EP2055386A1 - Procédé et dispositif destinés au broyage fin de matières solides - Google Patents

Procédé et dispositif destinés au broyage fin de matières solides Download PDF

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Publication number
EP2055386A1
EP2055386A1 EP08105572A EP08105572A EP2055386A1 EP 2055386 A1 EP2055386 A1 EP 2055386A1 EP 08105572 A EP08105572 A EP 08105572A EP 08105572 A EP08105572 A EP 08105572A EP 2055386 A1 EP2055386 A1 EP 2055386A1
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EP
European Patent Office
Prior art keywords
grinding
grinding container
container
cryogenic refrigerant
feed material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP08105572A
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German (de)
English (en)
Inventor
Oliver Dietrich
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Messer Group GmbH
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Messer Group GmbH
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Filing date
Publication date
Application filed by Messer Group GmbH filed Critical Messer Group GmbH
Publication of EP2055386A1 publication Critical patent/EP2055386A1/fr
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating 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
    • B02C17/04Disintegrating 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 with unperforated container

Definitions

  • the invention relates to a process for fine grinding of solids, in which a feed material is placed in a grinding container with grinding bodies and comminuted by means of the relative movement of the grinding bodies relative to one another and relative to the wall of the grinding container.
  • the invention further relates to a corresponding device.
  • additives are added to the feedstock, for example common salt or graphite, which are softer than that mecanicgut are and in which the particle fragments are distributed in the milling process in dispersed form.
  • the additive is removed - in the case of common salt, for example, by dissolution in water, in the case of graphite by burning, in the case of other substances by suitable solvents which, although they remove the additive, do not attack the material to be ground. In general, however, some impurities are left behind, which is unacceptable in many products.
  • Dry ice is characterized, in addition to a low hardness of about 2 MOHS, in particular characterized by sublimation when heated without residue.
  • a ball mill is used to achieve particularly fine grain sizes.
  • the mill is cooled indirectly by means of a cooling jacket with liquid nitrogen to a temperature of -80 ° C, just below the sublimation temperature of carbon dioxide. Subsequently, the millbase is added together with dry ice particles in the mill and ground.
  • the fine material mixed with the additive is separated from the grinding media and fed to an additive evaporation plant in which the dry ice sublimates without residue to gaseous carbon dioxide.
  • an additive evaporation plant in which the dry ice sublimates without residue to gaseous carbon dioxide.
  • the addition of additives enables the production of nanoscale particles. To produce particles in the range between 1 and 10 microns, however, these methods are too expensive; Moreover, this method can not be used if it can come to a chemical reaction between the millbase and the carbon dioxide used as an additive.
  • Object of the present invention is therefore to provide a method and apparatus for producing very fine particles, in particular from materials with elastic or plastic properties in the size range between 1 and 10 microns, which / works reliably and is easy and inexpensive to implement.
  • This object is achieved in a method of the type mentioned in that the feed material is cooled during the milling process by direct contact with a fed into the grinding container cryogenic refrigerant.
  • a mill with loose grinding media is used, such as, for example, a ball, rod, vibration, agitator, agitator ball or planetary mill.
  • the millbase is placed with the grinding media in a grinding container and ground under the movement of the grinding media against each other and against the container wall.
  • grinding media are balls, Cylpeps, rods, stones or coarse Mahlgutp
  • the direct contact of the feed with the cryogenic refrigerant in the grinding container leads to a very rapid cooling of the surfaces of the feed and thus to the formation of a large temperature difference of the surfaces relative to the core of theassiteilchen.
  • the resulting internal stresses reduce the strength of the mecanicteilchen and thereby in turn favor the crushing process.
  • the grinding media are cooled after a short time and no longer remove heat from the material to be ground; the subcooling of the ground material increases its hardness and thus its grinding ability, whereby the realization of smaller grain sizes is favored, at the same time reduces the agglomeration readiness of the milled material.
  • particle sizes of less than 10 .mu.m, in particular from 1 to 3 .mu.m can be realized with a relatively low outlay on equipment, even when grinding plastic, viscoelastic and rubber-elastic materials.
  • the addition of additives can be dispensed with; This eliminates the time-consuming separation of the ground material from the additive.
  • the at least predominantly registered in the solid or liquid state refrigerant evaporates during thermal contact with the feed material or the grinding media and is then discharged or for cooling a the grinding container downstream classification unit, such as a filter or a scraper used to prevent re-agglomeration in the classification.
  • a the grinding container downstream classification unit such as a filter or a scraper used to prevent re-agglomeration in the classification.
  • care must also be taken to ensure that no chemical reaction between the grinding stock and the refrigerant is triggered unless it is intended.
  • the milled material is classified and the oversize removed during the classification is expediently returned to the mill immediately after classification.
  • the usually still cold oversize contributes to the cooling of the grinding stock to be ground and thus reduces the consumption of refrigerant.
  • the preferred cryogenic refrigerant used is liquid nitrogen.
  • the feed can be cooled down to minus 196 ° C.
  • Very low temperatures lead to an extremely high degree of dissipation of the feed, which favors the production of very small particles. This applies in particular to partially vulcanized elastomers whose reactivity is already reduced at temperatures below -20 ° C. in such a way that fine grinding becomes possible and the flowability is essentially retained even after the grinding.
  • the supply of the cryogenic refrigerant is regulated in dependence on a temperature measured in the grinding container.
  • a further development of the invention provides that the cryogenic refrigerant, which is introduced into the grinding container in the liquid or solid state and evaporates on contact with the feed material and / or the grinding media and / or the wall of the grinding container, produces an overpressure relative to the outside atmosphere in the grinding container.
  • the evaporating refrigerant thus forms an inert gas atmosphere in the grinding container; Due to the overpressure, which may also be a rather slight overpressure of less than 0.1 bar, the penetration of moisture and / or atmospheric oxygen from the outside atmosphere is effectively prevented.
  • the object of the invention is also achieved by a device for fine grinding of solids, with a grinding container for receiving grinding media and a feed material to be ground and with a task unit for supplying the feed to the grinding container, which is characterized in that the task unit and / or Grist container is assigned a feed for a cryogenic refrigerant.
  • the only drawing ( Fig. 1 ) shows a schematic view of an inventive device for producing fines.
  • the apparatus 1 shown in the drawing is a grinding mill in which the feed material in the interior of a grinding container 2 by means of freely movable grinding media 3, such as balls, Cylpeps, rods, stones or coarse feed material particles, by mechanical stress of the feed material between the Mahl morn be comminuted with each other and / or between the grinding media 3 and the inner wall of the grinding container 2.
  • the grinding container 2 is in the exemplary embodiment to a rotatably mounted about its longitudinal axis 4 drum with thermally insulated or cooled walls. By rotation of the grinding container 2, the grinding media 3 located inside move together with the feed material and carry out the mentioned comminuting work.
  • the feed material is fed to the grinding container 2 by means of a feed unit 5.
  • the task unit 5 comprises a metering device, for example a screw 6, by means of which a precisely predetermined amount of feed material can be supplied to the grinding container 2 via a shaft 7.
  • a vortex screw cooler can be used, in which the feed material is already pre-cooled before being fed to the grinding container.
  • a retaining screen 9 In one of the task unit 5 opposite section of the grinding container 2 is a retaining screen 9, the mesh size is smaller than the diameter of the grinding media 3 is selected and thus the grinding media 3 inside holds back the grinding container.
  • the retention screen 9 separates in the grinding container 2 from the actual grinding area from a rear portion 10, in which a pouring opening 11 is provided for the ground Good.
  • the rear portion 10 of the grinding container 2 is rotatably received in a chute 12, in such a way that the ground material is introduced from the pouring opening 11 into the chute 12.
  • a device for sifting and filtering At the chute 12 is followed in a manner not shown here, a device for sifting and filtering. From the device for sifting and filtering can - in here also not shown way - return a return line to the task unit 5, which makes it possible to feed ground material with a grain size above a predetermined maximum value (oversize) of the re-grinding.
  • a supply line 14 which is in a manner not shown here with a source of cryogenic refrigerant in combination.
  • the cryogenic refrigerant used is preferably a cryogenic liquefied gas, for example nitrogen.
  • the supply line 14 is preferably equipped with a thermal insulation.
  • a cryogenic refrigerant and another liquefied gas can be used, for example, carbon dioxide, which is introduced under pressure and relaxes upon entry into the shaft 7 under strong cooling; In this case, at the confluence of the supply line 14 in the shaft 7 to provide a relaxation nozzle.
  • the source of the cryogenic refrigerant is, for example, a tank or a pipeline.
  • a valve 15 is further provided, which is connected via a control circuit 16 with a device 17 for temperature detection.
  • the optionally pre-cooled feed material is introduced via the metering unit 5 and the shaft 7 into the grinding container 2 and comminuted by mechanical loading by the grinding bodies 3.
  • the cryogenic refrigerant is introduced in the liquid state into the shaft 7 and from there into the grinding container 2 via the supply line 14.
  • the feed material in the shaft 7 and the feed material and the grinding media 3 in the grinding container 2 are cooled to a low temperature of, for example, minus 120 ° C. or below. Due to the strong cooling, the feed material in the grinding container. 2 be reliably ground to particle sizes of 1 to 3 microns.
  • the cooled and ground material is fed via the chute 12 to the sifting and filtering device.
  • the cryogenic refrigerant vaporizes to form a certain overpressure in the grinding container 2 and flows via the pouring opening 11 into the chute 12. From there it is passed through the device for filtering and sifting through and then optionally supplied to a further use, for example for the pre-cooling of the feedstock.
  • the device for sifting and filtering is cooled to a very low temperature, in which the flowability of the ground particles is maintained.
  • the device for filtering and screening is preferably also equipped with a thermal insulation or cooling. Via the control circuit 16, the temperature in the interior of the grinding container 2 can be set to a predetermined value or varied according to a predetermined program.
  • the device 1 it is possible to easily and inexpensively produce and classify fines with a particle size of 1 to 3 ⁇ m in the case of solids, in particular also with chemically active substances and substances having plastic or elastic properties.
  • the chemical and physical reactivity of the material to be ground, if present is reduced during the entire process and the risk of re-agglomeration is reduced.
  • the ingress of atmospheric moisture and / or atmospheric oxygen during the grinding process is effectively suppressed.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crushing And Grinding (AREA)
  • Disintegrating Or Milling (AREA)
EP08105572A 2007-10-29 2008-10-15 Procédé et dispositif destinés au broyage fin de matières solides Withdrawn EP2055386A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE200710051545 DE102007051545A1 (de) 2007-10-29 2007-10-29 Verfahren und Vorrichtung zur Feinstmahlung von Feststoffen

Publications (1)

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EP2055386A1 true EP2055386A1 (fr) 2009-05-06

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140341772A1 (en) * 2013-05-16 2014-11-20 Kennametal lndia Limited Methods Of Milling Carbide And Applications Thereof
CN105381848A (zh) * 2015-12-22 2016-03-09 常熟市方塔涂料化工有限公司 卧式涂料研磨机
WO2019073172A1 (fr) * 2017-10-12 2019-04-18 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procédé de broyage cryogénique avec média de broyage sous forme de gaz cryogénique solidifié
EP3608025A1 (fr) * 2018-08-09 2020-02-12 Synron Gmbh Dispositif de refroidissement et de broyage d'articles à traiter
CN113546745A (zh) * 2021-06-22 2021-10-26 国家能源集团宁夏煤业有限责任公司 制备聚合物粉末的深冷粉碎装置和深冷粉碎方法
CN113769845A (zh) * 2021-09-18 2021-12-10 方运平 一种超低温脱水粉碎机构、城市污泥的处理方法及其应用
CN116332385A (zh) * 2023-04-11 2023-06-27 南方环境科技(杭州)有限公司 一种高效一体化医疗废水处理设备

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010012448A1 (de) * 2010-03-24 2011-09-29 Messer Group Gmbh Verfahren und Vorrichtung zum Kaltmahlen
DE102015111488A1 (de) * 2015-07-15 2017-01-19 Thyssenkrupp Ag Verfahren zur Aufbereitung von Ersatzbrennstoff sowie ein Verfahren zur anschließenden Analyse des Ersatzbrennstoffs
CN108212407A (zh) * 2018-02-08 2018-06-29 西安航空学院 一种低温多级超微粉碎设备及方法

Citations (4)

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Publication number Priority date Publication date Assignee Title
US3734412A (en) * 1970-12-16 1973-05-22 Kloeckner Humboldt Deutz Ag Method and arrangement for performing low-temperature grinding operations in a vibrating mill
US3785575A (en) * 1970-11-21 1974-01-15 Kloeckner Humboldt Deutz Ag Vibrating mill with introduction of refrigerants into the solid material being ground in the grinding chamber
US5513809A (en) * 1995-07-03 1996-05-07 Tdf, Inc. Cryogenic vibratory mill apparatus
DE19832304A1 (de) 1998-07-17 2000-01-20 Reiner Weichert Verfahren und Vorrichtung zur Ultrafein-Mahlung von festen Materialien

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4220014A1 (de) * 1992-06-19 1993-12-23 Messer Griesheim Gmbh Verfahren zur Feinmahlung in Apparaten mit Mahlkörpern

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3785575A (en) * 1970-11-21 1974-01-15 Kloeckner Humboldt Deutz Ag Vibrating mill with introduction of refrigerants into the solid material being ground in the grinding chamber
US3734412A (en) * 1970-12-16 1973-05-22 Kloeckner Humboldt Deutz Ag Method and arrangement for performing low-temperature grinding operations in a vibrating mill
US5513809A (en) * 1995-07-03 1996-05-07 Tdf, Inc. Cryogenic vibratory mill apparatus
DE19832304A1 (de) 1998-07-17 2000-01-20 Reiner Weichert Verfahren und Vorrichtung zur Ultrafein-Mahlung von festen Materialien

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140341772A1 (en) * 2013-05-16 2014-11-20 Kennametal lndia Limited Methods Of Milling Carbide And Applications Thereof
CN104162476A (zh) * 2013-05-16 2014-11-26 钴碳化钨硬质合金印度有限公司 碾磨碳化物的方法及其应用
US10040123B2 (en) * 2013-05-16 2018-08-07 Kennametal India Limited Methods of milling carbide and applications thereof
CN105381848A (zh) * 2015-12-22 2016-03-09 常熟市方塔涂料化工有限公司 卧式涂料研磨机
WO2019073172A1 (fr) * 2017-10-12 2019-04-18 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procédé de broyage cryogénique avec média de broyage sous forme de gaz cryogénique solidifié
FR3072308A1 (fr) * 2017-10-12 2019-04-19 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procede de broyage cryogenique avec media de broyage sous forme de gaz cryogenique solidifie
JP2021508285A (ja) * 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 固化した低温ガスの形態の粉砕媒体を用いた低温粉砕のための装置及び方法
EP3608025A1 (fr) * 2018-08-09 2020-02-12 Synron Gmbh Dispositif de refroidissement et de broyage d'articles à traiter
CN113546745A (zh) * 2021-06-22 2021-10-26 国家能源集团宁夏煤业有限责任公司 制备聚合物粉末的深冷粉碎装置和深冷粉碎方法
CN113769845A (zh) * 2021-09-18 2021-12-10 方运平 一种超低温脱水粉碎机构、城市污泥的处理方法及其应用
CN116332385A (zh) * 2023-04-11 2023-06-27 南方环境科技(杭州)有限公司 一种高效一体化医疗废水处理设备

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