EP0618065B1 - Verfahren zum Verdichten von pulverförmigen Stoffen - Google Patents

Verfahren zum Verdichten von pulverförmigen Stoffen Download PDF

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Publication number
EP0618065B1
EP0618065B1 EP94100782A EP94100782A EP0618065B1 EP 0618065 B1 EP0618065 B1 EP 0618065B1 EP 94100782 A EP94100782 A EP 94100782A EP 94100782 A EP94100782 A EP 94100782A EP 0618065 B1 EP0618065 B1 EP 0618065B1
Authority
EP
European Patent Office
Prior art keywords
pressure vessel
powder
receptacle
powdered
compression
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
EP94100782A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0618065A1 (de
Inventor
Gerhard Dr. Sextl
Sabine Bartelt
Klaus Wilmes
Roland Reuter
Rudolf Dr. Schwarz
Friedel Worch
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.)
Evonik Operations GmbH
Original Assignee
Degussa 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 Degussa GmbH filed Critical Degussa GmbH
Publication of EP0618065A1 publication Critical patent/EP0618065A1/de
Application granted granted Critical
Publication of EP0618065B1 publication Critical patent/EP0618065B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B11/00Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
    • B30B11/001Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a flexible element, e.g. diaphragm, urged by fluid pressure; Isostatic presses

Definitions

  • the invention relates to a method for compacting powdery substances to a predetermined range of bulk density, the powder structure of the powder being retained.
  • the object was to find a method and a device for compacting powdery substances to a predetermined range of the bulk density, the powder structure of the powder being retained and shaped bodies, such as clods, lumps or the like, formed during the compaction by the powder coalescing. , be avoided or disintegrate again without significant mechanical influence.
  • the invention relates to a method for compacting powdery substances to a predetermined range of bulk density, the powder structure of the powder being retained, which is characterized in that the powdery substance is hermetically sealed in a container provided with a flexible, gas-impermeable wall (4) encloses this container in a closed pressure vessel (5), the space between the outer wall of the pressure vessel (5) and the container is acted upon by compressed gas, the pressure for a certain time maintained, relaxed and optionally removed the powdery substance with the container from the pressure vessel (5).
  • the container which has a flexible gas impermeable wall, can be a bag, a tube welded at the ends, a sack, a packet or the like.
  • the external form is of minor importance. It is essential that its wall does not allow gas to pass through.
  • the container containing the pulverulent substance when the pressure in the pressure vessel rises, the container containing the pulverulent substance is compressed from all sides (quasi isostatically) until the pressures in the pressure vessel and container are equal, with no gas exchange between the bag and the pressure vessel.
  • the container also compresses the powdery substance to a smaller volume.
  • the bag inflates again to the initial volume, but the powdery substance maintains the smaller volume.
  • the compression processes are shown schematically in FIG. 1 (phases 1 to 3).
  • the method according to the invention can be applied to all known powdery substances that can be pressed. It can be used advantageously for compacting synthetic silicas, such as precipitated silicas or pyrogenically produced silicas, and / or outside. In particular, it can be used to compact ground, such as Use air-blasted and / or steam-blasted precipitated silicas.
  • the process according to the invention has the advantage that a very homogeneously compacted powder is obtained.
  • the degree of compaction can be set to a specific range of bulk density.
  • the bulk density can be set in a targeted manner in the range from 50 to 95 g / l.
  • Another object of the invention is a device for compacting powdery substances to a predetermined range of bulk density, the powder structure of the powder being retained, which is characterized in that it consists of a preferably vertically arranged pressure vessel (5) which can be any, preferably has a circular cross-section, on the upper and on the lower cross-sectional side each has a hermetically closable opening (2), (3), and on the inside is equipped with a flexible, preferably tubular container made of gas-impermeable material (4), also open at the top and bottom is exists.
  • a pressure vessel (5) which can be any, preferably has a circular cross-section, on the upper and on the lower cross-sectional side each has a hermetically closable opening (2), (3), and on the inside is equipped with a flexible, preferably tubular container made of gas-impermeable material (4), also open at the top and bottom is exists.
  • the device can be arranged in a pipeline which carries the powdery substance.
  • the compacted powder which is present directly after the compacting process as a compacted molding or shaped body, and its shape may also form after the pressure has been released Maintaining an inelastic deformation can disintegrate into powder again without any significant mechanical effort, the actual powder structure being unchanged except for the bulk density.
  • the inventive method and the inventive device have the advantage that no mechanical parts are used to build up the pressure. Mechanical wear on the device cannot therefore occur.
  • the precipitated silica FK 500 DS manufactured by Degussa AG, Frankfurt, is used in the implementation of the example.
  • This precipitated silica has the following physico-chemical characteristics: Surface according to BET 1) m 2 / g 450 Medium size of the agglomerates ⁇ m 3.5 8) Ramming density 2) g / l 70 to 80 Loss of drying when leaving the delivery plant (2 h at 1000 ° C) 3) % 3rd Loss on ignition (2 h at 1000 ° C) 4) 9) % 5 pH value (in 5% aqueous dispersion) 5) 6.5 DBP absorption 6 ) 9) g / 100 g 330 SiO 2 10) % 98.5 Na 2 O 10) % 0.6 Fe 2 O 3 10) % 0.03 SO 3 10) % 0.7 Sieve residue (according to Mocker, 45 ⁇ m) 7) % 0.02 1) according to DIN 66 131 2) according to DIN ISO 787 / XI,
  • a cylindrical blast pressure vessel (autoclave) with a hemispherical bottom and a volume of approx. 50 l is available for the tests ( ⁇ : approx. 300 mm with a length of 700 mm).
  • the pressure vessel can be closed with a removable lid after inserting a rubber seal using 12 screws.
  • a pressure measuring device and a ball valve are flanged to the cover.
  • the autoclave can be completely vented using the ball valve before opening.
  • the connection for the compressed air supply is located on the side of the steel cylinder.
  • the autoclave is designed for a maximum operating pressure of approximately 10 bar; a corresponding pressure relief valve is installed.
  • PE bags are filled almost completely with the precipitated silica (weight: 1,200 g) and sealed.
  • the bags are dimensioned so that they fill about 80% of the autoclave volume when filled (the distance between the PE bag and the autoclave wall is around 3 to 5 cm). After placing a bag in the autoclave, the autoclave is closed.
  • the desired test pressure (1 bar to max. 4 bar overpressure) is set by carefully opening and interrupting the compressed air supply in good time. After the selected dwell time (0.5 to 3 min), the autoclave is slowly vented and then opened.
  • the PE bag polyethylene bag
  • the PE bag is only partially filled with precipitated silica after the compression tests, in contrast to before.
  • the compressed precipitated silica is partly in powder and partly in the form of soft clods. The clods disintegrate into powder even with slight mechanical stress. Samples are taken from the compressed precipitated silica and the bulk, tamped and clod densities are measured immediately.
  • the dwell times are varied with undried precipitated silica, in each case at 1, 1.5 and 2 bar compression overpressure; with dried precipitated silica FK 500 DS, the compression behavior is examined at 4 bar. The results are shown graphically in FIG.
  • the test results on the influence of the weight (autoclave filling) on the compression of FK 500 DS are summarized in Table 4.
  • the compression conditions for undried FK 500 DS are 2 bar overpressure with a residence time of 1.5 minutes, those for dried precipitated silica 4 bar overpressure with a residence time of 0.5 min.
  • the parameters are chosen so that approximately comparable degrees of compaction result for the dried and undried precipitated silica. The results are shown graphically in FIG.
  • Table 5 Measure to loosen silica Silica property Tamped density range (compressed silica) before loosening test (g / l) Change in tamped density after loosening attempt (g / l) a. free fall through pipe undried ⁇ 85 - 5th > 85 ⁇ 0 b. Snail dosing dried ⁇ 90 - 5th > 90 ⁇ 0
  • FIG. 5 shows an embodiment of the method and the device according to the invention.
  • the pulverulent substance is filled through the filling funnel 1.
  • the discharge valve 2 or flap
  • the filling slide 3 or flap
  • the powdery substance is in the space made by the filling slide 3, the discharge slide 2 and the compression membrane 4 made of rubber was formed.
  • the compression membrane 4 is tubular and its dimensions match the interior of the pressure vessel 5, which is attached to the frame 6. Compressed air is now introduced via the connection 7 into the space between the compression membrane 4 and the wall of the pressure vessel 5 until a pressure of 0.1 to 8 bar is set. This pressure is maintained over a longer period of time.
  • the compressed air is released via the outlet valve 8.
  • the discharge slide 2 is opened and the pulverulent substance is emptied into the filling container.
  • Complete emptying can be achieved by light pressure surges in the space between the pressure vessel wall 5 and the compression membrane 4 with the emptying slide 2 open.
  • the compression membrane 4 can expand depending on the pressure ratio (overpressure or underpressure) set in the intermediate space, so that the space enclosed by the compression membrane 4 becomes larger or smaller.
  • the expandable compression membrane 4 it is possible to suck the powder to be compressed into the device through the filler opening 1 when the filling slide 3 is open by applying negative pressure in the intermediate space.

Landscapes

  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Silicon Compounds (AREA)
  • Steroid Compounds (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Aiming, Guidance, Guns With A Light Source, Armor, Camouflage, And Targets (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Basic Packing Technique (AREA)
  • Disintegrating Or Milling (AREA)
  • Fats And Perfumes (AREA)
  • Containers And Packaging Bodies Having A Special Means To Remove Contents (AREA)
EP94100782A 1993-03-27 1994-01-20 Verfahren zum Verdichten von pulverförmigen Stoffen Expired - Lifetime EP0618065B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4309995 1993-03-27
DE4309995A DE4309995A1 (de) 1993-03-27 1993-03-27 Verfahren zum Verdichten von pulverförmigen Stoffen

Publications (2)

Publication Number Publication Date
EP0618065A1 EP0618065A1 (de) 1994-10-05
EP0618065B1 true EP0618065B1 (de) 1996-07-24

Family

ID=6484018

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94100782A Expired - Lifetime EP0618065B1 (de) 1993-03-27 1994-01-20 Verfahren zum Verdichten von pulverförmigen Stoffen

Country Status (11)

Country Link
US (2) US5580537A (enrdf_load_stackoverflow)
EP (1) EP0618065B1 (enrdf_load_stackoverflow)
JP (1) JP2519021B2 (enrdf_load_stackoverflow)
KR (1) KR0167807B1 (enrdf_load_stackoverflow)
AT (1) ATE140653T1 (enrdf_load_stackoverflow)
AU (1) AU671714B2 (enrdf_load_stackoverflow)
DE (2) DE4309995A1 (enrdf_load_stackoverflow)
DK (1) DK0618065T3 (enrdf_load_stackoverflow)
ES (1) ES2092340T3 (enrdf_load_stackoverflow)
GR (1) GR3020727T3 (enrdf_load_stackoverflow)
TW (1) TW240193B (enrdf_load_stackoverflow)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101437756B (zh) * 2006-01-25 2012-08-29 赢创德固赛有限责任公司 经压实产生外皮的热解制得的二氧化硅

Families Citing this family (19)

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IES940660A2 (en) * 1994-08-23 1996-01-24 Faircove Systems Improvements in and relating to dispensing apparatus
US6032300A (en) * 1998-09-22 2000-03-07 Brock Usa, Llc Protective padding for sports gear
US5920915A (en) * 1998-09-22 1999-07-13 Brock Usa, Llc Protective padding for sports gear
US6239197B1 (en) 1999-04-23 2001-05-29 Great Lakes Chemical Corporation Vacuum de-aerated powdered polymer additives
US7662468B2 (en) 2000-10-06 2010-02-16 Brock Usa, Llc Composite materials made from pretreated, adhesive coated beads
GB2380737A (en) * 2001-10-10 2003-04-16 Imerys Minerals Ltd Process for incorporating compacted calcium carbonate filler into a thermoplastic
US20040112456A1 (en) * 2002-12-16 2004-06-17 Bates James William Densification of aerated powders using positive pressure
US20050089678A1 (en) * 2003-08-20 2005-04-28 Mead Steven R. Multi-layered floorig composite including an acoustic underlayment
US7244477B2 (en) * 2003-08-20 2007-07-17 Brock Usa, Llc Multi-layered sports playing field with a water draining, padding layer
NL1025445C2 (nl) * 2004-02-09 2005-08-10 Arodo Bvba Inrichting voor het verdichten van stroombaar vast materiaal.
US7468465B2 (en) * 2005-05-31 2008-12-23 Exxonmobil Chemical Patents Inc. Method of making mixed metal oxide containing sulfur
DE102007036389A1 (de) * 2007-07-31 2009-02-12 Evonik Degussa Gmbh Verfahren zum Verdichten von pyrogen hergestellten Oxiden
DE102008040367A1 (de) 2008-07-11 2010-02-25 Evonik Degussa Gmbh Bauteil zur Herstellung von Vakuumisolationssystemen
US8578736B2 (en) * 2008-09-23 2013-11-12 Corning Incorporated Soot radial pressing for optical fiber overcladding
US8468852B2 (en) * 2009-12-03 2013-06-25 Corning Incorporated Soot pressing for optical fiber overcladding
US8869566B2 (en) * 2010-08-27 2014-10-28 Corning Incorporated Soot radial pressing for optical fiber overcladding
US9376338B2 (en) 2013-11-14 2016-06-28 Corning Incorporated Methods and apparatuses for forming optical preforms from glass soot
US10494291B2 (en) 2014-10-23 2019-12-03 Corning Incorporated Hygroscopic additives for silica soot compacts and methods for forming optical quality glass
WO2016138052A1 (en) 2015-02-27 2016-09-01 Corning Incorporated Methods for strengthening silica soot compacts with nanoparticles

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US1372190A (en) * 1920-07-30 1921-03-22 Goodyear S Metallic Rubber Sho Apparatus for compacting pulverulent material
US3063477A (en) * 1958-02-07 1962-11-13 Clarence W Vogt Method and apparatus for filling containers
US3116137A (en) * 1958-07-01 1963-12-31 Avco Mfg Corp Hot pressed material and method of producing the same
US3094384A (en) * 1958-09-29 1963-06-18 Standard Oil Co Method of controlling properties of porous metal oxides
US3058498A (en) * 1958-11-25 1962-10-16 Clarence W Vogt Continuous feeding mechanism for filling apparatus
US2937421A (en) * 1958-12-12 1960-05-24 Taccone Pneumatic Foundry Equi Machine for making molds for centrifugal castings
US3260285A (en) * 1963-08-05 1966-07-12 Clarence W Vogt Apparatus and method for filling containers for pulverulent material
SE339536B (enrdf_load_stackoverflow) * 1967-04-28 1971-10-11 Asea Ab
US3568733A (en) * 1968-07-16 1971-03-09 Black Products Co Method and apparatus for filling bags
DE1904439A1 (de) * 1969-01-30 1970-11-05 Lohrengel Dipl Ing Heinz Schnellverschluss fuer vollautomatische isostatische Pressanlagen
CH533537A (de) * 1970-12-21 1973-02-15 Gericke & Co Vorrichtung zum Abfüllen eines Behältnisses mit verdichtetem, pulvrigem Gut
GB2074086B (en) * 1980-04-11 1983-10-12 Morris K J Moulding apparatus for compacting powered materials
US4780108A (en) * 1984-08-15 1988-10-25 General Electric Company Method for increasing bulk density of fillers
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101437756B (zh) * 2006-01-25 2012-08-29 赢创德固赛有限责任公司 经压实产生外皮的热解制得的二氧化硅

Also Published As

Publication number Publication date
US5711215A (en) 1998-01-27
DE59400438D1 (de) 1996-08-29
GR3020727T3 (en) 1996-11-30
DK0618065T3 (da) 1996-11-25
JPH071198A (ja) 1995-01-06
JP2519021B2 (ja) 1996-07-31
TW240193B (enrdf_load_stackoverflow) 1995-02-11
ATE140653T1 (de) 1996-08-15
ES2092340T3 (es) 1996-11-16
AU671714B2 (en) 1996-09-05
KR0167807B1 (ko) 1999-01-15
US5580537A (en) 1996-12-03
DE4309995A1 (de) 1994-09-29
EP0618065A1 (de) 1994-10-05
AU5909394A (en) 1994-09-29

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