WO2014064239A1 - Procédé de granulation de matières fusibles - Google Patents

Procédé de granulation de matières fusibles Download PDF

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Publication number
WO2014064239A1
WO2014064239A1 PCT/EP2013/072366 EP2013072366W WO2014064239A1 WO 2014064239 A1 WO2014064239 A1 WO 2014064239A1 EP 2013072366 W EP2013072366 W EP 2013072366W WO 2014064239 A1 WO2014064239 A1 WO 2014064239A1
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WO
WIPO (PCT)
Prior art keywords
prills
spray
solidification
tower
koh
Prior art date
Application number
PCT/EP2013/072366
Other languages
German (de)
English (en)
Inventor
Axel GOTH
Pascal TRIBOLET
Original Assignee
Bertrams Chemieanlagen Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bertrams Chemieanlagen Ag filed Critical Bertrams Chemieanlagen Ag
Priority to CN201380067825.9A priority Critical patent/CN104884154B/zh
Priority to KR1020157013478A priority patent/KR20150081297A/ko
Publication of WO2014064239A1 publication Critical patent/WO2014064239A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
    • B01D45/02—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by utilising gravity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
    • B01D45/12—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces
    • B01D45/14—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces generated by rotating vanes, discs, drums or brushes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/12—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating drums
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/14—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating dishes or pans
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/14—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moving in free vortex flow apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B3/00—Spraying or sprinkling apparatus with moving outlet elements or moving deflecting elements
    • B05B3/02—Spraying or sprinkling apparatus with moving outlet elements or moving deflecting elements with rotating elements
    • B05B3/12—Spraying or sprinkling apparatus with moving outlet elements or moving deflecting elements with rotating elements with spray booms or the like rotating around an axis by means independent of the liquid or other fluent material discharged
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/10—Making granules by moulding the material, i.e. treating it in the molten state
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
    • C01D1/04—Hydroxides
    • C01D1/44—Preparation in the form of granules, pieces, or other shaped products
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28C—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA COME INTO DIRECT CONTACT WITHOUT CHEMICAL INTERACTION
    • F28C3/00—Other direct-contact heat-exchange apparatus
    • F28C3/06—Other direct-contact heat-exchange apparatus the heat-exchange media being a liquid and a gas or vapour
    • F28C3/08—Other direct-contact heat-exchange apparatus the heat-exchange media being a liquid and a gas or vapour with change of state, e.g. absorption, evaporation, condensation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28C—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA COME INTO DIRECT CONTACT WITHOUT CHEMICAL INTERACTION
    • F28C3/00—Other direct-contact heat-exchange apparatus
    • F28C3/10—Other direct-contact heat-exchange apparatus one heat-exchange medium at least being a fluent solid, e.g. a particulate material
    • F28C3/12—Other direct-contact heat-exchange apparatus one heat-exchange medium at least being a fluent solid, e.g. a particulate material the heat-exchange medium being a particulate material and a gas, vapour, or liquid
    • F28C3/14—Other direct-contact heat-exchange apparatus one heat-exchange medium at least being a fluent solid, e.g. a particulate material the heat-exchange medium being a particulate material and a gas, vapour, or liquid the particulate material moving by gravity, e.g. down a tube
    • G—PHYSICS
    • G05—CONTROLLING; REGULATING
    • G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D13/00—Control of linear speed; Control of angular speed; Control of acceleration or deceleration, e.g. of a prime mover

Definitions

  • the invention relates to a method for granulating fusible materials, wherein spherical prills are produced from the molten material and transported through a gaseous cooling medium flowing in the longitudinal direction and the outer surface of the spherical prills is cooled to a temperature less than or equal to the solidification temperature, whereupon the spherical prills be further cooled in a heat exchanger.
  • the invention relates to a solidification tower for granulating fusible materials, wherein spherical prills are produced from the molten substance, and transported longitudinally and cooled by a gaseous medium flowing through, with an upstream collecting tank for ⁇ ztkali, a downstream conveyor belt and heat exchanger for the prills, a conveying device, in particular a vibratory conveying element and a bucket elevator for the prills to a prillsilo and a Steuer imaginary.
  • Control device with at least one sensor for detecting at least one of the following measured values such as for the temperature, the volume and the flow velocities of the medium or the air and / or the prills.
  • the granules produced by spraying molten masses become small
  • Called pearls or prills To granulate a product from the melt, it is generally sprayed at the top of the solidification tower through a distributor formed as a showerhead, basket or rotating perforated plate. In these devices, the droplets of more or less equal size fall into the tower in which they are cooled by equal or countercurrent air and solidify into prills, which are collected at the foot of the tower and then cooled.
  • EP1243316A2 discloses a pelletizer for petroleum residues which are subjected to a prilling process in the molten state.
  • a prilling head with outlet openings rotating about a vertical axis, over which the molten material is thrown radially outward, is used.
  • the prilling head is disposed within an upright container. The spherical particles fall down and get into a located at the bottom of the container water bath. There is a cooling of the solidified pellets before they are removed from the container in a row.
  • US2714224A1 discloses a device for granulating chemical substances, in particular fertilizers.
  • a molten substance is introduced into a screening device or vibrating device.
  • Individual drops fall by gravity through the sieve in a container down and solidify during their fall.
  • the particles collect and are withdrawn.
  • cooling air is conveyed through the container in countercurrent to the falling particles.
  • DE 2409695 describes a method and an apparatus for granulating meltable substances or highly concentrated substances, in particular the production of granules of virtually the same particle size as fertilizers or sodium hydroxide and potassium hydroxide. Disadvantages of this method according to DE 2409695: no uniform Prill formation, no constant temperature distribution in the solidification tower, no simple cleaning and poor recovery of the process in the specification not compliant prills.
  • the object of the invention is thus to achieve a device and a method with uniform Prill Struktur, with a constant temperature distribution in the solidification tower, a simple cleaning of the solidification tower and a good recovery of the prills not according to the specification.
  • the object is achieved by a method of the type mentioned according to the invention by the following steps by the molten substance is introduced into a spray system with a pot-shaped spray head rotating about a vertical axis, while the spray basket rotates about the longitudinal axis and the droplets through openings in the mantle Sprühkorbes be discharged in the radial direction and fall between the shell of the spray basket and the inner wall of the solidification tower in the direction of the bottom outlet of the solidification tower and the rotational speed of the spray basket and the flow rate of the gaseous cooling medium is limited upwards such that the trajectories of at least a plurality of Droplets or prills within a Run imaginary cylindrical shell sheath whose diameter is slightly smaller than the diameter of the inner shell.
  • the invention also enables production of KOH prills having a uniform shape and structure. This is also supported by a constant and uniform cooling of the falling out of the spray prills in the counterflow or in DC with the fall direction. Also, in this production process, the non-specification prills are recycled by diluting the dissolved prills with fresh water and returning the solutions completely to the production process.
  • the solidification tower is in the first cleaning step with "wash water", with
  • KOH / K 2 CO 3 contaminated is cleaned and rinsed in a second step with fresh water.
  • the wash water may contain a maximum of 40% by weight KOH / K 2 CO 3 .
  • the apertures are circular, oval, polygonal or slit-shaped, whereby the discharge of the drops to the desired volumes can be easily adapted.
  • the walls of the jacket of the rotating spray basket are produced with openings with an area of a minimum of 0.007 mm. This results in prills of the desired shape and size.
  • Breakthroughs are made with a maximum area of 3.2mm. This results in prills of the desired shape and size.
  • Spray basket between 0.007mm 2 and 4.53mm 2, preferably between 0.032mm 2 and 3.2mm. This not only prills desired size can be made, but also the solidification process is improved after leaving the spray head, since the preferred size of the apertures an optimal relationship between the surface chip tion and the other mass forces acting on the droplets, which leads to an optimally spherical shape of the resulting prills.
  • the rotational speed is controlled or regulated in such a way that, depending on the supplied mass of the melted substance, the diameter of the spray head and the discharged volume of the droplets in a predeterminable unit of time, an equilibrium between the mass of the molten substance and the mass of droplets is achieved.
  • an optimization of the production process is achieved and also solved in that the rotating spray has revolutions of a maximum of 1500 revolutions per minute. This also allows a uniform size and shape of the prills.
  • the trajectories of the majority of the droplets have a distance of at least 0.1 mm from the shell of the solidification tower. This prevents the prills from having their outer surface cooled at least below the solidification point, from coming into contact with the wall of the solidification tower, and thus from being unable to adhere or stick there. This additionally increases the duration of use of the Storming Storm as the number of washings can be reduced.
  • the outer diameter of the spray basket in the production of KOH prills from a starting material having a KOH concentration of greater than 85%, in particular with a KOH concentration between 90% and 95% in the production of KOH prills from a starting material having a KOH concentration of greater than 85%, in particular with a KOH concentration between 90% and 95%, the outer diameter of the spray basket in
  • Ratio to the inner diameter of the shell of the solidification tower between 1 to 20 to 1 to 50. It has been found that this measure is optimal for the solidification process of KOH droplets after leaving the spray basket and the properties of KOH, especially density and viscosity optimally takes into account.
  • KOH has a density between 1750 and 1850 kg / m and a viscosity between 2.5 and 3.5 mPa.s.
  • the area of the holes in the spray basket shell is between 0.007mm 2 and 3.2mm 2 and the spray basket speed is between 100 and 1000 revolutions / minute.
  • Sprühkorbes device via a drive steplessly regulated by means of a control device.
  • a rapid readjustment can take place with changing temperatures of the etching crystal, so that the volume of the droplets ejected by the spray basket can be maintained with relatively small tolerances over a longer service life.
  • the speed of the spray basket is controlled or regulated as a function of the supplied mass of the molten substance and / or the viscosity of this mass. This produces prills of uniform shape and size.
  • a rapid adjustment of the volume of the droplets dispensed can also be promoted by the fact that with a change in the viscosity of the molten substance, the speed of the spray basket is changed in the same direction.
  • the speed of the spray basket is changed in the same direction.
  • the size and shape of the prills can be kept stable.
  • an air duct is carried out in cocurrent with the direction of fall of the prills in the solidification tower controlled and uniform cooling of the falling prills.
  • a control and regulation of the amount or temperature of the gaseous medium preferably formed by air in the guide in countercurrent to the direction of movement of the prills in the solidification tower, depending on the temperature of the medium or the air in the region of the medium outlet is regulated by at increasing temperature increases the amount of the supplied medium or the air and / or its temperature is reduced. This results in a controlled and uniform cooling of the falling prills.
  • the prills are precipitated with size and / or shape and / or weight deviating from the product specification and / or melting with high proportions of nickel or nickel oxide formed during the prill production process. This results in prills with high purity. It is also advantageous if the excreted prills dissolved, processed, possibly cleaned and again be introduced as ⁇ tzkali in the production process. As a result, material that has been lost during the production process, can be used again.
  • an advantageous procedure of the method can also be achieved if the lye-contacting parts of the spray basket, the deflection point and the collecting container are overlaid with nitrogen to contact with oxygen and prills adhering to the surface is not sufficiently cooled are to be avoided.
  • the nitrogen addition may be continuous or periodic to avoid contact with oxygen.
  • a procedure in which the solidification is stormy subjected to a cleaning and the wash water is pumped from the wash water tank in the upper part of the same solidification tower and the funnel-shaped outlet and the walls of the solidification tower with wash water and then washed with fresh water.
  • the washing water is treated again and can then be used again in the washing water circuit.
  • the fresh water There is a high degree of utilization of the washing water and the fresh water and thus a lower water consumption than in conventional systems.
  • wash water up to a concentration of less than or equal to 40% KOH / K 2 CO 3 is used for rinsing and is regenerated again in order to be used again for rinsing.
  • a long service life of the system can be conveniently achieved by the sprayer and the spray head are removed for cleaning from the solidification tower, heated for several hours in a steam bath at a maximum of 200 ° C and then preheated to a maximum of 400 ° C and the spray and the During the washing process, outside the solidification implosion, the second, already heated, spray basket is installed in the place of the soiling, in order to take the solidification tower out of operation for as short a time as possible.
  • a further method step is advantageous after the inner surface of the funnel-shaped outlet of the solidification storm is heated by an electrical heat tracing. This prevents the caking of hot prills on the inner surface and thus the clogging of the outlet funnel.
  • the inner surface of the outlet hopper it is also advantageous if the inner surface of the outlet hopper to a maximum temperature of 180 ° C, preferably to a maximum temperature of 100 ° C, heated. This prevents the caking of hot prills on the inner surface and thus the clogging of the outlet funnel.
  • a feeder line for the molten material in a spray system opens, which has a cup-shaped spray head, which has a substantially cylindrical spray with a vertical longitudinal axis comprises and the spray head is rotatably mounted about a longitudinal axis parallel to the axis of rotation and connected to a rotary drive and the jacket of the spray basket is formed with a plurality of distributed over the surface openings for discharging droplets of the molten substance in the radial direction.
  • openings in the spray basket are circular, oval, polygonal or slot-shaped is advantageous, as a result of which prills with different shapes can be produced.
  • the openings in the jacket of the rotating spray basket are formed with a maximum area of 0.007 mm - 3.2 mm. This results in prills of the desired shape and size.
  • the outer diameter of the spray basket in relation to the inner diameter of the shell of the solidification tower between is 1 to 20 to 1 to 200.
  • FIG. 1 shows a process diagram of a plant for the production of KOH prills in a highly simplified, schematic representation
  • Fig. 2 is a greatly simplified and schematic circuit diagram of the control and regulating device of the system of Fig. 1;
  • FIG. 3 shows a spray head of the system shown in Figure 1 in side view with the associated drive system in a highly simplified, schematic representation ..;
  • Fig. 4 is a spray basket of the spray head shown in Figure 2 on a larger scale partially cut with arranged in a part of the cylindrical shell of the spray basket openings.
  • FIG. 5 shows a process diagram of a plant for the production of KOH prills in a highly simplified, schematic representation.
  • the indication 1 to 10 should be understood to include all sub-ranges, starting from the lower limit 1 and the upper limit 10, i. all subregions begin with a lower limit of 1 or greater and end at an upper limit of 10 or less, e.g. 1 to 1.7, or 3.2 to 8.1 or 5.5 to 10.
  • FIG. 1 shows an optionally independent embodiment of the process for obtaining KOH prills, wherein the same reference numerals or component designations are again used for the same parts as in all figures. To avoid unnecessary repetition in subsequent drawings, reference is made to the detailed description in the preceding figures.
  • FIG. 1 shows a plant 1 with which KOH prills 2 are produced from concentrated caustic potash.
  • the liquid ⁇ tzkali 3 is supplied via a line 4 and a deflection point 5 and a subsequent line 6 to a collecting container 7.
  • a heat exchanger 8 with which the caustic potash is heated to a temperature of less than or equal to 400.degree.
  • the heat exchanger via the schematically indicated lines with a hot medium, for example steam, heated.
  • a line from below e.g. from the height of the foot of the freezing tower, to lead upwards.
  • the promotion of the meltable substance 3 to the upper part of the tower takes over in this case arranged in this line pump, which also ensures a continuous and controllable supply of the starting material for the prilling process.
  • the line coming from below could pass directly into the line 9 shown in FIG. 1, omitting a collecting container 7 or opening into it.
  • the heated caustic potash 3 is then fed via a line 9 into a spray basket 10 of a spray head 12 arranged within a solidification tower 11.
  • this spray head which can be set into rotation via a drive device, for example an electric motor, will be explained below with reference to FIG. 2.
  • the drops of the concentrated caustic potash discharged via the spray head are cooled in the interior of the solidification tower 11, in which at least the outer surface is cooled below the solidification temperature of the liquid caustic potash and so-called spherical, in particular spherical, KOH prills 2 are formed.
  • the cooling of the drops to form the KOH prills 2 takes place in the present exemplary embodiment by air in the conveying device 13, for example a blower or a compressor for a gaseous medium, preferably air, in the top-side, upper region of the solidification tower 11 via a line 14 is supplied, flows through them the solidification storms 11 in the vertical direction and in the direction of a bottom outlet.
  • the airflow is used to cool the prills 2.
  • the gaseous medium is sucked by means of negative pressure through the solidification storm 11.
  • a fan 55 generates in a vacuum container 54 a preferably controllable negative pressure.
  • Via line 53 gaseous medium from the solidification tower 11 is sucked.
  • a cooling flow is likewise produced parallel to the direction of the falling prills 2.
  • the prills 2 solidified at least in the region of the outer surface are fed to a conveying device, in particular a conveyor belt 17, via a line 16 which adjoins the bottom-side outlet 15 of the solidification storm 11. From this they are transported to a heat exchanger 18 and further cooled in this during transport.
  • the heat exchanger 18 can be flowed through the lines 19, for example, with a gaseous or liquid cooling medium.
  • the prills 2 are cooled to a maximum temperature of 80 ° C., preferably to a maximum temperature of 70 ° C., and fed via a subsequent vibratory conveying element 20 to a conveying device 21, for example a cup conveyor, with which the prills be deposited in a prillsilo 22.
  • a heating device 23 is arranged, for example, the particular funnel-shaped outlet 15 to a temperature between 50 ° C and 180 ° C, preferably between 50 ° C and 150 ° C, particularly preferred not more than 150 ° C, most preferably at most 100 ° C, heated or held at this temperature.
  • the caustic potash 3 and the prills 2 are very hygroscopic, it is advantageous if the entire plant 1, in particular those lines and spaces in which the caustic potash 3 and the prills 2 are produced, cooled, conveyed and deposited with dry gas, especially dry air, or even a noble gas are superimposed.
  • a washing water tank 24 is furthermore arranged.
  • This wash water tank 24 is connected to the bottom outlet 15 of the solidification tower 11 via a connecting line 25 and, on the other hand, wash water is supplied via this connecting line via a feed pump 26 into the cover-side inlet of the solidification tower 11.
  • a control or regulating device 28 is shown schematically, which can be connected to additional memories 29 and other computers and data measurement displays and receivers.
  • the control or regulating device 28 is, for example via a line 30 with a sensor 32 for measuring the
  • a sensor 34 preferably for measuring the flow rate of the cooling medium inside the solidification tower 11, in particular the flow velocity of the air
  • a line 30 with a sensor 32 for measuring the temperature at least the surface temperature of the prills 2, for example via a non-contact infrared scanner or the like.
  • additional sensors 35, 37, and 38 may be connected to the controller 28 via conduits 33 and 39.
  • All lines which are connected to the control or regulation device 28, regardless of whether these are lines to the sensors, 32, 34 to 38 or lines to the drives of the spray head 12 of the conveyor of the conveyor belt 17 of the vibratory conveyor 20 or conveying device 21 can also be formed by bus lines or a bus system, as is known from the prior art for such control devices 28 for the control expert working in this field.
  • FIG. 2 again shows the circuit diagram of the control and regulating device 28 with the associated sensor 28 for detecting the air temperature for cooling the spherical prills, the sensor Sor 32 for detecting the volume and the flow rate of the air, the sensor 32 for determining the temperature of the prills 2 in the funnel-shaped outlet 9 of the solidification tower shown.
  • the temperatures are determined by means of thermography, ie the temperature measurement of the prills 2 is detected contactless preferably areally and displayed on the basis of the temperature determination with heat-sensitive sensors 34 to 38.
  • the data are then eg in a microprocessor 28, the central control and regulating device 28th in which all components of a processor are combined on a microchip, collected, and evaluated by the processor unit and can alternatively be provided in the memory 29 for evaluation.
  • Fig. 3 the spray head 12 and the associated drive motor 40 is shown on a larger scale.
  • the drive motor 40 is connected via a coupling and a drive shaft 41 to the spray basket 10, so that it can be rotated about the longitudinal axis 42, which is preferably also identical to the longitudinal axis of the drive shaft 41 in rotation.
  • the spray basket 10 is schematically indicated here in dotted lines.
  • supply lines or feed devices 43, 44 are provided.
  • the melted ⁇ tzkali 3 is supplied through the line or feeding device 43 so that it can enter via an outlet 45 into the interior of the spray basket 10.
  • Nitrogen can be supplied to the interior of the spray basket 10 via the outlet 46 via the feed line or feed device 44).
  • the spray basket 10 shown in Fig. 4 on a larger scale is rotatably connected to the drive shaft 41 and thus rotates about the longitudinal axis 42.
  • the cylindrical shell of the spray basket 10 is provided with a distributed over this coat plurality of openings 47, of which only a few examples Fig. 4 are shown provided.
  • the passage cross section of these apertures 47 is dimensioned such that depending on the speed of the spray basket 10 and the mass of the supplied, molten ⁇ tzkali 3 drops can pass with a predeterminable volume through the openings 47 of a cylindrical shell 48 of the spray basket 10.
  • apertures 47 of the jacket 48 of the spray basket 10 with different shapes are exemplified, such as elliptical openings 49, round openings 50 and angular openings 51.
  • the KOH prills process is divided into four steps - Preparation of KOH prills - Treatment of KOH prills - Cleaning of the solidification tower - Re-provision of non-compliant prills to obtain KOH prills.
  • liquid caustic potash 3 is concentrated (less than or equal to 95% by weight) via the lines 4 and 6 to a deflection point 5 having a temperature of less than or equal to 400 ° C. into the collecting container 7 and from there via the line 9 into the rotating spray basket 10 with the spray head 12 which storm in the solidification 11 is arranged.
  • the caustic potash flows through the dead weight through the deflection point 5 into the collecting container 7.
  • the openings 47 in the jacket or the side walls of the spray basket 5 have a diameter or cross-section of at most 1 mm and is discharged through the forces exerted on the ⁇ tzkali by the rotation of the spray basket 10 centrifugal drops through the apertures 47 into the solidification tower 11.
  • the openings 47 in the walls of the jacket 48 of the rotating spray basket can be made with an area of 0.007 mm 2 - 3.2 mm 2.
  • the rotational speed of the spray basket 10 is controlled in dependence of the supplied mass of ⁇ tzkali 3, the diameter of the spray head 12 and the volume of the resulting droplets in a predetermined unit of time.
  • the rotational speed of the spray head 12 is between 200 to 1500 revolutions / minute and the speed of the
  • Sprühkorbes 10 can be steplessly controlled by a drive device by means of a control device but the speed of the spray 10 can also be determined in addition to or instead of the mass of the supplied ⁇ tzkali 3 and / or the viscosity of ⁇ tzkali 3.
  • the rotational speed of the spray head 12 or of the spray basket 10 is designed as a function of the abovementioned physical values of the medium or the rotational speed and the like such that the trajectory of the individual drops is at a distance from the inner wall of the jacket of the solidification tower 11 and at least have a distance of 0.1 mm from the inner wall of the solidification tower.
  • Drops of ⁇ tzkali are ejected by the rotation of the spray basket 10 through the openings 47 from the spray 10.
  • the discharged drops 2 are cooled with a gas stream, in particular ambient air or with noble gases in the solidification tower, crystallize while they fall in the solidification tower down. They are through the funnel-shaped end of the spray tower, which is provided with a heater 23, at a temperature between 50 ° C - 180 ° C, preferably between 110 ° C - 180 ° C, discharged.
  • the cooling air or the gas can be conducted in cocurrent with the falling prills 2. But it can also be a cooling and crystallization of the prills 2 with gas or air, which runs in countercurrent, take place.
  • the prills 2 fall from the solidification storm 11 via the line 16 on a conveyor belt 17 and are transported to the heat exchanger 18.
  • the heated after cooling the prills 2 air is removed via a ring collector which is connected to an exhaust fan on the scrubbing tower from the solidification tower 11. Due to the air supply and removal, a constant temperature, which as such may also vary. can be generated in the stagnation storm. As a result, unwanted water absorption from the resulting prills can be avoided.
  • the used air is washed and returned to the atmosphere. The wash water is discharged into the wash water tank 24 via an overflow.
  • Is used as a cooling medium for the spherical prills 2 ordinary ambient air it is fed into the solidification tower, then, after the air has left the solidification tower, washed and filtered and discharged back into the environment.
  • the cooling and crystallization of the prills with the aid of air or another gaseous medium can also be carried out in a closed system in which the air or gaseous medium is cleaned and circulated.
  • spherical prills 2 it is also premature to adjust the ratio of the outer diameter of the spray basket to the inner diameter of the jacket. Preferably good results can be obtained if the ratio 1 to 20 to 1 to 200 is set.
  • the mass and viscosity of the caustic potash 3 relative to the speed of the spray basket, i. If the mass or the viscosity is increased, it is advantageous to increase the speed of the spray basket 10. If the mass or viscosity drops, it is advantageous to reduce the speed of the spray basket.
  • KOH prills from a starting material with a KOH concentration of greater than 85%, in particular with a KOH concentration between 90% and 95%, preferably the area of the openings in the shell of the spray between
  • KOH prills from a starting material having a KOH concentration of greater than 85%, in particular having a KOH concentration between 90% and 95%
  • the following process parameters are used: At temperatures between 200 and 350 ° C and at concentrations between 90% and 95% KOH has a density between 1750 and 1850 kg / m3 and a viscosity between 2.5 and 3.5 mPa.s. In addition to these conditions, the area of the
  • Breakthroughs in the shell of the spray basket (hole size) between 0.007mm 2 and 3.2mm 2 and the spray basket speed is between 100 and 1000 revolutions / minute.
  • KOH prills can be made that will cool quickly and become firm and stable.
  • the prills are cooled in a rotating cylinder to a temperature of less than or equal to 80 ° C., preferably less than or equal to 50 ° C.
  • the prills are conveyed via a vibrating conveyor 20 and a conveyor 21 in the prill silo 22.
  • the caustic potash also introduces interfering nickel residues into the solidification tower, but especially into the spray basket 10, which block the openings 47 of the spray basket 10.
  • two spray baskets 10 are used - that is, the spray basket, which has been soiled with nickel, is manually replaced with a clean spray basket, cleaned and can then be used again cleanly.
  • the sprayer it is brought out with the spray head from the solidification storm, disassembled from the spray head, heated for several hours in a steam bath at 200 ° C, then preheated to a maximum of 400 ° C and the spray basket 10 is mounted again at the next cleaning process to the spray head in which the second spray basket has just been dismantled and introduced into the solidification tower 11. So only the sprayer must be exchanged, while the spray head is only briefly disconnected from the production process.
  • the cleaning process is carried out according to a defined degree of contamination.
  • the cleaning process can also be carried out periodically.
  • washing water is pumped out of the washing water tank 24 by means of the pump 26 in the upper part of the solidification tower 11, especially for cleaning the solidification tower 11.
  • the funnel-shaped outlet with the heating device 23 and the walls of the solidification tower are washed with washing water and then with cold water.
  • the wash water is used to a concentration of less than or equal to 40% KOH / K 2 CO 3 and then subjected to a neutralization reaction.
  • the heat exchanger 18 is also cleaned with washing water, the washing water collected and pumped into the washing water tank 24.
  • Spray head 51 Square openings

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Glanulating (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Automation & Control Theory (AREA)
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Abstract

L'invention concerne un procédé de granulation de matières fusibles, servant à produire des prills sphériques (2) à partir de la matière (3) en fusion. La matière (3) en fusion est introduite dans un système de pulvérisation comprenant une tête de pulvérisation (12) en forme de pot tournant sur un axe vertical, tandis qu'un panier de pulvérisation (10) tourne sur l'axe longitudinal et éjecte les gouttelettes dans le sens radial à travers des perçages de l'enveloppe du panier de pulvérisation (10). Les gouttelettes tombent entre l'enveloppe du panier de pulvérisation (10) et la paroi intérieure d'une tour de solidification (11) en direction de la sortie côté fond de la tour (11). Les prills (2) sont transportés par un milieu réfrigérant gazeux qui parcourt la tour de solidification (11) dans le sens longitudinal, ce qui a pour effet de refroidir la surface extérieure des prills (2) à une température inférieure ou égale à la température de solidification. La vitesse de rotation du panier de pulvérisation (10) et la vitesse d'écoulement du milieu réfrigérant gazeux sont limitées vers le haut de telle façon que les trajectoires de vol d'au moins une pluralité des gouttelettes ou des prills (2) se situent à l'intérieur d'une enveloppe cylindrique imaginaire dont le diamètre est à peine inférieur à celui de l'enveloppe intérieure de la tour de solidification (11). Les prills (2) sont refroidis encore plus dans un échangeur thermique (18).
PCT/EP2013/072366 2012-10-25 2013-10-25 Procédé de granulation de matières fusibles WO2014064239A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201380067825.9A CN104884154B (zh) 2012-10-25 2013-10-25 用于将可熔物质造粒的方法
KR1020157013478A KR20150081297A (ko) 2012-10-25 2013-10-25 용융성 물질의 입상화 방법

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ATA1161/2012A AT513566B1 (de) 2012-10-25 2012-10-25 Verfahren zum Granulieren von schmelzbaren Stoffen
ATA1161/2012 2012-10-25

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CN115155455A (zh) * 2022-07-05 2022-10-11 山西东锦肥业有限公司 一种防止硝酸镁颗粒挂壁的装置

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US11046631B2 (en) * 2017-02-21 2021-06-29 Rhodia Operations Diphenol and phenol prills and method for obtaining the same
CN107520992A (zh) * 2017-08-23 2017-12-29 黎明化工研究设计院有限责任公司 一种高分子量星型聚氧化乙烯醚造粒工艺及其设备
CN111220443B (zh) * 2020-03-18 2023-03-21 上海理工大学 一种弱接触试样浓缩提纯方法及应用
CN114073915A (zh) * 2020-08-21 2022-02-22 博特化工装置股份公司 用于生产碱金属氢氧化物颗粒的装置
CN114073914A (zh) * 2020-08-21 2022-02-22 博特化工装置股份公司 粒化装置

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EP1243316A2 (fr) * 2001-03-22 2002-09-25 Kellogg Brown & Root, Inc. Buse de pulvérisation pour granulateur
US20030037459A1 (en) * 1999-05-03 2003-02-27 Acusphere, Inc. Spray drying apparatus and methods of use

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DE2409695A1 (de) * 1973-03-02 1974-09-12 Roger Max Kaltenbach Verfahren zum granulieren von schmelzbaren stoffen
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US20030037459A1 (en) * 1999-05-03 2003-02-27 Acusphere, Inc. Spray drying apparatus and methods of use
EP1243316A2 (fr) * 2001-03-22 2002-09-25 Kellogg Brown & Root, Inc. Buse de pulvérisation pour granulateur

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115155455A (zh) * 2022-07-05 2022-10-11 山西东锦肥业有限公司 一种防止硝酸镁颗粒挂壁的装置
CN115155455B (zh) * 2022-07-05 2024-04-26 山西东锦肥业有限公司 一种防止硝酸镁颗粒挂壁的装置

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AT513566A1 (de) 2014-05-15
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AT513566B1 (de) 2015-04-15
CN104884154A (zh) 2015-09-02

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