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EP0276742B1 - Method and device for micronising solids in a jet mill - Google Patents

Method and device for micronising solids in a jet mill Download PDF

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Publication number
EP0276742B1
EP0276742B1 EP88100769A EP88100769A EP0276742B1 EP 0276742 B1 EP0276742 B1 EP 0276742B1 EP 88100769 A EP88100769 A EP 88100769A EP 88100769 A EP88100769 A EP 88100769A EP 0276742 B1 EP0276742 B1 EP 0276742B1
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EP
European Patent Office
Prior art keywords
solids
jet mill
jet
injector
steam
Prior art date
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EP88100769A
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German (de)
French (fr)
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EP0276742A2 (en
EP0276742A3 (en
Inventor
Hans-Günter Dipl.-Ing. Zander
Horst Dr. Bornefeld
Bernd-Michael Dr. Holle
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Kerr-Mcgee Pigments & Co KG GmbH
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Bayer AG
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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
    • B02C19/06—Jet mills

Definitions

  • the invention relates to a method for micronizing solids in jet mills, the solids being introduced into the jet mill by means of a propellant gas via an injector, and the micronization optionally being carried out in the presence of grinding and / or dispersing agents.
  • Jet mills consist of a grinding chamber into which water vapor or air jets are blown in at high speeds and the solids to be micronized (hereinafter also referred to as regrind) are injected with a propellant gas. Compressed air or water vapor (briefly in the following) is usually used as the propellant referred to as steam).
  • the solids are usually fed into the injector via an inlet funnel or an entry chute.
  • grinding aids are often added to the solid.
  • dispersing aids are mostly used which improve their dispersibility in various materials and at the same time also support the micronization of the pigments.
  • the above-mentioned type of entry of solids in jet mills has the disadvantage that grinding disturbances due to blockages of the injector and deposits of the ground material can occur on the walls of the inlet funnel.
  • regrind is pneumatically fed directly into a jet mill from a feed container via a pressure sealing element and a feed nozzle.
  • this arrangement leads to blockages.
  • the object of the invention was to provide a method for micronizing solids in jet mills that does not have the disadvantages described.
  • the term "forced feeding of the solids” means that the solids only have one degree of freedom for movement, i.e. the solids are transported in a forced direction of movement. There is no possibility of the solids evading in a different direction of movement, as was possible with the conventional feeding of the solids into the injector via inlet funnels or entry chutes (regrind from the jet mill due to blockages in the apparatus).
  • the invention thus relates to a process for micronizing solids in jet mills, the solids being introduced into the jet mill via an injector and the micronization optionally being carried out in the presence of grinding and / or dispersing auxiliaries, which is characterized in that the solids Injector, consisting of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a catch nozzle (15), forcibly and without recoil via an entry chute (6), a discharge lock (7), a blow-through lock (9) and a pneumatic conveyor (10) are supplied.
  • the solids Injector consisting of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a catch nozzle (15), forcibly and without recoil via an entry chute (6), a discharge lock (7), a blow-through lock (9) and a pneumatic conveyor (10) are supplied.
  • the solids are forcibly fed via a pneumatic conveyor.
  • the solids are fluidized with a propellant gas, preferably compressed air, and transported to the injector.
  • the fluidization of the solids can also be done with other gases such as steam.
  • a pressure lock In order to ensure trouble-free operation of the pneumatic conveying device, the solids are forced into it without recoil. This is done using a pressure lock.
  • Suitable pressure locks of various types can be used. For example, pressure locks that consist of a combination of a discharge lock and a pressure blow lock are used.
  • the uniform dosing is preferably carried out by dosing scales. However, it can also be done by measuring the volume of the solids. These process variants make it possible to maintain defined propellant gas / solid ratios in the pneumatic conveying device. Depending on the requirements, the propellant gas / solids ratio can be adjusted at any time by varying the amount of solids.
  • injectors which, according to FIG. 1, consist of a combination of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a collecting nozzle (15). This arrangement ensures a uniform entry of the solid / carrier gas mixture into the pressurized jet mill.
  • the forced feeding of the solids and optionally the addition of grinding and / or dispersing aids is carried out by means of a pressure measurement monitored on a device in the jet mill, the device optionally also serving as a grinding and / or dispersing agent feed device.
  • the pressure measurement is preferably carried out in measuring cycles, with a blockage of the device being prevented between the measuring cycles by a pressure surge or by a constant amount of purge air, which is superimposed by a pressure surge between the measuring cycles.
  • the method according to the invention can be used in the micronization of a wide variety of solids.
  • Pigments in particular inorganic pigments such as titanium dioxide pigments, iron oxide pigments, chromium oxide pigments and mixed phase pigments, can be micronized particularly advantageously by this process.
  • the special grinding or dispersing agent feed device in the jet mill ensures a uniform and homogeneous coating of the pigments with dispersing agents.
  • the described dosing and monitoring measures optimize the grinding process and the conveyance of the solids. This enables a significantly higher utilization of the jet mill without the quality of the micronized solids occurring.
  • the dosing device can consist of a wide variety of devices that enable dosing of solids. It is advantageous if, according to FIG. 1, it consists of a combination of a storage vessel (1), a swivel slide (2), a cellular wheel (3) and a dosing scale (5).
  • the jet mill can also be of various designs.
  • the forced entry device consists of a combination of an entry chute (6), a discharge chute (7), a blow-through lock (9) and a pneumatic conveying device (10).
  • the injector consists of a combination of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a collecting nozzle (15).
  • the injector can also be of conventional design. Such an injector is shown, for example, in Winnacker, Küchler, Chemische Technologie, 4th edition, volume 1, p. 93, Carl Hanser Verlag Kunststoff, Vienna, 1984.
  • a device according to the invention is also particularly preferred, in which a device (17) for pressure measurement is installed in the jet mill according to FIG. 1, which device optionally also serves as a grinding and / or dispersing agent feed device.
  • the ground material is placed in the storage vessel (1).
  • a swivel slide (2) with which the outlet can be closed and opened.
  • the regrind reaches the forced entry device via the dosing scale (5), which is fed by the cellular wheel (3).
  • the speed of rotation of the cellular wheel (3) is regulated depending on the desired feed quantity of the regrind.
  • the connecting line (4) serves to equalize the pressure.
  • the regrind passes through the entry chute (6) into the pressure lock, which consists of a discharge lock (7) and a blow-through lock (9).
  • the solids are forcibly transported into the pneumatic conveying device (10) without recoil via this special pressure lock.
  • the regrind is fluidized with compressed air and conveyed to the solid / steam / air mixing tube (14) of the injector. The amount of compressed air can be monitored with the measuring device (8).
  • the fluidized regrind is finally transported to the jet mill (16) via the catch nozzle (15) with steam, which is passed via the steam line (11) and the jet nozzle (13) to the solid / steam / air mixing tube (14).
  • the amount of steam is monitored with the measuring device (12).
  • the device At the entrance of the jet mill there is a device (17) for measuring the pressure, via which grinding and / or dispersing aids can also be added.
  • the device consists of a plurality of openings or pipe ends, an apparatus for pressure measurement being connected to one opening and one or more grinding and / or dispersing aids being able to be added to the fluidized solids via the other openings.
  • the grinding and / or dispersing aids are preferably added via metering pumps.
  • the pressure measurement is carried out in measuring cycles. Between the respective measuring cycles, a pressure surge or a constant amount of purge air, over which a pressure surge is superimposed, is applied to the device (17), thereby preventing the device from becoming clogged with solid.
  • the entire grinding process including the dosage of the regrind, the forced entry of the solids into the injector, the Operation of the injector and the addition of grinding and / or dispersing aids are monitored.
  • the grinding and / or dispersing aids can be added with the aid of the dosing scale and this special measuring device depending on the weight of the material to be ground.
  • the amount of the dispersing aid was 0.25% by weight, based on the dry pigment.
  • the dispersing aid was added to the fluidized pigment in the specified amount via a commercially available metering pump.
  • the pressure was measured using a pressure measuring device of the usual type.
  • the pneumatic conveyor was operated with air at a pressure of 4 bar. 130 cm3 (0.16 tons) of air were consumed per hour and per ton of the titanium dioxide pigment.
  • the throughput of the titanium dioxide pigment was 2.0 to 2.0 tons per hour.
  • Example 1 The titanium dioxide pigment used in Example 1 was micronized with the addition of the same dispersing aid in a conventional device as is shown in Winnacker, Küchler, Chemische Technologie, 4th edition, Volume 1, p. 93, Carl Hanser Verlag Kunststoff, Vienna, 1984 . A spiral jet mill of the same type as in Example 1 was used.
  • the pigment was introduced into the injector via an entry chute, the injector and the entry chute being of conventional design.
  • the dispersing aid was added in a known manner by continuously spraying the pigment in the feed chute in the same amount as stated in Example 1.
  • the operation of this device consumed 2.4 tons of steam per ton of titanium dioxide pigment for micronization.
  • the throughput of the titanium dioxide pigment was 1.5 to 1.8 tons per hour.
  • Example 1 A comparison with Example 1 shows that the throughput quantities of the titanium dioxide pigment could be increased considerably when using the method according to the invention. This was associated with a steam saving of 0.4 tons per ton of the titanium dioxide pigment and the production of pigment with reduced quality is certainly avoided.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Disintegrating Or Milling (AREA)
  • Crushing And Grinding (AREA)
  • Nozzles (AREA)
  • External Artificial Organs (AREA)
  • Road Signs Or Road Markings (AREA)
  • Control Of Vending Devices And Auxiliary Devices For Vending Devices (AREA)

Description

Die Erfindung betrifft ein Verfahren zum Mikronisieren von Feststoffen in Strahlmühlen, wobei die Feststoffe mittels eines Treibgases über einen Injektor in die Strahlmühle eingebracht werden und wobei die Mikronisierung gegebenenfalls in Gegenwart von Mahl- und/oder Dispergiermitteln erfolgt.The invention relates to a method for micronizing solids in jet mills, the solids being introduced into the jet mill by means of a propellant gas via an injector, and the micronization optionally being carried out in the presence of grinding and / or dispersing agents.

Die Mikronisierung von Feststoffen kann in Strahlmühlen, beispielsweise vom Typ der Spiral- oder Gegenrohrstrahlmühlen durchgeführt werden (vergl. Winnacker Küchler: Chemische Technologie, 4. Auflage, Band 1, S. 91-93, Carl Hanser Verlag München Wien 1984). Strahlmühlen bestehen aus einem Mahlraum, in der Wasserdampf- oder Luftstrahlen mit hohen Geschwindigkeiten eingeblasen und die zu mikronisierenden Feststoffe (im folgenden auch als Mahlgut bezeichnet) über einen Injektor mit einem Treibgas eingebracht werden. Als Treibgas wird dabei zumeist Druckluft oder Wasserdampf (im folgenden kurz als Dampf bezeichnet) verwendet. Die Zuführung der Feststoffe in den Injektor erfolgt in der Regel über einen Einlauftrichter bzw. eine Eintragsschurre.The micronization of solids can be carried out in jet mills, for example of the spiral or counter tube jet type (see Winnacker Küchler: Chemische Technologie, 4th Edition, Volume 1, pp. 91-93, Carl Hanser Verlag, Munich, Vienna 1984). Jet mills consist of a grinding chamber into which water vapor or air jets are blown in at high speeds and the solids to be micronized (hereinafter also referred to as regrind) are injected with a propellant gas. Compressed air or water vapor (briefly in the following) is usually used as the propellant referred to as steam). The solids are usually fed into the injector via an inlet funnel or an entry chute.

Zur Unterstützung der Mikronisierung werden oft auch Mahlhilfsmittel dem Feststoff zugegeben. Insbesondere bei Pigmenten werden darüber hinaus zumeist Dispergierhilfsmittel eingesetzt, die deren Dispergierbarkeit in verschiedenen Materialien verbessern und zugleich auch die Mikronisierung der Pigmente unterstützen. Die oben genannte Art des Eintrags von Feststoffen in Strahlmühlen hat den Nachteil, daß Mahlstörungen aufgrund von Verstopfungen des Injektors und Ablagerungen des Mahlgutes an den Wänden des Einlauftrichters auftreten können.To aid micronization, grinding aids are often added to the solid. In addition, in the case of pigments in particular, dispersing aids are mostly used which improve their dispersibility in various materials and at the same time also support the micronization of the pigments. The above-mentioned type of entry of solids in jet mills has the disadvantage that grinding disturbances due to blockages of the injector and deposits of the ground material can occur on the walls of the inlet funnel.

In der österreichischen Patentschrift 343 978 wird Mahlgut aus einem Aufgabebehälter über ein Druckdichtelement und eine Aufgabedüse pneumatisch direkt in eine Strahlmühle gegeben. Diese Anordnung führt jedoch zu Verstopfungen.In Austrian patent specification 343 978, regrind is pneumatically fed directly into a jet mill from a feed container via a pressure sealing element and a feed nozzle. However, this arrangement leads to blockages.

Diese Mahlstörungen führen in der Regel zu einer verminderten Qualität des mikronisierten Feststoffs. Zudem kann bei diesen Mahlstörungen Mahlgut aus der unter Überdruck stehenden Strahlmühle austreten.These grinding disorders usually lead to a reduced quality of the micronized solid. In addition, in the case of these grinding disorders, regrind can emerge from the pressurized jet mill.

Die Aufgabe der Erfindung bestand darin, ein Verfahren zum Mikronisieren von Feststoffen in Strahlmühlen bereitzustellen, daß die beschriebenen Nachteile nicht aufweist.The object of the invention was to provide a method for micronizing solids in jet mills that does not have the disadvantages described.

Es wurde nun gefunden, daß Mahlstörung und die damit verbundenen Probleme nicht auftreten, wenn die Feststoffe dem Injektor der Strahlmühle zwangsweise zugeführt werden.It has now been found that grinding disorder and the problems associated with it do not occur when the solids are forced to the jet mill injector.

Unter dem Begriff "zwangsweise Zuführung der Feststoffe" wird erfindungsgemäß verstanden, daß den Feststoffen nur ein Freiheitsgrad zur Bewegung zur Verfügung steht, d.h., daß die Feststoffe in einer erzwungenen Bewegungsrichtung transportiert werden. Ein Ausweichen der Feststoffe in eine andere Bewegungsrichtung, wie dies bei der herkömmlichen Zuführung der Feststoffe in den Injektor über Einlauftrichter bzw. Eintragsschurren möglich war (Austreten von Mahlgut aus der Strahlmühle aufgrund von Verstopfungen der Apparatur), ist ausgeschlossen.According to the invention, the term "forced feeding of the solids" means that the solids only have one degree of freedom for movement, i.e. the solids are transported in a forced direction of movement. There is no possibility of the solids evading in a different direction of movement, as was possible with the conventional feeding of the solids into the injector via inlet funnels or entry chutes (regrind from the jet mill due to blockages in the apparatus).

Gegenstand der Erfindung ist somit ein Verfahren zum Mikronisieren von Feststoffen in Strahlmühlen, wobei die Feststoffe über einen Injektor in die Strahlmühle eingebracht werden und wobei die Mikronisierung gegebenenfalls in Gegenwart von Mahl- und/oder Dispergierhilfsmitteln erfolgt, welches dadurch gekennzeichnet ist, daß die Feststoffe dem Injektor, bestehend aus einer Dampfleitung (11), einer Strahldüse (13), einem Feststoff/Dampf/Luftmischrohr (14) und einer Fangdüse (15), zwangsweise und rückstoßfrei über eine Eintragsschurre (6), eine Austragsschleuse (7), eine Durchblaseschleuse (9) und eine pneumatische Fördervorrichtung (10) zugeführt werden.The invention thus relates to a process for micronizing solids in jet mills, the solids being introduced into the jet mill via an injector and the micronization optionally being carried out in the presence of grinding and / or dispersing auxiliaries, which is characterized in that the solids Injector, consisting of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a catch nozzle (15), forcibly and without recoil via an entry chute (6), a discharge lock (7), a blow-through lock (9) and a pneumatic conveyor (10) are supplied.

Die zwangsweise Zuführung der Feststoffe erfolgt über eine pneumatische Fördervorrichtung. In dieser pneumatischen Fördervorrichtung werden die Feststoffe mit einem Treibgas, vorzugsweise Druckluft, fluidisiert und zum Injektor transportiert. Die Fluidisierung der Feststoffe kann auch mit anderen Gasen wie beispielsweise Dampf erfolgen.The solids are forcibly fed via a pneumatic conveyor. In this pneumatic conveying device, the solids are fluidized with a propellant gas, preferably compressed air, and transported to the injector. The fluidization of the solids can also be done with other gases such as steam.

Um einen störungsfreien Betrieb der pneumatischen Fördervorrichtung zu gewährleisten, werden die Feststoffe zwangsweise und rückstoßfrei in diese eingetragen. Dies geschieht mittels einer Druckschleuse. Dabei können geeignete Druckschleusen verschiedenster Bauart eingesetzt werden. Zum Beispiel werden Druckschleusen, die aus einer Kombination einer Austragsschleuse und einer Druckblaseschleuse bestehen, eingesetzt.In order to ensure trouble-free operation of the pneumatic conveying device, the solids are forced into it without recoil. This is done using a pressure lock. Suitable pressure locks of various types can be used. For example, pressure locks that consist of a combination of a discharge lock and a pressure blow lock are used.

Es ist besonders vorteilhaft, wenn die Zuführung der Feststoffe in die pneumatische Fördervorrichtung in gleichmäßiger Dosierung erfolgt.It is particularly advantageous if the solids are fed into the pneumatic conveying device in uniform doses.

Die gleichmäßige Dosierung wird vorzugsweise durch Dosierwaagen vorgenommen. Sie kann aber auch über eine Volumenmessung der Feststoffe erfolgen. Diese Verfahrensvarianten ermöglichen das Einhalten von definierten Treibgas-/Feststoffverhältnissen in der pneumatischen Fördervorrichtung. Je nach den Erfordernissen kann dadurch das Treibgas-/Feststoffverhältnis durch Variation der Feststoffmenge jederzeit Sollwerten angepaßt werden.The uniform dosing is preferably carried out by dosing scales. However, it can also be done by measuring the volume of the solids. These process variants make it possible to maintain defined propellant gas / solid ratios in the pneumatic conveying device. Depending on the requirements, the propellant gas / solids ratio can be adjusted at any time by varying the amount of solids.

Beim erfindungsgemäßen Verfahren werden Injektoren eingesetzt, die gemäß Fig. 1 aus einer Kombination von einer Dampfleitung (11), einer Strahldüse (13), einem Feststoff/ Dampf/Luftmischrohr (14) und einer Fangdüse (15) bestehen. Diese Anordnung gewährleistet einen gleichmäßigen Eintrag des Feststoff-/Trägergasgemisches in die unter Überdruck stehende Strahlmühle.In the method according to the invention, injectors are used which, according to FIG. 1, consist of a combination of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a collecting nozzle (15). This arrangement ensures a uniform entry of the solid / carrier gas mixture into the pressurized jet mill.

In einer sehr vorteilhaften Variante des erfindungsgemäßen Verfahrens wird die zwangsweise Zuführung der Feststoffe sowie gegebenenfalls die Zugabe von Mahl- und/oder Dispergierhilfsmittel über eine Druckmessung an einer Einrichtung in der Strahlmühle überwacht, wobei die Einrichtung gegebenenfalls zugleich als Mahl-und/oder Dispergierhilfsmittelaufgabevorrichtung dient.In a very advantageous variant of the method according to the invention, the forced feeding of the solids and optionally the addition of grinding and / or dispersing aids is carried out by means of a pressure measurement monitored on a device in the jet mill, the device optionally also serving as a grinding and / or dispersing agent feed device.

Die Druckmessung erfolgt vorzugsweise in Meßzyklen, wobei zwischen den Meßzyklen durch einen Druckstoß oder durch eine konstante Spülluftmenge, der zwischen den Meßzyklen ein Druckstoß überlagert ist, ein Verstopfen der Einrichtung verhindert wird.The pressure measurement is preferably carried out in measuring cycles, with a blockage of the device being prevented between the measuring cycles by a pressure surge or by a constant amount of purge air, which is superimposed by a pressure surge between the measuring cycles.

Das erfindungsgemäße Verfahren kann bei der Mikronisierung von verschiedensten Feststoffen eingesetzt werden. Besonders vorteilhaft können Pigmente, insbesondere anorganische Pigmente wie Titandioxidpigmente, Eisenoxidpigmente, Chromoxidpigmente und Mischphasenpigmente, nach diesem Verfahren mikronisiert werden. Durch die spezielle Mahl- bzw. Dispergierhilfsmittelaufgabevorrichtung in der Strahlmühle wird eine gleichmäßige und homogene Beschichtung der Pigmente mit Dispergierhilfsmitteln erreicht.The method according to the invention can be used in the micronization of a wide variety of solids. Pigments, in particular inorganic pigments such as titanium dioxide pigments, iron oxide pigments, chromium oxide pigments and mixed phase pigments, can be micronized particularly advantageously by this process. The special grinding or dispersing agent feed device in the jet mill ensures a uniform and homogeneous coating of the pigments with dispersing agents.

Bei der Durchführung des erfindungsgemäßen Verfahrens treten keine Mahlstörungen mit den damit verbundenen Problemen auf.When carrying out the method according to the invention, there are no grinding disturbances with the problems associated therewith.

Zudem wird durch die beschriebenen Dosier- und Überwachungsmaßnahmen der Mahlvorgang und die Förderung der Feststoffe optimiert. Dies ermöglicht eine wesentlich höhere Auslastung der Strahlmühle, ohne daß eine Qualitätsminderung der mikronisierten Feststoffe eintritt.In addition, the described dosing and monitoring measures optimize the grinding process and the conveyance of the solids. This enables a significantly higher utilization of the jet mill without the quality of the micronized solids occurring.

Gegenstand der Erfindung ist ferner eine Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens. Diese Vorrichtung besteht aus

  • a) einer Dosiervorrichtung,
  • b) einer Zwangseintragsvorrichtung bestehend aus
    • 1. einer Eintragsschurre (6),
    • 2. einer Austragsschleuse (7),
    • 3. einer Durchblaseschleuse (9) und
    • 4. einer pneumatischen Fördervorrichtung (10),
  • c) einem Injektor bestehend aus
    • 1. einer Dampfleitung (11),
    • 2. einer Strahldüse (13),
    • 3. einem Feststoff/Dampf/Luftmischrohr (14) und
    • 4. einer Fangdüse (15) und
  • d) einer Strahlmühle.
The invention further relates to a device for carrying out the method according to the invention. This device consists of
  • a) a dosing device,
  • b) a forced entry device consisting of
    • 1. an entry chute (6),
    • 2. a discharge lock (7),
    • 3. a blow-through lock (9) and
    • 4. a pneumatic conveyor device (10),
  • c) an injector consisting of
    • 1. a steam line (11),
    • 2. a jet nozzle (13),
    • 3. a solid / steam / air mixing tube (14) and
    • 4. a catch nozzle (15) and
  • d) a jet mill.

Die Dosiervorrichtung kann aus unterschiedlichsten Einrichtungen bestehen, die eine Dosierung von Feststoffen ermöglichen. Es ist vorteilhaft, wenn sie gemäß Fig. 1 aus einer Kombination eines Vorratsgefäßes (1), eines Schwenkschiebers (2), eines Zellenrades (3) und einer Dosierwaage (5) besteht.The dosing device can consist of a wide variety of devices that enable dosing of solids. It is advantageous if, according to FIG. 1, it consists of a combination of a storage vessel (1), a swivel slide (2), a cellular wheel (3) and a dosing scale (5).

Auch die Strahlmühle kann verschiedenster Bauart sein.The jet mill can also be of various designs.

Die Zwangseintragsvorrichtung besteht aus einer Kombination einer Eintragsschurre (6), einer Austragsschurre (7), einer Durchblaseschleuse (9) und einer pneumatischen Fördervorrichtung (10).The forced entry device consists of a combination of an entry chute (6), a discharge chute (7), a blow-through lock (9) and a pneumatic conveying device (10).

Einzelne Teile der Zwangseintragsvorrichtung können durch andere geeignete Teile bzw. Apparaturen ersetzt werden. Beispielsweise können anstatt der Austragsschleuse (7) und der Durchblaseschleuse (9), Druckschleusen anderer Art aber gleicher Funktionsweise eingebaut sein.Individual parts of the forced entry device can be replaced by other suitable parts or apparatus. For example, instead of the discharge lock (7) and the blow-through lock (9), pressure locks of a different type but of the same function can be installed.

In der erfindungsgemäßen Vorrichtung besteht der Injektor aus einer Kombination einer Dampfleitung (11), einer Strahldüse (13), einem Feststoff/Dampf/Luftmischrohr (14) und einer Fangdüse (15).In the device according to the invention, the injector consists of a combination of a steam line (11), a jet nozzle (13), a solid / steam / air mixing tube (14) and a collecting nozzle (15).

Der Injektor kann aber auch hekömmlicher Bauart sein. Ein solcher Injektor ist beispielsweise in Winnacker, Küchler, Chemische Technologie, 4. Auflage, Band 1, S. 93, Carl Hanser Verlag München, Wien, 1984, abgebildet.The injector can also be of conventional design. Such an injector is shown, for example, in Winnacker, Küchler, Chemische Technologie, 4th edition, volume 1, p. 93, Carl Hanser Verlag Munich, Vienna, 1984.

Besonders bevorzugt ist auch eine erfindungsgemäße Vorrichtung, bei der in der Strahlmühle gemäß Fig. 1 eine Einrichtung (17) zur Druckmessung eingebaut ist, die gegebenenfalls zugleich als Mahl- und/oder Dispergierhilfsmittelaufgabevorrichtung dient.A device according to the invention is also particularly preferred, in which a device (17) for pressure measurement is installed in the jet mill according to FIG. 1, which device optionally also serves as a grinding and / or dispersing agent feed device.

Das erfindungsgemäße Verfahren und die dazugehörende Vorrichtung sollen anhand der Fig. 1 näher erläutert werden.The method according to the invention and the associated device are to be explained in more detail with reference to FIG. 1.

Das Mahlgut wird in das Vorratsgefäß (1) gegeben. Am Auslauf des Vorratsgefäßes befindet sich ein Schwenkschieber (2), mit dem der Auslauf geschlossen und geöffnet werden kann. Über die Dosierwaage (5), die vom Zellenrad (3) gespeist wird, gelangt das Mahlgut zur Zwangseintragsvorrichtung. Die Drehzahl des Zellenrades (3) wird dabei in Abhängigkeit von der gewünschten Aufgabemenge des Mahlguts geregelt.The ground material is placed in the storage vessel (1). At the outlet of the storage vessel there is a swivel slide (2) with which the outlet can be closed and opened. The regrind reaches the forced entry device via the dosing scale (5), which is fed by the cellular wheel (3). The speed of rotation of the cellular wheel (3) is regulated depending on the desired feed quantity of the regrind.

Die Verbindungsleitung (4), an die sich ein Staubfilter anschließt, dient zum Druckausgleich. In der Zwangseintragsvorrichtung gelangt das Mahlgut über die Eintragsschurre (6) in die Druckschleuse, die aus einer Austragsschleuse (7) und einer Durchblaseschleuse (9) besteht. Über diese spezielle Druckschleuse werden die Feststoffe zwangsweise und rückstoßfrei in die pneumatische Fördervorrichtung (10) transportiert. In der pneumatischen Fördervorrichtung wird das Mahlgut mit Druckluft fluidisiert und zum Feststoff-/Dampf-/Luftmischrohr (14) des Injektors gefördert. Die Druckluftmenge kann dabei mit dem Meßgerät (8) überwacht werden. Das fluidisierte Mahlgut wird schließlich mit Dampf, der über die Dampfleitung (11) und die Strahldüse (13) zum Feststoff-/Dampf-/Luftmischrohr (14) geleitet wird, über die Fangdüse (15) in die Strahlmühle (16) transportiert. Die Dampfmenge wird dabei mit dem Meßgerät (12) überwacht.The connecting line (4), to which a dust filter connects, serves to equalize the pressure. In the forced entry device, the regrind passes through the entry chute (6) into the pressure lock, which consists of a discharge lock (7) and a blow-through lock (9). The solids are forcibly transported into the pneumatic conveying device (10) without recoil via this special pressure lock. In the pneumatic Conveying device, the regrind is fluidized with compressed air and conveyed to the solid / steam / air mixing tube (14) of the injector. The amount of compressed air can be monitored with the measuring device (8). The fluidized regrind is finally transported to the jet mill (16) via the catch nozzle (15) with steam, which is passed via the steam line (11) and the jet nozzle (13) to the solid / steam / air mixing tube (14). The amount of steam is monitored with the measuring device (12).

Am Eingang der Strahlmühle befindet sich eine Einrichtung (17) zur Druckmessung, über die auch Mahl- und/oder Dispergierhilfsmittel zugegeben werden können. Die Einrichtung besteht erfindungsgemäß aus mehreren Öffnungen bzw. Rohrenden, wobei sich an eine Öffnung eine Apparatur zur Druckmessung anschließt und über die anderen Öffnungen ein oder mehrere Mahl- und/oder Dispergierhilfsmittel den fluidisierten Feststoffen zugegeben werden können. Die Zugabe der Mahl- und/oder Dispergierhilfsmittel erfolgt dabei vorzugsweise über Dosierpumpen.At the entrance of the jet mill there is a device (17) for measuring the pressure, via which grinding and / or dispersing aids can also be added. According to the invention, the device consists of a plurality of openings or pipe ends, an apparatus for pressure measurement being connected to one opening and one or more grinding and / or dispersing aids being able to be added to the fluidized solids via the other openings. The grinding and / or dispersing aids are preferably added via metering pumps.

Die Druckmessung wird in Meßzyklen durchgeführt. Zwischen den jeweiligen Meßzyklen wird auf die Einrichtung (17) ein Druckstoß oder eine konstante Spülluftmenge, der ein Druckstoß überlagert ist, gegeben, wodurch ein Verstopfen der Einrichtung mit Feststoff verhindert wird.The pressure measurement is carried out in measuring cycles. Between the respective measuring cycles, a pressure surge or a constant amount of purge air, over which a pressure surge is superimposed, is applied to the device (17), thereby preventing the device from becoming clogged with solid.

Mit dieser speziellen Einrichtung kann der gesamte Mahlvorgang, einschließlich der Dosierung des Mahlguts, dem Zwangseintrag der Feststoffe in den Injektor, dem Betrieb des Injektors sowie der Zugabe von Mahl- und/oder Dispergierhilfsmitteln überwacht werden. Die Zugabe der Mahl- und/oder Dispergierhilfsmittel kann mit Hilfe der Dosierwaage und dieser speziellen Meßeinrichtung exakt in Abhängigkeit vom Gewicht des Mahlguts erfolgen.With this special device, the entire grinding process, including the dosage of the regrind, the forced entry of the solids into the injector, the Operation of the injector and the addition of grinding and / or dispersing aids are monitored. The grinding and / or dispersing aids can be added with the aid of the dosing scale and this special measuring device depending on the weight of the material to be ground.

Bei Abweichungen des Druckes innerhalb der Mühle von einem vorgegebenen Sollwert, d.h. Abweichungen von den optimalen Mahlbedingungen, können schnelle Korrekturmaßnahmen durchgeführt werden, wodurch Qualtitätsschwankungen bei den mikronisierten Feststoffen sicher vermieden werden.If the pressure inside the mill deviates from a predetermined setpoint, i.e. Deviations from the optimal grinding conditions, quick corrective measures can be carried out, whereby quality fluctuations in the micronized solids are reliably avoided.

Das folgende Beispiel zeigt die Vorteile des erfindungsgemäßen Verfahrens im Vergleich zu einem herkömmlichen Verfahren zum Mikronisieren von Feststoffen:The following example shows the advantages of the method according to the invention compared to a conventional method for micronizing solids:

Beispiel 1example 1

Ein nach dem Sulfatverfahren hergestelltes Titandioxidpigment mit Rutilstruktur, das mit 0,8 Gew.-% SiO₂ und 2,2 Gew.-% Al₂O₃ nachbehandelt war, wurde unter Zusatz eines Dispergierhilfsmittels in einer erfindungsgemäßen Vorrichtung gemäß Abb. 1 mikronisiert. Als Dispergierhilfsmittel wurde ein in Wasser gelöstes Umsetzungsprodukt von Trimethylolpropan mit Ethylenoxid eingesetzt, wie es in der DE-B-1 467 442, Beispiel 2, beschrieben ist. Die Menge des Dispergierhilfsmittels betrug 0,25 Gew.-% bezogen auf das trockene Pigment.A prepared by the sulfate titanium dioxide pigment with a rutile structure, which was aftertreated with 0.8 wt .-% SiO₂ and 2.2 wt .-% Al₂O₃, was micronized with the addition of a dispersing agent in a device according to the invention as shown in Fig. 1. A water-soluble reaction product of trimethylolpropane with ethylene oxide, as described in DE-B-1 467 442, example 2, was used as the dispersing aid. The amount of the dispersing aid was 0.25% by weight, based on the dry pigment.

Die Vorrichtung setzte sich aus folgenden Einzelteilen zusammen:

  • a) einer Dosiervorrichtung, bestehend aus einer Kombination eines Vorratssilos (1), eines Schwenkschiebers (2), eines Zellenrades (3) und einer Bandwaage (5), wobei sämtliche Geräte üblicher Bauart waren;
  • b) einer Zwangseintragsvorrichtung, bestehend aus einer Kombination einer Eintragsschurre (6) üblicher Bauart, einer Austrageschleuse (7), einer Durchblaseschleuse (9) und einer pneumatischen Fördervorrichtung (10), wobei die Austragschleuse und die Durchblaseschleuse handelsübliche Zellenräder aus V4A-Stahl mit einem Zellenraddurchmesser von 300 mm waren und die pneumatische Fördervorrichtung eine Preßluftleitung mit Meßblende war;
  • c) einem speziellen Injektor mit einer Dampfleitung (11) üblicher Bauart, einer Strahldüse (13), einem Feststoff-/Dampf-/Luftmischrohr (14) und einer Fangdüse (15), wobei die Strahldüse eine handelsübliche Düse aus Gußbronze war, die Fangdüse aus einem Venturirohr aus ST-60-Stahl bestand und das Feststoff-/Dampf-/Luftmischrohr (14) aus einem V4A-Stahlrohr mit einem Durchmesser von 80 mm gefertigt war;
  • d) einer Spiralstrahlmühle (16) üblicher Bauart mit einem Durchmesser von 915 mm, in der sich am Eingang der Mühle hinter der Fangdüse (15) eine Einrichtung zur Druckmessung (17) befand, über die auch die Dispergierhilfsmittelaufgabe erfolgte.
The device consisted of the following individual parts:
  • a) a dosing device, consisting of a combination of a storage silo (1), a swivel slide (2), a cellular wheel (3) and a belt scale (5), all devices being of conventional design;
  • b) a forced entry device, consisting of a combination of an entry chute (6) of conventional design, a discharge lock (7), a blow-through lock (9) and a pneumatic conveying device (10), the discharge lock and the blow-through lock using commercially available cell wheels made of V4A steel with a Cell wheel diameter of 300 mm and the pneumatic conveyor was a compressed air line with orifice;
  • c) a special injector with a steam line (11) of conventional design, a jet nozzle (13), a solid / steam / air mixing tube (14) and a catch nozzle (15), the jet nozzle being a commercially available nozzle made of cast bronze, the catch nozzle consisted of a Venturi tube made of ST-60 steel and the solid / steam / air mixing tube (14) was made of a V4A steel tube with a diameter of 80 mm;
  • d) a spiral jet mill (16) of conventional design with a diameter of 915 mm, in which there was a device for pressure measurement (17) at the entrance of the mill behind the collecting nozzle (15), via which the dispersing agent was also added.

Das Dispergierhilfsmittel wurde in der angegebenen Menge über eine handelsübliche Dosierpumpe dem fluidisierten Pigment zugegeben. Die Druckmessung erfolgte mit einer Druckmeßapparatur üblicher Bauart.The dispersing aid was added to the fluidized pigment in the specified amount via a commercially available metering pump. The pressure was measured using a pressure measuring device of the usual type.

Die pneumatische Fördervorrichtung wurde mit Luft mit einem Druck von 4 bar betrieben. Pro Stunde und pro Tonne des Titandioxidpigmentes wurden 130 cm³ (0,16 Tonnen) Luft verbraucht.The pneumatic conveyor was operated with air at a pressure of 4 bar. 130 cm³ (0.16 tons) of air were consumed per hour and per ton of the titanium dioxide pigment.

Zur Mikronisierung wurden 2,0 Tonnen Dampf pro Tonne des Titandioxidpigmentes benötigt.Micronization required 2.0 tons of steam per ton of the titanium dioxide pigment.

Der Durchsatz des Titandioxidpigmentes betrug 2,0 bis 2,0 Tonnen pro Stunde.The throughput of the titanium dioxide pigment was 2.0 to 2.0 tons per hour.

Beim Betrieb dieser Vorrichtung traten keinerlei Mahlstörungen auf und das mikronisierte Titandioxidpigment konnte in der gewünschten guten Qualität erhalten werden.No grinding disturbances occurred during the operation of this device and the micronized titanium dioxide pigment could be obtained in the desired good quality.

Beispiel 2 (Vergleichsbeispiel) Example 2 (comparative example )

Das in Beispiel 1 eingesetzte Titandioxidpigment wurde unter Zusatz des gleichen Dispergierhilfsmittels in einer herkömmlichen Vorrichtung mikronisiert, wie sie in Winnacker, Küchler, Chemische Technologie, 4. Auflage, Band 1, S. 93, Carl Hanser Verlag München, Wien, 1984, abgebildet ist. Es wurde eine Spiralstrahlmühle des gleichen Typs wie in Beispiel 1 eingesetzt.The titanium dioxide pigment used in Example 1 was micronized with the addition of the same dispersing aid in a conventional device as is shown in Winnacker, Küchler, Chemische Technologie, 4th edition, Volume 1, p. 93, Carl Hanser Verlag Munich, Vienna, 1984 . A spiral jet mill of the same type as in Example 1 was used.

Der Eintrag des Pigmentes in den Injektor erfolgte über eine Eintragsschurre, wobei der Injektor und die Eintragsschurre üblicher Bauart waren. Die Dispergierhilfsmittelzugabe erfolgte in bekannter Weise durch kontinuierliches Besprühen des Pigmentes in der Eintragsschurre in der gleichen Menge wie in Beispiel 1 angegben.The pigment was introduced into the injector via an entry chute, the injector and the entry chute being of conventional design. The dispersing aid was added in a known manner by continuously spraying the pigment in the feed chute in the same amount as stated in Example 1.

Beim Betrieb dieser Vorrichtung wurden zur Mikronisierung 2,4 Tonnen Dampf pro Tonne Titandioxidpigment verbraucht. Der Durchsatz des Titandioxidpigmentes betrug 1,5 bis 1,8 Tonnen pro Stunde.The operation of this device consumed 2.4 tons of steam per ton of titanium dioxide pigment for micronization. The throughput of the titanium dioxide pigment was 1.5 to 1.8 tons per hour.

Es traten bis zu zehn Mahlstörungen pro Tag auf, was damit verbunden auch zur Produktion von Pigment mit teilweise verminderter Qualität führte.Up to ten grinding disorders occurred per day, which also led to the production of pigment with partially reduced quality.

Der Vergleich zu Beispiel 1 zeigt, daß bei Anwendung des erfindungsgemäßen Verfahrens die Durchsatzmengen des Titandioxidpigmentes erheblich gesteigert werden konnten. Damit verbunden war eine Dampfersparnis von 0,4 Tonnen pro Tonne des Titandioxidpigmentes und die Produktion von Pigment mit verminderter Qualität wird sicher vermieden.A comparison with Example 1 shows that the throughput quantities of the titanium dioxide pigment could be increased considerably when using the method according to the invention. This was associated with a steam saving of 0.4 tons per ton of the titanium dioxide pigment and the production of pigment with reduced quality is certainly avoided.

Claims (6)

  1. A method for micronising solids in jet mills, the solids being introduced into the jet mill via an injector and the micronisation optionally taking place in the presence of milling and/or dispersing agents, characterised in that the solids are supplied to the injector comprising a steam line (11), a jet nozzle (13), a solids/steam/air mixing pipe (14) and a collecting nozzle (15) forcibly and without reflux via a feed chute (6), a discharge gate (7), a blower gate (9) and a pneumatic conveying device (10).
  2. A method according to claim 1, characterised in that the supply of solids into the pneumatic conveying device is metered in a uniform manner.
  3. A method according to claim 1 or 2, characterised in that the forced supply of solids and optionally the addition of milling and/or dispersing agents is monitored by means of a pressure measurement in a device in the jet mill, the device being optionally simultaneously used as a milling and/or dispersing agent feed device.
  4. A method according to claim 3, characterised in that the pressure measurement is effected in measuring cycles and a blockage of the measuring device is prevented in between measuring cycles by means of a pressure surge or a constant quantity of scavenging air, superimposed by a pressure surge in between measuring cycles.
  5. A device for carrying out the method according to one or more of claims 1 and 2, comprising
    a) a metering device
    b) a forced feed device comprising
    1. a feed chute (6),
    2. a discharge gate (7),
    3. a blower gate (9) and
    4. a pneumatic conveying device (10),
    c) an injector comprising
    1. a steam line (11),
    2. a jet nozzle (13),
    3. a solids/steam/air mixing pipe (14) and
    4. a collecting nozzle (15) and
    d) a jet mill.
  6. A device according to claim 5, characterised in that a device (17) for measuring pressure is arranged in the jet mill and is optionally simultaneously used as a milling and/or dispersing agent feed device.
EP88100769A 1987-01-30 1988-01-20 Method and device for micronising solids in a jet mill Expired - Lifetime EP0276742B1 (en)

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NO172787B (en) 1993-06-01
CA1332392C (en) 1994-10-11
US4880169A (en) 1989-11-14
FI880389A0 (en) 1988-01-28
NO172787C (en) 1993-09-08
AU600074B2 (en) 1990-08-02
BR8800362A (en) 1988-09-20
NO880172L (en) 1988-08-01
DE3865442D1 (en) 1991-11-21
JPS63194750A (en) 1988-08-11
DE3702787A1 (en) 1988-08-11
FI880389A (en) 1988-07-31
EP0276742A2 (en) 1988-08-03
FI87544B (en) 1992-10-15
NO880172D0 (en) 1988-01-15
JP2659045B2 (en) 1997-09-30
EP0276742A3 (en) 1989-08-30
FI87544C (en) 1993-01-25
AU1064088A (en) 1988-08-04
ZA88630B (en) 1988-08-02
US4917309A (en) 1990-04-17

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