EP2689855A1 - Modifizierte Mikronisierungsvorrichtung und ihre Verwendung - Google Patents

Modifizierte Mikronisierungsvorrichtung und ihre Verwendung Download PDF

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Publication number
EP2689855A1
EP2689855A1 EP12177709.8A EP12177709A EP2689855A1 EP 2689855 A1 EP2689855 A1 EP 2689855A1 EP 12177709 A EP12177709 A EP 12177709A EP 2689855 A1 EP2689855 A1 EP 2689855A1
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EP
European Patent Office
Prior art keywords
hitting elements
hitting
elements
micronization
triangular
Prior art date
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Granted
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EP12177709.8A
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English (en)
French (fr)
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EP2689855B1 (de
Inventor
Tihomir Lelas
Peter Ost
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Oekomineral AG
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Oekomineral AG
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Priority to DK12177709.8T priority Critical patent/DK2689855T3/en
Priority to EP12177709.8A priority patent/EP2689855B1/de
Publication of EP2689855A1 publication Critical patent/EP2689855A1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C13/00—Disintegrating by mills having rotary beater elements ; Hammer mills
    • B02C13/22—Disintegrating by mills having rotary beater elements ; Hammer mills with intermeshing pins ; Pin Disk Mills

Definitions

  • the present invention relates to a device for micronization according to the preamble of claim 1.
  • Micronization is a highly effective kind of milling which allows a direct production of very fine particles, typically 5-50 ⁇ m, from relatively coarse-grained starting material, of particle size, e.g. 0,1-1 mm.
  • micronization is widely used in production of active substances and excipients for pharmaceutical, cosmetic, and agrochemical industries, in chemical industry (e.g. fillers, pigments), and in many other fields.
  • Micronization can be accomplished by a prolonged milling in various classical mills (ball mill, jet mill, disintegrators etc,), wherein the milling process is based mainly on collisions of particles between themselves or with hitting elements of a milling device
  • Disintegrators of various types are known from the prior art. Examples of such disintegrators are for example disclosed in US 4,406,409 A1 and HR 990 263 A2 . Those disintegrators are principally based on the concept of two high-speed opposite rotating discs. The discs bear particular hitting elements, blades, which partially collide with particles directly, but mostly targeted to create an efficient airflow by mimicking turbines, driving particles into mutual collisions. In literature, there are described devices with various shaped blades on the discs:
  • the present invention provides an improved device for micronization based on the concept of desintegrator with two opposite rotating discs, known also as disintegration.
  • the present device modified for significant improvement in micronization process.
  • the main improvement of the present invention is a modification of particle hitting elements or blades, in positioning and shape.
  • Discs are situated within the micronizer in a way that the layers of blades of first and second disc enter into each other's.
  • Particles of the material being micronized carried by centrifugal force from the center of the device, pass through several layers of cubical and triangular shaped blades in the way to collide repeatedly with other particles and between rows of blades. Additionally, triangular blades, oppose to centrifugal particle flow by forcing them into repeated collisions, resulting in improved reduction of their size.
  • the present invention provides a modified device for an improved milling process, which is based on the concept of a disintegrator.
  • a device for micronization of substances comprises two rotors driven in a direction opposite to each other, each rotor carrying at least one row of multiple hitting elements forming a ring, said rings being arranged concentrically the rings of the different rotors engaging alternately with one another, the hitting elements being suitably arranged to provide transportation of the substance from inside the rings to the outside by effecting a suitable airflow, at least two directly adjoining rings carrying hitting elements with different foot print wherein at least a fist ring is equipped with trapezoidal hitting elements with trapezoidal foot print and at least one other ring directly adjoining the first ring is equipped with triangular hitting elements with triangular foot print.
  • the hitting elements according to the present invention provide a suitable air flow to effect inter particle collisions but also provide improved collisions between the particles and the hitting elements as well as permanent milling between the hitting elements of directly adjoining rings.
  • one side of the triangular hitting elements and/or one of the parallel sides of the trapezoidal hitting elements is perpendicularly oriented to a radius crossing the hitting element.
  • the hitting elements perpendicular to a radius crossing the respective hitting elements are suitably arranged to provide parallel arranged surfaces for milling of the substance between adjoining rings.
  • the trapezoidal hitting elements are of rectangular foot print.
  • the trapezoidal hitting elements may be of generally cubical shape. Compared to other shapes cubical hitting elements are easier to produce and thus cheaper in production.
  • the triangular hitting elements are of basically right angled triangular foot print.
  • the right angled triangular footprint allows manufacturing of the triangular hitting elements with rectangular base elements that are divided diagonally. It is thus possible to use base elements with rectangular footprint to manufacture both, the rectangular hitting elements and the triangular hitting elements.
  • the perpendicularly oriented side of the triangular hitting elements is the longer cathetus.
  • the longest cathetus is oriented to the outward circumference of it's respective ring.
  • the longer cathetus of the triangular hitting elements is thus tangentially oriented and may serve for milling.
  • the milling will take place between the tangentially oriented surface of the triangular hitting elements and surfaces of hitting elements of a cicumferring and directly adjoining ring.
  • the triangular hitting elements thus provide for sufficient air flow from the center of the rings to the outside.
  • the longest side of the triangular hitting elements is oriented in front in direction of rotation of the respective rotor.
  • this embodiment directs the particles in backward loops, i.e. backward in substantially radial direction, thus resulting in extended time within the device and thus more inter particle collisions.
  • the hitting elements of directly adjoining rings are suitably arranged to provide milling between the hitting elements of adjacent rings.
  • Each ring may carry a number of hitting elements equivalent to the diameter in cm of the respective ring.
  • the number of hitting elements per ring obtained by this rule provides an optimal ratio of hitting elements to spaces between the hitting elements and thus further enhances the efficacy of disintegration.
  • the hitting elements may be made of stainless steel or ceramics and/or coated with industrial diamond or ruby.
  • the above materials and/or coatings provide high durability of the hitting elements as well as high availability of the used materials.
  • the triangular hitting elements and the trapezoidal hitting elements may have at least two sides with coinciding length.
  • trapezoidal elements can serve as base elements for both, trapezoidal and triangular hitting elements.
  • Figure 1 shows a perspective view of a disintegrator 1.
  • the disintegrator 1 according to figure 1 is equipped with two electro motors 20 arranged opposite to each other and rotating in opposite direction ⁇ .
  • Each electro motor 20 is coupled directly or indirectly via a gearbox to a rotor 3 that is equipped with multiple concentrically arranged rings 9, 11 of hitting elements 5, 7 (hereinafter also called blades).
  • the rings 9, 11 of hitting elements 5, 7 of the two rotors 3 alternately engage with each other thus adjacent rings 9, 11 of hitting elements 5, 7 rotating in opposite direction ⁇ .
  • the rotors 3 are encapsulated in a casing 21 that may be opened according to the illustration in figure 1 .
  • the whole disintegrator 1 is located on a mount 22, e.g. a base frame that carries the electro motors 20 and the oppositely rotating rotors 3.
  • the disintegrator 1 exhibits a filler 23 with a hopper 24.
  • the filler 23 directs the material for micronization to the center of the rotors 3.
  • a sufficient airflow generated by the rotors 3 rotating in opposite direction ⁇ transports the material from the center of the rotors 3 to an outlet 25 at the circumference of the rotors 3 causing multiple inter particle and particle-hitting-element collisions.
  • the micronized material exits the casing 21 of the disintegrator 1 and either may be collected or again fed into the disintegrator 1.
  • Figure 2 clearly shows how the rings 9, 11 of hitting elements 5, 7 of the rotors 3 alternatively engage one another thus adjacent rings 9, 11 of hitting elements rotating in opposite directions ⁇ .
  • FIGS 3 to 6 show different views of hitting elements according to the prior art.
  • the hitting elements depicted in figures 3 and 4 are of blade-like footprint that mainly generates an airflow transporting particles from the center of the rotors 3 to the circumference, thus generating inter particle collisions. However due to the pitch of the blades the time the particles stay within the disintegrator 1 is quite low.
  • Figures 5 and 6 show exemplary traces of articles from the center of the rotors 3 to the outer circumference where the particle exit the disintegrator 1.
  • the improved device 1 according to the present invention has the similar device construction like the disintegrators 1 from the prior art [J.Durek: Disintegrator and the method for the operation thereof, US4406409 A ], [T. Lelas: Device for micronizing materials, HR990263 A2 (1999 )] shown in figures 1 and 2 .
  • FIG. 5 An embodiment of a blade design (design of the hitting elements) according to the present invention is shown in figures 5 to 11 .
  • a first ring 9 of trapezoidal blades carries hitting elements 5 with rectangular footprint and thus ob generally cubic shape.
  • Another ring 11, directly adjoining the first ring 9 carries triangular hitting elements 7 with a footprint of a right angled triangle. These triangular hitting elements 7 are tightly positioned and of generally prismatic shape.
  • the different footprints of the blades 5, 7 are shown in figure 5 .
  • Figure 5 shows a cross-section in the plane of rotation of the hitting elements 5, 7 thus depicting the different footprints of the hitting elements 5, 7 on the different rotors 3.
  • the rotor 3 rotating in clockwise manner carries tree rings 9 of trapezoidal hitting elements 5 with rectangular footprint.
  • the other rotor 3 (in the depicted view rotating counterclockwise) carries two rings 11 of triangular hitting elements 7 with triangular footprint.
  • the rings 9, 11 of hitting elements 5, 7 engage alternately thus on a ring 9 rotating in clockwise manner follows a ring 11 rotating in opposite direction, i.e. counterclockwise manner.
  • the present embodiment provides an elongated time of the particles within the disintegrator 1 and thus a enlarged number of inter particle collisions, permanent milling between the hitting elements 5, 7 of adjacent rings 9, 11 and a enlarged number of collisions between particles and the hitting elements 5, 7.
  • the trace of a particle being micronized in a disintegrator 1 according to the present embodiment is depicted in figure 8 . Due to the arrangement of the hitting elements 5, 7 the particles move in a loope-like manner thus resulting in a prolonged time within the disintegrator 1.
  • Figure 9 shows an enlarged cross-section of a triangular hitting element 7 according to the present embodiment.
  • the hitting element 7 is of basically triangular footprint with rounded edges. As depicted in figure 9 the footprint is in the shape of a right angled triangle.
  • the hypotenuse 15 of the right angled triangle is oriented tangentially to the outward circumference of the ring 11 built by the hitting elements 7 of it's respective ring.11
  • the arrow in figure 9 indicates the direction of rotation ⁇ of the respective hitting element 7, the longer cathetus 13 of the right enabled triangle thus being forward oriented.
  • a center of the hypotenuse 15 of the triangular shaped footprint is perpendicularly cut by a radius r of the respective ring 11.
  • the longer cathetus 13 thus is inclined relative to the radius r by an angle ⁇ of 60 degrees.
  • the other cathetus 14 is inclined relative to the radius r by an angle ⁇ of minus 30 degrees.
  • Figure 11 depicts two triangular hitting elements 7 arranged in a ring like manner.
  • the hitting elements 7 are spaced from one another by a distance A of 15 - 100% of the length of the hitting elements 7.
  • the longest side of the rectangular hitting elements 5 for example may be 30 mm. Accordingly the longer cathetus 13 of the triangular hitting elements 7 may be of the same length.
  • the course of the micronization process in the device 1 according to the present embodiment is actually the same as in the micronizer with hitting elements as disclosed in the prior art (shown in Figures 3 and 4 ).
  • Material being micronized is added in the hopper 24 of the filler 23. The latter brings the material into a central part of rotating discs 3 beside their axes. Due to a strong centrifugal force, particles of material being micronized pass through two or several layers of rotating hitting elements 5, 7 (blades) of opposite discs rotating at high speed (about 5000 - 8000 rounds per minute) in opposite direction.
  • the micronization device was equipped with two identical 20 kW power electro-motors that work at 220 V and 50 Hz.
  • the reason why zeolite is chosen is due to its NH 4 + sorption and retention capacity. It has been already demonstrated that zeolite can have significant improvement in sorption capacity, if micronized below one ⁇ m.
  • Table 1 shows the influence of the various shapes of hitting elements (blades) from different micronizing discs ( Figures 5, 6 and 8 ) on efficacy of micronization of zeolite clinoptilolite of starting particle size 50-100 ⁇ m. The goal was to achieve larger amount of submicron particles.
  • Table 2 shows the influence of the various shapes of hitting elements from different micronizing discs ( Figures 5, 6 and 8 ) on particle specific surface are of zeolite clinoptilolite of starting particle specific surface area 0.9 m 2 /g.
  • Table 3 shows the influence of the various shapes of hitting elements from different micronizing discs ( Figures 5, 6 and 8 ) on NH4+ sorption of zeolite clinoptilolite of starting capacity 0,23 mmol/g Table 3 MICRONIZATION-1 MICRONIZATION-2 MICRONIZATION-3 NH 4 + Sorption Capacity mmol/g 0.48 0.78 0.94
  • micronized samples were analyzed for particle size (Malvern MasterSizer 2000), while the extent of crystalline disorder of particles was quantified with isothermal calorimetry (IC TAM 3, TA instruments, USA). Data was recorded with proprietary software Digitam 4.2.
  • Table 4 shows the influence of the various shapes of hitting elements of different micronizing discs ( Figures 5, 6 and 8 ) on ursolic acid particle size after five repeated micronization procedures.
  • Table 4 MICRONIZATION-1 MICRONIZATION-2 MICRONIZATION-3 Particles size ( ⁇ m) Volume (%) under Volume (%) under Volume (%) under 0.105 0.00 0.00 0.00 0.120 0.00 0.00 0.138 0.00 0.00 0.00 0.158 0.00 0.00 0.28 0.182 0.00 0.00 1.38 0.209 0.00 0.12 2.73 0.240 0.00 0.46 3.69 0.275 0.01 1.19 5.39 0.316 0.06 1.97 8.42 0.363 0.23 2.83 11.76 0.417 0.50 4.09 14.01 0.479 0.87 5.36 19.32 0.550 1.12 7.01 25.19 0.631 2.02 9.13 31.12 0.724 3.29 11.51 36.14 0.832 4.78 13.61 42.72 0.955 6.12 16.29 50.02 1.096 8.44 19.17 59.80
  • Table 5 shows the influence of the various shapes of hitting elements from different micronizing discs ( Figures 3, 4 and 5 ) on amorphous content of ursolic acid after five repeated micronization procedures.
  • Table 5 MICRONIZATION-1 MICRONIZATION-2 MICRONIZATION-3 Amorphous Content (%, w/w) 3.68 6.12 19.23
  • the discs and hitting elements from the micronization device of the present invention can be built from various materials such as stainless steel 316, tungsten carbide or similar depending on the hardness of the materials to be micronized.
  • the micronization device of the present invention can be successfully used for milling of pure substances or mixtures of several substances, organic, inorganic or mixed compositions. Specifically it can be used for the processing of substances from the classes of raw materials, intermediates or final products in pharmaceutical, cosmetic, food, agrochemical or construction industry, in various kinds of chemical industries, agriculture, and in other fields of production.
  • a micronization process could induce defects in the crystalline network: these defects and increase of amorphous surface can improve the dissolubility of poorly soluble drugs.
  • poorly soluble drugs For example one such pharmaceutically active poorly soluble substance, is anti-ursodeoxycholic acid (UDCA).
  • UDCA's solubility can be significantly improved by the use of the present device in a cost effective way, thus achieving better oral bioavailability.
  • the present invention can potentially enhance qualitative characteristics of various food ingredients, enabling cost-effective production processes and avoiding the need for chemical interventions.
  • Micronizing macromolecular compounds can result in their more efficient processing, better solubility and oral bioavailability.
  • modified molecules positively influence taste and nutritive characteristics.
  • Micronized polysaccharides with high molecular mass can also improve gelling characteristic and stability of gelatinous substances. Ratio of soluble fibers in food can be also increased by application of the present invention (breakage of chains, surface area increase) which is otherwise established only by addition of enzymes and implementation of heating process.
  • the prior use of the present device on those substances can significantly improve related extraction time/quality and reduce the need for organic solvents due to smaller raw material particle size, increase of specific surface (better contact of solvent and raw material) and breakage of the bonds between active ingredient and raw material.
  • the present device can be also used for cost-effective processing of silica (including desert sand) to achieve more reactive nano size particles that can be used as advanced concrete additive for improvement of concrete properties or as added in certain percentage for brick production.
  • silica including desert sand
  • Such prepared samples of micronized Pterostilbene were subjected to particles size analyses and water solubility measurement. Average particle size after seven repeated processes of micronization were around 0.4 ⁇ m and significantly increased amorphous surface ratio (34% w/W). Solubility increased from 23 ⁇ g/ml, to 128 ⁇ g/ml.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crushing And Pulverization Processes (AREA)
  • Crushing And Grinding (AREA)
EP12177709.8A 2012-07-24 2012-07-24 Modifizierte Mikronisierungsvorrichtung und ihre Verwendung Active EP2689855B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DK12177709.8T DK2689855T3 (en) 2012-07-24 2012-07-24 Mikroniseringsindretning modified, and the use thereof
EP12177709.8A EP2689855B1 (de) 2012-07-24 2012-07-24 Modifizierte Mikronisierungsvorrichtung und ihre Verwendung

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EP12177709.8A EP2689855B1 (de) 2012-07-24 2012-07-24 Modifizierte Mikronisierungsvorrichtung und ihre Verwendung

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EP2689855A1 true EP2689855A1 (de) 2014-01-29
EP2689855B1 EP2689855B1 (de) 2015-07-01

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2563693C1 (ru) * 2014-07-08 2015-09-20 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Белгородский государственный технологический университет им. В.Г. Шухова" Дезинтегратор
WO2018121803A1 (en) 2016-12-28 2018-07-05 Houdek Jan Device and method for micronization of solid materials
JP2020510531A (ja) * 2017-02-24 2020-04-09 グリーンボルト ナノ インコーポレイテッドＧｒｅｅｎｖｏｌｔ Ｎａｎｏ Ｉｎｃ． ナノ粒子を形成するための装置及び方法
US11607693B2 (en) 2017-02-24 2023-03-21 Nanom Inc. Apparatus and method for forming nanoparticles

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4406409A (en) 1980-09-16 1983-09-27 Joachim Durek Disintegrator and method for the operation thereof
HRP990263A2 (hr) 1999-04-26 2009-04-30 Lelas Tihomir Uređaj za mikroniziranje materijala
WO2012025770A2 (en) * 2010-08-23 2012-03-01 Creogen D.O.O. Device for micronization of solid materials and its use

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4406409A (en) 1980-09-16 1983-09-27 Joachim Durek Disintegrator and method for the operation thereof
HRP990263A2 (hr) 1999-04-26 2009-04-30 Lelas Tihomir Uređaj za mikroniziranje materijala
WO2012025770A2 (en) * 2010-08-23 2012-03-01 Creogen D.O.O. Device for micronization of solid materials and its use

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2563693C1 (ru) * 2014-07-08 2015-09-20 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Белгородский государственный технологический университет им. В.Г. Шухова" Дезинтегратор
WO2018121803A1 (en) 2016-12-28 2018-07-05 Houdek Jan Device and method for micronization of solid materials
JP2020510531A (ja) * 2017-02-24 2020-04-09 グリーンボルト ナノ インコーポレイテッドＧｒｅｅｎｖｏｌｔ Ｎａｎｏ Ｉｎｃ． ナノ粒子を形成するための装置及び方法
JP2023022008A (ja) * 2017-02-24 2023-02-14 ナノム インコーポレイテッド ナノ粒子を形成するための装置及び方法
US11607693B2 (en) 2017-02-24 2023-03-21 Nanom Inc. Apparatus and method for forming nanoparticles

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DK2689855T3 (en) 2015-10-12

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