WO2015091527A1 - Procédé de production d'agglomérats de particules solides - Google Patents

Procédé de production d'agglomérats de particules solides Download PDF

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Publication number
WO2015091527A1
WO2015091527A1 PCT/EP2014/078031 EP2014078031W WO2015091527A1 WO 2015091527 A1 WO2015091527 A1 WO 2015091527A1 EP 2014078031 W EP2014078031 W EP 2014078031W WO 2015091527 A1 WO2015091527 A1 WO 2015091527A1
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liquid
substance
particle agglomerates
range
agglomerates
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PCT/EP2014/078031
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German (de)
English (en)
Inventor
Yunfei Zhou
Bernd Sachweh
Tobias Merkel
Lena Lore HECHT
Heike Petra SCHUCHMANN
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Basf Se
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Publication of WO2015091527A1 publication Critical patent/WO2015091527A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • 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
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3684—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology
    • 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 relates to a process for producing solid, stable particle agglomerates.
  • Particle agglomerates which are composed of primary particles with diameters in the nanometer or micrometer range, may have different interesting properties depending on the chemical composition and morphology of the primary particles and the size, morphology and chemical composition of the particle agglomerates formed.
  • the porosity of the particle agglomerates can be controlled and a shell-shaped structure of the agglomerates can be achieved by using different primary particle materials. This makes it possible, for example, to influence the release kinetics of active substances and effect substances.
  • Industrial applications for particle agglomerates are found, for example, in optical, electronic, chemical, biotechnological and medical systems.
  • the primary particles in such particle agglomerates are usually held together by van der Waals forces or liquid bridges, often water.
  • particle agglomerates are produced by re-agglomeration.
  • a three-phase material system is used, which is usually a suspension of the solid primary particles in a first liquid and another liquid, often referred to as binder liquid, which is not soluble in the first liquid or with this is not or only partially miscible.
  • binder liquid which is not soluble in the first liquid or with this is not or only partially miscible.
  • the rewet agglomeration for the production of liquid-bridged particle agglomerates is known in principle.
  • the object of the invention is to provide a process for the production of stable particle agglomerates, which in particular can be designed continuously.
  • the present invention relates to a process for producing solid particle agglomerates comprising
  • step ii) incorporating an aqueous liquid 2 in the non-aqueous suspension provided in step i) to obtain a suspension of particle agglomerates in which the particles are connected to one another by liquid bridges,
  • the properties of the inventively prepared particle agglomerates such as their size, roughness, porosity or morphology, and also control other characteristic parameters.
  • it is comparatively easily possible to obtain larger particle agglomerates by incorporating in step ii) a larger amount of liquid 2 into the nonaqueous suspension provided in step i).
  • the properties of the particle agglomerates produced according to the invention can be set comparatively easily, for example by changing the nozzle diameter.
  • the use of a high-pressure dispersing nozzle makes it possible, in particular, to produce the particle agglomerates produced according to the invention in the form of a continuous process.
  • the method according to the invention can also be carried out, for example, in a rotor-stator device such as a couette apparatus or flow devices.
  • the morphology of the particle agglomerates produced according to the invention can be influenced.
  • this can be used, for example, to obtain stable, particle-packed particle agglomerates having a higher primary particle density compared to liquid-bridged particle agglomerates obtainable by re-agglomeration.
  • the flow conditions it is also possible, for example, to obtain solids-bridged particle agglomerates having different fractal structures or to change the porosity of the resulting solids-bridged particle agglomerates.
  • the liquid 1 used in the process according to the invention is an organic liquid which has a solubility in water of at most 1 g / l at 20 ° C. and 1013 mbar.
  • the liquid 1 is selected from hydrocarbons and hydrocarbon mixtures.
  • the liquid 1 is preferably selected from Cs-C7 alkanes, particularly preferably Cs-C12 alkanes, very particular It prefers C6-Cio-alkanes.
  • liquids 1 are n-pentane, n-hexane, cyclohexane, n-heptane, n-octane, n-nonane, n-decane, n-undecane, n-dodecane and mixtures thereof.
  • the liquid 1 preferably comprises at least 20% by weight, more preferably at least 50% by weight, most preferably at least 80% by weight, of C5-C12 alkanes, based on the total weight of the liquid 1.
  • the liquid comprises 1 20 to 100 wt .-%, preferably 50 to 100 wt .-%, particularly preferably 80 to 100 wt .-% of Cs-Ci2 alkanes, based on the total weight of the liquid 1.
  • the liquid comprises 1 n -Decan and is in particular at least 90 wt .-%, based on the total weight of the liquid 1, of n-decane.
  • the liquid 1 comprises in particular 90 to 100 wt .-%, based on the total weight of the liquid 1, n-decane.
  • the liquid 2 is an aqueous liquid.
  • the liquid 2 can be used as such or preferably in the form of an emulsion in an organic liquid.
  • the liquid 2 is usually water or dilute aqueous acids or alkalis.
  • Preferred among the dilute aqueous acids are sulfuric acid and hydrochloric acid.
  • Preferred among the dilute aqueous liquors are sodium hydroxide solution, potassium hydroxide solution, aqueous solutions of ammonia and aqueous solutions of alkaline carbonates and bicarbonates such as sodium carbonate, potassium carbonate or sodium bicarbonate.
  • the concentration of acid or alkali is typically in the range from 0.01 to 5 mol / l, in particular in the range from 0.1 to 2 mol / l.
  • the water content of the liquid 2 is generally 20 to 100 wt .-%, preferably 40 to 100 wt .-%, particularly preferably 60 to 100 wt .-%, each based on the total weight of Liquid 2.
  • the liquid 2 is substantially exclusively water, i. h., The water content of the liquid 2 is specifically 98 to 100 wt .-%, based on the total weight of the liquid second
  • the liquid 2 is used in the form of an emulsion with an organic liquid, which is usually a water-in-oil emulsion.
  • an organic liquid which is usually a water-in-oil emulsion.
  • the concentration of the liquid 2 in the emulsion is preferably 1 to 20 wt .-%, particularly preferably 2 to 10 wt .-%, based on the total weight of the emulsion.
  • the organic liquid contained in the emulsion is one organic liquid which has a solubility in water of at most 1 g / L at 20 ° C and 1013 mbar, preferably by the liquid solvent 1, and in particular by the liquid solvent 1 preferably mentioned organic solvent.
  • an emulsion of water with n-decane is used.
  • the emulsion of liquid 2 with the organic liquid contains substantially no surfactant, in particular less than 0.01% by weight, based on the total weight of the emulsion.
  • the volume ratio of emulsion of the liquid 2 to the nonaqueous suspension of the liquid 1 provided in step i) is generally in the range from 4: 1 to 1:10.
  • solid particles which are also referred to as primary particles as described above
  • the nonaqueous suspension of the liquid 1 provided in step i) of the process according to the invention in principle all solid particles are suitable which have the desired size, do not dissolve significantly in the liquid 1 and / or the liquid 2 and sufficiently with the liquid 2 wet. Accordingly, the solid particles usually have a hydrophilic surface.
  • Suitable solid particles are preferably selected from particles of inorganic oxides, sulfides, sulfates, phosphates and carbonates.
  • the solid particles are selected from titania, silica, alumina, zinc sulfide, barium sulfate, calcium phosphate, calcium carbonate and mixtures thereof.
  • the solid particles are preferably selected from titanium dioxide, silicon dioxide and mixtures thereof.
  • the mean particle diameter of the solid particles in the suspension can vary over a wide range and is generally in the range of 1 nm to 10 ⁇ m, preferably 10 nm to 1 ⁇ m and more preferably 10 nm to 300 nm, determined by means of light scattering.
  • the concentration of the solid particles in the non-aqueous suspension provided in step i) is generally in the range from 1 to 30% by weight, preferably in the range from 2 to 20% by weight, based on the total weight of the suspension.
  • the weight ratio of the liquid 2 to the solid particles is generally in the range of 1:10 to 1: 1, preferably in the range of 1: 5 to 1: 2.
  • the substance S can be used as such or preferably as a solution in an organic solvent, preferably in a solvent mentioned for the liquid 1 and in particular a preferred for the liquid 1, in the process according to the invention. If the substance S is used as a solution in an organic solvent, the concentration of the substance S in the solution is generally 1 to 99% by weight, preferably 2 to 60% by weight, particularly preferably 5 to 40% by weight. , based on the total weight of the solution.
  • the substance S is generally a compound which reacts with the liquid 2, preferably water, by a chemical reaction to form a solid which is insoluble in the liquid 1 and the liquid 2.
  • Chemical reactions are, for example, the formation of metal or Halbmetalloxiden by hydrolysis of suitable metal or Halbmetallprecursoren and the formation of sparingly soluble salts.
  • the substance S is a compound which is soluble in the liquid 1 or is miscible with it.
  • the substance S generally has no halogen atom.
  • Preferred substances S are metal and semimetal compounds, especially those of titanium, zirconium, silicon, magnesium or aluminum, which react with the liquid 2 to form metal or semimetal oxides.
  • the substance S is preferably selected from metal and semimetal alkoxides which react with the liquid 2, in particular water, to form a solid.
  • alkoxides of titanium, zirconium, silicon, magnesium, aluminum and mixtures thereof in particular the alkoxides of the abovementioned metals and semimetals having 1 to 5 carbon atoms, where the metals or semimetals may optionally carry one or more alkyl radicals having preferably 1 to 5 carbon atoms
  • tetra-i-propyl titanate aluminum tri-sec-butoxide, tetraethoxysilane, zirconium tetra-n-propylate and magnesium dimethylate.
  • tetra-i-propyl titanate titanium (IV) isopropoxide.
  • the solid which is insoluble in the liquid 1 and the liquid 2 and which is formed during the reaction of the liquid bridges comprising the substance S, preferably consisting of water, is generally a hydrolysis product of the substance S.
  • this is a hydrolysis product of the abovementioned metal - and Semi-metal alkoxides, ie metal and semi-metal oxides such as titanium dioxide, silica and alumina.
  • the substance S can already be incorporated during the incorporation of the liquid 2 into the nonaqueous suspension provided in step i).
  • the incorporation of the substance S preferably in the form of a solution, but preferably after the incorporation of the liquid 2, for example by adding the substance S, preferably their solution, to the obtained in step ii) suspension of Fluid bridges associated particle agglomerates.
  • the incorporation of the liquid 2 into the non-aqueous suspension provided in step i) preferably takes place by means of a high-pressure dispersing nozzle.
  • a high-pressure dispersing nozzle eg. B. flat nozzles, pinhole diaphragms, slit diaphragms and deflection nozzles. It is also possible to use jet dispersants and counter jet dispersers.
  • the diameter of the nozzle opening is in the range of 50 to 700 ⁇ , preferably 70 to 400 ⁇ .
  • a preferred embodiment of a dispersing nozzle is the so-called pinhole.
  • Particularly suitable is a high-pressure dispersing nozzle, as described in WO 2008/1 16839. This document is hereby incorporated by reference in its entirety.
  • the arrangement shown in Figure 1 consists of a base body 10, which is provided in the axial direction, ie in the flow direction of the liquid 2 (8) with a through hole 1 1.
  • a base body 10 which is provided in the axial direction, ie in the flow direction of the liquid 2 (8) with a through hole 1 1.
  • an aperture 12 with a passage 13, preferably a bore with a circular cross section, in the flow direction of the liquid 2 in front of the mixing chamber 14 is arranged.
  • the passage 13 typically has a cross-sectional area in the range of 0.001 to 0.4 mm 2 , in particular in the range of 0.01 to 0.2 mm 2 .
  • the mixing chamber typically has a volume in the range of 0.5 to 5.5 cm 3 , in particular in the range of 0.7 to 3.5 cm 3 .
  • the arrangement further comprises radially arranged channels 15, via which the in step i) of According to the method provided non-aqueous suspension (9) of the mixing chamber 14 is supplied on.
  • the suspension of the liquid-bridged particle agglomerates exits via the outlet opening 16 and is preferably passed into a storage vessel (not shown).
  • the bore 1 1 and the passage 13 are arranged concentrically.
  • the base body 10, the aperture 12, the mixing chamber 14 and the outlet opening 16 are preferably also arranged concentrically.
  • the liquid 2 flowing into the mixing chamber through the dispersing nozzle entrains and mixes with the suspension fed behind the mixing nozzle. Behind the nozzle exit, the turbulent kinetic energy rises sharply. The inertial forces in the turbulent flows lead to a dispersion. The strong cross-sectional constriction leads to an increase in the flow velocity, so that the pressure in and behind the nozzle drops sharply.
  • at least one additional pump and / or a pressure vessel is usually necessary.
  • the first pressure p1 is generally in the range of 10 to 4000 bar, in particular in the range of 50 to 2000 bar and especially in the range of 100 to 1200 bar.
  • the second pressure p2 with which the suspension is fed into the mixing chamber behind the dispersing nozzle is usually in the range from 0.1 to 25 bar, if it is operated with counterpressure. If work is carried out without counter-pressure, the pressure p2 is preferably in the range from 0.1 to 10 bar and more preferably in the range from 0.5 to 5 bar.
  • the non-aqueous suspension provided in step i) is preferably supplied to the mixing chamber at an angle in the range from 30 ° to 150 ° to the outlet direction of the dispersing nozzle.
  • one will proceed so that one provides the non-aqueous suspension of solid particles in the liquid 1, for example by mixing and optionally stirring and predispersing of the solid particles with the liquid 1, for example by means of a rotor-stator device or means Ultrasonic.
  • a rotor-stator device or means Ultrasonic As a rule, an emulsion of the liquid 2, preferably in an organic solvent mentioned above for the liquid 1, especially in the same organic solvent or solvent mixture as the liquid 1, is also obtained.
  • a rotor-stator device for example, by stirring with the aid of a rotor-stator device, by ultrasound or emulsifying using a Hochdruckdispergierdüse.
  • the liquid 2 is then preferably incorporated into the nonaqueous suspension provided in step i) by means of the above-described high pressure dispersing nozzle by feeding the emulsion of the liquid 2 at a pressure p1 through a nozzle to a mixing chamber located immediately behind the nozzle and at the same time at a pressure p2 ⁇ p1 the non-aqueous suspension provided in step i) of the process according to the invention is fed behind the nozzle to the mixing chamber.
  • the preparation of the emulsion of the liquid 2 usually in an organic solvent mentioned above for the liquid 1, with the incorporation of this emulsion in the non-aqueous suspension provided in step i).
  • the emulsion is prepared and incorporated substantially simultaneously.
  • This liquid-bridged particle agglomerates can be obtained in high space-time yield.
  • the liquid 2 and an organic solvent or solvent mixture mentioned above for the liquid 1 are preferably fed simultaneously behind the dispersing nozzle to the mixing chamber, for example from different sides.
  • fluid particles 2 preferably water
  • these liquid-bridged particle agglomerates are generally stable enough to be prepared as a suspension in the liquid 1.
  • the substance S preferably in the form of a solution in the liquid 1, can already be fed to the mixing chamber together with the suspension in the liquid 1 provided in step i) during the production of the liquid-bridged particle agglomerates.
  • the substance S preferably in the form of a solution, preferably behind the nozzle, as a rule together with the liquid 2, leads to the mixing chamber. It is preferred to incorporate the substance S, preferably in the form of a solution, but into a suspension of the liquid-bridged particle agglomerates obtained by incorporation with the aid of the high-pressure dispersing nozzle.
  • the substance S preferably in the form of a solution in the liquid 1, will be incorporated directly behind the nozzle outlet into the resulting suspension of liquid-entrained particle agglomerates, for example by means of an inlet valve and / or by addition and optionally stirring in a collecting vessel.
  • the production of the particle agglomerates takes place in a flow device.
  • solid particle agglomerates produced according to the invention can be obtained in this way, which have various fractal structures and are therefore as a rule of different porosity or have a different solid particle density.
  • the solid particle agglomerates obtainable according to the invention also generally differ in their shape, depending on the flow conditions set.
  • Suitable flow devices are, for example, flow tubes or rotor-stator devices, such as preferably Couette devices.
  • the flow conditions can be set, for example, laminar or turbulent. Furthermore, solid particle agglomerates of different morphology can be obtained by setting different Reynolds numbers.
  • the liquid-bridged particle agglomerates are prepared with the aid of the high-pressure dispersion nozzle described above and pass the suspension of liquid-bridged particle agglomerates leaving the nozzle into the flow device, preferably a flow tube, which then flows through the suspension as it flows through the suspension Substance S, preferably in the form of a solution, is supplied from the outside.
  • the liquid-bridged particle agglomerates are prepared, preferably using a high-pressure dispersing nozzle or a rotor-stator device, for example a stirrer, and carrying the suspension of liquid-bridged particle agglomerates obtained in step ii) of the process according to the invention in a Couette apparatus.
  • a high-pressure dispersing nozzle or a rotor-stator device for example a stirrer
  • the temperature during the process according to the invention can in principle be adjusted over a wide range, but a temperature should not be exceeded above which the liquid-bridged particle agglomerates decompose.
  • the process according to the invention is carried out at a temperature in the range from 5 to 90.degree. C. and preferably in the range from 10 to 40.degree.
  • the process according to the invention is particularly preferably carried out at room temperature, ie about 20 ° C.
  • the particle agglomerates As a result of the process according to the invention, a suspension of solid particle agglomerates is obtained, the particle agglomerates having diameters in the nanometer, micrometer or millimeter range depending on the reaction procedure.
  • the particle agglomerates obtainable by the process according to the invention which may comprise, for example, filtration and / or centrifuging processes, obtain the particle agglomerates obtainable according to the invention as a solid, for example in the form of flakes or powders for a wide variety of applications ,
  • Figure 1 Schematic representation of the preferred Hochlichhomogenisators.
  • Figure 2 Left picture (a): Scanning electron micrograph of the untreated titanium dioxide primary particles from Example 1.
  • Figure right (b): Scanning electron micrograph of the solidified titanium dioxide agglomerates after addition of titanium (IV) - isopropoxide from Example 1.
  • Figure 3 Scanning electron micrograph of solid titanium dioxide agglomerates obtained after addition of titanium (IV) isopropoxide at laminar flow in a Couette apparatus with a Reynolds number of about 2100 (analogous to Example 2).
  • Figure 4 Scanning electron micrograph of solid titanium dioxide agglomerates obtained after addition of titanium (IV) isopropoxide in turbulent flow in a Couette apparatus with a Reynolds number of about 9300 (analogous to Example 2).
  • FIG. 5 Photographic image of the rotor used in Example 2.
  • Figure 6 Scanning electron micrograph showing a section of solid glass microbead agglomerates.
  • the solid glass microsphere agglomerates were prepared in Example 3.
  • Figure 7 Scanning electron micrograph of solid silica nanospheres agglomerates.
  • the solid silica nanospheres agglomerates were prepared in Example 4.
  • Titanium dioxide particles T1O2 P25, Evonik: average primary particle size 21 nm (manufacturer).
  • Glass microspheres (OMicron® NP3-P0, Sovitec): uncoated, average particle diameter 3 ⁇ m according to the manufacturer's instructions, particle size distribution up to 10 ⁇ m.
  • Silica nanospheres ( ⁇ ngströmSphere®, Fiber Optic Center Inc., USA): uncoated, dry, monodisperse powder, average particle diameter 0.1 ⁇ , standard deviation of particle size less than 10%.
  • SLS Static Light Scattering
  • the preparation of the solid particle agglomerates of titanium dioxide were carried out in a Couette flow apparatus.
  • the Couette device (see Figure 5) had a rotor with a cylindrical geometry, which had longitudinal grooves in the cylinder surface (dimensions: diameter 37 mm, height 60 mm). This rotor was used in a 250 mL beaker.
  • the drive was carried out with a stirrer RZR2021, Fa. Heidolph.
  • Example 2 5 g of the suspension of water-bridged particle agglomerates in n-decane obtained in Example 1 were added to the beaker and waited for 2 minutes. Then 1, 34 g of titanium (IV) isopropoxide was added to the beaker and stirred for 2 minutes. The reaction product was filtered off, dried at room temperature and examined by scanning electron microscopy.
  • the preparation of the solid glass microbead agglomerates was carried out analogously to Example 1, using glass microspheres instead of titanium dioxide particles.
  • the suspension used contained 1 g of glass microspheres, the emulsion used contained 0.1 g of water.
  • the amount of titanium (IV) isopropoxide added was 0.79 g. Solid-bridged glass microbead agglomerates were obtained (see FIG. 6).
  • the preparation of the solid silica nanospheres agglomerates was carried out analogously to Example 1, using silica nanospheres instead of titanium dioxide particles.
  • the suspension used contained 1 g of silica nanospheres, the emulsion used contained 0.1 g of water.
  • the amount of titanium (IV) isopropoxide added was 0.79 g. Solid-bridged silica nanospheres agglomerates were obtained (see FIG. 7).

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Abstract

La présente invention concerne un procédé de production d'agglomérats de particules solides stables, selon lequel des agglomérats de particules à ponts liquides sont préparés par agglomération par remouillage, les ponts liquides étant ensuite solidifiés par incorporation d'une substance S.
PCT/EP2014/078031 2013-12-17 2014-12-16 Procédé de production d'agglomérats de particules solides WO2015091527A1 (fr)

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EP13197766.2 2013-12-17
EP13197766 2013-12-17

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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US4011096A (en) * 1975-06-10 1977-03-08 E. I. Du Pont De Nemours And Company Vesiculated silica microspheres
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