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WO2016193087A1 - Procédé et processus technique de fabrication de micro-particules et nano-particules de différentes dimensions - Google Patents

Procédé et processus technique de fabrication de micro-particules et nano-particules de différentes dimensions Download PDF

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Publication number
WO2016193087A1
WO2016193087A1 PCT/EP2016/061773 EP2016061773W WO2016193087A1 WO 2016193087 A1 WO2016193087 A1 WO 2016193087A1 EP 2016061773 W EP2016061773 W EP 2016061773W WO 2016193087 A1 WO2016193087 A1 WO 2016193087A1
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WO
WIPO (PCT)
Prior art keywords
nozzle
particles
reaction
changing
outlet
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/EP2016/061773
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German (de)
English (en)
Inventor
Rainer Pommersheim
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.)
TULIPORT Sarl
Original Assignee
TULIPORT Sarl
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by TULIPORT Sarl filed Critical TULIPORT Sarl
Priority to EP16728852.1A priority Critical patent/EP3302778A1/fr
Priority to CN201680031756.XA priority patent/CN107683172B/zh
Publication of WO2016193087A1 publication Critical patent/WO2016193087A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium

Definitions

  • the invention relates to a method and a technical process for the production of small particles, which are synthesized in a preferably continuous process and whose size can be precisely adjusted in the process. This is done with the help of special nozzles, at the outlet of which two reactants are brought into contact so that small particles are formed.
  • the size of the particles is primarily determined by the flow parameters of the liquids at the outlet of the nozzle.
  • the addition of special surfactants in different concentrations to these liquids or the change in the concentration or temperature of the Christsiösungen the particle diameter can be additionally influenced.
  • the particle diameter can be in a granulometric range of a few nanometers to several micrometers.
  • the specially designed nozzles ensure a high yield and a narrow size distribution of the particles obtained.
  • Micro and nanoparticles such as e.g. Titanium oxide, zinc oxide are often used in sunscreen products as a so-called UV blocker.
  • sunscreen products e.g. Aluminum oxide particles are used as a stabilizer, while calcium phosphate particles are used in dentifrices as active ingredients on a biological model.
  • Particles of partially coated silicon dioxide are used, for example, to improve the flowability or of processing or surface properties.
  • Other particles such as carotenoids or titanium dioxide are used in different foods as a dye. 3. Paints and varnishes
  • particles for example of titanium oxide or barium sulfate are used as fillers or pigments.
  • Other particles improve the reflective properties of the colors or their UV or corrosion protection.
  • microparticles and nanoparticles such as e.g. highly dispersive silica as a drug transporter or depot.
  • Metal particles such as e.g. Silver gives special preparations an antibacterial effect, yet other particles are used as contrast agents in various diagnostic procedures.
  • a number of electronic components such as e.g. LED or even special capacitors could in today's quality without micro- and nanoparticles, e.g. nickel, silver, silicon, silicon carbide, etc. are not built.
  • Micro- and nanoparticles are also used in many other fields, such as in the textile industry or in the manufacture of special ceramics or detergents. All these examples show the high demand for such products. In particular, particles of high quality, ie those of the highest possible purity and monodispersibility, are needed.
  • Electrochemical process Here, metallic powder is obtained in the course of electrolysis or other electrochemical processes.
  • the laid-open specification DE 3703377A1 describes a process for the preparation of small barium sulfate particles by chemical precipitation from barium chloride and sodium sulfate.
  • nozzles or other devices are used to bring the two reactants as possible in a thin film or as a drop in contact.
  • the particle diameter obtained should in any case be less than 1 pm.
  • DE 10 2005 048 201 A1 likewise relates to a method in which nanoscale particles are produced.
  • the particles are obtained by the interaction of aqueous solutions in the interior of a specially designed microreactor in the presence of surface-active substances.
  • DE 23 47 375.8 a process for the production of finely divided, spherical nickel powder is described.
  • the metallic powder is obtained by the reduction of an aqueous-alcoholic suspension of nickel hydroxide with hydrogen at about 200 ° C and up to 100 at pressure in the presence of organic Ni- compounds.
  • the resulting particles have diameters in the range of 0.03pm-0.7pm.
  • the production of metallic mixed powders is concerned with the patent application AT 304 090 B.
  • the invention is based on the effect that when pouring particles of a metal B, which is more electronegative than a metal A in a salt solution of the metal A in the particles one Displacement of the metal B by A takes place. In this way receives composite metallic particles consisting of a central core of metal B and an outer layer of metal A.
  • a process for producing a nickel powder and a method for producing an electrically conductive paste for capacitors based thereon are the subject of patent application EP 1151815 A1.
  • the Ni powder is obtained in the course of the reduction of Ni-Suifat Hexaydrat with hydrazine in an alkaline medium at a corresponding temperature.
  • the reactants are simply added dropwise and stirred, and the precipitated Ni is filtered off. Since the complex of the resulting in the second phase of the reaction, the metallic nickel, forms in the liquid, its particle size and thus the resulting metallic grains is largely dictated by the mixing of the starting materials, which tends to expect unsatisfactory results.
  • the published patent application DE 102009057251A1 relates to a method for the production of small metallic particles, which are produced by precipitation of two reagents in the outlet region of a specially designed nozzle.
  • the size distribution of the particles obtained is very narrow. however, the process does not provide for adjusting the particle size by the flow parameters in the nozzle.
  • the present invention has the object to synthesize micro and nanoparticles in a continuous process on an industrial scale, in which the size of these particles can be specified by changing individual parameters of the process.
  • the basic idea of the process is to combine the reactants from which the particles are to be formed in the outlet region of a specially designed nozzle. By the contact of the different liquids they react with each other, whereby the particles arise.
  • the size of the particles is determined primarily by the flow conditions inside and at the outlet of the nozzle, which can be changed during the manufacturing process.
  • a central point in the method according to the invention is thus influencing the particle size by changing the physical parameters in the interior and at the outlet of the nozzle used.
  • a whole series of different nozzles are commercially available, a special construction must be used here.
  • the nozzle must ensure good mixing of the reactants with the smallest possible size distribution of the drops. At the same time, it must provide sufficient flow under preferably laminar flow conditions.
  • nozzles which are used for the dripping of highly viscous media.
  • Particularly suitable for this purpose are nozzles in which a gas stream is blown concentrically to the liquid-carrying capillaries, which ensures a clean drop break and a narrow droplet distribution.
  • Such nozzles are for example the subject of the published patent application DE102004026725A1.
  • multi-capillary nozzles are used here. In these nozzles, both the capillaries for liquid transport, as well as the channels for the concentric gas flowing around them are incorporated in superimposed plates.
  • nozzles were adapted as described above so that instead of the gas stream provided for the defined drop break, a second liquid stream could be passed through the nozzle.
  • This second liquid stream gets in contact with the first of the inner capillaries only at its outlet point, whereby the particles are formed.
  • a multiple nozzle is used, which is constructed as follows: Capillaries are located in the center of several, vertical, cylindrical channels. The inner diameter of the capillaries and the free cross section of the cylindrical channels has a diameter of a few millimeters. The capillaries and the cylindrical channels are flowed through by each of the reaction liquids.
  • the dimensions of the resulting cross-sections through which the liquids pass are comparable and selected so that, even in the case of laminar flows, the throughput per channel is in the region of a few liters per minute.
  • the individual cylindrical channels and the capillaries in their interior are interconnected within the nozzle by horizontal channels so that the flow conditions in each channel and in each capillary are almost equal.
  • the flow parameters also change through the capillaries and through the vertical, cylindrical channels. It could be proven experimentally that with laminar flows through the nozzle, thus at values of the Reynolds characteristic number under 10,000.
  • the diameter of the particles obtained is given by the flow velocity.
  • particle diameter in the order of well over 1 ⁇ , while at higher flow rates, which are close to the boundary to the turbulent flow. Particles with a diameter of about 0.5 pm are formed. In the area of turbulent flow, the particle diameter then remains constant at about 0.5 pm.
  • a surface-active liquid such as a detergent. the diameter of the particles obtained can be further reduced to below 0.1 pm. In this case, the smaller the particles, the higher the concentration of detergent in both of the nozzle supplied solutions. Similar effects can be observed by changing the concentration and / or the temperature of the reaction solutions.
  • Particles as described in the invention can be prepared as follows: Example 1
  • a 0.5 M aqueous solution of barium chloride is prepared and placed in a storage vessel.
  • an aqueous 0.5 M Natruimsulfatgins is filled.
  • These two solutions are then fed to a nozzle which is constructed as described above and in which the one solution flows through the capillary, the other the surrounding cylindrical channel.
  • barium sulfate particles are obtained in an aqueous suspension.
  • a 1 M aqueous magnesium chloride solution is prepared and placed in a storage vessel.
  • an aqueous 2 M Natruimhydroxidnaps is filled.
  • These two solutions are then fed to a nozzle which is constructed as described above and in which one solution flows through the capillary and the other through the surrounding cylindrical channel.
  • magnesium hydroxide is obtained as an aqueous suspension.
  • FIG. 2 An example of a possible engineering process for producing small particles as illustrated in the present invention is shown in FIG. 2:
  • the starting substances Komp. 1 and Komp. 2 are first placed in appropriate containers [V1 and V2], dissolved in water or other suitable solvent and adjusted to the concentration required for the process.
  • the solutions thus prepared are at the top of one or two continuously operated reactors [R1; R2] and are there reacted by a suitable nozzle or nozzle arrays.
  • the nozzles and the reactors can be brought to the required temperature by means of a heater.
  • the actual reaction takes place at the outlet of the nozzle device, where the particles are discharged as a suspension.
  • the diameter of the particles obtained is predetermined by the admission pressure to the nozzles or nozzle arrays. If necessary, a detergent can be added to the two reaction solutions in order to additionally influence the particle size.
  • the continuously operated reactor is suitably carried out, either as a heated flow tube, baffle plate or stirred tank, e.g. from the outside or by elements from the inside, heated or cooled to adjust the reaction temperature can.
  • the reactor may additionally contain internals which favor the reaction result.
  • a temperature gradient can additionally be set in the reactor.
  • the resulting suspension then passes into the two washing tanks [W1 and W2], and then into the filtration unit [filtration].
  • This unit can be designed both as a filter of different design as well as a decanter or centrifuge.
  • the now separated particles are then dried. For very small particles, it may be advantageous not to dry the particles and to use the filter cake as such.
  • FIG. 1 shows an exemplary embodiment of a nozzle array, as can be used in the method according to the invention.
  • the nozzle assembly At the top of the two reaction solutions are fed through openings in the cover plate the nozzle assembly, where they through holes directly on the distributor plate 1 meet.
  • the two liquid streams are divided into eight Einzetströme and so supplied to the distributor plate 2, wherein it is avoided that they come into contact with each other.
  • Seals 1 and 2 seal the structure to the outside and prevent the fluid streams from hitting each other.
  • the distributor plate 2 has the task of supplying the now 8 liquid streams of the first reaction solution and the 8 liquid streams of the second reaction solution separately to the 8 Kapiliarmodulen.
  • each capillary module the one reaction solution is passed through the capillaries, the other through a special channel in the module, which supplies the second reaction solution to the horizontal channels of the outlet plate, from where it enters the vertical holes of the outlet plate.
  • the capillaries of the modules are located in the center of these holes and are lapped by the second reaction solution.
  • the two reaction liquids come in this way only at the outlet, ie in the lower part of the outlet plate, in contact, where they react with each other.
  • a nozzle array as described herein may also be equipped with multiple or fewer capillary modules than indicated in the example. Also, the structure can be heated.
  • Such nozzle assemblies can be operated at different flow rates. Both laminar and turbulent flow conditions in the context of the present invention can be produced inside and at the outlet.
  • the constructions are also very suitable for large-scale technical applications, especially since volume flows of a few cubic meters per hour can be realized.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne une méthode ainsi qu'un processus technique de fabrication de petites particules, qui sont synthétisées au cours d'un processus de préférence continu et dont la dimension peut être réglée avec précision au cours du processus. Ceci est réalisé à l'aide de buses spéciales à la sortie desquelles deux réactifs sont amenés en contact de sorte qu'aucune petite particule ne se forme. La taille des particules est prédéfinie principalement par les paramètres d'écoulement des liquides à la sortie de la buse. L'ajout de substances tensio-actives spéciales dans une concentration différente à ces liquides ou la modification de la concentration ou de la température de la solution réactionnelle permet d'influencer en plus le diamètre des particules. L'invention concerne un processus technique uniforme et s'appuie sur des buses construites spécialement. Le fait que le diamètre des particules obtenues par modification des paramètres d'écoulement des solutions réactionnelles, parmi lesquels leurs propriétés de surface, leur concentration ou leur température, peut être prédéfini, a son importance. Un procédé de ce type peut être utilisé pour fabriquer des microparticules ou des nanoparticules métalliques ou non métalliques pour des applications très différentes.
PCT/EP2016/061773 2015-05-30 2016-05-25 Procédé et processus technique de fabrication de micro-particules et nano-particules de différentes dimensions Ceased WO2016193087A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP16728852.1A EP3302778A1 (fr) 2015-05-30 2016-05-25 Procédé et processus technique de fabrication de micro-particules et nano-particules de différentes dimensions
CN201680031756.XA CN107683172B (zh) 2015-05-30 2016-05-25 用于制备不同尺寸的微米颗粒和纳米颗粒的方法和工业过程

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015006727.3A DE102015006727A1 (de) 2015-05-30 2015-05-30 Verfahren und technischer Prozess zur Herstellung von Mikro- und Nanopartikeln unterschiedlicher Größe
DE102015006727.3 2015-05-30

Publications (1)

Publication Number Publication Date
WO2016193087A1 true WO2016193087A1 (fr) 2016-12-08

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PCT/EP2016/061773 Ceased WO2016193087A1 (fr) 2015-05-30 2016-05-25 Procédé et processus technique de fabrication de micro-particules et nano-particules de différentes dimensions

Country Status (4)

Country Link
EP (1) EP3302778A1 (fr)
CN (1) CN107683172B (fr)
DE (1) DE102015006727A1 (fr)
WO (1) WO2016193087A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023193981A1 (fr) 2022-04-07 2023-10-12 Rainer Pommersheim Procédé et dispositif de production de particules à haute teneur en magnésium à partir d'eau de mer
DE102023100537A1 (de) 2022-04-07 2023-10-12 Rainer Pommersheim Verfahren und Vorrichtung zur Herstellung von Partikeln mit einem hohen Magnesiumgehalt aus Meerwasser

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT304090B (de) 1969-08-12 1972-12-27 Nickel Le Verfahren zur direkten Herstellung eines homogenen, sehr reinen Mischpulvers
US3748118A (en) 1970-12-24 1973-07-24 Monticatini Edison Spa Process for preparing finely particled metallic nickel powder having a spheroidal form
DE2347375A1 (de) 1972-09-25 1974-04-04 Montedison Spa Verfahren zur herstellung von fein zerteiltem kugelfoermigen nickelpulver
DE3703377A1 (de) 1987-02-05 1988-08-18 Metallgesellschaft Ag Verfahren zur herstellung von ultrafeinem bariumsulfat durch faellung
EP1151815A1 (fr) 1999-11-10 2001-11-07 Mitsui Mining and Smelting Co., Ltd Poudre de nickel, procede de preparation de ladite poudre, et pate conductrice
DE102004026725A1 (de) 2004-05-28 2005-12-15 Cavis Microcaps Gmbh Modulares Düsensystem zur Erzeugung von Tropfen aus Flüssigkeiten unterschiedlicher Viskosität
DE102005048201A1 (de) 2004-10-11 2006-04-20 Penth, Bernd, Dr. Kontinuierliche Fällung von nanoskaligen Produkten in Mikroreaktoren
DE60212136T2 (de) 2001-07-20 2007-04-19 Protensive Ltd. Verfahren zur herstellung von teilchen
DE102009057251A1 (de) 2009-12-08 2011-06-09 Pommersheim, Rainer, Dr. Verfahren und technischer Prozess zur Herstellung von fein zerteiltem metallischem Pulver
WO2011116763A1 (fr) * 2010-03-22 2011-09-29 Mjr Pharmjet Gmbh Procédé et dispositif pour la fabrication de micro- ou de nanoparticules

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CN1278765C (zh) * 2003-06-20 2006-10-11 清华大学 一种将熔融液制成球形颗粒的造粒装置
ES2346137T3 (es) * 2003-12-23 2010-10-11 Yara International Asa Dispositivo de pulverizacion y procedimiento para la granulacion de un lecho fluidizado.
WO2005079964A1 (fr) * 2004-02-17 2005-09-01 Ehrfeld Mikrotechnik Bts Gmbh Micro-melangeur
CN1313184C (zh) * 2004-04-27 2007-05-02 贺文智 预成膜二流式喷嘴与带有该喷嘴的沉淀釜及利用该沉淀釜生产超细微粒的工艺
EP2205221A2 (fr) * 2007-10-23 2010-07-14 Koninklijke Philips Electronics N.V. Procédés de préparation de microparticules de polymère
WO2010133465A2 (fr) * 2009-05-18 2010-11-25 Basf Se Procédé de préparation de nanoparticules par utilisation de mini-émulsions
CN201632240U (zh) * 2010-02-25 2010-11-17 横店集团东磁股份有限公司 一种空气混合喷嘴
US8895962B2 (en) * 2010-06-29 2014-11-25 Nanogram Corporation Silicon/germanium nanoparticle inks, laser pyrolysis reactors for the synthesis of nanoparticles and associated methods
CN104248938A (zh) * 2013-06-27 2014-12-31 天津大学 一种水介质中成球颗粒的制备设备

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT304090B (de) 1969-08-12 1972-12-27 Nickel Le Verfahren zur direkten Herstellung eines homogenen, sehr reinen Mischpulvers
US3748118A (en) 1970-12-24 1973-07-24 Monticatini Edison Spa Process for preparing finely particled metallic nickel powder having a spheroidal form
DE2347375A1 (de) 1972-09-25 1974-04-04 Montedison Spa Verfahren zur herstellung von fein zerteiltem kugelfoermigen nickelpulver
DE3703377A1 (de) 1987-02-05 1988-08-18 Metallgesellschaft Ag Verfahren zur herstellung von ultrafeinem bariumsulfat durch faellung
EP1151815A1 (fr) 1999-11-10 2001-11-07 Mitsui Mining and Smelting Co., Ltd Poudre de nickel, procede de preparation de ladite poudre, et pate conductrice
DE60212136T2 (de) 2001-07-20 2007-04-19 Protensive Ltd. Verfahren zur herstellung von teilchen
DE102004026725A1 (de) 2004-05-28 2005-12-15 Cavis Microcaps Gmbh Modulares Düsensystem zur Erzeugung von Tropfen aus Flüssigkeiten unterschiedlicher Viskosität
DE102005048201A1 (de) 2004-10-11 2006-04-20 Penth, Bernd, Dr. Kontinuierliche Fällung von nanoskaligen Produkten in Mikroreaktoren
DE102009057251A1 (de) 2009-12-08 2011-06-09 Pommersheim, Rainer, Dr. Verfahren und technischer Prozess zur Herstellung von fein zerteiltem metallischem Pulver
WO2011116763A1 (fr) * 2010-03-22 2011-09-29 Mjr Pharmjet Gmbh Procédé et dispositif pour la fabrication de micro- ou de nanoparticules

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023193981A1 (fr) 2022-04-07 2023-10-12 Rainer Pommersheim Procédé et dispositif de production de particules à haute teneur en magnésium à partir d'eau de mer
DE102023100537A1 (de) 2022-04-07 2023-10-12 Rainer Pommersheim Verfahren und Vorrichtung zur Herstellung von Partikeln mit einem hohen Magnesiumgehalt aus Meerwasser

Also Published As

Publication number Publication date
EP3302778A1 (fr) 2018-04-11
CN107683172B (zh) 2021-11-16
CN107683172A (zh) 2018-02-09
DE102015006727A1 (de) 2016-12-01

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