Stock material or miscellaneous articles – Coated or structually defined flake – particle – cell – strand,... – Rod – strand – filament or fiber
Reexamination Certificate
1998-09-10
2001-02-13
Krynski, William (Department: 1774)
Stock material or miscellaneous articles
Coated or structually defined flake, particle, cell, strand,...
Rod, strand, filament or fiber
C428S397000, C428S398000
Reexamination Certificate
active
06187437
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to processes for forming multilobal filaments of a thermotropic liquid crystalline polymer. Specifically, the present invention provides processes for forming as-spun and heat-treated high denier multilobal filaments of a variety of thermotropic liquid crystalline wholly aromatic polyesters and polyesteramides. This invention also relates to as-spun and heat-treated high denier multilobal filaments of thermotropic liquid crystalline polyesters and polyesteramides.
2. Description of the Prior Art
Thermotropic liquid crystalline polymers (LCPs) are an important class of polymers, which are generally wholly aromatic molecules containing a variety of heteroatom linkages including ester and/or esteramide linkages. Upon heating to sufficiently high temperature, LCPs melt to form a liquid crystalline melt phase (often referred to as “anisotropic phase”) rather than an isotropic melt. Generally, LCPs consist of linear (“rigid rod”) molecules that can line up to yield the desired liquid crystalline order. As a result, LCPs feature low melt viscosity and thus improved performance and processabilities.
Because LCPs orient to form “rigid rod” linear molecules, LCPs exhibit extremely high mechanical properties. Thus, it is well known in the art that LCPs can be formed into shaped articles, such as films, rods, pipes, fibers, and various other molded articles. In addition, it is also known in the art that LCPs, particularly in the fiber form, exhibit exceptionally high mechanical properties after a heat treatment process. However, all of the known methods in the art describe formation of only the low denier fibers, e.g., of about 10 deniers per filament (dpf), which exhibit high mechanical properties in their as-spun as well as heat-treated forms. Furthermore, there are no reports in the prior art that filaments having multilobal cross-section can be made from LCPs. More importantly, filaments of LCPs generally do not adhere to various other similar or dissimilar materials.
Thus it is an object of the present invention to provide a process for forming uniformly oriented high denier multilobal LCP filaments. The high denier filament means a filament of higher than 50 dpf.
It is also an object of the present invention to provide a process for forming high denier LCP multilobal filaments of higher than 50 dpf, which exhibit enhanced mechanical, thermal and chemical resistance properties in the as-spun as well as heat-treated form.
It is further an object of the present invention to provide a process for forming high denier LCP multilobal filaments, which exhibit properties comparable to those of low denier LCP round filaments (i.e., filaments of less than 10 dpf) in their as-spun as well as heat treated states.
It is also an object of the present invention to provide high denier LCP multilobal filaments of higher than 50 dpf having properties comparable to those of low denier LCP round filaments of less than 10 dpf.
Finally, it is an object of the present invention to provide high denier LCP multilobal filaments that feature improved adhesion properties.
It is high desirability to forming uniformly oriented high denier LCP filaments, which filaments exhibit enhanced mechanical, thermal and chemical resistance properties in the as-spun as well as heat-treated form. For example, high denier LCP filaments can replace steel wires in steel belted tires. Furthermore, since LCP filaments are of substantially lower density when compared with steel wires, LCP filaments are expected to feature properties superior to those exhibited by steel wires. In addition the prior art indicates that there is a real need for high denier LCP filaments that exhibit enhanced mechanical, thermal, and chemical resistance properties.
3. Prior Art
The following references are disclosed as background prior art.
U.S. Pat. No. 4,183,895 describes a process for treating anisotropic melt forming polymeric products. A process of heat treatment reportedly yielded fibers having enhanced mechanical properties, and the fiber tenacity was reported as being increased by at least 50% and to at least 10 grams per denier.
U.S. Pat. No. 4,468,364 describes a process for extruding thermotropic liquid crystalline polymers (LCPs). It is claimed that extrusion of an LCP through a die orifice having an L/D ratio of less than 2 (preferably 0), and at a draw-down ratio of less than 4 (preferably 1), yields filaments featuring high mechanical properties.
U.S. Pat. No. 4,910,057 describes a highly elongated member of substantially uniform cross-sectional configuration which is capable of improved service as a stiffening support in an optical fiber cable.
U.S. Pat. No. 5,246,776 describes an aramid monofilament and method of making the same.
U.S. Pat. No. 5,427,165 describes a reinforcement assemblage formed at least in part of continuous monofilaments of liquid crystal organic polymer(s). The polymers used therein are primarily aramids.
Japanese laid open Patent No. 4-333616 describes a method of manufacturing filaments of 50 to 2000 dpf from molten liquid crystalline polymers. The heat-treated mechanical properties of these filaments were significantly inferior to the properties reported for the corresponding lower denier filaments of 5 to 10 dpf
J Rheology
1992, Vol. 36 (p. 1057-1078) reports a study of the rheology and orientation behavior of a thermotropic liquid crystalline polyester using capillary dies of different aspect ratios.
J. Appl. Polym. Sci. 1995, Vol. 55 (p. 1489-1493) reports orientation distribution in extruded rods of a thermotropic liquid crystalline polyesters. The orientation function increases with increasing apparent shear rate from 166 to 270 sec
−1
but decreases with increasing apparent shear rate from 566 to 780 sec
−1
.
All of the references described herein are incorporated herein by reference in their entirety.
SUMMARY OF THE INVENTION
Unexpectedly and surprisingly it has now been found that both as-spun and heat-treated high denier multilobal filaments of at least 50 denier per filaments can be made which feature essentially uniform molecular orientation across the filament cross-section. Furthermore, these high denier filaments feature remarkably good tensile properties, retaining at least 80 to 90 percent of the properties expected of conventional low denier −5 to 10 dpf filaments, which properties for high denier filament were hitherto unattainable by any of the known prior art references as briefly described hereinabove.
Thus, in accordance with this invention there is provided a process for forming a multilobal filament of a thermotropic liquid crystalline polymer having the following properties:
(i) denier of at least about 50 denier per filament;
(ii) tenacity of at least about 8 grams per denier;
(iii) modulus of at least about 450 grams per denier; and
(iv) elongation of at least about 2 percent.
The process of the present invention is comprised of the following steps:
(a) heating a thermotropic liquid crystalline polymer to a temperature of at least about 15° C. above its melting transition to form a fluid stream of said thermotropic polymer,
(b) passing said stream through a heated extrusion chamber, wherein said chamber is disposed with a suitable cylindrical orifice having a multilobal cross-section to form the multilobal filament of said polymer; and
(c) winding said filament at a take-up speed of at least about 200 meters per minute and at suitable draw-down (DD) so as to form the filament of essentially uniform molecular orientation across its cross-section and having a denier of at least about 50 denier per filament.
In another aspect of the invention there is also provided a process for forming a heat-treated multilobal filament of a thermotropic liquid crystalline polymer having the following properties:
(i) denier of at least about 50 denier per filament;
(ii) tenacity of at least about 20 grams per denier;
(iii) modulus of at least about 600 grams per denier; and
(iv) elongation of at least a
Cornetta John Edward
DiBiase Joseph J.
Flint John Anthony
Haider M. Ishaq
Jaffe Michael
Celanese Acetate LLC
Douglas Walter M.
Gray J. M.
Krynski William
LandOfFree
Process for making high denier multilobal filaments of... does not yet have a rating. At this time, there are no reviews or comments for this patent.
If you have personal experience with Process for making high denier multilobal filaments of..., we encourage you to share that experience with our LandOfFree.com community. Your opinion is very important and Process for making high denier multilobal filaments of... will most certainly appreciate the feedback.
Profile ID: LFUS-PAI-O-2604910