Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Processes of preparing a desired or intentional composition...
Reexamination Certificate
1994-07-11
2001-08-14
Mulcahy, Peter D. (Department: 1713)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Processes of preparing a desired or intentional composition...
Reexamination Certificate
active
06274656
ABSTRACT:
BACKGROUND OF THE INVENTION
This invention generally relates to the pelletization of polymers. More particularly, the invention relates to the pelletization of polyolefin copolymers and elastomeric materials. It further relates to the improvement in the ease of fabrication of extruded or molded articles, or otherwise shaped objects, formed from the melt processing of said polymeric materials.
Pelletization of polyolefin copolymer, for example, polybutylene copolymer, especially high melt flow, high ethylene (ethylene content higher than 0.75 wt %), has been very difficult when using either the underwater face cutter or the strand cutting pelletizer. The problem appears to relate to the slow crystallization rate of these polymers which exhibit extreme tackiness in pelletizing. It is known that as the pellets leave the cutting blades, they are very clear and tacky, and collide with other pellets to form agglomerates. With a longer residence time, the pellets change to an opaque color, as they complete their crystallization, become hard and lose their tackiness. These agglomerates frequently plug the pelletizer bowl and the spin dryer. The extrusion line has to be shut down in order to clean the plugged section resulting in undesirable production interruptions. Also, the high number of pellet marriages shown in the final product is not acceptable in the customers' fabrication process.
Using polyethylenes (such as HDPE powder) as an external pelletizing aid to eliminate the surface tackiness is known in the art. The success of this method depends on good dispersion and suspension of HDPE in the slurry water. Therefore, it generally requires the addition of extra portable mixers to the slurry water tank to keep the HDPE from foaming. This method of reducing surface tackiness is very messy and labor intensive. Even under the best of circumstances, a significant fraction (about 20%) of the production has to be discarded due to poor pellet quality and pellet agglomerations. Thus, there continues to exist the need for new and better methods and/or agents for preventing or minimizing stickiness of polymers and copolymers.
The use of a nucleating agent(s) to accelerate crystallization is also known in the art. However, the art clearly teaches that there is no evidence of a universally strong nucleating agent for all polymers, and that an effective nucleating agent for one polymer may be ineffective for even a closely related polymer. The art further teaches that even a compound closely related to an effective nucleating agent for one polymer may be ineffective for that same polymer. Thus, it can be correctly said that no cross-utility exists or is expected for nucleating agent(s), and that the discovery of new and effective nucleants for polymers, especially if such nucleants exhibit synergism continues to be unexpected and desirable.
SUMMARY OF THE INVENTION
It is a general object of the invention to facilitate the pelletization of polymers.
It is a specific object of the invention to provide a nucleating agent package and methods to facilitate the crystallization from the melt of high melt flow polyolefin copolymers.
Accordingly, it is now provided a method for promoting crystallization from the melt of polyolefin copolymers, such as polybutylene copolymers, which comprises adding to a composition comprising the polyolefin copolymer an effective amount of a nucleating package consisting essentially of high melt flow, polypropylene and stearamide.
It is also provided a rapidly melt crystallizable polyolefin copolymer composition comprising an effective amount of a nucleating package consisting essentially of high melt flow polypropylene and stearamide.
DETAILED DESCRIPTION OF THE INVENTION
The following terms when used in this specification including claims shall have the following meaning:
Low Melt Flow Polypropylene means polypropylene having a melt flow of from 0.2 to 2 dg/min.
Medium Melt Flow Polypropylene means polypropylene having from 2 to 8 dg/min.
High Melt Flow Polypropylene means polypropylene having a melt flow of from 8 dg/min. and above.
Broadly speaking all polymers are suitable in the practice of this invention. The term polymers as used herein, unless otherwise specified, includes homopolymers, copolymers, terpolymers and all other known combinations or forms of polymeric materials, including polymers which are elastomeric in nature. The homopolymers generally have less crystalline problems, and are not of the greatest concern.
Polyolefin copolymers typically exhibit slower crystallization rates leading to longer crystallization times. This is usually observed by their low crystallization temperatures which is believed to be caused by the alteration of the crystalline morphology of the primary polymer component. As has been earlier noted, the excessive stickiness resulting from slow crystallization is undesirable. This generally occurs in polyolefin copolymers made up from semi-crystalline polymers such as polyethylene, polypropylene, polybutylene, polyester, polyethylene terephthalate, ethylene vinyl acrylate, and elastomeric polymers such as KRATON® and rubber. Of particular concern are very high melt flow copolymers of butene-1 and ethylene (butene-1-ethylene copolymers).
Butene-1-ethylene copolymers including methods for their preparation are known in the art. Butene-1-ethylene copolymers suitable in the practice of this invention contain from about 0.1 to 8.0 wt % ethylene. Preferably, such butene-1-ethylene copolymers contain from about 0.1 to 7 wt % ethylene, and have melt indices ranging from about 0.2 to 1000 dg/min.
Nucleating agent(s) and/or nucleating packages useful in the practice of this invention generally include an organic fatty amide and a polymeric material with a higher melting point than the base polymer to be pelletized. This class of material hereinafter collectively referred to as nucleants, include stearamide, N,N′-ethylenebis(stearamide), polyethylene wax, and polypropylene. The preferred nucleant is high melt flow polypropylene and stearamide. Generally speaking, an effective amount of nucleants ranges from about 0.1 to 3 wt %, preferably from 0.25 to 2 wt % of the total composition including the base copolymer.
It is noted that the addition of oxidized high density polyethylene powder to the extruder or to the water tank during the process of practicing this invention will result in an improvement in processing conditions. Particularly evident was the resulting increase in the slurry water temperature. Oxidized high density polyethylene powder is commercially available as ACUMIST® and can be obtained from Allied Signal Company. When used, the oxidized high density polyethylene powder is typically present in an amount ranging from 0.1 to 0.5 wt %.
Various other conventional additives can also be listed in the practice of this invention. These additives include corrosion inhibitors, foaming inhibitors, buffers, and neutralizers.
The nucleant can be incorporated into the polyolefin copolymer by using conventional equipment and techniques known in the art. For example, this can be accomplished by blending all of the ingredients in an intensive blender prior to compounding the blend in an extruder. It can also be accomplished by incorporating the nucleant and other additives in a polyolefin copolymer masterbatch.
It is well known in the art that the nucleating ability of a nucleating agent can be assessed from its temperature of crystallization from the melt in a differential scanning calorimeter (DSC). The terms crystallization temperature or recrystallization temperature have been commonly and interchangeably used for this phenomenon. Higher values indicate nucleation improvement.
Subsequent to incorporating the nucleating package into the polyolefin copolymer, the crystallization temperatures of the various samples or runs can be measured in order to determine the efficacy of the nucleant. Alternatively, the pellet quality produced from the polyolefin copolymers comprising the nucleants can be visually inspected. Successful practi
Ma Chin-Yuan George
McCullough, Jr. James Douglas
Mulcahy Peter D.
Shell Oil Company
Tsang Y. Grace
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