WO2007096386A1 - Procédé de précipitation de nanoparticules - Google Patents

Procédé de précipitation de nanoparticules Download PDF

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Publication number
WO2007096386A1
WO2007096386A1 PCT/EP2007/051674 EP2007051674W WO2007096386A1 WO 2007096386 A1 WO2007096386 A1 WO 2007096386A1 EP 2007051674 W EP2007051674 W EP 2007051674W WO 2007096386 A1 WO2007096386 A1 WO 2007096386A1
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WO
WIPO (PCT)
Prior art keywords
reaction volume
nanoscale
inorganic particles
reactants
particles
Prior art date
Application number
PCT/EP2007/051674
Other languages
German (de)
English (en)
Inventor
Sonja Grothe
Jochen Winkler
Original Assignee
Sachtleben Chemie Gmbh
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 Sachtleben Chemie Gmbh filed Critical Sachtleben Chemie Gmbh
Publication of WO2007096386A1 publication Critical patent/WO2007096386A1/fr

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    • 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
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/23—Mixing by intersecting jets
    • 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
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002—Nozzle-type elements
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
    • C01B13/363—Mixtures of oxides or hydroxides by precipitation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/20—Methods for preparing sulfides or polysulfides, in general
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C01F11/462—Sulfates of Sr or Ba
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/08—Sulfides
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00015—Scale-up
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00164—Controlling or regulating processes controlling the flow
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00164—Controlling or regulating processes controlling the flow
    • B01J2219/00166—Controlling or regulating processes controlling the flow controlling the residence time inside the reactor vessel
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/00862—Dimensions of the reaction cavity itself
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00889—Mixing
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00891—Feeding or evacuation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • the present invention is a process for the preparation of inorganic nanoparticles by precipitation from solutions resulting from ultrafast mixing of multiple reactants.
  • the present invention is a process for the preparation of nanoscale, inorganic particles with particle sizes of dso ⁇ 500 nm and a narrow particle size distribution by precipitation from highly supersaturated solutions, which arise by ultrafast mixing of several reactants in a microreactor.
  • DE-A-10254567 discloses a process for the preparation of alkaline earth sulfate nanoparticles. In this process, the nanoparticles in a
  • Synthesized liquid phase synthesis mixture which is characterized in that the synthesis mixture is a non-aqueous solvent with coordinating
  • WO-A-00/61275 discloses a method and an apparatus for carrying out chemical and physical processes, wherein chemical and physical Processes are set in motion by at least two liquid media via pumps, preferably high-pressure pumps, are injected through a respective nozzle into a reactor chamber enclosed by a reactor chamber to a common collision point.
  • a gas, an evaporating liquid, a cooling liquid or a cooling gas for maintaining the gas atmosphere in the interior of the reaction, in particular at the collision point of the liquid jets, or for cooling the resulting products are introduced via an opening in the reactor space.
  • the resulting products and excess gas are removed through a further opening from the reactor housing by overpressure on the gas inlet side or by negative pressure on the product and gas outlet side.
  • the liquid media must be injected under a pressure of 50 bar and more in the reactor chamber.
  • the entire system including the periphery
  • a process with lower pressures is also preferable from the point of view of occupational safety.
  • the object of the present invention is to overcome the disadvantages of the prior art.
  • the object of the present invention is to provide a method in which:
  • Blockages are avoided by the described geometry of the precipitation cell and / or
  • the inventive method is characterized in that a uniform and high supersaturation and a short residence time of the precipitated particles are ensured in the reaction volume.
  • the reactants are preferably present as a fluid or in a fluid, for example as a liquid, solution or suspension.
  • the reactants are present in aqueous media.
  • the reactants, which form a sparingly soluble precipitate under the present conditions (pH, temperature), are used at sufficiently high concentrations so that supersaturation of the precipitate of S »100 is achieved when the reactants are mixed.
  • the reactants are mixed in a small volume V, the reaction volume, the reaction volume being delimited by a reactor housing or by a gas stream.
  • the reaction volume is from 1 ⁇ l to 1 ⁇ l, preferably from 5 ⁇ l to 5 ml, particularly preferably from 10 ⁇ l to 3 ml. If the reaction volume is limited by a gas flow, the reaction volume is 10 * "5 ul of 1 .mu.l to 100, preferably from 1 * 10 4 .mu.l to 10 .mu.l.
  • the mixing of the reactants is turbulent and the micromixing time is well below 1 s.
  • the mixing can also be done in a laminar flow.
  • the process is carried out, for example, so that the reactants are sprayed at high pressures of p> 1 bar into a small reaction volume.
  • the precipitation process can be controlled by a downstream pH electrode and the volume flow rates of the individual reactants can be controlled. Following the precipitation, the precipitation suspension is typically concentrated and washed.
  • the concentration and washing can be carried out using
  • Grinder a freeze dryer or a pulsation dryer used.
  • the barium sulfate particles prepared according to the invention can be used in the nanocomposite area, for example for improving the mechanical properties of plastics, preferably thermoplastics, thermosets and / or elastomers.
  • plastics preferably thermoplastics, thermosets and / or elastomers.
  • the barium sulfate particles produced according to the invention have a nucleating effect and the crystallinity of polymeric materials is increased.
  • Further examples of fields of use of the nanoparticles prepared according to the invention are: adhesives, composites in conjunction with metals or ceramic materials, cosmetics, synthetic fibers.
  • nanoscale particles having particle sizes d 5 o ⁇ 500 nm and a very narrow particle size distribution can be produced in a method which is both technically simple and economical. Due to their fineness, these particles have special properties in paints, adhesives and plastics. A special feature is the fact that the use of high concentrations of these nanoscale particles in transparent polymer systems does not lead to loss of transparency.
  • the process according to the invention has the advantage over the previously known processes that: 1. the precipitation of the nanoscale particles takes place in the aqueous medium,
  • reaction volume being from 1 ⁇ l to 10 ml, preferably from 5 ⁇ l to 5 ml, more preferably from 10 ⁇ l to 3 ml, when the reaction volume through the reactor housing is limited;
  • reaction volume is from 1 * 10 5 ⁇ l to 100 ⁇ l, preferably from 1 * 10 4 ⁇ l to 10 ⁇ l, when the reaction volume is limited by a gas stream;
  • the residence time of the precipitate in the reaction volume is less than 1 s, preferably in the range of 0.0001 ms to 100 ms;
  • a method of producing nanoscale inorganic particles wherein the mixing has micromixing times of from 0.0001 ms to 1 s, preferably from 0.0005 ms to 10 ms, particularly preferably from 0.001 ms to 1 ms;
  • the inorganic particles are metal hydroxides, mixed metal oxides, metal sulfides and / or alkaline earth sulfates, preferably barium sulfate;
  • nanoscale inorganic particles wherein the dispersions of the precipitated nanoparticles are washed, concentrated and preferably stabilized by the addition of a suitable dispersing aid; - nanoscale, inorganic particles whose primary particles have a logarithmic particle size distribution with a geometric standard deviation of ⁇ g
  • nanoscale, inorganic particles obtainable by the process according to the invention, wherein the precipitated primary particles have a logarithmic
  • nanoscale, inorganic particles obtainable by the process according to the invention
  • nanoscale, inorganic particles obtainable by the process according to the invention, wherein the precipitated primary particles have a logarithmic particle size distribution with a geometric standard deviation of ⁇ g
  • nanoscale, inorganic particles the stabilized dispersions of the precipitated nanoparticles being used in paints, inks, adhesives, plastics, metals, ceramics and / or cosmetics;
  • Figures 1, 2 and 3 show by way of example the structure of a 2-jet or a 3-jet precipitation reactor. Like reference numerals in Figures 1 a, 1 b, 2 a, 2 b, and 3 also denote like objects.
  • Reactant 1 Reactant 1
  • 2 reactant 2: 3: reaction volume (reaction space);
  • 4 Product; 5: nozzle reactant 1; 6: nozzle reactant 2; 7: nozzle product; 8: Reactant 3; 9: nozzle reactant 3; 10: housing of the reaction cell; 1 1; Collision point of the nozzle jets of Reaktandendüsen 5, 6 or 5, 6, 9; 12: gas flow.
  • FIG. 1 a) cross section through a 2-jet precipitation reactor; b) Top view of a 2-jet precipitation reactor:
  • FIG. 2 a) Cross section through a 3-jet precipitation reactor: b) Top view of a 3-jet precipitation reactor.
  • FIG. 3 a) longitudinal section through a 3-jet precipitation reactor:
  • 0.3 molar zinc sulfate solution and a 0.3 molar sodium sulfide solution is injected with high pressure pumps.
  • the throughput of the zinc sulfate solution is in the range of 70 to 90 L / h.
  • the flow rate of the sodium sulfide solution is also adjusted in the range of 70 to 90 L / h such that the precipitate has a pH of 4.
  • the average residence time of the precipitate in the reactor is about 0.045 s.
  • the precipitation suspension is washed by means of cross-flow filtration and concentrated. Subsequently, the product freeze-dried.
  • 0.4 molar barium hydroxide solution and 0.4 molar sulfuric acid is injected with high-pressure pumps.
  • the flow rate of the sulfuric acid is 40 L / h and the flow rate of the barium hydroxide solution is adjusted to reach a pH of 3.
  • the residence time of the precipitation suspension in the reaction volume is about 0.02 s.
  • the precipitate is adjusted to a pH of 6.5, washed by membrane filtration and concentrated to a solids content of about 20%.
  • the resulting paste is dried by spray drying.
  • Spray-drying has the advantage that the resulting relatively coarse spray-dryer agglomerates form a very readily flowable powder which, surprisingly, is very readily dispersible.
  • a precipitation reactor according to FIG. 2 is used;
  • volumetric throughputs of f 50 L / h per Reaktandendüse 5, 6 and 9.
  • a precipitation reactor according to FIG. 3 is used in which two reactants 1 and 2 are reacted.
  • the product 4 resulting from the mixing of the reactants is discharged through a gas stream 12.
  • the reactants used are 0.5 molar aqueous barium sulphide solution and 0.5 molar aqueous zinc sulphate solution. In the reaction cell the following reaction takes place:
  • the product of the reaction is a mixture of nanoscale zinc sulfide and nanoscale barium sulfate in water.

Abstract

La présente invention concerne un procédé de production de nanoparticules inorganiques par précipitation à partir de solutions obtenues en mélangeant plusieurs réactifs de façon ultra-rapide.
PCT/EP2007/051674 2006-02-21 2007-02-21 Procédé de précipitation de nanoparticules WO2007096386A1 (fr)

Applications Claiming Priority (2)

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DE102006008412.8 2006-02-21
DE102006008412 2006-02-21

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2168967A (en) * 1984-11-19 1986-07-02 Ube Industries Process for producing metal oxide particles having a very small and uniform size
WO1998022387A1 (fr) * 1996-11-18 1998-05-28 The University Of Connecticut Oxydes et hydroxydes nanostructures et leurs procedes de synthese
EP1227508A1 (fr) * 2001-01-22 2002-07-31 Kawatetsu Mining Co., LTD. Poudre de niobium et anode fabriquée a partir de celle ci pour un condensateur à électrolyte solide
US20040253170A1 (en) * 2001-07-27 2004-12-16 Yingyan Zhou Process for producing nano-powders and poeders of nano-particles loose aggregate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2168967A (en) * 1984-11-19 1986-07-02 Ube Industries Process for producing metal oxide particles having a very small and uniform size
WO1998022387A1 (fr) * 1996-11-18 1998-05-28 The University Of Connecticut Oxydes et hydroxydes nanostructures et leurs procedes de synthese
EP1227508A1 (fr) * 2001-01-22 2002-07-31 Kawatetsu Mining Co., LTD. Poudre de niobium et anode fabriquée a partir de celle ci pour un condensateur à électrolyte solide
US20040253170A1 (en) * 2001-07-27 2004-12-16 Yingyan Zhou Process for producing nano-powders and poeders of nano-particles loose aggregate

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