MXPA01008120A - Nanocomposite articles and process for making - Google Patents

Nanocomposite articles and process for making

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Publication number
MXPA01008120A
MXPA01008120A MXPA/A/2001/008120A MXPA01008120A MXPA01008120A MX PA01008120 A MXPA01008120 A MX PA01008120A MX PA01008120 A MXPA01008120 A MX PA01008120A MX PA01008120 A MXPA01008120 A MX PA01008120A
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Mexico
Prior art keywords
layers
silicate material
polymer
article
silicate
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MXPA/A/2001/008120A
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Spanish (es)
Inventor
Kyung W Suh
Richard F Fibiger
Mark A Barger
Joseph A Schomaker
Wenbin Liang
George A Mackey
Harvey C Tung
Original Assignee
Mark A Barger
Richard F Fibiger
Wenbin Liang
George A Mackey
Joseph A Schomaker
Kyung W Suh
The Dow Chemical Company
Harvey C Tung
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Application filed by Mark A Barger, Richard F Fibiger, Wenbin Liang, George A Mackey, Joseph A Schomaker, Kyung W Suh, The Dow Chemical Company, Harvey C Tung filed Critical Mark A Barger
Publication of MXPA01008120A publication Critical patent/MXPA01008120A/en

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Abstract

An improved process for making a structural foamed polymer, a multilayer polymer film, sheet or tube, a pultrusion polymer profile, a compression molded extruded fiber reinforced polymer pre-form, a strand foamed polymer and a SCORIM formed polymer article. The improvement includes the step of dispersing a multi-layered silicate material with the polymer so that the polymer has dispersed therein single layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the volume percent of the one, two, three, four and five layers of silicate material greater than the volume percent of the more then five layers of silicate material. In each of the above embodiments an important benefit of the instant invention is the orientation of the plane of the layers of silicate material. Preferably, most of the layers of silicate material have substantially the same orientation within thirty degrees of angle. Such orientation improves the properties of the product and provides a practical way to make larger products. The amount of multi-layered silicate material used is preferably between one and twenty percent.

Description

ARTICLES OF NANOCOMPUESTOS AND PROCESS TO MAKE THEM This application is under a contract from the US government with the Department of Commerce (NIST) - Avanza Technology Program Project # 70NANB7H3028.
BACKGROUND This invention relates to polymeric systems reinforced with laminated or delaminated multilayer silicates, that is, polymeric systems of nanocomposites. The nanocomposite polymers are compositions comprising a relatively high (but relatively low weight) number of exfoliated multilayer silicate material dispersed in a given volume of continuous polymer matrix, US Patent 5,717,000 for Seema V. Karande, Chai-Jing Chou , Jitka H. Solc and Kyun W. Suh, incorporated herein by reference. As discussed in the '000 patent and it is well known in the art, nanocomposite polymers exhibit many enhanced properties of physical properties at a much lower volume fill percentage than conventionally filled polymers. For example, when s form nanocomposite polymers in a film, the exfoliated multilayer silicate material can be oriented in the direction parallel to the surface of the film, which contributes to the barrier properties of the film, US Pat. , 164,460, incorporated herein by reference in its entirety.
BRIEF DESCRIPTION OF THE INVENTION The present invention has twelve modalities. The first embodiment is an improved process for making a structural foamed polymer comprising the steps of dispersing a gas-producing material in a fluid polymer at a first pressure, followed by a second pressure less than the first pressure, the difference between the first pressure and the second pressure to generate gas bubbles in fluid polymer. The improvement comprises the step of dispersing a multilayer silicate material with the polymer, so that the polymer has dispersed therein single layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the volume percentage of layers one, two, three, four and five of silicate material being greater than the volume percentage more than five layers of silicate material.
The second embodiment of the present invention is an improved foamed structural polymer comprising gas cells having polymer walls. The improvement comprises that the polymer has dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layer of silicate material, five layers of silicate material and more zinc layers. of silicate material, the percentage by volume of layers one, two, three, four and five of silicate material being greater than the volume percentage of the more than five layers of silicate material.
The third embodiment of the present invention is an improved process for making a multilayer polymer film or sheet comprising the step of coextruding layers of at least two different polymer or at least two different layers of the same polymer to form the film or film. multi-layered polymer. The improvement comprises the step of dispersing a multilayer silicate material with less one polymer, so that at least one polymer has dispersed therein simple layers of silicate material, double layers of silicate material, triple layers of silicate, four layers of silicate material, five layers of silicate material and more of zinc layers of silicate material, the volume percentage being greater d layers one, two, three, four and five of silicate material than percentage of volume of the more than five layers of silicate material.
The fourth embodiment of the present invention is a film, lamina or improved multilayer polymer tube, comprising layers of at least two different polymers or at least two layers of the same polymer. The improvement comprises at least one polymer which has dispersed therein single layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more of zinc layers of silicate material, the percentage by volume of layers one, two, three, four and five of silicate material being greater than the volume percentage of the more than five layers of silicate material.
The fifth embodiment of the present invention is an improved pultrusion process comprising the steps of impregnating a package of reinforcing fibers with a polymer and forming a structural profile. The improvement comprises the step of dispersing a multilayer silicate material with the polymer, so that the polymer has dispersed therein simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than zinc layers of silicate material, the volume percentage of layers one, two, three, four and five of silicate material being greater than the percentage by volume of more than five layers of silicate material. The sixth embodiment of the present invention is an improved pultruded structure profile comprising a pack of reinforcing fibers impregnated with a polymer. The improvement comprises the polymer which has dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the volume percentage of layers one, two, three, four and five of silicate material being greater than the volume percentage of the more than five layers of silicate material.
The seventh embodiment of the present invention is an improved compression molding process, comprising the step of compression molding a preform of fiber reinforced polymer, extruded. The improvement comprises the step of dispersing a multilayer silicate material. with the polymer, so that the polymer has scattered in it simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layer of silicate material, five layers of silicate material and more of zinc layers of silicate material, the percentage by volume of layers one, two, three, four and five of silicate material being greater than the volume percentage of the more than five layers of silicate material. The eighth embodiment of the present invention is an improved article, the article being made by compression molding a preform of extruded fiber reinforced polymer. The improvement comprises the polymer having dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the highest percentage of volume of layers one, two, three, four and five of the silicate material being the volume percentage of the more zinc layers of silicate material. The ninth embodiment of the present invention is an improved process for making foamed polymer in filament comprising the steps of extruding a polymer through a plurality of openings to form filaments and then conglutinating the filaments. The best comprises the step of dispersing a multi-layer silicate material with the polymer, so that the polymer has dispersed in the same simple layers of silicate material, double layers of silicate material triple layers of silicate material, four layers of silicate material five layers of silicate material and more than five layers of silicate material, the percentage by volume of layers one, two three, four and five of silicate material being greater than the percentage by volume d of more than Five layers of silicate material. The tenth embodiment of the present invention is an improved filament foamed polymer article. The improvement comprises the polymer having dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, being greater and percentage in volume of the layers one, two, three, four and five d silicate material that the percentage in volume of the more zinc layers of silicate material. The eleventh embodiment of the present invention is an improved SCORI M process for molding a polymer in an article comprising the step of introducing the polymer into a mold by reciprocating flow. The improvement comprises the step of dispersing a multilayer silicate material d with the polymer, so that the polymer has dispersed therein simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the volume percentage of layers one, two, three, four and five of silicate material being greater than the percentage by volume of more than five layers of silicate material. The twelfth embodiment of the present invention is an improved SCORIM molded polymer article. The improvement comprises the polymer which has dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, with a higher percentage by volume of layers one, two, three, four and five of silicate material than the volume percentage of more zinc layers of silicate material. In each of the above embodiments, an important benefit of the present invention is the orientation of the plane of the layers of silicate material. More specifically, most silicate material layers have substantially the same orientation (within thirty degrees of the greater surface area of the fabricated material or the interface of a multilayer structure) and this orientation improves the properties of the product. In the structural foamed polymer mode, the orientation is parallel to the wall of the cell with, for example, about seventy percent of the layers that are within thirty degrees of parallel with the cell wall In the embodiment of the cell. multilayer polymer film, sheet or tube, the orientation is parallel to a larger surface of the film sheet or tube. In the pultrusion mode, the orientation is parallel to the fiber bundle. In the compression molding mode, the orientation is parallel to the reinforcing fibers. In the foamed polymer d filament mode, the layers of silicate material are partially oriented by the initial extrusion process prior to foaming and furthermore, they are oriented parallel to the cell wall during foaming. Another important benefit of the present invention is that its articles can be relatively large (more than one kilogram) compared to articles made according to the prior art. The amount of multilayer silicate material used in the present invention is preferably between one and twenty percent by weight.
DETAILED DESCRIPTION OF THE INVENTION The term "multilayer silicate material" is well known in the nanocomposite art and includes layered silicates and silicate clays. Illustrative of such materials are smectite clay minerals, such as montmorillonite, nontronite, beidellite, hectorite, saponite, sauconite and vermiculite clay minerals. This term also includes ¡Hita minerals, such as ledikita and layered silicates, such as magadiite and kenyaite. The preferred multilayer silicate materials are type 2: 1 phyllosilicates, having a negative charge in the layers ranging from 0.25 to 1.5 loads per unit of formula and an equal number of interchangeable cations in the spaces between layers. . More preferred are smectite clay minerals, such as montmorillon ita, nontronite, beidellite, hectoria, saponite, sauconite and the silicates in magadiite and kenyaite layers. The technique used to disperse or "exfoliate" a multilayer silicate material in a non-critical polymer in the present invention, as long as the volume percentage of layers one, two, three, four and five of material of silicate as dispersed or "exfoliated" is greater than the volume percentage of the more than five layers of silicate material so dispersed or "exfoliated". For example, such a dispersion can be achieved by polymerizing one or more monomers with a treated multilayer silicate material, as described in US Pat. No. 5,973,053, incorporated herein by reference, or, for example, by mixing by melting a multi-layered silicate material treated with a polymer as described in US Pat. No. 5,385,776, incorporated herein by reference. The percentage by volume of layers one, two, three, four five and more than five layers of silicate material is determined herein by electron microscopic examination of a representative sample, wherein each layer by definition herein has same volume. The term "structural foamed polymer" and a basic teaching regarding its process and articles will be found in the Encyclopedia or Polymer Science and Engineering (Encyclopedia of Science and Engineering of Polymers), vol.15, 1989, p.771-797 , incorporated herein by reference in its entirety and is distinctly different from the foams discussed in U.S. Patent 5, 717, 000. The minimum density of such a foam product is often limited by the capacity of the foam walls. Cells to withstand the loads, which are applied during use, Conventional relatively large fillings, such as talcum powder, can be used to strengthen cell walls, however, this can lead to premature rupture of the wall. the cell when the thickness of the cell wall approaches the size of the filler particles, this may limit how low the density of the foam that can be prepared is. Furthermore, an increase in the melting strength of the polymer is desirable for thinner cell walls and that conventional fillers do not change the melting force substantially. The orientation of the ideally simple platelet-shaped nanofillers of the present invention (and the fact that, once oriented, they project a transverse section of less than a few nanometers through the thickness of the walls of the cells) can overcome these difficulties and conducts lower density foam products with good load carrying capacities. The high aspect ratio of the nanofillers of the present invention also dramatically increases the melting strength of the polymer and produces compositions in which the cell wall observes the maximum reinforcement in both the molten and solidified state. In this way, a lower density foam can be produced, which equals the performance of higher density products. The term "multilayer polymer film, foil or tube" is defined in, and a basic teaching regarding its process articles will be found in, the Encyclopedia of Polymer Science and Engineering (Encyclopedia of Polymer Science and Engineering), vol. 7, 1 987, p 106-1 27 incorporated herein by reference in its entirety and in US Patents 3,576,707, 4, 122, 138, 5,443,874, 5, 129,544, 5,441, 781, 4,005,967, 3, 739,052, 3,947,204 and 3,884,606, each of which is fully incorporated herein by reference. The multi-layer coextrusion process has been used commercially to make single items, tubes, sheets and films with 3 to 10 layers. It allows the manufacture of products with thinner layers can be made and handled as a single sheet. The layers can individually provide a specific attribute, such as barrier properties, mechanical strength, printing ability, adhesion to the overall structure. The multiple layer extrusion process of the present invention can, of course, be coupled with other processes, such as solid phase formation, blow molding, stretch blow molding, thermoforming injection molding to produce shaped articles. The multilayer coextrusion process of the prior art suffers from difficulties in equalizing the rheology of the separated layers. The poorly matched rheology can lead to poor interfacial adhesion, a wavy interphase, and in extreme cases, the breakdown of the interface. In this way, poor optical properties and reduced physical properties can be produced. It would also be advantageous to reduce the thickness of the individual layers in order to save material costs. The reduction in thickness requires improved performance, as well as very uniform layer structures. Conventional relatively large size fillings, such as talc, generally can not be used in layers below 50 micrometers in thickness, because such conventional fillers cause defects and flow instabilities. Processes for extrusion molding often provide improved strength in the machine direction (extrusion), but are much weaker in the transverse direction. Mechanical processes, such as rotation molding, have been developed to overcome this problem but require specialized additional equipment. A simple method is desired to maintain the force biaxially. In the embodiment of the present invention, it is found that the ease of orientation of the nanofillers with plates provides a method for optimizing the properties of both thin layers and relatively thick layers in a multi-layer coextruded article. The nanofillers as plates of the present invention provide added melt strength to low viscosity layers, which leads to more uniform layer thickness, are small enough so that they do not break even in the thinnest single layer and the process of Formation causes a high degree of orientation of the plates, thus maximizing the performance of the article produced. The small size of the plates makes them transparent, so they can be used in applications where clarity is required. The biaxial nature of the platelet reinforcement provides additional force in the transverse direction, which is inherently weak due to the manufacturing process. The compounds of the embodiment of the present invention are particularly applicable in multi-layered automotive fuel tanks, automotive gas filler neck / tube, fuel transport lines and hollow multi-layer moldings, such as bottles for carbonated drinks. In these situations, the nanofillers of the present invention can be incorporated into those layers responsible for, the desired property, for example, barrier for gases or vapors. The nanofiller of the present invention provides improved performance and clarity; the orientation imparted to nanoparticles in the extrusion process maximizes performance. In the case of fuel tanks or other large items, the multilayer sheet can be extruded, followed by thermoforming separate halves and welding the halves together to make a complete structure. In the case of other large articles, a multilayer (or "parison") tube can be extruded followed by blow molding or parison in the mold of the desired shape. The sinking of the parison during extrusion and before blow molding can cause difficulties in reproducibly controlling the process. The high aspect ratio of the nanofiller provides substantial reinforcement of the polymer melt and in this way, reduce the sinking problem of a large parison. Other applications of the embodiment of the present invention include semi-rigid containers for food and industrial materials, signage, machines and side panels of furniture and instruments. The number of layers can be five to ten or more than ten layers. In addition, the article made can be more than one kilogram of weight. Co-extrusion has been used commercially to manufacture films, sheets and single tubes ranging from as few as 3 layers to layers of layers, where the individual layers may be less than 1 00 nanometers thick. Fillers as plates are highly oriented in these films, mediating the extrusion process, which assists in the flow stability during extrusion / thus producing more intact layers. The thinner the layers, the greater the orientation and in this way, the greater the reinforcement The orientation of the nanofiller also improves the barrier and overall mechanical performance difference of the conventional fillers, the thinness of the nanofillers of the present invention allows its presence without interfering with the optical properties of the films (or sheets or tubes) Applications of the embodiment of the present invention include barrier packaging for food and medicine, decorative films, non-metallic mirrors for automotive and construction applications, transparent surfaces reflecting ultraviolet or infrared light for advantages and so on The term "pultrusion" is defined in, and a basic teaching with respect to its process and articles will be found in the Encyclopedia or Polymer Science and Engmeepng (Encyclopedia of science and engineering of polymers ), vol 4, 1 986, p 3-9 and 34 36, which was incorporated Now in this completely by reference The practice of these processes can produce low modulus in a direction perpendicular to the direction of the fiber (off-axis) and poor performance due to a loss in the bond between the reinforcing fibers and the material of matrix The loss in the un ion, which is attributed to an inequality in the coefficient of thermal expansion (CLTE) between the reinforcing fibers and the ream of mtriz, can be particularly poor with carbon fibers. One objective of this modality of the present is to improve the off-axis strength of the compound via nanocomposites with the high aspect ratio platelets. This improved performance may be more pronounced since the thickness of the composite is reduced due to the alignment of the nanocomposite plates via the induced cut in the pultrusion process. The reduction in the CLTE of the matrix due to the presence of nanorellen produces a better equalization of CLTEs between carbon fibers and the matrix resin, leading to a more intact interface. This performance is surprising because it tends not to take place with conventional fillers, such as talcum or calcium carbonate. The embodiment of the present invention can be used with thermoplastic and thermosetting resins, but it is often practiced with epoxies similar to thermosetting resin, vinyl esters, vinyl ethers and urethanes. Applications include, for example, intermodal containers, building walls and panels, structural profiles for bridges, automotive body panels, automotive door panels / modules and automobile fender bars. The term "compression molding" is defined in, and a basic teaching regarding its process and articles will be found in, the Encyclopedia of Polymer Science and Engineering, vol. 4, 1986, p. 79-85, 1 04 and 108, which is incorporated herein by reference in its entirety. A major problem with parts that have support edges, which are made by compression molding a fiber-reinforced, extruded polymer preform, can be "displayed along" the supporting edges when the thickness of the wall of the part is reduced below approximately 2 meters.
The use of a nanocomposite of the present invention in the preform of extruded fiber reinforced polymer reduces the "show along" edge by reducing the coefficient of thermal expansion of the polymer to more closely match that of the glass fibers. The extrusion process can optimize the orientation of the dispersed nanofiller of the present invention by using multi-slot dies. D this way, the reduction of the coefficient of linear expansion (CLTE) and optimized by the extrusion process. The use of a nanocomposite of the present invention can also produce or finish class A of the article superior to the use of conventional filler materials. The embodiment of the present invention is especially useful for making automotive parts, such as door panels, side panels, front end modules and structural instrument panel modules. The term "foamed polymer filament" is defined in, and a basic teaching with respect to its process articles will be found in, U.S. Patents 5, 527,573, 4,801, 484, 5,206, 082 and 4, 824, 720, each of which is incorporated herein by reference in its entirety. The density of filament foams can be further reduced over standard foams using nanocomposites, because the nanofiller plates of the present invention are optimally oriented by the initial fiber extrusion process prior to foaming. Unlike conventional fillers, the small size of the nanofiller of the present invention adds further thinning of the cell wall. The added orientation of the nanofiller of the present embodiment also improves the melting rheology of the polymer which leads to improved foam stability. The resulting higher dimensional stability and impact force makes the foams prepared according to this modality, very suitable for automobile fenders, front panels, insulation panels and interior automobile uprights. The term "SCORIM" (controlled orientation of molding cutting or injection molding) is defined in, and a basic teaching with respect to its process and articles will be found in, US Patents 4,994,220, 5,059,368, 4, 925, 161 and 5, 160,466 , each of which is fully incorporated by reference. The unique properties of the nanofiller as the plate of the present invention produce a high degree of alignment through a large cross section with minimal randomization of the particles, even during a prolonged cooling cycle. In this way, larger parts are possible via SCORIM injection molding. In addition, the nanofillers of the present invention can be used both for reinforcement and rheology modification of one or more of the layers in an injection molded or co-injected part. Applications of the embodiment of the present invention include refrigerator liners, automotive facías, containers and washing machine tubes.
EXAMPLE 1 Co-extruded films of nanocomposite polyolefin composites are prepared using a co-extrusion line consisting of two 1-millimeter single screw extruders, equipped with gear pumps (pumping capacity of 1.2 cm3 / revolution). The extruders provide two independent melt streams in a coextrusion feed block that provides an initial two-layer melt stream (ie, the first compound stream). This first stream of compound is subsequently passed through a series of multipliers. two-channel layers (similar in design to those shown by Schrenk, et al., in US 5,202,074, fully incorporated herein by reference), to create a second stream of compound having an increased number of layers according to the following equation: N = 2 (2n) where: N = total number of layers n = number of stages of multiplication of layers The second compound stream is subsequently passed through a flexible edge die 350 millimeters wide and onto a chilled dump drum to make a thin film. The materials used are polyolefin elastomer brand Engage EG8200 from Dupont-Dow Elastomers; poly (ethylene-co-acrylic acid) m arca PRI MACOR 3460 from The Dow Chemical Company; poly (ethylene-co-acrylic acid) brand PRIMACOR 1430 from The Dow Chemical Company; and multilayer silicate material of montmorillonite treated with quaternary ammonium brand Claytone HY from Southern Clay Products. The two grades PRIMACOR and Claytone HY are premixed using a Werner Pfleiderer ZSK30 co-rotating twin screw extruder in the following proportions by weight: Matter l% by weight PRI MACOR 1430 80 PRIMACOR 3460 16 Claytone HY 4 This compound (Compound "A", approximately 0.8% by volume of multilayer silicate) is then co-extruded with Engag (equal volumetric proportions) using the previously described process under the following conditions: Extruder A Material: Engage EG8200 Fixed extruder barrel temperatures (° C) Zone 1: 1 60 Zone 2: 1 85 Zone 3: 200 Gear pump temperature: 200 ° C Extruder screw speed: 70 rpm Pump speed: 35 rpm Extruder B Material: Compound A Fixed extruder barrel temperatures (° C) Zone 1: 1 55 Zone 2: 1 75 Zone 3: 1 90 Gear pump temperature: 190 ° C Extruder screw speed: 70 rpm Pump speed: 35 rpm Multiplier temperature of layers: 192 ° C Die temperature: 220 ° C The extruded films (thickness 0.00635 cm) were then tested for oxygen permeability and specular light transmission according to the test methods of ASTM D3985 and D 1003, respectively. The results are shown in the following table: Units of oxygen transmission rate: cm2-mil / 1 00 in2-day-atm.
EXAMPLE 2 The molded samples by injection of polypropylene structural foams are prepared using an Arburg reciprocating screw injection molding machine 170CMD, equipped with an 18 mm injection cylinder, a mechanical closure nozzle and a plac mold ( cavity dimensions: 65 mm x 65 mm x 6 m illimeters). The mold is fed through a blade of full thickness, full width blades. The specific material formulations in percent parts are described in the following table: I D PP 3150 Claytone HY FM 1 709H 71 .0 25.0 4.0 64.3 22.1 9.6 4.0 The materials are obtained from the following manufacturers: Polypropylene homopolymer (PP) H702-35: The Dow Chemical Company PP grafted Polybond 31 50: Uniroyal Chemical Montmorillonite treated with quaternary ammonium HY: Southern Clay Products (55% by weight silicate material multilayer, inorganic) FM 1 1 709H blowing agent: Equistar The blowing agent is based on azobisformamide and is in the form of a concentrate in a polyolefin carrier. The PP / Polybond / Claytone HY materials used in Formulation II were provided as a concentrate (67/23/1 0), prepared using a 25 mm high speed co-rotating twin screw extruder (30 HP) Krupp Werner Pfleiderer ZSK Mega Compounder) operating under the following conditions: Screw speed: 1 000 rpm Extrusion speed: 6.64 kg / h Torque: 35% of maximum Fixed barrel temperatures: 150 ° C Fixed die temperature: 1 90 ° C Melt discharge temperature: 230 ° C The respective materials for each formulation were weighed, physically mixed and then fed directly into the feed passage of the injection molding machine. The molding conditions that are employed, in general, are summarized below. Fixed barrel temperature (° C) Zone 1: 182 Zone 2: 210 Zone 3: 221 Nozzle: 221 Plasticizing speed (m / min): 10 Back pressure (Pa): 30x1 05 (I) 60x105 (II) Shot size (cm3): 18 Filling time (s): 0.5 Package pressure (Pa): 25x105 Package time (s): 1 Holding time (s): 130 Mold temperature (° C): 1 9 The foam samples exhibit a density of 416,494 ± 16.01 kg / m3, which represents the density reduction of 54% in relation to solid polymer. These foams are subsequently tested by compression properties in general following the procedure of ASTM D 1621-94. The results are summarized in the following table.
I D compression nodule (kg / cm2) Performance tension (kg / cm2) 0.8225 31 .4944 0.8646 37.6808 The nano-filled material exhibited an improvement of modulus and strength of yield of 5% and 20% in relation to the non-filled control. Nano-filled material also exhibits improved post-performance properties.
EJ EM PLO 3 Injection-molded samples of glass fiber reinforced polypropylene composites are prepared using an Arburg 170CM D reciprocating screw injection molding machine, equipped with a 1 8 mm injection cylinder and a Modified ASTM type I tension bar mold. The specific material formulations in percent parts are described in the following table: Homopoly grafted number Claytone Fiberglass I D. H702-35 PB 3150 HY R22Y-AA D 67 23 10 E 60 21 9 10 F 47 16 7 30 The materials are obtained from the following manufacturers: Polypropylene homopolymer (PP) H702-35: The Dow Chemical Company Polybond 3150: Uniroyal Chemical Multi-layered silicate treated with quaternary ammonium HY: Southern Clay Products (55% by weight of material silicate multilayer, inorganic) R22Y-AA: Owens Corning Fiberglas The PP / Polybond / Claytone HY materials used in DF are provided as a concentrate (67/23/1 0), prepared using a 25 mm high-speed co-rotating twin screw extruder (one 30 HP Krupp Werner Pfleiderer ZSK Mega Compounder) which operates under the following conditions: Screw speed: 1000 rpm Extrusion speed: 6.64 kg / h Torque: 35% of maximum Fixed barrel temperatures: 1 50 ° C Fixed die temperature: 1 90 ° C Fusing discharge temperature: 230 ° C The respective materials for each formulation were weighed, physically mixed and then fed directly into the feed passage of the injection molding machine. The molding conditions that are used, in a general way, are summarized in conjunction with this. Fixed barrel temperature (° C) Zone 1: 182 Zone 2: 204 Zone 3: 215 Nozzle: 215 Plastification speed (m / min): 5 Back pressure (Pa): 20x1 05 (200x1 05 for samples C and F) Shot size (cm3): 18 Fill time (s): 0.5 Package pressure (Pa): 500x105 Package time (s): 60 Mold temperature (° C): '20 The samples are subsequently tested for flexural properties and coefficient of thermal expansion (CTE) parallel to the longitude axis by the general processes of ASTM D790 (Method 1 Procedure A) and E831 (-30 ° C to 30 ° C), respectively. The results are summarized in the following table.
Sample ID Module CTE Flexural Strain Performance Performance D 20.8654 2.83 367.669 47 E 33.21 67 2.87 485.773 37 F 57.3155 1 .69 603.877 27 Flexural module in kg / cm2 Performance effort in percentage Performance stress in kg / cm2 CTE in micro m per m-grade C EXAMPLE 4 7.5 parts percent (pph) of multilayer silicate material Mark Closite 30 of Southern Clay Products is mixed in 1 8,925 I of Derakane 41 1 -350 (The Dow Chemical Company) at 7 ° C until homogeneous . 1.5 pph of a mold release agent (Axel PS 125) and 0.3 pph of an air release agent (BYK 51 5) are added, followed by 0.1 g of a mixed catalyst containing Peracodox 16N Trigonox 141 and Trigonox C A bundle of fibers consisting of 7 layers (1 = Nexus Veil 1 10 039, 2 = glass mat (M8643, 46.65 g), 3 = 4-filament glass twine (PPG 2026, yield 1 13), 4 = mat of glass, 5 = torzal d glass, 6 = glass mat, 7 = Nexus Veil) is impregnated with the resin via an immersion bath and extracted through a pultrusion die d flat plate 1 5x3 mm. The curing system consists of three heating zones of 20.32 cm (1 1 5.56 ° C)., 137.78 ° C and 1 37.78 ° C). The final parts were 3.94 mm thick, consisted of 52% by volume of resin and 48% by volume of glass with a density of 1.4-4.5 g / cm3. The test specimens are cut from the final parts and are tested with the following results. Tension force, 5083.53 kg / cm2; module, 239736.42 kg / cm2; effort to break, 2.3%; elongation to rupture,

Claims (5)

1 . A process for making an article, comprising the article or nanocomposite polymer, wherein the article is selected from the group consisting of a foamed structural polymer, a multilayer film, sheet or tubing, a pultruded structural profile, or article of compression molded polymer formed from a pre-formed fiber reinforced polymer preform, a foamed polymer article of filament and an article formed by the SCORIM process comprising the steps of: dispersing a multi-layer silicate material with the polymer, so that the polymer has dispersed in the same simple layers of silicate material, double layers of silicate material, triple layers of silicate material, four layers of silicate material, five layers of silicate material and more than five layers of silicate material, the percentage by volume of layers one, two, three, four and five of silicone material being higher ato that the percentage and volume of the more than five layers of silicate material, to form a nanocomposite polymer; the process is characterized by the process of forming the nanocomposite article by blowing the nanocomposite polymer to align the planes of layers one, two, three, four and five of silicate material, so that more than one half of the The planes have the same orientation within thirty degrees, as determined by electronic microscopy.
2. The process of claim 1, wherein the article is a multilayer polymer film, sheet or tube and wherein the number of layers is ten or more.
3. The process of claims 1-2, wherein the weight percent of the multilayer silicate material dispersed in the polymer is in the range of one to twenty percent.
4. The process of claims 1-2, wherein the weight percent of the multilayer silicate material l dispersed in the polymer is in the range of from two to ten percent.
5. An article made by the process of claims 1-4.
MXPA/A/2001/008120A 1999-02-12 2001-08-10 Nanocomposite articles and process for making MXPA01008120A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US60/119,816 1999-02-12

Publications (1)

Publication Number Publication Date
MXPA01008120A true MXPA01008120A (en) 2002-03-26

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