EP4577496A1 - Granules et poudre à base de silice réfléchissante destinés à être utilisés dans des matériaux de toiture et architecturaux et leurs procédés de fabrication - Google Patents

Granules et poudre à base de silice réfléchissante destinés à être utilisés dans des matériaux de toiture et architecturaux et leurs procédés de fabrication

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Publication number
EP4577496A1
EP4577496A1 EP23772376.2A EP23772376A EP4577496A1 EP 4577496 A1 EP4577496 A1 EP 4577496A1 EP 23772376 A EP23772376 A EP 23772376A EP 4577496 A1 EP4577496 A1 EP 4577496A1
Authority
EP
European Patent Office
Prior art keywords
silica
white
white silica
granules
feed material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP23772376.2A
Other languages
German (de)
English (en)
Inventor
John Squires JACKSON
Claud Eric Westbrook
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Covia Solutions LLC
Original Assignee
Covia Solutions LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Covia Solutions LLC filed Critical Covia Solutions LLC
Publication of EP4577496A1 publication Critical patent/EP4577496A1/fr
Pending legal-status Critical Current

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    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0016—Granular materials, e.g. microballoons
    • C04B20/002—Hollow or porous granular materials
    • C04B20/004—Hollow or porous granular materials inorganic
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    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10—Coating or impregnating
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    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse ; Residues
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    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
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    • C04B33/1324—Recycled material, e.g. tile dust, stone waste, spent refractory material
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
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    • C04B35/64—Burning or sintering processes
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62—L* (lightness axis)
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00586—Roofing materials
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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Definitions

  • Quartz sand ore processing normally begins with a series of steps carried out to liberate the desired quartz ore from gross impurities. These steps typically include crushing (if hard rock or sandstone), scrubbing, washing, hydro-sizing and desliming. If the ore contains dissimilar materials such as feldspar, garnets and mica, flotation may also be needed. Magnetic separation can also be used for removing magnetic or para-magnetic particles. Thereafter, the cleaned ore is normally dried and classified by size, which is typically done by bulk dewatering using cyclones and/or pile draining, heating to dryness (e.g., less than about 1 wt.% water) and sizing via screens or sifters.
  • steps typically include crushing (if hard rock or sandstone), scrubbing, washing, hydro-sizing and desliming. If the ore contains dissimilar materials such as feldspar, garnets and mica, flotation may also be needed. Magnetic separation can also be used for removing magnetic or para-magnetic particles
  • the feed material may be raw quartz sand which already has the desired relatively high level of silica purity or which can be easily and inexpensively cleaned such as by scrubbing, washing, hydro-sizing, desliming and the like to achieve this relatively high level of silica purity.
  • raw quartz sand will be understood to mean a naturally-occurring free-flowing, sand in which at least 95 wt.% of the silica present has a quartz crystal structure.
  • “naturally-occurring” will be understood to mean that, prior to when the thermal treatment process of this invention begins, the silica feed material has not been treated so as to convert it chemically to another material such as occurs, for example, when quartz silica is converted into an alkali metal silicate, an alkoxy silane or a hydrolyzed silica or to convert it physically to another material such as occurs, for example, when particulate silica is transformed into a silica sol or water-glass or when particulate silica is fired/sintered at temperatures high enough to change the phase structure of the silica from crystalline to amorphous and/or to change the shape of the silica particle to more-nearly spherical.
  • “naturally-occurring” means that the particulate product is found essentially as is in nature such as occurs, for example, in the case of beach sand, quarry sand, and sand obtained by crushing sandstone and the like.
  • a white silica-based product includes white or ultrawhite silica-based granules in accordance with the present disclosure, a white or ultra-white silica- based powder in accordance with the present disclosure, or combinations thereof.
  • the feed material may contain from about 0.2 wt.% to about 2.0 wt.%, from about 0.5 wt.% to about 2.0 wt.%, from about 0.6 wt.% to about 2.0 wt.%, from about 0.7 wt.% to about 2.0 wt.%, from about 0.8 wt.% to about 2.0 wt.%, from about 0.9 wt.% to about 2.0 wt.%, from about 0.2 wt.% to about 1.5 wt.%, from 0.5 wt.% to about 1.5 wt.%, from about 0.6 wt.% to about 1.5 wt.%, from about 0.7 wt.% to about 1.5 wt.%, from about 0.8 wt.% to about 1 .5 wt.%, from about 0.9 wt.% to about 1 .5 wt.%, from about 0.2 wt.% to about 1.0 wt.%, from about
  • the silica feed material will be a raw quartz sand having a particle size of 30 to 170 mesh (U.S.).
  • feed materials with other particle sizes can also be used.
  • the silica feed material can have a gravel particle size of 2.5 to 8 mesh (U.S.), a grit or coarse sand particle size of 8 to 70 mesh (U.S ), or a fine sand particle size of 70 to 170 mesh (U.S.).
  • Silica feed material having a particle size of 140 to 200 mesh (U.S.) can also be used, depending on the particular embodiment. It should be understood that the milling process described hereinbelow can enable the use of silica feed material having a wide variety of particle sizes.
  • waste sand fractions that are often found in various different sand plants may be used as a feed material.
  • Many industrial sand plants are operated to produce sand fractions of different particle sizes and/or particle size distributions for making different products such as glass, proppants, play sand, concrete sand, etc.
  • high quality, high purity sand fractions having particle sizes of limited commercial interest are often produced as by-products during the manufacture of commercial products.
  • These sand fractions are either not used as all, or in some instances, must be discharged to waste such as by burying them underground or otherwise returning them to the mine, beach, or other geological location from which they were originally obtained. Accordingly, these sand fractions, hereinafter “waste sand by-products” either have no value at all or, more commonly, have a negative value due the cost of discharging them to waste.
  • the feed material is subjected to a milling step.
  • the feed material is milled to a maximum mesh size of approximately 325 mesh.
  • Milling can be conducted using any suitable equipment and protocols known and used in the art.
  • the milling is effective to form angular powder particles having a mean particle size of from about 10-15 pm.
  • the milling is effective to generate particles having a particle size of from about 0.5 pm to about 50 pm.
  • the milled feed material is combined with a binding agent and water in an agglomeration step Tn various embodiments, the milled feed material may be combined with water and a binding agent, a fluxing agent, or both a fluxing agent and a binding agent in an agglomeration step.
  • the binding agent is a sodium-containing binding agent, such as, by way of example and not limitation, sodium silicate.
  • the fluxing agent is a sodium-containing fluxing agent, for example, sodium hydroxide.
  • binding agents such as sodium silicate
  • a binding agent e.g., to bind particles to one another
  • a fluxing agent e.g., cause the crystal structure of the silica to change from quartz to cristobalite and/or tridymite under reduced thermal conditions than would otherwise be the case.
  • the binding agent is present in an amount of from about 0.2 wt.% to about 10 wt.%, based on a total weight of the final product.
  • the binding agent can be present in an amount of from about 0.5 wt.% to about 10 wt.%, from about 0.5 wt.% to about 7.5 wt.%, from about 0.5 wt.% to about 5.0 wt.%, from about 1.0 wt.% to about 10 wt.%, from about 1.0 wt.% to about 7.5 wt.%, from about 1.0 wt.% to about 5.0 wt.%, from about 1 .5 wt.% to about 10 wt.%, from about 1 .5 wt.% to about 7.5 wt.%, from about 1.5 wt.% to about 5.0 wt.%, from about 2.0 wt.% to about 10 wt.%, from about 2.0 wt.% to about 7.5 wt.%, from about 2.0 wt.% to about 5.0 wt.%, from about 2.5 wt.% to about 10 wt.%, from
  • the water can be present in an amount of from about 10 wt.% to about 20 wt.%, based on a total weight of the final product.
  • the water can be present in an amount of from about 10 wt.% to about 20 wt.%, from about 11 wt.% to about 18 wt.%, or from about 12 wt.% to about 16 wt.%, including any and all ranges and subranges therein.
  • Water can be added as a separate component into the agglomerated mixture, as part of the binding agent (e.g., when the binding agent is added in an aqueous form), or as a combination thereof.
  • the binding agent is added as a 40 wt.% active sodium silicate aqueous solution, and auxiliary water is also added to the milled feed material.
  • the binding agent and water are applied to the milled feed material via spraying or pouring a diluted aqueous binding agent into a granulator, including, but not limited to, an Eirich mixer. Regardless of the application method, the milled feed material, binding agent, and water are mixed and granulated to provide an agglomerated mixture, sometimes referred to herein as granules. In other embodiments, water and the binding agent, the fluxing agent, or both the binding agent and the fluxing agent are applied to the milled feed material and mixed to form granules.
  • agglomeration can be conducted according to any suitable method known and used in the art, in various embodiments, the agglomeration can be carried out at ambient temperature.
  • the agglomerated mixture (i.e., the granules) flows into a rotary kiln where it is heated for a time and at a temperature which are sufficient to transform the crystal structure of a substantial amount of its silica content from quartz to cristobalite.
  • various embodiments provide a white or ultra-white silica-based product as an alternative product which performs essentially as well, or even just as well, as industrial cristobalite in many applications but at significantly lower cost.
  • the agglomerated mixture is heated to a temperature of no more than about 1550° C for no more than about an hour (z. e., about 60 minutes). In some embodiments, the agglomerated mixture is heated to a temperature of from about 1300° C to about 1550° C, from about 1325° C to about 1550° C, from about 1350° C to about 1550° C, or from about 1375° C to about 1550° C for a time of from about 40 minutes to about 60 minutes. Although the temperature can vary depending on the particular embodiment, in general, the temperature can be high enough to achieve a primarily cristobalite silica composition.
  • the milling of the feed sand produces particles that can be converted to cristobalite at a lower temperature than is required according to conventional methods.
  • the temperature can be sufficient to sinter the particles into cohesive granules, thereby providing mechanical integrity to the granules.
  • Heating can be carried out, for example, in a continuous manner in a rotary kiln, although other methods of heating are possible and contemplated.
  • a waterproofing or other functional coating can be applied to the white or ultra-white silica-based product while the white or ultra-white silica-based product is at a temperature of from about 75° C to about 100° C, and the coated silica can then be cooled to room temperature.
  • a functional coating can be applied to the white or ultra-white silica-based product while the white or ultra-white silica-based product is at a temperature of less than 50° C.
  • a functional coating can be applied to the white or ultra-white silica-based product at a temperature of from about 15° C to about 50° C.
  • the white or ultra- white silica-based product can be sieved for selection of granules having a particular size. Sieving can be carried out in any suitable method known and used in the art, including but not limited to the use of vibratory screens.
  • the granules are selected to have a particle size based on a -8/+35 mesh. In some embodiments, the granules have an average particle size of from about 0.45 mm to about 2.5 mm. However, in other embodiments, granules having larger or smaller particle sizes can be used, depending on the particular application.
  • the granules when the granules are intended for use in roofing applications (e.g., applied to the surface of a shingle or flat top roof), the granules can be selected to have a standard size #11 granule size or another standard size that is commonly used in the roofing industry. In other applications, such as when the granules will be used as a filler for pigments, coarser or finer granules can be used. As will be described in greater detail below, in some embodiments, granules that are coarser and/or finer than the granule size for the particular embodiment can be further processed.
  • the shape of the white or ultra-white silica-based granules is typically round, although it is contemplated that the agglomeration process described above could be altered to achieve granules having other shapes.
  • the bulk density of the white or ultra-white silica-based granules is less than about 75 lb/ft 3 .
  • the bulk density of the white or ultra-white granular silica-based filler is from about 30 lb/ft 3 to about 75 lb/ft 3 , from about 35 lb/ft 3 to about 75 lb/ft 3 , from about 40 lb/ft 3 to about 75 lb/ft 3 , from about 45 lb/ft 3 to about 75 lb/ft 3 , or from about 50 lb/ft 3 to about 75 lb/ft 3 .
  • the white or ultrawhite granular silica-based filler has a specific gravity (via helium pycnometry) of from about 2.32 to about 2.40, depending on the temperature and retention time during thermal processing. This is in contrast to a specific gravity of about 2.65 for the feed material of particular embodiments.
  • the specific gravity measurements of the granules via water pycnometry indicated a decrease of about 20% as compared to the feed material, suggesting a significant void volume within the granules that are produced by this method.
  • the white or ultra-white silica- based granules exhibit an L* value of from about 93 to about 98, such as from about 94 to about 97, from about 94 to about 98, from about 95 to about 98, from about 96 to about 98, from about 93 to about 97, from about 93 to about 96.5, from about 93 to about 96, from about 93 to about 95, or from about 95 to about 96.5.
  • the white or ultra-white silica- based granules exhibit an average visible light reflectance of between about 75% and about 85%, such as from about 77% to about 83% or from about 79% to about 82%.
  • the over-sized white or ultra-white silica fraction and the under-sized white or ultra-white silica fraction are combined for further processing.
  • the over-sized white or ultra-white silica fraction and the under-sized white or ultra-white silica fraction are primarily cristobalite and has a specific gravity (via helium pycnometry) of from about 2.32 to about 2.40, depending on the temperature and retention time during thermal processing.
  • the combined fractions can then be milled or ground to produce a powder having a maximum mesh size of 325 mesh.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

Un procédé de production d'un produit à base de silice blanche, tel qu'un granule (par ex., un granule de toiture) comprend le broyage d'un matériau d'alimentation pour former un matériau d'alimentation broyé ayant une taille d'environ 0,5 µm à environ 50 µm ; la combinaison du matériau d'alimentation broyé avec un agent de liaison et de l'eau pour fournir un mélange aggloméré ; et le chauffage du mélange aggloméré pendant une certaine durée et à une température d'environ 1 350 °C à moins d'environ 1 550 °C pour former le produit à base de silice blanche. Le mélange aggloméré est suffisamment chauffé de telle sorte que la cristobalite est la structure cristalline de silice prédominante dans le produit à base de silice blanche, et en outre de telle sorte que le produit à base de silice blanche présente une valeur L* dans l'espace chromatique CIELAB de 93 à 98.
EP23772376.2A 2022-08-23 2023-08-21 Granules et poudre à base de silice réfléchissante destinés à être utilisés dans des matériaux de toiture et architecturaux et leurs procédés de fabrication Pending EP4577496A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US202263373291P 2022-08-23 2022-08-23
PCT/US2023/072546 WO2024044527A1 (fr) 2022-08-23 2023-08-21 Granules et poudre à base de silice réfléchissante destinés à être utilisés dans des matériaux de toiture et architecturaux et leurs procédés de fabrication

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EP4577496A1 true EP4577496A1 (fr) 2025-07-02

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EP (1) EP4577496A1 (fr)
JP (1) JP2025527724A (fr)
KR (1) KR20250056218A (fr)
CN (1) CN119816470A (fr)
CA (1) CA3265651A1 (fr)
MX (1) MX2025002162A (fr)
WO (1) WO2024044527A1 (fr)

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WO2026037952A1 (fr) 2024-08-15 2026-02-19 Amberger Kaolinwerke Eduard Kick Gmbh & Co. Kg Matériau de revêtement de toit

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2876893C (fr) * 2012-06-19 2021-12-28 Specialty Granules, Inc. Granules de couverture blancs super brillants presentant un facteur de reflexion solaire eleve
CA3052110C (fr) * 2017-02-27 2022-07-26 Icopal, A/S Granule enrobe, et membrane bitumineuse de toiture comprenant une pluralite des granules enrobes
EP3771701B1 (fr) * 2019-07-31 2021-09-08 Cosentino Research & Development, S.L. Article de pierre agglomérée artificielle comprenant des granulés de silicate synthétique

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KR20250056218A (ko) 2025-04-25
WO2024044527A1 (fr) 2024-02-29
JP2025527724A (ja) 2025-08-22
CA3265651A1 (fr) 2024-02-29
CN119816470A (zh) 2025-04-11

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