EP2101918A1 - Verfahren zur erzeugung feinster partikel und strahlmühle dafür sowie windsichter und betriebsverfahren davon - Google Patents
Verfahren zur erzeugung feinster partikel und strahlmühle dafür sowie windsichter und betriebsverfahren davonInfo
- Publication number
- EP2101918A1 EP2101918A1 EP07817687A EP07817687A EP2101918A1 EP 2101918 A1 EP2101918 A1 EP 2101918A1 EP 07817687 A EP07817687 A EP 07817687A EP 07817687 A EP07817687 A EP 07817687A EP 2101918 A1 EP2101918 A1 EP 2101918A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- bar
- jet mill
- classifier
- approximately
- mill
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
-
- 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 with an integrated dynamic air classifier and a jet mill with such an air classifier, and an air classifier and an operating method thereof 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 jet mill wind miller.
- 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.
- jet mill in the grinding chamber of which at least one high-energy grinding mill is also known. Jet is introduced with high flow energy, the grinding chamber having, in addition to the inlet device for the at least one grinding jet, an inlet for the material to be ground and an outlet for the product, and wherein in the area of the meeting of ground material and at least one
- Milling jet of hot steam and regrind have at least about the same temperature.
- a corresponding air classifier is particularly suitable for a jet mill, e.g. from EP 0 472 930 Bl. This air classifier and its operating methods are basically extremely satisfactory.
- the present invention therefore has the aim of further optimizing a method for producing finest particles by means of a jet mill and a jet mill with an air classifier integrated therein.
- a generic method for producing finest particles by means of a jet mill with an integrated dynamic air classifier which includes a classifying wheel and a prepareradwelle and a classifier housing, wherein between the classifying wheel and the classifier housing a classifier gap and between the reformradwelle and the classifier housing a shaft passage is formed characterized in that a rinsing rinsing of classifier gap and / or shaft passage with compressed gases of low energy content, and that Mahlstrahleinlässe, in particular grinding nozzles or grinding nozzles contained therein, are present, which are fed with high-energy hot steam.
- the flushing gas is at a pressure of not more than at least approximately 0.4 bar, preferably not more than at least about 0.3 bar and in particular not more than about 0.2 bar is used above the mill internal pressure.
- the internal mill pressure can be at least approximately in the range from 0.1 bar to 0.5 bar.
- the purge gas at a temperature of about 80 0 C to about 120 0 C, in particular approximately 100 0 C is used, and / or if as purge gas low-energy compressed air in particular with about 0.3 bar to about 0 , 4 bar is used.
- the superheated steam preferably has a pressure of at least approximately 12 bar, preferably at least approximately 25 bar and more preferably at least approximately 40 bar, and / or becomes
- Temperature of the superheated steam chosen so that it is dry at the end of the process.
- a jet mill according to the invention with an integrated dynamic air classifier for the production of finest particles which 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, are also scavenging provided, by means of which a gap rinsing of classifier gap and / or shaft passage with compressed gases of low energy content is carried out, and is further provided that Mahlstrahleinlässe, such as grinding nozzles or grinding nozzles contained therein, are present, which are fed with high-energy hot steam.
- Mahlstrahleinlässe such as grinding nozzles or grinding nozzles contained therein
- the flushing devices are designed to supply the flushing gas at a pressure of not more than at least approximately 0.4 bar, preferably not more than at least approximately 0.3 bar and in particular not more than approximately 0 2 bar above the mill internal pressure. It is even more preferable if the mill interior pressure is at least approximately in the range of 0, 1 bar to 0, 5 bar.
- the H representeddatnpf a pressure of at least approximately 12 bar, preferably at least about 25 bar and more preferably at least about 40 bar, and / or that the temperature of the superheated steam is selected so that this is dry at the end of the process, and / or that one
- Source such as a tank for the superheated steam as resources included or assigned.
- the jet mill may be further developed by being a fluid bed jet mill or a dense bed jet mill.
- a further preferred embodiment is that grinding nozzles are provided, which are connected to a steam supply line, such as conduit means, which is equipped with expansion bends. It may further be provided with preference that the steam supply line is connected to a source of steam.
- the classifying rotor or the classifying wheel has an increasing clear height with decreasing radius. It is further preferred if the flow-through surface of the classifying rotor or wheel is at least approximately constant. _ c _
- the classifying rotor or the classifying wheel has an exchangeable, co-rotating dip tube, and / or that a fine-material outlet chamber is provided which has a cross-sectional widening in the flow direction.
- 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 avoid condensation and / or contain facilities for preventing condensation.
- the jet mill according to the invention can advantageously contain, in particular, an air classifier which contains individual features or combinations of features of the air classifier according to EP 0 472 930 B1.
- an air classifier which contains individual features or combinations of features of the air classifier according to EP 0 472 930 B1.
- the air classifier can contain means for reducing the flow components of the flow according to EP 0 472 930 B1.
- 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.
- the invention further provides a dynamic air classifier with a classifying wheel or classifying wheel, a classifying wheel shaft and a classifier housing, wherein a classifier gap is formed between the classifying wheel and the classifier housing, and a shaft passage is formed between the classifying wheel shaft and the classifier housing, and further provided rinsing units are by means of which a rinsing of the gap gap and / or shaft passage with compressed gases low T / DE2007 / 001852
- This dynamic air classifier can be further developed in that the purging devices are designed to supply the purging gas at a pressure of not more than at least approximately 0.4 bar, preferably not more than at least approximately 0.3 bar and in particular not more than approximately 0, 2 bar above the internal mill pressure. Alternatively or additionally, it may be provided that the internal mill pressure is at least approximately in the range of 0.1 bar to 0.5 bar.
- the purge gas at a temperature of about 80 0 C to about 120 0 C, in particular approximately 100 0 C is used, and / or if as purge gas low-energy compressed air in particular with about 0.3 bar to about 0 , 4 bar is used.
- the superheated steam has a pressure of at least approximately 12 bar, preferably at least approximately 25 bar and more preferably at least approximately 40 bar, and / or that the temperature of the superheated steam is selected such that this temperature dry at the end of the process.
- a source such as e.g. a tank containing or assigned to superheated steam as operating equipment.
- a classifying rotor or indexing wheel is included, which has an increasing height with decreasing radius.
- the area of the classifying rotor or rotor through which flowed through can be at least approximately constant.
- a classifying rotor or classifying wheel is included, which has an exchangeable, co-rotating immersion tube, and / or that a fine-material outlet chamber is provided, which in the flow direction is a
- Classifying rotor or wheel, a reformradwelle 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, is provided according to the invention that a rinsing rinsing of classifier gap and / or shaft passage with compressed gases low energy content occurs, and that Mahlstrahleinlässe, in particular grinding nozzles or grinding nozzles contained therein, are present, which are fed with high-energy hot steam.
- the rinsing gas at a temperature of about 80 0 C to about 120 0 C, in particular approximately 100 0 C is used.
- low-pressure compressed air in particular with about 0.3 bar to about 0.4 bar, is used as purge gas.
- the superheated steam may have a pressure of at least approximately 12 bar, preferably at least about 25 bar and 52
- the temperature of the superheated steam can be selected so that it is dry at the end of the process.
- the process is carried out in a grinding system (grinding apparatus), preferably in a grinding system comprising a jet mill, particularly preferably comprising an opposed jet mill.
- a feedstock to be comminuted is accelerated in expanding high-speed gas streams 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 sifter, preferably a dynamic sifter, more preferably a dynamic bucket wheel sifter or a sifter according to FIGS. 2 and 3.
- This dynamic air sifter contains a classifying wheel and a classifying wheel shaft and a classifier housing, wherein between the classifying wheel and the classifier housing, a classifier gap and between the bombardradwelle and the classifier housing, a shaft passage is formed, and is characterized in that a rinsing rinsing of classifier gap and / or shaft passage with compressed low-energy gases takes place.
- the upper particle is confined, 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 a sufficient fineness , from the sifter and from the mill is executed. Too coarse particles return to the milling zone and are subjected to further comminution.
- a classifier can be connected downstream as a separate unit of the mill, but preferably an integrated classifier is used.
- 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 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.
- the heating takes place in that hot gas is passed 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 vapor.
- 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. Preferably located for it in the grinding room inlets or nozzles. These inlets or nozzles can be the same inlets or nozzles through which the grinding jets are also passed during the grinding phase (grinding nozzles). But it is also possible that in the grinding chamber separate inlets or nozzles (heating nozzles) are present, through which the hot gas and / or gas mixture can be introduced.
- the heating gas or heating gas mixture is introduced by at least two, preferably three or more inlaid inlet or nozzles, which are arranged on the circumference of the preferably round mill container, that the rays all at one point in the interior of 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 equipment has a temperature of 200 to 800 0 C, more preferably 250 to 600 0 C and in particular 300 to 400 0 C.
- Fig. 1 diagrammatically shows an embodiment of a jet mill in a partially sectioned schematic drawing
- Fig. 3 shows a schematic representation and a vertical section of a classifying wheel of an air classifier.
- FIG. 1 shows an exemplary embodiment of a jet mill 1 with a cylindrical housing 2, which encloses a grinding chamber 3, a grinding material feed 4 approximately at half the height of the grinding chamber 3, at least one grinding jet inlet 5 in the lower region of the grinding chamber 3 and a product outlet 6 is shown in the upper region of the grinding chamber 3.
- 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 may be a classifying wheel which is common in air classifiers and whose blades (see, for example, in connection with FIG. 3) define radially extending blade channels, at the outer ends of which the classifying air enters and particles of smaller particle size or mass to the central outlet and to the pro Duct outlet 6 entrains, while larger particles or particles of larger mass are rejected under the influence of centrifugal force.
- the air classifier 7 and / or at least its classifying wheel 8 are equipped with at least one design feature according to EP 0 472 930 B1.
- Mahlstrahleinlass 5 for example, consisting of a single, radially directed inlet opening or inlet nozzle 9 to impinge a single grinding jet 10 on the Mahlgutpiety that come from the Mahlgutiergabe 4 in the area of the grinding jet 10, with high energy and the To dismantle regrind particles into smaller partial particles, which are sucked in by the classifying wheel 8 and, if they 01852
- two or more grinding jet inlets preferably grinding nozzles, in particular 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12 Mahlstrahleinlässe are 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 can 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.
- One, but preferably also several, particularly preferably 2, 3, 4, 5, 6, 7 or 8 heating openings or nozzles 5a may be included.
- the mill contains two heating nozzles or openings and three grinding nozzles or openings. 7 001852
- the processing temperature can be influenced by using an internal heat source 11 between the grinding material feed 4 and the area of the grinding jets 10 or a corresponding heating source 12 in the region outside the grinding material feed 4 or by processing particles of an already warm grinding material, avoiding Heat losses in the Mahlgutiergabe 4 passes, including 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 operable and selected according to market availability, so that further explanation is not 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.
- this temperature drop is to be compensated so far by the heating of the ground material that regrind and grinding jet 10 in the region of the center 17 of the grinding chamber 3 at least two colliding grinding jets 10 or a multiple of two grinding jets 10 have the same temperature. 7 001852
- Representing the present embodiment of 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 conduit means 19 to the grinding jet inlet 5 or the
- line devices 19 equipped with expansion bends which are then also referred to as steam supply lines, to the inlet or grinding nozzles 9, that is to say preferably when the steam supply line - device is connected to a source of steam as a reservoir or generating device 18.
- 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 accumulation.
- This can For example, be realized by using as thin as possible flanges in and to connect the conduit means 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 without jumps 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.
- the particles to be produced from the preferably processed material are 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
- 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 ⁇ m is disadvantageous for applications in coating systems, since it can not produce thin layers with a smooth surface.
- solids except for an average particle size d 50 of less than 1.5 microns to be ground and also to achieve a very narrow particle distribution.
- amorphous or crystalline solids having an average particle size d are so ⁇ 1.5 ⁇ m and / or a d 90 value ⁇ 2 ⁇ m and / or a d 99 value ⁇ 2 ⁇ m.
- amorphous solids may be gels but also those with different structure such.
- particles of agglomerates and / or aggregates Preference is given to solids containing or consisting of at least one (em) metal and / or at least one (e) m metal oxide, in particular amorphous oxides of metals of the 3rd and 4th main group of the Periodic Table of the Elements. This applies both to the gels and to the other amorphous solids, in particular those containing particles of agglomerates and / or aggregates.
- Particular preference is given to precipitated silicas, pyrogenic silicas, silicates and silica gels, where silica gels include both hydro- and aerogels as well as xerogels.
- Such amorphous solids in general with 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 described, for example, in US Pat. 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 Reagglotneration 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 of its preferred embodiments is 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.
- 01852 01852
- the inventive method also has the advantage that when starting up the grinding system no or very small amounts of condensate in the grinding system, especially in the mill arise. During cooling, dried gas can be used. This also arises when
- Cooling no condensate in the grinding system 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 milling 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.
- these particles are particulate substances that are perceptible by optical methods and not 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 have no three-dimensional network or at least no network of primary particles extending over the entire particle. Instead, they contain aggregates and agglomerates of primary particles. Examples of these are precipitated silicas and fumed silicas.
- the inventive technology may be any particles, in particular milled amorphous particles such that powdered solids having a mean particle size d as ⁇ 1.5 microns and / or a d 90 value of ⁇ 2 micrometers and / or a d 99 value of ⁇ 2 ⁇ m are obtained.
- a mean particle size d as ⁇ 1.5 microns and / or a d 90 value of ⁇ 2 micrometers and / or a d 99 value of ⁇ 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, especially preferably from 0.05 52
- TEM average particle size
- d 90 value ⁇ 2 ⁇ m preferably d 90 ⁇ 1.8 ⁇ m, particularly preferably d 90 from 0.1 to 1 , 5 ⁇ m, very particularly preferably d90 from 0.1 to 1.0 ⁇ m and particularly preferably d 90 from 0.1 to 0.5 ⁇ m, and / or a d 99 value ⁇ 2 ⁇ m, preferably d 99 ⁇ 1, 8 microns, more preferably d 99 ⁇ 1.5 microns, most preferably d 99 from 0.1 to 1.0 microns and more preferably d 99 from 0.25 to 1.0 microns. All previously mentioned particle sizes refer to the particle size determination by means of TEM analysis and image evaluation.
- These solids may be gels but also other types of amorphous or crystalline solids.
- the first specific embodiments of the solids in question are particulate solids containing aggregates and / or agglomerates, in particular precipitated silicas and / or fumed silicic acid 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
- the solids are gels, preferably silica gels, in particular xerogels or aerogels, having an average particle size d so ⁇ 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.
- a further alternative embodiment is a xerogel which, in addition to the d 50 , d 90 and d 99 values already contained in connection with the second type of exemplary embodiment, 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 illustration in FIG. 2 shows, an integrated air classifier 7, which, for example in the case of types of the jet mill 1 as a fluidized bed jet mill or as a dense bed jet mill, is a dynamic air classifier 7, which is advantageous in the art Center of the grinding chamber 3 of the jet mill 1 is arranged.
- an integrated air classifier 7 which, for example in the case of types of the jet mill 1 as a fluidized bed jet mill or as a dense bed jet mill, is a dynamic air classifier 7, which is advantageous in the art Center of the grinding chamber 3 of the jet mill 1 is arranged.
- the desired fineness of the material to be ground can be influenced.
- the entire vertical air classifier 7 is surrounded 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 by a hinge 26. connected so that the upper housing part 22 after loosening the Flanschrivssch with respect to the lower housing part 23 can be pivoted upward in the direction of the arrow 27 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 reformraumgephase 28 are at the top and bottom with flanges 30, 31 to each other and the two flanges 30,
- discharge cone 29 and reformraumgephase 28 are like the peripheral flanges 24, 25 connected by releasable fastening means (not shown).
- the assembled so terter housing 21 is suspended in or on support arms 28 a, 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 reformraumgephase 28.
- An essential part of the housing installations of the air classifier 7 is in turn the classifying wheel 8 with an upper cover disk 32, with a lower downstream cover disk 33 spaced axially therefrom and with the outer disks of the two cover disks 32 and 33 fixedly connected thereto and evenly around the circumference of the classifying wheel 8 distributed blades 34 with appropriate contour.
- the drive of the classifying wheel 8 on the upper cover plate
- the storage of the classifying wheel 8 comprises a sighting wheel shaft 35 which is forcibly driven in an expedient manner and which is led out of the classifier housing 21 with the upper end and rotatably supports the classifying wheel 8 with its lower end inside the classifier housing 21 in a flying bearing.
- the removal of the prepareradwelle 35 from the classifier housing 21 takes place in a pair of machined plates 36, 37, the classifier housing 21 at the upper end of a complete the top frusto-conical housing end portion 38, the sortradwelle 35 lead and seal this shaft passage without obstructing the rotational movement of the prepareradwelle 35.
- the upper plate 36 can be rotatably associated with the prepareradwelle 35 as a flange and rotatably supported via pivot bearings 35a on the lower 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 housing upper 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 integrated dynamic air classifier 7 of the jet mill 1 contains a classifying wheel 8 and a classifying wheel shaft 35 as well as a classifier housing 21, as already explained.
- a classifier gap 8a is defined between the classifying wheel 8 and the classifier housing 21, and a shaft passage 35b is formed between the classifying wheel shaft 35 and the classifier housing 21 (see FIGS. 2 and 3).
- a method for producing extremely fine particles is carried out with this jet mill 1 with an integrated dynamic air classifier 7.
- the innovation over conventional jet mills is that a rinsing of the gap gap of the separator 8a and / or shaft passage
- 35a is carried out with compressed gases of low energy content.
- the special of this design is just the combination in that milling jet inlets 5, in particular grinding nozzles or grinding nozzles contained therein, are present, which are charged with high-energy superheated steam. At the same time, high-energy media and low-energy media are used.
- the classifier housing 21 accommodates the tubular discharge nozzle 20 which is arranged coaxially with the classifying wheel 8 and lies with its upper end close to the downstream cover sheet 33 of the classifying wheel 8, but without being connected thereto.
- an outlet chamber 41 is attached coaxially, which is also tubular, but the diameter of which is substantially larger than the diameter of the Austrittsstut- zen 20 and in the present embodiment, at least twice as large as the diameter of the outlet nozzle 20th is. At the transition between the outlet nozzle 20 and the outlet chamber 41, therefore, there is a significant diameter jump.
- 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 Ringgephaseu- se 45, the lower, larger outer diameter at least approximately the diameter of the outlet chamber 41 and its upper, smaller outer diameter at least approximately corresponds to 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 device (not shown), the scavenging air the penetration of matter from the interior of the classifier housing 21 in the gap between the classifying wheel 8 or more precisely its lower cover plate 3 and the outlet nozzle 20th prevented.
- the support arms 44 are formed as tubes, with their outer end sections passed through the wall of the classifier housing 21 and via a suction filter 46 to a purge air source (not shown) ) connected.
- the annular housing 45 is closed at the top by a perforated plate 47 and the gap itself can be adjusted by an axially adjustable annular disc in the area between perforated plate 47 and lower cover plate 33 of the classifying wheel 8.
- the outlet from the outlet chamber 41 is formed by a fine-material discharge tube 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.
- the coarse material discharge 51 is detachably associated with the housing end portion 38, wherein a flange 52 is assigned to the lower end of the housing end portion 38 and a flange 53 to the upper end of the coarse material discharge 51 and both flanges 52 and 53 are in turn releasably connected to each other by known means, if the Air classifier 7 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 rises spirally 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 pipe 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 into a filter in which the operating medium in the form of a fluid, such as air, and fines are separated from each other.
- Coarser fines constituents are thrown radially out of the classifying wheel 8 and mixed with the coarse material in order to leave the classifier housing 21 with the coarse material or to circle in the classifier housing 21 until it has become fines of such a grain size that it is discharged with the classifying air.
- the wind sifter 7 can again be well maintained by dividing the classifier housing 21 in the manner described and assigning the classifier components to the individual part housings, and components which have become defective can be replaced with relatively little effort and within short maintenance times.
- the sighting wheel 8 with the two cover disks 32 and 33 and the blade ring 59 arranged therebetween with the blades 34 is still shown in already known, conventional form with parallel and parallel-sided cover disks 32 and 33, 3, the classifying wheel 8 is shown for a further embodiment of the air classifier 7 of an advantageous development.
- This classifying wheel 8 contains, in addition to the blade ring 59 with the blades 34, the upper cover disk 32 and the lower downstream cover disk 33 spaced axially therefrom and 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. 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 upper cover plate 32 and the lower cover plate 33 it is also possible that only one of these two cover plates 32 or 33 is conical in the manner explained and the other cover plate 33 or 32 is flat, as in the context of the embodiment shown in FIG. 2 for both shields 32 and 33 is the case.
- 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 milled was a precipitated silica prepared as follows:
- 117 m 3 of water are introduced into a 150 m 3 precipitation vessel 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 0 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 min.
- 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 h) and then broken to a particle size of about 1 cm. It is washed with deionized water at 30 - 50 0 C until the conductivity of the wash water is below 5 mS / cm.
- the hydrogel prepared as described above is aged with ammonia addition at pH 9 and 80 0 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%. Subsequently, it is 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 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 0 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 0 C to a Residual moisture of ⁇ 5% dried.
- the xerogel is pre-shredded to a particle size ⁇ 100 ⁇ m (Alpine AFG 200).
- a fluidized-bed counter jet mill In preparation for the actual grinding with superheated water vapor, a fluidized-bed counter jet mill according to Figure 1, 2 and 3 at first on the two heating nozzles 5a (of which shown in Figure 1 is only one), which are applied to 10 bar and 160 0 C hot compressed air, up to A mill outlet temperature of about 105 0 C heated.
- the mill is downstream of the filtration of a deposit of filter plant (not shown in Figure 1), the filter housing is heated in the lower third indirectly via mounted 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 encryption is supply to the heating nozzles with hot compressed air from and the charging of the three grinding nozzles with superheated steam (38 bar (abs), 330 0 C) is 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 launch 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 reach the one have sufficient fineness with the grinding steam in the fines exit and from there into the downstream separation system, while too coarse particles go back into the milling zone and are subjected to a further 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.
- Example 1 Example 2 Example 3a Example 3b Example 3c
- Example 1 Example 2 Example 3a Example 3b Example 3c
- peripheral flange 24 peripheral flange 25 peripheral flange
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006048864A DE102006048864A1 (de) | 2006-10-16 | 2006-10-16 | Verfahren zur Erzeugung feinster Partikel und Strahlmühle dafür sowie Windsichter und Betriebsverfahren davon |
PCT/DE2007/001852 WO2008046404A1 (de) | 2006-10-16 | 2007-10-16 | Verfahren zur erzeugung feinster partikel und strahlmühle dafür sowie windsichter und betriebsverfahren davon |
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EP2101918A1 true EP2101918A1 (de) | 2009-09-23 |
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EP07817687A Pending EP2101918A1 (de) | 2006-10-16 | 2007-10-16 | Verfahren zur erzeugung feinster partikel und strahlmühle dafür sowie windsichter und betriebsverfahren davon |
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US (1) | US8074907B2 (de) |
EP (1) | EP2101918A1 (de) |
JP (1) | JP5393467B2 (de) |
CN (1) | CN101616742B (de) |
BR (1) | BRPI0717167B1 (de) |
DE (2) | DE102006048864A1 (de) |
WO (1) | WO2008046404A1 (de) |
Families Citing this family (20)
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JP4785802B2 (ja) * | 2007-07-31 | 2011-10-05 | 株式会社日清製粉グループ本社 | 粉体分級装置 |
DE102009045116A1 (de) * | 2009-09-29 | 2011-03-31 | Evonik Degussa Gmbh | Niederdruckvermahlungsverfahren |
DE102011014643A1 (de) * | 2011-03-21 | 2012-09-27 | Roland Nied | Betriebsverfahren für eine Strahlmühlenanlage und Strahlmühlenanlage |
WO2013044911A1 (de) | 2011-09-29 | 2013-04-04 | Natural Green Gmbh | Pflanzenwachstumsförderer, verfahren zu dessen herstellung, suspensionen und verwendung als suspension |
DE102013000426A1 (de) * | 2013-01-14 | 2014-07-17 | Roland Nied | Verfahren zur Strahlmahlung sowie Strahlmühle dafür |
EP3307440A1 (de) * | 2015-06-15 | 2018-04-18 | NETZSCH Trockenmahltechnik GmbH | Verfahren zum zerkleinern von mahlgut und mühle dafür |
CN105013588A (zh) * | 2015-08-03 | 2015-11-04 | 昆山市密友装备制造有限责任公司 | 超细颗粒分级装置 |
CN107116030A (zh) * | 2016-02-25 | 2017-09-01 | 神华集团有限责任公司 | 固体混合物的分离系统和分离方法 |
US9682404B1 (en) * | 2016-05-05 | 2017-06-20 | Rec Silicon Inc | Method and apparatus for separating fine particulate material from a mixture of coarse particulate material and fine particulate material |
WO2018082789A1 (de) * | 2016-11-07 | 2018-05-11 | Wacker Chemie Ag | Verfahren zum mahlen von silizium enthaltenden feststoffen |
CN107096608A (zh) * | 2017-05-27 | 2017-08-29 | 广州天地实业有限公司 | 一种立式超微粉碎机 |
CN107745131A (zh) * | 2017-10-26 | 2018-03-02 | 余国华 | 合金粉分选装置 |
RU2668675C1 (ru) * | 2017-11-07 | 2018-10-02 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Томский государственный университет систем управления и радиоэлектроники" (ТУСУР) | Способ дезинтегрирования кускового сырья |
CN108405089A (zh) * | 2018-03-10 | 2018-08-17 | 洛阳晟源新材料有限公司 | 一种连续进料风选装置 |
DE102018112411A1 (de) * | 2018-05-24 | 2019-11-28 | Netzsch Trockenmahltechnik Gmbh | Verfahren und Anlage zur Herstellung eines Ausgangsmaterials für die Herstellung von Seltenerd-Magneten |
CN108672037A (zh) * | 2018-06-21 | 2018-10-19 | 太仓金溪粉碎设备有限公司 | 一种超微粉碎装置 |
CN114746191A (zh) * | 2019-10-03 | 2022-07-12 | 凡留艾什技术股份有限公司 | 用于分选粉末颗粒的装置 |
DE102020006724A1 (de) | 2020-11-03 | 2022-05-05 | Netzsch Trockenmahltechnik Gmbh | Betriebsverfahren für einen Sichter und Sichter zur Klassifizierung |
KR20230104729A (ko) | 2020-11-20 | 2023-07-10 | 바스프 에스이 | 제트 밀 |
CN113527915B (zh) * | 2021-08-25 | 2022-04-01 | 乌海黑猫炭黑有限责任公司 | 一种应用于皮革色浆的色素炭黑的生产方法 |
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- 2007-10-16 JP JP2009532678A patent/JP5393467B2/ja active Active
- 2007-10-16 DE DE112007003151T patent/DE112007003151A5/de active Pending
- 2007-10-16 CN CN200780038508.9A patent/CN101616742B/zh not_active Ceased
- 2007-10-16 EP EP07817687A patent/EP2101918A1/de active Pending
- 2007-10-16 BR BRPI0717167-6A patent/BRPI0717167B1/pt active IP Right Grant
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Also Published As
Publication number | Publication date |
---|---|
DE102006048864A1 (de) | 2008-04-17 |
US8074907B2 (en) | 2011-12-13 |
DE112007003151A5 (de) | 2009-09-24 |
US20090261187A1 (en) | 2009-10-22 |
BRPI0717167B1 (pt) | 2019-03-06 |
CN101616742A (zh) | 2009-12-30 |
CN101616742B (zh) | 2013-08-21 |
WO2008046404A1 (de) | 2008-04-24 |
BRPI0717167A2 (pt) | 2014-01-14 |
JP2010506707A (ja) | 2010-03-04 |
JP5393467B2 (ja) | 2014-01-22 |
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