WO1994000240A1 - Trituration process in devices provided with grinding bodies - Google Patents

Trituration process in devices provided with grinding bodies Download PDF

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Publication number
WO1994000240A1
WO1994000240A1 PCT/EP1993/001482 EP9301482W WO9400240A1 WO 1994000240 A1 WO1994000240 A1 WO 1994000240A1 EP 9301482 W EP9301482 W EP 9301482W WO 9400240 A1 WO9400240 A1 WO 9400240A1
Authority
WO
WIPO (PCT)
Prior art keywords
liquid
grinding
suspension
devices provided
nitrogen
Prior art date
Application number
PCT/EP1993/001482
Other languages
German (de)
French (fr)
Inventor
Wolfgang Volker
Dieter Steidl
Original Assignee
Messer Griesheim 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 Messer Griesheim Gmbh filed Critical Messer Griesheim Gmbh
Publication of WO1994000240A1 publication Critical patent/WO1994000240A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/18—Adding fluid, other than for crushing or disintegrating by fluid energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge

Definitions

  • the invention relates to a method for fine grinding in apparatus with grinding media, according to the preamble of claim 1.
  • Apparatuses with grinding media are, for example, ball mills, roller mills and in particular agitator ball mills.
  • the latter can be operated horizontally or vertically and are almost completely filled with balls.
  • the balls have very small diameters of 0.1 to 10 mm, depending on the grinding task. They can be made from ceramic, metallic or other material.
  • the balls are stirred by a central shaft and disks attached to it.
  • the invention has for its object to provide a method for fine grinding in apparatus with grinding media, which allows easy separation of the ground product and suspension liquid and facilitates the grinding of difficult to select solids such as plastics and waxes.
  • argon, oxygen, hydrogen and helium are suitable as cryogenic liquids, and also mixtures of liquid and solid carbon dioxide or of liquid nitrogen and solid carbon dioxide.
  • a plant for fine grinding of plastics is shown, in which, according to the invention, liquid nitrogen serves as the liquid for forming the suspension.
  • the system essentially consists of the ball mill 1, the mixing tank 2, the metering screw 3 and the filter 4.
  • the ball mill 1, the mixing tank 2 and the metering screw 3 are driven by the motors 5, 6 and 7.
  • the direction of flow of the material flows is indicated by arrows that are not identified in any more detail.
  • the solids to be milled go continuously from the dosing screw 3 as feed (educt) into the mixing container 2.
  • liquid nitrogen reaches the mixing container 2 through line 8 and the valve 9 provided with a level control Solids and the liquid nitrogen formed. So that this suspension does not separate due to the different weights, intensive stirring of the suspension by means of the motor 6 in the mixing container 2 is required.
  • the suspension passes through line 10 by means of the pump 11 into the ball mill 1.
  • the pump 11 is also provided with a level control.
  • the solids are finely ground in the ball mill 1 and then passed through the line 12 into the filter 4.
  • the resulting gaseous nitrogen is drawn off through line 13, the finely ground nitrogen-free product is removed through line 14 and the remaining liquid nitrogen passes through line 15 and pump 16 back into the mixing container 2.
  • Zirconium oxide balls 1-1, 5mm 0

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crushing And Grinding (AREA)

Abstract

In order to triturate solid bodies in devices provided with grinding bodies, in particular ball triturators (1) with a stirring mechanism, a suspension is formed with the solid bodies to be triturated and with a liquid, and the suspension is supplied to the device. After trituration the liquid is separated. In order to make separation easier, a liquid that evaporates without leaving residues is used, preferably a cryogenic medium such as liquid nitrogen.

Description

Verfahren zur Feinmahlung in Apparaten mit MahlkörpernProcess for fine grinding in devices with grinding media
Die Erfindung betrifft ein Verfahren zur Feinmahlung in Apparaten mit Mahlkörpern, nach dem Oberbegriff des An¬ spruches 1.The invention relates to a method for fine grinding in apparatus with grinding media, according to the preamble of claim 1.
Apparate mit Mahlkörperπ sind beispielsweise Kugelmüh¬ len, Rollenmühlen und insbesondere Rührwerkskugelmühlen Letztere können horizontal oder vertikal betrieben wer¬ den und sind fast vollständig mit Kugeln gefüllt. Die Kugeln haben entsprechend der Mahlaufgabe sehr geringe Durchmesser von 0,1 bis 10 mm. Sie können aus kerami¬ schem, metallischen oder sonstigen Material hergestellt sein. Durch eine Zentralwelle und auf ihr angebrachte Scheiben werden die Kugeln gerührt.Apparatuses with grinding media are, for example, ball mills, roller mills and in particular agitator ball mills. The latter can be operated horizontally or vertically and are almost completely filled with balls. The balls have very small diameters of 0.1 to 10 mm, depending on the grinding task. They can be made from ceramic, metallic or other material. The balls are stirred by a central shaft and disks attached to it.
Durch dieses gerührte Kugelbett wird ein Feststoff mit einer Flüssigkeit hindurchgepumpt. Entsprechend der Verweilzeit und einer Reihe anderer veränderlicher Parameter wird der Feststoff auf dem Weg durch die Müh¬ le gemahlen. Die Austragsstelle für die Flüssigkeit ist mit einem Sieb versehen, um das Hinausschleppen von Ku¬ geln zu verhindern. Somit ist gewährleistet, daß die für die Mahlung erforderlichen Kugeln in der Mühle ver¬ bleiben .Through this stirred ball bed is a solid pumped through a liquid. Depending on the residence time and a number of other variable parameters, the solid is ground on the way through the mill. The discharge point for the liquid is provided with a sieve to prevent balls from being dragged out. This ensures that the balls required for grinding remain in the mill.
Mit derartigen Apparaten lassen sich an sich sehr große Kornfeinheiten erreichen. Schwierigkeiten bereitet ins¬ besondere bei derartigen großen Kornfeinheiten die Ab¬ trennung der Suspensionsflüssigkeit, welche adsorptiv an den großen Oberflächen gebunden ist. Als Suspensions¬ flüssigkeit werden überwiegend Wasser und organische Lösungsmittel verwendet. Zu deren Abtrennung ist ein großer Aufwand nötig, beispielsweise Trocknung und Destillation. Die Schwierigkeiten steigen noch, wenn es sich um schwervermahlbare Feststoffe, vor allem Kunst¬ stoffe und Wachse, handelt.With such apparatus, very large grain sizes can be achieved. Difficulties arise in particular in the case of such large grain finenesses in the separation of the suspension liquid, which is adsorptively bound to the large surfaces. Water and organic solvents are predominantly used as the suspension liquid. A great deal of effort is required to separate them, for example drying and distillation. The difficulties increase when it comes to hard-to-grind solids, especially plastics and waxes.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Feinmahlung in Apparaten mit Mahlkörpern zu schaf¬ fen, welches eine leichte Trennung von gemahlenem Pro¬ dukt und Suspensionsflüssigkeit gestattet und die Ver¬ mahlung schwerver ahlbarer Feststoffe wie Kunststoffe und Wachse erleichtert.The invention has for its object to provide a method for fine grinding in apparatus with grinding media, which allows easy separation of the ground product and suspension liquid and facilitates the grinding of difficult to select solids such as plastics and waxes.
Ausgehend von dem im Oberbegriff des Anspruches 1 be¬ rücksichtigtem Stand der Technik ist diese Aufgabe er¬ findungsgemäß gelöst mit den im kennzeichnenden Teil des Anspruches 1 angegebenen Merkmalen.Starting from the prior art taken into account in the preamble of claim 1, this object is achieved according to the invention with the features specified in the characterizing part of claim 1.
Vorteilhafte Weiterbildungen der Erfindung sind in den Unteransprüchen angegeben. Infolge der erfindungsgemäßen Maßnahme, die Vermahlung mit einer bei atmosphärischen Bedingungen rückstands¬ frei verdampfenden Flüssigkeit durchzuführen, läßt sich die Trennung von feingemahlenem Produkt und Flüssigkeit ohne Schwierigkeiten und ohne großen Aufwand durchfüh¬ ren. Besonders geeignet sind kryogene Flüssigkeiten, insbesondere flüssiger Stickstoff, da sie einerseits die Mahlbarkeit wegen der Abkühlung der Feststoffe ver¬ bessern, andererseits besonders leicht vom gemahlenen Produkt durch Verdampfen entfernt werden können.Advantageous developments of the invention are specified in the subclaims. As a result of the measure according to the invention of carrying out grinding with a liquid which evaporates residue-free under atmospheric conditions, the separation of finely ground product and liquid can be carried out without difficulty and without great effort. Cryogenic liquids, in particular liquid nitrogen, are particularly suitable since they on the one hand improve the grindability due to the cooling of the solids, on the other hand can be removed particularly easily from the ground product by evaporation.
Außer Stickstoff sind als kryogene Flüssigkeiten Argon, Sauerstoff, Wasserstoff und Helium geeignet, ferner Mischungen aus flüssigem und festen Kohlendioxid oder aus flüssigem Stickstoff und festen Kohlendioxid.In addition to nitrogen, argon, oxygen, hydrogen and helium are suitable as cryogenic liquids, and also mixtures of liquid and solid carbon dioxide or of liquid nitrogen and solid carbon dioxide.
Grundsätzlich ändert sich an der Verfahrenstechnik der Mahlung nichts, wenn ein Feststoff, suspendiert in einer kryogenen Flüssigkeit, beispielsweise in einer Kugelmühle, vermählen wird. Aufgrund der tiefen Tempera¬ turen und der Besonderheiten einer sehr kalten aber leicht verdampfbaren Flüssigkeit müssen einige zusätz¬ liche Maßnahmen ergriffen werden. Insbesondere ist zu berücksichtigen, daß bei der Mahlung durch das Anein¬ anderreihen der Mahlkörper Wärme auf die Flüssigkeit übertragen wird und diese verdampft, wenn beispiels¬ weise flüssiger Stickstoff unter atmosphärischen Be¬ dingungen in der Mühle gehalten wird. Dieser ver¬ dampfende Stickstoff wird in einem nachgeschalteten Filtersystem, in welchem die Flüssigkeit vom Produkt getrennt wird, als Gas aus dem Prozeß entlassen. Zu einer nachteiligen Entmischung auf Grund unterschied¬ licher spezifischer Gewichte kann es nicht kommen, da infolge der Zwangsströmung und die Widerstände der Ku¬ gelpackungen starke Mischkräfte auftreten. Die Zeichnung veranschaulicht ein Ausführungsbeispiel der Erfindung anhand eines Verfahrensschemas.Basically, nothing changes in the process technology of grinding if a solid suspended in a cryogenic liquid, for example in a ball mill, is ground. Due to the low temperatures and the special features of a very cold but easily evaporable liquid, some additional measures have to be taken. In particular, it should be taken into account that during grinding, the grinding elements are lined up and heat is transferred to the liquid and this evaporates when, for example, liquid nitrogen is kept in the mill under atmospheric conditions. This evaporating nitrogen is released as gas from the process in a downstream filter system in which the liquid is separated from the product. There can be no disadvantageous separation due to different specific weights, since strong mixing forces occur as a result of the forced flow and the resistances of the ball packs. The drawing illustrates an embodiment of the invention using a process scheme.
Dargestellt ist eine Anlage zur Feinmahlung von Kunst¬ stoffen, bei der gemäß der Erfindung flüssiger Stick¬ stoff als Flüssigkeit zur Bildung der Suspension dient. Die Anlage besteht im wesentlichen aus der Kugelmühle 1, dem Mischbehälter 2, der Dosierschnecke 3 und dem Fil¬ ter 4. Die Kugelmühle 1, der Mischbehälter 2 und die Dosierschnecke 3 werden durch die Motoren 5,6 und 7 an¬ getrieben. Die Fließrichtung der Stoffströme ist durch nicht näher gekennzeichnete Pfeile angegeben.A plant for fine grinding of plastics is shown, in which, according to the invention, liquid nitrogen serves as the liquid for forming the suspension. The system essentially consists of the ball mill 1, the mixing tank 2, the metering screw 3 and the filter 4. The ball mill 1, the mixing tank 2 and the metering screw 3 are driven by the motors 5, 6 and 7. The direction of flow of the material flows is indicated by arrows that are not identified in any more detail.
Die zu vermählenden Festkörper gelangen aus der Dosier¬ schnecke 3 kontinuierlich als Aufgabegut (Edukt) in den Mischbehälter 2. Gleichzeitig gelangt durch Leitung 8 und das mit einer Niveauregelung versehene Ventil 9 flüssiger Stickstoff in den Mischbehälter 2. Hier wird eine Suspension aus den zu mahlenden Festkörpern und dem flüssigen Stickstoff gebildet. Damit sich diese Suspension wegen der unterschiedlichen Gewichte nicht entmischt, ist eine intensive Rührung der Suspension mittels des Motors 6 im Mischbehälter 2 erforderlich. Die Suspension gelangt durch Leitung 10 mittels der Pumpe 11 in die Kugelmühle 1. Die Pumpe 11 ist eben¬ falls mit einer Niveauregelung versehen. In der Kugel¬ mühle 1 werden die Festkörper fein gemahlen und an¬ schließend durch die Leitung 12 in den Filter 4 gelei¬ tet. Der entstandene gasförmige Stickstoff wird dort durch Leitung 13 abgezogen, das feingemahlene stick¬ stofffreie Produkt wird durch Leitung 14 entfernt und der verbliebene flüssige Stickstoff gelangt durch Lei¬ tung 15 und Pumpe 16 zurück in den Mischbehälter 2.The solids to be milled go continuously from the dosing screw 3 as feed (educt) into the mixing container 2. At the same time, liquid nitrogen reaches the mixing container 2 through line 8 and the valve 9 provided with a level control Solids and the liquid nitrogen formed. So that this suspension does not separate due to the different weights, intensive stirring of the suspension by means of the motor 6 in the mixing container 2 is required. The suspension passes through line 10 by means of the pump 11 into the ball mill 1. The pump 11 is also provided with a level control. The solids are finely ground in the ball mill 1 and then passed through the line 12 into the filter 4. The resulting gaseous nitrogen is drawn off through line 13, the finely ground nitrogen-free product is removed through line 14 and the remaining liquid nitrogen passes through line 15 and pump 16 back into the mixing container 2.
Nachfolgend werden die Verfahrensdaten einer mit flüs- sigem Stickstoff gemäß der Erfindung durchgeführten Vermahlung von Polyether-Imid wiedergegeben:The process data of a sigen nitrogen according to the invention performed grinding of polyether imide:
Aufgabe 0dg7<5OOμm d50ca .200μmTask 0d g7 <5OOμm d 50 approx. 200μm
Drehzahl 1040 1/minSpeed 1040 1 / min
Zirkon-Oxid-Kugeln: 1-1, 5mm 0Zirconium oxide balls: 1-1, 5mm 0
Füllgrad: 75Vol%Degree of filling: 75vol%
Feststoff-Gehalt: 25%Solids content: 25%
Durchsatz : 35kg/hThroughput: 35kg / h
Produkt : 0d5Q=17μmProduct: 0d 5Q = 17μm
Ba/Hi MG 1845 Ba / Hi MG 1845

Claims

Ansprüche Expectations
1. Verfahren zur Feinmahlung in Apparaten mit Mahlkör¬ pern, bei welchem dem Apparat eine Suspension aus den zu mahlenden Festkörpern und einer Flüssigkeit zugeführt wird, die Festkörper durch die Bewegung der Mahlkörper im Apparat zum Produkt fein gemahlen werden, das Gemisch aus Produkt und Flüssigkeit aus dem Apparat entfernt wird und anschließend das Pro¬ dukt von der Flüssigkeit getrennt wird, dadurch gekennzeichnet, daß die Bildung der Suspension mittels einer rück- staπdsfrei verdampfenden Flüssigkeit erfolgt.1. Process for fine grinding in apparatuses with grinding media, in which a suspension of the solids to be ground and a liquid is fed to the apparatus, the solids are finely ground to the product by the movement of the grinding media in the apparatus, the mixture of product and liquid is removed from the apparatus and then the product is separated from the liquid, characterized in that the suspension is formed by means of a residue-free evaporating liquid.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die rückstandsfrei verdampfende Flüssigkeit kryogen ist.2. The method according to claim 1, characterized in that the residue-free evaporating liquid is cryogenic.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die rückstandsfrei verdampfende Flüssigkeit Stickstoff ist.3. The method according to claim 2, characterized in that the residue-free evaporating liquid is nitrogen.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Feinmahlung in einer Kugelmühle (1) statt¬ findet . 4. The method according to any one of claims 1 to 3, characterized in that the fine grinding takes place in a ball mill (1).
PCT/EP1993/001482 1992-06-19 1993-06-11 Trituration process in devices provided with grinding bodies WO1994000240A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP4220014.8 1992-06-19
DE4220014A DE4220014A1 (en) 1992-06-19 1992-06-19 Process for fine grinding in apparatus with grinding media

Publications (1)

Publication Number Publication Date
WO1994000240A1 true WO1994000240A1 (en) 1994-01-06

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WO (1) WO1994000240A1 (en)
ZA (1) ZA934327B (en)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2019073172A1 (en) * 2017-10-12 2019-04-18 Commissariat A L'energie Atomique Et Aux Energies Alternatives Device and method for cryogenic grinding with grinding media in the form of solidified cryogenic gas

Families Citing this family (5)

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Publication number Priority date Publication date Assignee Title
DE19503914C2 (en) * 1995-02-07 1998-07-30 Christian Dipl Ing Schoepe Process for crushing bituminous sheets
DE19528958A1 (en) 1995-08-08 1997-02-13 Hoechst Ag Autogenous grinding of silicon nitride
DE10144886B4 (en) * 2001-09-12 2004-02-26 Peter Endres Device for crushing regrind
DE102007051545A1 (en) * 2007-10-29 2009-04-30 Messer Group Gmbh Method and device for fine grinding of solids
FR3137590A1 (en) * 2022-07-11 2024-01-12 Commissariat A L'energie Atomique Et Aux Energies Alternatives Powder dosing process

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Publication number Priority date Publication date Assignee Title
FR1094977A (en) * 1953-11-28 1955-05-25 Very low temperature grinding plant in the presence of liquefied gases
EP0367403A2 (en) * 1988-10-03 1990-05-09 The Carborundum Company Method for grinding an oxygen sensitive ceramic material and powder obtained by this method.
US5007589A (en) * 1987-03-26 1991-04-16 Metprotech Limited Process for simultaneously leaching and fine milling a subdivided source material

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DE3345974C2 (en) * 1983-12-20 1994-03-10 Schmidt Ulrich Dr Process for grinding crystalline solids
AT381651B (en) * 1985-02-28 1986-11-10 Voest Alpine Ag METHOD FOR GRINDING MINERALS WITH A MULTI-CHAMBER TUBE MILL, AND SYSTEM FOR CARRYING OUT THE METHOD
DE3833830A1 (en) * 1988-10-05 1990-04-12 Messer Griesheim Gmbh METHOD AND DEVICE FOR COLD GRINDING

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1094977A (en) * 1953-11-28 1955-05-25 Very low temperature grinding plant in the presence of liquefied gases
US5007589A (en) * 1987-03-26 1991-04-16 Metprotech Limited Process for simultaneously leaching and fine milling a subdivided source material
EP0367403A2 (en) * 1988-10-03 1990-05-09 The Carborundum Company Method for grinding an oxygen sensitive ceramic material and powder obtained by this method.

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019073172A1 (en) * 2017-10-12 2019-04-18 Commissariat A L'energie Atomique Et Aux Energies Alternatives Device and method for cryogenic grinding with grinding media in the form of solidified cryogenic gas
FR3072308A1 (en) * 2017-10-12 2019-04-19 Commissariat A L'energie Atomique Et Aux Energies Alternatives DEVICE AND METHOD FOR CRYOGENIC MILLING WITH CRYOGENIC GAS MILLING MEDIA SOLIDIFIED
JP2021508285A (en) * 2017-10-12 2021-03-04 コミッサリア ア レネルジー アトミーク エ オ ゼネルジ ザルタナテイヴ Equipment and methods for low temperature pulverization using a pulverization medium in the form of solidified low temperature gas

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Publication number Publication date
ZA934327B (en) 1994-08-10
DE4220014A1 (en) 1993-12-23

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