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A radiation curable, flexible, paintable composition produced from epoxy compounds and one or more polyol(s) has enhanced durability, thick and thin film adhesion, resistance to mold growth and dimensional changes while reducing solvent emissions. The composition can reduce, if not eliminate, runs and drips during the thermal bake cycles which are associated with using conventional compositions in automotive applications.
1. A method for providing a coating on an automotive body component from a composition comprising a combination comprising at least one epoxy compound, at least one polyol and at least one ultra-violet photoinitiator wherein said method comprises:
(a) applying the exposed composition onto the automotive body component wherein at least a portion of the automotive body component has a vertical surface, and,
(b) exposing the automotive body component to a source comprising ultra-violet radiation thereby forming a coating upon the automotive body component.
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15. A method of coating a brake rotor comprising:
(a) providing a composition comprising a combination comprising at least one epoxy, at least one polyol and at least one ultraviolet photo-initiator,
(b) applying the composition onto at least a portion of the brake rotor,
(c) exposing the brake rotor to a source of ultraviolet radiation, and;
(d) recovering a coated brake rotor.
16. The method according to
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18. A method for providing a coating on an automotive body component from a composition comprising a combination comprising at least one epoxy compound, at least one polyol and at least one ultra-violet photoinitiator wherein said method comprises:
(a) applying the composition onto the automotive body component wherein the automotive body component comprises a weld formed between at least two adjacent components, and,
(b) exposing the automotive body component to a source comprising ultra-violet radiation thereby forming a coating upon the automotive body component.
19. The method of
20. The method of
This is a continuation of U.S. patent application Ser. No. 09/448,810, filed on Nov. 24, 1999, now U.S. Pat. No. 6,461,691, that is a continuation in part of U.S. patent application Ser. No. 09/197,107, filed on Nov. 20, 1998, now U.S. Pat. No. 6,277,898 B1, that is in turn a continuation in part of Ser. No. 09/081,966, filed May 20, 1998, now U.S. Pat. No. 6,174,932, and entitled "Curable Sealant Composition". The disclosure of these prior filed patent application is hereby incorporated by reference.
The subject matter herein also claims benefit under 35 U.S.C. 111(a), 35 U.S.C. 119(e) and 35 U.S.C. 120 of U.S. Provisional Patent Application Ser. No. 60/047,290, filed on May 21, 1997, entitled "A UV-Curable Sealant Compositions"; and U.S. Provisional Patent Application Ser. No. 60/079,204, filed on Mar. 24, 1998, entitled "Radiation Curable Sealant Compositions". The disclosure of the aforementioned Provisional Patent Applications is hereby incorporated by reference.
The subject matter of the instant invention is also related to copending and commonly assigned Non-Provisional U.S. patent application Ser. No. 09/344,198, filed on Jun. 24, 1999, Ser. No. 09/300,930, filed on Apr. 28, 1999, Ser. No. 09/081,967, filed on May 20, 1998 and Ser. No. 09/197,124, filed on Nov. 20, 1998 and entitled "Novel Foaming Composition and Methods for Making and Using the Compositions". The disclosure of these commonly assigned patent applications is hereby incorporated by reference.
The invention relates to a curable composition, methods for applying the composition as well as end-uses for the cured composition.
Sealants are employed in a wide range of applications. For example, the automotive industry employs sealants between and upon metal seams and welds, within hollow cavities to impart structural and sound damping characteristics, among other locations.
One specific sealant environment involves the use of a sealant upon the welds in the so-called "roof-ditch" which is formed when joining the side panels of the body to the roof of the vehicle. The roof-ditch weld is conventionally covered with a bead or strip of polyvinyl chloride (PVC) based molding that is typically covered with a metal strip and painted. The PVC strip typically contains plasticizers, stabilizers. lubricants, among other compounds that can volatilize from the strip thereby causing cracking and shrinking. When the PVC strip cracks such can reduce the effectiveness of the strip and in turn allow the underlying metal to corrode.
Conventional sealants including those employed in roof ditches can also create conditions which are conducive to microbial, e.g., fungal, growth: especially in warm humid environments. The microbe growth occurs because the sealant contains substances that can be metabolized by the microbe. Consequently, there is a need in the sealant industry for a sealant with enhanced durability, and microbial resistance and cosmetic value that can be applied in an expedient manner. There is also a need in this industry for a sealant that can be repaired or replaced.
Methods for applying and curing/heating coatings are described in U.S. Pat. No. 4,844,947 (Kasner et al.), U.S. Pat. No. 5,348,604 (Neff) and U.S. Pat. No. 5,453,451 (Sokol). The disclosure of the previously identified patents is hereby incorporated by reference in their entirety for all purposes.
This invention is capable of solving problems associated with conventional practices by providing a radiation curable composition, which can be employed as a sealant that is easy to manipulate, durable, paintable, repairable/replaceable, crack and microbe resistant, e.g., mildew.
The inventive composition can be employed in a wide range of environments including in the automotive industry, e.g., as a roof-ditch sealant. The composition of the invention can be applied by using commercially available dispensing equipment, e.g., brushing, dipping, spraying or pumping, and cured in-situ, e.g., by a source of energy or radiation such as UV radiation, electron beam, laser, microwave, among other energy sources sufficient to cause curing sufficient to control sag or material flow for a specific application. If desired, the inventive composition can be painted.
In one aspect, the curable composition according to this invention comprises at least one epoxy compound, at least one carrier, e.g., polyol, and at least one suitable photoinitiators. In addition, the curable composition can optionally include at least one thickener or filler, as well as at least one monomers and/or at least one phenoxy resins. In one embodiment, the inventive composition can comprise: 1) at least one epoxy such as that supplied by UCB Radcure as Uvacure 1500, 1530, and 1534 or by Sartomer as SARCAT K126, 2) at least one and preferably two or more polyols such as the polyester polyols supplied by Union Carbide as Tone 0301 and by Huls America as Dynacoll 7110, 3) at least one photoinitiator such as sulfonium salt supplied by Union Carbide as Cyracure UVI 6974 and by Sartomer as CD 1010; and optionally, the following additional three components, 4) at least one thickener or filler such as silicon dioxide supplied by Cabot Corporation and 5) at least one monomer such as TONE M-100 also supplied by Union Carbide, a hydroxy polyester acrylate/hydroxyethyl acrylate blend or a monomer such as caprolactone acrylate supplied by Sartomer; and 6) at least one phenoxy resin such as phenoxy resin such as phenoxy resin PKHP 200 supplied by Phenoxy Specialties.
In another aspect, the curable composition is pre-initiated before contacting the substrate. By "pre-initiated", "pre-initiating" or "pre-initiate(s)" it is meant exposure to a suitable source of energy or radiation at least once: 1) while combining the components of the composition, 2) when preparing at least one component of the composition prior to combining with other components, 3) during transport of the composition or components thereof through a conduit or related handling equipment, among other suitable techniques to pre-initiate curing of the composition. If desired, the composition can be pre-initiated by a radiation source that is embedded or located within or upon a conduit or other member such that radiation can be supplied to the composition or components thereof, e.g, UV radiation is shown through a window on a conduit that delivers the composition to a substrate. The radiation source may also be embedded within the system for dispensing the composition, e.g., a UV source located within a nozzle that applies the composition onto a substrate. Pre-initiating the curable composition permits controlling the viscosity of the composition as well as reducing the curing time after being applied onto a substrate.
These and other aspects of the invention will become apparent from the specification and claims which follows.
A first aspect of the invention relates to a radiation curable composition comprising at least one epoxy, epoxy based compounds and epoxy functional or modified compounds, at least one carrier, e.g., polyols, and at least one photo-initiator.
The first of the components employed in the curable composition comprises an epoxy compound. While any suitable epoxy and epoxy functional compounds (or mixtures thereof) can be employed in the inventive composition, a curable liquid cationic epoxy compound and, in particular, a cycloaliphatic epoxy compound is preferred. Specific examples of suitable epoxy compounds comprise those materials supplied by UCB Radcure as Uvacure 1500, 1530, and 1534 or by Sartomer as SARCAT K126. Normally, the epoxy corresponds to about 40 to about 90 wt. % and preferably about 45 to about 60 wt. % of the composition prior to curing.
Without wishing to be bound by any theory or explanation, it is believed that the inventive composition employs a cationic reaction that can be photoinitiated, that continues as a cascade reaction; especially if heated. It is also believed that when the inventive composition is exposed to a source of suitable radiation, e .g., UV energy, a relatively thin "skin" forms substantially instantaneously upon the surface of the composition. This surface skin serves to stabilize the shape of the composition until the remainder of the composition has reacted, e.g., cross-linked, into a self-supporting structure. The thickness of the skin as well as the resultant article can be tailored to satisfy a particular end-use, e.g, an article having a thickness of from about 0.05 to at least about 10 mm as well as forming a skin upon an underlying uncured material.
While not necessary to obtain a useful composition, the effectiveness of the aforementioned epoxy compound is enhanced by the second component of the composition, at least one polyol. While it is believed that any polyol recognized in the art can be suitably employed in the invention, examples of preferred polyols comprise polyether polyols and polyester polyols such as those supplied commercially by manufacturers such as Union Carbide, Huls America and Arco. Specific examples include polyester polyols supplied by Union Carbide as Tone 0301 and by Huls America as Dynacoll 7110. The amount of polyol in the composition prior to curing preferably ranges from about 5 to about 50 wt. %, more preferably 10-25 wt. %.
Moreover, the epoxy to polyol ratio can range from about 1:1 to about 2:1. The use of more than one polyol is desired. By employing more than one polyol, the properties of the inventive composition can be more effectively controlled. Examples of properties that can be tailored include glass transition point, viscosity. adhesion to the underlying substrate (e.g., in the case of a roof ditch the automotive E-coat), degree of cross-linking in the cured composition, flexibility, among other desirable properties.
A photoinitiator is employed in the composition when using UV radiation for inducing an interaction among one or more components of the curable composition, typically the epoxy and polyol. The amount of photoinitiator normally corresponds to about 0.5 to about 2 wt. % of the composition prior to curing. While any suitable photoinitiator or mixtures thereof can be employed, UV photoinitiators are preferred. In particular, desirable results have been obtained by using a onium salts such as sulfonium salt, triarylsulfonium hexafluoroantimonate, diaryliodonium hexafluoroantimonate, and mixtures thereof, among others. Specific examples of suitable sulfonium salts include those supplied by Union Carbide as Cyracure UVI 6974 and by Sartomer as CD1010.
In another aspect of the invention, the photo initiator can be partially or completely replaced by an acid source such a Lewis acid. Examples of suitable Lewis acids include sulfonic acids, phosphoric acid, citric acid, carboxylic acid, tannic and oxalic acids, and mixtures thereof, among others. Normally, better results are obtained by using a source of phosphoric acid. In this aspect of the invention, the composition is employed in a two component system with the epoxy compound and the acid source being separately maintained until it is desirable to produce a self-supporting coating or an article. When the epoxy and acid are contacted a reaction occurs providing a product similar to the one described herein when a photoinitiator is used. The amount of acid normally corresponds to about 0.25% to about 3.0% wt. % of the composition prior to curing. The epoxy and/or acid can be admixed with other components of the inventive composition, e.g., the acid can be admixed with a polyol.
The ingredients of the two component system can be combined by using any art recognized mixing technique while ensuring that two components are segregated prior to usage. The components can be contacted either by hand in a suitable container, or dispensed through a commercially available static mixing tube and simultaneously applying the resulting fluid onto the substrate in question.
The curable compositions according to the invention can include other optional components depending on, among other factors, the ultimate end use of the cured material. To this end, at least one thickener or filler can be included as an optional component of the inventive composition. The amount of thickener normally corresponds to about 0.5 to about 5.0 wt. % of the composition prior to curing. While any suitable thickener can be employed fumed or aerosol silica can be used to obtain desirable results, e.g., fumed silicas commercially supplied by Cabot Corporation (M-5 Grade) and Degussa. Normally, precipitated silica is not employed.
The thickener is typically non-reactive and employed to create a thixotropic fluid, e.g., having a viscosity of about 20,000 to about 80,000 centipoise. Consequently, the thickener can be introduced into the composition in any expedient manner, e.g., added to the polyol and vacuum mixed. If desired, the thickener can comprise a treated silica such as a silica having a silane surface treatment, e.g., TS720 supplied by Cabot Corporation.
The viscosity of the composition or components thereof can also be modified by exposure to a radiation source, e.g., by pre-initiating the composition. Exposure to a radiation source causes at least a portion of the composition or components thereof to cure thereby causing an increased viscosity.
In addition, the curable composition can include a monomer component to facilitate formation of the cured material. Examples of suitable monomeric materials comprise acrylates, caprolatones, polycarbonates, and mixtures thereof, among others. The amount of monomer typically comprises about 1 to about 5% by wt. of the composition prior to curing. Without wishing to be bound by any theory or explanation, it is believed that the monomer component functions as a cross-linking agent during curing.
Yet other additives can also be included in the curable composition. Depending upon the inventive composition and particular end-use of a substrate which is coated with the inventive composition, suitable additives can comprise: bis-F epoxy, thickeners. fillers such as carbon black, polyproplyene, proplyene carbonate. calcium carbonate. microspheres (such as Micropearl, supplied by Pierce & Stevens. Corp.); surfactants, pH indicators, biocides/antifungal compounds, solvents, fire extinguishants, silanes. pigments, UV stabilizers, PVC, PTFE, resins such as ethylene-vinyl acetate co-polymers, among other compounds which do not adversely impact curing.
The additives should be selected so as to not effect transmission of the curing radiation. For example, when employing a UV curable system, best results are obtained by avoiding materials that affect UV light transmission. Because of this, the two component system and systems activated by an electron beam or other energy sources can include a wider range of materials such as dyes, pigments, UV light stabilizers, among others. While any suitable pigment can be employed, specific examples of pigments comprise at least one member selected from the group consisting of E2557 Green, E6824 Yellow, E4102 Red, 626 blue (all supplied by Akrochem) mixtures thereof, among others. Examples of suitable UV 1 stabilizers comprise at least one member of Oxalanilide class, mixtures thereof, among others. The amount of such additives. if present, normally comprises about 0.1 to about 2.0 wt. % of the composition, prior to curing.
If desired, the inventive composition can include fibers, platelets, particles, among other components in order to form a composite article. Typically, the amount of such additives will range from about 1 to about 15 wt percent of composition prior to curing. Normally, it is desirable to minimize the presence of basic materials and/or those that affect UV transmittance when a UV curable system is employed.
The uncured composition can be provided by any suitable means for admixing or combining the components of the composition. Normally, at least one of the epoxy or polyol will be heated to a temperature that is effective for increasing the rate at which the thickener, e.g., silica, can be dispersed. Bubbles formed during the mixing process can be removed by pulling a vacuum on the mixture. Greater details regarding the mixing process can be found in the forthcoming Examples.
A specific example of a curable composition according to this invention comprises the following:
The inventive composition can be applied and cured effectively at ambient temperatures. e.g., about 65 about 95° F., thereby obviating the need to heat the composition during application. In some cases, however, it may be desirable to monitor and control the curing temperature if ambient temperatures are extreme. By obviating the requirement for heat curing, the instant invention permits utilization of unheated dispensing equipment as well as application upon unheated substrates.
The particular substrate is not critical to the invention and clearly depends on the end use for the cured materials. Examples of suitable substrates can comprise one or more of steel, stainless steel, galvanized surfaces, surfaces having a coating such as E-coat, paint, among a virtually unlimited array of substrates. While heating is not necessary to apply the composition, once applied the cured composition can be baked or heated for improving the adhesion of the composition to the underlying substrate. For example, a source of infrared energy can be employed in combination with a source of UV or electron beam radiation, e.g., a UV lamp.
Curing of the inventive composition can be initiated via a source of radiation suitable for activating the photoinitiator. Since the use of UV curable initiators is preferred, the preferred radiation source provides ultraviolet radiation (UV). To this end, while curing can be initiated by naturally occurring UV light, normally, a man-made source of UV radiation is employed, e.g., to cross-link the polymeric matrix. The source of UV radiation can range widely such as a lamp mounted above a conveyor, a lamp mounted on a robot arm, a series of lamps mounted in a gantry located above or adjacent to a robot that dispenses the composition, among other apparatus for supplying UV radiation.
After applying the inventive composition upon a suitable substrate, the composition can be exposed to a high output source of energy, e.g., UV radiation (approx 2.5 J/cm2 @ 365 nm, which may vary with exposure time, distance from source and type of bulb), that initiates curing thereby locking or freezing the composition as a coating upon the substrate. The specific wavelength of UV can be tailored to satisfy a wide range of product uses, exposure times and distance from the composition to be cured; but, normally ranges from greater than about 250 to about 400 nm and having an output of about 2.5 to about 4.0 J/cm2. In some cases, it is desirable to employ one or more UV sources that emit differing UV wavelengths either simultaneously or sequentially. e.g., lamps that emit differing wavelengths and/or by one type of lamp having a filter. Examples of suitable UV curing systems and lamps are Model F600 System, "D", "V" and "H" lamps all of which are supplied by Fusion Systems Corporation, Rockville, Md.
The radiation exposure time of the inventive composition is typically about 1 to about 10 seconds. The specific exposure time can be tailored depending upon the distance from the radiation source, intensity of the source, relative speed between the composition to be cured and the radiation source, among other parameters. As described above, the source of, e.g., UV radiation, can be supplied by any suitable means such as a conveyor, UV lamp such as a Fusion Systems "H" bulb attached to or associated with an arm of a robot which dispenses uncured composition, e.g., as a bead within a roof ditch or a spray upon a substrate. Consequently, the inventive composition can be readily employed in conventional fabrication or manufacturing processes. Typically, a safety curtain or booth, which surrounds the radiation source, is desirable for minimizing any impact upon personnel. When the composition is employed in automotive applications such as a roof ditch, the radiation (UV) curing step can be followed by a thermal bake, which enhances formation of a permanent adhesive bond to the underlying surface, e.g., an electrocoat (E-Coat), and improves the final curing of the sealant's polymer matrix. The thermal bake is typically conducted at a temperature greater than about 340° F. and less than that which adversely impacts the coated substrate. While a thermal bake is not required for all applications of the inventive compositions, such a thermal bake can enhance the adhesion between the inventive composition and the underlying surface, and if desired can be employed in conjunction with radiation (UV) exposure.
The inventive composition also has the ability to cure with ultraviolet rays from the sun. While the sun can be employed as a source of UV radiation, the cure time is relatively long in comparison to curing with concentrated/high energy UV sources. Examples of applications that can employ natural UV curing include the building/construction industry such as roof panel joints for metal building, skylight seals, concrete/cement sealants, drywall joint-compound ("mud"), among other applications exposed to natural UV radiation. For example, the inventive composition can be applied or sprayed upon concrete/cement and cured in natural UV to form a water-proof paintable coating, e.g., an interior or exterior basement sealant and a swimming pool liner or seal.
Subsequent operations to the coated substrate will typically not disturb the coating, e.g., when the coating is employed as an automotive roof ditch sealant the coating will not drip or run during subsequent manufacturing steps such as painting. The long term dimensional stability of the cured inventive composition is improved in comparison to conventional PVC sealant compositions, e.g., no cracks or shrinkage become evident during UV exposure and repeated thermal bakes or environmental exposures. When shrinkage was measured substantially in accordance with ASTM D2453, the inventive composition had a shrinkage of about 0% when measured visually.
The inventive composition is a high cosmetic paintable material (a so-called Class A automotive). With proper application, the sealant provides excellent smoothness and gloss retention, e.g., the inventive sealant does not adversely impact the distinctiveness of image (DOI) of an overlying paint. When deposited within a channel or groove the cured composition typically forms a reverse miniscus, or "U-shaped" cross section. Such a configuration reduces paint cracking; especially when the inventive composition is employed for sealing automotive roof ditches.
The inventive composition possesses an improved adhesion to conventional paint systems such as standard solvent based pigmented and clear systems, water based, latex, powder paints, automotive E-coats, mixtures thereof, among others. The inventive composition also possesses a desirable resistance to the ambient environment, e.g. twelve month Florida exposure testing in accordance with conventional testing methods has proven the inventive composition's durability as well as its resistance to mold/mildew growth, cracking and chalking. The inventive composition is also resistant to paint staining, fading and cracking as a result of Xenon Arc exposure.
The chemistry of the inventive composition allows the composition to be tailored to possess a wide variety of physical characteristics. By utilizing the constituent ratios of the composition, the physical characteristics of the cured product will range from a flexible and relatively soft article to a hard sandable product. These characteristics can be obtained by varying the epoxy to polyol weight ratio e.g., the ratio can range from about 2:1 to about 4:1. Normally, an increased amount of epoxy will correspond to a harder cured coating. When the composition contains relatively large quantities of polyol, the hardness of the cured coating is reduced upon exposure to moisture, e.g, the Shore "A" Hardness when determined in accordance with conventional measuring techniques ranges from about 70 to at least about 95. The presence of relatively large quantities of polyol can, however, improve adhesion of the inventive composition to the underlying substrate.
The hardness of the composition can be increased by including a hardening resin such as a phenoxy resin. While any suitable hardening resin can be employed, examples of suitable resins comprise at least one member selected from the group consisting of phenoxy resin, solid epoxy (in particulate form), mixtures thereof, among others. Normally, the amount of hardening resin corresponds to about 1 to about 9 wt. % of the composition prior to curing. By including such a hardening resin, the Shore "D" hardness of the composition, subsequent to curing, can range from about 60 to about 80. The hardening resin also improves the solvent and moisture resistance of the cured composition.
In addition, the viscosity of an uncured composition can be tailored by adjusting the silica to polymer ratio and/or the polyol ratio. The viscosity of the uncured composition can also be increased by introducing a solid epoxy in addition to or as a replacement for the aforementioned epoxies. Examples of suitable solid epoxies comprise bis-phenol A, novalac resin, mixtures thereof, among others. The viscosity can be tailored to be similar to paint, or increased to a grease or paste-like consistency. The presence of a solid epoxy can also be employed for imparting enhanced resistance to moisture.
The inventive composition, prior to curing, is typically greater that 95 wt. %, preferably, about 98.5 to at least about 99.75 wt. % solids, e.g., about 99.5 wt. % solids. While the dimensional thickness of the inventive composition can be tailored to satisfy a wide range of end-uses, normally the composition is applied at a thickness of about 0.05 mm to about 10 mm thick, e.g., in the case of roof ditch the composition is about 5 mm thick. The ability of the inventive composition to form such relatively thick layers is in contrast to conventional practices and a marked improvement.
While the inventive composition is not adversely affected by most solvents, the composition can substantially reduce, if not eliminate, the presence of solvents, e.g., the inventive composition can be essentially volatile organic compound (VOC) free. The inventive can also be substantially free of polyvinyl chlorides and its monomers. That is, the uncured composition may include about 0.1 to about 5.0 wt. %. normally about 0.5 wt. %, of solvents and/or PVCs, e.g., a solvent which functions as a carrier for the photoinitiator, e.g., about 0.50 wt. % propylene carbonate.
As described above, the inventive radiation cured composition can be employed in a wide range of applications; especially in the automotive field. One such example comprises a roof ditch sealant which is a Class A paintable sealer. Once the inventive composition is applied, the composition is cured in situ by a source of concentrated UV light thereby permitting an "in-line" curing application. That is, a robotic arm can be a double functional tool, with both a dispensing nozzle for delivering the inventive composition into a roof ditch and the curing lamp attached in parallel. Alternatively, the curing lamp(s), e.g, one or more UV and infrared lamps, can be physically separate but operationally connected to the robot, e.g., the lamps are mounted above or beside the robot on a gantry wherein the movement/operation of the robot and lamps are controlled by computer. The inventive composition can be supplied to the robot arm by using any suitable pump such as a positive displacement reciprocating piston pump, e.g., Model No. 711008-662-000 5 gal. pump supplied by Graco Inc.
In one particular aspect of the aforementioned roof ditch application, a plurality of protrusions, studs or mechanical fastening means having any desirable shape can be located within and attached to the bottom of the ditch for enhancing the bond between the ditch and overlying radiation cured composition. When studs are employed, the studs can be welded within the ditch when forming the underlying weld that forms the ditch. e.g, when welding the automotive roof and side body panels together. Any protrusions can also be affixed within the ditch by a suitable adhesive, or by mechanical attachment. The height and specific configuration of the protrusions depends upon the application: but, normally, the protrusions are about 3 to about 7 mm tall. These protrusions can be fabricated from any suitable material such as thermoplastics such as nylon, metal. among other materials. When introduced into the ditch, the inventive flowing composition embeds the protrusions, fills the ditch and can form a self-leveling surface. These protrusions can also be utilized in after-market applications when repairing or replacing a roof ditch sealant.
The configuration of the roof ditch can be tailored for improving the mechanical bond between the ditch and radiation cured composition. For example, a ditch having trapezoidal cross-section can be employed. If desired, the previously described protrusions or studs can be employed within a tailored ditch configuration.
The inventive composition can also be applied upon non-planar surfaces. For example, the inventive composition can be employed as a Class A paintable automotive coach and coach joint sealant. Such joints can be on a horizontal or vertical surface. The ability of the inventive composition to be cured substantially simultaneously following application permits the composition to be employed on such vertical surfaces. In order to enhance vertical surface application, the viscosity of the inventive composition can be increased by adding about 3 to about 10 wt. % of a thickener such as CAB-O-SIL silica, elastomer modified or adducted epoxy, polyether polyol, mixtures thereof, among others.
Moreover, the inventive composition can be employed for repairing dents and scratches in a painted surface, e.g., an automotive door. That is, the composition can be applied upon a surface, exposed to a radiation source such as UV light, and, thereafter, sanded as needed and painted in accordance with conventional methods. Similarly, a two component system can be employed without using exposure to a radiation source. For example, a two component system based upon an interaction between an epoxy and acid can be combined, applied upon a surface as a gel, permitted to harden and adhere to the surface and, thereafter, prepared for painting by using conventional techniques. In some cases, the substrate being repaired and/or inventive composition can be heated to enhance adhesion to the substrate.
The inventive composition can be applied onto a wide range of substrates. The inventive composition can be employed in a method for applying one or more coatings upon an automotive surface. For example, an automotive assembly may be immersed within the inventive composition and, thereafter, cured by being exposed to radiation. Such an immersion may be employed, for example, as an enhancement or a replacement for conventional automotive E-coats. Once cured, the automotive assembly can be painted in accordance with conventional methods. Without wishing to be bound by any theory or explanation, it is believed that the composition may be tailored for application upon unpainted surfaces as a corrosion protectant, e.g., sprayed upon an automotive underbody, among other applications.
In one aspect of the invention, the inventive composition can be employed as an automotive brake rotor coating for imparting corrosion protection. The inventive composition can be applied via an aerosol or a spray upon the rotor to form a thin film coating. The resultant layer is sacrificial in that the layer is consumed or removed when contacted by the brake pad. In a related aspect, the inventive composition can be employed as a temporary corrosion protectant such as upon saw blades wherein friction or other usage of the protected article removes the coating. In such cases, it can be useful to add one or more surfactants, e.g., less than about 1.0 wt. % of Fluorad FC-171 fluorochemical available from 3M.
In another aspect of the invention, the inventive coating is employed as a Class B paintable coating. For example, the inventive coating is applied as a spray upon a painted or unpainted metal substrate such a lower automotive body panel in order to form an anti-chip coating (so-called stoneguard). The inventive composition can also be sprayed upon the floor pan, roof, among other regions of an automobile during assembly for improving acoustics, among other properties.
In another aspect of the invention, the inventive composition can be mixed. molded, extruded or shaped into an article that is subsequently exposed to a radiation source. If desired, the inventive composition can be co-extruded with another material thereby forming an article having a radiation curable surface. While a wide range of articles can be formed, one example of such an article comprises automotive moldings. Such moldings can be fabricated and shipped to an automotive assembly plant, or extruded and cured directly on the automobile.
Moreover, the inventive composition can be shaped into hollow spheres or other continuous surfaces by being shaped while being exposed to a source of radiation. The inventive composition can be sprayed/spray dried in a conventional manner while being exposed to radiation. The resultant spheres or product can be employed alone or incorporated into another matrix to obtain a composite. Similarly, the inventive composition can be cast into a film or web.
In a further aspect of the invention, the inventive composition is employed as a repair material for automotive coatings, seals, household applications, among other areas wherein it is desirable to have long-lasting, flexible and paintable sealants. For example, the inventive composition can be applied upon a substrate, cured with radiation and exposed to infrared (IR) radiation for 90 seconds thereby forming a seal to repair a crack in the underlying substrate or coating.
In a still further aspect of the invention, the inventive composition can be employed as a top-coating upon a wide range of articles including fasteners, end-fittings, couplings, among others. These articles can be immersed within the inventive composition, centrifuged (so-called dip-spin processing), and exposed to a radiation source thereby curing the composition and forming a durable outer or top-coating upon the articles.
The previously described curable compositions can be modified to obtain a gel consistency by adding a gelling agent. Examples of suitable gelling agents include treated or untreated silica, detergents, elastomer modified or adducted epoxy, polyether polyols, mixtures thereof, among others. When using a UV curable composition, the gelling agent should not adversely affect UV transmission through the composition. The gelling agent normally comprises about 0.5 to about 10 wt. % of an uncured compositions. By employing a gelling agent, the viscosity and handling characteristics of the inventive composition can be improved, e.g., the composition can be tailored to possess a putty or caulk-like consistency.
Moreover, the curable compositions can be modified to obtain an acid or radiation activated foam. Any suitable chemical or mechanical expansion agent can be added to these compositions. Examples of suitable chemical or mechanical expansion agent include water, hydrazide, diphenyloxide-4,4-disulphohydrazide, hexamethylene diamine carbamate, carbonamide, azocarbonamide, sodium bicarbonate, carbon dioxide, fluorocarbons, encapsulated materials, e.g, Expancel® supplied by H.M. Royal; mixtures thereof, among others. The expansion agent normally comprises about 0.5 to about 10 wt. % of an uncured compositions. The expansion agent becomes activated by being exposed to either UV or a suitable source of heat, e.g, an exothermic reaction between an epoxy and acid source. For example, when employing a UV curable composition and such a composition is exposed to UV light an exothermic reaction occurs that in turn causes the expansion agent to swell thereby increasing the volume of the composition. Similarly, when an acid activated composition is employed, the heat released when the acid contacts the epoxy causes the expansion agent to swell. Radiation activated foams are described in greater detail in copending and commonly assigned U.S. patent application Ser. No. 09/344,198, filed on Jun. 24, 1999 and entitled "Novel Foaming Composition and Methods for Making and Using the Composition"; the disclosure of which is hereby incorporated by reference.
While the above description places particular emphasis upon applying the inventive composition within an automotive roof ditch, the inventive composition can be applied to a wide range of substrates. Examples of suitable substrates include at least one member of the group consisting of metals such as stainless steel, galvanized steel. concrete, cement, glass, wood, among others. In the case of metal substrates, the inventive composition can be applied upon a welded joint including a joint formed by spot, wire and laser welding.
The composition of the instant invention can be applied to a substrate by any suitable method. Such methods include brushing, immersing, pumping, dipping, painting, spraying, among other suitable conventional methods. When the inventive composition is applied upon the weld in an automotive roof ditch, it is desirable to pump the composition into and along the ditch. Because of its low viscosity at, for example, at 77° F., the composition and its thixotropic behavior, equipment such as a reciprocating piston (positive displacement) pump, gear pump, pneumatic tube (such as that supplied by SEMCO), caulking tube (hand trigger), air or airless spray, squeeze tube, brush, among other commercially available equipment, may be used. The uncured composition may then be manipulated further, e.g., pressed or embossed, into a desired finish.
The inventive composition, once applied, is normally cured with a suitable, e.g., UV, radiation source. This can be done immediately upon application to a substrate, or delayed depending upon the characteristics desired in the coated substrate. For example, by delaying the cure, the composition can be shaped, or leveled/smoothed to better conform to the underlying substrate. As aforementioned, the cure may be followed by a bake, or allowed to finish curing naturally. The sealed joint or coated substrate may now be painted or otherwise finished. If desired, one or more layers of compositions which are chemically similar or distinct can be applied upon a cured composition, e.g. two or more layers of UV cured composition can be applied sequentially or used to form a laminate structure.
One method for applying the inventive composition is illustrated by the Drawings. Referring now to
More details regarding one method for applying the inventive composition are shown by FIG. 2. Referring now to
While the above description emphasizes curing an epoxy containing compound by exposure to a suitable radiation source, the inventive method can be achieved by employing other polymer systems such as silicones, urethanes, silanes, hydroxyl or caboxyl modified elastomers; hydroxyl, carboxyl or epoxy functional compounds, reactive liquid polymers such as Hycar®, among others. That is, a polymer system which when exposed to a suitable source of radiation including pre-iniating causes at least a portion of the system to cure.
The following Examples are provided to illustrate not limit the scope of the invention as defined by the appended claims. Unless indicated otherwise, the materials and equipment discussed below are commercially available.
The exemplary compositions were obtained by blending its constituents. The following equipment was employed for blending the constituents:
1) Heated mixing Vessel of suitable volume (50-300 gal)
2) Mixer (Rotor-Stator, or Dispersion Blade, or Double Planetary Paddle)
3) Vacuum
4) Heated Liquid Pump
5) Unheated Liquid Pump
6) Weight Scale
7) Shipping Container Filling Equipment (Tube, Pail, or Drum)
Blending began by pumping into the mixing vessel polyester polyol (Dynacoll 7110) at 250 F. One-hundred fifty-four pounds of a second polyester polyol (Tone 0301) was added to the mixing vessel. The polyols were blended until both polyol constituents are fully dissolved in each other. The polyol mixture is substantially transparent. The temperature within the mixing vessel was maintained at 180 F.
One-hundred thirty-five pounds of cyclaliphatic epoxy (Uvacure 1500) was then added to the mixing vessel. When all of the epoxy was uniformly mixed, 3.3 pounds of sulfonium salt (UVI-6974) were added to the vessel. Mixing was continued at a temperature of 180 F for 10 min.
Eleven pounds of silica (Cab-O-Sil) was then added to the mixing vessel. The silica was stirred into the mixture until wetted. Then another 11 pounds of silica (Cab-O-Sil) is added. Mixing was continued to fully dispersed the constituents of the vessel. Mixing was then performed at high shear rate under vacuum until substantially no lumps and no air bubbles were visible. It was important to eliminate all air bubbles, for they may cause a discontinuity in the delivery line during customer application, and therefore an undesirable inconsistent delivery.
When vacuuming was completed, the resultant mixture was warm and clear with a consistency of syrup. When the batch is cooled and the shear stresses diminished. the mixture was thickened to a near gel state while maintaining clarity. For best results, shipping or storage containers should filled prior to cooling.
After the containers are filled and material cooled, specific gravity and viscosity checks should be performed to insure batch quality. For best results and in order to avoid premature curing of the composition, all storage and shipping containers should be opaque or shielded from UV sources including sunlight and fluorescent lighting. Such exposure could result in cure initiation thereby preventing the contents from being pumped.
One inventive composition was produced in accordance with the following method. A two (2) gallon Ross Model PD2 planetary dispersion mixer was obtained and in connected to a Chromolox heater. The dispersion mixer was operated at a temperature of 190 F.
2824 grams of liquid polyol (Tone 0301) and 888 grams of the solid polyol (7110) were introduced into the mixer and mixed for 10 minutes. Sixty (60) percent (240 grams) of the silica thickener (Cabosil supplied by Cabot Corporation) was introduced into the mixer and the combination was mixed for another 10 minutes.
500 grams of epoxy (Uvacure 1500) and the remaining 40% (160 grams) of the silica were then added and mixed for 10 min. This was followed by adding 60 grams of the photoiniatitor (Cyracure 6974) and 2172 grams of epoxy (UVACure 1500) to the mixer and mixed for 5 minutes. The contents of the mixer were then mixed under vacuum for 10 minutes thereby producing 1.3 gallons of the inventive composition.
222 g of polyester polyol (Dynacoll 7110) at a temperature of 250 F were poured into the a gallon can. About 706 g of a second polyester polyol (Tone 0301) were added to the first polyol. The polyols were blended in a Rotor-Stator Mixer. This until both constituents are fully dissolved in each other. The mixture was transparent at this point. The temperature of this mixture was maintained at 180 F.
Approximately 618 g epoxy (Uvacure 1500) were admixed with the heated mixture. When all epoxy was uniformly mixed, 15 g of photoiniator (UVI-6974) were added. Mixing continued at a temperature of 180 F for 10 min.
To the mixture, about 50 g of silica (Cab-O-Sil) were added. The mixture was stirred until the silica was wetted into the mix. An addition 50 g of silica (Cab-O-Sil) was combined with the mixture while continuing mixing until the silica was fully dispersed.
The mixture was transferred to a vacuum chamber and maintained under vacuum until all bubbling ceased in the mixture. About ˝ gallon of the inventive composition was obtained.
The composition described by Examples 2 and 3 was applied to a metal substrate and cured in accordance with the instant Example. An ASEA Model 2000 Robot having a movable arm was employed to control the position of a SEMCO Dispensing tube. Movement of the arm was controlled by a ASEA (ABB) computer and software. Approximately 12 oz. of the inventive composition was applied at 40 psig via a Pyles High Flow Robot Gun that was mounted on the robot arm. The composition was dispensed through a round nozzle, approx. 1 cm. in diameter and cured subsequently by a shuttered UV lamp (1600 watt lamp) that was also attached to robot arm. A schematic drawing of this system is shown by aforementioned
The inventive composition was also applied from the robot arm by using a Pyles 5 gal. unheated pump (instead of the SEMCO tube), to supply the composition. A Pyles "snuff back" gun Model #12000 series was also substituted for the previously identified high flow gun. The gun also included a modified flattened nozzle that applied a ribbon stream of composition upon the substrate.
A UV curable composition comprising the following components was prepared:
The composition was prepared in a Ross DB-2 mixer and in accordance with the following method:
A UV curable composition comprising the following components was prepared:
The composition was combined in a Ross mixer and in accordance with the following method:
The temperate used for mixing in Examples 5 and 6 can range from about 150 to at least about 190 F. Acceptable results can also be obtained from formulations of Examples 5 and 6 that contain about 75 to about 95 wt. % epoxy and up to about 10 wt. % polyol and resin.
A UV curable composition comprising the following components was prepared:
The composition was combined in a Ross DB-2 mixer and in accordance with the following method:
A UV curable material comprising the following components was prepared:
The composition was prepared by combining the Uvacure 1500 and Tone 0301 in a mixing vessel. The mixture initially exhibited turbidity. The mixture was stirred until turbidity disappears and visually appears clear. The UVI-6974 and the Fluorad FC-171 were added to the mixture. Mixing was continued until the components were completely dispersed which occurred in about two minutes. The mixture was subjected to a vacuum to eliminate entrained air. The mixture was tested in accordance with conventional procedures and possessed the following characteristics:
One desirable characteristic of this composition is that it can be applied to a substrate via spraying, e.g., by using a commercially available air or airless spray gun.
A UV curable gel comprising the following components was prepared:
Gel A was prepared by mixing the Uvacure, Epalloy, and Tone together in a mixing vessel until the solution was clear. The UVI 6974 was added, and mixed until the components were dispersed (about 2 minutes). The Cab-O-Sil was added to the mixture to function as the gelling agent, and mixed until substantially lump-free. A vacuum was applied to the mixture until substantially all the air was removed (27 mm Hg, 10 minutes).
Gel B was prepared by mixing the Uvacure and Tone together in a mixing vessel until the solution was clear. The UVI 6974 was added, and mixed until the components were substantially dispersed (about 2 minutes). The Cab-O-Sil was added to the mixture and mixed until substantially lump-free. A vacuum was applied to the mixture until substantially all of the air was removed (27 mm Hg, 10 minutes). Mixture was gel-like, but was not self-supporting. A gelling agent comprising a surfactant was added to the gel-like mixture. A gel, thereafter, formed rapidly.
Gel C was prepared by mixing the Uvacure and polyol together in a mixing vessel until solution is clear. The UVI 6974 was added, and mixed until substantially dispersed (about 2 minutes). The Cab-O-Sil was added to mixture and mixed until the mixture was substantially lump free. A vacuum was applied upon the mixture until substantially all of the air was removed (27 mm Hg, 10 minutes).
The following Table lists the Brookfield Viscosity Data for Gels A, B and C (cps, in thousands) measured at 20 C using a number 6 spindle as a function of revolutions per minute (RPM).
A UV curable foam having the following components was prepared:
The above components were combined as follows. The Uvacure and polyol were added together in a mixing vessel and mixed until the solution was clear. The UVI 6974 was added to the mixture, and mixed until substantially completely dispersed (about 2 minutes). The Expancels spheres were added to the mixture and mixed until substantially lump free. For best results, the minimum amount of mixing time, and shear were employed
A UV curable composition comprising the following components was prepared:
This composition was prepared by heating the Uvacure, Epalloy, Dynacoll, and Tone together in a mixing vessel at a temperature of 180 F. The materials were mixed until the solution was clear. The UVI 6974 was added, and mixed until the components were dispersed (about 2 minutes). The Cab-O-Sil was added to the mixture and mixed until substantially lump-free. A vacuum was applied to the mixture until substantially all the air was removed (27 mm Hg, 10 minutes).
This composition was applied onto a bent 4×12 inch that had been coated with an automotive E-Coat, exposed to UV light, painted white, baked and then subjected to a South Florida Inland, 5° South, Direct Weathering Exposure to determine the microbial resistance of this composition. After periods of three months, six months, twelve months and twenty-four months, no mold, mildew or other microbe growth was detected by visual observation.
This Example illustrates a two component system that can be produced without radiation curing. The composition was obtained by contacting Part "A" with Part "B". Part "A" and Part "B" were pre-blended in a mixer and contacted by static mixer. The resulting composition was pumpable, paintable and can be employed for repairing damaged painted surfaces, e.g, an automotive body panel. The following tables list the components of Part A and Part B.
This Example illustrates using a robotic means for applying a UV curable material within an automotive roof ditch in order to seal the underlying weld. The UV curable composition of Example 5 was dispensed into an automotive roof ditch by a computer controlled robot by using a Pyles 5 gallon, reciprocating piston, positive displacement pump, SECO temperature controlled metering system and snuff back robot gun. Two robots were used for this application trial: a) Fanuc model F500 was employed to dispense the composition into the ditch and b) a Fanuc model 420i was employed to transport a UV light source along the ditch to cure the composition. The UV light source comprised a Fusion Systems model T-6, 500 watts/inch, 6 inch bulb, H type, mounted on the arm of the model 420i so that the UV bulb ran parallel to ditch. The composition was dispensed at a rate of 250 mm/sec and the UV light was passed over the dispensed composition at a rate of 250 mm/sec; for a total application and cure time of 30 seconds. The material was applied at ambient temperatures.
The following process steps were used to dispense and cure the composition:
This Example illustrates adding a silane compound to the curable composition of Example 5 for improving paint adhesion, high temperature resistance. e.g., to temperatures of greater than 340 F, among other properties.
A curable composition having the following components was prepared:
The above composition was prepared in a Ross DB-2 mixer and in accordance with the following method:
The mixed composition was applied onto a 4′×12′ ED5100 Electro-painted test panel and cured by exposure to UV light in accordance with Example 13. The cured composition was coated with a powder primer paint.
The powder paint comprised PCBV70100M supplied by PPG, Pittsburgh, Pa. The paint was applied in accordance with conventional practice by using an Eastwood Company applicator (HotCoat coating system part no. 1980) The powder paint coated test panel was baked within one hour of application at 340 F. for 20 minutes. The panel inspected visually and was uniformly coated with no visual defects.
This Example illustrates a pigment containing curable composition. The composition of Example 14 was modified by adding a pigment, E2557 green (or other color supplied by Akrochem). The curable material was applied and processed as in Example 14.
This Example illustrates a radiation curable composition that can be sprayed upon a substrate and subsequently cured. The following composition was prepared in accordance with the method of Example 14.
The above composition was sprayed at a pressure of 80 psi by using a DeVilibis type MBC spray gun onto a painted substrate. The substrate comprised a commerically available automobile body panel that had been painted with tan DuPont Centari Acrylic Enamel. The sprayed coating was cured by exposure to naturally occurring UV radiation.
This composition can be employed in a wide range of end-uses including upon a previously painted surface, e.g. an automotive body panel, for improving abrasion resistance, among other properties of the painted surface.
In an alternative embodiment of this Example, a temporary or removable coating can be applied onto a substrate. The coating can be applied onto a painted surface and, thereafter, either be removed or replaced. This type of coating can be obtained by either applied a surface tension agent, e.g., a commercially available wax or surface protectant, or by adding a relatively high amount of a surfactant, e.g., bis-F epoxy, to the sprayable composition. The removable spray composition can be applied onto a painted or unpainted surface in order to impart temporary protection, e.g., from extreme environment conditions, road hazards, transportation, etc., and, thereafter, removed or reapplied as desired.
This Example illustrates a method for using the UV curable composition formed in accordance with Example 14 to repair surface damage to a metallic surface. The repaired surface can be painted or re-painted.
PROCEDURE 1: Repair of dent, defect or hole in a metal panel
A substrate comprising a commercially available ED5100 laboratory test panel was cleaned with an alcohol/naptha containing wipe and coated in accordance with conventional methods with a DuPont 30S primer and DuPont Centari Acrylic Enamel (OEM recommendations or equivalent Body shop materials should be used).
The UV curable composition was applied by hand/brush and cured by being exposed to UV light so as to provide the curable composition protruding above intended repair area. The UV curable composition can be layered to achieve proper depth where required.
After being exposed to UV radiation, the cured composition was allowed to continuing curing under ambient conditions for a period of 3-4 Hrs. The cured composition was then sanded by hand with 180 through 360 grit sandpaper. The sanded surface was then coated with the aforementioned primer and paint.
Infared or convection heat sources can be used, if desired, for reducing the post cure time, e.g., about 150 to about 200 F.
PROCEDURE 2: Repair of existing sealer in seam.
The sealant applied in accordance with Example 14 was removed by sanding. The damaged area was cleared of dust or any other residue and cleaned with an alcohol/naptha wipe (any other suitable cleaner can be employed). The UV composition was applied by hand/brush and cured by being exposed to UV light so as to provide the sealer protruding above the surrounding area.
After being exposed to UV radiation, the cured composition was allowed to continuing curing under ambient conditions for a period of 3-4 Hrs. The cured composition was then sanded by hand with 180 through 360 grit sandpaper. The sanded surface was then coated in turn DuPont 30S primer and DuPont Centari Acrylic Enamel.
Infared or convection heat sources can be used, if desired, for reducing the post cure time, e.g., about 150 to about 200 F.
These Examples demonstrate that the inventive composition and method can be employed for repairing a damaged automotive body panel.
This Example demonstrates a UV curable material that is subsequently baked at a temperature of about 200 to 300 F.
This is a variation of the composition in Example 18 which retains the same epoxy to hydroxy ratio, henceforth known as the EHR. The EHR is the ratio of the number of epoxy groups in the formulation to the number of hydroxy groups present. Typical EHRs for the inventive composition can range from 20 to 2, depending on the raw materials used.
The paintability of the cured compositions formed in Examples 18 and 19 was tested by applying commercial automotive primer (DuPont White), then baking at the recommended time and temperature. This was followed by a coat of commercial basecoat (DuPont Toreador Red), which was also baked according to the recommended parameters. Testing for adhesion was performed according to a modified version of GM9071P, the General Motors specification for "Tape Adhesion Test for Paint Finished." The cured compositions of Examples 18 and Example 19 remained paintable, as determined by GM9071P, even after storage for 48 hours at 100% condensing humidity.
The Shore A Durometer Hardness of aged and cured compositions formed in Examples 18 and 19 was measured in accordance with conventional methods. The cured compositions were aged for 48 hours in room temperature (RT), and 48 hours in 100% relative humidity (RH). The results of the Shore A measurements are listed below.
This Example illustrates a UV curable composition having a decreased EHR.
This Example illustrates a UV curable composition having a decreased EHR.
This Example demonstrates a UV curable composition having an increased tensile strength. This Example also illustrates a composition having an increased EHR.
The following two examples (Examples 23 and 24) illustrate the addition of a non-functional resin as a component of the UV curable composition. When added in an effective amount, this resin functions as a toughener and/or flexibilizing agent.
The EVA copolymer resin was heated in a tin to a temperature of about 201° F. with an amount of the polyol sufficient to soften the EVA. While continuing to heat, the EVA copolymer was stirred into the polyol. Heating continued as the rest of the polyol was stirred in gradually. When the polyol/EVA mixture had cooled to a temperature of about 80° F. , the cycloaliphatic epoxy was added with stirring. When the addition of the epoxy was completed, the silicas were stirred into the mixture until completely dispersed. The mixed composition was then dispensed and cured in accordance with the method of Example 18.
This composition was mixed, dispensed and cured in accordance with the method of Example 23.
The following examples illustrate two-part systems that utilize a cationic type cure chemistry.
Part A was activated by exposing it to UV radiation from a suitable source. Part A and Part B were then mixed together in a tin by hand, and allowed to cure.
Worktime (WT) of the activated compositions was measured in minutes and seconds at defined intervals by ascertaining when the activated composition began to harden or increase in viscosity. WT is given in minutes (′) and seconds (″). The worktime of the activated composition can be adjusted by the dosage or wavelength of UV radiation it receives. Below is a table listing the worktimes obtained with Parts A and B above when they were irradiated at three (3) UV exposures which gave the dosages (Joules/cm2) listed below.
This Example illustrates a two component UV curable composition having a pre-iniated component.
A portion of Part A was irradiated with the UV radiation, but this time 5 minutes were allowed to pass before mixing with Part B. A reaction took place within 0.5 minutes.
Another portion of Part A was exposed to the UV radiation, but allowed to remain undisturbed for 1 hour before mixing with Part B. Reaction took place within 42 seconds.
This Example illustrates a two component system having at least one pre-initiated component and dispensing the components through a static tube mixer.
This Example illustrates a pre-iniated composition, and worktime of the composition as a function of time after being pre-iniated.
A skilled person in this art would understand that these Exemplary processes can be modified by manipulating process variables such as time and temperature of each aforementioned mixing step, mixing rate (RPM), time under vacuum, amount and type of energy source, and level of vacuum (mm Hg) as well as operating a continuous process. While the above Examples illustrate a batch process a skilled person in this art after having reviewed and understood the instant disclosure, would be capable of manipulating the aforementioned process variables to tailor the instant composition for a virtually unlimited array of product applications.
While the present invention has been described in certain preferred embodiments thereof, it will be apparent that various substitution, omissions, modifications, and other changes which may be made without departing from the spirit of the invention. Thus, the present invention should be limited only by the scope of the following claims including equivalents thereof.
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In Casablanca, Capt. Renault pockets his winnings and remarks, as he shuts down Rick's American Cafe, "I am shocked, shocked to find that gambling is going on in here!" After decades of presiding over the disastrous combination of declining quality and runaway costs of American higher education, the leaders of America's college-accrediting agencies are nearly as convincing as Capt. Renault as they loudly protest their injured innocence.
President Obama was right to collar them. Six accrediting agencies have for decades under federal law held the task of determining which colleges within their geographical regions -- nearly 3,000 schools -- are of sufficient quality to make them eligible for federal student aid. What is there to show for this enormously expensive investiture of power? Nearly seven in 10 employers now believe that higher-education quality must be improved for our graduates to remain competitive in the global economy, and two-thirds of college graduates hold debt to the tune of almost $27,000 on average. It's clear that accreditors are failing to do their job.
Obama appears to be out of patience with excuses from these guardians of the status quo. He envisions the possibility of "a new, alternative system of accreditation that would provide pathways for higher-education models and colleges to receive federal student aid based on performance and results."
In fact, such an alternative is already before Secretary of Education Arne Duncan. A bipartisan group within the federal advisory council on accreditation recently proposed a system that would base eligibility for federal student aid on clear measures of quality and effectiveness, such as graduation rates, student learning gains, job placement, financial stability and student loan default rates. There would be no intrusion on the autonomy of America's vibrant diversity of higher-education institutions, no micromanagement of their missions. Federal dollars would flow only to institutions that document successful outcomes, as President Obama said.

subset: commoncrawl


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Click Here to Watch the Whole Video in HD at All American Heroes
All-AmericanHeroes features amateur straight guys out of uniform. These straight men are REAL current or former cops, marines, firemen, lifeguards, military police.
26 year old, brown hair, blue eyed Fireman Logan is a striking fellow. We paired him with Buster, a student who plans on joining the police academy when he graduates. This is all new to Buster, while Logan admits that he has 'messed around' with another man one time when he was wasted. Although a little unsure at first, both of these hot studs start to get into it once they start jerking each other off. By the time they are sucking each other and stroking together you can feel the temperature rise, and the clothers come off. Buster is a real sport, taking as much of Fireman Logan's big pole down his throat as possible. Once things really get going Buster services Fireman Logan until he blows his hot sticky load onto Buster's face and chest. After the facial Buster just has to jerk off, so Logan sit's with him and winds up catching a bit of Buster's spunk.
Pixels: 320X240 | Bitrate: 350K
Pixels: 640X480 | Bitrate: 700K
Two really gorgeous young firemen! Seems they've been around the block on oral!
Two great looking guy. How do these str8 guys suck such cock so great.


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Lesson: DNA Extraction
I'm using a wonderful tool called Voicethread to demonstrate how to extract DNA from raw wheat germ. Click play on how to do the demo and to see how Voicethread can be used. Download the handout for more details.
I made ScienceFix.com to share my favorite demos that I do in my middle school science classes.
I'm using a wonderful tool called Voicethread to demonstrate how to extract DNA from raw wheat germ. Click play on how to do the demo and to see how Voicethread can be used. Download the handout for more details.
A while back I posted an item from Steve Spangler's Science site that demonstrated how to make lava lamps. I decided to go ahead and try it and I filmed it. The materials that are required for the demo are shown below. As the video shows the peanut butter jar is filled with 3/4 vegetable oil and 1/4 colored water. Place an 1/8 of an Alka-Seltzer tablet into the jar. The Alka-Seltzer reacts with the water to form carbon dioxide gas bubbles. The gas is less dense than the water or oil. The carbon dioxide gas bubble attach themselves to the colored water, causing them to rise to the surface. When the gas breaks through to the surface the higher density colored water droplets sink back down into the jar. The second part of the video shows the same demonstration, this time in a large test tube.
We're now into three weeks of summer vacation and I've fully surrended to it. I figured I'd better make a list before summer is over, so here it is.
My only complaint about summer break? It's way too short.
I know what you are thinking. How can an iPhone be of any educational value in the science classroom? You are right. As of this moment it's not quite ready to improve your students' learning, but there are some tantalizing possibilities in the near future. What features does an iPhone have that can be used in the classroom?
1. An accelerometer. You have seen commercials showing the iPhone's screen changing when the unit's position is changed. How does it do that? It has a built in accelerometer that detects change in position in the x, y and z axis, as well as a change in speed. Speed and direction together is velocity, and a change in velocity is acceleration. What are some apps that take advantage of the accelerometer?
Roller Coaster Physics (Silver Mana Software) This app measures vertical g-forces. Press the start button and it will plot the vertical g-forces on the y axis and time on the x axis. This is ideally meant for a person to keep the iPhone in a pocket while riding a roller coaster. The best feature is emailing the data to yourself. The data is in comma separated value form and can easily be imported into Excel for analysis.
G-Meter Lite (Silverview Consulting Inc.) This app measures "steering" (left/right) g forces and accelerating/braking g forces. It plots the data points on a four quadrant graph. Unfortunately this app doesn't save the data for use later analysis. It is merely a visual representation of real time forces, and thus it really isn't useful for data analysis. G FORCE and G-Force are also apps that do this very same thing.
2. A microphone. The iPhone obviously has a microphone or else it couldn't be used as a phone. What app can possibley be used in a science class that takes advantage of the microphone?
ioscilloscope (Gabe Jacobs Productions) This app shows the amplitude and wavelength of sound waves. Have a student bring in an instrument (or use prerecorded tones), like a trumpet or a sax and have the student play a single note at different volume levels to show the differences in amplitude. Then have the student play a series of higher pitched notes to show the different wavelengths (or frequencies).
3. A clock Don't all cell phones have a clock? Yes, so the iPhone isn't so special on this feature. Each year our science department buys 15+ stopwatches at about $6 each minimum. These are cheap stopwatches and their quality is also cheap. They don't last more than 10-20 uses because either the battery goes dead or the buttons break. Since they don't last more than a year they are considered consumables. This year I decided to end this cycle of spending. Most students now have cell phones and most of these cell phones have a stopwatch (timer) feature that measures to the nearest 0.01 seconds. Now when we need to measure time for learning activities I ask volunteers to use their own cell phones and the science department doesn't have to spend any more money.
Summary It's a little too soon to utilize a few of these iPhone apps to enhance learning in the science classroom. What is encouraging though is in probably 5 years most cell phones will be like the iPhone–a minicomputer that can collect all types of data. Today many physics and chemistry classes use expensive specialized probeware (like from Vernier and Pasco) to collect and upload data to computers. Students might bring their own data collection devices via their cell phones.
Educational Innovations' website teachersource.com sells tons of unique science related items. One of those items is the handboiler. When you wrap your hand around the base the colored liquid (probably alcohol) heats up and moves up to the top where it eventually bubbles. My guess is that the molecules of the liquid speed up causing them to move up. When you let go the liquid eventually cools and goes back down via gravity. You can make the liquid go down faster by grabbing the top with your hand. I do this demo with student volunteers. We make observations and they hypothesize what is causing it. We also record who is able to send the liquid up the fastest.
Precautions: Don't squeeze the handboiler. It can break easily.


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ANDREA NEAL: Candidates should consider sales tax cut
At 3.4 percent, Indiana's personal income tax is one of the nation's lowest. A half dozen states, including Texas and Florida, don't charge income tax at all; 41 states impose a rate higher than Indiana's.
At 7 percent, the Indiana sales tax ties for second highest with four other states. The only higher one is California's at 7.25 percent.
Indiana is one of just a few states that charge a sales tax for gasoline on top of an excise tax.
Our excise tax is 18 cents a gallon — relatively low — and doesn't change as gas prices fluctuate. Its revenues are used to pay for highways, roads and other infrastructure maintenance.
It's important to remember as Hoosiers consider the campaign tax proposals of our governor candidates, Democrat John Gregg and Republican Mike Pence.
Mr. Gregg wants to permanently eliminate the state sales tax on gas at a savings of $540 million a year. He figures that rising gas prices are pinching family budgets enough at the pump, and families could use the break.
Mr. Pence suggests cutting the state individual income tax by 10 percent, to 3.06 percent, which would save Indiana taxpayers $530 million a year. He says that's a good way to give their money back to taxpayers when the state is collecting more than it needs.
Both proposals seem off the mark if the goal is to deliver across-the-board relief.
An impact study by the Institute on Taxation and Economic Policy in Washington D.C. concluded that 12 percent of Hoosiers would "see no benefit" from the Pence plan.
Those are lower-income families who don't pay income taxes at all, but do pay sales taxes on most things they buy, groceries and medicine excluded.
Also, an income-tax cut at the state level results, somewhat ironically, in Hoosiers sending more money to Washington.
That's because taxpayers who itemize on their federal returns can deduct state and local income taxes.
According to the Institute, Mr. Pence's plan would erase $50 million in itemized deductions.
Mr. Gregg suffers from a similar flaw. It would give immediate relief to motorists, yet many of the lowest-income Hoosiers don't own cars and would get no benefit. Plus it gives unwarranted benefit to all those tourists passing through Indiana on their way to elsewhere.
This seems especially shortsighted at a time when fiscal experts are warning of dwindling resources to pay for upkeep of road, bridge, sewer and utility networks. With money about to run out from Gov. Mitch Daniels' Major Moves initiative, Indiana will have to look for new funding for infrastructure.
Some lawmakers have even suggested diverting gas sales tax money from the general fund to highway and bridge maintenance.
A compromise between the Gregg and Pence plans would be to roll back the sales tax to 6.5 percent. This would benefit all Hoosiers, cost about the same, help reverse Indiana's reputation as a high sales tax state, and bring the mix of taxes into healthier proportion.
As noted in the recent report, "Policy Choices for Indiana's Future," "Indiana's seven percent sales tax is high, and proceeds from the sales tax are now the largest component of state revenue" at 47 percent.
The report, a white paper prepared by the Indiana University Public Policy Institute, also recommended including services — not just goods — in the sales tax base. Although controversial, that idea would allow the state to reduce the sales tax further.
Indiana's tax climate is rated healthy by most economists, and our individual tax burden — as ranked by the Tax Foundation — is 25th, smack dab in the middle.
Mr. Gregg and Mr. Pence are both right when they say it could be better still. By cutting the sales tax, they could achieve their goals and nudge Indiana closer to the median. The top spots in a tax ranking are never a good place to be.
Andrea Neal is adjunct scholar with the Indiana Policy Review Foundation. Contact her at firstname.lastname@example.com. Nothing written here is to be construed as reflecting the views of the foundation or as an attempt to aid or hinder the passage of any bill before the legislature or to further any political campaign.
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Michael Matheson
Michael Matheson is a writer, editor, and book reviewer based in Toronto. He is also a submissions editor for Apex Magazine, and has been nominated for the Aurora Award a couple of times (in different capacities). His fiction is published or forthcoming in Ideomancer, and the anthologies Future Lovecraft, Dead North, and Chilling Tales 2, among others. Find out more at his website, A Dark and Terrible Beauty.


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Trapezoid design and road-tough build.
The Nady PTS515 Speaker Cabinet offers beefy full-range sound. A 12" woofer kicks it hard, while a broad 5" x 15" high-compression piezo-driven horn cranks out beautiful mids and highs from a slick-looking trapezoid cab. Carpet covered with protective corners and recessed handles. The Nady PTS515 is 18"W x 26"H x 14"D. 37 lbs.


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Session B26: Focus Session: Computational Nanoscience II: Mechanics, Dynamics, and Assembly
11:15 AM–2:15 PM, Monday, March 16, 2009
Room: 328
Sponsoring Units: DMP DCOMP
Chair: Dennis Rapaport,, Bar-Ilan University
Abstract ID: BAPS.2009.MAR.B26.9
Abstract: B26.00009 : Atomistic Simulations of Hydrodynamic and Interaction Forces on Functionalized Silica Nanoparticles
Preview Abstract MathJax On | Off Abstract
J. Matthew D. Lane
(Sandia National Labs)
Ahmed E. Ismail
(Sandia National Labs)
Michael Chandross
(Sandia National Labs)
Christian D. Lorenz
(King's College London)
Gary S. Grest
(Sandia National Labs)
It is often desired to prevent the flocculation and phase separation of nanoparticles in solution. This can be accomplished either by manipulating the solvent or by tailoring the surface chemistry of the nanoparticles through functionalization with a monolayer of oligomer chains. Since it is not known how these functionalized coatings affect the interactions between nanoparticles and with the surrounding solvent, we present results from a series of molecular dynamics simulations of polyethylene oxide (PEO) coated silica nanoparticles of varying size (5 to 20 nm diameter) in water. For a single nanoparticle we determined the Stokes drag on the nanoparticle as it moves through the solvent and as it approaches a wall. Due to hydrodynamic interactions there are large finite size effects which we estimate by varying the size of the simulation cell. We also determined both solvent-mediated (velocity-independent) and lubrication (velocity-dependent) forces between two nanoparticles as a function of the coverage and chain length of the PEO chains.
To cite this abstract, use the following reference: http://meetings.aps.org/link/BAPS.2009.MAR.B26.9


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If you're interested in being proactive against wrinkles and blemishes, it's time to reassess you daily skin care regimen. Too much sun and years of neglect can cause your face to look older. You might begin to feel like your appearance does not accurately reflect your age. Here are five ways to combat the signs of aging skin.
Our faces accumulate oil and dirt throughout the day, which can eventually lead to blemishes. If these areas become severe enough, they can lead to slight scarring. You can prevent blemishes by using a daily cleanser on your face. Try to find a product that won't make your face feel dry afterward. Cleaners can reduce the amount of oil and germs on your face, cutting down on the amount of blemishes that form.
Toners improve the overall smoothness of your skin by removing oil and tightening your pores. This beauty product has the added benefit of preventing blackhead buildup. Like cleaners, it's important for you to find a toner that won't result in dry skin or irritation. Apply the toner to a cotton ball and dab it across your face for the best results.
If your skin gets too dry, your skin and lose its elasticity. This can result in wrinkles, cracking, and peeling. Use a daily moisturizer to prevent your skin from drying out. If you will be spending significant time in the sun, then try to find a moisturizer and sunscreen combo. This can protect your face from the harmful UV rays of the sun. Sun damage can lead to significant skin damage, resulting in wrinkles and increasing your risk of skin cancer.
Exfoliate once or twice a week to give your pores a deep clean and remove impurities from your skin. This process helps you remove dead skin cells on your face, which can clog pores and lead to blemishes.
Skin Tightening
This procedure can leave your skin wrinkle free and smooth. As we age, our skin gets looser and less elastic. This can lead to the formation of wrinkles around our eyes and skin. Consult a skin care professional to learn more about laser skin procedures.
You must take a holistic approach to skincare to maintain a youthful appearance. A daily regimen of cleansing, toning, and moisturizing, followed by periodic exfoliation can help your skin stay healthy. Laser procedures can also make a significant different within a short period of time.


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Polish Magnate Landowner Records: Bringing "The Lords' Jews" to Life
Polish Magnate Landowner Records: Bringing "The Lords' Jews" to Life
with Pamela Weisberger & Natalie Dunai
Magnate records are often unstudied, but hold great genealogical and historical value. This talk covers a brief history of Galicia, explaining the symbiotic nature of the Magnate-Jewish interrelationship, where Jews sustained the economic institutions, while magnates furnished an environment for Jews to conduct religious and commercial activities. Magnate records are held in the Central State Historical Archive in Lviv and the Stefanyk National Scientific Library. Learn how to identify the magnates who owned the towns where your ancestors resided and access their files, along with the structure and contents of their record collections. View examples of "Inventories" dating to the 1700s using patronymics, lists of Jewish residents and tax-payers, contracts and occupation lists and records in 1853-1858 documents of the Austrian Empire State Commission on the liquidation of serfdom. Discover Jewish Magnates! Your "bubbe maises" about the great-grandfather who was a landowner (or even a Baron!) can be quite true.
Natalie Dunai, resides in Lviv, Ukraine. In 1991 she graduated from the Lviv University. Since 1996 she assists her husband Alex Dunai in genealogy research and since 2000 works full time as a professional genealogy researcher. She makes research in the archives all over Ukraine. Natalie combines archival research and tour assistance in her husband's firm. She is fluent in English, Russian, Polish, Ukrainian, reads handwritten German Gothic and Latin. Her particular area of expertise are 18-19 centuries' property records and using ancient maps for finding modern locations.
Pamela Weisberger is president and research coordinator for Gesher Galicia, 1st V.P. of the Jewish Genealogical Society of Los Angeles, and was co-chair of the 2010 IAJGS International Conference on Jewish Genealogy. She is a professional genealogist and internationally-known lecturer, having spoken to groups in the U.S. , Poland, Israel and Canada. She's researched in archives throughout Poland, Ukraine and Hungary, specializing in map and newspaper resources. She holds a B.A. from Washington University and an M.S. from Boston University.


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Full detailed profile on Winifred Leeds Played by Senta Moses on General Hospital Daytime Soap Opera.
Senta Moses (ABC)
Winifred Leeds
Actor: Senta Moses
Who played Winifred Leeds over the years
Senta Moses - (January 2, 2009 - April 30, 2009)
Useful information on Winifred Leeds
* She 'geeked it up' as part of her job to try to get information about Damian Spinelli.
Past: FBI agent
Winifred appeared on the scene as a computer geek who idolized Spinelli's cyber prowess. When she met him in real life she marveled over his skills and seemed to speak the same language he did. Maxie immediately turned green and forbade Spinelli to spend time with her because she surely was using him for something.
In the end, Maxie was right because although Winifred truly did idolize Spinelli, her job as an FBI agent was what brought her to investigate him. She had to turn over evidence that he broke laws as Jason Morgan's assistant.
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When Spinelli returns to his office, he finds Maxie waiting for him. She tells him that she thinks she's being stalked and lists the late-night phone calls and footsteps that she hears behind her lots of times. She tells him that she didn't know who else to turn to and he takes her hand and tells her to 'fear not'. After she leaves he gets busy. When Winifred shows up she can't believe that Spinelli didn't see through Maxie's ploy.
Sam meets Spinelli at Kelly's. He thanks her for her help in getting him off of the FBI wanted list. He goes on to say how impressed he was with her skills in the field, and in turn, she compliments his computer skills. He tells her that it would be a travesty to let their combined talent go to waste and suggests the "Jackal and McCall PI Company." Before she can respond, Winifred shows up upset. She pulls up a chair and says that her employment has been terminated because Rayner considers her a security risk. Spinelli is outraged, but Winifred says that if they fight it charges will be filed. She vows to find gainful employment. Spinelli comes to the conclusion that she should have immediate employment at "McCall & Jackal Private Investigations."
Click Here To Read Previous Related Archives On Winifred Leeds »


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Lenny Tristia Tambun & Tunggadewa Mattangkilang
The Jakarta and Balikpapan administrations are imposing stricter controls on no-smoking zones.
The capital is restricting the placement of smoking rooms to the outside of buildings, while Balikpapan has banned smoking altogether in eight areas.
Jakarta city administrators revised Gubernatorial Decree No. 88/2010 on no-smoking zones, which initially ordered an end to smoking rooms but is now allowing smoking rooms to be placed outside of buildings in order to comply with a recent Constitutional Court ruling.
The original decree stated that public buildings, "can provide special smoking rooms…"
The Supreme Court removed the option, making it mandatory to provide smoking rooms.
"The issuance of this new gubernatorial decree is to comply with the Constitutional Court's ruling on Law No. 36/2006 which removed the word 'can,' " said Mara Oloan Siregar, the Jakarta provincial assistant secretary for people's welfare.
"But that doesn't mean a special room [for smoking] has to be in the building. This new gubernatorial decree is more strict in terms of the implementation of the non-smoking zone."
He said that the new gubernatorial decree required building management and transportation operators to ensure that the decree was implemented, and that they provided a means for the public to file complaints by providing a hotline, SMS number or e-mail address.
Every supervisor will receive simple report cards to fill out, along with supervision guidelines, Mara said.
"There will also be an integrated team of supervisors who will supervise multipurpose buildings, such as malls and hotels," he added.
Mara said that the new gubernatorial decree intensified the implementation of non-smoking zone regulations through guidance, supervision, complaint mechanism and law enforcement.
Building owners must also place posters stating that smoking is banned inside the building and provide numbers for the public to lodge complaints.
"This one is new," Mara said. "We will ask them to provide the building management's number so that the public can file complaints. That way, if they see anybody smoking in the building, they can immediately report it through that number."
Meanwhile, the Balikpapan city administration declared eight areas as non-smoking zones, namely schools, sports areas, houses of worship, playgrounds, public facilities (airport, terminals and malls), hospitals, public transportation and offices. The ban is stipulated under Mayor's Decree No. 24/2012 regarding the smoking ban.
"To commemorate World Without Tobacco Day, we have declared eight non-smoking zones in Balikpapan," Balikpapan Health Agency head Dyah Muryani said.
She said the regulation was meant to protect residents who did not smoke because most active smokers came from the middle- to lower-income classes and that they smoked anywhere they liked, disturbing other people and making them feel uncomfortable.
The city administration is also providing health services in all communities to help residents kick their smoking habit. All of the officers have been trained to help residents quit smoking.
"Those who smoke the most are people with middle to lower incomes," Dyah said. "They are already poor, but they still smoke. That's just going to create more problems for them.
"We've also provided therapy for those who wish to quit smoking in 26 community health centers."
Active smokers in Balikpapan account for 34.5 percent of Balikpapan's total population of 600,000 people.


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Film: The Story of the Weeping Camel
Tue, March 23, 2010 • 7:00 PM • GRG 102 Geography building, corner of 24th and Whitis.
UT's Center for Russian, East European, and Eurasian Studies is proud to present a film series of rare comedies and dramas from Central Asia. These films are evidence that the most visually unique and charming films being produced today are coming out of a little known part of the world, Central Asia. You won't find most of these films being shown at your local cineplex or on Netflix. Toss your copy of 'Borat' out the window, and come see samples of Central Asian cinema that have been called transcendant, surrealist, and captivating.
Films will be shown on Tuesdays from February 23 – March 30 at 7:00pm in GRG 102 (Geography Building, corner of 24th and Whitis).
Films are in original language with English subtitles.
Tues. Mar. 23
The Story of the Weeping Camel - Mongolia (2004) 87 mins.
Critics raved about this Oscar-nominated uplifting drama. Beautifully shot in the open vistas of the Gobi desert, the film tells the story of two boys in search of a camel-whisperer.
"A real discovery!" Roger Ebert


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