WO2024014991A1 - Procédé de production de nanoparticules isolées sur la surface d'une base de liaison - Google Patents

Procédé de production de nanoparticules isolées sur la surface d'une base de liaison Download PDF

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Publication number
WO2024014991A1
WO2024014991A1 PCT/RU2023/050164 RU2023050164W WO2024014991A1 WO 2024014991 A1 WO2024014991 A1 WO 2024014991A1 RU 2023050164 W RU2023050164 W RU 2023050164W WO 2024014991 A1 WO2024014991 A1 WO 2024014991A1
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WO
WIPO (PCT)
Prior art keywords
nanomaterial
particles
cyclone separator
nanoparticles
unit
Prior art date
Application number
PCT/RU2023/050164
Other languages
English (en)
Russian (ru)
Inventor
Алексей Николаевич ГОЛДАЕВ
Original Assignee
Алексей Николаевич ГОЛДАЕВ
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
Priority claimed from RU2022118774A external-priority patent/RU2788886C1/ru
Application filed by Алексей Николаевич ГОЛДАЕВ filed Critical Алексей Николаевич ГОЛДАЕВ
Publication of WO2024014991A1 publication Critical patent/WO2024014991A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
    • B01D45/12—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/30—Mixing gases with solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/06—Jet mills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/06—Selection or use of additives to aid disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
    • B02C23/10—Separating or sorting of material, associated with crushing or disintegrating with separator arranged in discharge path of crushing or disintegrating zone
    • B02C23/12—Separating or sorting of material, associated with crushing or disintegrating with separator arranged in discharge path of crushing or disintegrating zone with return of oversize material to crushing or disintegrating zone
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
    • B02C23/14—Separating or sorting of material, associated with crushing or disintegrating with more than one separator
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/152—Fullerenes
    • C01B32/154—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation

Definitions

  • the invention relates to the field of nanotechnology and can be used to obtain monodisperse nanostructures, in particular, carbon nanotubes, fullerenes, graphene, etc., as well as composites based on them.
  • a prerequisite for the creation of the invention is the need to obtain uniformly distributed single (primary) nanoparticles, for the purpose of subsequent fixation on the surface of a binding layer, for example, polymer particles (microdroplets of wax, or another polymer, or another substance or composite, applicable for the deposition of nano-sized particles on its surface) or surfaces of tapes, threads, fibers, fabrics and other forms.
  • a binding layer for example, polymer particles (microdroplets of wax, or another polymer, or another substance or composite, applicable for the deposition of nano-sized particles on its surface) or surfaces of tapes, threads, fibers, fabrics and other forms.
  • the main problem in obtaining such single nanoparticles is the tendency of dispersed nano-sized structures to reconnect with each other and enlarge (aggregation and agglomeration). If these nanostructures are not fixed in time and conditions for their preservation in a separated state are not created, the quality of the target product is significantly reduced.
  • a method for dispersing carbon nanomaterial comprising introducing a flow of bulk particles in a first inert gas into the evaporation chamber, maintaining the evaporation chamber at a temperature sufficient to evaporate the bulk particles, introducing evaporated particles from the evaporation chamber into a rarefaction chamber, introducing a flow of a second inert gas into the rarefaction chamber through a rarefaction hole in the rarefaction chamber, sufficient to eject the bulk material from the outlet, thereby condensing the bulk material into single particles in a gas stream of sufficient volume to prevent agglomeration of single particles, while the larger particles remaining in the vacuum chamber (aggregates and agglomerates) are pumped out by a pump.
  • the main disadvantages of the known technical solution are the complexity and low efficiency of the technological process, due to the lack of further conservation of selected single particles in a separated state, which leads to their further enlargement and agglomeration, the high probability of larger particles passing through the outlet of the chamber, as well as the need to re-introduce dispersion system for large particles pumped out by a pump.
  • the known technical solution assumes the presence of waste in the form of agglomerated and aggregated nanomaterial particles deposited on the inner surface of the separator, subject to subsequent mechanical extraction for the purpose of reintroduction into the system, which significantly complicates the entire technological process. There is also no provision for further preservation of selected single particles in a separated state, which leads to their further enlargement and agglomeration. In this case, making the entire lateral inner surface of the cyclone separator cone-shaped does not provide effective separation of nanomaterial at the outlet, since there is a possibility of pushing both small and larger particles of nanomaterial into the hole of the vertical pipe.
  • the documents WO 2004043855 (A2) and CA 2983470 (A1) disclose methods for producing a nanomaterial with the fixation of carbon nanoparticles on the surface of a binder polymer, by depositing carbon nanoparticles on the surface with aerosol droplets from a melt of the polymer, after which microdroplets of the polymer, powdered with carbon nanoparticles, solidify and are selected as a finished fraction, in particular by sedimentation at the bottom of a cyclone (according to patent CA 2983470 (A1)).
  • the proposed invention solves the problem of creating a technology for separating single nanoparticles from agglomerates and combined nanostructures - aggregates (for example, single-walled nanotubes twisted into a bundle), which makes it possible to simplify the technological process itself through the use of a closed cycle for separating single nanoparticles, eliminating the formation of waste in the form of agglomerated and aggregated particles , and at the same time improve the quality of the target product through cyclic action on the nanomaterial at the stages of dispersion and further formation of finished nanostructures by fixing dispersed particles on the surface of the binder material in order to prevent their re-agglomeration.
  • the problem is solved by proposing a method for producing single nanoparticles dispersed from bundles and entangled agglomerates of nanoparticles on the surface of the binder base, which includes supplying bulk nanomaterial to a nanoparticle dispersion unit in a compressed gas flow, ensuring the primary movement of the nanomaterial through the first bypass, passing the resulting dispersion into the first cyclone separator for separating dispersed single particles from the remaining aggregated and agglomerated ones due to the effect of gravity and centrifugal forces on nanomaterial particles, sedimentation of aggregated and agglomerated particles with their subsequent transfer back to the said dispersion unit to repeat the dispersion cycle and subsequent separation of single nanoparticles from the remaining aggregated ones and agglomerated, selection of dispersed single nanoparticles separated by an ascending gas flow from the first cyclone separator into the central channel of the block forming the reaction zone for deposition of individual particles of nanomaterial on the surface of the binder base, supply of the formed composite material to the second
  • the dispersion unit at the entrance of the dispersion unit to the bulk nanomaterial, it can be provided for at least sequential exposure of the re-introduced cascade of flat-slit nozzles to a compressed gas flow in the direction codirected with the primary flow movement, further passage of the resulting dispersion through the Laval nozzle with subsequent exposure to ultrasonic vibrations. , and at the exit from the dispersion unit - by a re-introduced cascade of flat-slot nozzles with a flow of compressed gas in the direction co-directed with the primary flow movement.
  • Separation of the formed composite material from individual particles selected by an ascending gas flow that have not had time to attach to the surface of the binder base can be carried out due to the effect of gravitational and centrifugal forces on individual particles and the composite material.
  • the problem is also solved by an installation that implements the above method, consisting of interconnected recirculation circuits, the first of which includes: a pipe for supplying bulk nanomaterial in a compressed gas flow through a bypass into a nanoparticle dispersion unit, the outlet pipe of which is connected to the inlet pipe of the first cyclone separator, located in its upper cylindrical part, for the passage of the resulting dispersion of single, aggregated and agglomerated particles of nanomaterial, while at the base of the lower conical part, the first cyclone separator is connected to the supply pipe of bulk nanomaterial for the passage of aggregated and agglomerated particles deposited in the cyclone separator Due to the effect of gravitational and centrifugal forces on nanomaterial particles, the second recirculation circuit includes: a unit for deposition of individual particles of nanomaterial onto a binder base, connected by the inlet part to the vertical outlet pipe of the first cyclone separator, for supplying individual particles dispersed therein separated into the reaction zone formed a central channel
  • the dispersion unit may include sequentially installed at least an inlet pipe with a cascade of flat-slit injectors for compressed gas, a Laval nozzle, an ultrasonic emitter, and an outlet pipe with a cascade of flat-slit injectors for compressed gas.
  • FIG. 1 is a schematic illustration of a plant for producing single dispersed nanoparticles according to a preferred embodiment
  • FIG. 2 is a schematic representation of a first cyclone separator;
  • FIG. 3 schematic representation of a block for forming a composite material according to option a);
  • FIG. 4 schematic representation of the block for forming a composite material according to the first alternative option b);
  • FIG. 5 schematic representation of a block for forming a composite material according to the second alternative option b);
  • FIG. 6 schematic representation of a block for forming a composite material according to option c);
  • FIG. 8 micrograph of agglomerated nanoparticles using single-walled nanotubes as an example.
  • the proposed method can be implemented in an installation for dispersing nanoparticles, shown in Fig. 1.
  • the installation consists of two interconnected recirculation circuits.
  • the first recirculation circuit consists of a loading gate (1) installed on the pipe (2) with flat-slot nozzles (3), a nanomaterial particle dispersion unit (4) connected by a bypass to the pipe (2), as well as the first cyclone separator (13) connected to the upper cylindrical part (33) with a block (4), and at the base of the lower conical part (34) - with a pipe (2).
  • Block (4) in the preferred embodiment is a complex of the following sequential devices for deagglomeration of nanomaterial particles: inlet pipe (7) with a cascade of flat-slit nozzles (6), Laval nozzle (convergent-divergent nozzle) (8) with nozzle (30), ultrasonic emitter (9), output pipe (10) with a cascade of flat-slot nozzles (11), connected to the inlet pipe (12) located in the cylindrical part (33) of the cyclone separator (13) (Fig. 2).
  • the second recirculation circuit consists of a unit for separating individual particles of nanomaterial (16), connected by the inlet part to the vertical outlet pipe (14) of the block (13) and made with a central channel (31) forming the reaction zone and a device for forming a composite material, as well as a second cyclone separator (24) and a bypass (29) .
  • the cyclone separator (24) is similar in design to the cyclone separator (13), has at the base a storage tank (26) with a filter valve (27) for removing the gas flow, which is connected to the conical part through the lower pipe (25), and in the cylindrical area part of the cyclone separator (24) is connected by an inlet pipe (32) to the outlet part of the block (16).
  • the bypass (29) is connected on one side to the inlet part of the block (16), and on the other - to the vertical outlet pipe (28) of the cyclone separator (24).
  • the method for producing dispersed single nanoparticles according to FIG. 1 is carried out as follows.
  • a portion of bulk nanomaterial is metered or automatically fed into the nozzle (2), in which one or more nozzles (3) are located, directed along the axis of the nozzle towards the block (4).
  • pulses of compressed air move the nanomaterial and feed it through the bypass (5) into the primary dispersion zone of the block (4), at the entrance of which several flat-slit nozzles (6) are located opposite each other, directed at an angle to the axis of the nozzle (7) in the side aligned with the movement of the flow through which the compressed gas is supplied.
  • a high degree of turbulence occurs at the line of flow convergence, which activates primary dispersion.
  • the number of pairs of injectors (6) can be several and form a cascade.
  • the mixture of gas and nanomaterial having acquired a certain speed, enters the Laval nozzle (8), where the gas flow is accelerated many times and, at the exit from the nozzle, passes through the cavitation zone, where the dispersion process intensifies. This is where the ultrasonic emitter (9), the ultrasonic effect of which gives the nanoparticles additional mobility.
  • the gas flow passes through a pipe (10) with a cascade of flat-slit nozzles (11), where the nanomaterial is exposed to maximum impact from aggregated particles, for example, bundles of single-walled nanotubes (Fig.
  • nanomaterial particles agglomerates, catalyst, foreign inclusions
  • a slowed gas flow that has changed the direction of their movement move to the center of rotation and in an upward flow are carried out into a vertical pipe (14).
  • Aggregates and agglomerates through the lower pipe (15) again enter the space of the pipe (2) in front of the loading gate (1) into the zone of action of the nozzles (3), which ensure the primary movement of the nanomaterial, and then again find themselves in the dispersion zone of the block (4).
  • the type of gas (viscosity), temperature, pressure and entry speed into the cyclone separator are selected so that only the lightest (single) nanoparticles are retained in the upward flow.
  • the mixture of gas and individual particles through the pipe (14) of the cyclone separator (13) enters the reaction zone of the block (16), which can be organized in several ways: a) A spray nozzle is located in the channel of the reaction zone of the block (16)
  • the device has a receiving port (21) and a drawing mechanism with unwinders (22) and winders (23), which ensures constant movement of the adhesive material and adjustable exposure time in the flow of nanoparticles.
  • nanoparticles that have not had time to attach to the surface of the adhesive material are, by analogy with options a) and b), removed from the cyclone separator by a gas flow and returned through the bypass (29) to the deposition reaction zone.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • Toxicology (AREA)
  • Health & Medical Sciences (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention se rapporte au domaine de nanotechnologies et peut être utilisée pour produire des nanostructures monodispersées, notamment des nanoparticules identiques isolées à partir de brins et d'agglomérats entremêlés de nanoparticules sur la surface d'une base de liaison. Ce procédé consiste à envoyer un nanomatériau en vrac vers une unité de dispersion (4) de nanoparticules dans un flux de gaz comprimé assurant un déplacement primaire du nanomatériau à travers une dérivation (5), à faire passer la dispersion obtenue dans un premier séparateur à cyclone (13) afin de déparer les particules isolées dispersées des particules restantes agrégées et agglomérées du fait de l'action sur les particules de nanomatériau de la force de gravité et des forces centrifuges, déposer les particules agrégées et agglomérées avant de les renvoyer vers ladite unité de dispersion (4). Les nanoparticules isolées dispersées sont utilisées pour former du matériau composite dans l'unité (16) grâce à leur alimentation dans le canal central (31) de la zone de réaction pour leur sédimentation à la surface de la base de liaison. Dans un second séparateur à cyclone (24) le matériau composite formé est séparé des nanoparticules résiduelles qui sont sélectionnées par un flux de gaz montant et retournées dans la zone de réaction de l'unité de déposition (16). On extrait le produit composite via un conduit inférieur (25) et un récipient d'accumulation (26). Grâce au cycle fermé de séparation il est possible de simplifier le processus industriel et d'empêcher une nouvelle agglomération de nanoparticules.
PCT/RU2023/050164 2022-07-09 2023-07-04 Procédé de production de nanoparticules isolées sur la surface d'une base de liaison WO2024014991A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2022118774 2022-07-09
RU2022118774A RU2788886C1 (ru) 2022-07-09 Способ получения на поверхности связующей основы одиночных наночастиц, диспергированных из жгутов и спутанных агломератов наночастиц, и установка для его реализации

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WO2024014991A1 true WO2024014991A1 (fr) 2024-01-18

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004043855A2 (fr) * 2002-11-12 2004-05-27 Microcoating Technologies, Inc. Matieres carbonees
US20050123467A1 (en) * 2003-12-03 2005-06-09 Avetik Harutyunyan Systems and methods for production of carbon nanostructures
WO2007103256A2 (fr) * 2006-03-03 2007-09-13 Battelle Memorial Institute Procede et instrument pour generer de fortes concentrations massiques de nanoparticules.
RU2592306C2 (ru) * 2011-04-28 2016-07-20 Экомин С.Р.Л. Способ и устройство для сепарации частиц

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004043855A2 (fr) * 2002-11-12 2004-05-27 Microcoating Technologies, Inc. Matieres carbonees
US20050123467A1 (en) * 2003-12-03 2005-06-09 Avetik Harutyunyan Systems and methods for production of carbon nanostructures
WO2007103256A2 (fr) * 2006-03-03 2007-09-13 Battelle Memorial Institute Procede et instrument pour generer de fortes concentrations massiques de nanoparticules.
RU2592306C2 (ru) * 2011-04-28 2016-07-20 Экомин С.Р.Л. Способ и устройство для сепарации частиц

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