WO2021104917A1 - Processus pour éliminer l'eau d'un matériau particulaire humide - Google Patents

Processus pour éliminer l'eau d'un matériau particulaire humide Download PDF

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Publication number
WO2021104917A1
WO2021104917A1 PCT/EP2020/082274 EP2020082274W WO2021104917A1 WO 2021104917 A1 WO2021104917 A1 WO 2021104917A1 EP 2020082274 W EP2020082274 W EP 2020082274W WO 2021104917 A1 WO2021104917 A1 WO 2021104917A1
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Prior art keywords
rotary drum
drum reactor
wall
process according
reactor
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PCT/EP2020/082274
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English (en)
Inventor
Lothar Seidemann
Frank Kleine Jaeger
Johannes Felix HAUS
Matthias Rauls
Fatih CETINEL
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Basf Se
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Publication of WO2021104917A1 publication Critical patent/WO2021104917A1/fr

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    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/28—Moving reactors, e.g. rotary drums
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/0077—Baffles attached to the reactor wall inclined
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • B01J2219/0218—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of ceramic
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • B01J2219/0236—Metal based
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0869—Feeding or evacuating the reactor
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0892—Materials to be treated involving catalytically active material
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12—Processes employing electromagnetic waves
    • B01J2219/1203—Incoherent waves
    • B01J2219/1206—Microwaves
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18—Details relating to the spatial orientation of the reactor
    • B01J2219/187—Details relating to the spatial orientation of the reactor inclined at an angle to the horizontal or to the vertical plane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention is directed towards a process for removing water from a wet particulate material, said process comprising the step of introducing at least one particulate material with a residual moisture in the range of from 0.5 to 25 % by weight into a rotary drum reactor and mov ing it through the rotary drum reactor together with a flow of a gas, wherein said rotary drum re actor contains of the following elements:
  • reaction time is an average time. Both shortcuts and extremely long residence times of groups of particles need to be avoided due to incomplete reaction and undesired agglomeration of secondary particles, respectively.
  • a sparingly soluble compound of the transi tion metal(s) is made by precipitating it from a solution, for example a carbonate or a hydroxide.
  • This sparingly soluble salt is in many cases also referred to as a precursor.
  • Such precursors are expected to meet tight specifications with regard to their particle size distribution and internal physical structure, characterized by e.g. their degree of sphericity or specific surface area (BET surface).
  • said precursor is mixed with a lithium compound, for example U2CO3, LiOH or U2O, and calcined at high temperatures, for example at 600 to 1100°C.
  • a lithium compound for example U2CO3, LiOH or U2O
  • Water removal thus is crucial between the two stages.
  • a homogeneous precursor both in composition including water content, and morphology including particle size distribution is highly desired.
  • the precursor is separated from the mother liquor by solid- liquid separation methods, especially by filtration.
  • the resulting filter cake may contain up to 25% by weight of water.
  • inventive process is a continuous process.
  • the inventive process is performed at a temperature in the range of from 100 to 500°C, preferred are 150 to 450°C.
  • the temperature in this context refers to the highest temperature as measured in a distance of 1 cm to the inner wall. It is even more preferred to have a temperature profile, for example drying in a range of from 100 to 200°C and a pre-calci nation with a maximum temperature of up to 500°C, preferably up to 450°C.
  • Rotary drum reactors in the con text of the present invention are vessels that rotate along a longitudinal axis that may be hori zontal or tilted by 0.1 to 15 degrees and that have a length to diameter ratio in the range of from 0.1 to 20, preferably from 0.5 to 20.
  • rotary drum reactors may have a length in the range of from 1 to 20 meters, preferably 4 to 10 meters.
  • top and bottom phase of rotary drum reactors are preferably spherical.
  • rotary drum reactors in the context of the present invention are cylindrically shaped, preferably as right cylinders.
  • the rotary drum reactor is operated with 0.01 to 20 rounds per minute, preferred are 1 to 10 rounds per minute, and, in each case, continuously or in intervals.
  • operation in an interval mode it is possible, for example, to stop the rotation after one to 5 rounds for one to 60 minutes, and then to again perform 1 to 5 rounds and again stop for 1 to 60 minutes, and so forth.
  • the inventive process comprises the step of introducing a wet particulate solid into the rotary drum reactor and moving it through said rotary drum reactor with a flow of gas.
  • the flow of gas may be co-current or preferably counter-current.
  • the gas flow comprises air that is co-current or countercurrent with respect to the particulate solid, preference being given to countercurrent.
  • the particulate solid introduced in the inventive process is wet.
  • the wet particulate solid has a moisture content in the range of from 0.5 to 25% by weight. Its solids content is thus in the range of from 75 to 99.5% by weight.
  • the moisture content may be determined by drying in vacuo at a temperature of 100°C until the weight is remaining unchanged.
  • the wet particulate solid is provided as a filter cake.
  • Said particulate solid may have an average diameter (d50) in the range of from 1 pm to 1 mm, preferably 2 pm to 100 pm.
  • Said particulate solid may have an irregular shape but in a preferred embodiment, said particulate solid has a regular shape, for example spheroidal or even spheri cal.
  • the aspect ratio may be in the range of from 1 and 10, preferably from 1 to 3 and even more preferably from 1 to 1.1.
  • the wet particulate solid is provided as a fil ter cake from a precipitation or preferably co-precipitation of a precursor for cathode active ma terials for lithium ion batteries.
  • said particulate solid preferably has an av erage particle diameter (d50) in the range of from 2 to 20 pm and even more preferably from 3 to 15 pm.
  • the wet particulate solid may be provided as a filter cake from a precipi tation of nickel hydroxide or cobalt hydroxide.
  • precursors for cathode active materials for lithium ion batteries are mixed hydrox ides and mixed carbonate of transition metals, especially of nickel and at least one metal se lected from manganese and cobalt. Further metals may be present in the precursor such as, but not limited to Mg, Ca, Al, Ba, B, Ti, Zr, Nb, Ta, W, Mo, and Y. In such embodiments, the stoichiometry of the transition metals in the precursor corresponds to the stoichiometry of the transition metals in the targeted cathode active material.
  • the average residence time of the particulate solid is in the range of from 10 minutes to 12 hours, preferably 1 to 6 hours.
  • the aver age residence time refers to the average residence time of the particulate material in the rotary drum reactor.
  • the wet particulate solid is introduced into the ro tary drum reactor at ambient temperature. In another embodiment of the present invention, the wet particulate solid is introduced into the rotary drum reactor at a temperature of from 10°C to 100°C.
  • the wet particulate solid is moved through the rotary drum reactor. Upon moving wet particulate solid the moisture content decreases. Preferably, at the end of the inventive process the resid ual moisture content is in the range of from 10 ppm to 10,000 ppm, preferably 100 to 300 ppm by weight.
  • said particulate solid is moved through the rotary drum reactor with a co-current flow of gas.
  • said flow of gas and said particulate solid are moved through the rotary drum reactor counter-cur- rently.
  • the co-current flow has the disadvantage that the almost finished precursor is in contact with gas comparably rich in humidity and carbon dioxide. This disadvantage is avoided if flow of gas and motion of particulate solid are counter-current.
  • said rotary drum reactor has an inlet and an outlet for said gas.
  • the gas temperature at the inlet to the reactor is in the range of from 10°C to 800°C, preferably from 20°C to 400°C.
  • the average superficial velocity of the gas is in the range of from 0.005 m/s to 1 m/s, preferably 0.05 m/s to 0.2 m/s. With a higher superficial gas velocity, dust evolution may exceed a tolerable level.
  • the gas may be inert or oxidizing, such as in the case of alkanols in the case of alde hyde formation.
  • the gas is oxidizing, for example pure oxygen, oxygen-enriched air or air, oxygen-enriched air and air being preferred.
  • oxygen-enriched air is a mix ture of 1:0.5 by volume to 1:5 by volume air : oxygen, determined at ambient conditions.
  • the inventive process is performed at ambient pressure or ⁇ 50 mbar, preferably ambient pressure up to 20 mbar above ambient pressure.
  • the filling level of said rotary drum reactor is in the range of from 5 to 80%, preferred are 20 to 65% and even more preferred from 20 to 50%.
  • the filling level is determined under neglecting the voids between particles of particulate solid.
  • the rotary drum reactor contains the following elements:
  • (A) a double-wall steel drum, hereinafter also referred to as steel drum (A) or element (A), wherein the space of the outer and the inner wall is evacuated,
  • heating system (B) with an electrical heating system attached to the inner wall, hereinafter also referred to as heating system (B) or element (B),
  • (D) optionally, a corrosion protection layer attached to the electric heating system, hereinaf ter also referred to as layer (D) or element (D), (E) and, optionally, at least one additional inlet that is located in the rotary drum reactor and through which an extra gas stream can be introduced into the rotary drum reactor.
  • Element (A) is a double-wall steel drum.
  • the dis tance between the outer and the inner wall is in the range of from 1 to 20 cm, preferably 5 to 10 cm, determined at ambient temperature. The distance is an average value.
  • Each wall may have a thickness in the range of from 5 to 30 mm, preferred between 7 and 20 mm.
  • the inner and the outer wall may have the same or different thicknesses.
  • the outer wall is 1.5 to 3 times thicker than the inner wall.
  • Outer and inner wall may be kept apart by spacers.
  • spacers may have a round or polygo nal shape.
  • the length of the spacers may be in the range of from 10 to 100 mm, preferred are 20 to 70 mm.
  • both outer and inner wall are from stainless steel.
  • the space between outer and inner wall may be filled with gas, e.g., air, or it may be evacuated. “Evacuated” in the context of the present invention shall not be restricted to vacuum but also in clude a reduced pressure, that the pressure in this space is in the range of from 1 to 100 mbar.
  • the residual gas may be selected from nitrogen or noble gasses such as argon. However, the residual gas may be selected from air or oxygen and thereby cause a passivation of the hot sur face of the inner wall of the drum.
  • the space between outer and inner wall may be empty or contain loose elements.
  • the space between outer and inner wall contains rock wool or porous stone.
  • the rotary drum reactor further comprises a heating system (B).
  • the heating system (B) is elec tric and attached to the inner wall of the rotary drum reactor, and it may be selected from heat ing selected from resistance heating, inductive heating, and micro-wave heating.
  • the heating system (B) is attached to the inner wall in a way that it reaches into the rotary drum reactor. It is preferred to protect it against corrosion with a corrosion protection layer (D) since otherwise it is exposed to the reaction good.
  • the heating system (B) covers the inner surface of the inner drum to the extent of 70 to 100% of the inner surface of the inner drum.
  • the heating system (B) is attached to the inner wall through bolts or screws.
  • the heating system (B) is drum shaped and has the same outer diameter as the inner diameter of the inner drum, upon heating and thermal expansion, the heating system is pressed to the wall of the drum due to the thermal expansion.
  • the region of rotary drum reactors that is exposed to the heating system is the reaction zone of such rotary drum reactor.
  • a corrosion protection layer (D) is attached to the heating system (B).
  • Said layer (D) may be made from a ceramic matrix composite or an alloy selected from steels and nickel-based alloys and cobalt refractory alloys, or a metal selected from tungsten, molybdenum, iron, and nickel.
  • a ceramic matrix composite contains ceramic fibers, and it additionally comprises a ceramic ma trix material.
  • the fibers are in an ordered or non-ordered orientation, for example 0 90° layup or randomly criss-cross.
  • Ceramic fibers and ceramic matrix material may have identical or differ ent chemical compositions.
  • ceramic matrix composites comprise fibers embedded in ceramic oxide or non-oxide matrices. The bonding forces between the fibers and the matrix are comparatively low.
  • Oxide matrix materials such as aluminum oxide are preferably in particulate form.
  • Ceramic fibers and ceramic matrix materials may each be selected from oxide and non-oxide ceramics.
  • non-oxide ceramics are carbides and borides and nitrides. Particular ex amples of non-oxide ceramics are silicon carbide, silicon boride, silicon nitride, silicon-boron- nitride, hereinafter also referred to as SiBN, silicon carbon nitride, hereinafter also referred to as SiCN, and in particular combinations from SiC and Si3N4.
  • oxide ceramics herein after also referred to as oxide-based ceramics.
  • Oxide ceramics are oxides of at least one ele ment selected from Be, Mg, Ca, Sr, Ba, rare earth metals, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Zn, B, Al, Ga, Si, Ge, Sn, Re, Ru, Os, Ir, In, Y, and mixtures of at least two of the foregoing.
  • Oxide-based ceramics may be selected from doped ceramics, wherein one main component is doped with up to 1 molar % components other than the main component, and from reinforced ceramics, wherein one component is the main component, for example at least 50 molar %, and one or more further components - reinforcing components - are present in ranges from 1.1 to 25 molar %.
  • Further examples are titanates and silicates. Titanates and silicates each may have a stoichiometric composition.
  • titanates is aluminum titanate.
  • silicates is magnesium silicate.
  • reinforced ceramics are reinforced alumina and reinforced zirconia. They may contain two or more different reinforcement oxides and may thus be referred to as binary or ternary mixtures.
  • the following binary and ternary mixtures are preferred: aluminum oxide reinforced with 1.1 to 25% by weight of one of the following: cerium oxide CeC> 2 , ytterbium oxide Yb 2 C> 3 , magnesia (MgO), calcium oxide (CaO), scandium oxide (SC 2 O 3 ), zirconia (ZrC> 2 ), yttrium oxide (Y 2 O 3 ), boron oxide (B 2 O 3 ), combinations from SiC and (AI 2 O 3 ), or aluminum titanate. More preferred reinforcing components are B 2 O 3 , ZrC> 2 and Y 2 O 3 .
  • Preferred zirconia-reinforced alumina is AI2O3 with from 10 to 20 mole-% ZrC>2.
  • Preferred examples of reinforced zirconia are selected from ZrC>2 reinforced with from 10 to 20 mole-% CaO, in particular 16 mole-%, from 10 to 20 mole-% MgO, preferably 16 mole-%, or from 5 to 10 mole-% Y2O3, preferably 8 mole-%, or from 1 to 5 mole-% Y2O3, preferably 4 mole-%.
  • An example of a preferred ternary mixture is 80 mole-% AI2O3, 18.4 mole-% Zr0 2 and 1.6 mole-% Y2O3.
  • Preferred fiber materials are oxide ceramic materials, carbide ceramic materials, nitride ceramic materials, SiBCN fibers, basalt, boron nitride, tungsten carbide, aluminum nitride, titania, barium titanate, lead zirconate-titanate and boron carbide. Even more preferred fiber materials are AI2O3, mullite, SiC, and Zr0 2 fibers.
  • the fibers are made from aluminum oxide
  • the ceramic matrix composite comprises a ceramic matrix material selected from aluminum oxide, quartz, mullite, cordier- ite and combinations of at least two of the foregoing. Preferred is aluminum oxide.
  • creep resistant fibers are fibers that exhibit minimum - or no - permanent elongation or other permanent deformation at temperatures up to 1,400°C
  • ceramic fibers may have a diameter in the range of from 7 to 12 pm. Their length may be in the range of from 1 mm up to 1 km or even longer, so- called endless fibers. In one embodiment, several fibers are combined with each other to yarns, rovings (German: Multifilamentgarn), textile strips, hoses, or the like.
  • ceramic fibers used in the present invention have a tensile strength of at least 50 MPa, preferably at least 70 MPa, more preferably at least 100 MPa, and even more preferably at least 120 MPa.
  • a maximum value of the tensile strength of ceramic fibers used in the present invention is 3,100 MPa or even 10,000 MPa.
  • the tensile strength may be determined with a tensile tester. Typical measuring conditions are cross-head speeds of 1.2 to 1.3 cm/min, for example 1.27 cm/min, and 7.61 cm gauge.
  • the matrix is made from an oxide ceramic material or a carbide.
  • Preferred oxide ceramic materials for the matrix are AI2O3, mullite, SiC, ZrC>2 and spinel, MgAhCU.
  • Particularly preferred components are SiC/SiC, Zr02/ZrC>2, ZrC AhCh, AhCh/ZrC ⁇ , AI2O3/AI2O3 and mullite/mullite.
  • the fiber material is in each foregoing case the first and the matrix the second material.
  • such ceramic matrix composite comprises 20 to 60 % by volume ceramic fiber.
  • Ceramic matric composites are porous. In many cases, the total solids content of such ceramic matrix composite is from 50 to 80% of the theoretical, the rest is air or gas due to the pores.
  • such ceramic matrix composite has a porosity in the range of from 20 % to 50 %; thus, such ceramic matrix composite is not gas tight in the sense of DIN 623-2.
  • the ceramic matrix composite comprises fibers from aluminum oxide and a ceramic selected from aluminum oxide, quartz, mullite, cordierite and combinations of at least two of the foregoing, for example aluminum oxide and mullite or aluminum oxide and cordierite. Even more preferably, the ceramic matrix composite comprises fibers from aluminum oxide and aluminum oxide ceramic.
  • layer (D) has a thickness in the range of from 0.5 mm to 15 mm, preferably 2 mm to 8 mm.
  • layer (D) covers the entire surface of element (B) that would be otherwise exposed to the reactants.
  • the surface of layer (D) in contact with the particu late solids inside the drum reactor is not evenly cylindrical but shaped, having circumferential, axial or otherwise oriented strips or a checked pattern or any other pattern.
  • the surface of layer (D) in contact with the particu late solids inside the drum reactor is coated, for example with a ceramic coating.
  • the coating of layer (D) may have a barrier function or an abrasion protection function, or both functions, and it is exposed to the precursor.
  • Rotary drum reactors further contain one or more elements (C), for example 2 to 3.
  • Such inter nals) (C) are attached to the inner wall, or to the front and end surfaces of a non-rotating part of said rotating drum reactor. They then reach into the drum reactor. Preferably, they are attached to the inner wall.
  • Internal(s) (C) may be selected from baffles, plough shares, blades or shovels. Internals (C) may expand entirely from the wall to the center of the rotary drum or they may expand partially from the wall to center of the rotating drum. Preferably, from 1 to 10 internals (C) are distributed along the axis of the rotating drum and from 1 to 10 internals (C) are distributed along the cir cumference of the rotating drum. In total, from 2 to 100 internals (C) may be distributed inside the rotating drum, preferably, and preferably from 4 to 20 internals (C) may be distributed inside the rotating drum in a symmetric orientation.
  • the length of the drum is from 0.5 to 20 m, prefera bly from 1 to 10 m.
  • the diameter of the drum is in the range of from 0.25 to 5 m.
  • the rotating drum reactor comprises
  • (E) at least one additional inlet that is located in the rotary drum reactor and through which an extra gas stream can be introduced into the rotary drum reactor.
  • Said inlet (E) may com prise a nozzle.
  • the pressure of the gas stream is between 0,5 and 50 bar, most preferably between 1 and 10 bar, in order to enhance the required break-up of filter cake for more efficient drying.
  • a reduction of the diameter or a nozzle at the tip of the inlet pipe can be provided to increase the gas velocity for a further improvement of the deagglomeration function.
  • the composition of the gas stream of inlet (E) may be the same as the gas composition of the main gas flow, but it can be of any other composition in case of the required pressure of the ad ditional inlet is above of the pressure of the main gas stream.
  • Said inlet (E) may be located upstream or downstream in inventive reactors, upstream being preferred.
  • inlet (E) the gas stream is accelerated in order to disperse the wet particu late solid fed which may contain lumps or agglomerates, into the rotary drum reactor.
  • a further aspect of the present invention relates to rotary drum reactors in which the inventive process may be advantageously performed.
  • Such rotary drum reactors are also referred to as inventive rotary drum reactors.
  • inventive rotary drum reactors contain the following elements, hereinafter also referred to as elements (A) to (E):
  • (E) at least one inlet that is located downstream in the rotary drum reactor and through which an extra gas stream can be introduced into the rotary drum reactor.
  • At least some of the internals (C) serve as scrapers by removing incrustations of, e.g., sintered particulate solids from the inner walls.
  • Such internals (C) that serve as scrapers are preferably those that are at the end of the reaction zone of an in ventive rotary drum reactor.
  • inventive rotary drum reactors may further comprise elements such as gaskets, an entry system for introduction of wet particulate solid and a removal system for reacted particulate solid.
  • the gaskets support the axis.
  • Figure 1 shows an example of an inventive reactor.
  • Example of an inventive drum reactor Flow of gas and motion of particles are co-current.
  • the 4 pairs of internals move the particles in the course of the rotation of the rotary drum reac tor.
  • M motor to effect the rotation of the drum.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente invention concerne un processus pour éliminer l'eau d'un matériau particulaire humide, ledit processus comprenant l'étape consistant à introduire au moins un matériau particulaire avec une humidité résiduelle dans la plage de 0,5 à 25 % en poids dans un réacteur à tambour rotatif et au déplacer à travers le réacteur à tambour rotatif conjointement avec un écoulement d'un gaz, ledit réacteur à tambour rotatif contenant les éléments suivants : (A) un tambour en acier à double paroi, (B) avec un système de chauffage électrique fixé à la paroi interne, (C) un ou plusieurs internes fixés à la paroi interne, ou aux surfaces avant et d'extrémité d'une partie non rotative dudit tambour rotatif, (D) et, éventuellement, une couche de protection contre la corrosion fixée au système de chauffage électrique.
PCT/EP2020/082274 2019-11-25 2020-11-16 Processus pour éliminer l'eau d'un matériau particulaire humide WO2021104917A1 (fr)

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EP19211196 2019-11-25
EP19211196.1 2019-11-25

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WO2021104917A1 true WO2021104917A1 (fr) 2021-06-03

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4717338A (en) * 1985-04-12 1988-01-05 Cellier S.A. Heater drum for manufacturing process
US20120319037A1 (en) * 2011-01-21 2012-12-20 Jx Nippon Mining & Metals Corporation Method For Producing Positive Electrode Active Material For Lithium Ion Battery And Positive Electrode Active Material For Lithium Ion Battery
US20190062224A1 (en) * 2015-10-14 2019-02-28 Basf Se Heat-permeable tube containing composite fiber ceramic
WO2019057536A1 (fr) * 2017-09-20 2019-03-28 Basf Se Procédé de fabrication de matériau actif d'electrode
CN109654831A (zh) * 2018-11-29 2019-04-19 安徽五亩生态农业发展有限公司 一种便于操作的茶叶干燥筛选装置

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4717338A (en) * 1985-04-12 1988-01-05 Cellier S.A. Heater drum for manufacturing process
US20120319037A1 (en) * 2011-01-21 2012-12-20 Jx Nippon Mining & Metals Corporation Method For Producing Positive Electrode Active Material For Lithium Ion Battery And Positive Electrode Active Material For Lithium Ion Battery
US20190062224A1 (en) * 2015-10-14 2019-02-28 Basf Se Heat-permeable tube containing composite fiber ceramic
WO2019057536A1 (fr) * 2017-09-20 2019-03-28 Basf Se Procédé de fabrication de matériau actif d'electrode
CN109654831A (zh) * 2018-11-29 2019-04-19 安徽五亩生态农业发展有限公司 一种便于操作的茶叶干燥筛选装置

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