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Patent 1150008 Summary

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(12) Patent: (11) CA 1150008
(21) Application Number: 1150008
(54) English Title: FINISHES FOR POLYPROPYLENE TEXTILE MATERIALS, PROCESS AND PRODUCT THEREOF
(54) French Title: APPRETS POUR TISSUS EN POLYPROPYLENE; PROCEDE D'UTILISATION ET PRODUITS OBTENUS
Status: Term Expired - Post Grant
Bibliographic Data
(51) International Patent Classification (IPC):
  • D06M 13/00 (2006.01)
  • D06M 13/148 (2006.01)
  • D06M 13/292 (2006.01)
  • D06M 16/00 (2006.01)
(72) Inventors :
  • TAYLOR, PETER A. (United States of America)
(73) Owners :
  • PHILLIPS PETROLEUM COMPANY
(71) Applicants :
  • PHILLIPS PETROLEUM COMPANY (United States of America)
(74) Agent: OSLER, HOSKIN & HARCOURT LLP
(74) Associate agent:
(45) Issued: 1983-07-19
(22) Filed Date: 1979-10-05
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
957,786 (United States of America) 1978-11-06

Abstracts

English Abstract


Abstract of the Disclosure
A finishing composition for improving the thermal stability of poly-
propylene textile materials; comprising, an ethoxylated textile lubricant, in
an amount sufficient to impart lubricating properties to said composition, and
an antistatic agent comprising phosphate esters, in an amount sufficient to
impart antistatic propertied to said composition and increase the thermal
stability of said polypropylene textile materials. Also disclosed is a process
for utilizing the finishing composition and the products thereof.


Claims

Note: Claims are shown in the official language in which they were submitted.


The embodiments of the invention in which an exclusive
property or privilege is claimed are defined as follows:
1. A finish composition, for application to textile materials,
melt spun from a polypropylene resin containing a stabilizing system including
a hindered phenol to improve the stability thereof, comprising:
a) an ethoxylated textile lubricant, in an amount sufficient to
impart lubricating properties to said composition; and
b) an antistatic agent comprising phosphate esters, in an amount
sufficient to impart antistatic properties to said composition and increase
the stability of said polypropylene textile materials.
2. A composition in accordance with claim 1 wherein the composition
additionally contains a minor amount of a bactericide in an amount sufficient
to impart antibacterial properties to the finish composition.
3. A composition in accordance with claim 1 wherein the
polypropylene melt composition for preparing the polypropylene textile
material is lightly stabilized.
4. A composition in accordance with claim 3 wherein the
polypropylene melt composition contains between about 0.1 and about 0.6 weight
percent of a stabilizer system.
5. A composition in accordance with claim 1 wherein the antistatic
agent is a phosphate ester.
6. A composition in accordance with claim 1 wherein the antistatic
agent is an at least partially neutralized salt of a phosphoric acid ester
which exhibits a pH sufficient to inhibit color formation in the polypropylene
textile material.
7. A composition in accordance with claim 6 wherein the pH is
between about 3 and about 9.
8. A composition in accordance with claim 6 wherein the phosphoric
acid ester is neutralized with a composition including ammonia.
19

9. A composition in accordance with claim 6 wherein the phosphoric
acid ester is neutralized with a material selected from the group consisting
of monoethanolamine, diethanolamine, triethanolamine, sodium
hydroxide, lithium hydroxide, ammonium hydroxide and mixtures thereof.
10. A composition in accordance with claim 1 wherein the phosphoric
acid ester is an ethoxylated alkyl phosphate ester.
11. A composition in accordance with claim 1, 2 or 3 wherein the
ethoxylated lubricant is present in a major proportion and the antistatic
agent is present in a significant proportion.
12. A process for preparing a polypropylene textile material
comprising:
a) melt spinning a polypropylene resin containing a stabilizing
system including a hindered phenol; and
b) applying to said polypropylene resin during the melt spinning
thereof, a finish composition; comprising, an ethoxylated textile lubricant,
in an amount sufficient to impart lubricating properties to said composition,
and an antistatic agent comprising phosphate esters, in an amount sufficient
to impart antistatic properties to said composition and increase the stability
of said melt spun polypropylene textile materials.
13. A process in accordance with claim 12 wherein the finish
composition additionally contains a bectericide in an amount sufficient to
impart antibacterial properties to the finish composition.
14. A process in accordance with claim 12 wherein the polypropylene
melt is lightly stabilized.
15. A process in accordance with claim 14 wherein the polypropylene
melt composition contains between about 0.1 and about 0.6 weight percent of a
stabilizer system.
16. A process in accordance with claim 12 wherein the antistatic
agent is a phosphate ester.

17. A process in accordance with claim 12 wherein the antistatic
agent is an at least partially neutralized salt of a phosphoric acid ester
exhibiting a pH sufficient to inhibit color formation in the polypropylene
textile material.
18. A process in accordance with claim 17 wherein the pH is between
about 3 and about 9.
19. A process in accordance with claim 17 wherein the phosphoric
acid ester is neutralized with a composition including ammonia.
20. A process in accordance with claim 17 wherein the phosphoric
acid ester is neutralized with a material selected from the group consisting
of monoethanolamine, diethanolamine, triethanolamine, sodium hydroxide,
lithium hydroxide, ammonium hydroxide and mixtures thereof.
21. A process in accordance with claim 12 wherein the phosphoric
acid ester is an ethoxylated phosphate ester.
22. A process in accordance with claim 12, 13 or 14 in which the
ethoxylated lubricant is present in the finish composition in a major
proportion and the antistatic agent is present in said finish composition in a
significant proportion.
23. A process in accordance with claim 12, 13 or 14 wherein the
melt spun polypropylene is formed into a yarn and the yarn is draw-twisted.
24. A melt spun yarn product of improved stability, comprising; a
plurality of melt spun filaments formed from a polypropylene resin melt
containing a stabilizing system including a hindered phenol and having applied
thereto, during the melt spinning thereof, a finish composition; comprising an
ethoxylated textile lubricant, in an amount sufficient to impart lubricating
properties to said composition, and an antistatic agent comprising phosphate
esters, in an amount sufficient to impart antistatic properties to said
composition and to increase the stability of said melt spun polypropylene.
21

25. A product in accordance with claim 24 wherein the finish
composition additionally contains a bactericide, in an amount sufficient to
impart antibacterial properties to said composition.
26. A product in accordance with claim 24 wherein the polypropylene
melt which is melt spun is lightly stabilized.
27. A product in accordance with claim 26 wherein the polypropylene
melt composition contains between about 0.1 and about 0.6 weight percent of a
stabilizer system.
28. A product in accordance with claim 24 wherein the antistatic
agent is an at least partially neutralized salt of a phosphoric acid which
exhibits a pH sufficient to inhibit color formation in the polypropylene
textile material.
29. A product in accordance with claim 28 wherein the pH is between
about 3 and about 9.
30. A product in accordance with claim 28 wherein the ester is
neutralized with a neutralizing composition including ammonia.
31. A product in accordance with claim 28 wherein the phosphoric
acid ester is neutralized with a material selected from the group consisting
of a monoethanolamine, diethanolamine, triethanolamine, sodium hydroxide,
lithium hydroxide, ammonium hydroxide and mixtures thereof.
32. A product in accordance with claim 24 wherein the phosphoric
acid ester is an ethoxlated alkyl phosphate ester.
33. A product in accordance with claim 24, 25 or 26 wherein the
ethoxylated lubricant is present in a major proportion and the antistatic
agent is present in a significant proportion.
34. A product in accordance with claim 24, 25, or 26 wherein the
yarn product is a draw-twisted, melt spun polypropylene.
22

Description

Note: Descriptions are shown in the official language in which they were submitted.


27440
FINISHES FOR POLYPROPYLENE TEXTIIE MATERIALS,
PROCESS AND PROD~CT THEREO~ -
Background of tbe Invention
The present invention relates to an improved finishing composition
for filaments, yarns and other textile ma-terials. The present invention
further relates to an improved process for utilizing the novel finishing
composition and the textile products thereof.
In the formation of textile materials from melt spun polypropylene it
is normally necessary to apply a finishing composition to the filaments, yarns
and other textile embodiments thereof to make such materials more amenable to
the various operations to which they are subjected during processing, for
example, spinning, winding, yarn-forming, weaving, knitting, etc., and to
improve the properties of the finished products. In the processing of the
textile materials, the finishing composition is intended to reduce friction
between the yarn and various pieces of equipment with which it comes into
contact, such as guides, rollers and the like, and in both the processing and
use of the textile materials to reduce friction between the fibers themselves,
to prevent fiber and yarn breakage and to minimize excessive attraction or
repulsion of the filaments caused by electrostatic charges. Accordingly, such ~-
finishing compositions usually contain a lubricant and an antistatic agent.
~arious other additives such as bactericides, corrosion inhibitors, etc. may
also be added to the finishing composition.
However, it has been found that not all thermoplastic materials
respond to finishing compositions in the same manner, not all combinations of
finishing agents are compatible with one another and not all finishing agents
are compatible with stabili7ers and the like added to the thermoplastic melt.
Specifically, it has been found, in accordance wlth the present invention, that
polypropylenes do not respond to certain lubricants in the same manner as other
thermoplastic fiber-forming materials, particularly when the polypropylenes
contain less than the normal amounts of stabilzing agents, such as

antioxidants, or when they contain specific types of stabilizing agents. By
less than normal amounts of stabilizers is meant polypropylene containing from
about 0.1 to about 0.6 weight percent total stabilizers. It has also been
found that certain textile lubricants have an antagonistic effect on certain
stabilizers included in polypropylene melts.
It is therefore an object of the present invention to provide an
improved textile finish composition, a process utiliæing the same and the
products thereoi. A further object of the present invention is to provide an
improved textile finish composition including a textile lubricant and an anti-
static agent, a process utilizing the same and the products thereof. Yetanother object of the present invention is to provide an improved textile
finish composition which is useful in the treatment of polypropylene textiles,
a process for the utilization thereof and the products thereof. ~nother and
further object of the present invention is to provide an improved textile
finishing material for treatin8 polypropylene textiles containing certain
types of antioxidants, a process utilizing the same and the products thereof.
Yet another object of the present invention is to provide an improved finish
composition adapted to improve the thermal stability of polypropylene
textiles, a process for utilizing the same and the products thereof. A still
fur-ther object of the present invention is to provide an improved textile
finish composition adapted to improve the thermal, light and/or color stability
of polypropylene textile materials, a process for utilizing the same and the
products thereof.
These and other object of the present invention will be apparent from
the following description.
Summary of the Invention
In accordance with the present invention a textile finish
composition is provided for improving the stability of polypropylene textile
materials comprising, an ethoxylated textile lubricant, in amounts sufficient
to impart lubricating proper-ties to the composition~ and an antistatic agent
comprising phosphate esters, in an amount sufficient to impart antistatic

properties to the composition and increase the stability of the polypropylene
textile materials. In a more specific aspect, the improved finish composition
is particularly effective in the treatment of polypropylene textile materials
containing less than the normal amounts of stabilizers and still more
specifically stabilizers including hindered phenols. The method of preparing
an as-spun polypropylene textile material includes melt spinning a
polypropylene, particularly a polypropylene melt containing a hindered phenol
antioxidant, applying the specified finish composition to the filamentary
materials, forming a yarn from said filamentary materials and packaging the
yarn. The yarn may also be draw~twisted before or after the packaging of the
yarn. Such draw-twisted yarns may be woven into products particularly suitable
for use as dye bags, laundry bags, and the like.
Brief Descriptlon of the Drawings
FIGURE 1 of the drawings illustrates the process for preparing an as-
spun yarn in accordance with the present invention and FI&URE 2 illustrates one
embodiment of a pro~ess for draw-twisting the yarns produced by the process of
FIGURE 1.
Detailed Description of the Invention
Ethoxylated lubricants have heretofore been found to be highly
superior ~o conventio~al textile lubricants, particularly when utiliæed in
finish compositions for treating melt spun thermoplastic materials and
particularly polypropylenes. Accordingly, it is highly desirable to utilize
these synthetic lubricants in the inish composition. However, it has been
found in accordance with the present invention that melt spun polypropylene
textile materials are in some way deleteriously affected by the use of
ethoxylated textile lubricants. Specifically, it has been found that the
ethoxylated textile lubricants have a tendency to reduce the thermal, light
and/or color stability o the textile materials both during the processing
thereof and in the end products produced. This has been found to be
particularly true when the polypropylenes melts have been stabiliæed by the
inclusion therein of a stabili~er system including a tris-~4-

hydroxybenæyl)isocyanurate, a substituted pentaerythritol diphosphite, atrihydrocarbyl thiophosphite and optionally a thiomethylene phenol. It has
further been found that, when hindered phenols are included in stabilizer
systems for the polypropylene melt, some antagonistic reaction occurs between
an ethoxylated lubricant and the hindered phenol which results in decreasing
the thermal, light and/or color stability of the textile products.
It has been found, in accordance with the present invention, that, by
including significant amounts of at least one phosphate ester in a textile
finish composition containing an ethoxylated lubricant, the stability of poly-
propylene textile materials can be substantially improved. It has also beenfound that, in many cases, the color stability of such polypropylene textile
materials can also be improved by the speci-fied combination of synthetic
lubricant and antistatic agent. The finish composition optionally, but de-
sirably, contains minor amounts of a bactericide and may also contain minor
amounts of other known additives such as corrosion inhibitors and the like.
In accordance with one embodiment of the present invention, a poly-
propylene melt, particularly including minor amounts of a stabilizing sys-tem
and still more particularly a stabilizing s~ystem including at least one
hindered phenol, is melt spun, the subject combination of synthetic lubricant
and antistatic agent is applied thereto, the filamentary materials are formed
into a yarn and the yarn is then wound up to form a package. While the novel
finish composition may be applied to the textile materials at any time during
the processing thereof, it is preferably applied to the filaments as soon as
they have set, so that the full benefit of the stabilizing properties thereof
can be realized during the later processing thereof. Thus, in accordance with
this embodiment, there is produced as-spun polypropylene yarns of highly
improved thermal stability and in many cases of improved light and/or color
stability.
In a preferred embodiment of the present invention, the yarns thus
produced are draw-twisted and again packaged. The draw-twisting can also be
applied in a continuous process prior to the initial winding or packaging of

the yarn. The draw-twisted yarns have been found to be highly effective ~or
the production of dye bags, laundry bags and the like when woven and formed
into appropriate articles.
The thermoplastic tex-tile materials to which the present invention
is particularly direc-ted are homopolymers of propylene and copolymers of
propylene and another aliphatic l-olefin cont~ining 2 to 8 carbon atoms, in
which the comonomer constitutes up to about 20 mol percent of the copolymer.
The synthetic lubricants utilized in accordance with the present
invention include any of the known ethoxylated lubricants such as polyethylene
glycols, mixed polyethylene-polypropylene glycols, monoalkyl esters of mixed
polyethylene-polypropylene glycols, ethoxylated esters of fatty acids, rosin
acids and tall oil acids, ethoxylated castor oils, ethoxylated hydrogenated
castor oils, etc. More specifically, the ethoxylated lubricants includes,
ethoxylated aliphatic alcohols, ethoxylated alkylphenols, ethoxylated sorbitan
(anhydrosorbitol) esters, ethoxylated sorbitol esters, ethoxylated glycerol
esters, ethoxylated pentaerythritol esters, ethoxylated fatty acids,
ethoxylated fatty acid amides, ethoxylated-propoxylated fatty acids,
ethoxylated-propoxylated fatty acid esters, ethoxylated-propoxylated castor
oils, ethoxylated-propoxylated hydrogenated castor oils, ethoxylated-
propoxylated aliphatic alcohols, ethoxylated-propoxylated alkyl phenols, etc.
Presently preferred ethoxyla-ted lubricants include the random co-
polymers of the monobutyl ether of poly(oxyethylene-oxy-1,2-propylene) having
viscosities in terms of Saybolt Universal Seconds (SUS) at 100F (38C) ranging
from about 170 to about 5100 and even more preferably from about 250 to about
3500, the methyl ether of poly(oxyethylene-oxy-1,2-propylene) laurate wherein
the number of moles of combined ethylene oxide is about 7 and the number of
moles of combined propylene oxide is about 2, and the isododecyl
ether/poly(oxyethylene) adduct wherein the number of moles of combined
ethylene oxide is about 6 per mole hydrophobe.
A more complete description of the ethoxylated lubricants is given in
Kirk-Othmer, Encyclopedia o~ Chemical Technology, 2nd Edition 19, 531-554

(1969). A more complete description of the polyethylene glycols, etc. is
given in volume 10, pages 65~-659 of the reference encyclopedia.
When the polypropylene melt composition includes a stabilizing
system having a hindered phenol, the hindered phenols are utilized as thermal
stabilizers or antioxidants. Such materials are known in the art. Typical of
such stabilizers are 2,6-di-t-butyl-4-methylphenol (BHT); octadecyl[3-(3,5-di-
t-butyl-4-hydroxphenyl)] propionate (Irganox 1076, a trademark of Ciba-Geigy
Chemical Co.); tetrakis[methylene(3,5-di-t-butyl-4-hydroxhydrocinnimate)]
methane (Irganox 1010, a trademark of Ciba-Geigy Chemical Co.), di-n-octadecyl
(3,5-di-t-butyl-4-hydroxybenzyl) phosphonate; 1,3,5-trimethyl-2,4,6,-tris
(3,5-di-t-butyl-4-hydroxybenzyl) benzene and the like. Such thermal
stabilizers are generally added to the propylene melt composition in amounts
of from about 0.01 to about 1.0 part by weight per 100 parts by weight of -the
polymer (phr).
The phosphate-type antistatic materials utilized in accordance with
the present invention include hydrocarbyl phosphate esters, ethoxylated hydro-
carbyl phosphate esters, partially hydrolyzed hydrocarbyl phosphate esters or
their salts. By hydrocarbyl is meant a hydrocarbon radical selected from the
alkyl, cycloalkyl, aryl and combinations thereof such as alkylauryl~ etc., con-
taining from 1 to about 20 C atoms. Usually a mixture of di- and monoalkyl
esters are utilized but the composition is also effective when completely
esterified phosphoric acid compounds are employed. It has also been found -that
the use of the phosphate-type antistatic agents of the present invention are
are quite effective in inhibiting color formation during gas fired heat treat-
ments if the polypropylene melt composition contains a hindered phenol as an
antioxidant. It hs further been found that the inhibition of color formation
is influenced by the pH and the neutralizing cations employed. The lower the
pH the less color produced. Preferably, the pH is maintained be-tween abou-t 3
and about 9 and preferably between about 4 and about 7. The preferred phosphate-
type antistatic materials are the partially neutralized acid esters ofphosphoric acid or the equivalen-t partially hydrolyzed triesters of phosphoric
acid. The present order of neutralizing cations has been found to be ammonium

mono-, di- and triethanolammonium, lithium, sodium and potassium. The
potassium was found to be the least desirable, although useable in accordance
with the present invention.
The finish composition of the present invention also desirably
contains a bactericide such as 6-acetoxy-2,4-dimethyl-m-dioxane (Givgard
DXN~R), Givaudan Corp., Clifton, NJ).
The relative amounts of the ingredients of the finish composition of
the present application are not particularly critical. However, the
ethoxylated lubricant should of course be used in amounts sufficient to
lubricate the textile materials and the antistatic agent in amounts sufficient
to prevent undesirable electrostatic charges from building up in the textile
materials. Preferably, the ethoxylated lubricant is utilized in amounts
between about 50 and about 98 percent by weight of the finish composition and
most desirably between about 60 and 95 percent by weight of the composition.
The balance of the finish composition is pre~Eerably the antistatic agent in
amounts between about 2 and 50 percent by wei.ght and most desirably between
abont 5 and 40 percent by weight of the finish composition. The bactericide
may be present in amounts between about 0 and about 1.0 percent by weight of the
final composition and like minor amo~mts of other suitable additives may be
included, such as corrosion inhibitors.
A preferred embodiment of the present invention will be illustrated
by reference to the accompanying drawings.
In accordance with FI~URE 1, the polypropylene melt is extruded from
a plural orifice spinneret 2, of conventional design. While spinneret 2 is
shown in the drawings as producing a single threadline it is obvious that the
spinneret may produce two or more threadlines. The filaments from spinneret 2
are passed through a conventional quench zone 4 where the filaments are cooled
and set. Finish is applied by conventional finish applicator means 6 which may
take any appropriate form. For example, a "kiss" roll may be utilized to apply
finish to the filaments as a gathered threadline or yarn or as a band spread
across the finish roll. A slot type finish applicator could also be utilized,

the only requirement being that the finish be uniformly applied to the
filaments or yarn. The yarn is then wound on an appropriate conventional
winder 8 to form a yarn package 10. Appropriate guides, guide rolls, godet
rolls, and the like will of course be utili~ed. The process as illustrated in
FIGURE 1 produces a yarn in its as-spun state. However, it is also possible to
draw-twist the yarn before winding the same on package 10. Whether draw-
twisting is practiced as a part of the spinning operation will depend to some
extent upon whether the yarn is partially oriented yarn or a conventional
undrawn yarn. Normally it is considered that winder takeup speeds in excess of
about 1500 meters per minute will produce a partially oriented yarn whereas
takeup speeds of less than about 1500 meters per minute, for example about 800
meters per minute, produce an unoriented or undrawn yarn.
FIGVRE 2 illustrates a preferre~ draw-twisting operation in
accordance with the present invention. In FIGURE 2 yarn is withdrawn Erom yarn
package 10 by means of the draw means 12 made up of conventional draw rolls, 12a
and 12b, respectively. Thereafter, twist means 14 conventionally applies a
twist LO the drawn yarn. In the speciEic embodLment shown, twlst ls applled by
mea~s oi a flyer 16 as it is wound on package 18. Obviously any appropriate
drawing and twisting apparatus may be utilized. It will also be apparent to
one skilled in the art that the system would include appropriate guides, guide
rolls, draw heaters, etc.
The draw-twisted yarn when converted into an appropriate fabric and
formed into a bag or the like has been found to make excellent dye bags, laundry
bags and the like. The resultant products have superior temperature stability
compared with conventionally finished textile materials of polypropylene and
to conventional dye bag textiles. In addition, certain of the polypropylenes
have been found to have superior inhibition to color formation as compared with
conventionally finished polypropylenes and commercially available dye bag
textiles.
The following examples will illustrate the advantages of the present
invention.

p~ :
Example 1
The following series of tests were run to illustrate the thermal
stability benefits of the combination of ethoxylated lubricant and phosphate-
type antistatic agent in accordance with the prese~t invention. In this series
of tests a commercial resin having a melt flow of about 12 had added thereto the
finish compositions indicated in TabIe 1 below. Yarns, to which the designated
finishes had been applied, were tested for thermal stability by knitting
sleeves from the yarns, about one and one-half inches by two inches, and
placing the sleeves on wooden dowel rods in an electrically heated, forced air
oven at 130C. The specimens were examined periodically (typically every 24
hours) until the degradation appeared substantial. The number of hours until
degradation of the sample is given in Table 1 below.
Table 1
Wt. ~ Solids
Based on Wt.~ours to
Run Finishof Yarn Degradation
. _ .
1 Lubricant( ) 4.0 31
2 Lubricant(a)~20%
hexyl phosphate 3.6 230
3 ~ubricant(a)+20h
ethoxylated lauryl
phosphate 4.0 140
4 Multico~ onent
~inish ~.5 77
(a) Butyl ether of random copolymer, poly(oxyethylene-oxy-1,2-
propylene) having SUS viscosity of 260 (Union Carbide Co.~.
(b) 90 wt. % ethoxylated coconut acid ~9 moles ethylene oxide per
mole acid); 10 wt. % ethoxylated coconut amino ethanolamide
(3 moles ethylene oxide per mole coconut derivative) - com-
mercially available ethoxylated lubricants.
Example 2
The stability of polypropylene yarns with and without-the phosphate-
type antistatic agents was determined in laundering cycle tests in the present
example.
In this test, a polypropylene melt composition was prepared by adding
to the polypropylene 0.05 parts by weight per 100 parts of polypropylene (phr~

of calcium stearate, 0.3 phr tris(3,5-di-t-butylhydroxybenzyl)isocyanurate,
0.1 phr hydrolysis resistant distearyl pentaerythritol disphosphite, 0.1 phr
trilauryl trithiophosphite and about 0.375% titanium oxide. The polypropylene
had a melt flow of 12 and when combined with the specified stabilizing system
is designated hereinaf-ter as resin B.
The finish designated in Table 2 below as finish I con-tains the
followil1g:
90 wt. % ethoxylated coconut acid (~ moles ethylene oxide per mole
acid)
10 wt. % ethoxylated coconut amino ethanolamide (3 moles ethylene
oxide per mole coconut derivative) - commercially available
ethoxylated lubricants.
The finish designated as finish II contains the following:
Lubricant
32.15~ methyl ether of poly(oxyethylene- [7 moles] oxy-1,2-
propylene [2 moles] laurate ~TL lO38, a trademark of Imperial
Chemical, Inc.~
32.15% poly(oxyethylene [6.5 moles] isodecyl alcohol ether
(TL 1074, a trademark of Imperial Chemical, Inc.)
1~.4% butyl ether of random copolymer, polytoxyethylene-oxy-
1,2-propylene) having SUS viscosity of 2000 (Union Carbide Co.)
Antistatic Agent
13.19% mixture of di- and mono-hexyl phosphoric acid
(G2199, a trademark of Imperial Chemical, Inc.)
2.05% NaOH
0.96% diethanolamine
Bactericide
0.1% 6-acetoxy-2,4-dimethyl-m-dioxane
(Givgard DXN, a trademark of Givaudan Corp., ~lifton, N.J.)
The specified finishes were applied to the yarns at essentially -the
same rate as Example 1 above.
In the test, the yarn was knitted into a sleeve and the sleeve
trimmed so that the yarn could be easily unravelled for sampling. The sleeve,
weighing about 5 grams, was placed in a 500 millili-tter, flat bottom flask
fitted with a water cooled reflux condenser. 200 miililiters of a 0.2~ ~ATCC
Standard Soap Solution was bo:iled under reflux for 6 hours after which time the
sleeve was removed, rinsed free from the solution and squeezed dry. The sleeve
was then dried for 15 hours at 130C in an electrically heated, forced air oven
to complete the cycle. About a 5 foot sample of the yarn was removed from the
sleeve and tested for strength and elongation retention on an Instron Tensile
Tester after 3, 5 and 8 cycles, respectively.

The results of this test are set forth in Table 2 below:
Table 2
Cycles to% Strength Retention
Run Resin Finish Failure Af-ter 8 Cycles
B + TiO2 I < 3 _ ;
6 B + TiO2 II > ~ 103
~xample 3
The ultraviolet stability of the polypropylene yarns referred to in
Table 2 above was also tested.
lQ The ultraviolet stability was measured by exposing 2" by 3" knitted
sleeves mounted on black bac~ed ~tlas mounting fadeometer cards. Degradation
is either when the fabric tears or when the fabric flakes while being gently
scratched with a fingernail. Usually if the ~:leeve is of fine denier yarn the
fabric will tear and it is the sleeve surface closest to the black backing
which tears before the surface closest to the arc. With heavier denier fabrics
flaking of the surface facing the arc usually occurs before the fabric can be
torn. Table 3 below gives the results of these tests.
Table 3
Hours to Hours to
Run Resin Finish Flaking Break
7 B + TiO2 I 120 260
8 B + TiO2 II 260 >300
It is obvious from the above examples that finishes containing an
ethoxylated lubricant and the phosphate-type antistatic agen-ts, in accordance
with the present invention, (finish II) were vastly superior to finishes
containing only ethoxylated lubricants and balanced finishes containing the
ethoxylated lubricants and antistatic agents other than the phosphate-type
antistatic agents utilized in accordance with the present invention, which
other lubricant compositions have been highly successful as finishes for other
textile materials.

Example 4
In this example the finish compositions of the present invention were
tested for use as dye bag yarns. The yarns were made from a stabilized poly-
propylene melt designated resin B in the above examples and were finished with
either finishes -~ or II as specified in the previous examples. The finish was
metered onto the yarn with no problems. The yarn was draw-twisted using a
standard 1680/280 yarn process. Eight positions of a draw twister processing
1680/280 yarns were used. Again no problems were seen. The yarns were then
coned into ten ounce packages and knitted into dye bags for testing.
The following tes-ts were made:
Stability to up to 8 cycles of an accelerated mock
dyeing test
Stability up to 8 cycles of an accelerated laundering
test
Stability to C-Arc fadeometer exposure test
Stability to GMC-Arc fadeometer ex]posure test
Accelerated gas fade color developlnent test
~ATCC gas fade color development tlest
In addition to testing yarn with finish II of the present invention and -the
yarn with finish I as a control, in some cases competitive dye bag yarns,
designated C, were tested for comparison.
The mock dye cycle test is the same as the previously described
laundering cycle test except that the treating solution was 200 milliliters of
the following:
0.3~ Alkanol ND (a trademark of Dupont) - sodium alkyl diaryl sulfonate
0.16% Merpol OJS (a trademark of Dupont) - ethylene oxide condensate
0.3% MSP - monosodium phosphate
The GMC-Arc fadeometer exposure test was substantially the same as
the previously described carbon arc fadeometer test.
The accelerated gas fade color development test simulates processes
wh:ich involve heating and curing or drying in gas fired ovens. I-t also
produces colors which have been seen transiently under the same kinds of
; 12

storage conditions which have not heretofore been simulated. The test provides
for a 10 minute heating cycle at 130C followed by a 2-hour treatement in an
atmospheric fume chamber (AATCC test method 23-1975).
The regular gas fade test is described in AATCC test method 23-1975.
The results were recorded and the percent toughness retained was
calculated for each sample. The toughness is defined as:
Toughness = Tenacity x ~% Breaking Elongation)l/2
The results of this series of tests are set forth in Tables 4, 5, 6
and 7 below:
l3

a)
In _1
J' co u ~ o o
~ ~ ~ u ~ ~ o
E~ ~ o~ O
h U H
aJ O
~ X
'W ~
U
oo U7
~d ~1
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C~
a) ~ rl
CJ cr~ r~
. ~ ~ r~
O ~ U~
C~ ~ 00
~ o~ I ~
C~ ~ ;:
~ O
0 ~ ~ ~ O 0 00
d
h a) ~ ~ ~1 0
?~ u~ t~ gu~
F4 ~d
p~
O U~
.,~ )
4~ J~ ~
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~J U~ H E-l
,1 a)
~ .~ ~ ~1 o o
~ ~ ~ O
P~ ~ I ~O
~1 rl C'
C~
U ~ U~ O O
~1 lCs~ O oc)
~1 ~; ~
O
~rl
~1
~ c~ ~1
a) ta
.C ~0
~ a~
~1 H O
H H ,~
a
a~
o .,, .,~
F4 0 ~ C
a ~ a-- a~
U~ ~ O
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O~ DO ~ I
00 ~ ~ C~

g
0 ~ ~ ~ l`
~ ~o
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:~ o f
c~ ~
s~ ~a
a) r
~ ~ oo o ~o
¢ 1~ h
a) u ~D bO ~D00 C`l
.
U~
0 ~ .
~t C`l ~` 00
~I g
~0 U~ ~
1 h ~a
~ ~\ ~
P~ ~ ~0 ~O ~ ~ C~ O ~D
0 ~ ~ ~ ~ CS~
:~ C) U 1~ ~ ~ t
O U~ ~ ~ ~ ~
~1 P
O
o 0 ~
O 0 ~0 ~t ~t ~) ~D O
~rl ~1 1:: ~ ~ ~1
~ 1~ P~l
bf C~ ~
~ ~ ~i#
u~ ~ ~ a~ ~
~ ~ ~ bO ~ 00 ~t CO ~OCO
O ~ n~ cl ~ ~ o ~t Ln ~t ~ 0
~1 ~1 O ~ 1~ ~t ~ 00
~ ~ ,C ~ ~
h g
.,u V~
~d a ~ ~ a~ ~ oo ~
3~ .~ ~ 1~ ~ C~ I~ o o
~; ~ ~1
~o
rl
U
4~ oo ~ o C`l I~ o
a ~ o ~
0
U~
U
~o o
H H a H H ,~
H H
~Q~ FL~ O F~ m O ~ O
P~,1 a ~ ~ a ~ a ,~
rl O E~ ~O (L~
~t ~ ~0 O P~ I ~ O ~ O ~t h I
p~ ~ O ~ ~ C~

f.~
Table 6
Commercial Dye Bag Yarns
Number of ~aundering Cycles to Degradation
Commercial Dye % Cycles
Denier~ag Yarn ~inishto Failure
lS5/35 C Unknown 7
210/35 C Unknown 5
840/140 C Unknown 4
Table 7
Gas Fading of Dye Bag Yarns
Accelerated
Yarn ~inish 1 Cycle 2 Cycle 3 Cycle Gas Fade
Resin B II 4-5 3 2 4-5
~40/140
Commercial Unknown 4-5 3 2 4-5
Dye Bag Yarn C
165/35
Commercial Unknown 4 3-4 3 4-5
Dye Bag Yarn C
840/1~0
The above results are analyzed below.
Selection of commercial dye bag yarn C having a 165/35 denier for the
quanitative strength retention test was made on the basis of launderin~ cycle
tests in which three commercial dye bag yarns from the same manufacturer were
cycled to failure. The commercial yarn having a denier of 16S/35 was found to
be the most stable of the three yarns tested ~see Table 6 above).
In the quantitative dyeing/lsundering simulations it is the
elongation which is most rapidly affected, the toughness factor is used as the
critical criterion because it balances the elongation and the tenacity into a
property which has been found to be the equivalent to performance in actual
practice.
Although the color of the yarns has not been quantitatively
evaluated, the dye bag yarns in accordance with the present invention are
whiter than the control yarn and than the commercial dye bag yarn; it remains
whiter in the cycling test, the thermal stability tests and in actual

~ ~ r~
laboratory storage experiments. Accelerated gas fade tests showed no pinking
problems with the dye bag yarns of the present invention and no such problems
have been observed with the control yarns. In 3-cycle gas fade tests, the
yarns show quite a severe color development. However, this is not believed to
be a problem in dye bag yarns since the only place it will show up is after long
storage in a high nitrogen oxide atmosphere. The dye bag yarns would not be
subjected to such an environment since legislation has essentially ruled out
this kind of contamination.
Example 5
Tests were also conducted utilizing a 12 melt flow polypropylene melt
composition stabi]ized with 0.30% distearylthiodipropionate, 0.10% tetrakis-
[methylene(3,5-di-t-butyl-4-hydroxy hydrocinnimate)] methane and 0.05% calcium
stearate and a 12 melt flow polypropylene having a stabiliæer system;
comprising, 0.30% distearylthiodipropionate, 0.10~ tetrakis[methylene(3,5-di-
t-butyl-4-hydroxy hydrocinnimate)] methane (Irganox 1010, Ciba-Geigy), 0.05%
calcium stearate and 0.10% hydrolysis resistant distearyl pentaerythritol
diphosphate Weston 619, a product of Borg-Warnler Chemicals, Parkersburg, W. Va.
Both of the stabili~ing systems utilized in tlle polypropylene melt composition
are seen to contain hindered phenols. It was found that about 2% of an
ethoxylated textile lubricant applied to these textile materials will reduce
the thermal stability at 130C from 400 hours to 60 hours or from 1500 hours to
200 hours depending on the denier of the product. However, the presence of
about 10~ to 50% of the phosphates of the present invention and the same
ethoxylated lubricants the textile materials recover substantially all of the
strength thus lost.
It was also found that a further benefit from the use of the finish
compositions of the present invention is attained when the polypropylene melt
composition contains a hindered phenol. Specifically, inhibition of color
~formation during gas fired heat treatments is improved. For example, yarns
spun from resin formulations B and C above when heated to 130C and exposed for
2 hours in a nitrogen oxide gas Eade oven will turn pink. This pink color will

be increased in the presence of an ethoxylated textile lubricant-containing
finish unless the finish has added thereto a phosphate type antistatic agent as
taugh-t in the present invention.
While specific examples, materials and amounts of ingredients have
been set forth in the illustrative examples, it is to be understood that such
specific references are not to be considered limiting and variations thereof
will be apparent to one skilled in the art.

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Event History

Description Date
Inactive: IPC from MCD 2006-03-11
Inactive: IPC from MCD 2006-03-11
Inactive: IPC from MCD 2006-03-11
Inactive: First IPC assigned 2000-10-20
Inactive: Expired (old Act Patent) latest possible expiry date 2000-07-19
Grant by Issuance 1983-07-19

Abandonment History

There is no abandonment history.

Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
PHILLIPS PETROLEUM COMPANY
Past Owners on Record
PETER A. TAYLOR
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Claims 1994-01-25 4 142
Cover Page 1994-01-25 1 14
Abstract 1994-01-25 1 15
Drawings 1994-01-25 2 25
Descriptions 1994-01-25 18 629