TECHNICAL FIELD stream feeding of liquid ingredients in pasta production.
0001. The present disclosure relates in general to a process 0007. In the art of downstream feeding of mechanically
and composition for well dispersed, highly loaded color mas fragile materials, such as special effects pigments and func
terbatch formulations from a split stream extrusion process, tional fillers with high aspect ratio, U.S. Pat. No. 4.495.324,
optionally including one or more additives. The highly loaded Chako et al., January 1985, describes feeding short glass
color masterbatch may contain one colorant or a formulated fibers into an extruder downstream of the polymer pellet feed
blend of colorants. into the molten polymer to make a glass fiber reinforced
composite. Additional examples of downstream feeding of
BACKGROUND mechanically fragile materials include U.S. Pat. No. 5,621,
040, April 1997, and U.S. Pat. No. 5,723,520, March 1998,
0002 Colorants such as pigment preparations are often Akapeddi et al. U.S. Pat. No. 6,776,596, Brussel, August
produced for masterbatches. A masterbatch is an encapsu 2004, which describe feeding long glass fibers downstream
lated, pelletized, or granular, dust-free concentrate of a plas into the polymer stream, post melting, to create a high
tomeric or elastomeric polymer comprising a fraction of a strength glass reinforced composite. As described in U.S. Pat.
colorant. Masterbatches are used to color plastics, being No. 7,488,764, Hobbs et al., February 2009, high aspect ratios
added to the plastic to be colored prior to or during process are encapsulated in microspheres which are Subsequently fed
ing. Masterbatches are used because they provide better colo at the primary feed port along with polymer pellets and also
rant dispersion than neat colorant and eliminate dry colorant downstream of the pellets into the melt. U.S. Patent Applica
dust from the workplace. tion 2011/0073799, Magniet al., March 2011, describes com
0003) A variety of processes for producing masterbatches posites produced by downstream feeding up to 35% high
are known and the following processes are standard in the aspect ratio particles that enhance thermal conductivity of the
production of the masterbatches: a) the mixing of a suitable polymer.
matrix (polymers) with the colorant; b) dry blending/extru 0008. The downstream feeding of lubricants is described
sion and kneading with Subsequent grinding of the colorant in U.S. Pat. No. 4,446,090, Lovgren et al., May 1984, U.S.
concentrate; or c) dry blending/extrusion and subsequent fine Pat. No. 4,877,568, Austin, May 1988, and U.S. Pat. No.
spraying, hot chopping, or strand pelletizing. For example, as 5.531,923, Le Blanc et al., July 1996, which detail feeding
described in U.S. Pat. No. 7,442,742, a masterbatch compo liquid lubricants downstream of the polymer feed into the
sition is formed from dry blending/extrusion of a colorant, a molten polymer. In U.S. Pat. No. 5,486.327, Bemis et al.,
thermoplastic carrier, a metallocene polymer processing aid, describes a similar process in which liquidcolor concentrates,
and optionally an additive. In comparison to U.S. Pat. No. which often contain oils, are introduced downstream of the
7,442,742, the present invention enables up to 20% or higher polymer to extrude a colored plastic.
loadings of active ingredients. 0009. Whereas, downstream feeding of liquid compo
0004 Split stream feeding can be utilized in extrusion nents to adjust the viscosity of a material is described in U.S.
processing of plastics, food products, printing toners, latex, Pat. No. 5,316,578, Buehler et al., May 1994, and U.S. Pat.
and other materials. Split stream feeding describes the use of No. 5,480,923, Schmid et al., January 1996, with regard to
two or more feed streams directed to processing in an extrusion processing of Starch products and the introduction
extruder. of liquids downstream to reduce product viscosity in a con
0005. In the production of thermoplastic laminate struc trolled fashion.
tures, such as in U.S. Pat. No. 4,165,210, Corbett, August 0010. The downstream feeding of particulate additives
1979, plastic laminated sheet structures are produced by the and fillers is described in patent literature with regard to
combination of two streams of molten plastic and that create particulate functional additives and fillers in the production of
a laminar flow through a die yielding a laminar sheet or tube. plastics materials. U.S. Pat. No. 4,906.421, Plamthottam,
In U.S. Pat. No. 4,909,726, Bekele, March 1990, a coextru January 1990, describes downstream feeding of fillers, U.S.
sion process is described in which polymer streams from Pat. No. 5,969,089, October 1999, describes adding fillers
multiple extruders are combined at the die of one of the and functional additives downstream of resins, and U.S. Pat.
extruders to form a multilayer film. In U.S. Pat. No. 5,660, No. 6.242,127, June 2001, describes downstream addition of
922, Herridge et al., August 1997, a coextrusion process for functional additives in a film extrusion process.
making tapes is described in detail.
0006 With regard to downstream feeding of temperature 0011 Downstream feeding of flame retardant additives is
sensitive components in plastics and food processing, in U.S. described in U.S. Pat. No. 6,713,598, Selvaraj et al., March
Pat. No. 4,409,165, Kim, October 1983, describes how a 2004, U.S. Pat. No. 6,800,677, Yakobe, October 2004, which
temperature sensitive blowing agent is introduced as a sepa also includes downstream feeding of glass fibers for rein
rate feed downstream of the polymer feed at a point where the forcement, and U.S. Pat. No. 7,939.585, Gaggar et al., May
2011.
polymer is compacted but not yet molten, thereby reducing
the temperature at which fusion takes place. In U.S. Pat. No. (0012 U.S. Pat. No. 6,287,692, Luo et al., September 2001,
6,649,666, Read et al., November 2003, another process is describes extrusion processing of wire and cable compounds
described in which a feed stream of a blowing agent is intro in which particulate additives are introduced downstream of
duced separately from the polymer feed stream. In the extru the polymer feed.
sion processing of foods, water is often added as a separate (0013 U.S. Pat. No. 8.367,755 describes polyphenylene
feed stream, typically downstream to control evaporative ether thermoplastic compounds for sheet extrusion and mold
US 2016/0017144 A1 Jan. 21, 2016

ing in which additives are introduced downstream of the volume in the feed throat for adding colorants and additives
polymer feed during extrusion processing to make the com and (ii) start the pigment wetting process immediately upon
pounds. contact with the resin.
0014. The use of split resin streams in the production of (0021 Song et al. (U.S. Pat. No. 6,010,723, January 2000
polymer alloys and blends via extrusion processing is and earlier patents) describes feeding the output of an
described in U.S. Pat. No. 4,547,541, Golba, October 1985; extruder into the primary feed of a second extruder for the
U.S. Pat. No. 5.225,488, Baird et al., July 1993, U.S. Pat. No. purpose of introducing viscosity reducing additives via the
5,420,198, Papazoglou et al., May 1995: U.S. Pat. No. 7,182, second extruder. Whereas, in present invention, the majority
886, Elkovitchet al., February 2007; U.S. Pat. No. 7,868,090, of the resin component of a masterbatch formulation is pre
Ellul et al., January 2011; U.S. Pat. No. 8,148,466, Wood et melted, and serves as the carrier or binder to densify the
al., April, 2012. formulation to (i) create additional free volume in the feed
0015 Split stream feeding in reactive extrusion processes throat for adding colorants and additives and (ii) begin the
is known and described in U.S. Pat. No. 7,148,314, Gallucci pigment wetting process immediately upon contact with the
et al., December 2006, which details feeding of a component CS1.
with a desired functional group downstream of a polymer to 0022. The invention also differs from Corbett, U.S. Pat.
then react with it and yield a functionalized polymer, and U.S. No. 4,165.210, August 1979 which describes the concept of
Pat. No. 7,829,640, Barbieri et al., November 2010, which bringing streams of molten plastic together in a die to form
details an extrusion reaction process in which the output laminate structures. Similar difference exist between the cur
stream is fed back to the feed throat for further reaction. rent invention and the coextrusion processes described by
0016. Adding a colorantfeed downstream of the resin feed Bekele, U.S. Pat. No. 4,909,726, March 1990, and Herridgeet
is described in U.S. Pat. No. 6,352,654, Silvy et al., March al., U.S. Pat. No. 5,660,922, August 1997.
2002, and U.S. Pat. No. 6,776,929, Hossen, August 2004, 0023 The concept of adding pigments downstream of a
with regard to the production of an electrically conductive resin feed is known, for example, U.S. Pat. No. 6,352,654,
polymer via extrusion processing in which conductive carbon Silvy et al., March 2002, and U.S. Pat. No. 6,776,929, Hos
black powder or masterbatch is introduced downstream of the sen, August 2004 describe production of an electrically con
polymer feed into the melt. ductive polymer via extrusion processing in which conduc
0017 Utilization extrusion processing in which a molten tive carbon black powder or masterbatch is introduced
polymer is fed as a second feed stream has been described in downstream of the polymer feed into the melt, where the
U.S. Pat. No. 5,376,702, Stibel et al., December 1994, carbon black is a minor component of the total composition.
wherein a process in which a secondary polymer stream is However, the invention relates to the downstream addition of
split off, combined with other components, and then recom pigments comprising up to 80% of the total composition.
bined with the primary polymer stream. In U.S. Pat. No. 0024. Various patents describe downstream feeding offill
6,010,723, Song et al., January 2000, a process is described ers, such as short glass fibers and composites with up to 70%
for making chewing gum in which components of the recipe glass fiber, which are commercially available. Colorants,
are compounded in a first extruder which then feeds its output however, have a much higher Surface area to wet out, and as
to a second extruder into which are also fed components that noted above, are dosed in as minor components downstream.
will reduce the viscosity of the melt stream from extruder 1.
00.18 Extrusion compounding of a complex mixture of 0025. The prior art fails to describe introducing a pre
particulates, liquids, and resins in which a binder is fed down melted resin carrier feed downstream of the powder feed. Nor
stream has been discussed in U.S. Pat. No. 4,894,308, Maha is the concept of pre-melting the resin feed for the combined
badi et al., January 1990, wherein extrusion processing purposes of increasing the Volume available for the powders
occurs of electrostatic dry printing toners by utilizing a dry to achieve higher loading than previously possible and initi
blend of surfactants and pigments at the main feed port, which ating the wetting out process on contact. The invention
are melted under heat and pressure, and then conveyed past a described herein provides a volume enhancement in the pri
second feed port where a polymer is introduced as a powder mary feed in which the polymer melt feed and the colorant
or pellets. In U.S. Pat. No. 7,572.567, Chung et al., August mix feed are introduced at the same primary feed throat.
2009, describes a process in which an aqueous solution of Furthermore, none of the patents described relate to the intro
poly Aluminum Chloride is introduced downstream as a duction of the polymer feed as a molten stream that is the
coagulating binder into the melt stream of pigments and other output of a second melt processing unit, or feeding the resin
components of an electrostatic toner for dry printing. stream is upstream of the colorant mix feed. The methods
cited in the prior art describe an extrusion process in which
0019. The described art is related to materials that were the resin is compressed and melted in the extruder prior to
intended to be fabricated into parts or materials and methods reaching the Zone where the downstream feed port is located.
for fabricating constructions. In contrast, the present inven However, as described in detail herein, there are advantages in
tion relates to a process and materials for making an interme pre-melting the resin in a separate device: (i) the compres
diate that is used to color thermoplastic materials; specifi Sion, kneading, and melting Zones of the primary extruder can
cally, color and additive masterbatches. be minimized; (ii) the process is more energy efficient in that
0020. In Stibel et al. (U.S. Pat. No. 5,376,702, December more of the energy supplied to the extruder is used to affect
1994), a separate molten polymer stream is combined with incorporation and dispersion of the colorants and additives,
additives, and then recombined with a primary feed. In con enabling higher production rates, and (iii) a simple single
trast, the present invention describes the counter-intuitive screw extruder or melt pump can be used to pre-melt the
process of premelting the majority of the resin component of polymer. Based on this, the total cost of the combined system
a masterbatch formulation which serves as the carrier or can be lower or comparable than that of the conventional
binder to increase the density to (i) create additional free extruder alone.
US 2016/0017144 A1 Jan. 21, 2016

0026. Known masterbatches formed from dry blending/ 0033. In addition, other deficiencies in processing known
extrusion are generally formulated using a method which dry blending/extrusion masterbatch compositions are ineffi
includes a thermoplastic polymer, a colorant, a dispersant, ciencies of the work provided by the extruder and inefficien
and optionally one or more additives. The thermoplastic poly cies of the length of the extrusion cycle. Specifically, much of
mer is commonly referred to as a “carrier' or “carrier resin.” the energy and residence time is spent melting the polymer
A typical commercial formulation of a masterbatch, particu carrier instead of dispersing colorants.
larly formulated with a mixture of colorants (pigments and 0034 Presently, there is no known system or method for
dyes) includes about 30% by weight of colorant, about 5% by providing a masterbatch composition that avoids the forego
weight of dispersant, about 10% by weight of additive, and ing problems associated with conventional masterbatches.
about 55% by weight of a carrier. Accordingly, it is desirable to provide a masterbatch compo
0027. Unfortunately, known masterbatches formed from sition with improved processability that increases loading of
dry blending/extrusion, particularly those comprised of the masterbatch composition as well as the coloration of the
blends of colorants (pigments and dyes) have a relatively low end product without sacrificing production rate, production
colorant concentration. Thus, it has been found that many throughput, physical and mechanical properties of the col
known masterbatches introduce unnecessary costs and ored parts, and Surface appearance, all the while introducing
undesired amounts of auxiliary ingredients, such as carrier less carrier resin into the end part.
matrix. Particularly in the case of colorant formulations con 0035. The present application, as described and claimed
taining relatively high proportions of organic pigments, herein, addresses the above described deficiencies of prior art
higher loadings of colorant cannot be used in known master masterbatches and processes for developing the same.
batches produced from dry pigments due to insufficient dis SUMMARY
persion. Insufficient dispersion of the colorant particles can
lead to a decrease in physical and mechanical properties of the 0036. In one aspect, the present disclosure is directed to a
end product, Such as tensile strength, flexural modulus, elon process for making a masterbatch that includes mixing a
gation, and impact strength. Also, pigment agglomerates can colorant, an additive, a thermoplastic carrier, and optionally a
lead to Surface imperfections that affect the parts appear metallocene polymer processing aid, and then adding a
aCC.
majority of the carrier resin in a molten state either to a port
0028 Organic pigment dispersion in conventionally pro located at the primary feed, upstream the primary feed, down
duced masterbatches can be improved by using mostly or stream of the primary feed, or a combination thereof. While it
entirely powdered or finely granulated resins. However, this is not uncommon to introduce additives and colorants as a
practice results in introducing dry blend mixtures of resin, separate stream in melt processing thermoplastics, generally
colorants, and other ingredients having a significantly lower downstream of the main feed, it is counterintuitive in conven
bulk density than mixtures with resin pellets. Less material is tional masterbatch processing to introduce the majority of the
introduced into the extruder in any given time, resulting in a resin to a primary extruder as a melt stream generated by a
significant reduction in processing rate. secondary extruder or melt pump.
0029. Another deficiency in known dry blending/extru 0037. The present disclosure is directed to a masterbatch
sion masterbatch compositions is the inability to significantly composition produced by using a split stream feed, which
improve the processability of the masterbatch itself and the includes a main or primary feed having a colorant, a polymer
end product. processing aid, and optionally an additive and carrier resin,
0030. Another deficiency in known dry blending/extru and a secondary feed including a majority of the carrier resin
in a molten state either connected to the same feed as the
sion masterbatch processing is the blend Volume limitation in primary feed, upstream the primary feed, downstream of the
the feed throat of an extruder. Fixed volume in the feed throat
limits pigment and additive loadings, particularly in the case primary feed, or a combination thereof. The primary feed is
of organic pigments and certain effects pigments, such as largely composed of colorants, pigments, powdered resins,
pearlescent pigments, due to the low bulk density of these processing aids, and functional additives Such as UV, AO,
pigments. Similarly, these limitations on the amount of mate slip, antistats, anti-microbial, FR, etc. The primary feed may
rial introduced at the feed throat significantly reduce extru be a powder feed, a colorant mix feed, and/or a small granule
feed.
sion throughput and color strength. 0038. In a further aspect, the present disclosure is directed
0031 Problems due to the fixed volume in the feed throat to a process for making a colorized polymer that includes
could be alleviated by increasing the free volume in the feed introducing a highly-loaded masterbatch composition to a
throat by using thinner flights, adding deeper roots on the melt-processible polymer to form a melt feed polymer com
screw, and extending the length of the opening; however, all position, wherein the masterbatch comprises a colorant, a
of these attempts will only provide Small incremental gains in thermoplastic carrier, a metallocene polymer processing aid,
the volume space (e.g. 10-15% more free volume space), do and optionally an additive, and extruding the polymer com
not provide the desired increase in pigment and additive load position to form the colorized polymer.
ing, and sacrifice the strength and life of the screw. 0039. In an embodiment, a process for making a highly
0032. Another deficiency in known dry blending/extru loaded and well-dispersed masterbatch composition from a
sion masterbatch compositions is the inability to include rela split stream process comprises the following steps: a) mixing
tively significant amounts of loading with regard to additives a colorant in a mixture in a primary feed; b) pre-melting a
Such as ultraviolet light absorbers, light stabilizers, antioxi thermoplastic carrier in a secondary feed; and c) combining
dants, and blowing agents. Generally, additives are added the mixture of the primary feed and the melted thermoplastic
only if desired and then in small amounts. Otherwise, it is carrier of the secondary feed to form the masterbatch com
believed that the processability of the masterbatch would be position. Using the masterbatch composition from this pro
impaired. cess, a thermoplastic article may be produced.
US 2016/0017144 A1 Jan. 21, 2016

0040. In an embodiment, the mixing step includes an addi tion, wherein the masterbatch composition comprises a pig
tive in the primary feed, the secondary feed, or a combination ment, a thermoplastic carrier, and, greater than 5% to about
thereof. 60% by weight of an additive, wherein the additive is selected
0041. In an embodiment, the mixing step includes a met from the group consisting of antioxidants, ultraviolet light
allocene polymer processing aid in a primary feed, wherein absorbers, and light stabilizers; and b) processing the polymer
the metallocene polymer processing aid is a polyolefin. The composition to form the masterbatch composition.
metallocene polymer processing aid may be an amorphous
metallocene polypropylene copolymer obtained by polymer BRIEF DESCRIPTION OF THE DRAWINGS
izing a propylene monomer with about 2-15% ethylene 0049. The present disclosure may be better understood by
comonomer in the presence of a metallocene catalyst. Fur reference to the following detailed description taken in con
ther, the metallocene polymer processing aid may exhibit a nection with the following illustrations, wherein:
density of about 0.87–0.93 g/cm3, a drop point of about
80-145° C., and a viscosity of about 60-6300 mPas. 0050 FIG. 1 is a process flow diagram for making a highly
0042. The combining step may further include supplying loaded and well-dispersed masterbatch composition from a
the secondary feed to a port located by the primary feed, split stream process in an embodiment;
upstream the primary feed, downstream the primary feed, or 0051 FIG. 2 is a process flow diagram for making a highly
a combination thereof. The combining step may further loaded and well-dispersed masterbatch composition from a
include Supplying an additive in the primary feed, the second split stream process in another embodiment; and
ary feed, or a combination thereof. 0.052 FIG.3 is a process flow diagram for making a highly
0043. An additive may be selected from the group consist loaded and well-dispersed masterbatch composition from a
ing of antioxidants, ultraviolet light absorbers, light stabiliz split stream process in yet another embodiment.
ers, flame-retardants, antibacterial agents, Surface tension DETAILED DESCRIPTION
reducers, deodorizing agents, anti-static agents, anti-block
ing agents, plasticizer agents, fillers, and blowing agents. 0053 Reference will now be made in detail to exemplary
0044) The additive may further include an antioxidant of embodiments of the present teachings, examples of which are
about 0-15% by weight, a light stabilizer about 0-45% by illustrated in the accompanying drawings. It is to be under
weight, and an ultraviolet light absorber about 0-45% by stood that other embodiments may be utilized and structural
weight. In an embodiment, the additive is about 5-60% by and functional changes may be made without departing from
weight. the respective scope of the present teachings. Moreover, fea
0045. The colorant may be about 15-80% by weight, the tures of the various embodiments may be combined or altered
thermoplastic carrier is about 9-60% by weight, and the met without departing from the scope of the present teachings. As
allocene polymer is about 2-20% by weight. The colorant Such, the following description is presented by way of illus
may be selected from the group consisting of organic pig tration only and should not limit in any way the various
ment, inorganic pigment, single pigment dispersion, dye, alternatives and modifications that may be made to the illus
coated mica, powdered aluminum, optical brightener, fluo trated embodiments and still be within the spirit and scope of
rescent, and phosphorescent. The colorant may include an the present teachings.
organic pigment about 5-50% by weight. The colorant may 0054. A masterbatch composition having a colorant and
include an organic pigment about 10-40% by weight. The optionally one or more additives is provided. This disclosure
colorant may include an inorganic pigment about 0-80% by describes the use of split stream feed processing equipment to
weight. Further, the colorant may include an organic pigment make relatively highly loaded color concentrates and addi
about 3-40% by weight and an inorganic pigment about tives. The masterbatch composition of the present disclosure
10-60% by weight. exhibits excellent colorant dispersability, coloring properties,
0046. The thermoplastic carrier may be selected from at increased additive concentrations, as well as improved
least one of the following: homopolymers and copolymers of handleability, so that the colored end product has excellent
polyethylene, polypropylene, polystyrene, polyoxymethyl physical and mechanical strength as well as excellent colora
ene, polyethylene terephthalate, polybutylene terephthalate, tion. The present masterbatch composition optionally
polymethyl methacrylate, polyether Sulfones, polysulfones, includes a metallocene polymer processing aid that Substan
polyether ketones, polystyrene copolymers, acrylonitrile tially eliminates many of the practical problems and limita
butadiene-styrene terpolymers, polyamides, polycarbonate, tions encountered in the current art. The optional metallocene
and combinations thereof. polymer processing aid is compatible with various carrier
0047. The process may further include a dispersion pack resins, allows for decreasing the amount of conventional car
age. In an embodiment, a dispersion package is selected from rier resin, and also provides better mechanical and physical
the group consisting of waxes, metal salts, coupling agents, properties of the end products. The masterbatch split stream
and Surfactants. The dispersion package may be about 2-8% process allows for extraordinary increases in colorant loading
by weight. The process may further include one of the fol compared to known processes. As the concentration of colo
lowing: flame-retardants, antibacterial agents, Surface ten rants and additives is increased, the amount of the master
sion reducers, deodorizing agents, anti-static agents, anti batch composition required to achieve the desired end prod
blocking agents, plasticizer agents, fillers, and blowing uct properties can be appreciably lower than conventional
agents. masterbatch compositions. In addition, the optional metal
0048. A process for making a highly loaded and well locene processing aid also improves the handleability of the
dispersed masterbatch composition may further include the masterbatch composition, as the masterbatch composition
steps of: a) introducing a masterbatch composition formed melts at lower temperatures that allow it to “wet out” or
from a split stream process, as provided in claim 1, to a distribute more efficiently to provide better processability and
melt-processible polymer to form a feed polymer composi increased throughput.
US 2016/0017144 A1 Jan. 21, 2016

0055. The masterbatch compositions generally include a tures thereof. Pigments may be at least one or a combination
colorant, a thermoplastic carrier, and optionally a metal of organic pigments and inorganic pigments, and there is no
locene processing aid and additives, such as antioxidants, particular limitation. When organic pigments are used, the
ultraviolet light absorbers, and light stabilizers. In an embodi organic pigments may be present up to about 50% by weight
ment, the metallocene polymer processing aid is an amor of the masterbatch composition. In a preferred embodiment,
phous metallocene polypropylene copolymer obtained by the organic pigments are present in a range from about 10 to
polymerizing a propylene monomer with about 2-15%, about about 40% by weight of the masterbatch composition. If
2-10%, or about 5-10%, ethylene comonomer in the presence inorganic pigments are used, the inorganic pigments may be
of a metallocene catalyst. In an embodiment, the metallocene present up to about 75% by weight of the masterbatch com
polymer processing aid exhibits a density of about 0.87–0.93 position. In a preferred embodiment, the inorganic pigments
g/cm3, a drop point of about 80-145° C., and a viscosity of are present in a range from about 15% to about 75% by weight
about 60-6300 mPas. In an embodiment, the metallocene of the masterbatch composition. In another embodiment, both
polymer processing aid may have a range from amorphous to organic and inorganic pigments are used, and the organic
highly crystalline. pigments may be present up to about 20% and the inorganic
0056. In an embodiment, the processing aid is a metal pigments may be present up to about 60%. In one embodi
locene polymer which is a general term for a polymer in ment, the organic pigment is present from about 3% to about
which metallocene is used as a catalyst for polymerization. 20% and the inorganic pigment is present from about 10% to
The metallocene polymer processing aid is not a metallocene about 60%.
resin as is used in conventional masterbatches and has differ 0060 Illustrative examples of the organic pigments
ent structural and physical properties therefrom. This metal include azo and disazo pigments such as azo and disazo lake,
locene processing aid is a polymer having higher monodis Hansas, benzimidazolones, diarylides, pyrazolones, yellows
persibility and a narrower molecular weight distribution (for and reds; polycyclic pigments such as phthalocyanines,
instance, Mw/Mn<2 in the case of metallocene polyethylene) quinacridones, perylenes, perinones, dioxazines,
than a polymer in which a conventional Ziegler catalyst, anthraquinones, isoindolins, thioindigo, diary1 or quinoph
Ziegler-Natta catalyst or the like is used. It has been found thalone pigment, Aniline Black, or mixtures thereof. Illustra
that the metallocene polymer processing aid allows a large tive examples of the inorganic pigments include inorganic
amount of colorant to be evenly dispersed in the presence of pigments such as titanium oxide, titanium yellow, iron oxide,
a high additive concentration, giving the end product excel ultramarine blue, cobalt blue, chromic oxide green, Lead
lent coloration as well as better physical and mechanical Yellow, cadmium yellow and cadmium red, carbon black
properties. Accordingly, the composition can provide molded pigments, and mixtures thereof. The organic and inorganic
or extruded articles having excellent mechanical strength. pigments can be used singly or in combination. These pig
0057 Accordingly, the metallocene polymer is a preferred ments may be in any form of a dry powder, single pigment
processing aid because it has a low drop point, low viscosity, dispersions made conventionally or according to this process,
low density, and good wetting capability. The drop point of or mixtures thereof.
polymer ranges preferably from 80° C. to 120° C. The vis 0061. In an embodiment, the colorant is about 15-80% by
cosity of the polymer is preferably 60 to 6300 mPas. The weight, the thermoplastic carrier is about 9-60% by weight,
density of the polymer is preferably 0.87 to 0.93 g/cm. The and the metallocene polymer is about 2-20% by weight. In
metallocene polymer may be present in the masterbatch com another embodiment, the colorant is selected from the group
position up to about 20%, preferably from about 4% to about consisting of organic pigment, inorganic pigment, single pig
12%. Suitable metallocene polymers include homopolymers ment dispersion, dye, coated mica, powdered aluminum,
of propylene or copolymers of propylene with one or more optical brightener, fluorescent, and phosphorescent. In yet
olefins or grafted with other polymers. Copolymers of pro another embodiment, the colorant comprises an organic pig
pylene with ethylene are preferred. The ethylene content of ment about 5-50% by weight. In an embodiment, the colorant
the copolymers is from 0.1% to about 20%, preferably from comprises an organic pigment about 10-40% by weight. In an
about 2% to about 10%. embodiment, the colorant comprises an inorganic pigment
0058. The metallocene polymer processing aid is highly about 0-80% by weight. In an embodiment, the colorant com
compatible with various carrier resins. Illustrative examples prises an organic pigment about 3-40% by weight and an
of thermoplastic carriers are homopolymers or copolymers of inorganic pigment about 10-60% by weight.
high and low density polyethylene, high and low density 0062 Optionally, the masterbatch composition may also
polypropylene, polystyrene, polyoxymethylene, polyethyl comprise an additive. Illustrative examples are ultraviolet
ene terephthalate, polybutylene terephthalate, polymethyl light absorbers, light stabilizers, antioxidants, flame-retar
methacrylate, polyether Sulfones, polysulfones, polyether dants, antibacterial agents, Surface tension reducers, deodor
ketones, polystyrene copolymers, acrylonitrile-butadiene izing agents, anti-static agents, anti-blocking agents, plasti
styrene terpolymers, polyamides such as nylon-6 or nylon-6, cizer agents, blowing agents, fillers, and other known
6, polyvinyl chloride and copolymers of ethylene with 0.1-20 additives, or mixtures thereof.
mol % of 1-butene, 1-pentene, 1-hexene, 4-methyl-1-pen 0063 Ultraviolet light absorbers (UVA) shield the poly
tene, 1-octene, 1-decene, 1-undecene, other impact modified mer from LTV light by absorbing light energy and releasing
alloys, or mixtures thereof. The polymer to be and the carrier the absorbed light energy harmlessly as heat energy. Hin
polymer of the masterbatch can be, but do not have to be, the dered amine light stabilizers (HALS) scavenge radical inter
SaC. mediates formed in the photo-oxidation process. The higher
0059 Colorants added to the masterbatch may comprise the concentration of UVA and/or HALS, the greater the pro
pigments, single pigment dispersions, dyes, nano compos tection of the polymer (both the masterbatch carrier and the
ites, coated micas, powdered aluminum and other metals, end product) from degradation and the color from fading.
optical brighteners, fluorescents, phosphorescents, or mix UVAs and HALS can be added up to about 45% by weight of
US 2016/0017144 A1 Jan. 21, 2016

the masterbatch. Preferred UVAs and HALS include those of masterbatch. It is preferred in such embodiments that the
the TINUVINR) grades from BASF SE. Illustrative examples UVAs (and/or HALS) are added up to about 45% by weight of
of UVA’s and HALS include salicylic acid derivatives such as the masterbatch, and the antioxidant is added up to about 15%
phenyl salicylate, p-t-butyl salicylate, etc., benzophenone by weight of the masterbatch. Sterically hindered phenols or
system such as 2,4-dihydroxybenzophenone, 2-hydroxy-4- HALS are preferred antioxidants, particularly sterically hin
methoxybenzophenone, etc., benzotriazole system Such as dered phenols of the IrganoxR) grades from BASF SE. Other
2-(2-hydroxy-3',5'-di-t-butylphenyl)benzotriazole, 2-(2-hy illustrative examples of antioxidants include a phenol system
droxy-3'-t-butyl-5'-methylphenyl)-5-chlorobenzotriazole, such as 2,6-di-t-butyl-p-Cresol, pentaerythritol-tetrakis-(3.5-
etc., hindered amine system Such as bis(2.2.6.6-tetramethyl di-t-butyl-4-hydroxyphenyl)propionate methyl phenol, octa
4-piperidyl) sebacate, dimethyl Succinate-1-(2-hydroxy decyl-3-(3,5-di-t-butyl-4-hydroxyphenyl) propionate, etc.,
ethyl)-4-hydroxy-2.2.6.6-tetramethyl piperidine condensa phosphorus system Such as tris(2,4-di-t-butylphenyl)phos
tion product, 2-hydroxybenzophenones, e.g. 2,4- phate, distearylpnetaerythritol diphophate, tetrakis(2,4-di-t-
dihydroxybenzophenone, 2-hydroxy-4- butylphenyl)-4,4'-biphenylene phosphonate, etc., Sulfur sys
methoxybenzophenone, 2-hydroxy-4-Octoxybenzophenone, tem such as distearyl-3,3'-thiodipropionate, pentaerythritol
and 5.5'-methylene bis(2-hydroxy-4-methoxybenzophe tetrakis-(3-laurylthiopropionate), hindered phenol type
none), 2-(2-hydroxyphenyl)benzotriazoles, e.g. 2-(2-hy antioxidants and peroxide decomposers, HALS (as set
droxy-5'-methylphenyl)benzotriazole, 2-(2-hydroxy-5'-t- described above), or mixtures thereof.
octylphenyl)benzotriazole, -(2-hydroxy-3',5'-di-t- 0.066 Illustrative examples of hindered phenol type anti
butylphenyl)benzotriazole, 2-(2-hydroxy-3',5'-di-t- oxidants are 2,6-di-t-butyl-4-methylphenol, styrenated phe
butylphenyl)-5-chlorobenzotriazole, 2-(2-hydroxy-3'-t- nol, n-octadecyl-3-(3,5-di-t-butyl-4-hydroxylphenyl) propi
butyl-5'-methylphenyl)-5-chlorobenzotriazole, 2-(2- onate, 2,2'-methylene bis(4-methyl-6-t-butylphenol), 2-t-
hydroxy-3',5'-dicumylphenyl)benzotriazole, and 2,2'- butyl-6-(3-t-butyl-2-hydroxy-5-methylbenzyl)-4-
methylene bis(4-t-octyl-6-benzotriazolyl)phenol; benzoates, methylphenylacrylate, 2-1-(2-hydroxy-3,5-di-t-
e.g. phenylsalicylate, resorcinol monobenzoate, 2,4-di-t-bu pentylphenyl)ethyl-4,6-di-t-pentylphenyl acrylate, 4,4'-
tylphenyl-3',5'-di-t-butyl-4'-hydroxybenzoate, and hexade butylidene bis(3-methyl-6-t-butylphenol), 4,4'-thio-bis(3-
cyl-3,5-di-t-butyl-4-hydroxybenzoate; substituted oxanil methyl-6-t-butylphenol), alkylated bisphenol, tetrakis
ides, e.g. 2-ethyl-2'-ethoxyoxanilide and 2-ethoxy-4'- methylene-3-(3,5-di-t-butyl-4-hydroxyphenyl)-
dodecyloxanilide; cyanoacrylates, e.g. ethyl-alpha-cyano proprionate methane, 3.9-bis(2-3-(3-t-butyl-4-hydroxy-5-
beta, beta-diphenylacrylate and methyl-2-cyano-3-methyl-3- methylphenyl)-propionyloxy)-1,1-dimethylethyl-2.4.8.10
(p-methoxyphenyl)acrylate, and any other known UVA, or tetraoxyspiro5.5undecane, or mixtures thereof.
mixtures thereof. 0067 Illustrative examples of peroxide decomposers are
0064. Additional illustrative examples of HALS include organic phosphorus type peroxide decomposers. Such as tris
2.2.6.6-tetramethyl-4-piperidylstearate, 1.2.2.6,6-pentam nonylphenylphosphite, triphenylphosphite and tris(2,4-di-t-
ethyl-4-piperidylstearate, 2.2.6,6-tetramethyl-4-piperidyl butylphenyl)phosphite; and organic thio type peroxide
benzoate, bis(2.2.6,6-tetramethyl-4-piperidylsebacate, bis(1, decomposers, such as dilauryl-3,3'-thiodipropionate, dimyri
2.2.6,6-pentamethyl-4-piperidyl)sebacate, tetrakis(2.2.6.6- styl-3,3'-thiodipropionate, distearyl-3,3'-thiodipropionate,
tetramethyl-4-piperidyl)-1,2,3,4-butane tetracarboxylate, pentaerythrityltetrakis(3-laurylthiopropionate), ditridecyl-3,
tetrakis(1.2.2.6,6-pentamethyl-4-piperidyl)-1,2,3,4-butane 3'-thiodipropionate and 2-mercaptobenzimidazole, or mix
tetracarboxylate, bis(1.2.2.6,6-pentamethyl-4-piperidyl)-di tures thereof.
(tridecyl)-1,2,3,4-butane tetracarboxylate, bis(1.2.2.6,6-pen 0068 Illustrative examples of flame-retardants are phos
tamethyl-4-piperidyl)-2-butyl-2-(3',5'-di-t-butyl-4-hydr phoric acid systems such as allyl diallyl phosphate, cresyl
oxybenzyl)malonate, 1-(2-hydroxyethyl)-2.2.6,6- diphenyl phosphate, octyl diphenyl phosphate, triallyl phos
tetramethyl-4-piperidinol/diethyl Succinate polycondensate, phate, tributyl phosphate, triphenyl phosphate, tris(...beta.-
1,6-bis(2.2.6,6-tetramethyl-4-piperidylamino) hexane/di chloroethyl)phosphate, tris(dichloropropyl)phosphate, tris
bromoethane polycondensate, 1,6-bis(2.2.6.6-tetramethyl-4- (2,3-dibrompropyl)phosphate, tris(bromo-chloropropyl)
piperidylamino)hexane/2,4-dichloro-6-t-octy-1 amino-s-tri phosphate, etc., chlorine system such as chlorinated paraffin,
azine polycondensate, 1,6-bis(2.2.6,6-tetramethyl-4- chlorinated polyphenyl, perchloropentacyclodecane, etc.,
piperidylamino)hexane/2,4-dichloro-6-morpho-1 ino-S- bromine system Such as tetrabromoethane, tetrabromobu
triazine polycondensate, and the like, or mixtures thereof. tane, hexaborombenzene, decabromodiphenyloxide, polydi
0065 Antioxidants, including processing stabilizers, can brornophenyloxide, bis(tribromophenoxy)ethane, ethylene
be added to the masterbatch composition up to about 15% by bisbromonorbornane dicarboxylmide, ethylene bistetrabro
weight of the masterbatch. Peroxide polymer degradation mophthalimide, etc. reaction type such as chlorendic acid
generally occurs during processing (e.g. due to heat or shear), anhydride, tetrabromo phthalic anhydride, tetrabromo
or at the time of light exposure. Peroxide radicals may be bisphenol A, dietoxy-bis-(2-hydroxyethyl)-aminomethyl
formed during this period, which in turn may lead to the phosphate, dibormcresyl alycidyl ether, etc., or mixtures
formation of hyperoxides. Antioxidants are incorporated into thereof.
polymers to stabilize peroxide radicals to prevent degrada 0069 Illustrative examples of antibacterial agents include,
tion. Optimal polymer stability is achieved when the initial phenol ether based antibacterial agents, such as those having
molecular weight and/or the initial color of the polymer is the phenol group in the intramolecular skeleton, for example,
maintained. Therefore, the present masterbatch composition 10, 10'-oxybisphenoxa arsine, etc.: natural antibacterial
provides a higher degree of protection by achieving higher agents. Such as those having tropolone as a central skeleton,
additive concentrations without sacrificing colorant concen for example, hinokitiol, beta-dollabulin, etc., as glycerol ester
tration. In one embodiment, both UVAs (and/or HALS) and of fatty acid, lower fatty acid monoglycerol ester, Sucrose
an antioxidant may be added up to about 60% by weight of the fatty acid ester, polyglycerol fatty acid ester, for example,
US 2016/0017144 A1 Jan. 21, 2016

monoglyceride caprylate, monoglyceride caprate, lauric acid metering Zones, which may include, but not limited to knead
monoglyceride, Sugar-ester palpitate, decaglycerol monoca ing, compressing, reversing elements, etc.
prate, hexaglycerol caprylate, etc., Zeolite-based compounds, 0075. In an embodiment, the secondary feed includes a
part or whole of ion-exchangeable ion in Zeolite-based com majority of the carrier resin in a molten state. All or most of
pounds, for example, part or whole of sodium ion, calcium the carrier resin can be introduced to the masterbatch through
ion, potassium ion, magnesium ion, iron ion, etc. is Substi the secondary feed. In alternative embodiments, the second
tuted with ions with antibacterial property, Such as silver ion, ary feed is introduced in a molten state via a secondary feed
copper ion, Zinc ion, ammonium ion, etc. can be exemplified. port about 8 L/D upstream or downstream. The secondary
These compounds can be used singly or two or more kinds of feed may be produced by a relatively small secondary
them can be used in combination. extruder, Such as a low L/D single screw extruder, or a melt
0070 Fillers are typically inexpensive particulate materi pump. In one embodiment, the secondary feed can be intro
als that do not contribute to the color. Illustrative examples of duced by side feeding. In an embodiment, pre-melted resin
fillers include, among others, talcs, micas, clays, nano-clays, carrier in the secondary feed stream has an increased melt
silicas, or mixtures thereof. flow compared to the low melt/high processed powder from
0071. The masterbatch composition described herein may the primary feed stream.
contain other additives or ingredients and should not be lim 0076 Introduction of the carrier resin from the secondary
ited to the stated formulations. In one embodiment, a disper feed as a melt stream results in a higher density composition
sion package can be added to the masterbatch composition in as compared to the bulk density of the pellets, flakes, or
an amount up to about 25% by weight of the masterbatch. In powder. Combination of the main/primary and secondary
another embodiment, the dispersion package is added in an feeds allow for a higher volume of colorants and additives to
amount from about 2% to about 8% based on the weight of the be introduced via the primary feed. The secondary feed con
masterbatch. The dispersion package can be waxes, metal taining the molten carrier resin begins to wet out the pigment
salts, Surfactants, coupling agents, organometallic com immediately upon contact with the mixture from the main
pounds, and mixtures thereof. Illustrative examples include Stream.
conventional polyethylene and polypropylene waxes and 0077 Use of a secondary feed provides benefits from
derivatives thereof such as acid-modified products and metal maintenance and cleaning perspectives, as the corresponding
salts of acid-modified products, as well as Zinc Stearate, mag secondary extruder or melt pump requires a changeover only
nesium Stearate, aluminum Stearate, calcium Stearate and eth when the resin is altered orchanged. Such that merely a simple
ylene bisteramide, and mixtures thereof. purge with the next resin is needed. Based on this, the addition
0072 Before actual mixing of the masterbatch, the com of a carrier stream in the secondary feed saves time and
ponents for each of the main feed and the secondary feed can money with regard to maintenance and cleaning of at least the
be premixed if desired, for which drum or tumbler mixers secondary feed extruder/melt pump.
may be used. In the actual dry blend mixing process, the 0078. An additional benefit of using a secondary feed
mixing can be performed in a blade-type mixer. In one includes having additional room for active ingredients to be
embodiment, the colorant blend is mixed in a high intensity processed in the extruder and wetted out with molten poly
mixer along with some wax until the wax melts and encap mer, which takes up less free volume in the extruder than the
Sulates the colorants, resulting in a well dispersed, densified pellet form. This allows for processing an increased loading
colorant blend. Additional dispersion takes place in an of low bulk density ingredients.
extruder, for example a single-screw or twin-screw extruder, 007.9 Furthermore, use of a secondary feed, whether it is
however, any Suitable equipment known in the art may be concurrent, upstream, or downstream the primary feed, will
used. Illustrative examples include Buss kneaders, planetary increase the efficiency of the work that the extruder can pro
roll extruders, open double-trough kneaders, rapid stirrers, vide by filling flights with low bulk density ingredients with
internal fluxing mixers such as Banbury mixers and Farrel low temperature melting metallocene polymerand dispersing
continuous mixers, or the like. aids that will wet our early and add density to the powder
0073. In a main or primary feed the following are pro ingredients, so that once the molten resin is introduced in its
cessed in a dry blend/extrusion configuration: a colorant, and most dense state, the flights of the extruder are full of a
optionally an additive, a carrier resin, and a polymer process masterbatch, as opposed to being partially full (e.g. "/4 or /2).
ing aid. In one embodiment, the carrier resin in the primary Such as those of conventional masterbatch extrusion pro
feed may be present up to about 10% of the total formulation cesses. Filling flights allows for an increase of work and
weight and can be blended in with the pigments and additives pressure within the extruder, which facilitates dispersion and
in the primary feed in a dry blend stage to assist with the high throughput rates. Correspondingly, another advantage of
pigment wetting out process. Alternatively, no carrier resin utility of a secondary feed is that the length of the extrusion
can be added to the primary feed. time can be shortened because the resin does not need to be
0074 The primary feed is in connection with a secondary melted and there is increased efficiency of utilizing full
feed at the primary feed port, upstream the primary feed port, flights. Use of a secondary feed allows for many benefits
downstream the primary feed port, or a combination thereof. without sacrificing production rates.
As illustrated in FIG. 1, a process flow diagram is shown 0080. In an embodiment, the secondary feed is processed
wherein the primary feed is upstream the secondary feed, in as a continuous process operated via a single screw or con
FIG. 2, the secondary feed is illustrated upstream the primary tinuous mixer. In another embodiment, the secondary feed is
feed, and in FIG. 3, the primary feed and secondary feed are processed in a batch process.
connected at the same feed port. The feed port, as illustrated I0081 Furthermore, the secondary feed may be processed
in the Figures, may represent a meter, a valve, an opening, and by use of agentle screw configuration with minimal mixing,
any combination thereof. The conveying Zone illustrates the yet maintain a masterbatch composition with high loadings.
conveyance of the materials to the melting, dispersing, and In an embodiment, the secondary feed is paired with a gentle
US 2016/0017144 A1 Jan. 21, 2016

screw configuration, a dispersive Screw with mostly knead I0086 Table 2 illustrates the pigment loading for a Green
ers, a single screw extruder, or a twin-screw extruder. Formulation for Polyolefins of various masterbatch compo
0082 In another embodiment, a primary feed and a sec sitions formed from a split stream, wherein the ratio of the
ondary feed may be introduced at a first feed throat and yet primary feed to the secondary feed is 60:40, 65:35, 70:30,
maintain a masterbatch formulation with at least 50% inor
ganic pigment loading. 75:25, or 80:20 by weight. Similar to the above described
0083. In exemplary embodiments, as shown below in Table 1, as the ratio of the primary feed to secondary feed
Tables 1, 2, 3, and 4, a set of trials for Red (Red Formulation increases, the loading of pigment also increases. As shown in
for Polyolefins), Green (Green Formulation for Polyolefins), Table 2, an 80:20 split results in a higher bulk density of green
Purple (Purple Pearl Formulation for Polyolefins), and Yel pigment of approximately 48% higher loading than the G2
low (Yellow Formulation for Polyolefins) pigmented master
batch compositions are formulated from the split stream pro Formula.
cess described herein and compared to a conventional 0087 In exemplary embodiments, as shown below in
masterbatch formulated developed from a dry blend/extru
sion process as shown below. The components of the color Tables 3 and 4, a set of trials for Purple (Purple Pearl Formu
feed stream are dry blended and then introduced upstream of lation for Polyolefins) and Yellow (Yellow Formulation for
the molten resin feed stream. Polyolefins) pigmented masterbatch compositions are formu
0084 As referred to herein, the G2(R) Formula is developed lated from the split stream process described herein and com
according to U.S. Pat. No. 7,442,742, wherein G2 is a regis
tered trademark owned by Carolina Color Corporation pared to a conventional masterbatch formulated developed
located in Salisbury, N.C. from a dry blend/extrusion process:
TABLE 1
Red Formulation for Polyolefins
G2 Formula 60:40 Split 65:35 Split 70:30 Split 75:25 Split
Component % of Total % of Total % of Total % of Total % of Total
Pigment Red 122 11.86 13.47 14.59 15.72 16.84
Pigment Red 101 4.14 4.70 S.09 S.49 5.87
Pigment Red 170 12.65 14.37 15.57 16.77 17.96
Polymer Processing Aid S.OO 4.73 S.13 5.52 S.91
Dispersion Aid 3.00 3.78 4.10 4.42 4.73
PE Flake 2O.OO 1892 2O.SO 22.08 23.65
PE Pelets 43.33 40.OO 35.00 3O.OO 2S.OO
Pigment Loading v. Standard 100% 114% 123% 1.32% 1.42%

0085 Table 1 illustrates the pigment loading for a Red TABLE 3

Formulation for Polyolefins of various masterbatch compo
sitions formed from a split stream, wherein the ratio of the Purple Pearl Formulation for Polyolefins
primary feed to the secondary feed is 60:40, 65:35, 70:30, or G2 Formula 65:35 Split 80:20 Split
75:25 by weight. As the ratio of the primary feed to secondary Component % of Total % of Total % of Total
feed increases, the loading of pigment also increases. As Violet Satin Pearl S.90 6.85 8.44
shown in Table 1, a 75:25 split results in a higher bulk density Violet Sparkle Pearl S.90 6.85 8.44
ofred pigment of approximately 42% higher loading than the Red Satin Pearl 4.72 S.49 6.75
G2 Formula. Pigment Blue 29 9.44 10.97 13.51
Pigment Red 122 1.13 1.32 1.62
Polymer Processing Aid 4.OO 4.64 5.72
TABLE 2 Dispersion Aid 4...SO 4.99 5.79
Mineral Oil 2.OO 2.32 2.86
Green Formulation for Polyolefins Slip Agent 1334 1549 19.07
PPFake S.OO 5.81 7.15
G2 60:40 65:35 70:30 75:25 80:20 PP Peets 44.06 3S.OO 2O.OO
Formula Split Split Split Split Split Pigment Loading v. Standard 100% 11.2% 142%
% of 90 of 90 of 90 of 90 of 90 of
Component Total Total Total Total Total Total
I0088 Table 3 illustrates the pigment loading for a Purple
Pigment Yellow 194 S.09 S6S 6.13 6.60 7.07 7.54 Pearl Formulation for Polyolefins of various masterbatch
Pigment Green 17 16.30 18.11 1961. 21.12 22.63 24.14
Pigment Green 7 18.28 20.30 22.OO 23.69 25.38 27.07 compositions formed from a split stream, wherein the ratio of
Pigment Black 7 O.35 0.39 O.42 0.46 0.49 0.52 the primary feed to the secondary feed is 65:35 or 80:20 by
Dispersion Aid 4.OO 4.44 4.81 5.18 555 5.92 weight. Similar to the above described Tables 1 and 2, as the
Polymer Processing Aid 7.OO 6.48 7.02 7.56 8.1O 864 ratio of the primary feed to secondary feed increases, the
PE Flake
PE Pelets
S.OO
43.97
4.63 S.O1 S.40 S.78 6.17
40.OO 3S.OO 3 O.OO 2S.OO 20.OO
loading of pigment also increases. As shown in Table 3, an
Pigment Loading v. 100% 11.1%. 120%. 130%. 139%. 14.8%
80:20 split results in a higher bulk density of purple pigment
Standard of approximately 42% higher loading than the G2 Formula.
I0089. The blend containing an 80:20 split includes
approximately 58% active ingredients (e.g. pigments and slip
US 2016/0017144 A1 Jan. 21, 2016

agent), including approximately 19% slip agent. Due to the embodiments disclosed, but that the teachings described
reduced L/D for the primary extruder there is a brighter herein are capable of numerous rearrangements, modifica
appearance and less reduction of particle size for the Purple tions and Substitutions.
Pearl compared to the G2 Formula as run on a conventional 1. A process for making a highly loaded and well-dispersed
masterbatching twin screw. masterbatch composition from a split stream process com
prising the steps of:
TABLE 4 a) mixing a colorant in a mixture in a primary feed;
Yellow Formulation for Polyolefins b) pre-melting a thermoplastic carrier in a secondary feed;
and
G2 Formula 60:40 Split 70:30 Split c) combining the mixture of the primary feed and the
Component % of Total % of Total % of Total melted thermoplastic carrier of the secondary feed to
Pigment White 6 0.55 1.18 1.38 form the masterbatch composition.
Pigment Yellow 109 5.51 11.77 13.73 2. The process of claim 1, wherein the mixing step includes
Pigment 110 5.51 11.77 13.73 an additive in the primary feed, the secondary feed, or a
Solventyellow 33 4.41 941 10.99
Dispersion Aid 2.10 4.48 5.23 combination thereof.
SANPowder 1O.OO 21.38 24.94 3. The process of claim 1, wherein the mixing step includes
ABS Pellets 71.93 40.OO 30.00 a metallocene polymer processing aid in a primary feed,
Pigment Loading v. Standard 100% 21.2% 24.8% wherein the metallocene polymer processing aid is a polyole
fin.
0090 Table 4 illustrates the pigment loading for a Yellow 4. The process of claim 1, wherein the metallocene poly
Formulation for Polyolefins of various masterbatch compo mer processing aid is an amorphous metallocene polypropy
sitions formed from a split stream, wherein the ratio of the lene copolymer obtained by polymerizing a propylene mono
primary feed to the secondary feed is 60:40 or 70:30 by mer with about 2-15% ethylene comonomer in the presence
weight. Similar to the above described Tables 1, 2, and 3, as of a metallocene catalyst.
the ratio of the primary feed to secondary feed increases, the 5. The process of claim 1, wherein the metallocene poly
loading of pigment also increases. As shown in Table 4, a mer processing aid exhibits a density of about 0.87–0.93
70:30 split results in a higher bulk density of yellow pigment g/cm, a drop point of about 80-145° C., and a viscosity of
of approximately 48% higher loading than the G2 Formula. about 60-6300 mPas.
The blend containing a 70:30 split includes over approxi 6. The process of claim 1, wherein the combining step
mately 27% hard to disperse organic pigments, in addition to includes Supplying the secondary feed to a port located at the
approximately 11% dye. primary feed, upstream the primary feed, downstream the
0091. Each of the ratios described in Tables 3 and 4 have primary feed, or a combination thereof.
been verified by ash tests and by molding plaques. 7. The process of claim 1, wherein the combining step
0092. The masterbatch may be introduced to any compat includes an additive in the primary feed, the secondary feed,
or a combination thereof.
ible polymer and processed. It is understood that the master 8. The process of claim 7, wherein the additive is selected
batch composition of the present disclosure can be used for from the group consisting of antioxidants, ultraviolet light
coloring polymers formed into various shapes, such as sheet,
film, tube, bottles, containers, molded products and other absorbers, light stabilizers, flame-retardants, antibacterial
molded articles. The term processing is used herein to agents, Surface tension reducers, deodorizing agents, anti
describe the conversion of polymers into articles of a desired static agents, anti-blocking agents, plasticizer agents, fillers,
shape. Illustrative examples of processing are extrusion and blowing agents.
molding, injection molding, blow molding, compression 9. The process of claim 7, wherein the additive is about
molding and calendering. The addition of the masterbatch to 5-60% by weight.
the melt-processible polymer can be accomplished by any 10. The process of claim 7, wherein the additive comprises
means known in the art. It is possible to use the same methods an antioxidant about 0-15% by weight, a light stabilizer about
as for preparing the masterbatch itself. It is understood that 0-45% by weight, and an ultraviolet light absorber about
the masterbatch carrier polymer can be the same or different 0-45% by weight.
than the melt-processible polymer. The masterbatch compo 11. The process of claim 1, wherein the colorant is about
sition may be introduced and processed via a batch or con 15-80% by weight, the thermoplastic carrier is about 9-60%
tinuous process. In one illustrative embodiment, the master by weight, and the metallocene polymer is about 2-20% by
batch may be introduced to the melt-processible polymer and weight.
processed on a rubber compounding mill, simple kneader, or 12. The process of claim 1, wherein the colorant is selected
in a Banbury or other internal mixer or in a mixing extruder. from the group consisting of organic pigment, inorganic pig
Alternatively, the masterbatch can be metered to the feed ment, single pigment dispersion, dye, coated mica, powdered
section of an extruder by appropriate devices. Continuous aluminum, optical brightener, fluorescent, and phosphores
processes can be carried out, for example, in rapid mixers, Cent.
single-screw extruders, twin-screw extruders, Buss kneaders, 13. The process of claim 1, wherein the colorant comprises
planetary roll extruders, open double-trough kneaders or an organic pigment about 5-50% by weight.
rapid stirrers. Continuous processes are preferred. 14. The process of claim 1, wherein the colorant comprises
0093. Although the embodiments of the present teachings an inorganic pigment about 0-80% by weight.
have been described in the accompanying embodiments and 15. The process of claim 1, wherein the colorant comprises
in the foregoing detailed description, it is to be understood an organic pigment about 3-40% by weight and an inorganic
that the present teachings are not to be limited to just the pigment about 10-60% by weight.
US 2016/0017144 A1 Jan. 21, 2016

16. The process of claim 1, wherein the thermoplastic face tension reducers, deodorizing agents, anti-static agents,
carrier is selected from at least one of the following: anti-blocking agents, plasticizer agents, fillers, and blowing
homopolymers and copolymers of polyethylene, polypropy agents.
lene, polystyrene, polyoxymethylene, polyethylene tereph 21. A process for making a highly loaded and well-dis
thalate, polybutylene terephthalate, polymethyl methacry persed masterbatch composition comprising the steps of: a)
late, polyether Sulfones, polysulfones, polyether ketones, introducing a masterbatch composition formed from a split
polystyrene copolymers, acrylonitrile-butadiene-styrene ter stream process, as provided in claim 1, to a melt-processible
polymers, polyamides, polycarbonate, and combinations polymer to form a feed polymer composition, wherein the
thereof. masterbatch composition comprises a pigment, athermoplas
17. The process of claim 1, further comprising a dispersion tic carrier, and, greater than 5% to about 60% by weight of an
package. additive, wherein the additive is selected from the group
18. The process of claim 17, wherein a dispersion package consisting of antioxidants, ultraviolet light absorbers, and
is selected from the group consisting of waxes, metal salts, light stabilizers; and b) processing the polymer composition
coupling agents, and Surfactants. to form the masterbatch composition.
19. The process of claim 17, wherein the dispersion pack 22. Athermoplastic article produced using the masterbatch
age is about 2-8% by weight. composition formed from the process of claim 1.
20. The process of claim 1, further comprising at least one
of the following: flame-retardants, antibacterial agents, Sur k k k k k