EP1100620B1 - Verfahren und vorrichtung zur ultrafein-mahlung und -mischung von festen materialien - Google Patents

Verfahren und vorrichtung zur ultrafein-mahlung und -mischung von festen materialien Download PDF

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Publication number
EP1100620B1
EP1100620B1 EP99939380A EP99939380A EP1100620B1 EP 1100620 B1 EP1100620 B1 EP 1100620B1 EP 99939380 A EP99939380 A EP 99939380A EP 99939380 A EP99939380 A EP 99939380A EP 1100620 B1 EP1100620 B1 EP 1100620B1
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EP
European Patent Office
Prior art keywords
grinding
additive
mixing
processed
particle sizes
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.)
Expired - Lifetime
Application number
EP99939380A
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German (de)
English (en)
French (fr)
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EP1100620A1 (de
Inventor
Reiner Weichert
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Individual
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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
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C19/186—Use of cold or heat for disintegrating
    • 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
    • B02C17/14—Mills in which the charge to be ground is turned over by movements of the container other than by rotating, e.g. by swinging, vibrating, tilting
    • 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
    • B02C23/06—Selection or use of additives to aid disintegrating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
    • Y10S977/775—Nanosized powder or flake, e.g. nanosized catalyst
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/888—Shaping or removal of materials, e.g. etching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/90—Manufacture, treatment, or detection of nanostructure having step or means utilizing mechanical or thermal property, e.g. pressure, heat

Definitions

  • the invention relates to a method and the use of a known device for ultrafine grinding and - Mix of solid materials to medium grain sizes wide less than 1 ⁇ m or on so-called nano-fineness and / or Mixture of powders with medium grain sizes in the nano range (so-called nano powder), in which the feed and an additive placed in a grinding container with loose grinding media and by means of the releasable relocatable to each other Grinding media crushed or mixed to the desired fineness and then the additive from the regrind is separated.
  • mills with loose grinding media are used. Such mills are next to ball mills, vibratory mills and agitator mills also planetary ball mills.
  • Reagglomeration has been done by adding additives to the Tries to counteract regrind. You have to shred it Material soft substances, so-called additives, z. B. rock salt (DE 35 05 024 A1) or graphite are softer or more viscous than the regrind and in which the particle fragments when crushed in dispersed Form remain distributed. This allows particles produce in the size range of well below 1 ⁇ m, i.e. nano-particles. After grinding, the soft additive is removed - with rock salt by dissolving in water, with graphite by burning.
  • the invention has for its object a method and to indicate the use of a mill known per se for this purpose, with which particles in the nanometer range are generated and / or mix completely homogeneously for which the described restrictions no longer apply and the possible uses open up for materials that have existed up to now do not crush to finenesses well below 1 ⁇ m or in the nanometer range let mix.
  • This problem is solved with a method for ultrafine grinding from solid materials to grain sizes less than 1 ⁇ m and / or for mixing powders and agglomerates with grain sizes in the nanometer range, for the feed and an additive placed in a grinding container with loose grinding media and by means of the relative movement Walls and grinding bowl walls and, if necessary, grinding tools (agitator mills) crushed or mixed to the desired fineness and then the additive is separated from the material is, according to the invention in that the grinding in cooled Atmosphere in the presence of a frozen, facing each other inert to the goods, at ambient pressure at temperatures Additive vaporizable below 50 ° C at temperatures below its melting or sublimation temperature is carried out and that then the additive is removed from the ground material by evaporation.
  • the additive should be liquid or at ambient or room temperature vaporous or gaseous and in solid state during grinding / mixing available.
  • Water-ice has become an additive or carbon dioxide ice (solid carbon dioxide) or the like Substances such as refrigerant R134a have proven particularly effective.
  • refrigerant R134a refrigerant
  • the admixture of fine-grained water-ice or solid carbon dioxide as an additive for grinding / mixing at deep Temperatures have the advantage that the ground or mixed material is treated gently and that no impurities remain. A re-agglomeration of already shredded, very much fine particles are suppressed during grinding.
  • the grinding device works discontinuously.
  • a continuous grinding is also possible with appropriate flexible heat-insulated supply and discharge lines. Furthermore must constantly pre-cooled feed and fine-grained additive generated and abandoned. The same is the finished / mixed Good to drain continuously and are gfs. discharged Separate grinding media and, if necessary, in the circuit, possibly after Classification, attributed to the grinding room.
  • the fields of application of the invention include the generation of Using nanoparticles from pharmaceutical substances in particular of solid carbon dioxide as an additive, less often of water ice. Cold grinding makes even sensitive ones Substances not harmed. A conventional one Cool grinding without the addition of additives would not lead to production of nano-particles.
  • the invention can also be used in the production of high-purity nano-particles for nanostructured materials (Ceramics, metals, nano-composite materials, optoelectronic Nano-materials). Finally, the invention is also suitable for mixing nano powders made in a different way were. Nano-particles are extremely difficult to be homogeneous to mix with each other.
  • a vibratory mill 1 has a spring-loaded support on the floor 16 Grinding container 2, the cooling jacket 3 and one Isolation 4 is completely surrounded.
  • supply and discharge of a refrigerant are in the right end wall in FIG. 1 of the cooling jacket 3 supply connections 7 and discharge connections 8 for e.g. liquid nitrogen is provided as a refrigerant.
  • On the left side of the grinding container 2 in FIG. 1 a loading and unloading opening 10 is provided is closed by a cover 11. About this an insulating plate 5 is provided which is used to open the Cover is removable.
  • the loading takes place through the opening 10 of the grinding container 2 with grinding balls, the one to be crushed pre-shredded material and lumpy, sufficient fine-grained, solidified additive in the form of water-ice or sublimed carbon dioxide or equivalent Additive such as R134a refrigerant.
  • Fig. 3 shows the flow diagram of a continuously operated Plant with a vibrating mill 1 for performing the method according to the invention.
  • the vibratory mill 1 is a Line 44 from a pre-cooling device 30 for the regrind or the mix, which is at room temperature via a Line 31 supplied and discharged through a line 32 becomes.
  • the additive is transferred to a processing device 40 a line 41 is supplied and discharged via a line 42.
  • the device 40 serves to pre-cool the additive to To bring solidification and the solidified coarser particles pre-shred to obtain a fine-grained additive.
  • the Cooling jacket supplied via line 7 liquefied nitrogen and from which the nitrogen after heating, if necessary gaseous - is withdrawn via line 8.
  • the good is continuously discharged via a line 46, the Outlet of the grinding container with a separation device for retention the grinding balls can be provided.
  • the supply line 44 and the discharge line 46 must be flexible, the supply line 44 also be isolated.
  • the finished product is placed in an additive evaporator 50, from which the finished goods via the line 52 is subtracted.
  • the good withdrawn from line 46 can if necessary, all or only fine grinding media which are not were withheld. These can then be optional fed to the feed line 44 via a return line 48 become.
  • the additive evaporator 50 exits via a line 54 the additive in vapor form and can, if necessary, again processed and used again. That over the line 52 removed finished goods can optionally be used for drying abandoned a known freeze dryer be what is required when using water ice as an additive could be.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Disintegrating Or Milling (AREA)
  • Crushing And Grinding (AREA)
EP99939380A 1998-07-17 1999-07-16 Verfahren und vorrichtung zur ultrafein-mahlung und -mischung von festen materialien Expired - Lifetime EP1100620B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19832304A DE19832304A1 (de) 1998-07-17 1998-07-17 Verfahren und Vorrichtung zur Ultrafein-Mahlung von festen Materialien
DE19832304 1998-07-17
PCT/EP1999/005089 WO2000003806A1 (de) 1998-07-17 1999-07-16 Verfahren und vorrichtung zur ultrafein-mahlung und -mischung von festen materialien

Publications (2)

Publication Number Publication Date
EP1100620A1 EP1100620A1 (de) 2001-05-23
EP1100620B1 true EP1100620B1 (de) 2004-03-17

Family

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Application Number Title Priority Date Filing Date
EP99939380A Expired - Lifetime EP1100620B1 (de) 1998-07-17 1999-07-16 Verfahren und vorrichtung zur ultrafein-mahlung und -mischung von festen materialien

Country Status (6)

Country Link
US (1) US6520837B2 (ja)
EP (1) EP1100620B1 (ja)
JP (1) JP2002520155A (ja)
AT (1) ATE261775T1 (ja)
DE (2) DE19832304A1 (ja)
WO (1) WO2000003806A1 (ja)

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US20030234304A1 (en) * 2002-06-20 2003-12-25 Weifang Miao Superfine powders and methods for manufacture of said powders
US20090011237A1 (en) * 2002-06-20 2009-01-08 Weifang Miao Superfine powders and their methods of manufacture
DE10308722A1 (de) * 2003-02-28 2004-09-09 Degussa Ag Homogenisierung von nanoskaligen Pulvern
US7578457B2 (en) * 2003-03-11 2009-08-25 Primet Precision Materials, Inc. Method for producing fine dehydrided metal particles using grinding media
US7140567B1 (en) * 2003-03-11 2006-11-28 Primet Precision Materials, Inc. Multi-carbide material manufacture and use as grinding media
GB0515088D0 (en) * 2005-07-22 2005-08-31 Imerys Minerals Ltd Particulate glass compositions and methods of production
FR2891546B1 (fr) * 2005-10-04 2010-09-03 Solvay Utilisation de particules de carbonate de calcium dans des compositions polymeriques transparentes, compositions polymeriques transparentes et procede de fabrication de ces compositions
US20070098803A1 (en) 2005-10-27 2007-05-03 Primet Precision Materials, Inc. Small particle compositions and associated methods
EP1818380A1 (de) * 2006-02-08 2007-08-15 Solvay Infra Bad Hönningen GmbH Dispersionsklebstoff
US20080227753A1 (en) * 2007-02-26 2008-09-18 Kun Lian Nano-sized Bagasse Fiber
DE102007051545A1 (de) 2007-10-29 2009-04-30 Messer Group Gmbh Verfahren und Vorrichtung zur Feinstmahlung von Feststoffen
DE102010003711B4 (de) * 2010-04-08 2015-04-09 Jesalis Pharma Gmbh Verfahren zur Herstellung kristalliner Wirkstoffpartikel
DE102010052656A1 (de) * 2010-11-26 2012-05-31 Netzsch-Feinmahltechnik Gmbh Hydraulische Mahlkugel Zu- und Abfuhr für Rührwerkskugelmühlen
US9663372B2 (en) 2011-05-16 2017-05-30 Drexel University Disaggregation of aggregated nanodiamond clusters
CA2856395C (en) 2011-11-29 2020-08-18 N-Werkz Inc. Planetary mill and method of milling
FR2986443B1 (fr) * 2012-02-03 2014-03-07 Commissariat Energie Atomique Procede de broyage fin de charge de matiere carbonee avec ajouts d'additifs, installation de traitement en continu de biomasse et application a la gazeification associee.
FR2986444B1 (fr) * 2012-02-03 2014-03-14 Commissariat Energie Atomique Procede de broyage fin de charge de matiere carbonee, installation de traitement en continu de biomasse et application a la gazeification associee.
DK3102185T3 (da) * 2014-02-03 2021-10-04 Apurano Pharmaceuticals Gmbh Nanosuspension af naturlige materialer og fremgangsmåde til fremstilling deraf
PL239876B1 (pl) * 2015-03-27 2022-01-24 Univ Warszawski Kriogeniczna misa do młyna laboratoryjnego do mielenia próbek reaktywnych
CN105437057A (zh) * 2015-12-19 2016-03-30 重庆市璧山区闳博科技有限公司 可调式研磨工装
JP2018153774A (ja) * 2017-03-21 2018-10-04 日本コークス工業株式会社 粉砕処理システム
FR3072308B1 (fr) * 2017-10-12 2019-11-15 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
US11633835B2 (en) * 2018-12-14 2023-04-25 The Boeing Company Systems for managing abrasive media in cavitated fluid
WO2022034226A1 (en) 2020-08-14 2022-02-17 Universidad De Navarra Avermectin and milbemycin compositions for inhalation
CN112452497B (zh) * 2020-11-02 2022-04-15 昆明理工大学 利用高功率电磁脉冲制备尾矿纳米颗粒的方法和装置
CN112621572A (zh) * 2020-12-16 2021-04-09 安徽恒利增材制造科技有限公司 一种高强铝合金复杂构件增材制造方法
CN114750331A (zh) * 2021-01-12 2022-07-15 上海芯密科技有限公司 一种采用高分子材料制备微米级或亚微米级填料的方法
CN114151654B (zh) * 2021-11-15 2024-01-16 阿尔博波特兰(安庆)有限公司 白水泥磨机滑履隔热结构及其安装方法

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Also Published As

Publication number Publication date
US6520837B2 (en) 2003-02-18
ATE261775T1 (de) 2004-04-15
EP1100620A1 (de) 2001-05-23
DE59908901D1 (de) 2004-04-22
WO2000003806A1 (de) 2000-01-27
JP2002520155A (ja) 2002-07-09
DE19832304A1 (de) 2000-01-20
US20010016467A1 (en) 2001-08-23

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