MXPA00009196A - Composition for deactivating chemically and biologically active agents - Google Patents

Composition for deactivating chemically and biologically active agents

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Publication number
MXPA00009196A
MXPA00009196A MXPA/A/2000/009196A MXPA00009196A MXPA00009196A MX PA00009196 A MXPA00009196 A MX PA00009196A MX PA00009196 A MXPA00009196 A MX PA00009196A MX PA00009196 A MXPA00009196 A MX PA00009196A
Authority
MX
Mexico
Prior art keywords
resin
particles
resin particles
converted
coating
Prior art date
Application number
MXPA/A/2000/009196A
Other languages
Spanish (es)
Inventor
John S Moorehead
Lynnette D Blaney
David H Brown
Pierre J Messier
Norbert G Laderoute
Original Assignee
Battelle Memorial Institute
Triosyn Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Battelle Memorial Institute, Triosyn Corporation filed Critical Battelle Memorial Institute
Publication of MXPA00009196A publication Critical patent/MXPA00009196A/en

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Abstract

A substance capable of devitalizing hazardous biological agents and deactivating hazardous chemical agents comprising an activateed anion exchange resin having a particle size substantially in the range of about 0.1-300 microns, which resin particles have been iodinated by exposure to a sufficient amount of an iodine-substance absorbable by the anion exchange resin such that the resin particles absorb the iodine-substance so as to convert the resin particles into activated resin particles. The iodine-substance may be selected from the group consisting of I2 (i.e., diatomic iodine), and polyiodide ions having a valence of - 1. The activated resin particles may be placed into contact with the biological or chemical agent as a dry aerosol, by dust coating, or by admixing the particles with a carrier to form a coating.

Description

COMPOSITION TO DEACTIVATE CHEMICALLY AND BIOLOGICALLY ACTIVE AGENTS RELATED APPLICATION • 5 This application claims the benefit of US provisional patent application no. 60 / 078,642, filed March 19, 1998. BACKGROUND AND OBJECTIVES OF THE INVENTION The present invention relates generally to a resin composition, particularly impregnated resin particles. with halide, and a method to make them. Resin particles • impregnated with halide can be applied to a substrate in the form of a coating or a dry aerosol. It is believed that resin particles impregnated with halide can be used to deactivate or substantially reduce the effectiveness of certain agents chemically and biologically assets in contact. In this way, the present invention also relates to the use of halide impregnated particles to deactivate certain chemically and biologically active agents. U.S. Patent No. 5,639,452 to Messier, the content of which is incorporated herein by reference, describes a Disinfectant substance comprising an ion exchange resin impregnated with iodine and a process for the preparation thereof. The Messier patent describes that this disinfectant is a disinfectant of resin polyiodide, of broad spectrum demand type, useful for sterilizing fluids, and particularly a disinfectant of polyiodide, in which the iodine is associated more tenaciously with the resin than with the ,. ..? previously known disinfectants, so that it leaves residual diatomic iodine undetectable, or otherwise acceptable, in treated fluids. Thus, the patent teaches that iodinated resin can be used f to sterilize fluids, such as water, air and body secretions at Devitalize microorganisms, such as fungi, bacteria and viruses, that may be present in the fluid. It seems that this effect is generally achieved by causing the microorganisms in the fluid to contact the resin surface and / or the resin impregnated material. U.S. Patent No. 5,431, 908 for Lund, whose content is incorporated into the present by reference, also shows a method to prepare • ion exchange resins impregnated with halide useful to purify fluids, such as water. A devitalizing or disinfecting substance that incorporates the capabilities of a fluid disinfectant, such as that one, would be desirable. described by Messier or Lund, - but 'that it is suitable for use in connection with the disinfection of non-fluid objects and that it can be delivered in the form of an aerosol or incorporated in a coating. Such a substance could be used, for example, to decontaminate a non-fluid object that is exposed to biological agents, such as, pathogens transported by air, either continuously or intermittently. It could also be used to provide a protective coating on non-fluid objects that are likely to be exposed to biological people, so that the object would be able to devitalize these agents on demand, at least until the devitalizing substance present in the coating has been removed. exhausted, without significant damage to the usual utility of the object and without application of a substance or procedure of decontamination or discreet devitalization after exposure to the agent. Such a protective coating would be useful on objects that are likely to be exposed to biological agents on a more or less regular basis, for example, equipment used in emergency medical response or other health care applications, or surfaces in public washbasins and showers facilities. or institutional. The coating would also be useful on objects that can be exposed to such agents in the event of a catastrophe, such as a military conflict, terrorist incident or a spill of dangerous material. As used in this, "biological agent" refers to dangerous biological organisms including viruses and bacteria, either in the form of spores or otherwise, and eukaryotic parasites, such as, Giardia. It also includes biologically generated toxins, such as botulinum toxin. The term "devitalize" means to kill a biological agent that is an organism, or render a biological agent inactive or substantially less effective, including, without limitation, disinfection. It is expected that the devitalizing substance will be effective against biological agents that are susceptible to oxidation by ionic halides, such as polyiodide ions. It would also be desirable to have a deactivating substance capable of reaction with and at least a partial deactivation of certain chemical agents. As used herein, "chemical agent" means a hazardous chemical agent, including but not limited to chemical warfare agents, such as compounds known as GD, HD and VX, and hazardous industrial chemical agents. In addition, the term "deactivate" means rendering any such chemical agent inactive, ineffective or substantially less effective for its intended purpose of causing damage to animal life or health, and particularly human life and health.
As described above in relation to the devitalization of biological agents, it is expected that the deactivating substance will be effective against chemical warfare agents and other chemical agents susceptible to oxidation by ionic halides, such as polyiodide ions. The chemical agent deactivating substance described above could be used to decontaminate fluids that may contain agents • chemicals, to decontaminate non-fluid objects that may have such agents on their surfaces, or to provide a protective coating on non-fluid objects that will likely be exposed to such agents. Such a protective coating can provide resistance increased to chemical agents, even if it is not able to deactivate all those possible agents. A substance capable of devitalizing biological agents and deactivating chemical agents, would be particularly preferred.
F either independently or simultaneously depending on the circumstances. In connection with the use of a devitalizing or deactivating substance to decontaminate non-fluid articles, it would also be desirable to have such a substance in a dry aerosol form, so that finely divided particles of the substance can be dispersed over the article (s) to be treated. The dispersion of the substance in Dry aerosol, for example, by wrapping a room in mist, would allow the substance to penetrate into pores, cracks, or other surface irregularities that may be present in or on the article (s) to be treated. The substance could also be applied in this way to contaminated items, such as computers, electronic equipment and electrical, and other materials sensitive to water or reactive to water, which may be further damaged by contact with a devitalizing or deactivating liquid substance, and particularly a water-based substance. A suitable substance in the form of a dry aerosol can be selected based on the electrostatic properties of an article non-fluid, so that the resin particles deposited in ia • Surface tend to be held in engagement with the surface for a period. Alternatively, for non-fluid targets that are not liquid sensitive, the dry aerosol substance can be applied to the surface that has been treated by wetting with a wetting agent suitable for causing the resin particles to remain in engagement with the surface for a desired time. A dry aerosol could also be used to form a J protective coating on a substrate, for example by "powder coating". The devitalizing or deactivating substance in dry aerosol form could be applied to a wetted surface. The wetting agent causes the resin particles to adhere to or within the agent, so that the particles remain in contact with the surface after drying or curing of the wetting agent. For example, the wetting agent may be a paint-like coating, such as a chemical warfare-resistant coating (CARC) or a polymeric composition. It would also be desirable to cause the devitalizing or deactivating substance to be incorporated into a coating that can be applied to non-fluid objects to form a protective coating thereon. The resin particles can be mixed with a suitable carrier, and the resulting coating applied to a surface of the object by any suitable means, for example, brushing, rolling, atomizing, troweling, casting or the like. The carrier can be a coating type paint, such as a CARC based on water or solvent, or • a polymeric material. Such a coating that could be applied to objects will probably be exposed to chemically or biologically active agents, so that the deactivation and devitalization of these agents could begin in contact with the object and the object could be maintained. essentially free from contamination by such agents during the effective life of the halide resin composition. In addition, it would be advantageous to have a halide resin composition having superior characteristics to known iodide resin disinfectants. For example, a halide resin having an area of The surface increased to provide a more rapid deactivation of biologically active agents, and particularly a finely divided resin suitable for dispersion as a dry aerosol, would offer advantages. A halide resin composition capable of deactivating, or at least partially deactivating, chemically active agents, such as nerve gases, in addition to biologically active agents, would also offer particular advantages. These and other objects of the present invention will be apparent from the following specification and the appended claims. BRIEF DESCRIPTION OF THE INVENTION In accordance with these objectives, a resin composition capable of devitalizing biological agents and deactivating chemical agents can comprise halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into particles of Resin, having a particle size substantially in the range of • approximately 0.1 -1 5 microns. The halide resin can be characterized in that an activated halogenated resin is divided into particles substantially in the range of about 0.1 -15 microns, before exposure to a sufficient amount of a halogen absorbed by the activated resin, to form converted resin particles having a higher proportion of ionic halogen available, the halogen substance of the group being selected that jk consists of l2, Br2, and polyiodide ions having a valence of -1. The halide resin particles can have, for example, a size of particle substantially in the range of about 0.1 -3 micras, 3- 5 micras, 3-1 5 micras or 5-1 5 micras. The resin composition may also comprise halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into resin particles, and characterized because an activated halogenated resin is divided into particles substantially in the range of about 1 5-300 microns before exposure to a sufficient amount of a halogen substance absorbed by the activated resin to form converted resin particles having a greater proportion of ionic halogen available. The halogen substance is selected from the group consisting of l2, Br2, and polyiodide ions having a valence of -1. As used herein, the terms "polyhalide", "polyhalide ions" and the like, refer to, or characterize, a substance or a complex having three or more halogen atoms and a valence of -1, and which can be formed if a molecular halogen (eg, bromine as Br2) is combined with a monovalent trihalide ion (eg, triiodide ion) or pentahalide ion (eg, pentaiodide ion). Iodine and chlorine can also be used as a source of molecular halogen. Similarly, the terms "polyiodide", "polyiodide ions" and the like, refer to, or characterize, a substance or complex having three or more iodine atoms and which could be formed if the molecular iodine is combined with the triiodide ion monovalent The terms "triiodide", "triiodide ion" and the like, refer to, or characterize, a substance or a complex that contains three iodine atoms and has a valence of -1. Accordingly, the triiodide ion in the present is a complex, which can be considered as comprising molecular iodine (ie, iodine as 12) and an iodine ion (ie, I "). described can be able to be dispersed in the form of a dry aerosol.The converted resin may be able to reduce the activities of chemical agents, biological agents and toxins biologically generated objectives.A simple resin may be able to reduce the activities of both chemical agents and The devitalizing and deactivating resin can be a devitalizing and demand-type deactivator, it is • 5 say, a substance from which halide ions are released almost completely on a demand action basis upon contact with an objective agent, but which otherwise does not release substantial amounts of the devitalizing and deactivating substance into the environment . Such a demand-type substance would essentially be able to devitalize and deactivate target agents on demand, at least until the resin • Halide has been exhausted. The invention includes a method for making a resin composition, comprising the steps of: providing an activated halide resin; 15 form the activated resin into particles; selecting resin particles substantially in the range of about 0.1 -300 microns; and form converted resin particles having a higher • proportion of ionic halogen available. The step of selecting resin particles may include, for example, selecting particles substantially in the range of about 0.1 -3 microns, 3-5 microns, 3-1 5 microns, 5-1 5 microns or 1 5-300 microns. It may also include selecting an anionic triiodide resin or a divinyl styrene triiodide resin.
The converted resin particles can be formed by exposing the resin particles to a sufficient amount of a halogen substance to form converted resin particles, the halogen substance being selected from the group consisting of 12, Br 2, and 5 polyiodide ions having a valence of -1. The absorption of at least a portion of the halogen substance can be carried out at elevated temperatures, that is, temperatures higher than 100 ° C and up to 210 ° C, and high pressures, i.e., pressures greater than atmospheric pressure and up to 7.03 kg / cm2. The present invention also provides a deactivator of • chemical agent of demand, comprising halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated in the resin particles, having a particle size substantially in the range of about 0.1 -300 microns.
The resin particles of the deactivator may have, for example, a particle size substantially in the range of about 0.1-3 microns, 3-5 microns, 3-15 microns, 5-15 microns or 1 5-300 microns. The resin can be an anionic resin, a divinyl styrene resin, or a resin • Quaternary ammonium. The halide resin particles can be polyiodide resin particles, which may be predominantly triiodide resin particles. The deactivator may be capable of being dispersed in the form of a dry aerosol. The invention also provides a method for deactivating target agents, comprising the steps of: providing an activated halide resin; form the activated resin into particles; selecting resin particles substantially in the range of about 0.1 -300 microns; exposing the resin particles to a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles, having a higher proportion of ionic halogen available, the halogen substance being selected from the group consisting of 12, Br 2, and polyhalide ions having a valence of -1; and placing the resin particles converted in contact with a target agent selected from biological agents, biological agents and biologically generated toxins. The absorption of at least a portion of the halogen substance can be effected at elevated temperatures and high pressures as described above. The step of selecting resin particles may include selecting particles substantially in the range of about 0.1 -3 microns, 2-3 microns, 3-5 microns, 3-15 microns, 5-15 microns, 15-50 microns or 15-300 mieras The step of providing an activated halide resin can include selecting an activated halide resin having an electrostatic charge that helps to maintain resin particles converted into coupling with a substrate. In accordance with the objective of using the converted resin for decontamination of non-fluid objects, the step of placing resin particles in contact with a target agent may include dispersing the converted resin particles as a dry aerosol, imparting an electrostatic charge to the converted resin particles to assist in their maintenance in coupling with a surface, or providing a surface fc that is electrostatically charged to maintain the particles converted into coupling with the surface. The step of placing resin particles contacted with a target agent may also include providing a wetted surface and causing a portion of the converted particles to be deposited on the wetted surface. The step of providing a wetted surface may include selecting a surface wetting agent, capable of retaining converted resin particles deposited on a surface wetted with the wetting agent. In accordance with the objective of using the resin converted into a protective coating, the step of placing resin particles converted into contact with target agent can include the steps of: providing a carrier capable of supporting the resin particles converted into suspension; fc suspend the converted particles in the carrier; and apply the suspension to a surface. The step of providing a carrier can include selecting a carrier that does not materially interfere with the ion exchange capacity of the converted resin or that comprises a resistant coating of chemical agent. This step may also include providing a predetermined volume of pigment particles and the step of suspending the converted resin particles in the carrier may include suspending a volume of converted resin particles approximately equal to the volume of pigment particles. The invention also includes an aerosol capable of reducing the effectiveness of target agents, such as, chemical agents, agents biologically, and / or biologically generated toxins. The aerosol substance comprises halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into resin particles and characterized in that an activated halogenated resin is particulate substantially in the range of about 0.1-300 microns before exposure to a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles, having a higher proportion of ionic halogen available, with the halogen substance selected from the group consisting of 12, Br 2, and polyiodide ions having a valence of -1. The halide resin particles can be further characterized since an activated halogenated resin is divided into particles substantially in the range of about 0.1 -3 microns, 3-1 5 microns or 15-300 microns before exposure to the halogen substance . The converted resin particles are capable of being dispersed as a dry spray. The particles can be electrostatically charged to assist in the maintenance of the particles in coupling with a substrate, the particles being electrostatically charged before being dispersed. Preferably, the difference in electrostatic charge between the particles and the substrate will be sufficient to Allowing the particles to adhere to vertical surfaces and the like.
The converted resin particles can be passed, for example, through a nozzle, so that they couple a static charge inducing substance in the nozzle. The invention also includes a coating capable of reducing the effectiveness of target agents. The coating comprises halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into resin particles and characterized in that an activated halogenated resin is particulate substantially in the range of about 0.1-300 microns before exposure to a sufficient amount of a halogen substance • absorbable by the activated resin to form converted resin particles, having a higher proportion of ionic halogen available, the halogen substance being selected from the group consisting of l2, Br2 and polyiodide ions having a valence of -1; and a carrier that holds the resin particles converted into suspension. The converted resin is capable of reducing the effectiveness of targets including biological agents, biological agents and / or biologically generated toxins. • Halide resin particles can be characterized additionally since an activated halogenated resin is substantially particulate in the range of about 0.1 -3 microns, 3-1 5 microns or 15-300 microns before exposure to the halogen substance. The converted resin particles are at least 20 percent larger than the particles of any pigment present in the carrier.
Preferably, the carrier does not materially interfere with the ion exchange capacity of the converted resin. The carrier can be a coating resistant to chemical warfare agent, a coating resistant to hazardous industrial chemical, a coating that is selectively permeable to specific fluids, or a latex. The carrier may include a predetermined volume of pigment particles and the volume of resin particles converted suspended in the carrier may be approximately equal to the volume of pigment particles. The combined volumes of the pigment particles and the converted resin particles may approximate the critical pigment volume of the carrier or be at least about 90% of the critical pigment volume of the carrier. The invention further includes a method for making a protective coating, comprising the steps of: providing an activated halide resin; form the activated resin into particles; selecting resin particles substantially in the range of about 0. 1 -300 microns; exposing the resin particles to a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles, having a higher proportion of ionic halogen available, the halogen substance being selected from the group consisting of 12, Br 2 and polyhalide ions having a valence of -1; providing a carrier capable of holding resin particles converted to suspension; and suspend the activated particles in the carrier. The absorption of at least a portion of the halogen substance can • 5 be carried out at elevated temperatures and high pressures. The step of selecting resin particles may include selecting particles substantially in the range of about 0.1 -3 microns, 3-1 5 microns or 15-300 microns. This step may also include selecting particles that are at least twenty percent greater than the particles of any pigment present in the carrier. • The step of providing a carrier can include selecting a carrier comprising a chemical agent resistant coating. The step of providing a carrier may include providing a predetermined volume of pigment particles and the step of suspending the converted resin particles in the carrier, may include suspending a volume of converted resin particles approximately equal to the predetermined volume of pigment particles. . The method includes the step of selecting the predetermined volume of the pigment particles and a volume of converted resin particles 20, such that the combined volumes approach the critical pigment volume of the carrier, or are at least about 90% of the volume of critical pigment of the carrier. The method can also include the step of selecting a volume of the pigment particles and a volume of converted resin particles, so that the combined volumes do not exceed the capacity of the binding resin in the coating, to maintain physical integrity of the cured coating with the extended pigment volume or the step of selecting a pigment particle density greater than the density of the resin particles. The method can also include, the step of selecting environmental conditions to dry the coating, the environmental conditions to dry the coating, the environmental conditions comprising a combination of cure temperature and relative humidity that produce a sufficient drying time, to allow the resin particles to migrate. preferentially to the coating surface. Preferably, the cure temperature is in the range of about 1 5.56 ° C to 32.22 ° C, and the relative humidity is in the range of about 70 to 90 percent. The step of providing a carrier may include selecting a carrier that does not materially interfere with the ion exchange capacity of the converted resin. If the carrier interferes with the activity of the resin particles, the method may further include the steps of applying the coating to a substrate and treating the coating to improve the effectiveness of the resin particles. The treatment step may include mechanically spending or partially dissolving the coating surface to expose the resin particles, so that their activity against target agents is not impeded. The treatment step may also include applying a fixing layer to the surface of the coating and adhering a layer of resin particles to the fixing layer.
These and other objects of the invention will be apparent from the following detailed description. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a graph showing the effectiveness of an activated (but not converted) resin against liquid suspensions of selected biological agents. Fig. 2 is a graph showing the effectiveness of a triiodide resin according to the present invention against chemical warfare agents VX and GD. DETAILED DESCRIPTION OF THE PREFERRED MODEL (S) MODEL (S) MATERIAL OF I NICIO The composition of the present invention can be prepared by starting with a commercially available polyhalide resin having a sufficient amount of available ionic halogen (i.e. loose way). The starting resin comprises polyhalide ions having a valence of -1 absorbed or impregnated in the resin. The starting resin can be, in particular, a polyhalide resin, most preferably, triiodide resin (i.e., resin having triiodide ions of formula 13"absorbed therein.) Preferred starting resins include divinyl based resins. styrene iodides Triosyn®, available from Hydro Biotech, Quebec, Canada The starting polyhalide resin can have any commercially available form, for example, finely divided fragments, or granules, beads, plates or sheets, preferably the starting resin are pearls of consistent size Acceptable results have been obtained using Triosyn® resin beads of approximately 1.5 mm in diameter In general, the starting polyhalide resin is prepared from anion exchange resin, base strong, porous, in • 5 a form of salt. The anion exchange resin is exposed to a sufficient amount of a halogen substance (such as that described herein) absorbable by the anion exchange resin, in order to convert the anion exchange resin into a resin. activated. " For example, a suitable triiodide starting resin can be prepared from an ion exchange resin of • divinyl styrene, as described in U.S. Pat. 5,369,452 for Messier. It is believed that halogenated resins prepared using a quaternary ammonium ion exchange resin, as described in U.S. Pat. 5,431, 908 for Lund, and others Suitable anion exchange resins may also be useful in the practice of this invention. In general, the ion exchange resin used to prepare the starting resin should have physical and chemical properties, • such as plasticity and stability, compatible with the process of particular activation to be used, and will be able to bind to the ionic side of the halogen complexes, but not to the molecular side of these complexes. Ion exchange resins useful in the practice of the invention are usually available in the form of chloride or sulfate, in which case, the ion exchange resin is preferably reacted to obtain the iodide form (I ") or bromide (Br) of the resin before activation The halogen substances useful for preparing the activated resin will normally be selected from the group consisting of diatomic iodine, diatomic bromine and polyiodide ions having a valence of -1. Halogen "includes a solution of polyhalide salt carrier circulated in contact with an elemental halide as described by Lund. For at least some ion exchange resins, the absorption of at least a portion of the halogen substance is effected, preferably at elevated temperature and at high pressure GRINDING / MILLING The activated resin is processed to reach the resin particles the size of desired particle, preferably substantially in the range of, but not limited to, about 0.1 -300 microns, including, by way of example, ranges of approximately 0.1 -3 micras, 3-15 micras and 15-300 micras. Small particles are desirable not only because they provide a high surface area for interaction with chemical and / or biological agents, but also because they facilitate the dispersion of resin forms in dry aerosol and produce a more durable coating when applied as a mix. Particles in the range of about 3-5 microns (average mass diameter) are preferred for dry aerosol applications, although other particle sizes may be used in appropriate cases. Particles in the range of about 5-1 5 microns (average mass diameter) are preferred for coating applications, although somewhat larger or smaller particles may also be used depending on the application method and environmental conditions. Finally, the selection of particle size is based on the consideration of the size of the chemical and / or biological agent and the environment in which the application is used. As explained below, a narrower distribution of the particle size contributes to the effectiveness of the resin particles to devitalize and deactivate biological and chemical agents. Preferably, the size distribution is within 3 standard deviations (3). Resin particles of the desired size can be produced by processing the activated resin (preferably, starting with the bead form) using conventional non-cryogenic grinding and / or grinding devices. Satisfactory results have been obtained using an impact crusher with a stainless steel wheel in combination with a jet mill. Consistent extraction and feeding rates are useful. The resulting powder is sieved to remove larger particles, which can be reprocessed. The smaller particles are generally discharged during processing. The scaling was achieved using a cryogenic crushing process. Commercially available ion exchange resins (such as those used to produce the activated resin described herein) are extremely difficult to process into particles within the desired range of 0.1-300 microns prior to resin activation and it is expected that the proportions of loss will be unacceptable even when it is possible to do this. The halogenation of the resin alters its crystal structure, and in this way its fracture properties, making the • 5 slightly easier grinding and grinding. A resin having an iodine content of at least about 30% is preferred to achieve a reasonably crushable resin. Resins that have an even higher iodine content are likely to exhibit improved crushing capacity. The direct halogenation of exchange resin particles • Commercially available ions of the desired size are not favored for other reasons. It is believed that the processing of such ion exchange resins (eg, drying of divinyl styrene ion exchange resins) to improve their crushing capacity using Conventional methods can make it harder to halogenate the ion exchange resin particles or it can affect the ability of the ion exchange resin particles to absorb the halogen iA substance in sufficient amounts to produce an effective deactivating and devitalizing substance. For example, it is expected that directly halogenated ion exchange resin particles have less halogen in the particle core, and thus, a shorter effective life, than halide resin particles of the present invention. It is also believed that resins prepared by direct halogenation of commercial ion exchange resin particles will be more susceptible to agglomeration than the halide resins of the present invention. Thus, it is preferred that the resin be initially activated prior to grinding and / or milling, rather than grinding or grinding the strong base anion exchange resin prior to activation. CONVERSION (REACTIVATION) Crushing and / or milling of the activated resin into resin particles in the range of about 0.1 -300 microns, results in some particles predominantly having absorbed halogen ions in less available forms than the preferred trihalide ion. For optimum performance, it is therefore necessary to reactivate the activated resin particles, so that they have a higher proportion of available ionic halogen than that present in the activated resin particles. This reactivation of activated resin particles is referred to as conversion. Conversion is achieved by contacting finely divided particles of an activated halide resin with a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles having a higher proportion of available ionic halogen. This causes an increase in the proportion of ionic halogen available in the halide resin particles. Before starting the conversion, the activated resin can be treated to remove the components that can interfere with the absorption of the halide in the resin. For example, the resin can be washed with water to remove undesirable elements, such as material in ionic form. The wash water and other water used to make the converted resin should be free of interfering elements, such as interfering ions. Preferably, distilled or deionized water is used, with water obtained using double reverse osmosis being particularly preferred. The activated resin can also be subjected to an alcohol wash to dissolve undesirable organic material that can be adhered to the resin. The conversion can be achieved, for example, by exposing the activated resin particles to a sufficient amount of absorbable halogen substance by the activated resin to form converted resin particles. The halogen substance used to achieve this conversion can be any material or substance capable of donating a halogen member absorbable by the activated resin to form converted resin particles having a higher proportion of available ionic halogen, as long as the denoted halogen member it is diatomic iodine, diatomic bromine or a polyiodide ion having a valence of -1. Examples of such materials include compositions comprising iodine (12), bromine (Br2) and alkali metal or other halides, and such as potassium iodide, sodium iodide and ammonium iodide in association with water. For example, iodine can be combined with the preferred alkali metal halide, potassium iodide and a smaller amount of water, ie, a sufficient amount of water to avoid crystallization of 12. The composition will contain monovalent iodine ion which will be combined with diatomic iodine (12) to form a polyiodide ion. As used herein, "halogen substance" includes a solution of a polyhalide salt carrier circulated in contact with an elemental halide. Unless the preparation of a mixed halide resin is desired, the selected halogen substance should comprise the same halide present in the activated resin. For example, the halogen substance used for the conversion of an activated Triosyn® resin would comprise an iodine substance, that is, a substance selected from the group comprising iodine crystals (12) and polyiodide ions having • 5 a valence of -1. The molar ratio of halogen ion to diatomic halogen will determine the nature of the polyhalide ion present, ie, trihalide ion and mixtures of trihalide ion and larger polyhalide ions, for example, pentahalide ion. For example, the use of approximately 1 mole iodine ion per mole of diatomic iodine promotes ion formation • triiodide, while the use of a stoichiometric excess of diatomic iodine favors the formation of larger polyiodides. Preferably, the molar ratio of halogen ion to diatomic halogen will favor the association of the resin predominantly converted with trihalide ion, and particularly triiodide ion. Thus, the use of stoichiometric amounts of the halogen ion (e.g., iodine) and halogen molecule (e.g., iodine), (ie, one mole of l2 per mole of I ") is preferred.) The total amount of halogen to be contacted with the resin • activated, residence times, reaction conditions and the like, will depend on factors such as the nature of the polyhalide if it is desired to introduce into the structure of the activated resin, the nature of the activated resin, the intended use of the converted resin, and the desire to minimize the amount of unabsorbed halogen that must be be washed of the converted resin particles. For the use of resin in coatings, The ratio of iodine to resin in the converted resin composition will preferably be in the range of about 50%. It is thought that higher proportions of iodine to resin produce superior results in decontamination applications (eg, dispersion of the resin as a dry aerosol). According to the present invention, the conversion of the activated resin and particularly of the Triosyn® resin can be carried out at an elevated temperature higher than 100 ° C, for example in the range from 1 05 ° C to 1 50 ° C (for example example, 1 10 ° C-1 1 5 ° C to 150 ° C); the upper limit of the temperature used will depend, among other things, on the characteristics of the resin being used. The elevated pressure is any pressure above ambient pressure (eg, a pressure greater than atmospheric or barometric pressure, ie, 0 kg / cm2). The pressure may be, for example, 0.0703 kg / cm2 or greater, for example in the range of 0.3515 to 3.51 5 kg / cm2; the upper limit of the pressure will depend, among other things, on the characteristics of the resin being used. Conversion to elevated conditions can be effected in a reactor that can be pressurized during conversion, but can be opened for recovery of the resin product after a predetermined reaction time. The process can be, in this way, a batch process, where conversion to elevated temperature and pressure is effected once the reactor is sealed. The reactor can be sized and the amount of reagents determined in order to provide a vacuum in the reactor during the reaction, so that the contact takes place under an atmosphere essentially rich in halogen. The pressure in the closed vessel or reactor used to convert the resin to a polyhalide can be a function of temperature, so that the pressure can vary with temperature approximately according to the ideal gas equation PV = nRT, where V = the constant (free) volume of the reactor, n = moles of material in the reactor, R is the universal constant of the gases, T is the temperature and P is the pressure. In a closed vessel, the temperature of the system can therefore be used as a means to achieve or control the desired pressure in the vessel depending on the formation of the halogen substance in the reactor. Thus, a reaction mixture placed in a pressurized reactor can be subjected to, for example, a temperature of 1 05 ° C and a pressure of 200 mm Hg. Alternatively, a relatively inert gas can be injected into a sealed reactor to induce and / or increase the pressure in the reactor. The iodine, an inert gas (noble), air, carbon dioxide, nitrogen or the like, can be used as a pressurizing gas, provided that the chosen gas does not interfere unduly with the production of a suitable halogenated resin. If the pressure is to be induced by steam, steps should be taken to isolate the reaction mixture from excess water. The inert gas is preferably used to increase the resulting pressure from the use of elevated temperatures to effect the conversion. The contact or residence time in high conditions may vary depending on the starting materials, contact conditions, amount of halogen held tenaciously that is desired to be absorbed by the activated resin and other process factors. In this way, the contact time can assume any value; however, it is generally expected that the contact time under the conditions used will be sufficient to maximize the amount of sustained halogen tenaciously absorbed from the material containing the absorbable halogen substance. The residence time can be, for example, as little as 5 to 15 minutes (in the case where a pre-impregnation step is used, as described below) or several hours or more (for example, up to 8 or 9 hours or plus). The high temperature / pressure contact can be preceded by an initial impregnation or absorption step (first step), during which the reaction mixture can be shaken or stirred if desired. The residence time of such a first step can be only a few minutes (for example, from 1 to 10 minutes or more) or up to 24 hours or more (for example, from one hour or more, or from three to twenty-four hours). If the residence time is sufficiently short, so that the time corresponds scarcely to the time necessary to mix the reactants together, the conversion can be considered to be performed essentially in a simple stage at high conditions. The residence time of the first step depends, in part, on the desired final product resin. For example, a slurry containing triiodide ion water can be contacted with the activated resin at ambient temperature and pressure conditions to obtain an intermediate iodide resin conversion product that includes residual iodine substance. This step is preferably carried out in a batch reactor; the obtained intermediate composition comprising an intermediate iodide resin, can then be subjected to the higher temperature and pressure, according to the present invention in a batchwise manner as well. Such a first step can be used to initiate the formation of iodine within the resin matrix. The high temperature / pressure contact conditions can be chosen to maximize the halogen content of the obtained halide resin. For Triosyn® resins in which the halogen substance used during the conversion includes iodine crystals, it is believed that exposure of the activated resin to the halogen substance at a temperature and pressure at, or above, the triple point Crystalline iodine promotes the absorption of the maximum amount of iodine available. It is believed that mixed polyhalide resins may also be useful in the practice of the invention. The conversion of mixed halide resins can be carried out in two steps. In the first step, the activated resin can be exposed to a halogen substance containing a first elemental halogen (eg, diatomic iodine) in an amount sufficient to form some converted polyiodide resin and unconverted resin. In the second step, the resin mixture is exposed to a halogen substance containing a second elemental halogen (for example, diatomic bromine) in an amount sufficient to convert the unconverted resin to polybromide resin. The converted halide resin can be treated before being used to remove any water-repellent iodine, such as, for example, potassium iodide, from the surface of the halide resin, so that in drying the resin, no crystals of halogen compounds will form on the surface of the halide resin. The treatment (e.g., washing) can be continued until no detectable iodine is found (e.g., an iodine content of minus 5 of 0.1 parts per million) or other halogen in the wash water. Any suitable iodine test procedure can be used for iodine detection purposes, if desired. The present invention further comprises a process for preparing resin particles converted from an activated resin, the activated resin being a strong base anion exchange resin, • iodinated, (ie resin having polyiodide ions and with a valence of -1 absorbed or impregnated in the resin as described herein). The process includes the step of forming the activated resin into particles of a desired size, for example, by grinding and / or milling. The process further includes a conversion step, the conversion step comprising contacting the activated resin particles with a sufficient amount of an absorbable halogen substance by the activated resin to form resin particles. • converted having a higher proportion of ionic halogen available.
The halogen substance is selected from the group comprising 12 (ie, diatomic iodine), Br 2 (ie, diatomic bromine) and polyiodide ions having a valence of -1. The conversion step can be characterized in that the absorption of at least a portion of the halogen substance is effected to High temperature and high pressure, being 100 ° C the elevated temperature or higher (for example, a temperature higher than 100 ° C), and the high pressure being higher than the atmospheric pressure. The conversion can be effected essentially or at least partially at a high temperature and high pressure. Thus, the conversion can be carried out in one, two or more stages. For example, the high pressure / temperature conditions can be divided between two different pairs of high pressure / temperature conditions, for example, an initial pressure of 1.0545 kg / cm2 and a temperature of 1 21 ° C, and a subsequent pressure of 0.351 5 kg / cm2 and a temperature of 1 15 ° C. If the conversion is to be carried out in two steps, it may comprise, for example, a first step followed by a second step, and more particularly, a first step carried out at low temperature and pressure conditions (for example, at room temperature conditions). and ambient pressure) and a second step can be carried out at elevated conditions. For example, the first step can be carried out at a temperature of no more than 95 ° C; for example 1 5 ° C to 60 ° C; for example, ambient temperature or ambient temperature, such as a temperature from about 1 5 ° C to about 40 ° C, for example 20 ° C to 30 ° C, and a pressure from zero to less than 0.1406 kg / cm2; the pressure can be, in particular, essentially ambient pressure (i.e., a pressure of less than 0.0703 kg / cm2 at 0 kg / cm2). The second stage can be carried out at a temperature of 102 ° C or higher; for example, 1 05 ° C or higher; for example, 1 10 ° C or higher; for example, 1 1 5 ° C or higher; for example, up to 1 50 ° C at 21 0 ° C, for example 1 15 ° C to 1 35 ° C, and a pressure of 0. 1406 kg / cm 2 or more; for example 0.351 5 kg / cm2 or greater; for example 1 .0545 to 2.4605 kg / cm2; for example, up to 7.03 kg / cm2. In a two step conversion process, for example, the first step may comprise contacting an activated triiodide resin with an iodine substance at a temperature of 100 ° C or less, in order to obtain an intermediate composition, the composition comprising intermediate a residual absorbable iodine substance and an intermediate iodinated resin (ie, an activated resin comprising absorbed polyiodide ions having a valence of -1), and the second step can comprise subjecting the intermediate composition to elevated temperature and elevated pressure, the elevated temperature 1 00 ° C or higher (for example, a temperature greater than 100 ° C) and the pressure being higher than the atmospheric pressure. USE OF CONVERT RESID 1. AEROSOL The converted resin particles can be placed in contact with an objective biological or chemical agent by dispersing the resin particles as a dry aerosol, so that finely divided particles of the substance are dispersed on the article (s) to be treated. Particles in the range of about 3-5 microns (average mass diameter) are preferred for many dry spray applications. The resin particles can be dispersed using a conventional disperser with a Venturi current. A portable disperser can be used for decontamination in the field. The particles are preferably deagglomerated, for example, in a wiper, immediately before being dispersed. A. DECONTAMINATION Dispersed resin particles can be used in a manner • 5 effective alone in certain applications, such as decontaminating articles with rough or uneven surfaces, as well as computers, electronic and electrical equipment, and other materials or equipment that is sensitive to water or reactive with water. The dispersion of the dry aerosol substance is thought, for example, by the nebulization of a room or other area, will allow the substance to penetrate pores, cracks or other • surface irregularities that may be present in or on the article (s) to be treated. This would also allow the substance to be applied to items, such as computers, electronic and electrical equipment, and other materials sensitive to water or reactive with water, which may be further damaged by contact with a devitalizing or deactivating liquid substance, and particularly a water-based substance. Preferably, the size of the dispersed particles is • approximately equal to the size of the agent's particles or drops objective against which the resin particles are expected to be used. It is thought that dispersed resin particles in the range of about 3-5 microns in size are capable of penetrating equipment and structures to approximately the same degree of target agents of this size range, thereby enabling the converted resin particles to devitalize and deactivate the objective agents. A narrow particle size distribution is preferred so that the behavior of the resin particles, whether transported by air or in contact with the surfaces, more closely approximates that of the target agents. In addition, the use of particles in this size range minimizes the likelihood that contaminants will be able to fit between the particles that couple a surface. An amount of resin particles sufficient to cover evenly and deeply, the substrate of interest is necessary to achieve effective decontamination. If the resin particles are applied too thin or uneven, decontamination is likely to be less effective because the resin particles will not have been in contact with all areas of the substrate, allowing the target agents present in those areas to remain in contact with them. its active forms. The method of placing the devitalizing or deactivating substance in the form of a dry aerosol in contact with a substrate may depend on the substrate and the agent to be treated. It is likely that the dispersed particles adhere effectively to wet surfaces (such as those that have recently been in contact with a liquid or tarnished target agent) and horizontal surfaces in still air without additional steps. When these conditions are not present, the selection of the converted resin can be based on the electrostatic properties of the non-fluid targets to be contacted, so that resin particles deposited on the surface tend to be held in engagement with the surface during a period of time. period. It can also be caused that these resin particles contact a static charge inducing material, such as rubber in the barrel of the dispersing nozzle, before the particles enter the Venturi stream to impart an electrostatic charge to the particles. By way of • Alternatively, the substrate can be treated to impart an electrostatic charge that tends to attract the resin particles. A sufficient difference between the electrostatic properties of the resin particles and the substrate is generally necessary to retain the substance in contact with non-horizontal surfaces for a desired time. 10 The application of dry spray for decontamination could also • include providing a treated surface capable of retaining dispersed resin particles in coupling with the substrate. For example, the surface of the substrate can be treated so that the resin particles deposited on the treated surface tend to be held in coupling with the surface for a period. For non-fluid objects that are not liquid sensitive, the application of aerosol may include providing a wetted surface and causing a portion of the dispersed particles to be deposited on the wetted substrate. Any suitable wetting agent (ie, an agent) can be used. humectant compatible with the surface and that does not interfere in any material degree with the capacity of ion exchange of the converted resin). In this way, the method may also include selecting a suitable wetting agent to be applied to the substrate. B. RECLOSING MY DUST PO BOX In addition to being used in decontamination, the devitalizing or deactivating substance in the form of a dry aerosol can also be used to form a protective coating by dispersing or "spraying" the particles onto a wetted surface. Therefore, placement of the devitalizing or deactivating substance in contact with a chemical or biological agent may include providing a treated surface capable of retaining dispersed resin particles in coupling with the substrate for a period. The method may also include the step of selecting a wetting agent to be applied to the surface. Any wetting agent (ie, a wetting agent compatible with the surface and which does not interfere in any material degree with the ion exchange capacity of the converted resin) can be used. The wetting agent preferably comprises a composition which causes the resin particles to adhere to or within the composition, so that the particles remain in contact with the surface after the drying or curing of the wetting agent. Accordingly, the wetting agent may be a paint-like coating, preferably, a chemical warfare resistant coating (CARC) or a hazardous industrial chemical resistant coating. As used herein, "CARC" means a solvent-based coating (the solvent being water or an organic liquid) which, when cured, is resistant to degradation by chemical warfare agents, and is readily and effectively decontaminated. after exposure to such agents. The properties of CARCs are discussed in more detail in MI L-C-29475 (for CARCs transported by water) and MIL-C-46168 (for CARCs transported by solvent), the content of which is incorporated herein by reference. It is believed that the dispersed resin can be used in combination with any suitable CARC, provided that the CARC, either in cured or uncured form, does not interfere in any material degree with the ion exchange capacity of the resin particles. The wetting agent may also comprise a polymeric material. A deep coating or spray is necessary for satisfactory results. Generally, a coating produced by mixing resin particles with a base coating will be preferred over a powder type coating. The resin particles are not embedded in the coating as well as in powder coatings, so that these coatings tend to be more susceptible to abrasion. Powder coatings also tend to have a less uniform appearance and a more gritty texture. It is also more difficult to control the color of powder coatings. However, powder coating can offer advantages in some circumstances. For example, the more gritty texture associated with the powder coating may be preferred for shower floors and the like, because the slip resistance increases. 2. RECEIVING MY ENTOS The resin of the present invention can be incorporated into a coating that can be applied to non-fluid objects to form a film or protective layer thereon. The coating can be made by suspending the resin converted into a suitable base coat or carrier, so that the resin particles are dispersed more or less homogeneously in the carrier. If the converted resin particles are agglomerated as a result of grinding or other previous processing steps, they should be deagglomerated, for example, in a wiper, before being added to the carrier. The particle size of the converted resin is preferably selected such that the particles are slightly larger (by at least about one diameter), and preferably at least 20 percent larger, than any pigment particles present. in the coating. The pigment particles are usually in the range of 3-5 microns, so resin particle sizes in the range of about 4-15 microns (average mass diameter) are generally preferred. This helps provide access to the surface of the converted resin particles adhered to the coating without causing undue interference with the conventional properties of the applied coating, such as abrasion resistance. The largest size limitation refers to the size of the ^ fc commercially available paint spray nozzle instead of a limitation based on the effectiveness of resin particles to devitalize or deactivate chemical and biological agents, so that the use of larger particles would probably reduce the efficiency of the spray application. Larger particles may also be used, for example, in coatings without atomization. A narrow particle size distribution also intensifies the performance of devitalizing and deactivating agents in coatings. It is likely that particles substantially greater than the preferred range cause surface defects and render the coated surface more susceptible to abrasion. Particles substantially less than the preferred range are unlikely to be effective because it is unlikely that any part of their surfaces will be exposed above the level of the coating. An excess of substantially smaller particles will also increase the distance between the exposed particles of the preferred size, so that the surface areas may be unprotected. The carrier can be any material that is compatible with the surface to be coated and that does not interfere, either in cured or uncured form, in any material degree with the ion exchange capacity of the converted resin. Preferably, the volume and consistency of the carrier will allow migration of the converted resin particles to the surface of the coating during drying and / or curing. The properties of the carrier can be selected based on the performance criteria applicable to a particular substrate, such as flexibility, abrasion resistance and chemical resistance. The carrier can, for example, comprise a paint-like coating, such as a CARC transported in water or solvent or coating resistant to a hazardous industrial chemical or a polymeric material. The carrier may also comprise a coating that is selectively permeable to specific fluids, such as polytetrafluoroethylene. Preferably, the carrier will comprise pigments and extenders, although it is also possible to use the converted resin particles in combination with a non-pigmented carrier ("clear coat"). As used herein, "extender" means a paint resin system (but not including the converted resin of the present invention), solvents, and other non-pigmented coating components. It is thought that such carrier systems offer superior abrasion resistance than polymer carriers that are not transported by solvent. Organic and water-based solvents can be used as long as they do not interfere in any material degree with the ion exchange capacity of the converted resin. It is believed, for example, that hexane would not be a suitable solvent. The extender can also be a polymeric material, such as a flexible urethane (polyurea), enamel, acrylic, latex or epoxy. For pigmented base coatings, the volume of the resin particles converted preferably is approximately equal to the volume of pigment particles. This contributes to a uniform distribution of the resin particles converted to the coating after it is applied. Preferably, the pigment particle density is greater than the density of the resin particles. The amount of the converted resin blended with the carrier can vary with the nature of the carrier and the desired performance characteristics in the coating. The amount of resin converted can also vary with the color of coatings using a common extender system due to changes in the pigments. Generally, the determination of the amount of resin converted to be mixed with the carrier involves balancing the ion exchange activity (deactivating and devitalizing) against the integrity of the coating. Preferably, sufficient resin is provided to form a monolayer of resin particles from the surface of the substrate after the drying / curing of the coating is completed. • A higher devitalizing and deactivating activity is expected in the applied coating when the converted resin particles are added to a carrier until an almost critical volume of pigment is obtained. As used herein, "critical pigment volume" means the maximum volume of particles (pigment and converted resin) which can be added to a given amount of a coating. The almost critical pigment volume means a pigment volume in excess of 90% of the critical volume. A resin content approaching the critical pigment volume will provide adequate ion exchange while maintaining the integrity of the coating.
Most preferably, for pigmented base coatings, "resin -" pigment = Vcp't? Co where Vresma is the volume of resin particles converted, Vpigment is the volume of pigment and Vcrit1Co is the volume of critical pigment. The proportion of converted resin particles is likely to result in an optimum amount of converted resin particles distributed substantially uniformly on the surface of the substrate to which the coating is applied.The combined volumes of the pigment particles and the resin particles The converted mixture should not exceed the capacity of the binding resin in the coating to maintain the physical integrity of the cured coating with the volume of pigment spread.The resulting mixture can be applied to a surface of the object to be coated by any suitable conventional means, for example. example, brushing, rolling, atomizing, troweling, emptying or similar The mixture can be applied in multiple coatings if necessary, but it is believed that multiple coatings either help or obstruct the performance of the devitalizing or deactivating substance. The control of environmental conditions, such as cure temperature and relative humidity, during drying of the coating, may allow the resin particles to migrate preferentially to the coating surface. Although these conditions vary with the binding resin present in the carrier, the curing temperatures in the range of about 15.56 ° C to 32.22 ° C and relative humidity in the range of about 70 to 90 percent, generally favor sufficient drying time. to allow migration of the resin particles to the coating surface. It may be advantageous to apply a primer to the substrate prior to the application of the topcoat of mixture to minimize the migration of chemicals from the topcoat to the substrate. It may also be advantageous to apply the mixture to a substrate using processes known in the art that provide an electrostatic charge to the substrate surface to provide more uniform coverage and assist migration of the converted resin particles to the surface of the coating.
Although the selection of a suitable coating for the inclusion of resin particles is generally preferred, however, coatings that are not suitable for the inclusion of resin particles due to the interference of the binding resin or the pigment particles can not be used, especially when these coatings otherwise have particularly preferred physical properties. Such coatings can be treated to allow them to be used in combination with resin particles. For example, the surface of an otherwise inadequate coating can be worn mechanically or partially dissolved to expose the particles of • resin, so that its activity against target agents is not impeded. A fixing layer, such as an adhesive or topcoat, can also be applied to the surface of an otherwise inadequate coating and a layer of resin particles adhered to it. the fixing layer. The long-term effectiveness of the devitalizing and deactivating substance in coatings has not yet been studied, although this will probably vary with the conditions to which the substances are exposed. • coated objects. It is thought that under ordinary conditions, life The effective amount of the converted resin particles will be at least approximately comparable with the effective life of the overall coating. A field test has not been developed to monitor the effectiveness of the coating, although iodine detection tests are available for other applications. 25 DEVITALIZING / DEACTIVATING As described above, converted resin particles can be used to decontaminate non-fluid objects that have been exposed to biological agents. They can also be used to provide a protective coating on non-fluid objects that are likely to be exposed to biological agents, so that the coating is capable of devitalizing these agents on demand (at least until the devitalizing substance present in the coating has been exhausted). without significant damage to the usual utility of the object and without application of a substance or procedure of decontamination or discreet devitalization after exposure to the agent. The protective coating can be applied not only to objects that are likely to be exposed to biological agents on a more or less regular basis, but also to objects that can be exposed to such agents in the event of a catastrophe. The converted resin particles can also be used to deactivate chemical agents and other industrial toxic chemicals with a sufficient energy bond to facilitate the reaction with iodine. The chemical agent deactivating particles may be used to decontaminate fluids that may contain chemical agents, to decontaminate non-fluid objects that may have such agents on their surfaces, or to provide a protective coating on non-fluid objects that will likely be exposed to such agents. The protective coating can provide increased resistance to chemical agents, even if it is not capable of deactivating all those possible agents. In certain circumstances, chemical agent deactivating particles may also be able to devitalize biological agents. The effectiveness of the converted resin particles to achieve devitalization and deactivation depends on the ionization potential of the target agent, the distance between the agent and the ion source of converted resin, and the existence of a route between the agent and the source of ions that a halide ion can travel. For example, it is thought that the pore size of some coatings is sufficiently large so that the iodine ions can pass through the pores and the acceptable level of devitalization and / or deactivation can be achieved, even when the • Resin particles do not directly contact the agent. However, access to the iodine ions associated with the resin particles is critical. If the converted resin particles are completely covered by an adhesive, for example, the effectiveness of the devitalization and deactivation is greatly reduced. The success to devitalize and deactivate biological and chemical agents depends greatly on putting the resin converted in contact with such agents. Higher results are obtained when the converted resin is able to directly contact the agent and remain in contact with the agent for a predetermined time. The time necessary for the effect of the devitalization and deactivation capacity of the resin particles depends on the proximity of the contact between the particles and the target agent and the type of agent. Devitalization, if it is going to occur, can take place within a few minutes or less for vegetative cells, and within tens of minutes for spores. The deactivation of chemical agents, if it is going to occur, can take place within tens of minutes. PRU EBAS The iodide resin of the present invention has been successfully tested against chemical warfare agents GD and VX, as well as viruses and spore-forming bacteria. Activated Triosyn® T40 and T50 resins containing 40% and 50% iodine, respectively, in the form of beads or fragments, were tested against liquid suspensions of various biological agents, including spores of Bacillus subtilis var. niger ("spores Bg") and Erwinia herbicola ("Eh"). A non-active resin was used as a control. The non-active resin refers to a non-halogenated ion exchange resin in the form of beads of about 1.5 mm in diameter (i.e., ion exchange resin beads that have not been activated, ground into finely divided particles) , or converted as described above), but which have been washed and otherwise processed through the stages described before activation. The type and form of activated resin, exposure time, target organism and percentage of reduction are shown in Table 1. Table 1 As shown in Table 1, the reduction in viability was generally at least 80% effective at the indicated exposure times, without any reduction in viability observed with the resin not • active. The results are shown graphically in Fig. 1 . Table 2 • Table 2 provides reduction values for coating samples prepared with a triiodide resin according to the present invention. The converted resin was prepared from Tríosyn® resin T-50 that had been crushed into particles in the range of about 3-1 5 microns and converted using iodine crystals, of, so that the converted resin contained approximately 50% iodine. The converted resin was added to samples of commercially available coatings. The CARC transported with water had 50% resin added based on paint solids and the CARC transported 5 in solvent, latex and enamel each had 75% resin added based on paint solids. Non-iodized samples of the same base coat formulations were used as controls. The coatings were applied to test coupons and allowed to cure. The test coupons were coated with a liquid suspension of Erwinia herbicola (Eh) at 1 x 106 colony forming units (CFU) per milliliter. The contact time was 1 5 minutes. The paint coupons were extracted in phosphate buffered saline and platinized to determine remaining cultivable CFUs. The values of The reduction percentage represents the average reduction in cultivable CFUs in the test coupons compared to the remaining average CFUs in the appropriate control samples. A triiodide resin according to the present invention was tested against chemical warfare agents GD, H D and VX. The resin The converted was prepared from the Triosyn® T-50 resin that had been crushed to particles in the range of about 3-1 5 microns and converted using iodine crystals, so that the converted resin contained approximately 50% iodine. Converted resin samples of 10 g were driven with 2 microliters of GD, HD and VX, respectively (the "initial amount" shown graphically in Fig. 2 for GD and VX). Non-iodized ion exchange resin beads (approximately 1.5 mm in diameter) used as a control were also nailed with 2 microliters of each of these agents. After an exposure time of one hour, the agents were extracted from the samples using chloroform and analyzed by gas chromatography to give the "recovery amount" or amount of the unreacted agent remaining in the sample at the end of this weather. The amount of decomposition products resulting from the interaction of the agents with the converted resin was also determined for GD and VX. As shown in Fig. 2, a significant reduction in the effective amount of VX was observed. A minimal reduction for DG was observed, although the presence of decomposition products suggests that the reduction may be occurring at low speed. Based on the preliminary data, it is expected that the recovery amounts for H D are similar to those observed for GD. No measurable reduction was noted for non-active resin control samples. Throughout this specification, when a range of conditions or a group of substances is defined with respect to a particular characteristic (e.g., temperature, pressure, time and the like) of the present invention, the present invention relates to, and explicitly incorporates, each and every one of the specific members and combinations of sub-ranges or sub-groups in it. Any specified rank or group will be understood as a brief way of referring to each and every one of the members of a rank or group individually, as well as each and every one of the possible sub-ranges and sub-groups included in it; and similarly with respect to any sub-range or sub-group therein. Thus, for example, a pressure greater than atmospheric will be understood as specifically incorporating • 5 each and every one of the individual pressure states, as well as sub-range, above atmospheric, such as, for example, 0.1406 kg / cm2, 0.351 5 kg / cm2, 1 .406 kg / cm2, 2.4956 kg / cm2, 0.3515 to 0.5624 kg / cm2, 0.351 5 to 2.4605 kg / cm2, 0.703 to 1.7575 kg / cm2, 1 .406 to 2.812 kg / cm2, 2.4605 to 3.515 kg / cm2, 0.1406 to 7.03 kg / cm2, etc. Although a specific embodiment of the invention has been described in • the present in detail, it is understood that variations may be made thereto by those skilled in the art without departing from the spirit of the invention or the scope of the appended claims. •

Claims (49)

  1. CLAIMING IS 1 . A substance capable of reducing the effectiveness of target agents, comprising: • 5 halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated in the resin particles and characterized in that an activated halogenated resin is substantially particulate in the range of approximately 0.1-300 microns before exposure to a sufficient amount of a substance 10 of absorbable halogen by the activated resin to form particles of • converted resin having a higher proportion of available ionic halogen, said halogen substance being selected from the group consisting of l2, Br2 and polyiodide ions having a valence of -1, said converted resin particles being capable of being dispersed as 15 a dry spray.
  2. 2. A substance according to claim 1, wherein the halide resin particles are further characterized in that an activated halogenated resin is particulate split substantially in the • range of approximately 0.1-3 microns before exposure to 20 halogen substance.
  3. 3. A substance according to claim 1, wherein the halide resin particles are further characterized in that an activated halogenated resin is divided into particles substantially in the range of about 3-1 5 microns before exposure to the 25 halogen substance.
  4. 4. A substance according to claim 1, wherein the halide resin particles are further characterized in that an activated halogenated resin is divided into particles substantially in the range of about 1 5-300 microns prior to exposure to the 5 halogen substance. The composition according to claim 1, wherein the converted resin particles are electrostatically charged to help maintain said particles in coupling with a substrate. The composition according to claim 1, wherein the converted resin particles are electrostatically charged before • to be dispersed. The composition according to claim 1, wherein the converted resin particles are passed through a nozzle, said converted resin particles being coupled to a substance 15 static charge inducer in the nozzle. 8. A coating capable of reducing the effectiveness of target agents, comprising: halide resin particles comprising polyhalide ions Having a valency of -1 absorbed or impregnated in resin particles and characterized in that an activated halogenated resin is divided into particles substantially in the range of about 0.1-300 microns before exposure to a sufficient amount of an absorbable halogen substance by activated resin to form converted resin particles having a higher proportion of ionic halogen • available, said halogen substance being selected from the group consisting of l2, Br2 and polyiodide ions having a valence of -1; and a carrier holding said resin particles converted into suspension, said suspension being suitable for use as a coating. The coating according to claim 8, wherein the halide resin particles are further characterized in that an activated halogenated resin is divided into particles substantially in the range of about 0.1-3 microns before exposure to the 10 halogen substance. • 1 0. The coating according to claim 8, wherein the halide resin particles are further characterized in that an activated halogenated resin is divided into particles substantially in the range of about 3-15 microns before exposure to the 15 halogen substance. eleven . The coating according to claim 8, wherein the halide resin particles are further characterized in that an activated halogenated resin is substantially particulate • in the range of approximately 1 5-300 microns before exposure to 20 halogen substance. The coating according to claim 8, wherein the carrier does not materially interfere with the ion exchange capacity of said converted resin. The coating according to claim 8, wherein the carrier includes a predetermined volume of pigment particles and the volume of resin particles converted suspended in said carrier is approximately equal to the volume of pigment particles. 14. The coating according to claim 1 3, wherein the combined volumes of the pigment particles and the particles of The converted resin approximates the critical pigment volume of the carrier. The coating according to claim 14, wherein the combined volumes of the pigment particles and the converted resin particles are at least about 90% of the volume of 10 critical pigment of the carrier. 16. The coating according to claim 8, wherein the carrier includes pigment particles, the combined volume of the pigment particles and the converted resin particles approaching the critical pigment volume of the carrier. The coating according to claim 8, wherein the particles of the converted resin are at least 20 percent larger than the particles of any pigment present in the carrier. 18. The coating according to claim 8, wherein the • carrier comprises a coating resistant to chemical agent of 20 war. 9. The coating according to claim 8, wherein the converted resin is capable of reducing the effectiveness of target agents selected from the group consisting of biologically generated chemical agents, biological agents and toxins. 20. The coating according to claim 8, wherein the carrier comprises a coating resistant to hazardous industrial chemical. twenty-one . The coating according to claim 8, wherein the carrier comprises a coating that is selectively permeable to specific fluids. 22. The coating according to claim 8, wherein the carrier comprises a latex. 23. A method for making a protective coating, comprising the steps of: providing an activated halide resin; form the activated resin into particles; selecting resin particles substantially in the range of about 0.1 -300 microns; exposing the resin particles to a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles having a higher proportion of available ionic halogen, the halogen substance being selected from the group consisting of 12, Br 2 and ions polyhalide having a valence of -1; providing a carrier capable of supporting said resin particles converted into suspension; and suspending said activated particles in said carrier. The method according to claim 23, wherein the step of selecting resin particles includes the step of: - selecting resin particles substantially in the range of about 0.1 -3 microns. 25. The method according to claim 23, wherein the step of selecting resin particles includes the step of: selecting resin particles substantially in the range of about 3-1 5 microns. 26. The method according to claim 23, wherein the step of selecting resin particles includes the step of: selecting resin particles substantially in the range of about 1 5-300 microns. 27. The method according to claim 23, wherein the step of exposing the resin particles to a sufficient amount of a halogen substance to form converted resin particles includes the step of: causing at least a portion of said Halogen substance is absorbed by the activated resin at an elevated temperature and at high pressure, said elevated temperature being a temperature greater than 1 00 ° C and up to 21 0 ° C, said elevated pressure being a pressure greater than the atmospheric pressure and up to 7.03 kg / cm2. 28. The method according to claim 23, wherein the step of providing a carrier includes the step of: selecting a carrier that does not materially interfere with the exchange capacity of the converted resin. 29. The method according to claim 23, wherein the step of 25 providing a carrier includes the step of: selecting a carrier comprising a chemical agent resistant coating. The method according to claim 23, wherein the step of providing a carrier includes the step of providing a predetermined volume of pigment particles and the step of suspending the resin particles converted to the carrier includes the step of suspending a volume of converted resin particles approximately equal to the volume of pigment particles. 31 The method according to claim 30, further comprising the step of: selecting the predetermined volume of the pigment particles and a volume of converted resin particles, such that the combined volumes approach the critical pigmented volume of the carrier. 32. The method according to claim 31, further including the step of: selecting the predetermined volume of the pigment particles and a volume of converted resin particles, such that the combined volumes are at least about 90% of the volume of critical pigment of the carrier. The method according to claim 23, wherein the step of providing a carrier includes the step of providing a carrier including pigment particles and the method further includes the step of: * * selecting a volume of pigment particles and a volume of converted resin particles, so that the combined volumes approach the critical pigment volume of the carrier. 34. The method according to claim 23, wherein the step of selecting resin particles includes the step of: selecting resin particles that are at least twenty percent larger than the particles of any pigment present in the carrier. 35. The method according to claim 31, wherein the step of providing a carrier includes the step of providing a carrier having a binding resin and the method further includes the step of: selecting a volume of the pigment particles and a volume of converted resin particles, so that the combined volumes do not exceed the capacity of the binding resin to maintain the physical integrity of the cured coating with the volume of pigment spread. 36. The method according to claim 23, further comprising the step of: selecting a pigment particle density greater than the density of the resin particles. 37. The method according to claim 23, further comprising the step of: selecting the environmental conditions for drying the coating, said environmental conditions comprising a combination of cure temperature and relative humidity that produce a drying time? > sufficient to allow the resin particles to migrate preferentially to the coating surface. 38. The method according to claim 37, wherein the cure temperature is in the range of about 15.56 ° C to 5 32.22 ° C, and the relative humidity is in the range of approximately 70 to 90 percent. 39. The method according to claim 23, wherein the carrier interferes with the activity of the resin particles, said method further including the steps of: applying the coating to a substrate; and treating the coating to improve the effectiveness of the resin particles. 40. The method according to claim 39, wherein the treatment step includes the step of: mechanically spending the coating surface to expose the resin particles, so that their activity against target agents is not impeded. 41 The method according to claim 39, wherein the treatment step includes the step of: partially dissolving the coating surface to expose the resin particles, so that their activity against target agents is not impeded. 42. The method according to claim 39, wherein the treatment step includes the steps of: applying a fixing layer to the coating surface; Y ti t-u -.-. fca-a f *} Adhere a layer of resin particles to the fixing layer. 43. A chemical agent deactivator of demand, comprising: halide resin particles having a particle size substantially in the range of about 0. 1 -300 microns, 5 said halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated in resin particles. 44. A resin composition, comprising: halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into particles of • resin having a particle size substantially in the range of about 0.1 -15 microns. 45. The resin according to claim 44, wherein said halide resin is characterized in that an activated halogenated resin is 15 divided into particles substantially in the range of about 0.1-1.5 microns prior to exposure to a sufficient amount of a halogen substance absorbed by the activated resin to form converted resin particles having a greater proportion of • ionic halogen available, said substance being selected from 20 halogen of the group consisting of l2, Br2 and polyiodide ions having a valence of -1. 46. A resin composition, comprising: halide resin particles comprising polyhalide ions having a valence of -1 absorbed or impregnated into particles of 25 resin and characterized in that an activated halogenated resin is divided < » in particles substantially in the range of about 1 5-300 microns before exposure to a sufficient amount of a halogen substance absorbable by the activated resin, to form converted resin particles having a higher proportion of ionic halogen 5 available, being selected said halogen substance of the group consisting of l2, Br2 and polyiodide ions having a valence of -1. 47. A method for making a resin composition, comprising the steps of: providing an activated halide resin; 10 form the activated resin into particles; selecting resin particles substantially in the range of about 0.1 -300 microns; and forming converted resin particles having a higher proportion of available ionic halogen. 48. A method for deactivating a target agent, comprising the steps of: providing an activated halide resin; form the activated resin into particles; selecting resin particles substantially in the range of about 0.1 -300 microns; exposing the resin particles to a sufficient amount of a halogen substance absorbable by the activated resin to form converted resin particles having a higher proportion of ionic halogen available, the halogen substance being selected < / "* - of the group consisting of l2, Br2 and polyhalide ions having a valence of -1, and placing said resin particles contacted with a target agent selected from the group consisting of chemical agents, • biological agents and biologically generated toxins. 49. The method according to claim 48, wherein the step of placing resin particles contacted with a target agent includes the steps of: providing a carrier capable of holding said particles of 10 resin in suspension; Suspend said converted particles in said carrier; and apply the suspension to a surface. - ^ P to SUMMARY A substance capable of devitalizing dangerous biological agents and deactivating dangerous chemical agents that comprise a resin of • anionic exchange having a particle size substantially in the range of about 0.1 -300 microns, said resin particles have been iodized through exposure to a sufficient amount of an iodine substance absorbable by the anion exchange resin, so that the resin particles absorb the iodine substance for 10 convert the resin particles into activated resin particles. The iodine substance can be selected from the group consisting of 12 (example: biatomic iodine) and polyiodide ions having a valence of -1. The activated resin particles can be contacted with the biological and chemical agent as a dry aerosol, by coating 15 of powder, or by mixing the particles with a carrier to form a coating.
MXPA/A/2000/009196A 1998-03-19 2000-09-19 Composition for deactivating chemically and biologically active agents MXPA00009196A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US60/078,642 1998-03-19
US09270636 1999-03-17

Publications (1)

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MXPA00009196A true MXPA00009196A (en) 2002-07-25

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