Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Cellular products or processes of preparing a cellular...
Reexamination Certificate
1999-07-19
2001-12-04
Cooney, Jr., John M. (Department: 1711)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Cellular products or processes of preparing a cellular...
C521S079000, C521S142000
Reexamination Certificate
active
06326411
ABSTRACT:
The present invention relates to a mixture for the manufacture of a cellular polymer product comprising more than 90% by volume of closed cells, and to a manufacturing process utilizing said mixture for obtaining said product.
For numerous applications, particularly for hot water pipes or the pipes of a district heating installation, it is sought to obtain insulation for the pipes having the lowest possible thermal conductivity. For this purpose, the pipes may be covered with an insulating layer of cellular material, preferably an expanded polymer.
By means of polymer extrusion technology, cellular structure materials of very variable apparent densities can be producted.
For obtaining relatively low expansion rates, so called “chemical” blowing agents are ordinarly used, which are organic or inorganic compounds capable of generating gaseous by-products by thermal decomposition or by any other chemical reaction capable of being triggered in the extruder or later on by heating the product in an oven.
For obtaining high rates of expansion, the technology most frequently has recourse to the injection of gases or liquids having a low boiling point (so-called “physical” blowing agents) which can be injected in sufficient quantity into the mass of molten polymer kept under high pressure in the extruder. In this case, the process usually requires the use of high-pressure metering pumps or compressors which are a major technological complication and add to the cost of the installation.
U.S. Pat. No. 3,344,215 discloses a process using injection of a volatile liquid foaming agent into the plastic mass of the polymer, in an extruder.
According to U.S. Pat. No. 4,407,768, a composition is provided which is able to feed an extruder. The composition contains hydrated alumina as filler precursor, which loses its water of hydration upon heating.
A further development of this technology is taught by U.S. Pat. No. 4,506,037, where water is used as an expansion agent. The aqueous medium is treated together with the other ingredients for producing a resin compound as the result of a melt-adhesion process. After a complex compounding operation the resin compound is able to feed an extruder.
To insure a cellular structure which is uniform, all the ingredients used must be mixed in the most homogeneous possible manner, particularly the nucleating agent, and there must be no significant temperature deviation within the mass of polymer at the time of formation of the cellular structure, despite the fact that this mass must be cooled before leaving the extruder. For at that time, its temperature must be as close as possible to the solidification temperature of the polymer. For these various reasons, the recourse has most often been sophisticated to equipment, calling for twin-screw extruders or two extruders in cascade.
In a first aspect, the present invention is a mixture for manufacturing an expanded cellular product including more than 90% by volume of closed cells, comprising a basic polymer in the form of powder or fine granules, a liquid expansion agent, an adsorbing agent capable of adsorbing the liquid expansion agent and a nucleating agent.
The preparation of mixtures comprising all the necessary ingredients for effecting the expansion at the outlet of the extruder is an improvement with respect to the processes necessitating injection of an expansion agent in a particular region of an extruder. However, the last-mentioned reference still requires sophisticated equipment for effecting the “melt-adhesion” step of the process.
Research undertaken by the Applicant has shown that a mixture as stated hereabove, prepared in a very simple manner by a proper choice of the ingredients, unexpectedly leads to a drastic reduction in the cost of production of well-aimed expanded cellular products having a very high rate of expansion.
Thus the present invention, according to its first aspect, is a mixture with the essential characteristics defined in claim
1
, while the claims depending therefrom define its secondary characteristics.
A second aspect of this invention is a process utilizing the mixture of claim
1
, said process being defined by claim
10
, while the claims depending therefrom define particular features of the process.
The product is produced by extrusion of a mixture containing the polymer and the necessary ingredients about a tube or any other article of similar shape or by extrusion directly in the form of a section. The cellular structure is produced continuously immediately at the outlet of the extruder, within the die or at the outlet thereof. This cellular structure thus makes it possible to reduce the specific gravity of the product greatly and to lessen its thermal conductivity significantly.
The present invention contributes a number of technological simplifications inasmuch as all the ingredients necessary for obtaining the cellular structure product are mixed mechanically at ambient pressure and temperature before being placed in the extruder. Furthermore, the choice of ingredients is such that the phase of homogenizing the mixture in the extruder is simplified thereby and that despite the presence of one or more liquids, the mixture of ingredients flows without difficulty and without any tendency to agglomerate and can therefore be metered easily in the extruder as is usually done with pellets. Moreover, the process requires the use of only one single-screw extruder.
The extruder is fed with a mixture containing the polymer or polymers, as well as all the ingredients necessary for the process. In the extruder, the volumetric metering, melting, pressurizing of the mixture and homogenizing thereof (materials and temperature) are carried out. The extruder is provided with an extrusion head for shaping the product, as well as for creating a cellular structure such as described above. As a variation, it allows the co-extrusion of an outer layer having no cellular structure. Calibrating and cooling of the product are carried out according to the rules of the art normally applied for the products concerned (tubes, sections, and the like).
The following list describes the main and secondary characteristics, as well as the possible variations of the mixture according to the invention and of the process according to the invention.
(a) The basic polymer is preferably a polymer of the polyolefin group or a mixture of several polymers of that group.
(b) The basic polymer, in whole or in major part, is preferably in the form of a powder or of very fine granules. If necessary, the mixture may contain up to 20% of polymer pellets of ordinary size (e.g., 2.5 mm in diameter, 3 mm in length).
(c) The cells are formed by the vaporization and expansion of a liquid, or of a mixture of several low boiling-point liquids. Such liquids are called expansion agents. Among the liquids usable for this purpose are the low boiling-point alcohols, such as ethanol, or the alkane liquids, such as pentane or hexane. In general, any liquid having a boiling point at least about 20° C. below the melting point of the polymer may be used. Preferably, water is used as the expansion agent.
(d) The expansion agent is adsorbed at the surface of an inorganic filler preferably made up wholly or for the most part of fumed silica. This filler is called an adsorption agent.
(e) Nucleation of the bubbles is brought about by the addition of a solid inorganic or organic filler having a particle size adapted to this function. A mixture of several inorganic or organic fillers may be used, either of the inert type or capable of generating gaseous by-products by thermal decomposition. This filler or mixture of fillers is called a nucleating agent. Another endothermic or exothermic expansion agent of the “chemical” type may also be used for this purpose in combination with one or more inert-type inorganic or organic fillers. Along these lines, commercially available products containing activated azodicarbonamide, allowing a high reaction rate during passage through the extruder, make it possible to improve the quality of the cellular
Affolter Eric
Desarzens Philippe
Cooney Jr. John M.
Nextrom Holding SA
Oliff & Berridg,e PLC
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