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WO2025097577A1 - Procédé et dispositif de préparation de type à écoulement pour nanomatériau - Google Patents

Procédé et dispositif de préparation de type à écoulement pour nanomatériau Download PDF

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Publication number
WO2025097577A1
WO2025097577A1 PCT/CN2023/142681 CN2023142681W WO2025097577A1 WO 2025097577 A1 WO2025097577 A1 WO 2025097577A1 CN 2023142681 W CN2023142681 W CN 2023142681W WO 2025097577 A1 WO2025097577 A1 WO 2025097577A1
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WO
WIPO (PCT)
Prior art keywords
solution
reaction
container
collector
micro
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
PCT/CN2023/142681
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English (en)
Chinese (zh)
Inventor
杨冠南
何伟伟
笪贤豪
崔成强
张昱
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.)
Guangdong University of Technology
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Guangdong University of Technology
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Filing date
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Application filed by Guangdong University of Technology filed Critical Guangdong University of Technology
Publication of WO2025097577A1 publication Critical patent/WO2025097577A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1856—Stationary reactors having moving elements inside placed in parallel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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

Definitions

  • the present invention relates to the field of nano material technology preparation, and in particular to a flow-type preparation method and device for nano material.
  • micro-nano materials is a new system constructed or created according to certain rules based on nanoscale material units, including nano-array systems, mesoporous assembly systems, and thin film mosaic systems.
  • nanoscale material units including nano-array systems, mesoporous assembly systems, and thin film mosaic systems.
  • micro-nano materials generally refer to materials with sizes at the micron and nanometer levels, which have unique physical, chemical and biological properties.
  • micro-nano materials can be single crystals, polycrystalline or amorphous structures.
  • micro-nano materials include nanoparticles, nanowires, nanosheets, nanotubes, etc., and their size will not only affect the electronic, optical, thermal and other properties of micro-nano materials, but also their oxidation and reduction reactions.
  • the core-shell structure of core-shell materials is an ordered assembly structure formed by one micro-nano material encapsulating another material through chemical bonds or other forces.
  • the surface properties of the core particles can be tailored, the surface charge, functional groups and reaction characteristics of the core can be changed, and the stability and dispersibility of the core can be improved. Its unique structural characteristics can give the material different properties. It plays an important role in catalysis, photocatalysis, batteries, gas storage and separation.
  • the commonly used preparation methods of existing nanometal particles include chemical reduction, vapor deposition, hydrothermal synthesis, sol-gel method, photochemical method, microemulsion method, template method, phase transfer method, ultrasonic method, etc.
  • the methods such as the radiation method are easily affected by the reaction conditions during the preparation process, and the reaction process is difficult to accurately control.
  • its morphology is usually restricted by the raw material container or the template during synthesis, and there are problems such as difficulty in continuous and large-scale preparation. These problems have hindered the mass production of nanomaterials.
  • the present invention provides a flow-type preparation method and device for nanomaterials.
  • an embodiment of the present invention provides a continuous preparation method of nanomaterials, which comprises:
  • Step S4 drawing the unreacted complete solution from the solution collector through a reflux pipe and returning it to the reactant container;
  • the micro-nano metal solution comprises micro-nano metal particles and a solvent.
  • the micro-nano metal particles are bidirectional metal particles.
  • the solvent includes deionized water and an organic solvent
  • the organic solvent is an alcohol organic solvent or a ketone organic solvent.
  • the flow rate of the metal ion solution and the micro-nano metal solution flowing into the reaction channel is 4:1 or 1:1 or 2:1.
  • the reaction channel is controlled by applying any one of ultrasound, ultraviolet rays and high temperature to the metal ion solution and the micro-nano metal solution, so that the metal ion solution and the micro-nano metal solution are fully contacted and undergo a displacement reaction to form a reaction mixed solution.
  • An embodiment of the present invention also provides a continuous preparation device for nanomaterials, including a reactant container, a particle collector arranged relative to the reactant container, a reaction channel connected to both the reactant container and the particle collector, a solution collector connected to the particle collector, and a reflux mechanism connected to both the solution collector and the reactant container.
  • the reactant container includes a first reaction container, a first replenishing channel and a first reflux port arranged on two opposite sides of the first reaction container, a second reaction container spaced apart from the first reaction container, a second replenishing channel and a second reflux port arranged on two opposite sides of the second reaction container, and a connecting pipe connected to the bottom of both the first reaction container and the second reaction container.
  • the reaction channel comprises a water bath ultrasonic container located between the connecting pipe and the particle collector and a hollow pipe located in the water bath ultrasonic container, one end of the hollow pipe is connected to the connecting pipe, and the other end of the hollow pipe is connected to the particle collector; the shape of the hollow pipe is linear or spiral.
  • the particle collector includes a processing mechanism connected to one end of the hollow pipe away from the connecting pipe and a particle collecting mechanism detachably connected to the processing mechanism, the solution collector is connected to the particle collecting mechanism, and the reflux mechanism is simultaneously connected to the solution collector, the first reflux port and the second reflux port; the processing mechanism is a filter and/or a centrifuge.
  • the metal ion solution and the micro-nano metal solution undergo a replacement reaction in the reaction channel under the setting of the communicating vessel principle to form a reaction mixture solution, and the reaction mixture solution includes a completely reacted solution and an unreacted solution.
  • the reaction mixture solution then flows into a particle collector, and the completely reacted solution forms the required nanomaterial particles to be adsorbed in the particle collector; the unreacted solution flows into the solution collector, and the reflux mechanism extracts the unreacted solution in the solution collector, and the micro-nano metal solution and the metal ion solution in the unreacted solution are correspondingly refluxed into the corresponding reactant containers, and then the nanomaterial particles in the particle collector are collected.
  • the flow-type preparation method and device of nanomaterials provided by the present invention realize large-scale flow-type continuous production of nanomaterial particles, and can directly collect the completely reacted particles, effectively improving production efficiency and output, and is particularly suitable for the industrial field. It has good industrialization prospects.
  • FIG1 is a schematic flow diagram of a flow-type preparation method of a nanomaterial according to the present invention.
  • FIG2 is a schematic structural diagram of a flow-type preparation device for nanomaterials according to the present invention.
  • FIG3 is a schematic structural diagram of another embodiment of a flow-type preparation device for nanomaterials according to the present invention.
  • the present invention provides a flow-type preparation method of nanomaterials, comprising:
  • Step S1 placing one or more metal ion solutions and micro-nano metal solutions in a reactant container;
  • Step S2 respectively controlling the metal ion solution and the micro-nano metal solution to flow into the reaction channel at a specific flow rate at the same time, so that the metal ion solution and the micro-nano metal solution are fully in contact and undergo a replacement reaction to form a reaction mixed solution, wherein the reaction mixed solution includes a completely reacted solution and an unreacted completely solution;
  • Step S3 controlling the completely reacted solution and the unreacted completely reacted solution to flow into a particle collector and a solution collector respectively;
  • Step S4 drawing the unreacted complete solution from the solution collector through a reflux pipe and returning it to the reactant container;
  • Step S5 looping the process from step S1 to step S4.
  • the micro-nano metal solution includes micro-nano metal particles and a solvent, wherein the micro-nano metal particles are bidirectional metal particles, such as copper particles, antimony particles, zinc particles and nickel particles.
  • the solvent includes deionized water and an organic solvent, and the organic solvent is an alcohol organic solvent or a ketone organic solvent.
  • the flow rate of the metal ion solution and the micro-nano metal solution flowing into the reaction channel is 4:1 or 1:1 or 2:1.
  • the specific flow rate is set according to different reaction solutions. Different flow rate ratios, for example, the reactant containers are used to hold the solution containing copper salt after pretreatment and the reducing agent ascorbic acid and the protective agent polyvinyl pyrrolidone K30 to form a reduction system. Through the principle of communicating vessels, it can generally be determined according to specific experimental requirements and reaction conditions. The flow rate ratio can be selected as 1:1 or 2:1. If the reactant containers are used to hold silver ammonia solution and nano copper particles containing ethanol solution, the flow rates on both sides are controlled to 4:1 through the principle of communicating vessels.
  • the reaction channel is controlled by applying any one of ultrasound, ultraviolet rays and high temperature to the metal ion solution and the micro-nano metal solution, so that the metal ion solution and the micro-nano metal solution can fully contact each other to undergo a replacement reaction.
  • a flow-type preparation device 100 of nanomaterials includes a reactant container 1, a particle collector 2 arranged relatively to the reactant container 1, a reaction channel 3 connected to both the reactant container 1 and the particle collector 2, a solution collector 4 connected to the particle collector 2, and a reflux mechanism 5 connected to both the solution collector 4 and the reactant container 1.
  • the reactant container 1 can contain liquid or solid-liquid mixture.
  • the reactant container 1 is connected to the reaction channel 3, and the solution stored in the reactant container 1 will flow into the reaction channel 3 at the same time or enter the reaction channel 3 in sequence according to the set sequence.
  • the end of the reaction channel 3 is connected to the particle collector 2.
  • the reactant container 1 includes a first reaction container 11, a first replenishing channel 12 and a first reflux port 13 arranged on two opposite sides of the first reaction container 11, a second reaction container 14 spaced apart from the first reaction container 11, a second replenishing channel 15 and a second reflux port 16 arranged on two opposite sides of the second reaction container 14, and a connecting pipe 17 connected to the bottom of both the first reaction container 11 and the second reaction container 14.
  • the reaction container is provided with two, namely a first reaction container 11 and a second reaction container 12.
  • the reaction container 14 is not limited thereto, and its specific number can be adjusted according to actual conditions, and the reaction container can contain liquid or solid-liquid mixture.
  • the temperature of the reaction solution can be controlled in the reaction container and stirring can be applied to make the reaction solution uniform; at the same time, the first reaction container 11 and the second reaction container 1 are respectively provided with a first supplementary channel 12 and a second supplementary channel 15 on the periphery thereof, so that the reactants can be supplemented in time and quickly to avoid the phenomenon of insufficient reactants.
  • the reaction channel 3 includes a water bath ultrasonic container 31 located between the connecting pipe 17 and the particle collector 4 and a hollow pipe 32 located in the water bath ultrasonic container 31, one end of the hollow pipe 32 is connected to the connecting pipe 17, and the other end of the hollow pipe 32 is connected to the particle collector 4.
  • the shape of the hollow pipe 32 is linear or spiral, and in order to more conveniently control the flow rate of the reaction solution in the hollow pipe 32, a flow rate control valve can be added to the hollow pipe 32.
  • the water bath ultrasonic container 31 contains an aqueous solution, and the hollow pipe 32 is partially immersed in the aqueous solution contained in the water bath ultrasonic container 31, and the water bath ultrasonic container 31 can apply ultrasound or temperature control to the hollow pipe 32 to promote the metal ion solution to fully contact with the micro-nano metal solution to cause a replacement reaction.
  • the particle collector 2 includes a processing mechanism 21 connected to one end of the hollow pipe 32 away from the connecting pipe 17 and a particle collecting mechanism 22 that is detachably connected to the processing mechanism 21, the solution collector 4 is connected to the particle collecting mechanism 22, and the reflux mechanism 5 is simultaneously connected to the solution collector 4, the first reflux port 13 and the second reflux port 16.
  • the number of the particle collecting mechanism 22 can be one or more, and is not limited thereto.
  • the processing mechanism 21 is a suction filter and/or a centrifuge. If the processing mechanism 21 is a suction filter, the nano material particles are deposited in the particle collecting mechanism 22, thereby achieving collection; if the processing mechanism 21 is a centrifuge, the nano material particles are deposited in the inner side wall of the particle collecting mechanism 22, thereby achieving collection.
  • the particle collection mechanism 22 and the processing mechanism 21 form a detachable connection, which is convenient for changing different collection modes to meet different collection needs.
  • the collected particles can also be removed by disassembly, which reduces time cost and improves production efficiency.
  • the flow-type preparation device 100 of nanomaterials provided by the present invention can also disassemble the solution collector 4 and the reflux mechanism 5, and can still realize the large-scale flow-type continuous production of the above-mentioned nanomaterial particles.
  • the metal ion solution and the micro-nano metal solution undergo a replacement reaction in the reaction channel under the setting of the communicating vessel principle to form a reaction mixed solution
  • the reaction mixed solution includes a reaction complete solution and an unreacted complete solution
  • the reaction mixed solution flows into the particle collector, and the reaction complete solution forms the required nanomaterial particles to be adsorbed in the particle collector;
  • the unreacted solution flows into the solution collector, the reflux mechanism extracts the unreacted solution in the solution collector, and the micro-nano metal solution and the metal ion solution in the unreacted solution are correspondingly refluxed into the corresponding reactant container, and then the nanomaterial particles in the particle collector are collected.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un procédé de préparation en continu de type à écoulement pour un nanomatériau, comprenant : étape S1, placer une solution d'ions métalliques et une solution métallique à l'échelle micro-nanométrique dans un contenant de réactif ; étape S2, commander séparément la solution d'ions métalliques et la solution métallique à l'échelle micro-nanométrique afin qu'elles s'écoulent simultanément dans un canal de réaction à un débit spécifique, de telle sorte que les deux solutions soient en contact complet l'une avec l'autre et subissent une réaction de déplacement pour former une solution de réaction mélangée, la solution de réaction mélangée comprenant une solution de réaction complète et une solution de réaction incomplète ; étape S3, commander la solution de réaction complète et la solution de réaction incomplète afin qu'elles s'écoulent respectivement dans un collecteur de particules et un collecteur de solution ; étape S4, extraire la solution de réaction incomplète du collecteur de solution au moyen d'un conduit de retour pour permettre à celle-ci de refluer dans le contenant de réactif ; et étape S5, répéter les étapes S1 à S4. La présente invention concerne en outre un dispositif pour la mise en œuvre du procédé de préparation en continu de type à écoulement pour un nanomatériau, parvient à une production en continu, augmente considérablement le taux d'utilisation de solutions de réaction, réduit les coûts, est appropriée pour le domaine industriel, et possède de grandes perspectives d'industrialisation.
PCT/CN2023/142681 2023-11-08 2023-12-28 Procédé et dispositif de préparation de type à écoulement pour nanomatériau Pending WO2025097577A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202311488007.8 2023-11-08
CN202311488007.8A CN117483778A (zh) 2023-11-08 2023-11-08 一种纳米材料的流动式制备方法及装置

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CN119747650A (zh) * 2024-12-23 2025-04-04 广东工业大学 一种封装基板用金属化浆料的制备方法及其装置

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CN115888591A (zh) * 2022-12-02 2023-04-04 电子科技大学长三角研究院(湖州) 一种连续自循环制备纳米颗粒的毫流控装置及控制方法

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