EP0473942A1 - Procédé pour imprègner des particules solides avec des liants liquides et son application - Google Patents

Procédé pour imprègner des particules solides avec des liants liquides et son application Download PDF

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Publication number
EP0473942A1
EP0473942A1 EP91112939A EP91112939A EP0473942A1 EP 0473942 A1 EP0473942 A1 EP 0473942A1 EP 91112939 A EP91112939 A EP 91112939A EP 91112939 A EP91112939 A EP 91112939A EP 0473942 A1 EP0473942 A1 EP 0473942A1
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EP
European Patent Office
Prior art keywords
binder
vacuum
solids
mixing
liquid
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.)
Granted
Application number
EP91112939A
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German (de)
English (en)
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EP0473942B1 (fr
Inventor
Herbert Dürr
Walter Eirich
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.)
EIRICH, HUBERT
EIRICH, PAUL
EIRICH, WALTER
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Individual
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Publication of EP0473942A1 publication Critical patent/EP0473942A1/fr
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Publication of EP0473942B1 publication Critical patent/EP0473942B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming

Definitions

  • the binder When using preheated dry materials, the binder, also preheated, is added in liquid form. When the dryers are heated in the mixer, solid binders that are melted during the heating process can also be processed.
  • the primary grain is only impregnated to a negligible extent.
  • liquid binders into the pores of the primary grain is also made more difficult by the fact that the air contained in the pores expands during the heating and thus counteracts any capillary forces which could lead to the binding agent being sucked in.
  • the viscosity of the binder is so high that the capillary forces alone are not sufficient to suck the binder into the pores of the primary grain.
  • an increased surface tension may make it more difficult for the binder to penetrate into the pores of the primary grain.
  • binder fractions also evaporate, which are lost to the mixture and must also be disposed of.
  • undesirable oxidation phenomena and cracking processes can also occur on the binder.
  • the invention has for its object to provide a method for impregnating solids with liquid or liquefiable binders, in which the impregnation of the primary grain is achieved while avoiding the disadvantages described above.
  • the binder can be liquid at the addition temperature. However, it can also be added in powder form and only liquefy during mixing, either by supplying heat from the outside or by the heat of the material to be mixed.
  • a liquefiable binder is a synthetic resin melting at the specified temperatures.
  • preheated raw materials are used in the refractory industry and the resin is added in powder form.
  • the required thermal energy is supplied by the mechanical energy of the mixing process.
  • heated mixers can also be used.
  • the mixing process could proceed as follows: the heated mixture is added to the mixer or the mixture is heated in the mixer, whereupon a powdered binder is added and briefly premixed, whereupon a vacuum is applied and the resin powder is liquefied, followed by pressure equalization.
  • the impregnation of the primary grain with the liquid or liquefied binder takes place mainly in the pressure equalization following the vacuum treatment, in which air flows into the pores and thereby takes the liquid or liquefied binder into the pores.
  • the process according to the invention can be carried out batchwise or continuously.
  • the desiccants could be fed through a rotary valve as a pressure lock.
  • a vacuum press can be arranged in a pressure-tight manner, which ensures a pressure-tight one discharge possible. In many applications, the press can also cause the mix to be deformed or pre-deformed at the same time.
  • the above-mentioned suction of the liquid or liquefied binder into the pores of the primary grain can be carried out by temporarily equalizing or reducing the vacuum during the continuous treatment.
  • a vacuum press for example, a higher vacuum could be used in the mixing room than in the press.
  • the vacuum can also be varied in the mixer itself, either by canceling it at regular intervals by pressure equalization or by short-term mixer closure at regular intervals.
  • the intervals of reducing or increasing the vacuum must be matched to the residence time of the material to be mixed in the mixer, so that the vacuum is reduced or released at least once during the residence time of the material to be mixed in the mixer.
  • Block anodes are used in the melting tanks for the supply of the electrical energy.
  • Block anodes usually consist of a mixture of 85% petroleum coke and 15% pitch as a binder.
  • petroleum coke is either heated outside of a mixer in a suitable device to approx. 180 ° C or is introduced into the mixing room at ambient temperature and heated by external jacket heating.
  • the binder is also introduced as a liquid melt at a temperature of approx. 180 ° C into the moving mix and mixed there with the petroleum coke. This type of impregnation creates a crumbly, adhesive mass which is then pressed into anode blocks in appropriate molding presses.
  • anode blocks Before the anode blocks can be inserted into the melting tank, they have to be subjected to a further thermal treatment. They are heated to approx. 1050 to 1100 ° C, whereby the volatile components are expelled from the liquid binder components and the binder cokes.
  • the air within the porous solid part expands in accordance with the temperature development, so that the bond between binder and solid part in the micro range is disturbed. This leads to a deterioration in the electrical properties of the anode in the melting furnace, and the mechanical resistance under operating conditions is reduced.
  • the pressure at the end of the vacuum application is advantageously not only equalized to atmospheric pressure, but is increased to superatmospheric pressure. This makes it possible to completely fill the remaining volumes of the evacuated pores, which have not yet been completely filled, with binders, because a pressure difference of approx. 1 bar may not be sufficient to overcome surface tensions, etc.
  • the task of the fine powder components is to form the densest possible packing of a shaped body with the coarse-grained components by storing them in the interstices of the coarse components, it is entirely sufficient if they are added at the end of the mixing process and on the wetted surfaces of the Coarse components stick.
  • the product temperature during the preparation plays an important role in the processing of the anode mass in the molding presses. It is known to adjust the temperature of the mixture to a corresponding temperature by adding water during the mixing process and by allowing the water to evaporate.
  • the addition of water in addition to the problems resulting from the disposal of the vapors, has the further disadvantage that the complete removal of the water from the mix is problematic. Residual water in an anode mass leads to significantly deteriorated product qualities.
  • the method is therefore proposed in a further advantageous embodiment proposed to provide the binder with such an additional amount of solvent so that after the impregnation process has ended under vacuum and the evaporation of the solvent that has taken place, the desired temperature is achieved using the enthalpy of evaporation.
  • the use of solvent for cooling the anode mass has the decisive advantage that even if small residual components were left in the mass, they would also crack to carbon during the thermal aftertreatment.
  • petroleum coke is first heated to 180 ° C. either outside or inside the mixing room by external jacket heating.
  • the mixing space and the solids therein are evacuated before the binder is added, so that the air in the pores of the solids is practically completely removed.
  • the liquid binder which also has a temperature of 180 ° C, is introduced into the moving mix.
  • the mixing process is first continued under vacuum, so that the solid is wetted on all sides by the binder. Due to the air-free pores of the solids, capillary forces can be fully effective, so that the binder can penetrate into the pores.
  • the binder After the end of the vacuum process and due to the pressure equalization with the surrounding atmosphere, the binder is "pressed" into the hollow spaces of the solid particles, which are still under vacuum.
  • the proportion of binder, based on the binder can be increased by 4 to 9%.
  • the density of the anode after the pressing process and also after the thermal treatment is correspondingly higher. This leads u. a. to improved electrical properties and also to a significant increase in the service life in the melting tank.
  • a countercurrent mixer in a vacuum version with a rotating mixing container and eccentrically arranged high-speed mixing tool 800 kg of anode mass, consisting of 640 kg of petroleum coke and 160 kg of pitch, are impregnated under the conditions according to the invention.
  • the temperature of the mixed material is 170 ° C and should be reduced by 30 ° C to 140 ° C for the subsequent deformation.
  • m-cresol with the chemical formula C7 Hg 0 is used as a proportionate solvent to lower the viscosity of the binder (pitch) and to cool the mass by evaporation.
  • the specific heat of the anode mass is known at 1.05 kJ / kg and the enthalpy of vaporization of m-cresol at 423 kJ / kg.
  • the amount of solvent required for evaporative cooling can thus be calculated. According to the calculation, 59.5 kg m-cresol are required.
  • FIG. 1 denotes the vacuum mixing device shown schematically.
  • the solid, e.g. B. coke is weighed in a device not shown here and brought with the screw 2 an electrical heating device 3, which uses the electrical resistance of the coke for heating.
  • the schematically illustrated pair of electrodes for introducing the current bears the numbers 4 and 5.
  • the preheated liquid binder is added from the schematically illustrated balance 6.
  • the vacuum pump 7 is provided for generating the vacuum.
  • a condenser 8 with cooling water supply 9 and cooling water discharge 10 is arranged between vacuum pump 7 and vacuum mixing device 1.
  • the condensed solvent enters the collecting container 11 and is fed with a feed pump 12 to the metering device 13 designed as a balance. For the sake of clarity, the necessary fittings, control devices, etc. have not been shown.
  • the method described above is used analogously in the production of refractory products that are bound with tar, pitch or liquid synthetic resin, as well as in other carbon products with tar or pitch bonds, e.g. B. for graphite electrodes for arc furnaces, carbon brushes and the like.
  • the above method can also be used sensibly in mixing processes with highly porous, moisture-absorbing substances, such as. B. expanded clay, slag, brick split, etc., soft with a hydraulic binder, for. B. cement to be bound.
  • highly porous, moisture-absorbing substances such as. B. expanded clay, slag, brick split, etc.
  • a hydraulic binder for. B. cement to be bound.
  • the above-mentioned aggregates, expanded clay, slag, brick split, etc. are first evacuated so that the pores are free of air will.
  • the water is introduced under vacuum into the moving mix, which fills the cavities with water according to the principle of action described above.
  • the hydraulically setting binder e.g. B. cement
  • FIG. 2 shows an embodiment of the method according to the invention with continuous operation.
  • the vacuum mixing device has the reference symbol 21.
  • a vacuum level p1 is set with the aid of the vacuum pump 27.
  • the mixing device 21 is fed continuously from the storage containers 22 and 24.
  • the dosing is done with a differential balance.
  • a cell lock 23 is provided as a pressure shut-off device and discharge device for the solid matter in the storage container 22.
  • the liquid is also fed from the reservoir 24 using a differential balance.
  • a control valve 25 is provided between the reservoir 24 and the vacuum mixing device 21.
  • the residence time or fill level of the mixed material in the vacuum mixing device 21 is kept constant by means of a controllable discharge flap 26.
  • Appropriate level sensors can be used to control the level or the mixer can be placed on a scale.
  • the mixture emerging from the discharge flap 26 is fed via a transfer hopper 34 to a twin-screw press which has a first screw conveyor 29 driven by a drive 30 and a second screw conveyor 31 driven by a drive 33 with a mouthpiece 32.
  • the screw 29 serves on the one hand to separate the two vacuum spaces from one another, and on the other hand to achieve a certain mechanical pre-compression of the mix in front of the deformation screw.
  • the deformation screw is the screw 31.
  • a plug of mixed material in the mouthpiece 32 makes it possible to generate a vacuum p2 with the aid of the vacuum pump 28.
  • the vacuum in the vacuum mixing device 21 need not be interrupted, since when the material to be mixed passes into the screw press and thus into a room with a lower vacuum, the liquid binder penetrates into the pores of the primary grain before this Mixed material is subjected to the deformation in the screw 31 with the mouthpiece 32.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
  • Electrolytic Production Of Metals (AREA)
EP91112939A 1990-09-05 1991-08-01 Procédé pour imprègner des particules solides avec des liants liquides et son application Expired - Lifetime EP0473942B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4028078 1990-09-05
DE4028078A DE4028078A1 (de) 1990-09-05 1990-09-05 Verfahren zum impraegnieren von feststoffen mit fluessigen bindemitteln und dessen anwendung

Publications (2)

Publication Number Publication Date
EP0473942A1 true EP0473942A1 (fr) 1992-03-11
EP0473942B1 EP0473942B1 (fr) 1995-05-03

Family

ID=6413602

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91112939A Expired - Lifetime EP0473942B1 (fr) 1990-09-05 1991-08-01 Procédé pour imprègner des particules solides avec des liants liquides et son application

Country Status (4)

Country Link
EP (1) EP0473942B1 (fr)
JP (1) JP3220186B2 (fr)
CA (1) CA2048916A1 (fr)
DE (2) DE4028078A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GR1003305B (el) * 1998-12-30 2000-01-25 Μεθοδος πυρομεταλλουργικης επεξεργασιας οξυγονουχων σιδηρονικελιουχων μεταλλευματων με επιλεκτικη προσθηκη μεταλλικου αναγωγικου μεσου και προσθηκη προαναχθεντος σιδηρου - ή σιδηρονικελιουχου μεταλλευματος για βελτιωση αποδοσης νικελιου ως και ρυθμιση ..
EP1029652A1 (fr) * 1999-02-15 2000-08-23 Secmer Dispositif mélangeur sous vide pour la coulée de matériaux plastiques polymérisables
WO2002100521A1 (fr) * 2001-06-08 2002-12-19 Kansai Paint Co., Ltd. Appareil de pulverisation
EP1967258A1 (fr) * 2007-03-06 2008-09-10 Interglass Technology AG Procédé de mélange d'un liquide avec au moins deux autres substances et dégazage du mélange et pour la distribution du mélange
IT201900018311A1 (it) * 2019-10-09 2021-04-09 Eurostar Concrete Tech S P A “Mescolatrice planetaria per la produzione di agglomerati a base cementizia o di resina, in particolare calcestruzzo, e metodo di produzione di agglomerati"

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105169981B (zh) * 2015-08-12 2018-02-06 东莞兆舜有机硅科技股份有限公司 电子灌封胶生产方法
CN109764693B (zh) * 2019-01-24 2020-08-25 中南大学 一种利用烟气热量的预热方法及系统

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB587698A (en) * 1944-11-28 1947-05-02 Lionel Walker Improvements in or relating to the mixing of granular material with water
US2516436A (en) * 1944-11-28 1950-07-25 Walker Lionel Mixing of granular material with liquids
DE1220834B (de) * 1964-01-07 1966-07-14 Spangenberg Maschf G Verfahren und Vorrichtung zum Vakuummischen zur Koagulationsbildung neigender Gueter
US3429726A (en) * 1962-10-14 1969-02-25 Toshiaki Takabayashi Method of producing cement mortar or concrete
US4020154A (en) * 1973-01-22 1977-04-26 Colgate-Palmolive Company Manufacture of gas-free dentifrice
DE2600607A1 (de) * 1975-11-10 1977-05-18 Kaelin J R Verfahren zum mischen von schlamm mit zusatzmaterialien und einrichtung zur durchfuehrung des verfahrens
GB1478830A (en) * 1975-08-28 1977-07-06 Caterpillar Tractor Co Vacuum mixing of concrete
US4057227A (en) * 1976-08-27 1977-11-08 United Technologies Corporation Method for making ceramic casting slurries
US4361405A (en) * 1980-12-18 1982-11-30 Alfelder Maschinen-Und Modell-Fabrik Kunkel, Wagner & Co. K.G. Method and apparatus for preparing, more particularly for the cooling and mixing of moulding sand
DE3405092A1 (de) * 1983-02-24 1984-08-30 Luciano Mailand/Milano Occelli Verfahren und vorrichtung zur vakuummischung von massen fuer zahntechniker, goldschmiede und dergl.
DE3734526A1 (de) * 1987-10-13 1989-05-03 Gmt Medizinische Technik Gmbh Verfahren und vorrichtung zum mischen von substanzen, die gasfoermige anteile enthalten

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB587698A (en) * 1944-11-28 1947-05-02 Lionel Walker Improvements in or relating to the mixing of granular material with water
US2516436A (en) * 1944-11-28 1950-07-25 Walker Lionel Mixing of granular material with liquids
US3429726A (en) * 1962-10-14 1969-02-25 Toshiaki Takabayashi Method of producing cement mortar or concrete
DE1220834B (de) * 1964-01-07 1966-07-14 Spangenberg Maschf G Verfahren und Vorrichtung zum Vakuummischen zur Koagulationsbildung neigender Gueter
US4020154A (en) * 1973-01-22 1977-04-26 Colgate-Palmolive Company Manufacture of gas-free dentifrice
GB1478830A (en) * 1975-08-28 1977-07-06 Caterpillar Tractor Co Vacuum mixing of concrete
DE2600607A1 (de) * 1975-11-10 1977-05-18 Kaelin J R Verfahren zum mischen von schlamm mit zusatzmaterialien und einrichtung zur durchfuehrung des verfahrens
US4057227A (en) * 1976-08-27 1977-11-08 United Technologies Corporation Method for making ceramic casting slurries
US4361405A (en) * 1980-12-18 1982-11-30 Alfelder Maschinen-Und Modell-Fabrik Kunkel, Wagner & Co. K.G. Method and apparatus for preparing, more particularly for the cooling and mixing of moulding sand
DE3405092A1 (de) * 1983-02-24 1984-08-30 Luciano Mailand/Milano Occelli Verfahren und vorrichtung zur vakuummischung von massen fuer zahntechniker, goldschmiede und dergl.
DE3734526A1 (de) * 1987-10-13 1989-05-03 Gmt Medizinische Technik Gmbh Verfahren und vorrichtung zum mischen von substanzen, die gasfoermige anteile enthalten

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN, Band 11, Nr. 371 (C-462)[2818], 3. Dezember 1987; & JP-A-62 144 740 (NITSUKUU) 27-06-1987 *
PATENT ABSTRACTS OF JAPAN, Band 11, Nr. 44 (M-560)[2491], 10. Februar 1987; & JP-A-61 209 110 (MATSUSHITA) 17-09-1986 *
PATENT ABSTRACTS OF JAPAN, Band 7, Nr. 155 (C-175)[1300], 7. Juli 1983; & JP-A-58 67 328 (TANEZOU) 21-04-1983 *
PATENT ABSTRACTS OF JAPAN, Band 9, Nr. 78 (C-274)[1801], 6. April 1985; & JP-A-59 213 429 (TOOKIYOO) 03-12-1984 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GR1003305B (el) * 1998-12-30 2000-01-25 Μεθοδος πυρομεταλλουργικης επεξεργασιας οξυγονουχων σιδηρονικελιουχων μεταλλευματων με επιλεκτικη προσθηκη μεταλλικου αναγωγικου μεσου και προσθηκη προαναχθεντος σιδηρου - ή σιδηρονικελιουχου μεταλλευματος για βελτιωση αποδοσης νικελιου ως και ρυθμιση ..
EP1029652A1 (fr) * 1999-02-15 2000-08-23 Secmer Dispositif mélangeur sous vide pour la coulée de matériaux plastiques polymérisables
WO2002100521A1 (fr) * 2001-06-08 2002-12-19 Kansai Paint Co., Ltd. Appareil de pulverisation
US6921028B2 (en) 2001-06-08 2005-07-26 Kansai Paint Co., Ltd. Dispersing apparatus
EP1967258A1 (fr) * 2007-03-06 2008-09-10 Interglass Technology AG Procédé de mélange d'un liquide avec au moins deux autres substances et dégazage du mélange et pour la distribution du mélange
WO2008107413A1 (fr) * 2007-03-06 2008-09-12 Interglass Technology Ag Procédé permettant de mélanger un liquide avec au moins une autre substance, de dégazer ce mélange et de distribuer ce mélange
IT201900018311A1 (it) * 2019-10-09 2021-04-09 Eurostar Concrete Tech S P A “Mescolatrice planetaria per la produzione di agglomerati a base cementizia o di resina, in particolare calcestruzzo, e metodo di produzione di agglomerati"

Also Published As

Publication number Publication date
EP0473942B1 (fr) 1995-05-03
JP3220186B2 (ja) 2001-10-22
DE59105370D1 (de) 1995-06-08
DE4028078A1 (de) 1992-03-12
CA2048916A1 (fr) 1992-03-06
JPH05295581A (ja) 1993-11-09

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