WO2017061884A1 - Procédé de production d'une poudre de basalte, de fibres de basalte et autres produits façonnés - Google Patents

Procédé de production d'une poudre de basalte, de fibres de basalte et autres produits façonnés Download PDF

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Publication number
WO2017061884A1
WO2017061884A1 PCT/PL2016/000114 PL2016000114W WO2017061884A1 WO 2017061884 A1 WO2017061884 A1 WO 2017061884A1 PL 2016000114 W PL2016000114 W PL 2016000114W WO 2017061884 A1 WO2017061884 A1 WO 2017061884A1
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WIPO (PCT)
Prior art keywords
basalt
water
particles
powder
fibers
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.)
Ceased
Application number
PCT/PL2016/000114
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English (en)
Inventor
Marek Majcher
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.)
Przedsiebiorstwo Budowlano-Montazowe Flisbud Stanislaw Flis
Original Assignee
Przedsiebiorstwo Budowlano-Montazowe Flisbud Stanislaw Flis
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Publication of WO2017061884A1 publication Critical patent/WO2017061884A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B1/00—Preparing the batches
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients
    • C03C1/022—Purification of silica sand or other minerals
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions
    • C03C13/06—Mineral fibres, e.g. slag wool, mineral wool, rock wool
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/042—Electrodes formed of a single material
    • C25B11/043—Carbon, e.g. diamond or graphene
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features

Definitions

  • the present invention relates to a method of manufacturing basalt powder, basalt fibers and other shaped products by melting basalt powder at high temperature to produce malleable basaltic magma.
  • the molten basalt rock has many applications as it is possible to produce basalt fibers or threads from it.
  • Basalt fibers can be produced through different technologies and the obtained products possess various properties. Produced fibers may have a diameter from a few to tens of micrometers, and different applications.
  • Basalt fibers, pure or in combination with other additives are used as raw materials for the production of insulating materials for constructions (i.e. wool available as Rockwooi), or for the manufacture of prefabricated elements reinforced by short (discontinuous) basalt fibers, which play the similar role as glass fibers. Reinforcement mats or bars with addition of multicore basalt thread are also produced and dedicated for the constructions sector.
  • a basalt thread may be a filament (roving) surrounded by segmental yarn from aramid, polyamide or polypropylene epoxidized vegetable oils, or polypropylene or the fabric can be completely woven using only basalt threads. It is also possible to twist multiple filaments of basalt to produce a stronger fabrics/mats, which further constitute the matrix for hardenable resins like epoxy, vinyl or polyester resins.
  • Basalt nonwoven fabrics may also be used for production of various kinds of filters, especially when the filters must operate at high temperatures.
  • basalt is pre-treated, grinded and annealed, and then it is melted at high temperature until liquid state at approx. 1500°C.
  • Various techniques are then applied to produce basalt filaments, fibers or yarns, usually having a diameter of from 10 to 22 am.
  • General information about the use and properties of basalt fibers can be, for example, found in the on-line available publication "Basalt fibers as reinforcement for composites," Van de Velde K., Kiekens P., Van LANGENHOVE L, Department of Textiles, Ghent University, Technologiepark 907, B -9052 Zwijnaarde, Belgium.
  • basalt fiber Compared to glass fiber, basalt fiber has a relatively large content of iron and phosphorus compounds.
  • the object of the present invention is the method of manufacturing basalt powder, basalt fibers and other shaped products, comprising grinding the raw material of basalt and optionally melting the basalt by heating it to a temperature in the range of 1450°C to 1550°C, characterized in that, the raw material of basalt is crushed to obtain a particle size of less than 5 mm, preferably in the range of from 1 to 3 mm, then, the thus obtained powdery raw material is combined with water in a ratio of 5 to 50 liters of water per 100 g of basalt, and obtained suspension is homogenized, processed through further fragmentation and purification in the reaction chamber equipped with electric pulse generator, wherein the water and basalt powder suspension is simultaneously electrolyzed within the same chamber, equipped with at least one carbon based electrode, on which retain basalt impurities, then solid particles of basalt are separated from the water and dried under anaerobic conditions, and then optionally melted in a temperature in the range of 1450°C to 1550°C and optionally basalt fibers, or other
  • Solid basalt particles are separated from the water by filtration or centrifugation, and basalt particles separated from water are dried at a temperature in the range of 300 to 400°C.
  • Dried basalt particles have a very small size, that at least 50% by weight of the particles have the size below 200 ⁇ .
  • dried basalt particles have a content of not more than 1 ppm of iron compounds.
  • the basalt particles are purified by removing 99.9% of the impurities of iron, manganese and phosphorus compounds.
  • the object of the present invention is also using the basalt powder, obtained by the defined above method of preparation of basalt fibers in 3D printing.
  • the method, according to the invention makes basalt fibers production process more economical and reduces energy consumption.
  • Conventional methods of basalt fiber production include additional initial basalt ignition step at even 900°C, which demands huge amounts of energy.
  • the method, according to the invention enables purification of basalt grains (basalt powder) from detrimental impurities, such as iron compounds, usually present in a form of oxides or phosphorus compounds present as phosphates. In the last stage of the method of producing basalt fibers, these impurities have negative impact on the properties of produced basalt fibers. Also, the impurities force long lasting heating until the basaltic magma processing is stable to enable to draw the fiber.
  • basalt fiber for the purpose of this invention should be understood broadly, i.e. it includes or is synonymous with other terms such as the basalt thread, basalt yarn, basalt silk, etc.
  • Grinding of the basalt may be carried out by various known methods, e.g. it may be performed by conical grinding mills, ball mills or electromagnetic mills and other mills, which are adapted to grinding hard minerals.
  • obtained basalt grains size after the grinding process is less than 5 mm, e.g. of 1 to 3 mm.
  • sieves with determined mesh sizes and assure the ability to return the bulk of the raw materia! to be milled again, depending on the needs.
  • the water used in the process. ⁇ according to the invention is preferably ordinary industrial water, which was not subjected to any special treatment.
  • Preferred is the use of chlorinated water, which supports processes occurring in aqueous suspension between the basalt particles, and the water treated by ultrasounds, and in the course of electrolysis.
  • a large excess of water in relation to the basalt is used and it varies from 5 to 50 liters of water per 100 grams of basalt, in particular from 20 to 50 liters of water per 100 grams of basalt, wherein, for the low iron content basalt, water proportion falls the bottom limit of the indicated range.
  • proportion of water in the treated suspension should be the highest, not lower than 5 liters per 1 gram of bounded iron present in the basalt rock.
  • Dry raw material feed and water feed to the reaction chamber is performed periodically to allow saturation of the water with compounds passing from the solid phase to the aqueous phase, while the suspension is exposed to electrical pulses, and to allow the separation of impurities from the aqueous phase to the graphite electrodes.
  • Production of basalt fibers in the last step of the process according to the invention can be performed by any known method which is suitable for spinning of mineral fibers such as basalt fibers.
  • it can be carried out using the spinner, wherein the molten mineral material is spread on the wall of the spinner, wherein the spinner has numerous nozzles with small diameter.
  • the nozzles are used for centrifuging of mineral material at appropriately high temperature. Fibers can be drawn up directing the stream of gas along the wall of the spinner.
  • the nozzles of the spinner can have diameters from 0.1 to 0.7 mm, which allows production of fibers adapted to the needs of a diverse diameter.
  • the molten basalt powder can be used to produce other shapes such as rods or sheets, which are produced in the glass technology, the flotation method may be particularly useful there. Due to some analogies in the processes of basalt and glass processing, we can apply similar methods for the production of basalt shapes i.e. heat treatment (melting dry mineral ingredients).
  • the purified basalt powder obtained through the process according to the invention can be used for production of basalt fibers "in situ" in 3D printers as a fiber used for forming the desired end product.
  • Dry powder basalt fills the developer cartridge in the printer.
  • basalt powder is heated to the desired temperature in the range 1450-1550°C to form basalt yarn.
  • the aqueous basalt suspension was sonicated with use of the pulse generator, as the source of the ultrasounds, which assures further fragmentation of basalt grains. Under the effect of pulses, also some physico-chemical and sonochemical phenomenon occur on the edge of the water-mineral grains phase.
  • electro burst activation technology allows impurities to be separated from basalt grains.
  • the method is energy-efficient, versatile and can be applied to the raw material of various origin, without any pre- treatment.
  • the reaction chamber in which the method according to the invention is carried out, is equipped with a pulse generator.
  • the generator voltage to the discharge is delivered in a form of short pulses with a duration of a few micro- to milliseconds.
  • the excitation and ionization phenomena which both non-linear!y depend on the electric field, are much more intense, in the case of the pulse generator than other plasma technologies.
  • Phenomenon which occur during impulse discharge should be treated as short-term DC discharge, followed by a long period of time without unloading (hereinafter called afterglow), until the next voltage pulse.
  • the short-duration voltage pulse energies of electrons reach much higher values (at a few eV level), than the energy of other plasma particles (less than 0.1 eV).
  • Discharge impulse reactor operates at pressures of 100 Pa, voltage pulses with a peak value of 500 V and a running time of 100 microseconds.
  • the geometrical dimensions of this type of reactor can be relatively large and have a few cubic meters (see Henryka Danuta Stryczewska, Plasma technologies in the energy and environmental engineering, Publishing University of Lublin, Lublin 2009).
  • a reaction chamber with a capacity to process 350 kg of basalt material per hour has been applied.
  • the process is a continuous process.
  • Grinded and purified basalt (basalt micro particles) gravitationally settles down on the bottom part of the reaction chamber and is collected in this place.
  • Basalt raw material feed preferably is carried out from the top of the chamber.
  • the ultrasounds generator is placed on the bottom of the reaction chamber, where the suspension density is high. Electrodes, which retain impurities are placed in the top part of the reaction chamber, where the suspension has a lower density and a higher proportion of water.
  • the basalt grains suspension in water is treated by electric impulses in the reaction chamber, that simultaneously cause the electrolysis and settlement of the basalt contaminants on the electrodes based on carbon.
  • the gases from anions destruction can be emitted from the suspension.
  • not desired components of basalt are separated, which allows to obtain suspension of micro- and nanoparticles of purified basalt, in which 99.9% by weight of any impurities (compounds of iron, phosphorus, manganese) have been eliminated.
  • the reactor is equipped with at least one graphite based electrode, preferably with two, three or four electrodes e.g. titanium-graphite electrodes.
  • the reactor housing acts as an opposite electrode - the anode.
  • Graphite/carbon based electrodes operate on 1 to 3.5 ampere current and the voltage at 500 to 1200 volts.
  • Graphite-based electrodes act periodically in the process and are replaced once worn out.
  • Purified basalt is subjected to filtration or centrifugation, then is dried and calcined at 300-400°C, preferably 350°C in a vacuum furnace in anaerobic conditions; for example, in environment of nitrogen or carbon dioxide. This step of drying the basalt powder may take 15 minutes to 2 hours; for example, 30 minutes or 1 hour.
  • Obtained powdered basalt raw material can be packaged using any available vacuum method, preferably method performed without oxygen.
  • the basalt powder can be further used in goods thermoforming, or as paints, varnishes, protective coatings additive.
  • basalt which needs 3 times shorter residence time in the basaltic magma melting chamber and is purified from iron, phosphates and other pollutants.
  • the method of the invention may also comprise further stages of basalt powder processing e.g. melting it to obtain basaltic magma and then forming products such as fibers or profiles, shaped and molded products, construction elements.
  • basalt powder processing e.g. melting it to obtain basaltic magma and then forming products such as fibers or profiles, shaped and molded products, construction elements.
  • the process energy demand for the method carried out until the final shaped products such as basalt fiber is between 8 to 10 kWh per 1 kg of basalt.
  • Basalt magma is obtained in a standard temp, approx. 1500°C, however, required heating time may be reduced to 1 -2 hours, or about one hour.
  • Obtained purified basalt powder particles have powdered (micronized) micron size below 20 ⁇ , and below 100 ⁇ and even below 10 ⁇ e.g. 50% of the particles of obtained powder are basalt nanoparticles having size less than 200 ⁇ or even 90% of the particles of obtained powder have size below 200 ⁇ .
  • basaltic magma When basaltic magma is used to produce molded products, the magma temperature is then maintained within its area of operation.
  • Thermal forming facilities can produce various molded products, fittings, shapes, for example: rods, granules, threads, plates, spheres, shapes like channel section, C- profiles, T-profiles etc. Obtained through the applied method according to the invention, processed and purified basalt grains are also subject for further heat treatment and/or chemical treatment in the anti-corrosion protecting means production process, e.g. paints and varnishes, which, due to their properties are the best among all the currently used anti-corrosion agents.
  • Basalt anticorrosive coatings are resistant to all aggressive factors including alkalis and acids, except hydrofluoric acid or hydro-acidic acids, which do not contain oxygen. Such coatings can also be used as fire protection, sound and thermal insulation as well as fire resistant cable sheaths and other.
  • Basalt with a high iron compounds content (9% wt.) was grinded in a cone mill to obtain particles with size of 1-3 mm.
  • Grinded material in a powder form is a reactor feed in, the reactor is equipped with electrical impulses reactor wherein the impulse discharges need to be supplied with voltage of 2 kV, a pulse width of about 10 microseconds and a repetition rate of 200 Hz.
  • Quoted parameters allow to generate impulses up to 1 A and respectively up to 2 kW.
  • the basalt powder purification process was carried out in presence of water using a ratio of 5 I of water per 10 grams of basalt grains.
  • the reactor was equipped with three titanium and graphite electrodes. The process was conducted in 1 hour, the 350 kg of basalt were treated in this time and 99.9% by weight of impurities (iron, manganese and phosphorus) of obtained product were removed.
  • Basalt powder was separated from the water using filtration method, obtained paste was dried in nitrogen environment at 350°C for 1 hour. Above 60% of obtained dry basalt particles had size below 200 ⁇ . Dry basa!t powder was vacuum packed in plastic bags.
  • the dry powder obtained according to example 1 was melted at 1450- 1550°C and processed for 1 hour in a spinner dedicated for mineral fibers manufacture.
  • the basalt yarn have been manufactured.
  • Example 3 The process according to Example 1 was performed. Basalt powder with low content of iron (4% by weight) was processed. 2 liters of water per 10 grams of basalt grains were used in the process of making basalt water suspension. Obtained basalt powder has properties as described in example 1. The dried powder was stored with no air access and then used in a 3D printer as a cartridge filling calling, desired high hardness products were obtained.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Fibers (AREA)

Abstract

La présente invention concerne le procédé de production d'une poudre de basalte, de fibres de basalte et autres produits façonnés, comprenant le broyage d'un matériau de basalte brut et éventuellement la fusion du basalte par chauffage jusqu'à une température dans la plage de 1450 à 1550°C, le procédé étant caractérisé en ce que le matériau de basalte brut est concassé pour obtenir une taille de particule inférieure à 5 mm, de préférence dans la plage de 1 à 3 mm, puis le matériau brut pulvérulent ainsi obtenu est combiné à de l'eau dans un rapport de 5 à 50 litres d'eau pour 100 g de basalte, et la suspension obtenue est homogénéisée, traitée par fragmentation supplémentaire et purification dans la chambre de réaction équipée d'un générateur d'impulsions électriques, la suspension d'eau et de poudre de basalte étant simultanément électrolysée dans la même chambre, équipée d'au moins une électrode à base de carbone qui retient les impuretés du basalte, puis les particules solides de basalte sont séparées de l'eau et séchées dans des conditions anaérobies, et éventuellement fondues à une température dans la plage de 1450 à 1550°C et éventuellement des fibres de basalte, ou autres produits façonnés sont préparés.
PCT/PL2016/000114 2015-10-09 2016-10-07 Procédé de production d'une poudre de basalte, de fibres de basalte et autres produits façonnés Ceased WO2017061884A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PL414330A PL414330A1 (pl) 2015-10-09 2015-10-09 Sposób wytwarzania proszku bazaltowego, włókna bazaltowego i innych wyrobów kształtowych
PLP.414330 2015-10-09

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WO2017061884A1 true WO2017061884A1 (fr) 2017-04-13

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201800010449A1 (it) * 2018-11-20 2020-05-20 Basalti Orvieto S R L Con Unico Socio Corroborante minerale per uso fogliare
WO2023047432A1 (fr) * 2021-09-21 2023-03-30 The University Of Jordan Composition de béton et son procédé de préparation

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0525816A1 (fr) 1991-08-02 1993-02-03 Isover Saint-Gobain Procédé et appareil pour la fabrication de la laine minérale et laine minérale ainsi produite
EP0583792A1 (fr) 1992-08-20 1994-02-23 Isover Saint-Gobain Procédé et appareil de fabrication de la laine minérale et laine minérale ainsi produite
US5352260A (en) 1993-09-16 1994-10-04 Industrial Fibers, Inc. Manufacture of mineral fiber
EP0957068A1 (fr) 1996-11-19 1999-11-17 Damanov, Gennady Panteleimonovich Procede de fabrication de fibres de basalte et dispositif prevu a cet effet
KR20020081613A (ko) 2001-04-19 2002-10-30 하판석 현무암 섬유 제조장치
WO2014169312A1 (fr) * 2013-04-19 2014-10-23 Alexander Schneider Centrale d'accumulation d'air comprimé comprenant une pompe à induction et procédé de fabrication de cette centrale d'accumulation d'air comprimé
WO2015057575A1 (fr) * 2013-10-15 2015-04-23 Halliburton Energy Services, Inc. Procédés pour séparer des impuretés de minéraux industriels à l'aide d'une électrocoagulation

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0525816A1 (fr) 1991-08-02 1993-02-03 Isover Saint-Gobain Procédé et appareil pour la fabrication de la laine minérale et laine minérale ainsi produite
EP0583792A1 (fr) 1992-08-20 1994-02-23 Isover Saint-Gobain Procédé et appareil de fabrication de la laine minérale et laine minérale ainsi produite
US5352260A (en) 1993-09-16 1994-10-04 Industrial Fibers, Inc. Manufacture of mineral fiber
EP0957068A1 (fr) 1996-11-19 1999-11-17 Damanov, Gennady Panteleimonovich Procede de fabrication de fibres de basalte et dispositif prevu a cet effet
KR20020081613A (ko) 2001-04-19 2002-10-30 하판석 현무암 섬유 제조장치
WO2014169312A1 (fr) * 2013-04-19 2014-10-23 Alexander Schneider Centrale d'accumulation d'air comprimé comprenant une pompe à induction et procédé de fabrication de cette centrale d'accumulation d'air comprimé
WO2015057575A1 (fr) * 2013-10-15 2015-04-23 Halliburton Energy Services, Inc. Procédés pour séparer des impuretés de minéraux industriels à l'aide d'une électrocoagulation

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
BETHANY C. GROSS ET AL: "Evaluation of 3D Printing and Its Potential Impact on Biotechnology and the Chemical Sciences", ANALYTICAL CHEMISTRY, vol. 86, no. 7, 16 January 2014 (2014-01-16), US, pages 3240 - 3253, XP055333027, ISSN: 0003-2700, DOI: 10.1021/ac403397r *
HENRYKA DANUTA STRYCZEWSKA, PLASMA TECHNOLOGIES IN THE ENERGY AND ENVIRONMENTAL ENGINEERING, 2009
VAN DE VELDE K.; KIEKENS P.; VAN LANGENHOVE L., BASALT FIBERS AS REINFORCEMENT FOR COMPOSITES

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201800010449A1 (it) * 2018-11-20 2020-05-20 Basalti Orvieto S R L Con Unico Socio Corroborante minerale per uso fogliare
WO2023047432A1 (fr) * 2021-09-21 2023-03-30 The University Of Jordan Composition de béton et son procédé de préparation

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