EP2959975A1 - Procede de production de particules fines a l'aide d'un broyeur a jet et broyeur a jet associe - Google Patents

Procede de production de particules fines a l'aide d'un broyeur a jet et broyeur a jet associe Download PDF

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Publication number
EP2959975A1
EP2959975A1 EP15002331.5A EP15002331A EP2959975A1 EP 2959975 A1 EP2959975 A1 EP 2959975A1 EP 15002331 A EP15002331 A EP 15002331A EP 2959975 A1 EP2959975 A1 EP 2959975A1
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EP
European Patent Office
Prior art keywords
jet mill
grinding
air
jet
classifier
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Pending
Application number
EP15002331.5A
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German (de)
English (en)
Inventor
Roland Nied
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.)
Netzsch Trockenmahltechnik GmbH
Original Assignee
Nied Roland Dr-Ing
Netzsch Trockenmahltechnik GmbH
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Application filed by Nied Roland Dr-Ing, Netzsch Trockenmahltechnik GmbH filed Critical Nied Roland Dr-Ing
Publication of EP2959975A1 publication Critical patent/EP2959975A1/fr
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Classifications

    • 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
    • B02C19/068—Jet mills of the fluidised-bed type
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B11/00—Arrangement of accessories in apparatus for separating solids from solids using gas currents
    • B07B11/04—Control arrangements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B7/00—Selective separation of solid materials carried by, or dispersed in, gas currents
    • B07B7/08—Selective separation of solid materials carried by, or dispersed in, gas currents using centrifugal force
    • B07B7/083—Selective separation of solid materials carried by, or dispersed in, gas currents using centrifugal force generated by rotating vanes, discs, drums, or brushes

Definitions

  • the present invention relates to a method for producing finest particles by means of a jet mill and a jet mill therefor according to the preambles of the independent claims.
  • the material to be sighted or ground consists of coarser and finer particles which are entrained in an air stream and form the product stream which is introduced into a housing of a wind sifter of the jet mill.
  • the product flow passes in the radial direction into a classifying wheel of the air classifier.
  • the coarser particles are eliminated from the air stream and the air stream leaves the classifying wheel with the fine particles axially through a discharge pipe.
  • the air flow with the fine particles to be filtered out or produced can then be supplied to a filter in which a fluid, such as air, and fine particles are separated from each other.
  • Such a jet mill is known, in the grinding chamber further at least one high-energy jet jet of hot steam with high flow energy is introduced, wherein the grinding chamber except the inlet means for the at least one grinding jet has an inlet for the material to be ground and an outlet for the product, and wherein in the area of the coincidence of regrind and at least one grinding jet of hot steam and millbase have at least about the same temperature.
  • the present invention therefore has the aim of further optimizing a method for producing very fine particles by means of a jet mill and a jet mill, in particular with an air classifier integrated therein.
  • a generic method for producing very fine particles by means of a jet mill is characterized in that a fluid, in particular gases or vapors, is used as the operating medium, which has a higher and, in particular, significantly higher sound velocity than air (343 m / s).
  • the operating medium used is a fluid, in particular gases or vapors, which has a speed of sound of at least 450 m / s.
  • the invention further provides a jet mill, which includes or is associated with a source of equipment having a higher and, in particular, much higher velocity of sound than air (343 m / s).
  • a source for a resource is included or assigned, which has a speed of sound of at least 450 m / s.
  • a source of equipment is contained or associated with gases or vapors, in particular containing or associated with a source of a resource containing water vapor, hydrogen gas or helium gas.
  • the jet mill is a fluidized bed jet mill or a dense bed jet mill.
  • grinding or inlet nozzles are provided, which are connected to a steam supply line, which is equipped with expansion bends, ie when the steam supply line is connected to a source of steam.
  • the flow paths are at least largely free of projections, and / or if the components of the jet mill are designed to prevent mass accumulation.
  • the components of the jet mill are designed to prevent condensation.
  • devices for preventing condensation can accordingly preferably be contained.
  • a fine-material outlet chamber which has a cross-sectional widening in the flow direction.
  • the jet mill according to the invention can advantageously contain, in particular, an air classifier which can combine individual characteristics or combinations of features of the air classifier according to the EP 0 472 930 B1 contains.
  • the air classifier may comprise means for reducing the peripheral components of the flow according to the EP 0 472 930 B1 contain.
  • a discharge nozzle assigned to the classifying wheel of the air classifier which is constructed as a dip tube, has a cross-sectional widening designed to be rounded in the direction of flow, preferably in order to avoid vortex formations.
  • a proposed integrated dynamic air classifier with a debuterrad is preferably associated with a source of a resource having a higher velocity of sound than air (343 m / s).
  • a resource associated with a much higher velocity of sound than air (343 m / s) is associated with and / or associated with a resource (B) source having a speed of sound of at least 450 m / s.
  • a source is associated with a resource containing gases or vapors, in particular the water vapor, hydrogen gas or helium gas.
  • a classifying rotor or indexing wheel is included, which has an increasing height with decreasing radius.
  • the surface of the classifying rotor or wheel which is flowed through is at least approximately constant, and / or that a classifying rotor or indexing wheel is included, which has an exchangeable, co-rotating dip tube. It may further be provided that a fine-material outlet chamber is provided, which has a cross-sectional widening in the flow direction, and / or that the flow paths are at least largely free of projections.
  • a fluid, in particular gases or vapors is used, which has a higher and especially much higher velocity of sound than air (343 m / s).
  • a fluid, in particular gases or vapors which has a much higher speed of sound than air (343 m / s)
  • a fluid, in particular gases or vapors is used as the operating medium which has a speed of sound of at least 450 m / s.
  • water vapor, hydrogen gas or helium gas as the resource.
  • the process is carried out in a grinding system (milling apparatus), preferably in a milling system comprising a jet mill, particularly preferably comprising an opposed jet mill.
  • a feed to be crushed is accelerated in expanding high-speed gas jets and comminuted by particle-particle collisions.
  • jet mills very particular preference is given to using fluid bed counter-jet mills or dense-bed jet mills or spiral jet mills.
  • two or more grinding jet inlets are located in the lower third of the grinding chamber, preferably in the form of grinding nozzles, which are preferably located in a horizontal plane.
  • the Mahlstrahleinlässe are particularly preferably arranged on the circumference of the preferably round mill container, that the grinding jets all meet at a point inside the grinding container.
  • the grinding jet inlets are distributed uniformly over the circumference of the grinding container. In the case of three Mahlstrahleinlässe the distance would thus each be 120 °.
  • the grinding system comprises a separator, preferably a dynamic separator, particularly preferably a dynamic Schaufelradsichter or a separator according to the Fig. 2 and 3 ,
  • This dynamic air classifier includes a classifying wheel and a bombardradwelle and a classifier housing, wherein between the classifying wheel and the classifier housing a classifier gap and between the prepareradwelle and the classifier housing a shaft passage is formed, and is characterized in that a rinsing gap of the classifier gap and / or shaft passage with compressed Low energy gases take place.
  • the upper particle is confined, with the product particles rising together with the expanded gas jets being passed through the classifier from the center of the grinding container and subsequently the product having sufficient flow Fineness, is carried out of the classifier and from the mill. Too coarse particles return to the milling zone and are subjected to further comminution.
  • an air classifier can be connected downstream as a separate unit of the jet mill, but preferably an integrated air classifier is used.
  • a further possible feature of the method according to the invention is that the actual grinding step is preceded by a heating phase in which it is ensured that the grinding chamber, particularly preferably all essential components of the jet mill and / or grinding system, could condense water and / or water vapor is heated in such a way that its / its temperature is above the dew point of the steam.
  • the heating can be done in principle by any heating method. However, the heating is preferably carried out by passing hot gas through the mill and / or the entire grinding system so that the temperature of the gas at the mill outlet is higher than the dew point of the steam. Particular care is taken here that the hot gas preferably heats all essential components of the mill and / or the entire grinding system, which come into contact with the steam, sufficiently.
  • any gas and / or gas mixtures can be used as the heating gas, but hot air and / or combustion gases and / or inert gases are preferably used.
  • the temperature of the hot gas is preferably above the dew point of the water vapor.
  • the hot gas can in principle be introduced into the milling space as desired.
  • the heating gas or heating gas mixture is introduced by at least two, preferably three or more, arranged in a plane inlets or nozzles, which are arranged on the circumference of the preferably round mill container, that the rays all at a point inside the grinding container to meet.
  • the inlets or nozzles are distributed uniformly over the circumference of the grinding container.
  • a gas and / or a vapor preferably water vapor and / or a gas / steam mixture is depressurized by the grinding jet inlets, preferably in the form of grinding nozzles.
  • This equipment usually has a much higher speed of sound than air (343 m / s), preferably at least 450 m / s on.
  • the equipment comprises water vapor and / or hydrogen gas and / or argon and / or helium. Particularly preferred is superheated steam.
  • the operating means at a pressure of 15 to 250 bar, more preferably from 20 to 150 bar, most preferably 30 to 70 bar and particularly preferably 40 to 65 bar relaxed in the mill.
  • the operating means has a temperature of 200 to 800 ° C, particularly preferably 250 to 600 ° C and in particular 300 to 400 ° C.
  • FIG. 1 is an embodiment of a jet mill 1 with a cylindrical housing 2 enclosing a grinding chamber 3, a Mahlgutholzgabe 4 approximately half the height of the grinding chamber 3, at least one Mahlstrahleinlass 5 in the lower region of the grinding chamber 3 and a product outlet 6 in the upper region of the grinding chamber. 3 shown.
  • an air classifier 7 is arranged with a rotatable classifying wheel 8, with which the material to be ground (not shown) is classified in order to discharge only material to be ground below a certain particle size through the product outlet 6 from the grinding chamber 3 and ground material having a particle size above the selected value to another To feed grinding.
  • the classifying wheel 8 can be a classifying wheel which is common in air classifiers and whose blades (see later eg in connection with FIG Fig. 3 ) define radially extending blade channels, at the outer ends of which the classifying air enters and entrains particles of smaller grain size or mass to the central outlet and to the product outlet 6, while larger particles or particles of larger mass are rejected under the influence of centrifugal force.
  • the Wind sifter 7 and / or at least its classifying wheel 8 with at least one design feature according to the EP 0 472 930 B1 fitted.
  • two or more Mahlstrahleinlässe preferably grinding nozzles, in particular 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12 Mahlstrahleinlässe used, which are mounted in the lower third of the particular cylindrical housing of the grinding chamber.
  • Mahlstrahleinlässe are ideally arranged in a plane and evenly distributed over the circumference of the grinding container, so that the grinding jets all meet at a point inside the Mahl discloseders.
  • the inlets or nozzles are distributed uniformly over the circumference of the grinding container. With three grinding jets this would be an angle of 120 ° between the respective inlets or nozzles. In general one can say that the larger the grinding chamber, the more inlets or grinding nozzles are used.
  • the grinding chamber may contain, in addition to the grinding jet inlets, heating openings 5a, preferably in the form of heating nozzles, through which hot gas can be passed into the mill in the heating phase.
  • heating openings 5a preferably in the form of heating nozzles, through which hot gas can be passed into the mill in the heating phase.
  • these nozzles or openings can be arranged in the same plane as the grinding openings or nozzles 5.
  • the mill contains two heating nozzles or openings and three grinding nozzles or openings.
  • the processing temperature can be influenced by using an internal heat source 11 between Mahlgutiergabe 4 and the range of grinding jets 10 or a corresponding heat source 12 in the area outside the Mahlgutiergabe 4 or by processing particles of already warm ground material, while avoiding heat loss in the Mahlgutiergabe 4 passes, to which a feed tube 13 is surrounded by a temperature-insulating jacket 14.
  • the heating source 11 or 12 may, when used, be basically arbitrary and therefore purposely operational and according to availability on the market, so that no further explanation is required.
  • the temperature of the grinding jet or the grinding jets 10 is relevant and the temperature of the material to be ground should at least approximately correspond to this grinding jet temperature.
  • the jet mill 1 is representative of any supply of a resource or medium B, a reservoir or generating means 18, such as a tank 18 a shown, from which the resource or operating medium B via line devices 19 to the Mahlstrahleinlass 5 or the Mahlstrahleinlässen. 5 to the formation of the grinding jet 10 and the grinding jets 10 is passed.
  • a reservoir or generating means 18 such as a tank 18 a shown
  • the relevant embodiments being intended and to be understood as exemplary only and not as limiting, a method for producing very fine particles is carried out with this jet mill 1 with an integrated dynamic air classifier 7 .
  • gases or vapors B which have a higher and in particular significantly higher speed of sound than air (343 m / s).
  • gases or vapors B having an acoustic velocity of at least 450 m / s are used as the operating means.
  • a fluid is used, preferably the water vapor already mentioned, but also hydrogen gas or helium gas.
  • the jet mill 1 is equipped with a source such as the reservoir or generating means 18 for steam or superheated steam or other suitable reservoir or generating means for a resource B or is associated with such a resource source, resulting in a resource B for operation with a higher and in particular much higher speed of sound than air (343 m / s), such as preferably a speed of sound of at least 450 m / s, is fed.
  • This resource such as the steam or hot steam reservoir or generator 18, contains gases or vapors B for use in operation of the jet mill 1, particularly the water vapor already mentioned above, but hydrogen gas or helium gas are also preferred alternatives.
  • Another advantageous aspect when using steam as operating medium B is to provide the jet mill 1 with as small a surface as possible, or in other words, to optimize the jet mill 1 with regard to the smallest possible surface area.
  • This purpose is also served by the further alternative or additional design measure, namely to design or optimize the components of the jet mill 1 in order to avoid mass accumulations. This can be realized, for example, by using as thin as possible flanges in and for connecting the line devices 19.
  • Energy loss and other flow-related impairments can also be contained or avoided if the components of the jet mill 1 are designed or optimized to avoid condensation. It may even be included for this purpose special equipment (not shown) for condensation prevention. Furthermore, it is advantageous if the flow paths are optimized at least largely free of projections or to that extent. In other words, with these design variants, individually or in any combination, the principle is implemented to avoid as much as possible or anything that can become cold and where condensation can occur.
  • the classifying rotor has a clear height which increases with decreasing radius, that is to say towards its axis, wherein in particular the throughflow area of the classifying rotor is at least approximately constant.
  • a fine-material outlet chamber may be provided which has a cross-sectional widening in the flow direction.
  • a particularly preferred embodiment of the jet mill 1 is that the sifting rotor 8 has an exchangeable, co-rotating dip tube 20.
  • amorphous SiO 2 or other amorphous chemical products which are comminuted with the jet mill.
  • Further materials are silicic acids, silica gels or silicates.
  • the method according to the invention and the apparatuses to be used and designed for this purpose relate to pulverulent amorphous or crystalline solids having a very small average particle size and a narrow particle size distribution, to a process for their preparation, and to their use.
  • Fine-particle, amorphous silicic acid and silicates have been industrially produced for decades. It is known that the achievable particle diameter is proportional to the root of the reciprocal of the collision velocity of the particles. The impact speed will turn predetermined by the jet velocity of the expanding gas jets of the respective grinding medium from the nozzles used. For this reason, preferably superheated steam can be used to generate very small particle sizes, since the acceleration capacity of steam is about 50% greater than that of air.
  • the use of steam has the disadvantage that, in particular during start-up of the mill, condensation can occur in the entire grinding system, which generally results in the formation of agglomerates and crusts during the grinding process.
  • the average particle diameter d 50 obtained using conventional jet mills in the milling of amorphous silica, silicates or silica gels was therefore far above 1 ⁇ m.
  • the particles after treatment with prior art methods and devices according to the prior art a broad particle size distribution with particle diameters, for example, from 0.1 to 5.5 microns and a proportion of particles> 2 microns of 15 to 20%.
  • a high proportion of large particles, ie> 2 microns is disadvantageous for applications in coating systems, as it can not be produced thin films with a smooth surface.
  • amorphous or crystalline solids having an average particle size d 50 ⁇ 1.5 ⁇ m and / or a d 90 value ⁇ 2 ⁇ m and / or a d 99 value ⁇ 2 ⁇ m are thus used.
  • amorphous solids may be gels but also those with different structure such.
  • Such amorphous solids generally having an average particle size d 50 ⁇ 1.5 microns and / or a d 90 value ⁇ 2 microns and / or a d 99 value ⁇ 2 microns are z. B. used in surface coating systems.
  • the process according to the invention has the advantage that it is a dry milling process which leads directly to pulverulent products with a very small mean particle size, which can also advantageously have a high porosity ,
  • the problem of reagglomeration during drying is eliminated because no grinding of the downstream drying step is necessary.
  • Another advantage of the method according to the invention in one his preferred embodiments is to be seen in the fact that the grinding can take place simultaneously with the drying, so that z. B. a filter cake can be further processed directly. This saves an additional drying step and at the same time increases the space-time yield.
  • the inventive method also has the advantage that no or only very small amounts of condensate in the grinding system, especially in the mill arise when starting up the grinding system.
  • dried gas can be used.
  • no condensate is produced in the grinding system during cooling and the cooling phase is significantly shortened.
  • the effective machine running times can thus be increased.
  • the fact that no or very little condensate is formed when starting in the milling system prevents an already dried ground material is wet again, whereby the formation of agglomerates and crusts during the grinding process can be prevented.
  • the amorphous pulverulent solids produced by means of the process according to the invention have particularly good properties when used in surface coating systems, for example because of the very special and unique average particle sizes and particle size distributions.
  • As a rheological aid in paper coating and in paints or varnishes.
  • the products obtained in this way allow z. B. due to the very small average particle size and in particular the low d 90 value and d 99 value to produce very thin coatings.
  • powder and pulverulent solids are used interchangeably in the context of the present invention and each denote finely comminuted, solid substances from small dry particles, dry particles meaning that they are externally dry particles.
  • these particles usually have a water content, this water is so firmly bound to the particles or in their capillaries that it is not released at room temperature and atmospheric pressure. In other words, they are perceptible by optical methods particulate matter and not to suspensions or dispersions.
  • these may be both surface-modified and non-surface-modified solids.
  • the surface modification is preferably carried out with carbon-containing coating agents and can be carried out both before and after the grinding.
  • the solids according to the invention can be present as gel or as particles containing agglomerates and / or aggregates.
  • Gel means that the solids are composed of a stable, three-dimensional, preferably homogeneous network of primary particles. Examples are z. B. silica gels.
  • Particles comprising aggregates and / or agglomerates in the sense of the present invention do not have a three-dimensional network or at least not a particle that extends over the entire particle Network of primary particles. Instead, they have aggregates and agglomerates of primary particles. Examples of these are precipitated silicas and fumed silicas.
  • any particles in particular amorphous particles, can be ground in such a way that pulverulent solids having an average particle size d 50 ⁇ 1.5 ⁇ m and / or a d 90 value ⁇ 2 ⁇ m and / or a d 99 value ⁇ 2 ⁇ m are obtained.
  • Such particular amorphous solids are characterized in that they have an average particle size (TEM) d 50 ⁇ 1.5 ⁇ m, preferably d 50 ⁇ 1 ⁇ m, particularly preferably d 50 from 0.01 to 1 ⁇ m, very particularly preferably d 50 of 0.05 to 0.9 ⁇ m, particularly preferably d 50 from 0.05 to 0.8 ⁇ m, particularly preferably from 0.05 to 0.5 ⁇ m and very particularly preferably from 0.08 to 0.25 ⁇ m, and / or a d 90 value ⁇ 2 microns, preferably d 90 ⁇ 1.8 microns, more preferably d 90 from 0.1 to 1.5 microns, most preferably d90 from 0.1 to 1.0 microns and most preferably d 90 from 0.1 to 0.5 microns, and / or a d 99 value ⁇ 2 microns, preferably d 99 ⁇ 1.8 microns, more preferably d 99 ⁇ 1.5 microns, most preferably d 99 of 0.1 to 1.0 microns, and
  • These solids may be gels but also other types of amorphous or crystalline solids.
  • the solids concerned are particulate solids containing aggregates and / or agglomerates, in particular precipitated silica and / or fumed silica and / or silicates and / or mixtures thereof, having an average particle size d 50 ⁇ 1.5 ⁇ m, preferably d 50 ⁇ 1 ⁇ m, more preferably d 50 from 0.01 to 1 ⁇ m, very particularly preferably d 50 from 0.05 to 0.9 ⁇ m, particularly preferably d 50 from 0.05 to 0.8 ⁇ m, especially preferably from 0.05 to 0.5 ⁇ m and very particularly preferably from 0.1 to 0.25 ⁇ m, and / or a d 90 value ⁇ 2 ⁇ m, preferably d 90 ⁇ 1.8 ⁇ m, particularly preferably d 90 of 0.1 to 1.5 microns, most preferably d 90 from 0.1 to 1.0 microns, more preferably d 90 from 0.1 to 0.5 microns and more preferably d 90 from 0.2 to 0.4 ⁇ m
  • the solids are gels, preferably silica gels, in particular xerogels or aerogels, having an average particle size d 50 ⁇ 1.5 ⁇ m, preferably d 50 ⁇ 1 ⁇ m, particularly preferably d 50 of 0, 01-1 microns, most preferably 50 d from 0.05 to 0.9 .mu.m, particularly preferably d 50 of 0.05 to 0.8 microns, especially preferably from 0.05 to 0.5 micrometers and especially preferably from 0.1 to 0.25 ⁇ m, and / or a d 90 value ⁇ 2 ⁇ m, preferably d 90 0.05 to 1.8 ⁇ m, particularly preferably d 90 from 0.1 to 1.5 ⁇ m, very particularly preferably d 90 is from 0.1 to 1.0 ⁇ m, particularly preferably d 90 from 0.1 to 0.5 ⁇ m and especially preferably d 90 from 0.2 to 0.4 ⁇ m, and / or a d 99 value ⁇ 2 ⁇ m, preferably d 99
  • it is a small-pored xerogel, in addition to the d 50 , d 90 and d 99 values already contained in the embodiments explained directly above, in addition a pore volume of 0.2 to 0.7 ml / g, preferably 0.3 to 0.4 ml / g.
  • it is a xerogel that, in addition to the d 50 , d 90 and d 99 values already contained in connection with the second type of exemplary embodiments, has a pore volume of 0.8 to 1.4 ml / g , preferably 0.9 to 1.2 ml / g.
  • a xerogel that, in addition to the already given d 50 , d 90 and d 99 values, additionally has a pore volume of 1.5 to 2.1 ml / g, preferably 1.7 to 1.9 ml / g.
  • the jet mill 1 contains, as the schematic representation in the Fig. 2 It can be seen, an integrated air classifier 7, which is for example in types of jet mill 1 as fluidized bed jet mill or as a dense bed jet mill to a dynamic air classifier 7, which is advantageously arranged in the center of the grinding chamber 3 of the jet mill 1. Depending on the grinding gas volume flow and classifier speed, the desired fineness of the material to be ground can be influenced.
  • the entire vertical air classifier 7 is enclosed by a classifier housing 21, which consists essentially of the upper housing part 22 and the lower housing part 23.
  • the upper housing part 22 and the lower housing part 23 are provided at the upper or lower edge, each with an outwardly directed peripheral flange 24 and 25 respectively.
  • the two peripheral flanges 24, 25 are in the installation or functional state of the air classifier 8 on each other and are fixed by suitable means against each other. Suitable means for fixing are, for example, screw connections (not shown). As releasable fastening means may also serve brackets (not shown) or the like.
  • both circumferential flanges 24 and 25 are connected to one another by a hinge 26 so that the upper housing part 22 can be pivoted upward in the direction of the arrow 27 after loosening the flange connecting means relative to the lower housing part 23 and the upper housing part 22 from below and the lower housing part 23 are accessible from above.
  • the lower housing part 23 in turn is formed in two parts and it consists essentially of the cylindrical withdrawraumgephaseuse 28 with the peripheral flange 25 at its upper open end and a discharge cone 29, which tapers conically downwards.
  • the discharge cone 29 and the reformraumgephasepuruse 28 are at the upper and lower ends with flanges 30, 31 on each other and the two flanges 30, 31 of discharge cone 29 and reformraumgephase 28 are like the peripheral flanges 24, 25 connected by releasable fastening means (not shown).
  • the thus assembled classifier housing 21 is suspended in or on support arms 28a, of which a plurality of evenly spaced around the circumference of the classifier or compressor housing 21 of the air classifier 7 of the jet mill 1 are distributed and attack the cylindrical withdrawraumgephase 28.
  • An essential part of the housing installations of the air classifier 7 is in turn the classifying wheel 8 with an upper cover plate 32, with an axially spaced lower downstream cover plate 33 and arranged between the outer edges of the two cover plates 32 and 33, fixedly connected to these and evenly around the circumference of Classifying wheel 8 distributed blades 34 with appropriate contour.
  • the drive of the classifying wheel 8 is effected via the upper cover disk 32, while the lower cover disk 33 is the downstream cover disk.
  • the storage of the classifying wheel 8 comprises a positively driven forcibly digestradwelle 35, which is led out with the upper end of the classifier housing 21 and rotatably supports the classifying wheel 8 with its lower end within the classifier housing 21 in flying storage.
  • the removal of the sortradwelle 35 from the classifier housing 21 takes place in a pair of machined plates 36, 37 which close the classifier housing 21 at the upper end of an upwardly frustoconical housing end portion 38, the reformradwelle 35 lead and seal this shaft passage without obstructing the rotational movement of the prepareradwelle 35 ,
  • the upper plate 36 as a rotatably associated with the prepareradwelle 35 and rotatable about pivot bearings 35a on the lower Supported plate 37, which in turn is associated with a housing end portion 38.
  • the underside of the downstream cover disk 33 lies in the common plane between the peripheral flanges 24 and 25, so that the classifying wheel 8 is arranged in its entirety within the hinged housing upper part 22.
  • the upper housing part 22 also has a tubular product feed nozzle 39 of the Mahlgutholzgabe 4, the longitudinal axis parallel to the axis of rotation 40 of the classifying wheel 8 and its drive or withdrawradwelle 35 and as far as possible from this axis of rotation 40 of the classifying wheel 8 and its Drive or prepareradwelle removed 35, the housing upper part 22 is disposed radially outboard.
  • the classifier housing 21 receives the coaxial with the classifying wheel 8 arranged tubular outlet nozzle 20 which lies with its upper end just below the downstream cover plate 33 of the classifying wheel 8, but without being connected thereto.
  • an outlet chamber 41 is attached coaxially, which is also tubular, but whose diameter is substantially greater than the diameter of the outlet nozzle 20 and in the present embodiment, at least twice as large as the diameter of the outlet nozzle 20.
  • the outlet nozzle 20 is inserted into an upper cover plate 42 of the outlet chamber 41. Below the outlet chamber 41 is closed by a removable cover 43.
  • outlet nozzle 20 and outlet chamber 41 is held in a plurality of support arms 44 which are evenly distributed star-shaped around the circumference of the unit, connected with their inner ends in the region of the outlet nozzle 20 fixed to the unit and secured with their outer ends on the classifier housing 21.
  • the outlet nozzle 20 is surrounded by a conical annular housing 45 whose lower, larger outer diameter corresponds at least approximately to the diameter of the outlet chamber 41 and its upper, smaller outer diameter at least approximately the diameter of the classifying wheel 8.
  • the support arms 44 terminate and are firmly connected to this wall, which in turn is part of the assembly of outlet nozzle 20 and outlet chamber 41.
  • the support arms 44 and the annular housing 45 are parts of a scavenging air device (not shown), wherein the scavenging air prevents the ingress of matter from the interior of the classifier housing 21 into the gap between the classifying wheel 8 or more precisely its lower cover disk 3 and the outlet nozzle 20.
  • the support arms 44 are formed as tubes, with their outer end portions passed through the wall of the classifier housing 21 and connected via a suction filter 46 to a purge air source (not shown) ,
  • the annular housing 45 is closed at the top by a perforated plate 47 and the gap itself can by an axial adjustable annular disc in the area between the perforated plate 47 and lower cover plate 33 of the classifying wheel 8 be adjustable.
  • the outlet from the outlet chamber 41 is formed by a fines discharge pipe 48, which is led into the separator housing 21 from the outside and is connected in a tangential arrangement to the outlet chamber 41.
  • the fine material discharge pipe 48 is part of the product outlet 6.
  • the lining of the junction of the fine material discharge pipe 48 with the outlet chamber 41 serves as a deflecting cone 49.
  • a sighting air inlet spiral 50 and a coarse material discharge 51 are assigned to the housing end section 38 in a horizontal arrangement.
  • the direction of rotation of the sighting air inlet spiral 50 is opposite to the direction of rotation of the classifying wheel 8.
  • Grobgutaustrag 51 is the housing end portion 38 detachably associated with the lower end of the Gescousendabiteses 38 a flange 52 and the upper end of Grobgutaustrages 51 assigned a flange 53 and both flanges 52 and 53 are in turn releasably connected together by known means when the air classifier is ready for use.
  • the dispersing zone to be designed is designated 54.
  • Flanges machined on the inner edge (chamfered) for a clean flow guidance and a simple lining are designated with 55.
  • a replaceable protective tube 56 is still applied to the inner wall of the outlet nozzle 20 as a wear part and a corresponding replaceable protective tube 57 may be applied to the inner wall of the outlet chamber 41.
  • view air is introduced into the air classifier 7 at a pressure gradient and at a suitably chosen entry speed via the sighting air inlet spiral 50.
  • the classifying air spirals upward into the region of the classifying wheel 8.
  • the "product" of solid particles of different mass is introduced into the classifier housing 21 via the product feed port 39. From this product, the coarse material, ie the proportion of particles with a greater mass against the classifying air in the range of Grobgutaustrages 51 and is provided for further processing.
  • the fine material ie the particle fraction with a smaller mass is mixed with the classifying air, passes radially from outside to inside through the classifying wheel 8 into the outlet nozzle 20, into the outlet chamber 41 and finally via a fine material outlet pipe 48 into a fine material outlet or outlet 58, as well as from there in a filter in which the resources in the form of a fluid, such as air, and fines are separated.
  • Coarser fines constituents are thrown radially out of the classifying wheel 8 and added to the coarse material to the classifier housing 21 with the coarse material leave or so long in the classifier housing 21 to circle until it has become fines of such a grain that it is discharged with the classifying air.
  • the air classifier 7 can again be well maintained by the division of the classifier housing 21 in the manner described and the assignment of the classifier components to the individual sub-housings and components which have become defective can be replaced with relatively little effort and within short maintenance times.
  • This classifying wheel 8 according to the Fig. 3
  • the upper cover plate 32 and the axially spaced lower downstream cover plate 33 is rotatable about the axis of rotation 40 and thus the longitudinal axis of the air classifier 7.
  • the diametrical extent of the classifying wheel 8 is perpendicular to the axis of rotation 40, ie to the longitudinal axis of the air classifier 7, regardless of whether the axis of rotation 40 and thus said longitudinal axis is vertical or horizontal.
  • the lower downstream cover disk 33 concentrically encloses the outlet nozzle 20.
  • the blades 34 are connected to both cover disks 33 and 32.
  • the two cover plates 32 and 33 are deviating now deviating from the prior art conical and was preferably such that the distance between the upper cover plate 32 from the downstream cover plate 33 from the rim 59 of the blades 34 inward, ie towards the axis of rotation 40 back, and Although preferably continuous, such as linear or non-linear, and with further preference so that the surface of the flow-through cylinder jacket for each radius between the blade outlet edges and outlet nozzle 20 remains at least approximately constant.
  • the decreasing due to the decreasing radius in known solutions outflow rate remains at least approximately constant in this solution.
  • the shape of the non-parallel-sided cover disk may be such that at least approximately so that the surface of the cylinder jacket through which flows through remains constant for each radius between blade outlet edges and outlet nozzle 20.
  • the raw material to be ground was a precipitated silica prepared as follows:
  • 117 m 3 of water are placed in a 150 m 3 precipitation tank with inclined base, MIG inclined blade agitation system and Ekato fluid shear turbine and 2.7 m 3 of water glass are added.
  • the ratio of water glass to water is adjusted so that there is an alkali number of 7.
  • the template is heated to 90 ° C.
  • water glass at a metering rate of 10.2 m 3 / h and sulfuric acid at a metering rate of 1.55 m 3 / h are metered in simultaneously with stirring over a period of 75 minutes.
  • silica 1 The data of silica 1 are given in Table 1.
  • 45% strength by weight sulfuric acid and soda water glass are intensively mixed in such a way that a reactant ratio corresponding to an excess of acid (0.25 N) and an SiO 2 concentration of 18.5% by weight is established.
  • the resulting hydrogel is stored overnight (about 12 hours) and then broken to a particle size of about 1 cm. It is washed with deionized water at 30-50 ° C until the conductivity of the wash water is below 5mS / cm.
  • the hydrogel prepared as described above is aged with ammonia addition at pH 9 and 80 ° C for 10-12 hours, and then adjusted to pH 3 with 45 wt .-% sulfuric acid.
  • the hydrogel then has a solids content of 34-35%. It is then coarsely ground on a pin mill (Alpine Type 160Z) to a particle size of approx. 150 ⁇ m.
  • the hydrogel has a residual moisture of 67%.
  • silica 2 The data of silica 2 are given in Table 1.
  • silica 3a The data of silica 3a are given in Table 1.
  • the hydrogel prepared as described above is further washed at about 80 ° C until the conductivity of the wash water is less than 2 mS / cm and dried in a convection oven (Fresenberger POH 1600.200) at 160 ° C to a residual moisture content of ⁇ 5%.
  • the xerogel is pre-shredded to a particle size ⁇ 100 ⁇ m (Alpine AFG 200).
  • silica 3b The data of silica 3b are given in Table 1.
  • the hydrogel prepared as described above is aged with addition of ammonia at pH 9 and 80 ° C for 4 hours, then adjusted with 45 wt .-% sulfuric acid to about pH 3 and in a convection oven (Fresenberger POH 1600.200) at 160 ° C to a Residual moisture of ⁇ 5% dried.
  • the xerogel is pre-shredded to a particle size ⁇ 100 ⁇ m (Alpine AFG 200).
  • silica 3c The data of silica 3c are given in Table 1.
  • Table 1 - Physico-chemical data of the unmilled starting materials Silica 1 silica 2 silica 3a silica 3b silica 3c particle size distribution by laser diffraction (Horiba LA 920) d 50 [ ⁇ m] 22.3 nb nb nb d 99 [ ⁇ m] 85.1 nb nb nb nb d 10 [ ⁇ m] 8.8 nb nb nb nb Particle size distribution using sieve analysis > 250 ⁇ m% nb nb nb 0.0 0.2 > 125 ⁇ m% nb nb nb 1.06 2.8 > 63 ⁇ m% nb nb nb 43.6 57.8 > 45 ⁇ m% nb nb nb 44.0 36.0 ⁇ 45 ⁇ m% nb nb 10.8 2.9 Humidity% 4.8 67 ⁇ 3
  • a fluidized bed counter-jet mill according to FIG. 1 . 2 and 3 first via the two heating nozzles 5a (of which in FIG. 1 only one shown), which are charged with 10 bar and 160 ° C hot compressed air, heated to a mill outlet temperature of about 105 ° C.
  • the mill is downstream of the filtration of the ground material a filter unit (not in FIG. 1 shown), the filter housing is heated in the lower third indirectly via attached heating coils by means of 6 bar saturated steam also to prevent condensation. All equipment surfaces in the area of the mill, the separation filter, as well as the supply lines for steam and hot compressed air are particularly insulated.
  • the supply of the heating nozzles with hot compressed air is started and the admission of the three grinding nozzles with superheated steam (38 bar (abs), 330 ° C) started.
  • water is injected in the starting phase and during grinding in the grinding chamber of the mill via a two-fluid nozzle operated with compressed air in dependence on the mill outlet temperature.
  • the product task is started when the relevant process parameters (see Table 2) are constant.
  • the regulation of the feed quantity is dependent on the self-adjusting stream.
  • the classifier flow regulates the feed quantity such that approx. 70% of the nominal flow can not be exceeded.
  • the crushing of the coarse material takes place in the expanding steam jets (grinding gas). Together with the expanded grinding gas, the product particles in the center of the mill container rise to the classifying wheel. Depending on the set speed of the sifter and the amount of grinding steam (see Table 1), the particles which have a sufficient fineness pass with the grinding steam into the fine-material outlet and from there into the downstream separation system, while coarse particles return to the milling zone and are subjected to repeated comminution.
  • the discharge of the separated fine material from the separation filter in the subsequent ensiling and packaging is done by means of rotary valve.
  • the grinding pressure of the grinding gas prevailing at the grinding nozzles, or the resulting amount of grinding gas in conjunction with the speed of the dynamic Schaufelradsichters determine the fineness of the grain distribution function and the upper grain limit.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Combined Means For Separation Of Solids (AREA)
  • Disintegrating Or Milling (AREA)
EP15002331.5A 2006-10-16 2007-10-16 Procede de production de particules fines a l'aide d'un broyeur a jet et broyeur a jet associe Pending EP2959975A1 (fr)

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DE102006048865A DE102006048865A1 (de) 2006-10-16 2006-10-16 Verfahren zur Erzeugung feinster Partikel und Strahlmühle dafür sowie Windsichter und Betriebsverfahren davon
EP07817686A EP2091652A1 (fr) 2006-10-16 2007-10-16 Procédé de production de particules extrêmement fines, pulvérisateur à jet approprié, séparateur pneumatique et procédé d'exploitation correspondant

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EP15002331.5A Pending EP2959975A1 (fr) 2006-10-16 2007-10-16 Procede de production de particules fines a l'aide d'un broyeur a jet et broyeur a jet associe

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EP3991858A1 (fr) * 2020-11-03 2022-05-04 NETZSCH Trockenmahltechnik GmbH Procédés de fonctionnement pour un trieur et trieur de classification

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TW201446329A (zh) 2013-03-11 2014-12-16 道達爾研究及技術弗呂公司 用噴射磨製造形態優化的細顆粒的方法、用於該方法的噴射磨和所製造的顆粒
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JP6380365B2 (ja) * 2015-12-22 2018-08-29 Ｊｆｅスチール株式会社 製造設備およびそのメンテナンス方法
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EP3386638B1 (fr) 2016-11-07 2019-03-13 Wacker Chemie AG Procédé de broyage de matierès solides contenant silicium
CN116033969A (zh) 2020-11-20 2023-04-28 巴斯夫欧洲公司 喷射磨
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EP3991858A1 (fr) * 2020-11-03 2022-05-04 NETZSCH Trockenmahltechnik GmbH Procédés de fonctionnement pour un trieur et trieur de classification

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CN101557877A (zh) 2009-10-14
JP2010506706A (ja) 2010-03-04
US20090236451A1 (en) 2009-09-24
BRPI0717607B1 (pt) 2019-08-20
WO2008046403A1 (fr) 2008-04-24
CN101557877B (zh) 2013-04-10
JP5393466B2 (ja) 2014-01-22
DE102006048865A1 (de) 2008-04-17
BRPI0717607A2 (pt) 2014-01-14
DE112007003097A5 (de) 2009-09-17
EP2091652A1 (fr) 2009-08-26
US7866582B2 (en) 2011-01-11

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