CLAIM FOR PRIORITY

[0001] This PCT International Application claims the benefit of priority of U.S.

Provisional Application No. 62/373,727, fled August 11 , 2016, the subject matter of which is incorporated herein by reference in its entirety.

DESCRIPTION

Field

[0002] This disclosure is related to antimicrobial compositions, more specifically to antimicrobial compositions including at least one mineral and an antimicrobial metal compound, and related methods of use.

BACKGROUND

[0003] In many filtration applications, a filtration device may include a filter element, such as a septum, and a filter-aid material. The filter element may be of any form such that it may support a filter-aid material. For example, the filter element may include a cylindrical tube or wafer-Ike structure covered with a plastic or metal fabric of sufflclentty fine weave. The filter element may be a porous structure with a filter element void to allow material of a oartain size to pass through the titration device. The Miter-aid material may include one or more filtration components, which, for example, may be Inorganic powders or organic fibrous materials. Such a filter-aid material may be used In combination with a filter element to enhance fUtratJon performance of a filtration device.

[0004] For example, the fitter-eld material may Initially be applied to a septum of a After element In a process known as "pre-coating." Pre-coating may generally involve mixing a slurry of water and fitter-aid material, and introduchg the slurry Into a stream flowing through the septum. During this process, a thin layer, such as, for example, about 1.5 mm to about 3.0 mm, of fitter-aid material may eventually be deposited on the septum, thus pre- coating the septum.

[0005] During filtration of a fluid, various insoluble particles hi the fluid may become trapped by the filter-aid material. The combined layers of fitter-aid material and particles and/or constituents to be removed accumulate on the surface of the septum. Those combined layers are known as "fitter cake." As more and more particles and/or constituents are deposited on the filter cake, the flter cake may become saturated with debris to the point where fluid Is no longer able to pass through the septum.

[0006] To combat this situation, a process known as "body feeding" may be used. Body feeding la the process of Introducing additional fitter-aid material into the fluid to be filtered before the fluid reaches the filter cake. The filter-aid material will follow the path of the unflttered fluid and wfll oventualy reach the fitter cake. Upon reaching the fitter cake, the added fitter-aid material wiB bind to the cake in a simlar manner to how the filter-aid material is bound to the septum during the p re-coating process. The additional layer of filter-aid material may cause the filter cake to swel and thicken, and may increase the capacity of the filter cake to entrap additional debris. The filter aid typically has an open porous structure, which maintains an open structure in the filter cake, thus ensuring continued permeabiity of the filter cake.

[0007] In the field of fluid filtration, diatomaceous earth and minerals such as perflte are commonly employed as fitter aide. Diatomaceous earth products may be obtained from diatomaceous earth (also caBed "DE" or "diatom its"), which Is generaly known as a sediment-enriched in biogenic silica (i.e., silca produced or brought about by Rvfcng organisms) in the form of sHceous skeletons (frustules) of diatoms. Diatoms are a diverse array of microscopic, slngle-ceHed, golden-brown akjae generally of the class

Bartlariophyceae that possess an ornate siliceous skeleton of varied and intricate structures including two valves that, in the living diatom, fit together much Ike a pil box.

[0008] Diatomaceous earth may form from the remains of water-borne diatoms and, therefore, diatomaceous earth deposits may be found close to either current or former bodies of water. Those deposits are generally divided Into two categories based on source: freshwater and saltwater. Freshwater diatomaceous earth is generally mined from dry lakebeds and may be characterized as having a low crystallne silica content and a high iron content In contrast, saltwater diatomaceous earth is generally extracted from oceanic areas and may be characterized as having a high crystallne slica content and a low iron content

[0009] In the field of filtration, methods of particle separation from fluids may employ diatomaceous earth products or glass products as fitter aids. The intricate and porous structure unique to diatomaceous earth may, In some Instances, be effective for the physical entrapment of particles in filtration processes. It is known to employ diatomaceous earth products to improve the clarity of fluids that exhibit "turbidity" or contain suspended particles or particulate matter. Turbidity is the cloudiness or haziness of a fluid, where the haze may be caused by Individual particles that are suspended In the fluid. Materials that may cause a fluid to be turbkJ include, for example, clay, silt, organic matter, inorganic matter, and microscopic organisms. [0010] Existing fitters may be costly and/or Ineffective at removing aD microscopic organisms from a fluid. Additionally, cleansing compositions may include various additives to improve the ability of those cleansing compositions to dean various surfaces. However, certain additives may not be effective at reducing undesirable microscopic organisms after use.

[0011] Thus, it may be desirable to provide compositions that assist with removing or Idling microscopic organisms. That is, It may be desirable to provide compositions that assist with reducing or Idling undesirable germs and bacteria.

SUMMARY

[0012] It Is to be understood that both the foregoing general description and the following delated description are exemplary and explanatory only and are not restrictive of the disclosure, as claimed.

[0013] In one embodiment, the present disclosure is directed to a composite titer aid including a mineral associated with an antimicrobial metal compound. The fitter aid may have a permeability ranging from 0.1 to 20 darcys.

[0014] The fitter aid may have e permeablHy ranging from 0.1 - 0.3 Darcys, 0.3 - 0.5 Darcys, 0.5 to 1.0 Darcys, 1 to 2 darcys, from 2 to 20 darcys, from 2 to 10 darcys, or from 2 to 5 darcys. A ratio of the antimicrobial metal compound to the mineral may range from 1:1000 to 1:4 by weight, from 1:100 to 1:5 by weight, from 1:100 to 1:10 by weight, from 120 to 1 :5 by weight, or from 1 :20 to 320 by weight.

[0015] The antimicrobial metal compound may include at least one of zinc, copper, and slver. The antimicrobial metal compound may include zinc oxide. The antimicrobial metal compound may Include antimicrobial metal compound particles, and the antimicrobial metal compound particles may be attached to a surface of the mineral. The antimicrobial metal compound particles have a particle size less than 200 nm, less than 150 nm, less than 100 nm, less than 50 nm, less than 25 nm, less than 20 nm, less than 15 nm, less than 10 nm, or less than 5 nm.

[0016] The mineral may include diatomaceous earth. The diatomaceous earth may be obtained from a freshwater source. The diatomaceous earth may be obtained from a saltwater source. The diatomaceous earth may have a d ₁₀ ranging from 3 d ₁₀ to 20 urn. The diatomaceous earth may have a median particle size (d ₉₀ ) ranging from 10 d ₁₀ to 50 urn. The dlatomaceoue earth may have a top particle size (dto) ranging from 30 d ₁₀ to 120 urn. The diatomaceous earth may have a pore volume ranging from about 2 ml/g to about 8 ml/g. The diatomaceous earth may have a median pore diameter ranging from about 1 d ₁₀ to about 8 μm. The diatom aceous earth may have a bulk density ranging from about 4 fa/It* to about 15 to/ft*. The dlatomaceous earth may be non-calcined, calcined, or flux-calcined.

[0017] The mineral may Include at least one of perltte, volcanic ash, pumice, shirasu, obsidian, pitch stone, and rice hull ash. The mineral may oeperiite. The perirte may include expanded perirte. The periite may include milled, expanded perirte. The perltte may Include unexpended periite. The periite may have an aspect ratio of 1:1 to 1:50. The perirte may have an aspect ratio of 1:2 to 1:35. The mineral may also include at least one of kaoRn, tab, vermlculltB, mica, and wollastonite.

[0018] The fitter aid may have a pore volume ranging from about 2 ml/g to about 8 ml/g. The fitter aid may have a median pore diameter ranging from 1 μm to about 8 urn. The filter aid may have a d ₁₀ ranging from 5 μm to 30 urn. The filter aid may have a median particle size (d ₅₀ ) ranging from 10 d ₁₀ to 70 μmι. The filter aid may have a top particle size (dm) ranging from 80 d ₁₀ to 120 urn. The filter aid may have a wet density ranging from about 12 Ib/ft ³ to about 25 Ibft ³ . The fitter aid may have a buk density ranging from about 5 Ib/ft ³ to about 14 lb/ft ³ . The fitter aid may have a beer soluble iron content of less than 5 pd ₁₀ , as measured by ASBC, or toss than 1 ppm, as measured by ASBC. The filter aid may have a cristobalite content of less than 20 percent by weight, less than 10 percent by weight, less than 8 percent by weight, or less than 1 percent by weight The filter aid may have a BET surface area ranging from 1 m ² /g to about 50 m ² /g.

[0019] A method may include filtering a fluid with the filter aid as set forth above. The fluid may be a beverage. The beverage may be beer, wine, or juice. The fluid may be oil. The oil may be edible oil or biodiesel.

[0020] In another embodiment, the present disclosure Is directed to a method of filtering a fluid with an antimicrobial filter aid. The method may include passing the fluid through a filter containing the antimicrobial fitter aid, and the antimicrobial fitter aid may Include a mineral associated with an antimicrobial metal compound. This method may Include any of the features set forth above wtth respect to the composite filter aid.

[0021] The fluid may be a beverage. The beverage may be beer, wine, or juice. The method may remove or eliminate lactic acid bacteria from the beer, wine, or juice. The fluid may be ol. The oil may be edible oil or biodiesel. The lactic acid bacteria can be selected from any of Oenococcus oeni, and various species of Lactobac&us and Pedkxoccus.

[0022] In yet another embodiment, the present disclosure is directed to a method of filtering a fluid. The method may include Simula neou sly removing particulate from the fluid and reducing micro-organism content of the fluid. This method may Include any of the features set forth above wtth respect to the composite titer aid. [0023] The fluid may be a beverage. The beverage may be beer, wine, or Juice. The method may remove or eliminate tactic acid bacteria from the beer, wine, or juice. The fluid may be oil. The oil may be edible oil or b!odieset. The micro-organism content may be lactic acid bacteria content

[0024] In yet another embodiment, the present disclosure is directed to a composition including a mineral selected from one of diatom aceous earth, talc, wollastonite, kaolin, and bentonite, and an antimicrobial metal compound associated with the mineral. This composition may include any of the features set forth above with respect to the various disclosed minerals and antimicrobial metal compounds.

[0025] The composition may be a personal care composition, a cosmetic composition, or a cleaning composition. The composition may be an exfblating cleansing composition. The composition may be a shower gel or bath gel. The composition may be a hair shampoo. The hair shampoo may be an anti-dandruff shampoo. The composition may be an exfoliating cosmetic composition. The composition may be a paint composition. The composition may be a polymer filer. The composition may be a dentrifice composition. The dentifrice composition may exhbit an RDA value less than 200, or less than 150. The dentifrice composition may exhibit a PCR value of at least 80, at least 100, or at least 120. The composition may include a toothpaste base. The toothpaste base may include at least one of binders, humectants, abrasives, detergents, flavoring agents, and preventatives.

[0026] In yet another embodiment, the present disclosure is directed to a sunscreen composition including a mineral selected from one of dhrtomaceous earth, talc, wollastonite, kaolin, bentonite, calcium carbonate, mica, and perite, and zinc oxide associated with the mineral, wherein a ratio of the zinc oxide to the mineral Is at least 1 : 1 by weight This sunscreen composition may include any of the features set forth above with respect to the various disclosed minerals and zinc oxide.

[0027] The ratio oflhe zinc oxide to the mineral ranges from 1:1 to 9:1 by weight from 1:1 to 4:1 by weight, from 3:2 to 4:1 by weight or from 3:2 to 3:1 by weight The mineral may be talc. The talc may be delaminated. The talc may have a BET surface area of least about 10.0 rrf/g. The talc may have a lamellarity index of at least about 3.0. The talc may have a lamellarity index of at least about 4.0. The talc may be uncoated. The sunscreen composition may Include one or more emollenta, emutslfiers, hydrants, thickeners and/or surfactants. The composition may be a cream, ointment, lotion, or in sprayable form. The sunscreen composition may have a SPF of at least about 6.0. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Fig. 1 is a scanning electron micrograph of a sample of an exemplary embodiment of zinc oxide treated diatomaceous earth. The bright small particles are the nano zinc oxide particles deposited on the DE surface.

[0028] Fig. 2 is another scanning electron micrograph of a sample of an exemplary embodiment of zinc oxide treated diatomaceous earth. The bright particles are the nano zinc oxide particles deposited on the DE surface.

[0030] Fig. 3 is a graph of an energy-dispersive x-ray spectrum of an exemplary embodiment of zinc oxide treated diatomaceous earth. The Zn peak in the spectrum confirms nano ZnO particles deposited on the DE surface.

DESCRIPTION OF EXEMPLARITY EMBODIMENT

[0031] Particular embodiments of the present disclosure are described In greater detail below. The terms and definitions provided herein control, if in conflict wftfi terms and/or definitions incorporated by reference.

[0032] As used herein, the terms "comprises," "comprising," or any other variation thereof are Intended to cover a non-exclusive inclusion, such that a process, method, composition, article, or apparatus that comprises a list of elements does not include only those elements, but may include other elements not expressly listed or inherent to such process, method, composition, article, or apparatus. The term "exemplary" Is used in the sense of "example" rather than "Ideal."

[0033] As used herein, the singular forms "a," "an," and the' include plural reference unless the context dictates otherwise. The terms "approximately" and "about" refer to being nearly the same as a referenced number or value. As used herein, the terms "approximately" and "about" should be understood to encompass 15 percent of a specified amount or value.

[0034] Compositions of the present disclosure may include a mineral and an antimicrobial compound associated wtth the mineral. The mineral may include one or more of diatomaceous earth, perlite, mica, talc, clay, kaolin, smectite, wollastonite, bentonite, and calcium carbonate, and the antimicrobial compound may be an antimicrobial metal compound, such as, e.g., zinc oxide, although other suitable antimicrobial metal compounds, discussed in further detal below, also are contemplated.

[0035? In some embodiments, the at least one diatomaceous earth is obtained from a saltwater source. In some embodiments, the at least one diatomaceous earth Is obtained from a freshwater source. In further embodiments, the at least one diatomacaous earth is any dlatomaceous earth material that may be capable of use in composite material such as a composite fitter aid, either In its crude form or after subjecting the material to one or more processing steps In some embodiments, the at least one dlatomaceous earth is any dlatomaceous earth material that has not been subjected to at least one thermal treatment In still other embodiments, the at least one dlatomaceous earth is any diatomacaous earth material that has not been subjected to caicihation. Average particle size for the

dlatomaceous earth can range from 5 to 200 μm, surface area ranges from 1 to 80 rrrVg, pore volume ranges from 1 to 10 L/mg with median pore size from 1 to 20 d ₁₀ .

[0038] According to some embodiments, the dlatomaceous earth is any

dlatomaceous earth material that has been subjected to at least one thermal treatment In stn other embodiments, the dlatomaceous earth is any dlatomaceous earth material that has been subjected to calcination, for example, being ether non-flux calcined or flux-calcined.

[0037] According to some embodiments, the dlatomaceous earth material has not boon subjected to thermal treatment (e.g., calcination) sufficient to induce formation of greater than 1 percent Cristobalite.

[0038] As stated eerier, dtotomaceous earth is, in general, a sedimentary biogenic silica deposit including the fossilized skeletons of diatoms, one-celled algae-like plants that accumulate in marine or fresh water environments. Honeycomb silica structures generaly give dlatomaceous earth useful characterieticB such as absorptive capadty and surface area, chemical stability, and low-butt density. In some embodiments, dlatomaceous earth includes about 90 percent SiO ₂ mixed with other substances. In some embodiments, crude dlatomaceous earth includes about 90 percent SK¾, plus various metal oxides, such as, but not limited to, AI-. Fe-, Ca-, and Mg-oxides.

[0039] The at least one dlatomaceous earth may have any of various appropriate forms now known to the skied artisan or hereafter discovered. In some embodiments, the at least one dlatomaceous earth is unprocessed (e.g., K is not subjected to chemical and/or physical modification processes). Without wishing to be bound by theory, the impurities in dlatomaceous earth, such as clays and organic matters, may, in some instances, provide higher cation exchange capacity. In some embodiments, the at least one diatomacaous earth undergoes minimal processing following mining or extraction. In some embodiments, the at least one dlatomaceous earth is subjected to at least one physical modification process. Some examples of possible physical modification processes include, but are not limited to, milling, drying, and air classifying. In some embodiments, the at least one dlatomaceous earth Is subjected to at least one chemical modification process. An example of a chemical modification processes to silanization, but other chemical modification processes are contemplated. Silantzation may be used to render the surfaces of the at least one dlatomaceoua earth either more hydrophobic or hydrophlllc using the methods appropriate for silcate minerals. The dlatomaceous earth may have a typical median particle size (du) ranging from about 10 μm to about 30 urn, or from about 20 d ₁₀ to about 50 μm, may have a pore volume ranging from about 2 mL/g to about 8 mug, or from about 3 mL/g to about 5 mL/g, may have a median pore size ranging from about 1 μιτι to about 8 um, or from about from about 2 d ₁₀ to about 6 d ₁₀ , may have a surface area ranging from about 1 m ² /g to about 40 m ² /g, and/or may have a buk density ranging from about 4 lbs/ft ¹ to about 15 Ibs/ft ³ . The dlatomaceous earth may have a top particle size (dw) ranging from about 60 d ₁₀ to about 120 um, and a (d ₁₀ ) particle size from about 5 d ₁₀ to about 20 d ₁₀ .

[0040] Other minerals suitable for use hi filtration Include, for example, perflte, pumice, pumlclte, shirasu, obsidian, rice hull ash, and pftchstone. Prior to processing, perlite may be gray to green in color with abundant spherical cracks that cause ft to break into small pearl-Ike masses. Pumice Is a fcjhtweight glassy vesicular rock. Obsidian may be dark in color with a vitreous luster and a characteristic conchoidal fracture. PHchstone has a waxy resinous luster and may be brown, green, or gray. Volcanic glasses such as peritte end pumice occur in massive deposits and find wide commercial use. Volcanic ash, often referred to as "tuff when In consolidated form, Includes smal particles or fragments that may be In glassy form. Some minerals may be chemically equivalent to rhyoJite. Other natural glasses may be chemicaly equivalent to trachyte, dacfte, andeefte, iatite, and basalt The term "obsidian" Is generally applied to large numbers of natural glasses that are rich In silca. Obsidian may be classified Into subcategories according to their silica content with myelitic obsidians (containing typically about 73 percent SiO ₂ by weight) being the most common.

[0041] Perlite is a hydrated mineral that may contain, for example, about 72 to about 75 percent SiO ₂ , about 12 to about 14 percent Al ₂ O ₃ , about 0.5 to about 2 percent Fe ₂ O ₃ about 3 to about 5 percent Na ₂ O, about 4 to about 5 percent K ₂ O, about 0.4 to about 1.5 percent CaO (by weight), and small amounts of other metallic elements. Perlite may be distinguished from other minerals by a higher content (such as about 2 to about 5 percent by weight) of chemically-bonded water, the presence of a vitreous, pearly luster, and characteristic concentric or arcuate onion akin-like (I.e., perlitic) fractures.

[0042] Perlite products may be prepared by millng and thermal expansion, and may possess unique physical properties such as high porosity, low bulk density, and chemical Inertness. Average particle size for the milled expanded peritte ranges from 5 to 200 d ₁₀ , pore volume ranges from 2 to 10 L/mg with median pore size from 5 to 20 μπι, although other suitable values, set forth below, are also contemplated.

[0043] Pertite particles having a size greater than about 50 μm tend to be generaly three-dimensional, multi-angular particles. In contrast, fine perllte particles from the fine fraction of the classified product having a stze less than about 50 μm tend to be generally two-dimensional and relatively more ptaty than the larger particles. Thus, pertite particles (e.g., expanded perllte particles) having a size greater than about 50 μm may be more abrasive than particles having a smaller size. Further, smaller, platy parUdee may break down to even smaller particles more easly during, for example, a cleaning process.

[0044] According to some exemplary embodiments, perlKe, for example, commercially-available perlltes such as expanded perllte, may be milled and classified, such that the ml led and classified pertite has a top particle stze (d ₉₀ ) less than 50 urn. For example, an un-dassrfied, expanded perfte having atop particle size (d ₉₀ ) of 112 d ₁₀ , a median particle size (dm) of 60 urn, and a (d ₁₀ ) particle size of 22 d ₁₀ may be milled and/or classified according to methods known to those skilled in art to obtain periite having a top particle size (d ₅₀ ) less than 50 urn. A particle size designated "top particle size (d ₉₀ )" Is defined as the size for which 90 percent of the volume of the particles is smaller than the indicated size. A particle size designated "median particle size (d ₉₀ )" Is defined as the size for which 50 percent of the volume of the particles Is smaller than the Indicated size.

According to some exemplary embodiments, the milled and/or classified perfte (e.g., expended periite) may have a median particle size (d ₅₀ ) less than 30 urn. For example, the perfte may have a median partide size (d ₉₀ ) less than 25 d ₁₀ , such as, for example, a median particle size (d ₅₀ ) less than 20 d ₁₀ . Some embodiments have a median particle size (d ₅₀ ) ranging from 5 d ₁₀ to 25 urn, such as, for example, from 10 μm to 20 urn. In yet other examples, perllte may have a typical median particle size ( d ₅₀ ) ranging from about 20 d ₁₀ to about 70 d ₁₀ , a pore volume ranging from about from 3 mL/g to about 8 mL/g, a median pore stze ranging from about 10 d ₁₀ to about 30 d ₁₀ , a surface area ranging from about 1 m ² /g to about 10 rrrVg, a buk density ranging from about 2 lbs/ft ³ to about 6 lbs/ft ⁹ .

[0045] In some embodiments, the expanded pertite may have an aspect ratio of about 1:1 to about 1:50, about 1:2 to about 1:35, or about 1:5 to about 1:20. Aspect ratios can be calculated by the Sphericity Model from experimentally determined (using electron microscopy) surface area data as described in U.S. Pat. No. 5,846,309.

[0046] Pumice is a mineral characterized by a mesoporous structure (e.g., having pores or vesicles with a stze up to about 1 mm). The porous nature of pumice gives it a very tow apparent density, in many cases slowing It to float on the surface of water. Most commercial pumice contains from about 60 percent to about 70 percent SiO ₂ by weight Pumice may be processed by milling and classification, and pumice products may be used as lightweight aggregates and also as abrasives, adsorbente, and fillers. Unexpended pumice and thermally-expanded pumice may also be used as filtration components. Other Minerals

[0047] Other minerals that may be used in the compositions of the present disclosure include mica, talc, clay, kaolin, smectite, woHastonite, bentonite, and calcium carbonate. For example, mica is a mineral having a layered or ptaty texture. Mica may occur In Igneous, metamorphlc, and sedimentary regimes. Large crystals of mica may be typically mined from granitic pegmatites. Mica may have a median particle size ranging from, for example, about 20 μm to about 60 μm, and/or may have an aspect ratio ranging from, for example, about 1 :20 to about 1 :60.

Antimicrobial Compounds

[0048] According to some embodiments, to add antimicrobial properties to the composition, an antimicrobial metal compound (e.g., a nano-antlmlcroblal metal compound) may be precipitated and attached to the mineral surface to form an antimicrobial composition. According to some embodiments, the antimicrobial compositions may include at least one of zinc, copper, silver, and/or any other metal compounds known to those sidled In the art as having antimicrobial properties. For example, the antimicrobial metal compound may include zinc oxide, for example, a nano-sized zinc oxide fnano zinc oodde"). According to some embodiments, the antimicrobial metal compound may range from 1 percent to 30 percent by weight of the antimicrobial composition. For example, the antimicrobial metal compound may range from 1 percent to 20 percent by weight of the antimicrobial composition, from 1 percent to 10 percent by weight of the antimicrobial composition, or from 1 percent to 5 percent by weight of the antimicrobial composition. According to some embodiments, the nano-antimlcroblal particles precipitated and attached to the mineral surface may range from 1 nanometer (nm) to 250 nm.

[0049] In some embodiments of the present disclosure, a ratio of the antimicrobial metal compound to the mineral ranges from 1 :1000 to 1 :4 by weight, from 1 :100 to 1 :5 by weight, from 1:100 to 1 :10 by weight, from 1:20 to 1:5 by weight, from 1:20 to 3:20 by weight, or to in another suitable range.

[0050] The antimicrobial metal compound particles may have a particle size less than 250 nm, less than 200 nm, less than 150 nm, less than 100 nm, less than 50 nm, less than 25 nm, less than 20 nm, less than 15 nm, less than 10 nm, or less than 5 nm. Binder

[0051] The various minerals described above may be subjected to at least one co- aggtomeration with at least one binder. For example, In some embodiments, the binder Is at least one alkali silicate binder. In some embodiments, the binder Is at least one of sodium silicate and potassium slicate. In some embodiments, the binder Is at least one of alkal carbonate as the flux for high temperature calcination. In some embodiments, the binder Is at least one of sodium carbonate and potassium carbonate.

[0052] According to another embodiment, the binder may include at least one of an inorganic binder, an organic binder, or an organlc-to-inorganlc binder.

[0053] According to one embodiment, the binder can include an Inorganic binder such as an a kali silicate such as, for example, sodium sllcate, potassium slicate, and mixtures thereof. According to another embodiment, the Inorganic binder may include a cement, such as a calcium alumkiate cement In another embodiment, the inorganic binder may include a cement such as a calcium phosphate cement, a magnesium phosphate cement. In another embodiment, the inorganic binder may Include a magnesium aluminum slicate clay.

[0054] According to another embodiment, the binder can include an organlc-to- inorganic binder such as a slicone or ethyl silicate.

[0055] According to a further embodiment, the binder can include one or more organic binders or btopoiymens. For example, the binder can include a cellulose, polyethylene grycol.(PEG), polyvinyl alcohol (PVA), polyvlnylpyrroldone (PVP), starch, Candallla wax, a polyacrytate or related copolymer (e.g., acrylic acid-acrylamde , etc.), a poiydlanyldimethylamrTKXilum chloride polymer or copolymer (pDADMAC, etc.), dextrin, Ignosulfonato, sodium alginate, magnesium stearate, or mixtures thereof.

Conglomeration

[0056] Co-aglomeration of a first mineral, such as, diatomaceoue earth material and/or other filtration minerals, a second mineral, and a binder, or of heat-treated dlatomaceous earth and/or heat-treated perilte, a second mineral, and a binder (e.g., a silica binder), may occur through any appropriate agglomeration processes now known to the skilled artisan or hereafter discovered. For example, In some embodiments, co- agglomeration includes preparing at least one aqueous solution of the binder, and contacting the binder solution with a blend of the first mineral and the second mineral. One or more agglomerations may be performed, for example, when multiple binders, multiple first minerals, and/or multiple second minerals are used. [0057] In some embodiments, contacting Includes mixing the binder solution with a blend of the first and second minerals. In some embodiments, the mixing includes agitation. In some embodiments, the blend of the first mineral, the second mineral, and the binder solution is mixed sufficiently to at least substantially uniformly distribute the binder solution among the agglomeration points of contact of the first and second minerals. In some embodiments, the blend of the first and second minerals and the binder solution Is mixed with sufficient agitation to at least substantially uniformly distribute the binder solution among the agglomeration points of contact of the blend of first and second minerals without damaging the structure of the diatomaceous earth or perilte. In some embodiments, the contacting includes low-shear mbdng.

[0058] In some embodiments, mixing occurs for about one hour. In other embodiments, mbdng occurs for less than about one hour. In further embodiments, mixing occurs for about 30 minutes. In yet other embodiments, mbdng occurs for about 20 minutes. In soil further embodiments, mbdng occurs for about 10 minutes.

[0059] In some embodiments, mixing occurs at about room temperature (i.e., from about 20"C to about 23"C). In other embodiments, mbdng occurs at a temperature ranging from about 20'C to about 50"C. In further embodiments, mbdng occurs at a temperature ranging from about 30"C to about 45ºC. In still other embodiments, mbdng occurs at a temperature of from about 35ºC to about 40ºC.

[0060] According to some embodiments, contacting includes spraying the Mend of first and second minerals with at least one binder solution. In some embodiments, the spraying is Intermittent. In other embodiments, the spraying is continuous. In further embodiments, spraying Includes mbdng the blend of the first and second minerals while spraying with at least one binder solution, for example, to expose different agglomeration points of contacts to the spray. In some embodiments, such mbdng is intermttent. In other embodiments, such mbdng Is continuous.

[0061] In some embodiments, the at least one binder is present In the binder solution in an amount less than about 40 percent by weight, relative to the weight of the at least one binder solution. In some embodiments, the at least one binder ranges from about 1 percent to about 10 percent by weight. In further embodiments, the at least one Under ranges from about 1 percent to about 5 percent by weight.

[0062] The at least one aqueous solution of the at least one binder may be prepared with water. In some embodiments, the water ^' is dekxiized water. In some embodiments, the water Is ultra pure water. In further embodiments, the water has been treated to remove or decrease the levels of metals, toxins, and/or other undesirable elements before K is contacted with the at least one binder. [0063] The amount of at least one aqueous solution contacted with the blend of the first and second minerals may range from about 0.25 parts to about 1.5 parts of aqueous solution to one part blend. In some embodiments, about 1 part aqueous solution is contacted with about 1 part blend.

[0064] Before and/or after the agglomeration, the first and/or second minerals may be subjected to at least one classification step. For example, before and/or after at least one heat treatment, dlatomaceous earth may, In some embodiments, be subjected to at least one classification step. In some embodiments, the particle size of the dlatomaceous earth material and/or periite may be adjusted to a suitable or desired size using any one of several techniques well known in the art. In some embodiments, the first and/or second minerals may be subjected to at least one mechanical separation to adjust the powder size distribution. Appropriate mechanical separation techniques are well known to the skilled artisan and include, but are not limited to, mllng, grinding, screening, extrusion, triboelectric separation, liquid classification, aging, and air classification. Heat Treatment.

[0065] The first and/or second minerals and/or co-agglomerated minerals may be subjected to at least one heat treatment. Appropriate heat treatment processes are well- known to the skilled artisan and include those now known or that may hereinafter be discovered. In some embodiments, the at least one heat treatment decreases the amount of organic* and/or volatOes In the heat-treated first and/or second minerals. In some embodiments, the at least one heat treatment Includes at least one calcination. In some embodiments, the at least one heat treatment includes at leaet'one flux calcination. In some embedments, the at least one heat treatment includes at least one roasting.

[0066] Calcination may be conducted according to any appropriate process now known to the sklled artisan or hereafter discovered. In some embodiments, calcination to conducted at temperatures below the melting point of the first and/or second minerals. In some embodiments, calcination is conducted at a temperature ranging from about 600"C to about 1100 ºC. In some embodiments, the calcination temperature ranges from about 600°C to about 700'C. In some embodiments, the caJdnatJon temperature ranges from about 700"C to about 800 ºC . In some embodiments, the calcination temperature ranges from about 800ºC to about 900'C. In some embodiments, the calcination temperature la chosen from the group consisting of about 600°C, about 700°C, about BOO'C, about 900"C, about 1000ºC, and about 1100"C. Heat treatment at a lower temperature may result In an energy savings over other processes for the preparation of the first and/or second minerals.

[0067] Flux calcination includes conducting at least one calcination in the presence of at least one fluxing agent Flux calcination may be conducted according to any appropriate process now known to the skilled artisan or hereafter discovered. In some embodiments, the at least one fluxing agent is any material now known to the skilled artisan or hereafter discovered that may act as a fluxing agent In some embodiments, the at least one fluxing agent is a salt including at least one a Bui Li metal. In some embodiments, the at least one fluxing agent Is chosen from the group consisting of carbonate, sllcate, chloride, and hydroxide salts. In other embodiments, the at least one fluxing agent is chosen from the group consisting of sodium, potassium, rubidium, and cesium salts. In still further embodiments, the at least one fluxing agent Is chosen from the group consisting of sodium, potassium, rubidium, and cesium carbonate salts.

[0068] Roasting may be conducted according to any appropriate process now known to the skHled artisan or hereafter discovered. In some embodiments, roasting is a calcination process conducted at a generally lower temperature that helps to avoid formation of crystalline sllca in, for example, the dlatomaceous earth and/or perlKe. In some

embodiments, roasting is conducted at a temperature ranging from about 450"C to about 900'C. In some embodiments, the roasting temperature ranges from about 500'C to about 800 ^a C. in some embodiments, the roasting temperature ranges from about 800"C to about 700°C. In some embodiments, the roasting temperature ranges from about 700'C to about 900"C. In some embodiments, the roasting temperature is chosen from the group consisting of about 450'C, about 500 ^a C, about 600 ºC , about 700'C, about 8O0"C, and about 900'C.

[0069] According to some embodiments, the first and/or second minerals may be subjected to at least one heat treatment, folowed by co-agglomerating the heat-treated first and/or second minerals with at toast one binder.

Fltration.

[0070] Embodiments of the present disclosure include filtration devices and compositions having antimicrobial capability and methods of use thereof.

[0071] A filtration device may include a fitter element, such as a septum, and a fitter- aid material. The composite filter aid or composite material made by the processes described herein may have one or more beneficial attributes, making them desirable for use in one or a number of given applications. In some emboolments, the composite filter aids or composite materials may be useful as part of a finer aid composition. In some embodiments, a fitter aid composition may include at toast one composite material. [0072] The composite flier akto disclosed herein may have a permeablBty suitable for use In a filter aid composition. Permeablity may be measured by any appropriate measurement technique now known to the skilled artisan or hereafter discovered.

Permeabflrty is gen era By measured in darcy units or darcy, as determined by the permeability of a porous bed 1 cm high and with a 1 cm ² section through which flows a fluid with a viscosity of 1 mPa-s with a flow rate of 1 cm'/sec under an applied pressure differential of 1 atmosphere. The principles for measuring permeablity have been previously derived for porous media from Darc/s taw (see, for example, J. Bear, The [Equation of Motion of a Homogeneous Fluid: Derivations of Darc/s Law," in Dynamics of Fluids in Porous Media 161-177 (2nd ed. 1988)). An array of devices and methods are in existence that may correlate with permeability. In one exemplary method useful for measuring permeability, a specially constructed device Is designed to form a filter cake on a septum from a suspension of filtration media in water; and the time required for a specified volume of water to flow through a measured thickness of filter cake of known cross sectional area is measured.

[0073] In some embodiments, the composite material has a permeability ranging from about 0.1 darcys to about 20 darcys.ln some embodiments, the composite material has a permeablity ranging from about 0.1 darcys to 0.5 darcys. In some embodiments, the composite material has a permeability ranging from about 0.5 darcys to 2 darcys. in some embodiments, the composite material has a permeablity ranging from about 2 darcys to about 20 darcys. In some embodiments, permeabilty ranges from about 2 darcys to about 10 darcys. In some embodiments, the permeability ranges from about 2 darcys to about 5 darcys.

[0074] In some embodiments, the d ₁₀ of the composite material ranges from about 5 μm to about 30 d ₁₀ . In some embodiments, the d ₁₀ ranges from about 15 μm to about 30 d ₁₀ . In some embodiments, the d ₁₀ ranges from about 20 d ₁₀ to about 30 d ₁₀ . In some embodiments, the d _B of the composite material ranges from about 10 d ₁₀ to about 70 um. In some embodiments, the d ₅₀ ranges from about 20 um to about 50 d ₁₀ . In some

embodiments, the d ₅₀ ranges from about 50 um to about 70 d ₁₀ . In some embodiments, the d ₅₀ ranges from about 60 d ₁₀ to about 70 d ₁₀ . In some embodiments, the d ₉₀ of the composite material ranges from about 60 d ₁₀ to about 120 um. In some embodiments, the dn ranges from about 90 d ₁₀ to about 120 d ₁₀ . in some embodiments, the d ₉₀ ranges from about 100 d ₁₀ to about 120 d ₁₀ . In some embodiments, the d ₉₀ ranges from about 110 d ₁₀ to about 120 d ₁₀ .

[0075] The composite materials disclosed herein may have a low crystalline silica content Forms of crystalline silica include, but are not limited to, quartz, cristobalte, and tridymite. In some embodiments, the composite material has a lower content of at least one crystalline silica than a composite material not subjected to at least one co-agglomeration wfth at least one silica binder.

[0076] The composite materials disclosed herein may have a low cristobalite content Cristobalite content may be measured by any appropriate measurement technique now known to the skilied artisan or hereafter discovered. In one exemplary method, cristobalite content is measured by X-ray diffraction. Cristobalite content may be measured, for example, by the quantitative X-ray diffraction method outlined In H. P. Klug and L. E. Alexander, X-Ray Diffraction Procedures for Polycrystalllne and Amorphous Materials 531- 563 (2nd ed. 1972). According to one example of that method, a sample is milled in a mortar end pestle to a fine powder, then back-loaded into a sample holder. The sample and Its holder are placed into the beam path of an X-ray diffraction system and exposed to colllmated X-rays using an accelerating voltage of 40 kV and a current of 20 mA focused on a copper target Diffraction data are acquired by step-ecannlng over the angular region representing the Interplanar spacing within the crystalline lattice structure of cristobalite, yielding the greatest diffracted Intensity. That region ranges from 21 to 2326 (2-theta), with data colected in 0.0526 steps, counted for 20 seconds per step. The net integrated peak intensity Is compared with those of standards of cristobaRte prepared by the standard additions method In amorphous slica to determine the weight percent of the cristobalite phase In a sample.

[0077] In some embodiments, the cristobalite content is less than about 20 percent by weight, less than about 10 percent by weight, less than about 6 percent by weight, or less than about 1 percent by weight. In some embodiments, the composite material has a lower cristobalite content than materials not subjected to co-agglomeration wNh, for example, a perlte and/or a second mineral, and at least one binder (e.g., at least one silica binder).

[0078] Composite materials disclosed herein may have a low quartz content Quartz content may be measured by any appropriate measurement technique now known to the sklled artisan or hereafter discovered. In one exemplary method, quartz content is measured by x-ray diffraction. For example, quartz content may be measured by the same x- ray diffraction method described above for cristobalte content, except the that 26 region ranges from 26.0 to 27.5 degrees. In some embodiments, the quartz content is less than about 0.5 percent by weight, less than about 0.25 percent by weight less than about 0.1 percent by weight, or to about 0 percent by weight. In some embodiments, the quartz content ranges from about 0 percent to about 0.5 percent by weight. In some embodiments, the quartz content ranges from about 0 percent to about 0.25 percent by weight [0079] Composite materials disclosed herein may have a measurable pore volume. Pore volume may be measured by any appropriate measurement technique now known to the skilled artisan or hereafter discovered. In one exemplary method, pore volume is measured with an AutoPore IV Θ50Ό series mercury porosimeterfrom MlcromeritJcs Instrument Corporation (Norcross, Georgia, USA), which can determine measure pore diameters ranging from 0.006 to 600 urn. As used to measure the pore volume of the composite materials disclosed herein, that porosimeter's contact angle was set at 130 degrees, and the pressure ranged from 0 to 33,000 pel. In some embodiments, the pore volume is about equal to at least one diatomaceous earth, pertte, and/or second mineral, from which it is made. In some embodiments, the pore volume ranges from about 1 mUg to about 10 mL/g, from about 4 mL/g to about 8 mUg, from about 5 mL/g to about 7 mL/g, or Is about 6 mL/g.

[0080] Composite materials disclosed herein may have a measurable median pore diameter. Median pore diameter may be measured by any appropriate measurement technique now known to the skilled artisan or hereafter discovered. In one exemplary method, median pore diameter b measured wtth an AutoPore IV 9500 series mercury porosimeter, as described above. In some embodiments, the median pore diameter ranges from about 1 μm to about 40 d ₁₀ . In some embodiments, the median pore diameter ranges from about 1 μm to about 8 urn. In some embodiments, the median pore diameter ranges from about 15 um to about 30 μm. In some embodiments, the median pore diameter ranges from about 20 um to about 30 d ₁₀ .

[0081] Composite materials disclosed herein may have a measurable wet density, which as used herein refers to measurement of centrtfuged wet density. According to one exemplary method, to measure wet densky, a composite material sample of known weight from about 1.00 to about 2.00 g is placed in a calibrated 15 ml centrifuge tube to which dekxitzed water is added to make up a volume of approximately 10 ml. The mixture is shaken thoroughly untfl all of the sample is wetted, and no powder remains. Additional dekxitzed water is added around the top of the centrifuge tube to rinse down any mixture adhering to the side of the tube from shaking. The tube is centrifuged for 5 minutes at 2500 rpm on an IEC CentraO MP-4R centrifuge, equipped with a Model 221 swinging bucket rotor (International Equipment Company; Needham Heights, Massachusetts, USA). Following oentrifugation, the tube is carefully removed without disturbing the solids, and the level (i.e., volume) of the settled matter Is measured in cm*. The centrifuged wet density of powder is readily calculated by dividing the sample weight by the measured volume. In some embodiments, the wet density ranges from about 10 lbs/ft ³ to about 22 lbs/ft ³ . In some embodiments, the wet density ranges from about 10 lbs/ft ⁹ to about 16 lbs/ft ⁹ , or from about 12 lbs/ft ³ to about 19 lbs/ft ¹ . In some embodiments, the filter aid has a bulk density ranging from about 7 lb/ft ³ to about 14 lb/ft ³ .

[0082] Composite materials disclosed herein may include at least one soluble metal. As used herein, the term "soluble metal" refers to any metal that may be dissolved In at least one Rquld. Soluble metals are known to those of skill in the art and Include, but are not limited to, Iron, aluminum, calcium, vanadium, chromium, copper, zinc, nickel, cadmium, and mercury. When a filter aid Including a composite material is used to filter at least one liquid, at least one soluble metal may dissociate from the composite material filter aid and enter the liquid. In many appflcatJons, such an increase In metal content of the liquid may be undesirable and/or unacceptable. For example, when a filter aid including a composite material is used to filter beer, a high level of iron dissolved in the beer from the filter aid may adversely affect sensory or other properties, including but not limited to taste and shelf-life.

[0083] Any appropriate protocol or test for measuring levels of at least one soluble metal in composite materials may be used, including those now known to the skilled artisan or hereafter discovered. For example, the brewing Industry has developed at least one protocol to measure the beer soluble iron (BSI) of composite material filter aids. BSI refers to the iron content, which may be measured in parts per million, of a filter aid Including a material that dissociates in the presence of a liquid, such as beer, as measured, for example, by the American Society of Brewing Chemists (ASBC). For example, the fitter aid may have a BSI content of less than 5 ppm, or less than 1 ppm, as measured by ASBC. In the United States, ASBC has set forth a method to measure the BSI content in parts per milion, wherein a sample of, e.g., BUDWEISER® beer Is contacted wfth the filter aid and the resulting Iron content in the beer Is measured.

[0084] In the ASBC method, for example; BSI content may be measured by placing a 5 g earn pie of diatom ite in 200 mL of decarbonated beer (for example, BUDWEISER®) at room temperature, and the mixture to swirled Intermittently for an elapsed time of 5 minutes and SO seconds. The mixture Is then immediately transferred to a funnel containing 25 cm diameter filter paper, from which the filtrate collected during the first 30 seconds to discarded. Filtrate is collected for the next 150 seconds, and a 25 mL portion Is treated with approximately 25 mg of ascorbic add (i.e., C8H806) to reduce dissolved Iron lone to the ferrous (I.e., Fe2+) state (thus yielding a "sample extract")- The color is developed by addition of 1 mL of 0.3 percent (w/v) 1 ,10-phenanthroline, and after 30 minutes, the absorbance of the resulting sample solution to compared to a standard calibration curve. The caJbratJon curve is prepared from standard iron solutions of known concentration In beer. Untreated filtrate is used as a method blank to correct for turbidity and color. Absorbance is measured at 505 nm using a spectrophotometer. [0085] In some embodiments, the beer soluble Iron of the composite material disclosed herein ranges from less about 1 ppm to about 5 ppm, when measured using an ASBC method. In some embodiments, the beer soluble Iron ranges from about 1 ppm to about 4 ppm, from about 1 pd ₁₀ to about 2 pd ₁₀ , or Is less than about 1 pd ₁₀ when measured using an ASBC method.

[0086] The European Beverage Convention (EBC) method for determining the beer soluble iron content contacts Squid potassium hydrogen phthalate wfth the finer aid and then analyzes the liquid fdor iron content. More specMlcaly, the EBC method uses, for example, a 10 g/L solution of potassium hydrogen phthalate (KHP, KHC8H404) as the extracts nt along with a given quantity of fitter aid material, with a total contact time of two hours. Extracts are then analyzed for iron concentration by the FERROZINE method.

[0087] In some embodiments, the beer soluble Iron of composite material ranges from about 100 pd ₁₀ to about 150 pd ₁₀ , from about 100 pd ₁₀ to about 120 pd ₁₀ from about 110 pd ₁₀ to about 120 pd ₁₀ , about 20 pd ₁₀ , about 80 pd ₁₀ , or less than about 150 pd ₁₀ , less than about 100 pd ₁₀ , less than about 80 pd ₁₀ , when measured using an EBC method.

[0088] The composite materials disclosed herein may have a measurable BET surface area. BET surface area, as used herein, refers to the technique for calculating specific surface area of physical absorption molecules according to Brunauer, Emmett, and Teller ("BET) theory. BET surface area may be measured by any appropriate measurement technique now known to the ski led artisan or hereafter discovered. In one exemplary method, BET surface area Is measured with a Gemini III 2375 Surface Area Analyzer, using pure nitrogen as the sorbent gas, from Micromertics Instrument Corporation (Norcross, Georgia, USA). In some embodiments, the BET surface area is greater than for a material not produced according to embodiments described herein (e.g., without co-agglomerating diatomaceous earth and perlit with at least one si lea binder). In some embodiments, the BET surface area ranges from about 1 m ² /g to about 50 rrrVg, from about 5 rrrVg to about 50 m2/g, or is greater than about 10 m2/g.

[0089] The exemplary composite materials disclosed herein may be used in any of a variety of processes, applications, and materials. For example, the composite materials may be used In at least one process, application, or material in which such a product with a high BET surface area is desirable.

[0090] The composite materials may be incorporated into a filter aid material or composition. A filter aid composition Including at least one composite material may optionally include at least one additional fitter aid medium. Examples of suitable additional filter aid media In elude, but are not limited to, natural or synthetic silicate or aluminosilicate materials, unimproved diatomaceous earth, saltwater diatomaceous earth, expanded perfite, pumicite, celuloee, rice hull aeh, activated charcoal, feldspars, nephelne syenite, sepiolite, zeolite, mica, talk, clay, kaolin, smectite, wolastonite, and combinations thereof.

[0091] The at least one additional filter medium may be present in any appropriate amount. For example, the at least one additional filter medium may be present from about 0.01 to about 100 parts of at least one additional filter medium per part of the composite material. In some embodiments, the at least one additional filter medium Is present from about 0.1 to about 10 parts. In some embodiments, the at least one additional fitter medium is present from about 0.5 to 5 parts.

[0092] The filter aid composition may be formed Into sheets, pads, cartridges, or other monolithic or aggregate media capable of being used as supports or substrates in a filter process. Considerations In the manufacture of fitter aid compositions may Include a variety of parameters, including but not limited to total soluble metal content of the composition, median soluble metal content of the composition, particle size distribution, pore size, cost, and availability.

[0093] A filter aid composition including at least one composts material with antimicrobial capability may be used In a variety of processes and compositions. In some embodiments, the fitter aid composition is applied to a filter septum to protect It and/or to improve clarity of the liquid to be filtered in a filtration process. In some embodiments, the flner aid composition is added dferectry to a beverage to be filtered to increase flow rate and/or extend the filtration cycle. In some embodiments, the filter aid composition Is used as pre-coatJng, in body feeding, or a combination of both pre-coatJng and body feeding, in a nitration process.

[0094] Embodknents of the composite material may also be used In a variety of filtering methods. In some embodiments, the fitering method includes pre-coatJng at least one fitter element with at least one composite material, and contacting at least one liquid to be fittered with the at least one coated fitter element. In such embodiments, the contacting may Include passing the liquid through the fitter element In some embodiments, the filtering method includes suspending at least one composite material filter aid in at least one liquid containing particles to be removed from the liquid, and thereafter separating the filter aid from the filered squid.

[0095] FRter aids including at least one composite material disclosed herein may also be employed to fitter various types of liquids. The ski led artisan is readily aware of liquids that may be desirably fittered with a process including the fitter aids including at least composite material disclosed herein. In some embodiments, the liquid Is a beverage.

(Exemplary beverages include, but are not limited to, vegetable-based juices, fruit juices, distilled spirits, and malt-based RqukJs. [Exemplary matt-based liquids include, but are not limited to, beer and wine. In some embodiments, the liquid is one that tends to form haze upon chilling. In some embodiments, the liquid is a beverage that tends to form haze upon ending. In some embodiments, the Iquid is a beer. In some embodiments, the liquid is an oil _? In some embodiments, the Iquid Is an edible oil. In some embodiments, the liquid Is a fuel oil. In some embodiments, the liquid Is water, inducing but not limited to waste water. In some embodiments, the liquid Is blood. In some embodiments, the liquid is a sake. In some embodiments, the liquid is a sweetener, such as, for example, com syrup or molasses.

[0096] The filtering method may remove or substantially eliminate bacteria from the filtered liquid. The method may remove or substantially eliminate bacteria from genera including, but not limited to, Pedtoooccus, Lactobacillus, Acatobacter, and Oanococcua. These bacteria are known to produce acetic acid from sugar, and for some species, even biogenic amines from free amino acids. It Is also contemplated that the methods and devices of the present disclosure may remove or substantJaBy eiminate other types of bacteria from the ffltered liquids.

Otrwr Applications

[0097] The antimicrobial composite materials disclosed herein may also be used In applications other than filtration. In some embodiments, the composite materials may be used as composites In filler applications, such as, for example, fliers in construction or buMing materials. In some embodiments, the composite materials may be used to alter the appearance and/or properties of paints, enamels, lacquers, or related coatings and finishes. In some embodiments, the composite materials may be used in paper formulations and/or paper processing applications. In some embodiments, the composite materials may be used to provide anti-block and/or reinforcing properties to polymere. In some embodiments, the composite materials may be used as or In abrasives. In some embodiments, the composite materials may be used for buffing or tn buffing compositions. In some embodiments, the composite materials may be used for polishing or in polishing compositions. In some embodiments, the composite materials may be used in the processing and/or preparation of catalysts. In some embodiments, the composite materials may be used as chromatographic supports or other support media. In some embodiments, the composite materials may be blended, mixed, or otherwise combined with other Ingredients to make monolithic or aggregate media useful tn a variety of applcatJons, including but not limited to supports (e.g., for microbe immobilization) and substrates (e.g., for enzyme krvnobillzatlon). Cleansing and Cosmetic Uses

[0098] The mtneralB described above, such as, e.g., diatomaceoue earth, talc, wollastonlte, kaolin, bentonHe, mica, and perllte may be incorporated In a variety of com position 8. In some embodiments, the composition is a personal care composition, for example, a personal care cleansing composition. In some embodiments, the composition is a cosmetic. In other embodiments, the composition is a cleaning composition other than a personal care cleaning composition, for example, a household cleaning product (e.g., surface cleaner).

[0099] In one embodiment, the mineral may include perlite microspheres having antimicrobial capability and/or a modified visual appearance, for example, an enhanced visual appearance may be utilized. It is also contemplated the microspheres Including other minerals may be used. Antimicrobial pertte microspheres having a modified visual appearance may be utilized to enhance the appearance and, thus, enhance user-appeal of the composition. Thus, the perllte microspheres may be used as visually enhanced exfoliating component in personal care, cosmetic or cleaning compositions owing, at least In part, to Its advantageous scrub-feel properties and enhanced visual appearance.

[0100] In some embodiments, the compositions further comprise a cosmetically acceptable base.

[0101] In some embodiments, the composition Is a personal care cleansing composition, for example, a gel, for example, a shower gel, optionally wherein the perlite microspheres provide a scrub feel, skin exfolation, or both. In some embodiments, the personal care cleansing composition is a hair shampoo, for example, an anti-dandruff shampoo, optionaty wherein the perlite microspheres aid or provide exfoliation of the skin of the scalp.

[0102] In some embodiments, the amount of mineral present in the composition, for example, personal care composition (e.g., personal care cleaning composition), cosmetic or cleaning composition is an arrrauntof from about 0.1 percent to about 40 percent, based on the total weight of the personal care cleansing composition, for example, from about 0.1 percent to about 30 percent, or from about 0.1 percent to about 20 percent, or from about 0.1 percent to about 15 percent, or from about 0.1 percent to about 10 percent, or from about 0.1 percent to about 9.0 percent, or from about 0.2 percent to about 8.0 percent, or from about 0.3 percent to about 7.0 percent, or from about 0.4 percent to about 6.0 percent, or from about 0.5 percent to about 5.0 percent, or from about 0.5 percent to about 4.0 percent, or from about 0.5 percent to about 3.0 percent, or from about 0.5 percent to about 2.0 percent, or from about 0.75 percent to about 5.0 percent, or from about 0.75 percent to about 3.0 percent, or from about 0.75 percent to about 2.5 percent, or from about 1 percent about 3.0 percent, or from about 1.5 percent to about 5.0 percent or from about 2.0 percent to about 10 percent or from about 2.0 percent to about 5.0 percent or from about 2.5 percent to about 5 percent, or from about 3.0 percent to about 10 percent or from about 3.0 percent to about 8 percent

[0103] The cosmetically acceptable base may be in the form a liquid, gel, emulsion, lotion or paste. In some embodiments, the base Is a gel, whle in others, base is a liquid. In some embodiments, the cosmetically acceptable base comprises or constitutes the components of the composition other than the mineral.

[0104] Thus, the personal care, cosmetic or cleaning composition may contain one or more additional components suitable for the intended use.

[0105] For example, in some embodiments, the personal care, cosmetic or cleaning composition comprises one or more surfactants. The one or more surfactants may constitute the detergent base of a gel. The one or more surfactants may be selected from zwrtterionlc, anionic, non-Ionic and amphoteric surfactants, and mixtures thereof.

[0106] In some embodiments, the surfactants) are present In a total amount ranging from about 1 percent to about 60 percent, based on the total weight of the composition, for example, from about 5 percent to about 50 percent or from about 5 percent to about 30 percent The skilled person will be able to select suitable amounts of surfactant for

Incorporation in the base, based on the amount of surfactant in the final composition and Its Intended use

[0107] In some embodiments in which the personal care cleansing composition is a hair shampoo, the hair shampoo comprises one or more of sodium laureth sulfate, sodium C14-16 olefin sulfonate, sodium lauryl sulfoacetate, sodium cocoyl isethionate, sodium methyl cocoyl taurate, cocoamidopropyl betaine, cocoamide MEA, and mixtures thereof.

[0108] In some embodiments in which the hair shampoo is an anti-dandruff shampoo, the shampoo additJonaly comprises one or more additives, i.e., chemicals, for treating dandruff. In some embodiments, the additive for treating dandruff, I.e., anti-dandruff chemical is one or more of zinc pyrithone, a corticosteroid, an imidazole antifungal agent such as, for example, ketoconazole, selenium sulfide, and a hydoxypirldone such as, for example, ciclopirox. In some embodiments, the anti-dandruff chemical comprises or is zinc pyrithone. In some embodiments, the anti-dandruff chemical comprises or is ketoconazole. The anti-dandruff chemical may be used in a suitable, e.g., effective, amount. Suitable amounts may range from about 0.1 percent to about 5 percent, based on the total weight of the hair shampoo, for example, from about 0.1 percent to about 3 percent or from about 0.1 percent to about 2 percent. The sklled person will be able to select suitable amounts of artti- dandruff chem!cal(8) for Incorporation in the base, baaed on the amount of anti-dandruff chemlcaKs) in the final composition.

[0109] In some embodiments, the shampoo comprises conditioning (anti-static) surfactants to soothe the scalp after washing with the anti-dandruff shampoo. (Exemplary conditioning surfactants are riydraxyprcpyltriironium chloride and pofygrycerol laurate.

[0110] The personal care or cosmetic composition may contain other components conventionally found in cosmetic applications for skin and hair, including, without limitation, skin oonditioning/rnoiaturlzing agents, haJrconditfoning/moiaturizing agents perfumes, fragrances, opacfflers, peariesdng agents, colorings, preservatives, chelating agents, humectants, herb and/or plant extracts, essential oils, proteins, phi adjusting agents, and antimicrobials. The total amount of other components may be present In amount of from about 0.1 to about 30 percent based on the total weight of the personal care cleansing composition, for example, from about 0.1 percent to about 20 percent, or from about 0.1 percent to about 15 percent, or from about 0.5 percent to about 10 percent, or from about 1 percent to about 10 percent, or from about 1 percent about 5 percent. The skilled person will be able to select suitable amounts of each component for Incorporation In the base, based on the amount of the component in the final composition.

[0111] The term "cleaning composition," as used herein to refer to a household product, means a composition which Is compatible with hard surfaces and/or tableware. In some embodiments, the cleaning composition is a hard surface cleansing composition or tableware cleansing composition. It is an advantage of the compositions according to the present disclosure that they may be used to dean/cleanse inanimate surfaces made of a variety of materials lice glazed and non-glazed ceramic tiles, enamel, stainless steel, ΙηοχΦ, Formica®, vinyl, no-wax vinyl, linoleum, melamine, glass, plastics, Teflon®, painted surfaces and the Ike.

[0112] The term "hard surface clean sing composition" or tableware cleansing composition" as used herein means a composition comprising a sold (e.g., a powder), or a liquid, such as a gel of water and bases (e.g., RqukJ soap). Liquid compositions include com positions having a water-Ike viscosity as well as thickened compositions, such as gels and pastes.

[0113] The compositions in accordance wfth certain embodiments of the present disclosure may be made by conventional methods of preparing personal care cleansing compositions, e.g., shower gels or anti-dandruff shampoos.

[0114] As used herein, the term "cosmetic composition" means a composition intended to be applied to the human body for beautifying, promoting attractiveness, or altering the appearance without affecting the body's structure or functions. In some embodiments, the cosmetic composition Is a decorative cosmetic. Cosmetics include concealers, foundations, and powders requiring high or full coverage and homogeneity, including corrective and camouflage products.

[0115] In some embodiments, the cosmetic composition is a powder (e.g., pressed or loose), a liquid, a gel, a cream (e.g., a cream emulsion), a dispersion or an anhydrous stick. In some embodiments, the cosmetic composition is a powder, for example, a pressed powder such as, but not Imited to, a powdered cosmetic compact In some embodiments, the cosmetic composition is a makeup, for example, a face makeup including, but not Imited to, primer, concealer, foundation, blush (also known as rouge or blusher), bronzer, eye shadow, mascara, lipstick, contour powder, face powder (often used to set a foundation), highlighter, eyeliner, or eyebrow applicator (e.g., pencil). Loose powders include body powder, for example, baby powder.

[0116] In some embodiments, the cosmetic composHon comprises from about 1 percent by weight to about 96 percent by weight of mineral (I.e., based on the total weight of the cosmetic composition) for example, from about 20 percent to about 90 percent by weight, or from about 30 percent to about 90 percent by weight, or from about 40 percent to about 90 percent by weight, or from about 50 percent to about 90 percent by weight, or from about 60 percent to about 90 percent by weight, or from about 65 percent to about 85 percent by weight, or from about 70 percent to about 85 percent by weight, or from about 75 percent to about 85 percent by weight, or up to about 95 percent by weight, or up to about 90 percent by weight, or up to about 85 percent by weight, or up to about 80 percent by weight.

[0117] In some embodiments, the cosmetic composition comprises colorant and/or binder and/or cosmetically acceptable base in addition to the mineral. In some embodiments, the binder, when present, may be a constituent of the cosmetically acceptable base. In some embodiments, the cosmetic composition comprises colorant and binder, in addition to the mineral.

[0118] When present, the cosmetically acceptable base may be any base suitable for the intended purpose. In some embodiments, the base Is an oil and/or wax containing material. The base and, thus, the cosmetic composition, may comprise other components such as humectants, preservative, emoiient, fragrance and antioxidant Sunscreen

[0119] According to some other embodiments, an antimicrobial composition may also be incorporated into sunscreens or other personal care products in order to provide protection from ultraviolet radiation. In one embodiment, the sunscreen can be in a form such as lotions, sprays, gels or other topical products that absorb or reflect some of the sun's ultraviolet (UV) radation on the skin exposed to sun light and thus help protect against sunburn.

[0120] The sunscreen may include a mineral selected from one of diatomaceous earth, talc, wotastonlte, kaolin, bentonlte, mica, and partite. The sunscreen also may Include an antimicrobial compound such as, e.g., zinc oxide or titanium dioxide associated with the mineral. The antimicrobial compound also may act as a mechanical sun blocker and as a UV-fltsr In the sunscreen composition.

[0121] In some embodiments, the ratio of the zinc oxide to the mineral Is at least 1 :1 by weight. In other embodiments, the ratio of the zinc oxide to the mineral ranges from 1:1 to 9:1 by weight, ranges from 1 :1 to 4:1 by weight, ranges from 3:2 to 4:1 by weight, ranges from 3:2 to 3:1 by weight, or Is In another suitable range.

[0122] In some embodiments, the sunscreen composition may further comprise one or more components selected from the group of emollients, emulsifiers, hydrants, thickeners and/or surfactants, and may be present in the form of a cream, or an ointment, or a lotion, or in a sprayable form. Such compositions have been found to have Improved organoleptic properties while maintaining good SPF.

[0123] According to one embodiment, the mineral of the sunscreen composition is talc with a BET surface area of at least about 10 m ² /g, such as for example, at least about 15 m ^z /g, or at least about 20 m ² /g.

[0124] As used herein, the term "delaminated talc" refers to a talc prepared according to a process for treating lamella-type minerals. Lamellar type minerals have a structure consisting of stacks of elementary leaves. During delamlnatlon they are treated to obtain a powder with high lamella rity.

[0125] As used herein, the lamella lamelarity index" characterizes the shape of the particle, and more particularty Its aspect ratio (targe cflmension / thickness). In all the following, this lamellarity Index will be measured by the difference between, on the one hand, the value of the mean dimension of the particles of the powder obtained by a particle size measurement by Malvern laser diffraction D50 las using a wet method (standard AFNOR NFX11-666) and on the other hand, the value of the mean diameter D50 sed obtained by a measurement by sedimentation using a "Sedkjraph" (standard AFNOR XII-683), this difference being related to the mean diameter D50. Reference may be made to the article «G. BAUDET and J. P. ROMA, Ind. Mki. Mines et Carr. Lee techn. June, July 1990, pp 55-61» which shows that this index is correlated to the mean ratio of the largest dimension of the particle to its smallest dimension. [0126] As used herein, "high lamellarity" Is understood to mean a powder of which the lameliarity index is high and in particular greater than 2.8. According to one embodiment, the talc used herein can have a lamellartty Index of at least about 3.0, such as for example at least about 3.5, or at least about 4.0.

[0127] As used herein, "SPF Is the Sun Protection Factor, determined by in vitro measurements based on transmfttance according to forthcoming ISO 24445 (pre-lrredlation and spectrophotometer).

[0128] The present disclosure provides sun care compositions having Improved organoleptic characteristics. Talc powders can be employed to complement, or extend, or partially or entirety replace mineral or organic UV fitters in order to improve organoleptic characteristics whle maintaining a good SPF value. Some talc grades may Improve the SPF and organoleptic characteristics of sun cream, providing that the talc Is either de laminated, or the talc has a BEET surface area of at least about 10 rrrVg, or the talc Is uncoated, or a combination of these properties.

[0129] Talc In itself does not absorb UV radiation and cannot be considered as a mineral UV filter in its own right Nevertheless, It has been found, for example, that certain talcs (e.g. detaminated talcs), in combination with UV organic filters, maintain Sun Protection Factor (SPF) high even in the absence of a UV mineral filter such as ΊΊ02. Without wanting to be bound by theory, It is thought that some of these unexpected good results might be due to some talc grades acting as extenders for organic UV fitters. In fact, the lipophilic surfaces of talc might absorb or ink to some chemical groups of organic UV filters. This may cause a better dispersion of the filters and finally a better UV protection in a sun care composition.

[0130] The obtained compositions may have an SPF of 6 or more, such as for example 15 or more, 30 or more or 50 or more. According to other embodiments, the sun care composition SPF can for example range from 6 to 70, from 10 to 50, or from 15 to 50. The use of talc in sunscreen may improve organoleptic characteristics thereof. The organoleptic characteristics concern the visual appearance and tactile sensation of a composition when applied to the human skin, such as for example ease of application (applicability), sensation on touching the skin, for example consistency, softness or stickiness, and the appearance of streaking as unwanted white fines on the skin after application.

Toothpaste

[0131] Dentrifice compositions for cleaning teeth may include any of the minerals set forth above, such as, e.g.; diatomaceous earth, talc, woUastonite, kaolin, bentonite, calcium carbonate, and mica with the exemplary particle size characteristics aat forth above, and may result in compositions that effectively dean teeth without adversely Increasing the abrasiveness of the composition. Without wishing to be bound by theory, It Is believed that thJe may result from the relatively smafcsr mineral particles having a relatively piety characteristic that Increases the area of contact wrth the tooth relative to the point-Ike contact of the three-dimensional and angular nature of relatively larger mineral particles. Further, and without wishing to be bound by theory, K Is beloved that addition of an antimicrobial metal compound (e.g., coating the mineral with antimicrobial metal compound) may result in providing an agent for reducing or klllng germs and/or bacteria associated with oral hygiene (e.g., Streptococcus mutans).

[0132] The minerals may be associated wrth an antimicrobial metal compound as set forth above. When used In dentrtflce compositions, e.g., toothpaste, antimicrobial compositions may reduce bacteria associated wtth oral hygiene.

[0133] Exemplary embodiments of antimicrobial compositions (e.g., btoddaJ abrasive compositions) include minerals and exhibit a relative dentin abrasion (RDA) value less than 220. RDA testing is a method of measuring of the erosive effect on tooth dentin of abrasives in compositions for cleaning teeth, and RDA value is standardized in accordance with DIM/ISO standard 11609, a standard that has been adopted by the American Dental Association (ADA). Higher RDA values Indicate higher levels of abrasiveness. For example, some embodiments of antimicrobial compositions include one or more minerals and exhibit an RDA value less than 200, for example, less than 180.

[001] Some exemplary embodiments of antimicrobial compositions include one or more minerals and exhibit a PCR value of at least 110. For example, some embodiments include one or more minerals and exhbit a PCR value of at least 120.

[002] The PCR value is an indication of the abilty of Dentifrices to remove stained pelicle (i-e., an Indication of the cleaning ability of dentifrice formulations). Previous studies (J. Dent Res., 61:1236, 1982) have indicated that the results of this test with dentifrice slurries compare favorably with those obtained in controlled clinical trials. Thus, the results of this test using dentifrice slurries may be considered to predict clinical findings with a reasonable degree of confidence.

[0134] Some embodiments of antimicrobial compositions are dentifrice compositions. According to some embodiments, the dentifrice composition is toothpaste, in particular, a dentifrice composition Including a toothpaste base. For example, the toothpaste base may include at least one Ingredient chosen from binders, such as thickening agents and/or gelling agents, humectants, foaming agents such as detergents, and polishing agents. The toothpaste base may also contain at least one additional ingredient chosen from, for example, water, preservative agents, flavoring agents, sweeteners, and fluoride containing compounds. It will be readly apparent to the sidled ardsan that the components and their relative amounts in the toothpaste base may be modified to achieve the desired toothpaste product

[0135] The toothpaste base according to some embodiments may contain at least one binder, such as thickeners, which may also be referred to as geRIng agents. Any art- recognized gelling or thickening agent may be used. Thickening or geling agents may be selected from natural, synthetic, and gum-Ike materials, Including, but not limited to, carboxyl methyl cellulose, carrageenan, xantham gum, and bentontte. The at least one thickening or geling agent may be present in the toothpaste base in an amount ranging from, for example, about 0.1 percent to about 5 percent by weight, for example, from about 0.1 percent to about 3 percent by weight According to some embodiments, the at least one thickening or gelling agent is present in the toothpaste base in an amount ranging from, for example, about 0.5 percent to about 1.5 percent by weight

[0136] According to some embodiments, the toothpaste base may also contain at least one ingredient chosen from detergents and surfactants. Suitable non-limiting examples of appropriate detergents for use In the toothpaste base include anionic surfactants, such as sodium alkylsulfates, sodium laurytsulfate, sodium myristytsultate and surfosucclnic acid surfactants; dialkyl sodium suifbeucclnato; non-ankxiic surfactants; and amphoteric surfactants. The at least one ingredient chosen from detergents and surfactants may be present in the toothpaste base in an amount ranging from, for example, about 0.1 percent to about 10 percent by weight, for example, from about 0.1 percent to about 5 percent by weight, and further, for example, from about 0.5 percent to about 3 percent by weight

[0137] According to some embodiments, the toothpaste base may also contain at least one humectant such as, for example, humectants chosen from glycerin, sorbitol, propylene glycols, polyethylene glycols, and mixtures thereof. The at least one humectant may be present In the toothpaste base In an amount ranging from, for example, about 10 percent to about 90 percent by weight, for example, from about 20 percent to about 80 percent by weight. According to some embodiments, the at least one humectant may be present in an amount ranging from about 30 percent to about 70 percent by weight

[0138] Some embodiments of toothpaste base may contain at least one coloring or whitening agent Any art-recognized coloring or whitening agent may be used. Coloring and whitening agents may include, for example, titanium dioxide. Coloring or whitening agents may be present In the toothpaste base in an amount ranging from about 0.1 percent to about 5 percent by weight, for example, ranging from about 0.1 percent to about 3 percent by weight, or, for example, ranging from about 0.1 percent to about 1 percent by weight. [0139] The toothpaste base according to some embodiments may contain at least one preservative. Any art-recognized preservative may be used. For example, preservatives may be selected from sodium benzoate and methyl paraben. Preservatives may be present in the toothpaste base in an amount ranging from, for example, about 0.1 percent to about 3 percent, by weight, for example, ranging from about 0.1 percent to about 1 percent by weight and further, for example, from about 0.1 percent to about 0.5 percent by weight The toothpaste base may further contain at least one additional Ingredient chosen from therapeutic Ingredients and preventatives such as water-Insoluble non-catlonic antibacterial agents, for example, tricloean, and cation ic antibacterial agents.

[0140] The toothpaste base may also contain at least one foaming agent. Any art-recognized foaming agent may be used, and appropriate foaming agents will be readily apparent to the sidled artisan. Further, the toothpaste base may contain at least one flavoring agent. Any art-recognized flavoring agent may be used, and appropriate flavoring agents will be readily apparent to the skilled artisan. For example, flavoring agents may be chosen from oils of spearmint, peppermint, wintergreen, sassafras, dove, sage, eucalyptus, cinnamon, lemon, orange, and methyl saicylate.

[0141] The toothpaste base may contain at least one sweetener. Any art-recognized sweetener may be used, and appropriate sweeteners wfll be readily apparent to the sidled artisan. For example, sweeteners may be chosen from at least one of sucrose, lactose, maltose, xylitol, sodium cyciamate, perillartlne, aspartyl phenyl alanine methyl ester, and saccharine.

[0142] The toothpaste base may contain fluoride, such as, any compatible composition that will dissociate and release fluorine-containing ions in water. Fluoride compositions may be chosen from one or more of sodium fluoride, stannous fluoride, sodium rncnofluorophoephate, potassium fluoride, potassium stannous fluoride, sodium

fhjorostannate, stannous chlofoftuortde, and amine fluoride. Fluorides may be present in the toothpaste base in an amount ranging from about, for example, 0.1 percent to about 3 percent, by weight for example, from about 0.1 percent to about 1 percent by weight, and further, for example, from about 0.2 percent to about 0.8 percent by weight

[0143] Compositions (e.g., biockJal abrasive compositions) according to some embodiments may also include abrasive materials chosen from any fluoride compatible abrasive material. Suitable non-limUng examples of abrasive materials that may be used may be chosen from, for example, glass, sllca, alumina, alumlnosMcate, dlcalclum phosphate, sodium bicarbonate, sodium meta phosphate, potassium mataphosphata, tricalclum phosphate, calcium pyrophosphate, calcium carbonate, and bentontte. According to some embodiments, abrasives may be present in an amount ranging from about 4 percent to about 25 percent by weight, relative to the total weight of the antimicrobial abrasive composition.

[0144] According to some embodiments, a method of making an antimicrobial composition (e.g., a biocklal abrasive composition) may include providing one or more minerals and contacting the one or more m in era Is with an antimicrobial metal compound to form antimicrobial metal-treated mineral. Providing the one or more minerals may Include providing one or more minerals having a top particle size (dn) less than SO d ₁₀ and a median particle size (dn) less than 30 d ₁₀ . The one or more minerals may range from 0.1 percent to 20 percent by weight of the composition. According to some embodiments, an antimicrobial metal compound precipitated and attached to the surface of the one or more minerals may be achieved, for example, by contacting the one or more minerals with an antimicrobial metal compound, which may include contacting the one or more minerals with a metal compound Including at toast one of zinc, copper, and slver. For example, contacting the one or more minerals with an antimicrobial metal compound may Include contacting the one or more minerals with a metal compound Including zinc oxide (e.g., nano-zinc oxide) using a binder. According to some embodiments, the method may further include precipitating and attaching the antimicrobial metal compound on the surface of the one or more minerals. According to some embodiments, the one or more minerals may be coated with antimicrobial metal compound.

[0145] The following examples are intended to Illustrate the present disclosure without, however, being ImirJng in nature. It is understood that the present disclosure encompasses additional embodiments and embodiments consistent with the foregoing description and following examples.

Preparation of a nano zinc oxide coated filter aid

[0146] A desired amount of zinc acetate (Table 1) was dissolved in water at room temperature. The pH of the zinc acetate solution was adjusted to about 6.3 by adding NaOH. The zinc acetate solution was then slowly added to 120 g or 200 g (as shown in the Table) of diatomaceoue earth fitter aid in a Hobart food mixer. Two commercial filter aid products were used as the feed materials: CeJite Standard Super-eel from Lompoc deposit for [Examples 1- 5 and Celite Standard Super-cel from Murat deposit for (Examples 6-10. After mixing for 15 minutes, the mixture was brushed through a 14 mesh screen with a 1.40 mm opening to disperse large lumps. The first screening through the 14 mesh screen may disperse wet large lumps. After drying In a 150ºC oven overnight, the material was brushed through a 30 mesh (0.595 mm opening) screen. The second screening through the 30 mesh screen may break/remove dried large granules, which may be present In relatively small amounts. Zinc content In the antimicrobial tiller was measured by Inductively coupled plasma (ICP).

Table 1: Antimicrobial fitter aid saffiple preparation

Anti-mlcroblaJ testing

[0147] Malctactic Cultures from White Labs (San Diego, CA) were used to grow lactic acid bacteria in unfittered apple Juice solution. The juice solution was prepared using 25 percent (volume) Dl water and 75 percent (volume) unfittered apple Juice. 35 mL of Malotactic Cultures was added to 250 mL of Juice and water solution. The solution with Malolactic Cultures was then kept in a 30°C oven for 7 days for lactic acid bacteria growth.

[0146] For antibacterial treatment, 1 g of antimicrobial filter aid was added to 50 ml of the lactic acid bacteria solution and stirred for 30 minutes. The solution was then filtered through a 0.45 um filter paper. The filtrate was sent out to a contract tab (EMSL Analytical, Inc.) for tactic acid bacteria measurement using petrifllm Aerobic Count (AC) Plates, a sample-ready culture medium system which contains standard methods nutrients, a cold- w >ater-soluble gelling agent, and a tetrazolium indicator that facilitates colony enumeration.

[0149] The results of the above-described test showed that lactic acid bacteria count was reduced by ΘΘ.5 percent after treatment wtth antimicrobial flier aid. Table 2 shows the lactic acid bacteria count when treated wtth the Example 6 fitter aid sample, compared to the bacteria count for an untreated control solution.

Table 2: Lactic Acid Bacteria Count

Preparation of a nano zinc oxide coated filter

[0150] Antimicrobial filler can be prepared using the same method as the antimicrobial filter aid. A commercial natural dlatomto fMerfrom Mexico with a median particle size of 14 microns was used as the feed material for nano zinc oxide coating in (Examples 11 - 17 (Table 3). A commercial expanded peritte with a median particle size of 25 micro Π8 was used as the feed material in [Example 18. Table 4 lists the particle size, Hunter scale L, a, b color data (The L value Indicates the level of light or dark, the a^value indicates the level of redness or greenness, and the b- value indicates the level of yellowness or blueness), wet density and ol absorption of the antimicrobial diatomite and perl He fillers.

[0151] Table 5 Illustrates how Streptococcus mutens bacteria counts were affected by various zinc oxide coated diatomaceous earth preparations.

[0152] A direct bacterial kHng experiment was done using spiral plating to measure the viability of the Streptococcus mutens UA159 (ATCC 700810) (S. mutans). Streptococcus mutens is facultative anaerobic, gram-positive coccus-shaped bacterium commonly found In the human oral cavity and is a significant contributor to tooth decay. [0153] All of the teats on Examples 11-16 were measured bBndry without any knowledge of their composMon. This was accomplished by pipetting 1 ml of the diluted sample powder particles (100 mg/ml) into 3 ml of Tryptic Soy broth containing 1% sucrose (T5BS) and 20 μΙ of an overnight culture of S. mutana. The inoculated suspensions were Incubated for 24 hours at 37 ^a C In 5% C¾, diluted 1:10 and 1:1000, and spiral plated onto blood agar plates. The colonies on the ptates were counted In a Colony Forming Unit (CFU) after 24 hours of incubation. A 0.12% chlorhexidine (CHX) was used as a positive control, and sterile water was used as a negative control. Zinc content in the antimicrobial filer was measured by Inductively coupled plasma (ICP).

Table 5: Streptococcus mutans Bacteria Count

[0154] As shown In Table 5, Streptococcus mutana bacteria can be significantly reduced by the antimicrobial filler. The reduction (killing) of bacteria increases with increasing zinc content in the antimicrobial filler. At 6.6% zinc, the antimicrobial effect is the same as the negative control of chlorhexidine. All bacteria are killed when zinc content is at 7.82%.

[0155] Similar to zinc acetate, zinc sulfate solution wRh various zinc sulfate concentrations can also be used to make zinc and diatomHe composite materials using the similar method for the zinc acetate (Table 6). A natural Mexican DE with a median particle size of 14 microns was used as feed material. Alter coating, the coated materials were dried/neat-treated at 120ºC to 300'C.

[0156] A commercial perHe product with a mean particle size of 20 μm was mixed with a commercial zinc oodde product such as Akrochem XF-11 with a mean particle size of 0.11 μm in a Hobart food mixer according to the mixing ratio in Table 7.

[0157] 3 g of sodium silicate was dispersed in 20 g of Dl water and then slowly added to the mixture of periite and zinc oxide in the Hobart food mixer. After mixing with sodium silicate solution for 15 minutes, the mixture was dried In a 150°C oven overnight. The dried material was then brushed through a 30 mesh (0.6 mm opening) screen.

[0158] The same procedure was used to prepare periite and titanium oxide composites. A commercial titanium oxide such as TVPure™ R-900 rutfle titanium oxide with a mean particle size of 0.41 d ₁₀ was used. A sample with 10 g periite and 90 g of titanium oxide was prepared. The same procedures can also be used to prepare DE and zinc oxide/titanium oxide for other appications.

Calcined zinc cndde and DE composites

[0159] Zinc and DE composites can also be prepared by calcination of the DE with zinc oxide at high temperature. A natural DE from Lompoc with a median particle size of 20 microns was used as feed material. A desired amount of DE and zinc oxide was mixed homogenousiy and then placed in a ceramic boat and calcined at high temperature In a muffle furnace (Table 8).

Calcined and flux calcined zinc oxide and DE/perfite compostes.

[0160] Zinc and DE/perlKe composites can also be praparad by calcination of the DE/perike composites with zinc oxide at high temperature. A natural DE from Nouvelle with a median particle size of 15 microns and an expanded periite with a median particle size of 40 microns were used as feed materials. A desired amount of DE and periite mixture and zinc oxide were mixed homogenously and then placed in a ceramic boat and calcined at high temperature in a muffle furnace (Table Θ). For [Examples 36 and 37, sodium carbonate was added as flux for high temperature calcination.

[0161] As further examples, summarized hi Table 10 below, desired amounts of zinc acetate were dissolved in water, added to a filter aid comprising periite, and tested for permeability and wet density. The methods of example preparation and testing are consistent with those used to determine the data Isted In Table 1 above. As these examples illustrate, adding the zinc oxide to different filter aid feeds results In permeability and wet density values that may be desirable for particular fittering applications.

Table 10: Antimicrobial filter aid sample preparation

[0162] Other embodiments of the disclosure will be apparent to thoee ski led in the art from consideration of the specification and practice of the disclosure disclosed herein. It Is intended that the specrfication and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.