MXPA04007835A

MXPA04007835A - Formable, porous, chemiluminescent reactant compositions and device therefor.

Info

Publication number: MXPA04007835A
Application number: MXPA04007835A
Authority: MX
Inventors: L Palmer Stephen
Original assignee: Omniglow Corp
Priority date: 2002-02-12
Filing date: 2003-01-23
Publication date: 2005-09-30
Also published as: KR20050004778A; CN1643103A; EP1481034A1; JP3996165B2; EP1481034A4; CA2476317C; KR100945094B1; JP2005534768A; AU2003214881A1; WO2004013249A1; CA2476317A1

Abstract

A formable, porous chemiluminescent reactant composition, device (11) therefore, and a process for production thereof is disclosed. The fluidizable solid admixture (12) of the instant invention may be cured to a more or less rigid form with or without the use of a mold. The cured solid is useful as a chemiluminescent reactant component and is useful in a variety of environments.

Description

REACTIVE COMPOSITIONS THAT CAN BE FORMED, POROSAS, QUIMIOLUMINESCENTES, AND AN APPARATUS FOR THE SAME Field of the Invention The present invention is directed to the field of chemiluminescent compositions, and more particularly, to apparatuses that produce light from an immobilized chemiluminescent material. Background of the Invention The term "chemiluminescent reagent", "reagent with chemiluminescence" or "chemiluminescent reagent composition" is interpreted as a mixture or component thereof, which will result in the production of chemiluminescent light when reacted with other necessary reagents in the processes described in the present invention. The term "fluorescent compound" is interpreted as a compound that fluoresces in a chemiluminescent reaction. The term "chemiluminescent composition" is interpreted as a mixture that will result in a chemiluminescence. The term "de-agglomerate" is interpreted as a break or loosening of a compact part of an accumulation or mass. The term "fluidizable solid mixture" is interpreted as a non-liquid mixture which, when agitated, behaves like a pseudo-fluid but has properties of a solid when at rest. The production of chemiluminescent light generally uses a two-component system to generate light in chemical form. Chemiluminescent light is produced by combining the two components, which are usually in the form of chemical solutions referred to as the "oxalate" component and the "activator" component. For use in the present invention, all suitable activator and oxalate compositions are contemplated, including those of various fluorescers, catalysts and the like, known as useful in the prior art. The two components are kept physically separate before activation, through a variety of means. Frequently, a fragile, sealed glass bottle containing a component is housed in a flexible outer container containing the other component. This external container is sealed to contain both the second component and the fragile, filled bottle. The forces created by intimate contact with the inner bottle, for example, by bending, cause the bottle to rupture thereby releasing the first component, and allowing the first and second components to mix and produce light. Since the objective of this type of apparatus is to produce a usable light output, the external bottle is usually composed of a clear or translucent material, such as polyethylene or polypropylene, which allows the light produced through the chemiluminescent system to be transmitted through the walls of the bottle. These apparatuses can be designed to allow a variety of colors, either by adding an ink or fluorescent compound to one or both of the chemiluminescent reagent compositions or to the bottle. In addition, the apparatus can be modified to transmit light only of parts of it chosen in a special way. U.S. Patent No. 5,043,851 to Kaplan, includes examples of a chemiluminescent system. Kaplan describes a polygonal chemiluminescent light generation apparatus, which concentrates the light in the corners of the same, increasing in this way the visibility of the light emanating from the part of the light cartridge of the apparatus and optimizing the quantity and distribution of light radiated. U.S. Patent No. 4,626,383 to Richter et al. Describes chemiluminescent catalysts in a method for producing light of short duration, high intensity systems and low temperature systems. This invention relates to catalysts for two-component chemiluminescent systems, wherein one component is a hydrogen peroxide component and the other component is an oxalate ester-fluorescer component. Lithium carboxylic acid salt catalysts, such as lithium salicylate, are considered which decrease the activation energy of the reaction and also reduce the temperature dependence of the light emission process.

U.S. Patent No. 5,121,302 to Bay et al. Describes a solid, thin, chemiluminescent apparatus that emits light in one direction. The apparatus is comprised of a backsheet of a laminated metal sheet having a two-component front sheet heat sealed thereon at its edges and a temporary separation means positioned to divide the internal area into two compartments. The bi-component includes a first component which is a sheet of rolled metal and a second component which is a transparent or translucent polyolefin sheet. The metal sheet of the bi-component offers thermal stability, increased shelf life and a relative impermeability to volatile components of the activating solution. The sheet metal laminate for the storage of the activating solution allows the activating solution to retain its viability due to the impermeability of the metal sheet. US Pat. No. 6,062,380 to Dorney, discloses a glow-cup system with lighting capabilities. The apparatus is a generally cylindrical shaped container made of a semi-solid material, with a preferred embodiment comprised of a translucent plastic material, to allow limited flexibility in the outer layer of the cup, because its shape may be temporarily altered to a certain extent. point when applying pressure to the side parts. A cavity is located inside the side wall of the cup. The cavity contains a plurality of rupturing ampules containing a chemiluminescent fluid. The chemiluminescent fluid inside the lamp is an oxalate. A second chemiluminescent fluid resides within the cavity, so that when the ampule ruptures, the two fluids make contact and provide illumination. When the user applies pressure to the outer layer of the cup that is at the point of the cavity, the ampule is broken. The lower part of the cup contains a stopper, which may or may not be removable, which seals the second chemiluminescent component within the space of the cavity. In addition, it is advisable to produce chemiluminescent light from objects of various shapes and designs. U.S. Patent No. 4,814,949, filed by Elliott, describes a means for making chemi-luminescent shaped objects, two-dimensional. Conventional liquid chemiluminescent reagents are combined to produce light. A non-woven absorbent article with a desired shape is allowed to absorb the chemiluminescent reagents after mixing and activation, so that the article emits light from a desired shape. Although the shape may be simple or complex, as desired, it is essentially limited to a two-dimensional surface and is further limited to producing a single color of light per apparatus. In U.S. Patent No. 3,816,325 filed by Rauhut et al., An example is described for creating a chemiluminescent system with the ability to produce light from a swellable polymeric composition. Two principal means are employed to produce solid chemiluminescent systems. The first system relies on the diffusion of a chemiluminescent oxalate solution into a solid polymer oxalate, such as the length of a flexible vinyl pipe. The diffusion process occurs when a length of the vinyl tubing is immersed in a suitable chemiluminescent reagent for a prolonged period of time. After removing the tube from the oxalate solution, the application of a liquid activator to the surface of the pipe causes the pipe to emit light. Since the solid polymer is relatively non-porous, it is difficult to rapidly and completely activate the oxalate within the pipeline, because the diffusion process, which is relatively slow, must also count on allowing the activating solution reach the chemiluminescent reagent diffused into the polymer before light can be generated. In a further embodiment of the US Patent No. 3, 816,325, the chemiluminescent oxalate solution is mixed with a polyvinyl fluoride (PVC) resin powder to form a paste, which is subsequently dispersed on a substrate and baked in an oven to form a flexible, elastic film. Although this embodiment is operative, the described polyvinyl chloride sheet exhibits weakness in terms of uniformity, strength, flexibility, and most importantly, porosity. In addition, the described processes are mainly suitable for producing only relatively thin objects. U.S. Patent No. 5,173,218 to Cohen et al. Discloses a combination of PVC polymer resins to produce a porous, chemiluminescent, flexible structure from liquid pastes. Although an improvement in the art is provided, products produced in this way still suffer from a variety of drawbacks, particularly if the solid, chemiluminescent objects that will be produced are not relatively flat, thin objects. A thin "pad" is produced from a mixture of polymer resins, which is strong and flexible, and exhibits satisfactory activating fluid absorption properties. However, the processes focus on producing pads that are made by pouring a mixture of liquid paste into molds. Therefore, the dough and the shape of the resulting pad is limited to the shape of the mold, into which the dough is poured and gathered. Furthermore, it is well known to those skilled in the art that the forms and processes used in the prior art can produce chemiluminescent pads with a relatively tough impermeable "cover" provided the pulp has been in contact with the mold during the cooking process. . This cover is easily recognized as a darker and more transparent region of the pad that is highly impermeable. As a result, it does not have the ability to rapidly absorb the light-activating solution, and therefore, contributes minimally to the light output of the apparatus. The thickness of this cover varies with the time and temperature of the cooking process, although in any case, this cover represents a wasted material from which little usable light can be produced. It has been determined that this cover is created by an inability of the paste to extract air (or other gases) during the cooking process. To achieve a significantly porous product, air must enter the paste mixture during the cooking process of the exposed surfaces of the paste assembly. During the curing process, air is usually extracted into the pad to replace the volume occupied by the solvents that are absorbed in the PVC resins. This process continues as the air is drawn to the ever increasing depths within the pad, first as the upper regions of the pad cure and subsequently as the successively lower regions of the pad cure. It is this inclusion of air within the pad within the cooking process, where the percentage of open pore space and thus the absorption capacity of the pad is determined. At some point during the cooking process described, the bottom part of the mold can reach a temperature, at which the paste mixture that is in contact with this mold region begins to curdle and heal, even when a mold can not be created. air path of the exposed surfaces of the paste to this lower region. Due to a lack of available air for this paste setting, this "bottom" curing process results in a pad that is considered to be dense and virtually non-porous in the region of the pad next to the bottom of the pad. mold, and to a lesser degree, the edges of the mold. You can minimize certain adverse effects of this healing process from the bottom up, if the lower part of the mold is placed in a cold thermal mass in the curing furnace, thereby providing heating or curing of the lower part of the paste following the rest of it. However, the undesirable production of a hard and impermeable covering layer remains unattended. During cooking processes, such as those described in US Pat. No. 5,173,218, the paste expands as air is drawn into the polymer matrix, where air is added to the volume of the matrix. As a result, significant problems develop when trying to cure a mass of this relatively large paste. For example, if a liquid paste mixture, such as the one described in the '218 patent, is poured into a test tube and cooked for a suitable time for curing, a dense, hard mass exhibiting a porosity will be produced. very deficient, and therefore, a poor absorbency in most of the mass. This is due, in part, to the "bottom-up" healing process described above, where insufficient air is extracted into the paste from the curing process, due to the existence of an airtight liquid cap on top of the paste that is being cured near the bottom of the mold. Furthermore, it has been unexpectedly discovered that the pulp materials do not extract the necessary air, if the pulp is not allowed to expand during the curing process. In the case of the previous example of the test tube, the side walls of the test tube limit the paste to expand and extract the required air to produce a cured matrix with a high degree of porosity and absorbency that is required to allow the activation of the product with the liquid activator. Even when the pulp is free to expand vertically in the test tube during the curing process, the lateral restriction of the pulp along the walls of the test tube is sufficient to avoid the optimal expansion of the pulp and the induction of the pulp. air inside the dough during the healing process. Therefore, the cured mass will exhibit low porosity and will produce poor light output, which is a limitation in the art. It is often desired to provide a chemiluminescent apparatus which not only has the ability to produce light, but to produce light with a variety of colors. U.S. Patent No. 5,508,893, filed by Nowak et al., Is directed to a multi-color chemiluminescent light generating apparatus and method for producing the product. This apparatus is comprised of a flexible tube at least partially filled with an activating solution, a plurality of oxalate-containing ampoules located within the tube, and at least one barrier element between the amps to prevent mixing of the colors. This device has the ability to impart different chemiluminescent colors after activation. U.S. Patent No. 5,705,103 filed by Chopdekar et al. Describes a composition for producing chemiluminescent light with controllable duration. The composition is comprised of an oxalate component (which includes an oxalate ester) in a solvent, an activating component (a peroxide compound and a catalyst) in a solvent and a fluorescer. Through proper selection of the molecular weight of the homopolymer for the oxalate component, the control of the total glow time and the point in time at which light production begins can be varied. Although this apparatus provides a controllable duration or stability of light, there is no evidence of a composition for controlling the generation of gas produced or a composition that can be independent of a container, that is, can not be formed or porous. Therefore, the technique lacks a means to produce three-dimensional objects, which can be self-illuminated by means of chemiluminescence, and to produce a highly porous composition exhibiting rapid activation and excellent light output. In addition, the prior art fails to contemplate a product that can be independent of a container, minimize dark areas due to gas generation, and have the ability to simultaneously generate a plurality of separate wavelengths of chemiluminescent light. Summary of the Invention The present invention shows a means to produce three-dimensional objects, which self-illuminate. The objects can be as simple or as complex as desired. The objects are produced through a method that employs a chemiluminescent reagent composition, which can be formed. This composition is of a nature that can be quickly placed in containers of various forms, and subsequently cured in containers, whereby the composition becomes solid and has a shape that precisely matches the container in which it was formed. Once formed, the composition is semi-rigid and can be removed from the container if desired. In addition, the present invention provides a chemiluminescent reagent composition which is exceptionally porous and is not limited to relatively flat material strips, as is the case in the prior art. Also, the objects produced by means of the present invention can be hollow so that a minimum amount of material can be used to produce three-dimensional glowing objects. In addition, these objects can have multiple colors, that is, a single object can be created which has the ability to simultaneously generate a plurality of separate colors or wavelengths of chemiluminescent light. A fundamental object of the present invention is that a significant part of the interstitial spaces in the solid product necessary for a fast and reliable activation through a liquid activator is believed before curing. Therefore, the system does not depend mainly on the porosity created during the healing process, in which the air must enter from outside to the matrix. Since the final porosity of the product of the present invention is primarily a function of the degree of densification before curing, the final porosity of the product can be controlled accurately and conveniently. Normally, it is desirable to provide a product that is activated as soon as possible. For this to occur, the activating solution must react quickly and completely with the oxalate part of the chemiluminescent system. However, there are times when it may be desirable to slow down the reaction range or possibly at least slow down the range in which the activator has the ability to reach and react with the oxalate component. Since the product of the present invention can be densified to practically any desirable degree, the available interstitial space through which the activator communicates with the solid product can be reduced as desired, thereby reducing the mobility of the activator and its ability to react with the component that contains the oxalate. In addition, because most of the porosity of the chemiluminescent solid is determined by the degree of densification before curing, the product of the present invention can be cured in a relatively confined space, such as a test tube, and the The resulting product will be highly porous and receptive to the activating solution. Accordingly, it is an object of the present invention to provide a means for producing three-dimensional objects having the ability of self-illumination through chemiluminescence, and wherein the objects can simultaneously generate a plurality of separate colors or waveforms. . It is a further object of the present invention, produce a three-dimensional chemi-luminescent object that is highly porous. It is a further object of the present invention to provide a three-dimensional chemiluminescent object in which the porosity can be controlled quickly and accurately.

It is still a further object of the present invention to provide a three-dimensional chemiluminescent object that can be produced by forming in a mold, which does not allow for significant expansion of the chemiluminescent reagent composition during the curing process.

It is still another object of the present invention to provide three-dimensional chemiluminescent objects that have little or no dark regions due to the "cover" effect caused by improper curing. It is a further object of the present invention to provide a three-dimensional chemiluminescent object that can be formed in such a way that the object remains hollow. It is still a further object of the present invention to provide a three-dimensional chemiluminescent object in which a substantial part of the porosity is created before the curing process. It is still another object of the present invention to provide a formulation for a chemiluminescent reagent composition that can be formed, and therefore, can easily be formed into a desired shape, either with or without the use of a mold or shape. Other objects and advantages of the present invention can be appreciated, starting from the description that follows when taken in conjunction with the accompanying drawings, in which certain modalities are established, by way of illustration and example. of the present invention. The drawings constitute a part of this specification and include exemplary embodiments of the present invention and illustrate various objectives and features thereof. Brief Description of the Figures Figure 1 is a graph illustrating the light output versus the activation time for different bulk densities of the solid oxalate; Figure 2 is an illustrative view of an exemplary embodiment of the present invention; Figure 3 is a cross-sectional view of the exemplary embodiment of Figure 2 illustrating the placement of the chemiluminescent reagent composition; Figure 4 is a cross-sectional view of Figure 3 illustrating the densification of the chemiluminescent reagent composition using a tamping tool; Figure 5 is a cross-sectional view of the exemplary embodiment after densification, illustrating the second placement of the chemiluminescent reactive component ampule and a void in the fluidizable solid mixture; Figure 6 is a cross-sectional view of another example embodiment of the present invention illustrating the placement of the chemiluminescent reagent composition; Figure 7 is a cross-sectional view of the embodiment of Figure 6 illustrating the placement of a compression tool within the chemiluminescent reagent composition; Figure 8 is a cross-sectional view of an embodiment of the present invention illustrating the densification of the chemiluminescent reagent composition through the compression tool of Figure 7; and Figure 9 is a cross-sectional view of one embodiment of the present invention illustrating the densified chemiluminescent reagent composition. Detailed Description of the Invention The present invention is directed to a formulation, manufacturing process and apparatus for use with respect to a chemiluminescent reagent composition which can be formed, and can be used to produce a multidimensional object. This composition overcomes the weakness of the prior art and implements the use of a novel forming process which will be applied to a chemiluminescent material, thereby constructing a highly porous chemoluminescent object, uniquely formed. The process of the present invention is not limited to the conventional casting process that produces the flat and relatively thin objects described in the prior art. The porous and can be formed powder of the present invention, it can easily be compacted up to several degrees, and at the time of curing by heating, a relatively strong, flexible and highly porous mass can be formed. The apparent density of a material is easily controlled through the degree of compaction or densification. Therefore, an object of any apparent and desirable density can be produced. Because the bulk density directly affects the rate of absorption of the activator, chemiluminescent activation can be conveniently controlled. Referring now to the figures, Figure 1 is a graph illustrating how the control of bulk product density can be used to vary the activation time. Two apparatuses were produced and tested, each comprising a chemiluminescent reagent composition which is in the form of a composition containing solid oxalate, hereinafter referred to as a solid oxalate. The first apparatus had a volume density of approximately 0.54 g / cc and reached a maximum light output in approximately 10 minutes after activation. The second apparatus, with a volume density of approximately 0.72 g / cc, reached its peak light output in approximately 37 minutes after activation. These data indicate that the activation time is affected by the volume density with more compact objects that require a longer period to activate. The ability to control the light output curve enables the production of chemiluminescent devices to meet a wide range of needs in the market. By way of example, for the production of large chemiluminescent objects, a hollow chemoluminescent form can be preferred to a solid one, since there is a decrease in the return effect as the light produced from the depth of the solid form inefficiently reaches the surface and can not be emitted in the form of useful light. In addition, a hollow chemiluminescent form provides a convenient and pleasant means for introducing a second component reactive to the product. A vial or bottle containing a second reactive component can be placed into the hollow in a hollow form. When the ampule or vial is broken, the second component is rapidly absorbed by the inner surface of the hollow shape and is rapidly transferred by capillary action through the porous, chemiluminescent matrix until the entire mass is moistened and light is produced through of chemiluminescence. By placing the second component inside the hole, it is achieved that it is not visible and allows the production of an aesthetically pleasing product. An example of a form that can be produced using the teachings of the present invention is that of a chemiluminescent candle. Candles provide a safe and reliable alternative for real candles. The flame of real candles can ignite other objects. Unlike conventional candles, chemiluminescent candles are resistant to wind and water and by employing the present invention, they can be produced to emit light in any desired color or in any combination of colors or waveforms from a single apparatus. . Previous attempts to produce these "candles" which use chemiluminescent systems in the form of light sources have met with several drawbacks. Normally, an apparatus that generates chemiluminescent light, such as a light cartridge, which uses liquids, has a top space in the apparatus that represents approximately 30% of the volume of the container. Light can not be produced in this area of higher space. Japanese Patent Application No. 10-170263 discloses an air bubble capture means in which the upper gaseous space (or bubble) that is above the liquid chemiluminescent fluid in a sealed chemiluminescent apparatus is trapped in a region of the apparatus different to the top. By placing the bubble of the upper tip part of a sealed chemiluminescent apparatus, such as, for example, a candle, the whole part of the tip of the flame of the candle will appear resplendent during the chemiluminescent reaction. If the bubble has been allowed to remain at the tip of the flame, it can create a dark region near the top of the flame, since the area of the bubble will not produce any light. Said dark region could subtract the general visual acceptability of the apparatus. Carbon dioxide, carbon monoxide, and oxygen are common gases released in peroxy-luminescent systems. These gases rise to the top of any liquid chemiluminescent system and form bubbles in the upper part of the apparatus. Therefore, although the apparatus described in Japanese Patent Application No. 10-170263 can effectively eliminate the problem of bubbles initially contained in the upper part of a chemiluminescent apparatus, a method for displacing the bubbles that are provided is not provided. they are generated during the chemiluminescence process. The present invention allows that in a candle or any other desired chemiluminescent object that is desired to be produced, any upper initial bubble in the apparatus and any accumulation of visibly significant bubbles in the apparatus as the chemiluminescent process proceeds is eliminated. Furthermore, the present invention does not require traps, channels or valves specially formed in the apparatus to make this benefit possible. Since the mass that can be formed from the chemiluminescent system of the present invention is a solid, there is no space to add and combine bubbles. Although the gases generated during the chemiluminescence process are still produced, these gases are limited to arise in the solid mass that can be formed and evenly distributed through the solid, which subsequently results in a seemingly perfect light output. Figure 2 establishes a preferred embodiment of the present invention in the form of a chemiluminescent candle 10, which comprises a blow-molded envelope in the form of a candle cartridge. When the device is activated, the part of the flame of the candle shines. A candle wrap 11, such as that illustrated in Figure 3, can be created by blow molding or other suitable forming means from materials such as, but not limited to, polyethylene and polypropylene. Preferably, the distal end of the envelope of the candle opposite the flame is left open. The envelope of the candle 11 is placed so that at the open end it faces upwards, a chemiluminescent reagent composition 12 can be formed of the present invention, in a candle wrap 11, so that the envelope is partially full. Although the fluidizable solid mixture can flow, it also exhibits a degree of cohesion, and produces a wet powder that can be packaged and formed. Accordingly, an auxiliary feeding means, such as a vibrating feeder for assisting in the feeding of the chemiluminescent reagent composition that can be formed can be useful. Once the chemiluminescent reagent composition that can be formed is in the Sail wrap 11 may be lightly compacted with a tapping tool 13, such as that illustrated in Figure 4, designed for this purpose. This compression process not only serves to assist the composition in conforming to the shape of the envelope of the candle 11, but also densifies the composition and compresses it so that it does not flow or move additionally into the envelope of the candle. the candle 11 in case the orientation of the envelope is altered. However, if desired, the composition can be removed from the wrapper by applying sufficient vibratory forces to cause a liquefying of the compacted chemiluminescent reagent composition 15. A tapping tool 13 can be designed with a tapered tip. 14, so that it not only compacts the composition but also produces a cavity 16, as illustrated in FIG. 5, in the resulting compacted composition. The cavity 16 provides a convenient means for facilitating the distribution of a second chemiluminescent reactive component 18, such as within an ampule 17 that promotes uniform and rapid activation of the apparatus. Once the second chemiluminescent reactive component is in place, a plug 19 can be heat sealed at the distal end of the candle wrap 11. In addition, the cavity 16 provides a space within which the composition can expand during the healing process, so that an exceptionally porous product can be produced. The cavity is not required to produce products that are highly porous, but can be used in certain cases to produce products with exceptional porosity. Such cavities are not possible with the process considered in the prior art. As set forth in FIG. 6, a chemiluminescent envelope in the form of a rose 21 is produced through a first blow molding of a wrapper, for example of polyethylene, in the form of a rose bud with a stick attached. The diameter of the stem is considerably smaller than that of the button. For this preferred modality, it is advisable to produce a rose button where the entire surface of the button is illuminated by chemiluminescence. It is also advisable to produce the article using as little chemiluminescent material as possible, which will create the desired effect. The rose-shaped envelope 21 is filled with a small amount of chemiluminescent reagent composition that can be formed 12. Referring now to Figure 7, inserted into the rose-shaped envelope 21 with a chemiluminescent reagent composition 12, there is a compression tool 22 comprising a hollow needle 23 equipped with an expandable bladder 24, which for purposes of illustration, is illustrated as being held in place through at least one retaining ring 25. The distal end of the hollow needle 23, cap and a hole in the side of the needle under the expandable bladder 24, allows an air pressure from inside the needle to fill and inflate the expandable bladder 24. The bladder expands, as illustrated in FIG. 8, using air pressure for inflation purposes, wherein the chemiluminescent reagent composition that can be formed surrounds the inflated bladder 24 and the compact to the inner wall of the rose button wrap. Figure 9 illustrates the composition of compact chemiluminescent reagent 15 in a semi-solid state. After this compression process, the bladder is deflated and the needle probe is removed, leaving a cavity 16. In a preferred embodiment, the compact chemiluminescent reagent composition can be subsequently cured by cooking, while in place within the Rose button wrap at a temperature of 95 ° C for 10 minutes. Once the composition is cooled, a sealed vial containing a solution of the second chemiluminescent reagent component is inserted into the rose-shaped envelope 21, and a stopper can be fitted to the stem and heat sealed to form an airtight seal, as previously described for the modality of the sail. The resulting product is an object that looks like a real rose stem, which, when activated, emits light from the entire surface of the button. Activation is achieved, by way of example, by simply flexing the stem of the rose to fracture the ampule and release the second component which is subsequently absorbed into the chemiluminescent reagent composition or the solid mixture that may be formed. Since the compact chemiluminescent reagent composition largely conforms to the inner wall of the envelope, through the process of the present invention, even small details, such as the petals of the rose, are captured.

With respect to the modalities of the candle and the rose described, it is assumed that the cured solid product will remain in the polymer shell, however, the material can only be melted and cured in a mold and subsequently removed. Solid chemiluminescent objects can be produced using the present invention, through, for example, the use of centrifugal compression or molding. The individually formed products produced through the process of the present invention can be included as free floating objects that could glow if placed in a bottle containing a second solution of a chemiluminescent reactive component. Such a system can produce, by way of example, a "snow globe" containing glowing snow particles. Since the mass that can be formed of the chemiluminescent reagent composition of the present invention is in solid form, a plurality of colors can be used which can be fixedly placed and separated in a single apparatus. For example, a pink button may be produced in which the button is red with orange strips. A significant advantage of the present invention with respect to a fully liquid chemiluminescent system, such as that found in conventional light cartridges, is that if desired, the entire surface of the object may be resplendent. Since the product resulting from the present invention is a solid chemiluminescent material, the product can be used in situations where it is impractical or impossible to use a liquid chemiluminescent system that depends on its container. The examples that follow describe the experimental process carried out to achieve the novel aspects of the present invention. A series of experiments were considered to identify the optimum materials and formulas necessary to produce a porous, chemiluminescent, reactive composition that can be formed. As considered in the prior art, a pre-paste can be prepared by dissolving approximately 2 parts of PVC resin (Geon Corp. # 121) with 98 parts of a chemiluminescent reactive solution, which is exemplified in the present invention as a solution of oxalate. A paste was prepared, also according to the '218 patent, by mixing 59 parts of a previous oxalate paste (as described above) with 31 parts of PVC powder resin with average particle size (Geon # 218) and 9. PVC resin parts of large size particles (Geon # 30). The resulting material is a liquid paste that can be poured. Examples 1 to 6 Six tests were carried out to determine the effects of the various curing times and temperatures, as well as the thickness of the pulp in terms of porosity. In each test, approximately 7 grams of liquid paste was placed in a small aluminum tray, which was then placed in a spacer, so that the bottom of the tray was slightly tilted to create a paste that has a fluctuating depth 0.0381 cm to 0.4572 cm (0.015 inches to 0.180 inches). During each test, the tray was placed on a metal grid in an oven with air circulation. After curing for the specified time, each sample was removed from the tray, sectioned and examined for adequate cure and porosity. A properly cured sample is defined, one in which all the oxalate solution has been absorbed into the PVC matrix, and which exhibits no signs of overcooking. In a properly cured matrix, the lower molecular weight PVC particles melt together. However, the higher molecular weight PVC particles, while absorbing the liquid oxalate solution, do not fuse together significantly. If the curing time and temperature are excessive, the higher molecular weight PVC particles will fuse together, resulting in a matrix which is over-cured, as can be seen through the presence of dark and / or glossy regions inside the cured sample, referred to as a pad. This over-cured matrix will exhibit very low porosity. Table 1 illustrates the results obtained using various paste curing conditions. Table 1 - Pasta Cure In test article 1, it was found that the PVC particles did not completely absorb the oxalate solution, since the material was pasty and contained significant amounts of free liquid. In tests 2 to 5, it was found that the material was less pasty, although only the exposed surface of each cured sample was determined to be porous. Each of test items 1 to 5 was activated with a chemiluminescent activation reagent. Items 2 through 5 shone from the surface, but did not produce significant light from the non-porous dark areas. Article 1 produced very little light with respect to most of its surface, presumably because the liquid oxalate solution that was not absorbed in the PVC matrix during the curing process presented a barrier, preventing the activation solution will reach the equilibrium of the liquid oxalate below the surface. A certain glow was observed near the surface of the matrix in the end layer, where the activation and oxalate solutions were combined. Article 6 was cured at a lower temperature, since articles 1 to 5 appeared to be over-cured by the application of excessive heat, causing the high molecular weight PVC particles to melt together. However, the results of the article 6 test contradicted this theory. Even in the lower time and temperature used to cure article 6, dark, dense regions were observed where the pad has been in contact with the tray. Example 7 A chemiluminescent candle produced using the same liquid paste formation as that used in tests 1 to 6 above was produced. To make this candle, approximately 3.2 grams of a liquid paste in a polyethylene candle wrap was injected using a syringe. A glass ampule containing a chemiluminescent activator was inserted into this paste, so that the lower end of the ampule made contact with the lower part of the candle envelope. The assembly was placed in an oven with air circulation adjusted to a temperature of 82 ° C and allowed to cure for 12 minutes. After the removal, the assembly was allowed to cool to room temperature, whereby the candle wrap and the cured paste were sectioned for observation. The PVC matrix (cured paste) seemed to be completely cured, although it was dark and dense. The parts of the PVC matrix were removed from the wrap and placed in an aluminum tray. The chemiluminescent activating reagent was added to these parts, where the cured paste glowed with dim light. It was observed that the activator reacted only with the top surface of the cured paste and could not reach the inside of the cured paste. This lack of absorption of the activating solution in the cured paste was determined not as a result of the over-cure or sub-cure of the paste, but was due to a very low porosity exhibited by the pad. The porosity, or pore space within the matrix, is derived from two sources. A small part of this porosity results from the already porous PVC particles found in the matrix. A more significant factor in determining the resulting porosity of the cured paste is the ability of the air to be induced throughout the volume of the paste during the curing process. It was observed when the liquid paste formulation shown in the '218 patent is used, that if a sufficient heat to cure the paste reaches the inner region before the outer regions are completely cured and porous, the inner region will be cured with a porosity very low. This effect is due to the inability of the air to migrate through this liquid region that surrounds the interior. Example 8 With these results in mind, an aliquot of pulp was supported on an air permeable substrate., for example, a 10 cm x 10 cm section of a 2 mm thick nonwoven polyester cloth and placed in an air circulation oven, which was maintained at a temperature of 82 ° C, for 8 minutes. The expectation was that the rag could provide uniform access of air to the pulp and that the heat could cure the pulp from the outside, so that dark, non-porous regions would not form, as had been the case in the pulp previously. Cured in waterproof aluminum trays. Since each successive layer of the paste was cured from the outside, it can become porous, thus allowing the air to reach the subsequent layers. This sample was removed from the oven and allowed to cool. At the time of the inspection, it was observed that the pad had no dark or dense areas and that it was extremely porous. The sample was activated with a chemiluminescent activating reagent, where the sample shone brilliantly and uniformly in its entirety.

A model that explains the formation of interstitial spaces in PVC particle / solvent pastes, is one in which large, rigorously spherical PVC particles are joined together through smaller, lower molecular weight PVC particles to form a matrix. The PVC particles absorb the solvent with which the interstitial spaces between these particles were initially filled. If air is allowed to enter the matrix during this curing process, the PVC particles will swell and expand as the solvent is absorbed into the particles. Example 9 To determine if air access through the pulp could be achieved by using a higher percentage of PVC weight of larger particles, a new pulp preparation was created and tested. This new paste contained 56 parts of a previous paste, 29 parts of resin of average size particles (Geon # 218) and 15 parts with large size particles (Geon # 30). Approximately 2.5 ml of this liquid paste was placed in a polyethylene candle wrap to which a glass activator was added. The article was cured at a temperature of 75 ° C for 12 minutes and allowed to cool. It was appreciated after the dissection, that the paste had been cured, but that it still contained dark regions that were not porous. The theory was developed and tested that a liquid PVC and oxalate resin formulation could be produced in such a way as to result in a material that allows air to move through the formulation at all times before and during curing. EXAMPLE 10 A new formulation was created which used the previous pulp described above, dissolving approximately 2 parts of PVC resin (Geon Corp. # 121) with 98 parts of an oxalate solution. Although in this example the oxalate solution was propylene glycol base dibenzoate, any compound based on the art is contemplated. In this new formulation, a higher percentage by weight of a single PVC particle was used instead of the PVC resins with average and large particles used in the pulps previously described. Approximately 40 parts of a previous paste were added to 60 parts of resin (Geon # 466). The resulting composition was not a liquid paste, but rather a wet, packable and shaped powder characterized as a fluidizable solid mixture. The resin should be selected to contain a particle size or range thereof, sufficient to provide the fluidizable solid mixture. In an illustrative, but not limiting, mode, this resin is a PVC resin having an average particle size distribution of about 125 microns. A large variety of polymers can be used in the polymer composition: polyethylene, polypropylene, po I i (vini I chloride), poly (methyl methacrylate), po I i (vini I benzoate), po I i (in I acetate) , cellulose, po I i (vi or I pyrrolidone), polyacrylamide, epoxies, silicones, po I i (vini I butiral), polyurethane, nylons, poly acetal, polycarbonate, polyesters, and polyethers, as non-limiting examples. Non-crosslinked polymers can also be employed, such as polystyrene-poly (divinyl benzene), polyacrylamide-poly (methylenebisacrylamide), polybutadiene-copolymers, and the like. For most applications, the polymer must be selected together with the activating hydrogen peroxide liquid so that it can be dissolved, swollen or otherwise permeable to the activation liquid. Said permeability is normally recommended to allow an efficient contact between the activation liquid, the chemiluminescent material and (when desired or necessary) the fluorescent material. It will often be advisable to select the polymer and activating liquid to provide a particular activation range, and thereby control the intensity and duration of light emission. Some useful polymer-solvent combinations are: 1) poly (vinyl pyrrolidone) -water, 2) p or I i (v i n i I styrene-polydivinyl benzene), copolymer-ethylbenzene, 3) po I i (i n i I chloride-ethyl benzoate), 4) poly (methyl methacrylate dimethyl phthalate). The permeability of the polymers to the solvents is well known in the art and is a considerable issue for selecting useful polymer / solvent combinations. Solvents used as plasticizers are particularly convenient. It is not necessary that either the chemiluminescent material or the fluorescent material be soluble in the polymer itself, although where the polymer does not itself provide solubility for both of these solvents, the activation liquid must provide at least a partial solubility. Alternatively, the polymer can be plasticized with a solubilization plasticizer. The wet powder of the resulting chemiluminescent reagent composition has a consistency similar to that of light brown sugar. Due to the cohesive nature of the fluidizable solid mixture, it has been found to be beneficial to deagglomerate or release any compressed parts through a method, such as being screened through a mesh sieve or shaken with a tool to ensure that the wet powder can not be compacted before being used. To help place the material, a vibratory feeding system can also be useful. Although the foregoing serves as an example for dropping compact parts, any means for deagglomerating the fluidizable solid mixture can be used. The newly created formula along with the discovery that the interstitial spaces previously existing in the material, are important for the healing process to result in an immediate and significant improvement in the time required to complete the absorption of the chemiluminescent activating reagent and correspondingly the light output. The chemiluminescent reagent composition, which can be formed, therefore comprises a first chemiluminescent reactive component in combination with a quantity of particles of the first polymeric resin effective to produce a uniform dispersion, visualized as a liquid paste. Subsequently, a quantity of particles of the second polymeric resin is provided in combination with the uniform dispersion of an effective amount to produce a solid fluidizable mixture. This solid fluidizable mixture can be molded to form a specific shape. A means for deagglomerating the fluidizable solid mixture can be provided in order to loosen any parts of the dough that may have been compacted during the preparation. A means for curing the fluidizable solid mixture can also be provided with and without the use of a mold. In a preferred embodiment, the particles of the first polymeric resin and the particles of the second polymeric resin are each polyvinyl chloride resin. Although an activation solution is commonly added to the composition to begin with the emission of light, the oxalate and activator of the present invention can be exchanged. In such a case, the first chemiluminescent reactive component may comprise an oxalate, and the second chemiluminescent reactive component may subsequently comprise an activator. Optionally, the first chemiluminescent reactive component should comprise the activator and the second chemiluminescent reactive component should then comprise an oxalate. In order to provide a chemiluminescent system, the second component must be included. Accordingly, a first chemiluminescent composition of the present invention comprises a first chemiluminescent reagent that includes a first chemiluminescently reactive component in combination with a quantity of particles of the first polymeric resin effective to produce a uniform dispersion and a quantity of particles of the second resin polymer in combination with the uniform dispersion in an effective amount to produce a solid fluidizable mixture. A second chemiluminescent reagent component is included, wherein the contact between the first and second chemiluminescent reactive components will result in the generation of light. The generation of light includes at least one different wavelength, within the visible or invisible spectrum. A means for controllably activating the fluidizable solid mixture can be provided.

Also described is a multidimensional chemiluminescent apparatus comprising at least a first chemiluminescent reagent that includes a first chemiluminescently reactive component in combination with a quantity of particles of the first polymeric resin effective to produce a uniform dispersion and a quantity of particles of the second polymeric resin in combination with the uniform dispersion in an effective amount to produce a fluidizable solid mixture. At least one fluidizable solid mixture is dispersed within a multidimensional container, wherein the densification of the fluidizable solid mixture results in the formation of the multidimensional chemiluminescent apparatus. By compacting the apparatus with a second chemiluminescent reactive component, the generation of chemiluminescent light will result. As noted above, the resulting light emission may be more than one wavelength or different color. The means for compacting or densifying the fluidizable solid mixture thus provides a means for controllably activating the fluidizable solid mixture and can be achieved by a variety of techniques, all contemplated by the present invention. By way of example, the densification of the fluidizable solid mixture is by means of a molding technique, wherein a moldable object or a hollow object is formed having areas of controlled densification. These variations in density are illustrative of a control parameter for the light emission reaction, and result in an object which is termed as controllably activated. A process for the production of a chemiluminescent reagent composition of the present invention comprises providing a first polymeric resin, subsequently combining a first active chemiluminescent component, usually in the form of a solution, with an effective amount of the first polymeric resin to create a paste. . A second polymeric resin is provided which is combined with the paste in an amount effective to create a solid fluidizable mixture. Also included is a means for providing controllable activation of the fluidizable solid mixture, which can be achieved by compacting the mixture to a desired degree. As illustrated in Figure 1, the more compact the mass, the longer it takes to reach a peak light output. This solid fluidizable mixture is significantly different from the liquid paste shown in US Pat. No. 5,173,218, since it is not liquid and will not seek its own level. The fluidizable solid mixture is also significantly different from the pulp described in US Patent No. 3,816,325, since it is flowable, but neither will it sink or collapse. More significantly, this powder composition has interstitial air spaces with an intrinsically high degree of porosity and interconnection. In addition, the fluidizable solid mixture has a cohesive nature which allows it to be formed into definitive solid forms by simply pressing the moist powder with moderate force. By way of example, the material can be manipulated manually, or placed between two plates to create a thin sheet. In addition, the cohesion exhibited by the wet powder is sufficient to retain a desired shape after pressing. By way of example, the fluidizable solid mixture can be pressed into small pastes, either with or without the use of shapes and simply cured by baking in an oven, whereby the individual particles in the powder will be united in a single porous mass. In an alternative embodiment, the fluidizable solid mixture can be placed in a mold and baked (cured) to form a solid object which has a shape that precisely matches that of the mold. Since the wet powder, once it is slightly compact, can not flow as a dry powder or a liquid paste could do, the fluidizable solid mixture of the present invention, can be formed, processed or manipulated in another way, in such a way that a hollow object is produced. Said hollow chemiluminescent objects have great value since the external surface, which emits light from the object can be formed into any desired shape while maintaining a hollow interior. This hollow interior only allows the preservation of the chemiluminescent material, and therefore reduces costs, but also allows relatively large chemiluminescent objects to be produced which exhibit a high gloss on the surface with minimal cost. Although PVC is the preferred polymeric resin, the polymer composition is not limited thereto. In the chemiluminescent reagent composition of the present invention, various methods of forming and / or processing are applicable. Examples of such methods include, but are not limited to, injection molding, extrusion, compression molding, cast molding, powder molding or electrostatic deposition, such as xerography. The powder comprises the dry milling of the wet powder and a curable additive to form a mouldable composition.

In addition, the solid fluidizable mixture can be deposited electrostatically through a process such as xerography, wherein an electrical charge is provided to the surface of a container that retains the chemiluminescent reagent composition. Adhesion between the chemiluminescent reagent composition and the surface of the container occurs only in the charged areas to allow a particular placement of a chemiluminescent reagent composition within a container. All patents and publications are incorporated herein by reference to the same extent as if each individual publication was specifically indicated to be incorporated by reference. It will be understood that although some form of the present invention is illustrated, it is not limited to the specific form or adaptation described and illustrated herein. Those skilled in the art will appreciate that various changes can be made without departing from the scope of the present invention, and that it is not considered to be limited to what is shown and described in the specification and drawings / figures. One skilled in the art will readily appreciate that the present invention is also adapted to carry out the objectives and have the purposes and advantages mentioned, as well as those inherent therein. The modalities, methods, procedures and techniques described herein as being representative of the preferred embodiments at present, are projected to be the example and are not intended to be limitations of the scope of the present invention. Those skilled in the art will appreciate changes thereto, which are within the spirit of the present invention and are defined by the scope of the appended claims. Although the present invention has been described in connection with specific preferred embodiments, it should be understood that the present invention, as claimed, should not be unduly limited to said specific embodiments. In fact, various modifications of the modes described to carry out the present invention will be obvious to those skilled in the art, which are intended to be within the scope of the appended claims.

Claims

R E I V I N D I C A C I O N S 1. A chemiluminescent reagent composition comprising: a chemiluminescent reactive solution and a first polymeric particulate resin in effective amounts to produce a paste at the time of mixing thereof; and a second polymeric particulate resin mixed with the paste in an effective amount to produce a fluidizable solid mixture.
2. The composition according to claim 1, characterized in that the fluidizable solid mixture is deagglomerated.
3. The composition according to claim 1, characterized in that the fluidizable solid mixture is cured.
4. The composition according to claim 1, characterized in that the fluidizable solid mixture is molded to form a specific form.
The composition according to claim 1, characterized in that the first polymeric particulate resin is a polyvinyl chloride.
6. The composition according to claim 1, characterized in that the second polymeric particulate resin is a polyvinyl chloride.
The composition according to claim 6, characterized in that the second polymeric particulate resin is porous.
The composition according to claim 6, characterized in that the second polymeric particulate resin has a sufficient average particle size distribution to provide the fluidizable solid mixture.
The composition according to claim 8, characterized in that the second polymeric particulate resin has an average particle size of about 125 microns.
10. The composition according to claim 1, characterized in that the paste has a uniform dispersion.
11. The composition in accordance with the claim 1, characterized in that the chemiluminescent reactive solution comprises an oxalate.
12. The composition according to claim 1, characterized in that the chemiluminescent reactive solution comprises an activator.
13. A chemiluminescent composition comprising: a first chemiluminescent reactive component including a chemiluminescent reactive solution and a first polymeric particulate resin in effective amounts to produce a paste at the time of mixing thereof and a second particulate polymeric resin that is mixing with the paste in an amount effective to produce a fluidized solid mixture; and a second chemiluminescent reactive component; wherein the contact between the first and second chemiluminescent reactive components will result in the generation of chemiluminescent light.
14. The composition according to claim 13, characterized in that the fluidized solid mixture is deagglomerated.
15. The composition according to claim 13, characterized in that the fluidized solid mixture is cured.
16. The composition according to claim 13, characterized in that the fluidized solid mixture is formed in a specific manner.
17. The composition according to claim 13, characterized in that the first particulate polymer resin is a polyvinyl chloride.
18. The composition according to claim 12, characterized in that the second polymeric particulate resin is a polyvinyl chloride.
19. The composition according to claim 18, characterized in that the second particulate polymer resin is a porous polyvinyl chloride.
20. The composition according to claim 18, characterized in that the second particulate polymer resin has a sufficient average particle size distribution to provide the stable solid mixture.
21. The composition according to claim 13, characterized in that the paste has a uniform dispersion.
22. The composition according to claim 13, characterized in that the first chemiluminescent reactive component includes an oxalate and the second chemiluminescent reactive component includes an activator.
23. The composition according to claim 13, characterized in that the first chemiluminescent reactive component includes an activator and the second chemiluminescent reactive component includes an oxalate.
24. The composition according to claim 13, characterized in that the generation of light includes at least a different wavelength or color.
25. The composition according to claim 13, characterized in that the solid fluidizable mixture is activated in a controllable manner.
26. A process for the production of a chemiluminescent reagent composition, comprising: mixing a chemiluminescent reactive component with a first polymeric particulate resin in an amount effective to produce a paste; mixing a second polymeric particulate resin with the paste, in an amount effective to produce a fluidizable solid mixture.
27. The process according to claim 26, characterized in that the first particulate polymer resin is polyvinyl chloride.
28. The process according to claim 26, characterized in that the second polymeric particulate resin is polyvinyl chloride.
29. The process according to claim 28, characterized in that the second particulate polyvinyl chloride is porous.
30. The process according to claim 28, characterized in that the second particulate polyvinyl chloride has an average particle size distribution, sufficient to provide the fluidizable solid mixture.
31. The process according to claim 26, characterized in that the paste has a uniform dispersion.
32. The process according to claim 26, characterized in that the fluidizable solid mixture is cured.
33. The process according to claim 26, characterized in that the first chemiluminescent reactive component includes an oxalate.
34. The process according to claim 26, characterized in that the first chemiluminescent reactive component includes an activator.
35. The process according to claim 26, characterized in that the fluidizable solid mixture is deagglomerated.
36. The process according to claim 26, characterized in that the solid fluidizable mixture is formed in a specific manner.
37. A multidimensional chemiluminescent apparatus comprising: at least a first chemiluminescent reagent composition that includes a first chemiluminescent reactive component having a first polymeric particulate resin in an amount effective to produce a paste and a second particulate polymer resin mixed with the dough, in an amount effective to produce at least one fluidizable solid mixture; wherein the at least one fluidizable solid mixture is dispersed within a multidimensional container, whereby the densification of the fluidizable solid mixture causes the formation of the chemiluminescent apparatus m u 11 i d i m n n i i n a I; wherein contacting the apparatus with a second chemiluminescent reactive component will result in the generation of chemiluminescent light.
38. The composition according to claim 37, characterized in that the fluidizable solid mixture is deagglomerated.
39. The apparatus according to claim 37, characterized in that the solid fluidizable mixture is cured.
40. The apparatus according to claim 37, characterized in that the fluidizable solid mixture is formed in a specific manner.
41. The apparatus according to claim 37, characterized in that the first particulate polymer resin is a polyvinyl chloride.
42. The apparatus according to claim 37, characterized in that the second polymeric particulate resin is a polyvinyl chloride.
43. The apparatus according to claim 42, characterized in that the second particulate polyvinyl chloride is porous.
44. The apparatus according to claim 42, characterized in that the second particulate polyvinyl chloride resin has a sufficient average particle size distribution to provide the fluidizable solid mixture.
45. The apparatus according to claim 37, characterized in that the paste has a uniform dispersion.
46. The apparatus according to claim 37, characterized in that the first chemiluminescent reactive component includes an oxalate and the second chemiluminescent reactive component includes an activator.
47. The apparatus according to claim 37, characterized in that the first chemiluminescent reactive component includes an activator and the second chemiluminescent reactive component includes an oxalate.
48. The apparatus according to claim 37, characterized in that the generation of light includes at least a different wavelength or color.
49. The apparatus according to claim 37, characterized in that the densification provides a means to controllably activate the fluidizable solid mixture.
50. The apparatus according to claim 37, characterized in that the densification of the solid fluidizable mixture is by a molding technique, wherein a hollow object is formed. SUMMARIZES A reactive, porous, chemiluminescent, reactive composition is described, an apparatus (1) therefor and a process for the production thereof. The fluidizable solid mixture (12) of the present invention can be cured to a more or less rigid shape with or without the use of a mold. The cured solid is useful in the form of a luminescent reactive component and is useful in a variety of environments.