Rock particle preparation, use and process for obtaining it.
A top-down comminution process produces rock particles with nanometric size and high purity, addressing the limitations of existing methods to create scalable, high-purity rock particles for diverse industrial uses.
Patent Information
- Application Number
- BR102024026683
- Authority / Receiving Office
- BR · BR
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-12-19
- Publication Date
- 2026-07-07
AI Technical Summary
Existing methods fail to produce rock particles with predominantly or entirely nanometric particle size distribution and high purity on a large scale, limiting their use in high-value industrial applications.
A top-down comminution process using high-energy mills and jet mills with controlled conditions to produce rock particles predominantly or entirely in the nanometer range, achieving high purity and defined particle size distribution without chemical reactions.
Enables the large-scale production of rock particles with defined particle size distribution and high specific surface area, suitable for various industrial applications, including modulating mechanical and electromagnetic properties of materials.
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Description
16 Descriptive Report of Invention Patent: ROCK PARTICLE PREPARATION, USE AND PROCESS FOR OBTAINING IT Field of Invention
[0001] This report covers confidential knowledge, information and / or data usable in industry, commerce or service provision, for which the holder requests: the protection established in item XXIX of Article 5 of the Federal Constitution; the maintenance of the legal status of confidentiality / secrecy; the maintenance of the physical status of confidentiality / secrecy for the time stipulated in Law 9.279 / 96, the Industrial Property Law; and the rights provided for in Article 195 of Law 9.279 / 96. The present invention is situated in the field of materials engineering and nanotechnology. More specifically, the invention describes a rock particle preparation, its use, and a process for obtaining it by comminution, i.e., a top-down process. The particle preparation of the invention solves these and other problems and has peculiar composition, purity, particle size distribution and specific surface area, being useful in a variety of applications.The invention also discloses a process for obtaining particles of rock-containing mineral species, for example basaltic rock, by means of controlled comminution and without chemical reactions or contamination with reagents typical of nanoparticle synthesis. The present invention, in stark contrast to the prior art, provides for the large-scale production of rock particles with high purity, a defined particle size distribution, and a very high specific surface area, making their use in various industrial applications practically feasible. Background of the Invention
[0002] Volcanic rocks containing plagioclase and pyroxene (components of basalt fiber) are found, for example, throughout the region. Petition 870240108404, dated 12 / 19 / 2024, page 5 / 33 / 16 Central-Southern Brazil in the geological formation known as the Serra Geral Formation (FSG).
[0003] Adding value to materials extracted from nature is a constant challenge in the technical field of materials engineering. The current high demand for materials for a wide variety of applications makes the development of alternatives to the most commonly used materials fundamental. Furthermore, adding value relates to the more rational use of materials extracted from nature. For example, basaltic rocks from the Serra Geral Formation (FSG) are more commonly used for the production of paving stones and construction materials, such as basements, sinks, and sidewalks.
[0004] Thus, the development of new materials based on available resources to obtain alternative materials for high-tech applications is a constant demand in the field of materials engineering, and technologies in this technical area can have a significant impact on the economic development of a region, as well as a significant environmental impact by promoting the more rational use of materials extracted from nature.
[0005] Therefore, its incorporation into high value-added products is a constant need in the technical field.
[0006] Of particular relevance in the context of the present invention is the difference between: (i) preparations containing a fraction of nanoparticles among the other particles; (ii) preparations containing particles predominantly or entirely in the nanometer particle size range; and (iii) preparations of nanoparticles predominantly or entirely in the nanometer particle size range with a defined particle size distribution profile. The present invention provides these last two.
[0007] Rock particle preparations may eventually contain small fractions of nanoparticles, but the predominance of much larger particles, in the micrometer / micron range, prevents characterization. Petition 870240108404, dated 12 / 19 / 2024, page 6 / 33 / 16 of such preparations as actual nanoparticle preparations. Furthermore, it is known that the behavior of materials at the nanoscale changes substantially and, therefore, the availability on a large scale and with high purity of a preparation containing rock particles predominantly or entirely in the nanometer range and with high purity, without contaminations typical of synthesis processes, is highly desirable. The present invention solves these and other technical problems.
[0008] Grinding / comminution / pulverization methods usually aim to increase the specific surface area and enable various industrial uses. In the case of rocks or materials containing rocks, known methods are limited to obtaining particles with a granulometry in the micrometer range. As of the filing date of this patent application, the present inventors are unaware of any rock grinding methods that would yield preparations entirely containing nanoparticles.
[0009] Based on what can be inferred from the literature reviewed, no documents were found that anticipate or suggest the teachings of the present invention. Summary of the Invention
[0010] The present invention solves several problems of the prior art related to rock preparations with predominantly or entirely nanometric particle size distribution.
[0011] One of the objects of the invention is to provide a preparation of rock nanoparticles with high purity.
[0012] One of the objects of the invention is to provide a preparation of rock particles of chemically defined composition.
[0013] One of the objects of the invention is to provide a preparation of rock particles with d50 to d99 in the nanometer granulometric range.
[0014] One of the objects of the invention is to provide a preparation of rock particles with d90 to d99 in the nanometer granulometric range.
[0015] In some embodiments, the rock particle preparation has Petition 870240108404, dated 12 / 19 / 2024, page 7 / 33 / 16 average particle size (d50) between 403 and 516 nm.
[0016] One of the objects of the invention is to provide a preparation of rock particles in the granulometric range predominantly below 1000 nanometers.
[0017] In some embodiments, the rock particle preparation has the following particle size distribution: d10: between 132 and 153 nm; d50: between 403 and 516 nm; and d90: between 5573 and 7986 nm.
[0018] The particle preparation of the invention is useful in various applications, including: modulating or improving the mechanical properties of steels, metallic and non-metallic alloys, ceramics and / or polymers; composite materials; doping materials to modulate electromagnetic properties for use in electronic components, battery cells, energy storage systems, solar panels, sensors and piezoelectric actuators; modulating the optical properties of glasses or other transparent or translucent materials; use as a component of catalysts; in the preparation of stable liquid / colloidal compositions.
[0019] Another object of the invention is to provide a process for preparing a rock particle preparation by a top-down approach, i.e., by comminution without chemical or mechanochemical synthesis. Said process is large-scale and suitable for the economic viability and effective availability of preparations.
[0020] The invention process comprises the following steps: - Feeding rock particles to a comminuting unit selected from: high-energy mill and steam mill; - Adjust the selected comminution conditions from among: - in a high-energy mill: - Suspend particles to be comminuted in a liquid, at a concentration between 1 and 90% w / w, and stabilize the suspension until a stable colloidal suspension is obtained; and - place the aforementioned suspension and grinding balls into the grinding chamber with Petition 870240108404, dated 12 / 19 / 2024, page 8 / 33 / 16 selected diameter between 5 µm and 1.3 mm; adjust the mill rotation speed between 500 and 4500 rpm; and grind the particles at a temperature below 60 °C; or - In a jet mill with superheated fluid or a Steammill, feed particles smaller than 40 micrometers; adjust the air classifier rotation between 1,000 and 25,000 rpm; adjust the compressed steam pressure between 10 and 100 bar and the temperature between 230 and 360 °C. - comminute the particles until the desired particle size distribution is obtained.
[0021] In one embodiment, the stabilization of the colloidal suspension to be placed in the grinding chamber of the high-energy mill referred to above is selected from: adjusting the pH of the polar liquid medium to the range between 2 and 13, and optionally adding surfactants; or adding surfactants in a non-polar liquid medium.
[0022] In one embodiment, the process of obtaining the rock particles includes grinding in a high-energy mill operating with spheres of special materials, such as Zirconia, Yttria-stabilized Zirconia, Rock-stabilized Zirconia, or combinations thereof, by adjusting specific parameters.
[0023] In another embodiment, the process of obtaining rock particles includes grinding in a jet mill with superheated steam, superheated steam or steammill, by adjusting specific parameters.
[0024] These and other objects of the invention will be immediately appreciated by those skilled in the art and will be described in detail below. Brief Description of the Figures
[0025] The following figures are presented:
[0026] Figure 1 shows the particle size distribution curves of the triplicates from the first rock sample analysis (SN 20 002).
[0027] Figure 2 shows the cumulative volume curves of the triplicates from the first rock sample analysis (SN 20 002). Petition 870240108404, dated 12 / 19 / 2024, page 9 / 33 / 16
[0028] Figure 3 shows the particle size distribution curves of the triplicates from the second rock sample analysis (SN 20 002).
[0029] Figure 4 shows the cumulative volume curves of the triplicates from the second rock sample analysis (SN 20 002).
[0030] Figure 5 shows the particle size distribution curves of the triplicates from the third rock sample analysis (SN 20 002).
[0031] Figure 6 shows the cumulative volume curves of the triplicates from the third rock sample analysis (SN 20 002).
[0032] Figure 7 shows the compiled particle size distribution curves from all rock samples and triplicates (SN 20 002).
[0033] Figure 8 shows the cumulative volume curves compiled from all rock samples and triplicates (SN 20 002).
[0034] Figure 9 shows the zeta potential graph of the analyses of all rock samples (SN 20 002). The x-axis shows time in seconds, the left y-axis shows the zeta potential in mV, and the right y-axis shows the pH. Detailed Description of the Invention
[0035] The present invention solves several problems of the prior art and provides a rock particle preparation that simultaneously meets the following technical characteristics: particles predominantly or entirely in the nanometer granulometric range; high purity; an industrial-scale process that enables supply and use on an economical scale. The said preparation comprises basaltic rock particles, plutonic rock, or combinations thereof.
[0036] In the context of the present invention, the expression “basaltic rock particle” encompasses various chemical entities comprising basaltic rock composition as defined by the TAS diagram (Total-Alkali vs. Silica diagram, which is known to one skilled in the art - % by mass of Na2O + K2O by % by mass of Si2O). Including but not limited to Basalt, Basaltic Andesite, Andesite and Dacite as defined in the TAS diagram. Petition 870240108404, dated 12 / 19 / 2024, page 10 / 33 / 16 Including micro, sub-micro, and nanoparticles, according to their particle size distribution.
[0037] In the context of the present invention, the expression "plutonic rock particle" encompasses particles of various chemical entities formed by the cooling of magma at depth, i.e., within the lithosphere, in such a way that the material does not erupt to the Earth's surface. They are also known as intrusive rocks. Including but not limited to granite, diorite, tourmaline, syenite, and gabbro. Comprising micro, submicro, and nanoparticles, according to their granulometric distribution.
[0038] The invention is also defined by the following clauses.
[0039] Rock particle preparation comprising a content equal to or greater than 95% by weight of rock particles, wherein 10% to 50% of the particles (d10 to d50) are in the granulometric range of 10 to 1000 nanometers (nm).
[0040] Particle preparation as defined above comprising a content of 99% or more by weight of rock particles.
[0041] Particle preparation as defined above wherein said rock is basaltic rock, plutonic rock or combinations thereof. In one embodiment, said rock is basaltic rock. In one embodiment, said rock is plutonic rock.
[0042] Particle preparation as defined above wherein 50% to 99% of the particles (d50 to d99) are in the particle size range of 403 to 19426 nanometers (nm).
[0043] Particle preparation as defined above wherein 90% to 99% of the particles (d90 to d99) are in the particle size range of 5573 to 19426 nanometers (nm).
[0044] Particle preparation as defined above having particle size distribution d10: between 132 and 153 nm; d50: between 403 and 516 nm; and d90: between 5572 and 7986 nm.
[0045] Particle preparation as defined above wherein the specific surface area is from 0.5 to 150 m2 / g. Petition 870240108404, dated 12 / 19 / 2024, page 11 / 33 / 16
[0046] Particle preparation as defined above wherein the average specific surface area is 40 to 70 m2 / g.
[0047] Use of the particle preparation described above for adjusting the rheological properties of other particle or nanoparticle preparations, adjusting packing degrees, flowability, void fractions or other properties of the final preparation.
[0048] Use of the particle preparation described above for the preparation of: stable colloidal compositions; steels, metallic and non-metallic alloys, ceramics and / or polymers; composite materials, electronic components, battery cells, energy storage systems, piezoelectric sensors and actuators, solar panels; glasses, glass-ceramics or other transparent and translucent materials; catalysts.
[0049] Process for obtaining rock particles comprising the following steps: - Feeding rock particles to a comminuting unit selected from: high-energy mill and steam mill; - Adjust the selected comminution conditions from among: - In a high-energy mill: suspend particles to be comminuted in a liquid, at a concentration between 1 and 90% w / w, and stabilize the suspension until a stable colloidal suspension is obtained; place the suspension and grinding beads with a diameter selected between 5 µm and 1.3 mm in the grinding chamber; adjust the mill's rotation speed between 500 and 4500 rpm; and grind the particles at a temperature below 60 °C; or - In a jet mill with superheated fluid or a Steammill, feed particles smaller than 40 micrometers; adjust the air classifier rotation between 1,000 and 25,000 rpm; adjust the compressed steam pressure between 10 and 100 bar and the temperature between 230 and 360 °C; - comminute the particles until the desired particle size distribution is obtained.
[0050] Process as described above in which the stabilization of the colloidal suspension to be placed in the grinding chamber of the high-energy mill is Petition 870240108404, dated 12 / 19 / 2024, page 12 / 33 / 16 selected from: adjusting the pH of the polar liquid medium to the range between 2 and 13, and optionally adding surfactants; or adding surfactants to a non-polar liquid medium.
[0051] Process as described above further comprising a pre-comminution step of the rock particles before the feeding step to the comminuting equipment, said pre-comminution being carried out until the average particle size is less than 40 micrometers. In one embodiment, said pre-comminution being carried out until the average particle size is between 1 and 40 micrometers.
[0052] Process in which the aforementioned pre-comminution is carried out in a ball mill, disc mill or high-energy mill.
[0053] Process in which the aforementioned pre-comminution is carried out in a jet mill or jetmill.
[0054] Process as described above comprising the following steps: - feeding a high-energy mill with rock particles, wherein said particles are micrometric; - feed the mill with a liquid and adjust the pH to the range between 5 and 10; - feeding the aforementioned mill with spheres with a diameter selected between 50 µm and 400 µm; - Adjust the mill's rotation speed between 2000 and 4000 rpm; and - Grind the particles at a temperature below 60 °C until the desired particle size distribution is obtained.
[0055] Process as described above wherein the high-energy mill is of the agitated type and the spheres said are selected from: Zirconia, Silicon carbide, alumina, the spheres said being optionally stabilized with Yttria or rock, or combinations thereof.
[0056] Process as described above in which the superheated temperature jet mill or Steammill is adjusted with the following parameters: air classifier rotation at 20,000 rpm; steam pressure Petition 870240108404, dated 12 / 19 / 2024, page 13 / 33 / 16 compressed at 50 bar; and superheated fluid temperature of 280 °C.
[0057] Process as described above where the operating pH in the mill is 6 to 10.
[0058] Process as described above where the operating temperature in the mill is 30 to 40 °C.
[0059] In some embodiments, the particle preparation of the invention comprises particles with defined particle size fractions, such as, for example, a preparation with particles entirely between 100 and 1000 nm, a preparation with particles entirely between 1 and 100 nanometers, and preparations with particles of intermediate values and with particle size fractions of defined value.
[0060] In some embodiments of the present invention, as is already common practice in the industry, the distribution of particle size fractions is defined by d10, d50, d90 and occasionally d99, notations which reflect the cumulative % volume of particles corresponding to each notation, d10 referring to 10% of the particle volume, d50 to 50% of the volume and so on.
[0061] Product comprising the particle preparation as described above and a material selected from metal, non-metal, ceramic, polymer, glass, glass-ceramics or combinations thereof.
[0062] Product as described above being a stable colloidal composition; steels, metallic and non-metallic alloys, composite materials, electronic components, battery cells, energy storage systems, piezoelectric sensors and actuators, solar panels; transparent and translucent materials; catalysts.
[0063] The particle preparation of the invention is useful in various applications, including: the preparation of stable colloidal suspensions; the modulation or improvement of the mechanical properties of steels, metallic and non-metallic alloys, ceramics and / or polymers; composite materials; the doping of materials to modulate electromagnetic properties for use in electronic components, battery cells, energy storage systems, panels Petition 870240108404, dated 12 / 19 / 2024, page 14 / 33 / 16 solar, piezoelectric sensors and actuators; the modulation of optical properties of glasses or other transparent materials; the use as a component of catalysts.
[0064] In one embodiment, the use of the particle preparation of the invention provided the obtaining of stable liquid compositions or colloidal suspensions, in which the particles remain in suspension for a long time, providing a long shelf life.
[0065] The process for obtaining rock particles differs from other similar processes in that it is a top-down process, without chemical reactions or mechanochemistry. The fact that pure or highly pure rock particles are used for comminution allows for the production of highly pure particle preparations, since the process does not add impurities or lead to the formation of reaction products, as is the case with state-of-the-art bottom-up, synthesis, or mechanochemical processes.
[0066] The invention process comprises the following steps: - Feeding rock particles to a comminuting machine selected from: high-energy mill; and steammill; - Adjust the selected comminution conditions from among: - in a high-energy mill: - Suspend particles to be comminuted in a liquid, at a concentration between 1 and 90% w / w, and stabilize the suspension until a stable colloidal suspension is obtained; and - Place the aforementioned suspension and grinding balls with a selected diameter between 5 µm and 1.3 mm in the grinding chamber; adjust the mill rotation speed between 500 and 4500 rpm; and grind the particles at a temperature below 60 °C; - In a superheated jet mill or Steammill, feed particles smaller than 40 micrometers; adjust the air classifier rotation between 1,000 and 25,000 rpm; adjust the compressed steam pressure between 10 and 100 bar and the temperature between 230 and 360 °C; and Petition 870240108404, dated 12 / 19 / 2024, page 15 / 33 / 16 - comminute the particles until the desired particle size distribution is obtained.
[0067] Reducing the average particle size before the process as demonstrated above is particularly useful for improving the performance of the subsequent comminution process in a high-energy mill, as demonstrated in Examples 1-4, or in a steammill comminution process, described in Example 3 below.
[0068] In one embodiment, the process involves wet milling in a high-energy mill and enables, on an industrial scale, for the first time, the production of rock particles predominantly or entirely in the nanometer granulometric range. In embodiments where comminution is carried out in wet high-energy mills, the stabilization of the colloidal suspension to be placed in the milling chamber of the high-energy mill is a very important step, and is selected from among: adjusting the pH of the polar liquid medium to the range between 2 and 13, and optionally adding surfactants; or adding surfactants in a non-polar liquid medium.
[0069] In one embodiment, a known prior art mill is used, such as a high-energy mill with yttria-stabilized zirconia (ZrO2 + Y2O3) spheres, by adjusting specific parameters, including rotation time, pH, and temperature. In one embodiment, the grinding medium includes zirconia balls, ZTA (yttria- or alumina-reinforced zirconia), and alumina. Preferably, zirconia spheres stabilized with 5% w / w yttria are used.
[0070] In another embodiment, the process involves comminution by jet mill with superheated steam (steammill), to which particles smaller than 40 microns are fed, with the rotation of the air classifier adjusted between 1,000 and 25,000 rpm, the pressure of the compressed steam between 10 and 100 bar, and the temperature between 230 and 360 °C.
[0071] Examples
[0072] The examples shown here are intended only to illustrate some of the various ways of carrying out the invention, however without limitation, the Petition 870240108404, dated 12 / 19 / 2024, p. 16 / 33 / 16 scope of the same.
[0073] Example 1 - Wet grinding process of basaltic rock in a high-energy mill
[0074] A Labstar LS01 (Netzsch) stirred-ball mill was fed with micrometric basaltic rock particles. The process involved high-energy wet milling. The particle suspension was 17.7 wt%, consisting of approximately 3500 g of milli-Q water + 10 M NaOH and 750 g of the solid sample, which was prepared and stabilized in the mill's mixing tank at pH 9 and titrated with 10 M NaOH. The milling spheres used were yttria-stabilized zirconia, 400 μm in diameter. The milling chamber was filled to 80% vol and the suspension temperature was below 40 °C. The mill rotation speed was set to 3000 rpm and milling was conducted for 8 hours. To stabilize the suspension at pH 9, 10 M NaOH was added during milling, and samples were taken periodically to measure particle sizes.
[0075] Particle size measurements were performed using a Fritsch Analysette 22 instrument, with an accessory unit for wet particle size measurement. Particle size distribution measurements were performed using static light scattering. The analytical medium was distilled water. An aliquot of the suspension with 17.7% w / w, during the grinding process, was analyzed in ten repetitions using the equipment. The results in Table 2 present the measurements (average of 10 measurements) and the PSD (particle size distribution) obtained at each grinding time under the conditions indicated above.
[0076] Example 2 - Comminution of basaltic rock by Jetmill
[0077] In the present example, a jet mill was used to pre-comminute basaltic rock particles, in order to improve the performance of the subsequent comminution process until the particle size distribution is fully (d99) in the nanometer range.
[0078] Example 3 - Comminution of basaltic rock by Steammill Petition 870240108404, dated 12 / 19 / 2024, page 17 / 33 / 16
[0079] In this embodiment, basaltic rock particles with the distribution profile dD90=22.3 μm; D50=8.88 μm; d10=2.77 μm were fed to a steammill.
[0080] Next, the air classifier rotation was adjusted to 20,000 rpm and the compressed steam pressure to 50 bar. The temperature of the superheated fluid was 280 °C.
[0081] Example 4 - Characterization of the particles obtained
[0082] Results of particle size analyses
[0083] Table 1 shows the particle size distribution (DTP) of basaltic rock.
[0084] Table 1: DTP of basaltic rock. Q3(x) [%] Average [pm] CV [%] #4470 #4473 #4476 #4477 #4478 #4479 #4480 #4481 #4482 5 0.107 5.885 0.111 0.103 0.101 0.101 0.100 0.117 0.117 0.109 0.109 10 0.142 5.516 0.148 0.137 0.133 0.132 0.132 0.153 0.152 0.142 0.141 25 0.230 5.740 0.248 0.227 0.217 0.215 0.214 0.248 0.246 0.229 0.227 50 0.449 7.906 0.516 0.455 0.419 0.407 0.403 0.486 0.473 0.442 0.438 75 1.680 20.753 2.246 1.972 1.377 1.182 1.162 1.849 1.654 1.825 1.855 90 6.537 13.148 7.585 7.985 5.915 5.574 5.707 6.363 5.646 7.296 6.758 95 10.237 10,313 11,0258 12,369 9,803 9,517 9,588 9,538 8,797 11,317 10,173 99 16,389 8,3618 16,991 19,425 16,260 15,891 15,727 15,108 14,638 17,644 15,813
[0085] Figures 1-6 show the curves corresponding to the particle size distribution profile of three samples of the present invention. The x-axis shows the equivalent particle diameter in micrometers, the left y-axis the cumulative volume %, and the right y-axis the volume %.
[0086] Results of zeta potential analyses
[0087] Table 2 shows the results of the mean zeta potential analyses of each of the basaltic rock nanoparticle samples analyzed.
[0088] Table 2: Results of zeta potential analyses of rock samples. Sample Average zeta potential (mV) Maximum zeta potential Average pH Average conductivity (S / cm) Average temperature (°C) Petition 870240108404, dated 12 / 19 / 2024, page 18 / 33 / 16 (mV) 1 -41.8 -41.7 9.4 172.7u 20.6 2 -43.3 -43.2 9.5 174.3u 20.3 3 -44.0 -43.7 9.4 175.3u 20.2
[0089] Figure 9 shows the result of the zeta potential analysis of each of the basalt rock nanoparticle samples. The x-axis shows the time in seconds, the left y-axis shows the zeta potential in mV, and the right y-axis shows the pH.
[0090] Summary of results
[0091] The summary compiling the average values obtained for the rock sample (SN 20 002) from all characterization analyses performed is presented in Table 3.
[0092] Table 3: Summary of the results of the rock sample analyses (SN 20 002). Property of Rock (SN 20 002) Electrical conductivity (S / cm) 174.1 pH 9.4 Zeta potential (mV) -43.0 d10 (nm) 141.2 d50 (nm) 448.8 d90 (nm) 6536.7 * average values
[0093] The zeta potential, pH, and electrical conductivity results obtained for the rock suspension sample (SN 20 002) are presented in Table 4.
[0094] Table 4: Zeta potential, pH, and electrical conductivity results of the rock samples (SN 20 002). SN 20 002 Zeta Potential (mV) pH Electrical Conductivity (S / cm) Analysis 1 -41.8 9.4 172.7 Analysis 2 -43.3 9.5 174.3 Petition 870240108404, dated 12 / 19 / 2024, page 19 / 33 / 16 Analysis 3 -44.0 9.4 175.3 Average -43.0 9.4 174.1
[0095] The particle size results d10, d50 and d90 obtained for the rock sample (SN 20 002) are presented in Table 5. The compilation of the particle size distribution curves and accumulated volume obtained for the rock sample (SN 20 002) are presented in Figure 7 and Figure 8, respectively.
[0096] Table 5: Particle size results of the rock sample (SN 20 002) SN 20 002 d10 (nm) d50 (nm) d90 (nm) Analysis 1.1 147.72 515.82 7585.24 Analysis 1.2 136.93 455.39 7985.35 Analysis 1.3 132.79 419.15 5915.51 Analysis 2.1 132.51 407.07 5573.82 Analysis 2.2 132.13 403.45 5706.92 Analysis 2.3 152.82 485.88 6363.49 Analysis 3.1 152.19 472.82 5646.10 Analysis 3.2 141.97 442.11 7295.82 Analysis 3.3 141.44 437.75 6757.74 Average 141.17 448.82 6536.66
[0097] Those skilled in the art will appreciate the knowledge presented here and may reproduce the invention in the forms presented and in other variants and alternatives, covered by the scope of the following claims. Petition 870240108404, dated 12 / 19 / 2024, p. 20 / 33
Claims
1 / 4 Claims 1. Rock particle preparation characterized by comprising a content equal to or greater than 95% by weight of rock particles, wherein 10% to 50% of the particles (d10 to d50) are in the granulometric range of 10 to 1000 nanometers (nm).
2. Rock particle preparation according to claim 1, characterized in that its content is equal to or greater than 99% by weight of rock particles.
3. Rock particle preparation according to claim 1, characterized in that said rock is basaltic rock, plutonic rock or combinations thereof.
4. Rock particle preparation according to claim 3, characterized in that said rock is basaltic rock.
5. Preparation of rock particles according to claim 3, characterized in that said rock is plutonic rock.
6. Prepared according to claim 1 characterized in that 50% to 99% of the particles (d50 to d99) are in the particle size range of 403 to 19426 nanometers (nm).
7. Prepared according to claim 1, characterized in that 90% to 99% of the particles (d90 to d99) are in the particle size range of 5573 to 19426 nanometers (nm).
8. Prepared according to any one of claims 1 to 7, characterized by the following particle size distribution profile: d10: between 132 and 153 nm; d50: between 403 and 516 nm; and d90: between 5573 and 7986 nm.
9. Prepared according to any one of claims 1 to 8, characterized by a specific surface area of 0.5 to 150 m² / g.
10. Prepared according to claim 9, characterized by an average specific surface area of 40 to 70 m² / g.
11. Use of the preparation as defined in any of the claims 1 Petition 870240108404, dated 12 / 19 / 2024, page 21 / 33 2 / 4 to 10 characterized by being for obtaining other preparations of particles or nanoparticles with adjusted rheological properties, adjusted degrees of packing or void fractions, adjusted flowability of the final preparation.
12. Use of the preparation as defined in any one of claims 1 to 10, characterized by being for the preparation of: stable colloidal compositions; steels, metallic and non-metallic alloys, ceramics and / or polymers; composite materials, electronic components, battery cells, energy storage systems, piezoelectric sensors and actuators, solar panels; glasses, glass-ceramics, transparent and translucent materials; catalysts.
13. Process for obtaining rock particles characterized by comprising the steps of: - feeding rock particles to a comminuting equipment selected from: high-energy mill, ball mill and steammill; - adjusting the comminution conditions selected from: - in a high-energy mill: suspend particles to be comminuted in a liquid, at a concentration between 1% and 90% w / w, and stabilize the suspension until a stable colloidal suspension is obtained; place the said suspension and grinding spheres with a diameter selected between 5 µm and 1.3 mm in the grinding chamber; adjust the mill rotation speed between 500 and 4500 rpm; and grind the particles at a temperature below 60 °C; or - in a jet mill with superheated fluid or Steammill, feed particles smaller than 40 micrometers; adjust the rotation of the air classifier between 1000 and 25.000 rpm; adjust the compressed steam pressure between 10 and 100 bar and the temperature between 230 and 360 °C; and - comminute the particles until the desired particle size distribution is obtained.
14. Process according to claim 13 characterized in that the stabilization of the colloidal suspension is achieved by: adjusting the pH of the polar liquid medium to the range between 2 and 13, and optionally adding surfactants; or adding surfactants to the non-polar liquid medium. Petition 870240108404, dated 12 / 19 / 2024, page 22 / 33 3 / 4 15. Process according to claim 13 characterized by further comprising a pre-comminution step of the rock particles before the feeding step to the comminuting equipment, said pre-comminution being carried out until an average particle size of less than 40 micrometers is reached.
16. Process according to claim 15 characterized in that said pre-minution is carried out in a ball mill, disc mill or high-energy mill or in a jet mill.
17. A process according to any one of claims 13 to 16, characterized by comprising the steps of: - feeding a high-energy mill with rock particles, wherein said particles are micrometric; - feeding said mill with a liquid and adjusting the pH in the range between 5 and 10; - feeding said mill with spheres with a diameter selected between 50 µm and 400 µm; - adjusting the rotation speed of the mill between 2000 and 4000 rpm; and - grinding the particles at a temperature below 60 °C until the desired particle size profile is obtained.
18. Process according to claim 17 characterized in that the high-energy mill is of the agitated type and said spheres are selected from: Zirconia, Silicon carbide, alumina, said spheres being optionally stabilized with Yttria or Niobium Pentoxide, or combinations thereof.
19. Process according to claim 13 characterized by the superheated temperature jet mill or Steammill being adjusted with the following parameters: air classifier rotation at 20,000 rpm; compressed steam pressure at 50 bar; and superheated fluid temperature at 280 °C.
20. Product characterized by comprising the particle preparation, as defined in any of claims 1 to 10, and a material selected from metal, non-metal, ceramic, polymer, glass, glass-ceramics or combinations thereof.
21. Product according to claim 20 characterized by being a stable colloidal composition; steels, metallic and non-metallic alloys, composite materials, electronic components, battery cells, energy storage systems, piezoelectric sensors and actuators, solar panels; transparent and translucent materials; catalysts. Petition 870240108404, dated 12 / 19 / 2024, pp. 24 / 33