EP3393646A1 - Dispositif et procédé de modification de matières solides poreuses - Google Patents

Dispositif et procédé de modification de matières solides poreuses

Info

Publication number
EP3393646A1
EP3393646A1 EP16781321.1A EP16781321A EP3393646A1 EP 3393646 A1 EP3393646 A1 EP 3393646A1 EP 16781321 A EP16781321 A EP 16781321A EP 3393646 A1 EP3393646 A1 EP 3393646A1
Authority
EP
European Patent Office
Prior art keywords
impregnating
range
activated carbon
container
impregnation
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
Application number
EP16781321.1A
Other languages
German (de)
English (en)
Inventor
Jann-Michael Giebelhausen
Christian Dr. SCHRAGE
Sven Dr. FICHTNER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bluecher GmbH
Original Assignee
Bluecher GmbH
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 Bluecher GmbH filed Critical Bluecher GmbH
Publication of EP3393646A1 publication Critical patent/EP3393646A1/fr
Pending legal-status Critical Current

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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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/09—Stirrers characterised by the mounting of the stirrers with respect to the receptacle
    • B01F27/091—Stirrers characterised by the mounting of the stirrers with respect to the receptacle with elements co-operating with receptacle wall or bottom, e.g. for scraping the receptacle wall
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/50—Mixing receptacles
    • B01F35/53—Mixing receptacles characterised by the configuration of the interior, e.g. baffles for facilitating the mixing of components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/95—Heating or cooling systems using heated or cooled stirrers
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • 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
    • B01J8/082—Controlling processes
    • 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
    • B01J8/087—Heating or cooling 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
    • 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
    • B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/354—After-treatment
    • C01B32/372—Coating; Grafting; Microencapsulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F2035/99—Heating
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00212—Plates; Jackets; Cylinders
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
    • B01J2208/00407—Controlling the temperature using electric heating or cooling elements outside the reactor bed
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
    • B01J2208/00415—Controlling the temperature using electric heating or cooling elements electric resistance heaters
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00539—Pressure
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00548—Flow
    • B01J2208/00557—Flow controlling the residence time inside the reactor vessel
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00654—Controlling the process by measures relating to the particulate material
    • B01J2208/00699—Moisture content regulation
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00858—Moving elements
    • B01J2208/00867—Moving elements inside the bed, e.g. rotary mixer
    • 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
    • B01J2219/19—Details relating to the geometry of the reactor
    • B01J2219/194—Details relating to the geometry of the reactor round
    • B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
    • B01J2219/1946—Details relating to the geometry of the reactor round circular or disk-shaped conical

Definitions

  • the present invention relates to the technical field of equipping adsorptive materials with catalytic or reactive properties.
  • the present invention relates in particular to the technical field of impregnating or finishing activated carbon with reactive or catalytic activity or with reactive and / or catalytic properties.
  • the present invention relates to a process for impregnating an activated carbon, in particular for equipping an activated carbon with reactive or catalytic activity.
  • the present invention relates to a production plant for impregnating an activated carbon, in particular for equipping the activated carbon with reactive or catalytic activity, or in particular for carrying out the method according to the invention.
  • the present invention also relates to the use of the production plant according to the invention for the impregnation of an activated carbon, as stated above, or for carrying out the method according to the invention.
  • the present invention also relates to an impregnating apparatus as such, which in particular has an impregnating container, preferably in the form of an impregnating reactor, and which for the purpose of impregnating an activated carbon, in particular for equipping an activated carbon with reactive or catalytic activity, or for Implementation of the method according to the invention can be used.
  • the invention also relates to the use of the impregnating device according to the invention for the impregnation of an activated carbon, as stated above, or for carrying out the method according to the invention.
  • the present invention also relates to an impregnated activated carbon as such, which is obtainable by the process according to the invention or which is obtained by the process according to the invention.
  • Activated carbon is the most widely used adsorbent due to its rather unspecific adsorptive properties. Legal requirements, but also the increasing awareness of the responsibility for the environment, lead to an increasing need for activated carbon.
  • activated carbon with overall improved or tailor-made adsorption properties, in which respect activated carbon should also be provided, which is equipped with a catalytically active or reactive component. In this way, the adsorption capacity of the activated carbon can be increased overall.
  • Activated carbon can generally be produced from vegetable, animal, mineral or petrochemical substances, it being possible to use as starting materials, for example, wood, peat, nut shells, brown coal or hard coal or various plastics.
  • Activated carbon is generally obtained by carbonation (synonymously also referred to as carbonization, pyrolysis, incineration or the like) and subsequent activation of the carbonaceous starting compounds or starting materials (starting materials), preference being given to starting compounds which lead to economically reasonable yields.
  • starting materials For the weight or material losses which occur in particular due to elimination of volatile constituents during the carbonation and the subsequent burnup during the activation are sometimes considerable, which is disadvantageous also in terms of process economics.
  • H. v. For example. Kienle and E. Bäder, "Activated Carbon and its Industrial Application", Enke Verlag Stuttgart, 1980.
  • Carbonization generally involves conversion of the carbonaceous feedstock to carbon, i. in other words, the starting material is charred, so to speak.
  • the nature of the activated carbon produced - such as fine or coarse-pored, solid or brittle, etc. - depends largely on the starting material used.
  • the basic principle of the subsequent activation of the carbonization is to selectively decompose or burn off part of the carbon generated during the carbonization under suitable conditions. This creates numerous pores, crevices and cracks, with the mass surface area increasing. During activation, a targeted burnup of the previously carbonized material is thus carried out. Since activation is degraded by carbon (in particular by oxidative processes), a certain loss of substance occurs in this process, which under optimum conditions is equivalent to the increase in porosity and an increase in the internal surface area and thus in the pore volume. Activation generally occurs under selective, or generally controlled, oxidizing conditions.
  • Activated carbon is used in various forms, such as powdered carbon, chipping coal or coal, coal and since the late 1970s also spherical activated carbon ("ball coal").
  • Spherical activated carbon has a number of advantages over other forms of activated carbon, which make it particularly valuable or even indispensable for certain applications: Spherical activated carbon is free-flowing, relatively abrasion-resistant and, in this context, also relatively hard. Due to its properties, ball carbon is very interesting for special applications.
  • Activated carbon is significantly produced by multi-stage and sometimes complex process, with a known method in the production of pellets of coal tar pitch and suitable asphalt-like residues of petroleum chemistry.
  • the starting material is oxidized, so that it becomes infusible, and subsequently scalded or activated.
  • activated carbon in particular in spherical form, can also be produced in a multistage process starting from bitumen, these multistage processes being very cost-intensive, and the associated high price of the resulting activated carbon prevents their use in numerous applications.
  • WO 98/07655 A1 describes a process for producing activated carbon in spherical form, in which first a mixture comprising a distillation residue from the production of diisocyanate, a carbonaceous processing aid and optionally one or more further additives , is processed into giant-shaped beads and then carbonized the resulting beads and subsequently activated.
  • the porosity in particular the total pore volume and the adsorption capacity on the one hand and the distribution of the pores, ie the proportion of micro, meso and macropores in Relation to the total pore volume, on the other hand;
  • the porosity can be selectively controlled by the selection of the starting materials and the process conditions.
  • micropores refers to pores having pore diameters of less than 2 nm
  • mesopores refers to pores having pore diameters in the range of 2 nm (ie 2 nm inclusive) to 50 nm inclusive and the term macropores such pores having pore diameters greater than 50 nm (ie> 50 nm).
  • activated carbon Due to its good adsorptive properties, activated carbon is used for a large number of applications. For example, activated carbon is used in medicine or pharmacy, but also in the food industry. Activated carbon also has wide-ranging applications for filter applications (eg filtration of gases and liquids, removal of undesirable or harmful or toxic gases, etc.).
  • activated carbon can be used in adsorption filter materials, especially especially in protective materials against poisons, such as chemical and biological warfare agents, such as ABC protective clothing.
  • adsorption filter materials especially especially in protective materials against poisons, such as chemical and biological warfare agents, such as ABC protective clothing.
  • chemical and biological warfare agents such as ABC protective clothing.
  • air and water vapor permeable protective suits against chemical warfare agents are known for this purpose; Such air and water vapor permeable suits often have an activated carbon adsorption filter layer which adsorbs the chemical poisons.
  • permeable adsorptive filter systems are often equipped with a catalytically active or reactive component by providing the activated carbon, for example, with a biocidal or biostatic catalyst, in particular based on metals or metal compounds .
  • a protective material is described, for example, in DE 195 19 869 A1, which contains a multilayer, textile, gas-permeable filter material with an adsorption layer based on activated carbon, in particular in the form of carbonized fibers, containing a catalyst from the group of copper, cadmium , Platinum, palladium, mercury and zinc in amounts of 0.05 to 12 wt .-%, based on the activated carbon material impregnated.
  • the equipment or impregnation of an activated carbon with a reactive or catalytic component is generally carried out such that activated carbon is brought as such in the form of the starting material first in contact with the catalyst component in a separate or separate device.
  • the combination of activated carbon, on the one hand, and the catalyst component on the other hand, generally takes place in devices or apparatuses specially designed for this purpose, such as stirred kettles or the like.
  • drying is generally carried out in a separate or independent drying apparatus or apparatus with concomitant transfer of the moist material to obtain the activated carbon equipped with a corresponding reactive or catalytic activity.
  • an activation of the catalyst component can take place, which in turn takes place in separate activation devices or apparatuses which are capable of enabling a corresponding heating of the material. Again, the material must first be transferred again.
  • stirred tanks are known as such, which are designed exclusively for contacting the activated carbon with a corresponding liquid medium. Due to their special design, stirred tanks of this kind are suitable, in particular, for drying, and not for thermal aftertreatment of solids, in order to ensure thorough mixing.
  • so-called solid dryers are used in the prior art for drying purposes of the previously treated with a fluid or liquid medium particulate solid in the form of activated carbon.
  • Such prior art dryers can not be used to suspend solids in fluid media nor to thermally post-treat solids.
  • activation devices are used, which should ensure, for example, by oxidative or reductive processes, a possible activation of the catalyst component.
  • a distinction is generally made depending on the energy source used between directly (ie generation of thermal energy directly on the activation furnace, for example by means of direct electrical heat generation) and indirectly (ie Generation of thermal energy far away from the activation furnace via separate heating systems and supply of a heat-transferring medium to the device, for example by means of a previously heated thermal fluid or the like) heated devices or activation furnaces.
  • the product quality of the activated carbons with reactive or catalytic activity obtained on the basis of the prior art is often not optimal due to the impaired controllability of the devices used.
  • the repeated removal and transfer of the (intermediate) products from or into the respective devices leads to material losses and damage.
  • the impregnating devices used in the prior art are also not optimal insofar as sometimes complete mixing of the components on which the impregnation is based (impregnating agent on the one hand and activated carbon on the other) is ensured.
  • the devices of the prior art often also have the disadvantage that in particular the activated carbon to be impregnated on the wall above the mixture or the liquid level of the suspension of activated carbon and impregnating agent accumulates by adhering and thus mixing with the impregnating agent and thus a complete impregnation is no longer available, which deteriorates the quality of the resulting impregnated product as a whole, since previously adhering activated carbon can be fed back especially when emptying the activated carbon charge.
  • drying devices used in the prior art do not always lead to optimum drying results, in particular with regard to a satisfactory or complete removal of the liquid carrier medium or solvent on which the impregnating agent is based.
  • removal of the liquid carrier medium is often possible only with high energy input.
  • the devices used in the prior art for after treatment or activation of the catalyst component are sometimes not energetically optimal and do not always lead to a uniform heating or to a uniform contact of the previously impregnated activated carbon with any activation media (such as a reactive (ambient) Atmosphere or the like).
  • the object of the present invention is therefore to provide a method and a special production system or a device as such, which at least largely avoids or at least attenuates the previously described disadvantages of the prior art.
  • a simplified method and a simplified production plant or impregnation device are to be provided as such, wherein in particular also the use or the number of equipment or equipment to be used should be reduced.
  • a further object of the present invention is also to be seen in providing a corresponding method for impregnating an activated carbon or for equipping an activated carbon with reactive or catalytic activity, which is optimized with regard to the process control or the process sequence and in which in particular the handling of the materials used, in order to also provide a cost-efficient and high-performance production method on this basis.
  • Yet another object of the present invention is also to provide a corresponding production plant or an impregnating device as such, in particular for carrying out the method according to the invention, which is less complex in terms of apparatus and which results in an efficient implementation of the method according to the invention
  • the use of energy is reduced and the quality of the products obtained in the form of impregnated activated carbon with reactive or catalytic activity should be increased.
  • a corresponding production plant or an associated impregnating apparatus is to be provided, which enables an efficient implementation of the method provided according to the invention for obtaining an impregnated activated carbon according to the invention and which is improved in terms of their performance compared with those of the prior art.
  • Yet another object of the present invention is also to be seen to provide a corresponding activated carbon as such, which as a result of the application of the method according to the invention or the use of the production plant or impregnation device according to the invention has improved overall properties, in particular as the equipment of the activated carbon As far as the reactive or catalytically active components are concerned.
  • the present invention thus proposes, according to a first aspect of the present invention, a process for impregnating an activated carbon, in particular for equipping an activated carbon with reactive or catalytic activity, according to the independent method claim; Further, particularly advantageous embodiments of the method according to the invention are the subject of the relevant subclaims.
  • the present invention relates to a production plant for impregnating an activated carbon, in particular for equipping an activated carbon having a reactive or catalytic activity, or for carrying out the process according to the invention, as described in the corresponding US Pat.
  • the production plant according to the invention claim is defined; Further, particularly advantageous embodiments of the production plant according to the invention are the subject of the relevant subclaims.
  • the present invention - according to a third aspect of the present invention - also relates to the use of the production plant according to the invention for impregnating an activated carbon or for carrying out the process according to the invention, as defined in the corresponding use claim.
  • the present invention also relates - according to a fourth aspect of the present invention - also an impregnating apparatus as such, which in particular has at least one impregnation container, for impregnating an activated carbon or for carrying out the method according to the invention, as defined in the corresponding device claim.
  • an impregnating apparatus as such, which in particular has at least one impregnation container, for impregnating an activated carbon or for carrying out the method according to the invention, as defined in the corresponding device claim.
  • advantageous embodiments of the impregnating device according to the invention are the subject of the relevant subclaim.
  • the present invention - according to a fifth aspect of the present invention - also relates to the use of the impregnating device according to the invention for impregnating an activated carbon or for carrying out the method according to the invention, as described in the corresponding independent use according to this aspect Claim is defined.
  • the present invention also relates to an impregnated activated carbon as such which is obtainable by the process according to the invention and as defined in the corresponding claim relating to the activated carbon.
  • the present invention thus - according to a first aspect of the present invention - the method for impregnating an activated carbon, in particular for equipping an activated carbon with reactive and / or catalytic activity, wherein the activated carbon is subjected to a particular multi-stage impregnation treatment, wherein the impregnation treatment to follow steps (a) to (c), in particular in the sequence specified below, comprises: (A) contacting the activated carbon, in particular a plurality of discrete activated carbon particles, with at least one impregnating agent, in particular in the form of a solution and / or dispersion, wherein the impregnating agent comprises at least one liquid carrier medium and at least one impregnating, in particular at least one catalytically active component; then
  • step (c) optionally thermal aftertreatment of the impregnated activated carbon resulting from step (b), in particular for activating and / or further fixing the impregnating component, in particular the catalytically active component, preferably under heat and / or heating;
  • impregnation treatment in particular the steps (a) to (c), in a single and / or common impregnation, in particular impregnation (impregnation reactor) is performed.
  • a central idea of the present invention is thus to be seen in that all process steps according to the invention for the impregnation of an activated carbon for the purpose of equipping the activated carbon in question with reactive or catalytic activity - namely both the contacting of the activated carbon with the impregnating agent and the removal of the liquid carrier medium of the impregnating agent or the drying of the impregnated activated carbon and the subsequently optionally provided thermal aftertreatment of the impregnated activated carbon - are carried out in a single or in one and the same impregnating device.
  • a special and the method according to the invention structurally adapted impregnating, which for example have an impregnating container or an impregnating or in the form of an impregnating or impregnating reactor, used.
  • the impregnating device used according to the invention which is also part of the production plant according to the invention, has a special structural design Particular features and embodiments, which make it possible to perform all the steps in this device itself.
  • a central feature of the present invention is thus that the various basic operations of the process according to the invention with the contacting or suspending the activated carbon in the impregnating agent, the removal of the liquid carrier medium or any excess impregnating agent together with the drying of the impregnated activated carbon and with the optionally provided thermal aftertreatment for purposes of activation of the catalytic or reactive component in a single (common) device performed and thus summarized or combined can be implemented.
  • the yield of the product obtained in accordance with the invention in the form of the impregnated activated carbon or in the form of the activated carbon with reactive or catalytic activity is also increased insofar as the impregnating device used according to the invention has regard to its construction or structure is further optimized in such a way that an adhesion of activated carbon particles or particles to the wall of the impregnating device during the process is avoided, so that at least substantially no matter with respect to the amount of activated carbon used. loss of material - and this at the same time high or homogeneous equipment of the activated carbon with the reactive or catalytically active component. In addition, in this connection with the production plant according to the invention, the loss of possibly excess impregnating agent is reduced, which also leads to a simpler recycling of the impregnating agent used.
  • the invention also provides a cost-effective method or a related production plant or impregnation device, since on the one hand the energy expenditure arising during the process is reduced and, on the other hand, the purchase and maintenance of further devices or apparatuses is eliminated.
  • the space or space requirement for installing the production system provided according to the invention and for carrying out the method according to the invention is significantly reduced, which also enables a large-scale implementation of the method according to the invention in connection with the aforementioned advantages and properties.
  • the production plant is operated semi- or quasi-continuously, which is associated with further procedural advantages.
  • the production plant according to the invention can also be coupled with a production plant for activated carbon as such or operated in direct connection to such a production plant.
  • a further advantage associated with the present invention can be seen in the fact that, due to the special process control, namely contacting the activated carbon with the impregnating agent or exposing the impregnating agent to the activated carbon and subsequently removing the liquid carrier medium of the impregnating agent (Drying of the activated carbon) and the optionally thermal aftertreatment is carried out in a single or common impregnating, overall a higher or more homogeneous impregnation of the resulting activated carbon with less formation of encrustations (ie unwanted deposits of the impregnating agent or the impregnating on the Surface of the activated carbon) results on the activated carbon, which is in particular due to the associated with the use of a single device or apparatus improved controllability of the process parameters.
  • a further advantage of the present invention is the fact that, with regard to the production plant or impregnating device provided according to the invention, the maintenance or cleaning effort is significantly reduced, since only one apparatus or device exists as such and is maintained or cleaned will need.
  • contacting the activated carbon, in particular a plurality of discrete activated carbon particles, with at least one impregnating agent is to be understood very broadly according to the invention.
  • the abovementioned formulation can be understood to mean that, as part of contacting, the impregnating agent is exposed to the impregnating component on the activated carbon, which is used in particular in the form of a multiplicity of discrete particles or particles.
  • the contacting or the exposure is accompanied in particular by an at least substantially complete wetting or coating of the activated carbon with the impregnating agent or the impregnating component, in particular as far as the outer and the inner surface of the activated carbon is concerned.
  • the impregnating device used for the process may have at least one, in particular, closable impregnating container, preferably in the form of an impregnating vessel (stirred tank).
  • the impregnating device in particular the impregnating container, can have at least one stirring or mixing device, in particular a stirring or mixing device having a multiplicity of mixing elements (stirring elements). Due to the good mixing of the components used according to the method (impregnation), the use of a stirring or mixing device nierffen on the one hand and activated carbon on the other hand) further improves the contacting of the activated carbon with the impregnating agent. In addition, the removal of the liquid medium or, if appropriate, excess impregnating agent and optionally provided thermal aftertreatment, carried out in the same device, are also improved as a result of the good mixing of the components.
  • the impregnation device in particular the impregnation container, preferably the wall (shell) or the housing of the impregnation container, on the one hand and / or the stirring or mixing device, preferably the mixing elements, on the other hand can be heated be formed.
  • the method is such that the impregnating container and the stirring or mixing device are designed to be heatable.
  • uniform heating of the components used according to the invention can be carried out, as it were, from the outside (i.e., in particular through the impregnation container) and from the inside (i.e., in particular, by the mixer). Due to the stirring or mixing device, there is also a good heat distribution in relation to the components used as a result of the mixing with the mixer.
  • an impregnation container with a specific geometry or shape:
  • the impregnation container in particular the upper portion of the impregnation container, can taper in the direction of the upper end of the impregnation container.
  • the upper portion of the impregnation container can be frusto-conical or conical.
  • the impregnation container, in particular the lower portion of the impregnation container can taper towards the lower end of the impregnation container.
  • the lower portion of the impregnation container may be frusto-conical or conical.
  • the impregnation container is designed to be double conical or double frustoconical or in the form of a double cone or a double truncated cone. This achieves, on the one hand, a further improvement in the mixing of the components in the respective process steps and a reduction in the adhesion, in particular of the activated carbon, to the wall of the impregnation container and improved discharge of the respective components from the impregnation container.
  • the mixing elements are adapted to the geometry of the impregnation container.
  • the mixing elements can be formed such that the ends of the respective mixing elements to the wall or the housing of the impregnation are at least substantially equal spaced or that the ends of the respective mixing elements with the course of the wall or the housing of the impregnation at least substantially constant spacing.
  • the stirring or mixing device is designed as a (rotary) agitator with an agitator shaft arranged at least substantially parallel or along the longitudinal axis of the impregnating container.
  • the stirring shaft should in this context be arranged or positioned at least substantially centrally in the impregnating container.
  • the mixing elements can be arranged or positioned radially extending on the stirring shaft.
  • the stirring shaft can be designed as a rotation shaft with mixing elements extending radially therefrom.
  • the mixing elements arranged along the agitator shaft or aligned with the longitudinal axis of the impregnation container and extending radially therefrom each have at their respective ends a similar spacing to the (housing) wall of the impregnation container.
  • the mixing elements can be formed or arranged or positioned along the agitator shaft such that in the operating or application state mixing or transport of the impregnating agent or the activated carbon in the axial and / or radial direction, in particular in the axial and radial directions , is present.
  • an impregnating device or impregnating container which has at least one introduction opening (feed opening), in particular for introducing the impregnating agent or the activated carbon.
  • the insertion opening can be arranged or positioned at the upper end or in the region of the upper section of the impregnating container.
  • the impregnating device, in particular the impregnating container can have at least one outlet opening (discharge opening), in particular for removing or draining liquid carrier medium and / or any excess impregnating agent or impregnated activated carbon or an optionally used washing medium.
  • the outlet opening can be arranged or positioned at the lower end or in the region of the lower section of the impregnating container.
  • the impregnating device in particular the impregnation container, at least one further outlet opening (discharge opening) in particular for removing in particular gaseous substances or media (such as in particular previously transferred by heating in the gas phase carrier medium of the impregnating agent) or for removing or discharging any Have excess impregnant.
  • the further outlet opening can be arranged or positioned at the upper end or in the region of the upper section of the impregnation container.
  • the further outlet opening can have a pipeline extending into the region of the lower section of the impregnating container, which preferably runs along the (inner) wall of the impregnating container, in order to perform the function of the stirring. Mixer not to interfere.
  • the carrier medium of the impregnating agent can be removed in the gaseous state, or else generally be sucked off in liquid form, in particular during drying with the associated heating of the components.
  • any excess impregnating agent can also be removed, in particular by suction.
  • an efficient filling or charging or an efficient removal or removal of the respective components can be carried out.
  • the impregnating agent, in particular the impregnating component may contain at least one metal, in particular in the form of a metal compound.
  • the impregnating agent in particular the impregnating component, can have at least one metal in a positive oxidation state, in particular at least one metal cation.
  • the oxidation state of the metal may be in the range of + 1 to + VII, in particular in the range of + 1 to + IV, preferably in the range of + 1 to + III, and more preferably + 1 or + II.
  • the impregnating agent, in particular the impregnating at least one metal selected from the group of metals of the main and subgroups of the Periodic Table of the Elements and the lanthanides having.
  • the impregnating agent in particular the impregnating, at least one metal selected from elements of main group IV or subgroups I, II, III, IV, V, VI, VII and VII I of the Periodic Table of the Elements, in particular from elements of the main group IV or subgroups I and II of the Periodic Table of the Elements.
  • the impregnating agent in particular the impregnating component, contains at least one metal selected from the group consisting of Cu, Ag, Au, Zn, Hg, Sn, Ce, Ti, Zr, V, Nb, Cr, Mo, W, Mn, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd and Pt, especially Zn, Ag, Sn, Ni and Cu.
  • the impregnating agent in particular the impregnating component, has at least one metal compound which is soluble or dissociable in the impregnating agent, in particular in the liquid carrier medium, preferably based on at least one previously defined metal.
  • the impregnating agent, in particular the impregnating component at least one inorganic or organic metal compound, preferred on the basis of at least one previously defined metal, in particular a metal salt or metal oxide, preferably a metal salt.
  • the impregnating agent in particular the impregnating component, may comprise at least one organic or inorganic metal salt, preferably based on at least one previously defined metal.
  • the salt can be selected from the group of halide salts, sulfates, sulfides, sulfites, nitrates, nitrites, phosphates, phosphides, phosphites, carbamates, alcohols and carboxylic acid salts, in particular halide salts and carboxylic acid salts.
  • the impregnating agent in particular the impregnating, at least one metal halide, preferably based on at least one previously defined metal, in particular a fluoride, chloride, bromide or iodide, preferably chloride, or a carboxylic acid salt of a metal, in particular acetate.
  • the impregnating agent in particular the impregnating, at least one acidic or basic compound, in particular based on phosphoric acid, calcium carbonate, trimethanolamine, 2-amino-1, 3-propanediol or Sulfur, has.
  • the impregnating agent in particular the impregnating component, comprises at least one enzymatically active substance (enzyme).
  • enzyme enzymatically active substance
  • the amount of the impregnating component in the impregnating agent can vary within wide limits. Particularly good results are obtained when the impregnating the impregnating in an amount of at least 1 wt .-%, in particular at least 2 wt .-%, preferably at least 5 wt .-%, preferably at least 10 wt .-%, based on the liquid Carrier medium of the impregnating agent containing.
  • the impregnating agent may comprise the impregnating component in an amount in the range of from 1% to 80%, more preferably in the range of from 2% to 70%, preferably in the range of from 5% to 5% 60 wt .-%, preferably in the range of 10 wt .-% to 50% by weight, based on the liquid carrier medium of the impregnating agent.
  • the liquid carrier medium of the impregnating agent comprises or consists of an inorganic solvent or that the liquid carrier medium is based on water or comprises water or consists thereof.
  • the liquid carrier medium may comprise or consist of an organic solvent, in particular selected from the group of hydrocarbons, in particular alcohols, ketones, aldehydes and their combinations and / or mixtures, preferably alcohols.
  • step (a) the impregnating agent is used in a weight-related excess or in a weight-related excess to the activated carbon, preferably in a weight-related excess to the activated carbon.
  • the procedure can be such that the components are in the form of a suspension having liquid properties in the impregnating device.
  • the process control according to the invention makes it possible, in particular also due to the special design of the impregnating device or the impregnation ratio, to use large quantitative ranges of the respective components based on the impregnating agent on the one hand and the activated carbon on the other hand.
  • the process according to the invention can thus be carried out as a wet impregnation or as a dry impregnation, preferably wet impregnation.
  • step (a) the impregnating agent on the one hand and the activated carbon on the other hand in a weight ratio (impregnating: activated carbon) in the range of 6: 1 to 1: 3, in particular in the range of 5: 1 to 1 : 2, preferably in the range of 4: 1 to 1: 1, preferably in the range of 3: 1 to 1: 1, can be used.
  • the impregnating agent on the one hand and the activated carbon on the other hand independently of one another, in particular via the at least one insertion opening of the impregnating device, in particular of the impregnating agent, preferably each via separate or separate insertion into the impregnation, in particular in the impregnation, filled or introduced.
  • the impregnating device or the impregnating container may in this context have an insertion opening for the impregnating agent and a further insertion opening for the activated carbon.
  • the procedure is generally such that in step (a) the impregnating agent, on the one hand, and the activated carbon, on the other hand, are mixed, in particular to obtain a suspension, in particular a homogeneous suspension.
  • step (a) with the introduction of stirring or shearing forces, in particular with stirring, preferably with the use of the stirring or mixing device of the impregnating device, in particular of the impregnating container.
  • step (a) in step (a) at least substantially complete wetting or coating of the activated carbon with the impregnating agent, in particular with the impregnating, in particular both the outer and the inner surfaces, preferably the micro-, meso- and / or macropores, the activated carbon occurs.
  • the impregnating agent in particular with the impregnating, in particular both the outer and the inner surfaces, preferably the micro-, meso- and / or macropores.
  • activated carbons can be used in a wide variety of training. However, particularly good results are achieved if the activated carbon used is a particulate or particulate activated carbon or activated carbon particle, preferably in the form of activated carbon particles in the form of granules ("granular carbon") or spherical form (“spherical carbon”).
  • granular carbon granules
  • spherical carbon spherical carbon
  • the diameter of the activated carbon in particular the particulate or particulate activated carbon or the activated carbon particles, vary within wide ranges. However, it is advantageous if the diameter of the activated carbon in the range of 0.01 mm to 5 mm, preferably in the range of 0.02 mm to 4 mm, preferably in the range of 0.03 mm to 3 mm, particularly preferably in the range from 0.05 mm to 2 mm, most preferably in the range of 0.1 mm to 1 mm.
  • the average diameter, in particular the average diameter D 50 , of the activated carbon, in particular the particulate or particulate activated carbon or the activated carbon particles in the range of 0.01 mm to 4 mm, in particular in the range of 0.03 mm to 3 mm, preferably in the range of 0.05 mm to 2 mm, particularly preferably in the range of 0.1 mm to 1 mm, very particularly preferably in the range of 0.2 mm to 0.8 mm.
  • the corresponding particle sizes can be determined in particular on the basis of the method according to ASTM D2862-97 / 04.
  • the aforementioned quantities can be determined using determination methods based on a sieve analysis, on the basis of a sieve analysis, on the basis of X-ray diffraction, laser diffractometry or the like.
  • the respective determination methods are well known to the person skilled in the art, so that no further explanation is required in this regard.
  • the activated carbon may be obtainable by carbonization and subsequent activation of a synthetic or non-natural-based starting material, in particular based on organic polymers.
  • a synthetic or non-natural-based starting material in particular based on organic polymers.
  • particularly hard and abrasion-resistant activated carbons are obtained, which also have a defined porosity.
  • Such activated carbons are particularly suitable for use in the context of the method according to the invention. This also applies in particular to those activated carbons which are obtained from a starting material based on organic polymers, in particular based on sulfonated organic polymers, preferably based on divinylbenzene-crosslinked polystyrene, preferably based on styrene / divinylbenzene copolymers, in particular by carbonation and subsequent activation of the starting material.
  • the content of divinylbenzene in the starting material can be in the range from 1% by weight to 20% by weight, in particular from 1% by weight to 15% by weight, preferably from 1.5% by weight 12.5 wt .-%, preferably 2 wt .-% to 10 wt .-%, based on the starting material, are.
  • the activated carbons used according to the invention can also be activated carbons which are obtained from a starting material based on an ion exchange resin, in particular of the gel type, containing in particular sulfonated or sulfonic acid groups.
  • a polymer-based spherical activated carbon PBSAC, polymer-based Spherical Activated Carbon
  • PBSAC polymer-based Spherical Activated Carbon
  • the activated carbon has a total pore volume, in particular a total pore volume according to Gurvich, in the range from 0.3 cm 3 / g to 4 cm 3 / g, in particular in the range from 0.4 cm 3 / g to 3 , 5 cm 3 / g, preferably in the range of 0.5 cm 3 / g to 3 cm 3 / g, more preferably in the range of 0.6 cm 3 / g to 2.5 cm 3 / g, most preferably in Range of 0.5 cm 3 / g to 1, 5 cm 3 / g.
  • At least 65%, in particular at least 70%, preferably at least 75%, preferably at least 80%, of the total pore volume, in particular of the total Gurvich pore volume, of the activated carbon through pores having pore diameters of at most 50 nm, in particular by Micro and / or mesopores are formed.
  • the activated carbon can be a pore volume formed by pores with pore diameters of at most 2 nm (ie ⁇ 2 nm), in particular microporous volumes after carbon black, in the range from 0.05 cm 3 / g to 2.5 cm 3 / g, in particular 0.15 cm 3 / g to 2 cm 3 / g, preferably 0.3 cm 3 / g to 1, 5 cm 3 / g.
  • the activated carbon may have a BET specific surface area of 600 m 2 / g to 4,000 m 2 / g, in particular 800 m 2 / g to 3,500 m 2 / g, preferably from 1, 000 m 2 / g to 3,000 m 2 / g, more preferably from 1 .200 m 2 / g to 2,750 m 2 / g, very particularly preferably from 1 .300 m 2 / g to 2,500 m 2 / g.
  • the carbon black determination method is known per se to the person skilled in the art, and moreover, for further details on the determination of the pore surface and pore volume for carbon black, reference can be made, for example, to RW Magee, Evaluation of the External Surface Area of Carbon Black by Nitrogen Adsorption, Presented at the Meeting of the Rubber Division of the American Chem. Soc., October 1994, z. B.
  • the determination of the specific surface area according to BET is generally known to the person skilled in the art, so that in this regard no further details need to be carried out. All BET surface area information refers to the determination in accordance with ASTM D6556-04.
  • MP-BET MultiPoint BET determination method
  • MP-BET MultiPoint BET determination method
  • the procedure can be such that the contacting is carried out at temperatures above the freezing or solidification temperature of the impregnating agent or below the boiling or decomposition temperature of the impregnating agent.
  • the temperatures stated in this regard are based on atmospheric pressure (1 .013,25 hPa or 1, 01325 bar).
  • the contacting provided in step (a) takes place in such a way that, so to speak, the impregnating agent is allowed to penetrate or penetrate with the relevant catalytically active component in relation to the activated carbon used according to the invention, as stated above.
  • step (a) the contacting at temperatures in the range of 1 ° C to 150 ° C, in particular in the range of 5 ° C to 100 ° C, preferably in the range of 10 ° C to 75 ° C, preferably in the range of 15 ° C to 60 ° C, more preferably in the range of 20 ° C to 50 ° C, most preferably in the range of 20 ° C to 40 ° C, are performed.
  • the temperatures provided in step (a) can be achieved by heating the impregnating device, in particular the impregnating container, preferably the wall or the housing of the impregnating container, and / or by heating the stirring or mixing device, preferably the mixing elements of the stirring or mixing device Mixing device, can be adjusted.
  • step (a) the contacting for a period of time in the range of 0.01 h to 48 h, in particular in the range of 0.05 h to 24 h, preferably in the range of 0, 1 h to 12 h, preferably in the range from 0.5 h to 10 h, particularly preferably in the range from 1 h to 8 h, very particularly preferably in the range from 2 h to 8 h.
  • step (a) below atmospheric pressure (atmospheric pressure) (1 .013,25 hPa) can be moved.
  • atmospheric pressure atmospheric pressure
  • step (b) of the process according to the invention in addition to the removal of the liquid carrier medium of the impregnating agent, it is also possible to remove any excess impregnating agent as such.
  • step (b) it is possible in particular to proceed in such a way that in step (b) the removal of the liquid carrier medium or of any excess impregnating agent under pressurization or increased pressure (pressing out of the liquid carrier medium or of the impregnating agent) or under reduced pressure or reduced pressure (Removal of the liquid carrier medium or the impregnating agent) takes place.
  • step (b) it is also possible to proceed in step (b) such that the removal of the liquid carrier medium takes place under atmospheric pressure (1 .013.25 hPa) or normal pressure, for example by discharging the liquid media at the outlet opening provided in particular in the region of the lower end which can be equipped for this purpose with a filter unit for the retention of the activated carbon or the like.
  • step (b) the removal of the liquid carrier medium or of any excess impregnating agent can thus take place via the at least one outlet opening, in particular for removing the liquid carrier medium or excess impregnating agent (lower outlet opening) and / or via the at least one Outlet opening in particular for the removal of gaseous substances takes place (upper outlet opening).
  • step (b) the removal of the liquid carrier medium or of any excess impregnating agent, preferably the removal of the liquid carrier medium, takes place by evaporation. Removal by evaporation may also be carried out following any removal of the carrier medium or, if appropriate, excess impregnant in liquid form, as described above.
  • the removal of the liquid carrier medium or of any excess impregnating agent should be carried out at temperatures above the boiling point of the liquid carrier medium or of the impregnating agent, in particular of the liquid carrier medium.
  • step (b) at temperatures in the range of 1 ° C to 300 ° C, in particular in the range of 10 ° C to 250 ° C, preferably in the range of 15 ° C to 200 ° C, preferably in the range of 20 ° C. up to 175.degree. C., more preferably in the range from 50.degree. C. to 150.degree.
  • the temperatures provided in step (b) can likewise be achieved by heating the impregnating device, in particular the impregnating container, preferably the wall or housing of the impregnating container, and / or by heating the mixing device, preferably the mixing elements of the stirring or mixing device. Mixing device to be adjusted.
  • step (b) the removal of the liquid carrier medium or of any excess impregnating agent for a period in the range of 0.01 h to 36 h, in particular in the range of 0.05 h to 20 h, preferably in the range of 0, 1 h to 10 h, preferably in the range of 0.5 h to 8 h, particularly preferably in the range of 1 h to 6 h.
  • step (b) with the introduction of stirring or shearing forces, in particular with stirring, preferably using the stirring or mixing device of the impregnating device, in particular of the impregnating container.
  • step (b) the removal of the liquid carrier medium and / or of any excess impregnating agent via the at least one outlet opening, in particular for removal of the liquid carrier medium and / or of optionally excess impregnating agent and / or via the further outlet opening, in particular for removal in particular gaseous Substances and / or media and / or for removing and / or draining off any excess impregnating agent.
  • liquid carrier medium removed in step (b) and / or the optionally excess impregnating agent can be recycled.
  • step (b) the impregnated activated carbon has a residual moisture content in the range from 1% by weight to 50% by weight, in particular in the range from 5% by weight to 40% by weight. , preferably in the range from 10% to 30% by weight, based on the impregnated activated carbon.
  • step (b) the removal of the impregnated activated carbon can take place via the at least one outlet opening, in particular for the removal of the impregnated activated carbon.
  • step (c) the optionally provided thermal aftertreatment can be carried out at temperatures above the temperatures set or intended for the drying in step (b).
  • the catalytic activity can be increased or achieved or obtained if necessary.
  • the catalytically active component can be further fixed to the activated carbon, optionally with the formation of chemical bonds.
  • step (c) at temperatures in the range of 50 ° C to 800 ° C, in particular in the range of 75 ° C to 500 ° C, preferably in the range of 90 ° C to 300 ° C, are moved.
  • the temperatures provided in step (c) can be set by heating the impregnating device, in particular the impregnating container, preferably the wall or the housing of the impregnating container, and / or by heating the stirring or mixing device, preferably the mixing elements.
  • the impregnated activated carbon can be heated particularly effectively and uniformly to the desired temperatures for purposes of activating the impregnating component.
  • the thermal aftertreatment can be carried out under atmospheric pressure or atmospheric pressure (1 .013,25 hPa).
  • step (c) it may be provided in step (c) that the thermal aftertreatment takes place with adjustment of the (activation) atmosphere.
  • step (c) in particular under ambient atmosphere (ambient air), in particular air, or under an inert atmosphere, in particular nitrogen atmosphere, or in particular slightly oxidizing atmosphere, in particular oxygen-containing atmosphere, or in particular slightly reducing atmosphere, in particular hydrogen-containing atmosphere, method.
  • the impregnating device can also be equipped with corresponding openings for the exchange or adjustment of the respective atmosphere.
  • the thermal aftertreatment may be for a period in the range of 0.01 h to 30 h, in particular in the range of 0.05 h to 20 h, preferably in the range of 0, 1 h to 10 h, preferably in the range from 0.5 h to 8 h.
  • step (c) with the introduction of stirring or shearing forces, in particular with stirring, preferably with the use of the stirring or mixing device of the impregnating device, in particular of the impregnating container.
  • step (c) the removal of the activated impregnated activated carbon can take place via the at least one outlet opening, in particular for the removal of the impregnated activated carbon, in particular after cooling of the resulting impregnated activated carbon.
  • step (a) in particular between step (a) and step (b), or after carrying out step (b), in particular between step (b) and step (c) or, after carrying out step (c), at least one washing or purifying step is carried out with a washing or purifying of the impregnated activated carbon, if appropriate followed by at least one drying step.
  • the washing or purification step can be carried out using at least one in particular liquid washing or purification medium or agent, in particular aqueous-based washing or purification medium, preferably an especially alkaline washing or purification solution.
  • the washing or purification medium may contain at least one basic component, in particular at least one alkali metal hydroxide, preferably sodium hydroxide (NaOH).
  • alkali metal hydroxide preferably sodium hydroxide (NaOH).
  • washing or purification medium in a weight ratio related to the activated carbon (washing or purification medium: activated carbon) in the range from 5: 1 to 1: 5, in particular in the range from 4: 1 to 1: 4, preferably in the range from 4: 1 to 1: 3, preferably in the range from 3: 1 to 1: 1.
  • the washing or purification step can take place at temperatures in the range from 1 ° C. to 150 ° C., in particular in the range from 5 ° C. to 100 ° C., preferably in the range from 10 ° C. to 75 ° C., preferably in the range from 15 ° C to 60 ° C, more preferably in the range of 20 ° C to 50 ° C, most preferably in the range of 20 ° C to 40 ° C, are performed.
  • the temperatures provided in the washing or purification step can be set by heating the impregnating device, in particular the impregnating container, preferably the wall (shell) or the housing of the impregnating container, or by heating the stirring or mixing device, preferably the mixing elements become.
  • the washing or purification step can be carried out for a period of time in the range from 0.01 h to 48 h, in particular in the range from 0.05 h to 24 h, preferably in the range from 0.1 h to 12 h, preferably in the range from 0.5 h to 10 h, particularly preferably in the range from 1 h to 8 h, very particularly preferably in the range from 2 h to 8 h.
  • the washing or purification step can be carried out under atmospheric pressure or atmospheric pressure (1 .013,25 hPa).
  • step (a), step (b) and step (c) and, if appropriate, the washing or purification step are carried out in succession or directly following one another, which also results from the use of a common or single Impregnating, in particular impregnation, is made possible. In this way, a further increase in the efficiency of the method according to the invention can be achieved.
  • the method according to the invention may be carried out using a production line as defined below or using an impregnating device as defined below.
  • FIG. 1 shows a preferred embodiment of the method according to the invention, according to which the process is carried out with the relevant steps (a) to (c) according to the invention using a production plant P and a common impregnation treatment or impregnation unit 4.
  • the present invention further relates - according to a second aspect of the present invention - also a production plant for impregnating an activated carbon, in particular for equipping an activated carbon with reactive or catalytic activity, in particular for carrying out the previously described method according to the invention, according to which Production plant relevant claim, with further advantageous embodiments of this aspect of the invention is the subject of the corresponding subclaims.
  • Fig. 1 is a schematic representation of the use of the invention
  • step (a) The process of contacting the activated carbon with the impregnating agent according to step (a), the subsequent removal of the liquid carrier medium or optionally excess impregnating agent according to step (a) b) and the subsequent thermal aftertreatment of the impregnated activated carbon according to step (c) are carried out in a single or common and thus in one and the same impregnating device of the production plant according to the invention;
  • 2A is a schematic representation of a production plant P according to the invention according to a first embodiment of the invention, according to which the impregnation device 4 used for the production plant P is formed on the basis of an impregnation container 6, in which the lower portion 6 "tapers conically to the lower end of the impregnation container 6 and the upper section 6 'of the impregnating holds 6 arched or formed in the manner of a dome lid; 2A also shows an embodiment of the arrangement of a stirring and mixing plant in the impregnating container 6 which is preferred according to the invention, wherein the stirring or mixing unit 8 has a corresponding agitating shaft 10 with mixing elements 9, the mixing elements 9 being adapted to the geometry of the impregnating container 6 are;
  • both the lower section 6 'and the upper section 6 "of the impregnating container 6 are thus cone-shaped or truncated-like, and the arrangement of the stirring or mixing unit 8 with a stirring shaft 10 is also in the FIG Impregnating container 6 and the geometry of the impregnation container 6 adapted training of the mixing elements 9 shown.
  • the present invention thus also relates to the production plant P for impregnation, as illustrated in FIGS. 2A and 2B an activated carbon, in particular for equipping an activated carbon having reactive and / or catalytic activity, in particular for carrying out the method according to the invention described above, the production plant P comprising the following devices 1, 2, 3, 4:
  • At least one first storage unit 1 for receiving or storing at least one impregnating agent, in particular in the form of a solution or dispersion, wherein the impregnating agent comprises at least one liquid carrier medium and at least one impregnating component, in particular at least one catalytically active component;
  • At least one second storage unit 2 for receiving or storing at least one activated carbon, in particular a plurality of discrete activated carbon particles; at least one impregnating device (impregnating treatment unit) 4 arranged downstream of the first storage unit 1 and the optionally present second storage unit 2, in particular wherein the impregnating device 4 comprises at least one impregnating container (impregnating reactor) 6, wherein the impregnating device 4 is designed such that
  • (C) optionally a thermal aftertreatment of the resulting impregnated activated carbon, in particular for the activation or further fixing of the impregnating component, preferably under the effect of heat and / or heating;
  • the production plant P in particular the impregnating device 4 has at least one, in particular, impregnable impregnating container 6, in particular impregnating vessel (stirred tank) (FIGS. 2A and 2B).
  • the impregnation container 6 may be arranged or aligned, in particular in the operating or application state, at least substantially vertically or upright, in particular with respect to the longitudinal axis L of the impregnation container 6.
  • the impregnation container 6 is preferred operated in a vertical arrangement or positioning with reference to its longitudinal axis L, as illustrated equally in Fig. 2A and Fig. 2B.
  • the impregnation container 6 has an upper and a lower end.
  • the impregnation container 6 may have an upper portion 6 'and a lower portion 6 ".
  • the term" portion "as used in the invention refers to one
  • section as used in the invention may also refer to a component as such of the impregnation container 6, in particular wherein the constituents are connected to one another and thus form the impregnation container 6 as a unit.
  • the production plant P has at least one first supply device 3 ', in particular in the form of a pipeline, preferably for feeding or for introducing the impregnating agent into the impregnation container 6, as shown in FIGS. 2A and 2B.
  • the first supply device 3 ' can be arranged in particular downstream of the first storage unit 1 or upstream of the impregnation container 6.
  • the first supply device 3 'can also connect the first storage unit 1 and the impregnation container 6 with each other.
  • first supply device 3 'at the upper end or the upper portion 6' of the impregnation container 6 can be connected to the impregnation container 6, in particular via a first insertion opening for the impregnation agent 1 1 of the impregnation container 6.
  • the production plant P can have at least one second feed device 3 ", in particular in the form of a pipeline or a conveyor belt or a screw conveyor, preferably for feeding or for introducing the activated carbon into the impregnation container 6.
  • the second Feeder 3 "in particular downstream of the second storage unit 2 and upstream of the impregnation container 6 may be arranged.
  • the second supply device 3" can be connected to the impregnation container 6 at the upper end or the upper section 6 'of the impregnation container 6, in particular via an insertion opening for activated carbon 1 1 of the impregnation container. 6
  • the first supply device 3 'or the second supply device 3 "thus generally serve to charge the impregnating device 4 or the impregnating container 6 with the starting materials in the form of the impregnating agent on the one hand and the activated carbon to be treated on the other hand 3 'and the second feeding device 3 ", independently, in particular to be connected to the subsequently described at least one insertion opening 1 1.
  • the production plant P as illustrated in FIGS. 2A and 2B, may have at least one first removal device 5 ', in particular in the form of a pipeline, preferably for discharging or discharging the liquid carrier medium of the impregnating agent or of any excess impregnating agent from the impregnation container 6, have.
  • the first discharge device 5 ' can be arranged downstream of the impregnation container 6.
  • the first discharge device 5 'at the lower end or at the lower portion 6' in particular via an outlet opening for the carrier or impregnating agent 12 of the impregnation 6 and / or a filter device 14 of the impregnation 6, or at the upper end or the upper section 6 "of the impregnating container 6 with the impregnating container 6, in particular via a further outlet opening 13 of the impregnating container 6.
  • the arrangement at the lower end or lower section 6 ' is particularly suitable when the carrier medium or container is used the excess impregnating agent in the respective liquid form is to be removed from the impregnation container 6.
  • the arrangement of the first removal device 5 'at the upper end or the upper portion 6' is particularly suitable when in particular the previously liquid carrier medium or Impregnating agent in gaseous form, ex For example, by evaporation, to be dissipated.
  • An arrangement at the upper end or the upper portion 6 ' is also considered when the liquid carrier medium or impregnating agent is to be aspirated so to speak from above from the impregnation container 6.
  • the first discharge device 5 ' may be in communication with the outlet opening 12 or the further outlet opening 13 which will be described below. For this purpose, reference may also be made to FIGS. 2A and 2B.
  • the production plant P at least a second discharge device 5 ", in particular in the form of a pipe or a conveyor belt or a screw conveyor, preferably in the form of a pipe, preferably for discharging or for discharging the impregnated Activated carbon from the impregnation container 6, in this connection, the second removal device 5 "can be arranged downstream of the impregnation container 6 or upstream of the receiving device 5.
  • the second discharge device 5 can connect the impregnation container 6 and the receiving device 5.
  • the second removal device 5" can be connected to the lower end or the lower portion 6 'of the impregnation container 6 may be connected to the impregnation container 6, in particular via an outlet opening for impregnated activated carbon 12.
  • the second discharge device 5 will be in connection with the discharge opening 12 described below.
  • the impregnation container 6 in particular the upper portion 6 'or the lower portion 6 ", at least substantially rotationally symmetrical and / or at least substantially hollow or by a wall
  • the longitudinal axis L of the impregnation container 6 represents, in particular, the axis of rotation of the rotation body.
  • the impregnation container 6, in particular the upper portion 6 ' have an at least substantially circular cross-section, preferably a circular or circular cross-section, in particular in the horizontal plane or in a plane perpendicular to the longitudinal axis L of the impregnation container 6.
  • the impregnation container 6, in particular the upper portion 6 'of the impregnation container 6, tapers in the direction of the upper end of the impregnation container 6.
  • the upper portion 6 'of the impregnation container 6 is frusto-conical or conical, as shown in Fig. 2B.
  • the upper section 6 'of the impregnating container 6 may be arched or hemispherical in shape.
  • the upper portion 6 ' may be formed, for example, as a dished lid or basket top.
  • the impregnation container 6, in particular the lower portion 6 " has an at least substantially round cross-section (cross-sectional shape), preferably a circular or circular cross-section, in particular in the horizontal plane or in a plane perpendicular to the longitudinal axis L of the impregnation container 6 (FIGS. 2A and 2B).
  • the impregnation container 6, in particular the lower portion 6 "of the impregnation container 6, taper towards the lower end of the impregnation container 6.
  • the lower portion 6 "of the impregnation container 6 is frusto-conical and / or conical.
  • the upper portion 6 'and the lower portion 6 are each formed in the shape of a straight truncated cone.
  • the Applicant has found in completely surprising manner that such a vote of the respective sections to each other to overall improved material yields with good impregnation due to an effective mixing of the components is present.
  • the upper section 6 'of the impregnation container 6 and the lower section 6 "of the impregnation container 6 have at least substantially surface-identical base surfaces (base surfaces) . This also leads to an optimum fit of the adjoining sections .
  • the base surfaces of the upper portion 6 'of the impregnation container 6 and of the lower portion 6 "of the impregnation container 6 are in each case material-free or open or formed by the respective jacket material of the upper portion 6' of the impregnation container 6 or of the lower portion 6" of FIG Impregnation container 6 bordered or formed edge. Accordingly, the respective sections 6 'and 6 "are hollow bodies with an open base area or base surface As shown in FIGS. 2A and 2B, according to the invention, in particular, the upper section 6' of the impregnation container 6 and the lower portion 6 "of the impregnation container 6 in the region of their bases abut each other or are arranged to each other. Consequently, the upper section 6 'and the lower section 6 "form a coherent hollow body, which in particular forms the reaction space, in the form of the impregnating container 6.
  • the ratio of the height hi of the upper portion 6 'of the impregnation container 6 and the height h 2 of the lower portion 6 "of the impregnation container 6 in the range of 2: 1 to 1: 5, in particular in the range of 1, 5: 1 to 1: 4, preferably in the range of 1: 1 to 1: 3, preferably in the range of 1: 1, 25 to 1: 2.
  • it is the distance between the respective top surface of the preferably frusto-conical sections 6 ', 6 "in the perpendicular direction to the respective base surface.
  • the impregnation container 6 is designed to be double conical or double frustoconical or in the form of a double cone or a double truncated cone. According to the invention, this is particularly the case in that the impregnation container 6 tapers in the direction of the lower end of the impregnation container 6 and in the direction of the upper end of the impregnation container 6, in particular in the shape of a cone or cone.
  • the impregnating device 4, in particular the impregnation container 6, preferably the wall (shell) or the housing of the impregnation container 6, can be heated, in particular directly or indirectly heated, preferably indirectly heated
  • the impregnating device 4, in particular the impregnating container 6, has at least one heating device 7, in particular for direct or indirect heating, preferably indirect heating.
  • the heating device 7 can preferably be positioned or arranged on the outside of the wall or the housing of the impregnating container 6.
  • the heating device 7 may also be part of the wall or of the housing of the impregnation container 6.
  • Figs. 2A and 2B reference may be made to Figs. 2A and 2B.
  • the term “indirect heating”, as used according to the invention, is understood in particular such that the heat required for heating the impregnating container 6 is generated, so to speak, directly in the heating device, as is the case, for example, in the case of an electrically operated heating device Case is. Accordingly, the term “indirect heating” as used according to the invention is to be understood as meaning that the heating device 7 or the impregnation container 6 is heated indirectly, in particular by using a heat-transporting heating or thermal medium which heats away from the heating device is and which, for example, supplied via corresponding leads of the heater and is led away via corresponding discharges from the heater for purposes of reheating in a remote from the impregnating device 4 arranged heating system or device.
  • the direct heating of the impregnating device 4, in particular of the impregnating container 6, takes place electrically.
  • the direct heating of the impregnating device 4, in particular of the impregnating container 6, can take place using at least one electric heating device 7, as described above.
  • heating cables or the like may be used.
  • the indirect heating of the impregnating device 4, in particular of the impregnating container 6, can take place using at least one heating or thermal medium, in particular at least one heating and / or thermal fluid.
  • the indirect heating of the impregnating device 4, in particular of the impregnating container 6, can take place by using at least one heating device 7 having at least one heating or thermal medium, in particular at least one heating and / or thermal fluid.
  • the heating or thermo-medium-carrying piping systems or casings can be used.
  • the wall or the housing of the impregnating container 6 is at least partially or double-walled, in particular for receiving the heating device 7 or for receiving or for flowing through at least one heating or thermal medium, in particular at least one heating or thermal fluid, in particular in the resulting space or in the cavity as such.
  • the wall or the housing of the impregnating container 6 is at least partially or double-walled, in particular for receiving the heating device 7 or for receiving or for flowing through at least one heating or thermal medium, in particular at least one heating or thermal fluid, in particular in the resulting space or in the cavity as such.
  • the impregnation container 6 is applied at least partially or partially to an outside on the wall or the housing of the impregnation container 6 or positioned thermal insulation device, in particular in the form of a foam or the like.
  • the impregnating device or the impregnating container 6 may moreover comprise at least one stirring or mixing device 8, in particular an agitating or mixing device 8 arranged or located at least partially or in sections, preferably at least substantially completely in the impregnating container 6, such as for example, in Fig. 2A and Fig. 2B.
  • the stirring or mixing device 8 is in particular designed such that it is used for all process steps (a) to (c) and for the optionally provided washing step against the background of ensuring effective mixing and uniform heating
  • the use of a special stirring or mixing device further improves the contacting of the activated carbon with the impregnating agent for the purpose of finishing with the impregnating component.
  • step (b) of the method according to the invention the targeted use of a stirring or mixing device means that the effectiveness of the drying can be increased, in particular because of the mixing and heating, the liquid carrier medium or optionally excess impregnating agent effectively from the impregnated activated carbon can be removed or removed, in particular by evaporation.
  • the use of a stirring or mixing device in the context of the thermal aftertreatment according to step (c) leads to a more uniform heating due to the mixing of the activated activated carbon, so that an overall improved or homogeneous activation of the material is present.
  • dead zones or rest zones in the impregnating device 4, in particular in the impregnating container 6, are avoided in an efficient manner.
  • the stirring or mixing device as shown in FIGS. 2A and 2B, a plurality of mixing elements (stirring elements) 9 has.
  • the stirring or mixing device 8 at least two mixing elements 9, in particular at least three mixing elements 9, preferably at least four mixing elements 9, preferably at least four mixing elements 9, preferably at least five mixing elements 9, more preferably at least six mixing elements 9, have.
  • the stirring or mixing device 8 has a total of 2 to 20 mixing elements 9, in particular 3 to 15 mixing elements. te 9, preferably 4 to 12 mixing elements 9, preferably 5 to 10 mixing elements 9, has.
  • the mixing elements 9, independently of one another are formed like a shovel, a paddle, a wing, and / or a bar.
  • the mixing elements 9 are formed, independently of one another, straight (straight) or curved, preferably straight (rectilinear), in particular with respect to the longitudinal extent of the mixing elements 9 (cf. 2A and 2B).
  • the mixing elements 9, independently of one another have an at least substantially round cross-section (cross-sectional shape), preferably a circular and / or circular cross-section, or a polygonal cross-section, preferably a polygonal cross-section.
  • the mixing elements 9, independently of one another have a triangular, quadrilateral or pentagonal shape, preferably a triangular cross section.
  • the mixing elements 9, independently of one another can have a cross section in the form of an equilateral or isosceles, in particular equilateral, triangle.
  • all mixing elements 9 of Rlick standing. Mixing device have the same shape or the same cross-section.
  • the concrete design of the size of the mixing elements 9 also plays an important role.
  • the mixing elements 9, independently of one another have a diameter or an edge length on the cross section, in the range of 5 mm to 100 mm, in particular 10 mm to 75 mm, preferably 15 mm to 50 mm.
  • the mixing elements 9, independently of each other are arranged such that the longest side of the cross section of the mixing elements 9, in particular the Hypotenuse of the cross section of the mixing elements 9 forming triangle, based on the other sides of the cross section of the mixing elements 9, is arranged below or positioned or arranged to the lower end of the impregnation container 6.
  • the mixing elements 9, independently of one another, can be arranged at least substantially horizontally or with an angle of attack in the range from 0 ° to 45 °.
  • the angle of attack is defined as the angle between the longest side of the cross section, in particular the lower side of the cross section, the respective mixing element 9 and the horizontal.
  • the mixing elements 9 have at least substantially the same cross-section or that the mixing elements 9 have at least substantially the same cross-sectional area or area or the same angle of attack.
  • the mixing elements 9 can also be designed in particular such that the ends of the respective mixing elements 9 are at least substantially equal to the wall or the housing of the impregnation container 6.
  • the mixing elements 9 are formed such that the respective ends of the mixing elements 9 follow the course of the wall or the housing of the impregnation container 6 with at least substantially constant or constant or the same spacing.
  • the mixing elements 9 are adapted to the geometry of the impregnation container 6, as shown in FIGS. 2A and 2B.
  • the ends of the mixing elements 9 directed or positioned towards the wall or the housing of the impregnating container 6 are to be understood.
  • the stirring or mixing device 8 is designed as an agitator, in particular a rotary agitator.
  • the stirring or mixing device 8 may have a stirring shaft (drive shaft) 10, as shown equally in FIGS.
  • the stirring shaft 10 may be arranged or positioned at least substantially parallel or along the longitudinal axis L of the impregnating container 6 in the impregnating container 6.
  • the stirring shaft 10 is arranged or positioned at least substantially centrally in the impregnating container 6. In this way, an optimal mixing and a constant spacing of the mixing elements to the housing wall of the impregnation container is ensured even during (rotary) operation of the stirring or mixing device.
  • the stirring shaft 10 may be formed as a rotation shaft, which rotates or rotates about its own axis in the application or operating state.
  • the stirring or mixing device 8 has at least one drive unit 10 ', in particular for preferably rotating drive of the stirring shaft 10.
  • the drive unit 10 is here in particular outside the impregnation container 6, preferably at the (upper) end of the rotary shaft 10.
  • the mixing elements 9 may be arranged or positioned radially on the agitator shaft 10, in particular extending radially along the agitator shaft 10 in each case.
  • the mixing elements 9 can be arranged or positioned along the agitator shaft 10 or the lengths of the mixing elements 9 can be designed such that the ends of the respective mixing elements 9 are at least substantially equidistant from the wall or the housing of the impregnation container 6.
  • the mixing elements 9 are arranged or positioned along the agitator shaft 10 or that the lengths of the mixing elements 9 are formed such that the ends of the respective mixing elements 9 the course of the wall or the housing of Impregnation container 6 with at least substantially constant spacing follow ( Figures 2A and 2B).
  • the spacing between the ends of the respective mixing elements 9 and the wall or housing of the impregnation container 6 is in the range from 0.2 cm to 15 cm, in particular in the range from 0.5 cm to 10 cm cm, preferably in the range of 1 cm to 8 cm, preferably in the range of 2 cm to 6 cm, particularly preferably in the range of 3 cm to 5 cm.
  • the spacing of the ends of the respective mixing elements 9 to the wall or the housing of the impregnation 6 in the range of 1/5 to 1/500, in particular in the range of 1/10 to 1/200, preferably in the range of 1 / 20th to 1/100, the maximum inner diameter of the impregnation container 6 are.
  • the above details are, in particular, the clear dimension between the respective mixing element 9 and the (inner) wall or the housing of the impregnation container 6.
  • the mixing elements 9 may be disposed along the agitator shaft 10.
  • the mixing elements 9 can be arranged along the agitator shaft 10 with at least substantially the same distance or at least substantially equidistantly from one another (cf. FIGS. 2A and 2B).
  • the mixing elements 9 succeeding each other along the agitator shaft 10 may be offset in the range of 0 ° to 360 °, in particular in the range of 45 ° to 315 °, preferably in the range of 90 ° to 270 °, preferably in the range of 135 ° to 225 °, in particular with respect to a plane perpendicular to the agitator shaft 10, be arranged or positioned relative to one another.
  • the mixing elements 9 succeeding each other along the agitator shaft 10 can be arranged with an offset of at least 45 °, in particular of at least 90 °, preferably of at least 135 °, preferably of at least 180 °, in particular with respect to a plane perpendicular to the agitator shaft 10 be positioned.
  • the mixing elements 9 are formed or positioned or positioned along the agitator shaft 10 in such a way that mixing or transport of the impregnating agent or the activated carbon in the operating or application state axial or radial direction, in particular in the axial and radial directions, is present or takes place.
  • the stirring or mixing device 8, in particular the mixing elements 9 or the agitator shaft 10 is hollow or present as a hollow body.
  • the mixing or mixing device 8, in particular the mixing elements 9 or the stirring shaft 10 have or consist of a hollow profile.
  • the heatability of the stirring or mixing device 8, in particular of the mixing elements 9 and the agitator shaft 10, is associated with the central advantage that in an appropriate manner an additional heat input into the impregnation 6 for purposes of heating the components located in the impregnation 6 can, so that the material in the impregnation 6 located material is heated so to speak from the inside out.
  • the concomitant homogenization of the heating and the higher input of heat energy, in particular the drying or activation times and the total energy costs can be reduced, which due to the homogeneity of the heating also improved overall impregnation results are obtained, including what the subsequent downstream activation As far as the previously impregnated activated carbon is concerned.
  • the stirring or mixing device has at least one heating device, in particular for direct or indirect heating, preferably indirect heating.
  • the heating device can preferably be positioned on the inside in the stirring or mixing device 8, in particular in the mixing elements 9 and / or the stirring shaft 10 and / or in the cavity of the mixing elements 9 and / or in the cavity of the stirring shaft 10. be arranged.
  • the direct heating of the stirring or mixing device 8, in particular of the mixing elements 9 or of the stirring shaft 10, takes place electrically.
  • the direct heating of the stirring or mixing device 8, in particular of the mixing elements 9 or the stirring shaft 10 can take place using at least one electric heating device.
  • the stirring or mixing device 8, in particular the mixing elements 9 and the stirring shaft 10 are indirectly heated:
  • the indirect heating of the stirring or Mixing device 8 using at least one heating and / or thermal medium, in particular at least one heating and / or thermal fluid takes place.
  • the indirect heating of the stirring or mixing device 8, in particular of the mixing elements 9 or of the stirring shaft 10 can take place using at least one heating medium or thermal medium.
  • the heating or thermal medium, in particular the heating or thermal fluid, in the cavity of the stirring or mixing device 8, in particular in the cavity of the mixing elements 9 and the stirring shaft 10, be introduced or flow through this.
  • corresponding external heating devices such as heating burners or the like
  • corresponding supply lines and outlets and corresponding pumping devices can be used.
  • the impregnation container 6 preferably the wall (shell) or the housing of the impregnation container 6, on the one hand and the stirring or mixing device, in particular, behave like this 8, in particular the mixing elements 9 and the stirring shaft 10, on the other hand heated, in particular directly or indirectly heated, preferably indirectly heated, are formed.
  • the impregnating device 4, in particular the impregnating container 6, has at least one insertion opening 11, in particular for introducing the impregnating agent or the activated carbon.
  • the insertion opening 1 1 can be arranged or positioned at the upper end or in the region of the upper portion 6 'of the impregnation container 6.
  • the impregnation device 4, in particular the impregnation container 6, can have at least one outlet opening 12, in particular for removing or draining liquid carrier medium or any excess impregnating agent or impregnated activated carbon or a washing medium.
  • the outlet opening 12 can be arranged or positioned at the lower end or in the region of the lower section 6 "of the impregnating container 6.
  • the impregnating device 4, in particular the impregnating container 6, at least one further outlet opening 13 in particular for removing in particular gaseous substances or media (for example, previously transferred by heating in the gas phase liquid carrier medium) or for removing or discharging liquid carrier medium or any excess impregnating agent.
  • the further outlet opening 13 can be arranged or positioned at the upper end or in the region of the upper section 6 'of the impregnating container 6.
  • the further outlet opening 13 can have a pipeline extending into the region of the lower section 6 "of the impregnating container 6, in particular for removing, preferably aspirating, any excess impregnating agent This will further reduce the loss of activated carbon.
  • the filter device 14 may be formed in a sieve.
  • the filter device 14 may be part of the outlet device 12 or of the further outlet device 13.
  • the following invention also relates, according to a further aspect of the present invention, also to the use of the production plant according to the invention, preferably as defined above, in particular for equipping an activated carbon having a reactive or catalytic activity, in particular for carrying out the previously mentioned process according to the invention.
  • Another object of the present invention is also - according to yet another aspect of the present invention - also an impregnating device as such, which has in particular at least one impregnating reactor, for impregnating an activated carbon, in particular for equipping an activated carbon with reactive or catalytic activity, in particular to carry out the method according to the invention described above, as also described in the relevant device claims and reproduced in the relevant figure representations.
  • the impregnating device 4 is in particular designed such that
  • (C) optionally a thermal aftertreatment of the resulting impregnated activated carbon, in particular for the activation and / or further fixing of the impregnating component, preferably under the effect of heat and / or heating;
  • the impregnating device 4 has at least one impregnating container 6, in particular as defined above.
  • the comments on the further aspects of the present invention and to the corresponding representations according to FIG. 1 and FIGS. 2A and 2B are also be made to the comments on the further aspects of the present invention and to the corresponding representations according to FIG. 1 and FIGS. 2A and 2B.
  • the present invention also relates to the impregnated activated carbon obtainable by the process according to the invention described above, in particular activated carbon having reactive or catalytic activity, which is obtained by the process described above is obtained or obtained according to the invention.
  • the activated carbon according to the invention has a particularly high loading quantity of the impregnating component or of the catalytically active components with at the same time homogeneous formation of the impregnation.
  • the activated carbons according to the invention have an improved and more uniform surface structure due to the very special process control, namely, that is, with a single common device, since there is less abrasion or breakage of material due to the lower mechanical stress. Accordingly, the activated carbons according to the invention have outstanding adsorptive properties combined with a uniform geometry, which improves, for example, the flow through behavior in filter applications or the like.
  • the present invention is based on the idea of providing a production plant or a device within the scope of the process according to the invention which is capable of producing the porous solids in the form of activated carbon, which in particular is in suspension within the scope of the process according to the invention
  • Base of the activated carbon on the one hand and the impregnating agent On the other hand, not only to impregnate, but also to dry and, if necessary, to thermally post-treat.
  • the Applicant has found, in a completely surprising manner, that the above-mentioned process steps and, if appropriate, further process steps carried out in the context of the present invention can be carried out in a special impregnation device, in particular based on an impregnation vessel or stirred reactor. which in this context, as stated below, has a special physical shape or geometry of the housing or of the agitator used in this respect.
  • the impregnating device provided according to the invention is thus suitable for impregnating, drying and modifying (for example activating) porous solids in the form of particulate activated carbon, the impregnating device in particular depending on the ratio between impregnating agent on the one hand and activated carbon used according to the invention both in a liquid and solid Phase as well as in all transitional phase can be operated, as they may occur, for example, in the drying of the impregnated activated carbon (humid condition).
  • the impregnating device used according to the invention for example in the form of a special stirred reactor, is suitable for impregnating and drying the particulate activated carbon used and to be impregnated, but also for its thermal aftertreatment, if required or desired in particular for purposes of activating or fixing the impregnating component.
  • an impregnating device which combines the basic procedural operations based on the preparation of a suspension (bringing the activated carbon into contact with the impregnating agent with respect thereto, subsequently removing the liquid carrier medium of the impregnating agent or excess impregnating agent or impregnating solution, Drying and optionally final thermal aftertreatment of the impregnated activated carbon) in a single apparatus allows.
  • the impregnating device can be operated both in the fluid phase and in the solid phase.
  • step (a) with the contacting and the present suspension of the activated carbon in the impregnating agent is carried out at least substantially completely in the fluid phase.
  • step (b) with the removal of the liquid carrier medium of As far as the impregnating agent or any excess impregnating agent is concerned it may be carried out at least partly in the fluid phase and at least partly in the solid phase (after drying), with the optionally carried out drying.
  • step (b) can also be carried out in an earth-moist phase or in the earth-moist state of the impregnated activated carbon.
  • step (c) with the performed thermal aftertreatment of the impregnated activated carbon so this step can be operated or carried out in particular completely in the solid phase of the impregnated activated carbon.
  • the impregnating device in particular the impregnating container or the impregnating vessel, can thus be operated during step (a) up to the drying of the earth-moist impregnated activated carbon in step (b), in particular in the fluid phase.
  • the operating state is left with the fluid phase of the impregnating, in which case in particular a (dried) solid in the form of the impregnated activated carbon in the Impregnating device is moved.
  • the impregnating device due to a purposeful geometric adaptation or design of the impregnating device with the additionally present special stirring or mixing device to take into account the respective requirements with respect to the operating modes mentioned.
  • the impregnating device used according to the invention which may be in the form of a stirred tank in particular, it is, as stated above, hollow, preferably with a housing tapering towards the lower end or with a lower one End tapered wall equipped, this (s) in particular coconus or frusto-conical shape is formed with a defined angle.
  • this ensures, in particular, that the solid present in the dry phase in the form of the impregnated activated carbon (ie in particular after drying in step (b) or within the optionally provided thermal aftertreatment according to step (c) is free-flowing
  • This basis is at least substantially complete emptying of the impregnating device in relation to the dried and optionally nachle treated impregnated activated carbon to ensure, which is taken in particular at the lower end of the impregnating device.
  • the mixing or stirring device provided according to the invention can be used both in the liquid and in the solid phase and in the corresponding transitional forms.
  • the mixing or agitator used according to the invention is capable both of the liquid suspension present in particular in step (a) and of the earth-moist phase up to the dry solid according to steps (b) and (c), to ensure effective radial and axial mixing of the components.
  • the impregnating device provided according to the invention also particularly takes into account the removal of the liquid carrier medium of the impregnating agent or of any excess impregnating agent provided in step (b).
  • the liquid medium can thus be effectively removed from the impregnating device, for which purpose the procedure is also used can that the impregnation device is operated in a slight overpressure, so to speak, so to speak, which push out the liquid medium or the impregnating solution from the kettle, accompanied by a further reduction of the time required.
  • a solids filter with a corresponding removal or drainage possibility can be provided at the lowest or lowest point of the impregnation device or the impregnation container.
  • the filter used in particular solid filter, is designed to be flushed, for example using nitrogen. In this way, the emergence of a dense and less permeable activated carbon layer or an undesirable activated charcoal discharge can be avoided in the removal or release of the liquid medium.
  • the removal of the liquid carrier medium of the impregnating agent or of any excess impregnating agent it is in particular such that the suspension or the activated carbon remaining in the impregnating device, so to speak with increasing removal of the liquid constituents, in particular in step ( b) is increasingly moist with earth, this earth-moist composition is equally effectively mixed or mixed by the stirring or mixing device provided according to the invention, as stated above.
  • any larger conglomerates of the activated carbon which may occur are moved so that they continuously decompose, possibly accompanied by a renewed agglomeration and subsequent disintegration, which leads to an effective thorough mixing as well leads to an effective discharge of residual moisture.
  • the impregnating device as such and the (rotating) stirring or (rotating) mixing device used in this regard can be designed to be heatable.
  • a heatable stirrer can preferably be used with mixing elements designed in the form of a delta profile.
  • the heatability of the stirring or mixing device increases the sustainable (total) heating surface and thus reduces the necessary drying time of the impregnated activated carbon.
  • a particularly effective mixing is achieved both by the shape of the mixing elements and against the background that the length of the mixing elements or the relevant stirring arms are adapted to the reactor geometry or the geometry of the impregnating device. This leads to a maximum mixing.
  • the impregnating device used also tapers towards its upper end, wherein a conical shape or a configuration in the form of a truncated cone can be provided in this respect.
  • a conical shape or a configuration in the form of a truncated cone can be provided in this respect.
  • activated carbons impregnated by the applicant or equipped with a reactive or catalytic activity are prepared on the basis of the process according to the invention and corresponding comparative processes:
  • a corresponding impregnating device in a production plant as shown in FIG. 2B, a corresponding impregnating device is moved, wherein the impregnating device contains a stirring or mixing device.
  • the device used according to the invention and the relevant mixing or mixing device can be heated, for which purpose a corresponding heating fluid is used.
  • the catalytically active component used is copper based on copper nitrate (Cu (NO 3) 2 ).
  • the activated carbon used is a particulate or spherical activated carbon in the form of a polymer-based spherical activated carbon (PBSAC).
  • PBSAC polymer-based spherical activated carbon
  • the amount of particulate activated carbon used is 250 kg.
  • 80 kg of the impregnating component in the form of Cu (N03) 2 * 2.5 H 2 0 are also dissolved in 500 l of deionized water.
  • the activated carbon on the one hand and the impregnating agent on the other hand are introduced with stirring into the impregnating device.
  • the contacting of the activated carbon in the form of the plurality of discrete activated carbon particles with the impregnating agent in the form of the relevant solution or dispersion with the corresponding impregnating and the accompanying equipment or impregnation of the activated carbon with the impregnating component is in the device at a temperature of 20 ° C under Stirring (number of revolutions or stirrer speed about 5 to 10 revolutions per minute (rpm)) carried out for a period of 10 hours.
  • the liquid carrier medium (water) or excess impregnating agent is removed via a corresponding filter device.
  • the liquid carrier medium or the excess impregnating agent is discharged via a corresponding outlet opening.
  • both the impregnating device as such and the stirring or mixing device with the relevant mixing arms using a Thermal oil which is pumped through the hollow stirring or mixing device or through the intermediate space of the partially double-walled impregnation, are heated to a temperature of about 150 ° C.
  • the impregnated activated carbon is dried by evaporation, in particular of the remaining liquid carrier medium in the impregnating device.
  • the occurring gases are thereby removed by a corresponding outlet opening at the upper end of the impregnating device.
  • the drying is likewise carried out with stirring.
  • the result is an impregnated activated carbon having a residual moisture of 15 wt .-% to 20 wt .-%, based on the impregnated activated carbon.
  • the dried impregnated activated carbon is then subjected to a thermal after-treatment in the same impregnating device for purposes of activation or further fixing of the impregnating component, for which purpose the impregnating device and the stirring or mixing device are heated to a temperature of about 200 ° C. Activation is carried out with continued stirring for a period of about one hour.
  • the result is a first active carbon according to the invention A, which is removed after cooling by a corresponding outlet opening of the impregnating device.
  • washing solution is prepared from 85 l of a 50% NaOH solution and about 500 l of deionized water.
  • the washing solution is likewise introduced with stirring into the impregnating device.
  • the washing step is carried out at a temperature of 20 ° C with continuous stirring for a period of 15 minutes.
  • Example 3 the washing medium or the washing solution is discharged at the lower end of the impregnating device via a corresponding outlet opening.
  • a renewed drying of the impregnated and washed activated carbon is carried out, namely at a temperature of 150 ° C. (heating of the impregnating container and of the mixing or mixing device); the duration of drying This is equal to two hours.
  • the resulting activated carbon B according to the invention is removed from the impregnating device.
  • an impregnated activated carbon is prepared based on a comparison process.
  • the procedure is basically as described in Example 1), but with the proviso that the respective steps of contacting, removing the liquid carrier medium or excess impregnating agent or the drying of the impregnated activated carbon and beyond the thermal aftertreatment or Activation of the impregnated activated carbon are carried out in separate, separate devices.
  • a corresponding impregnating device in the form of a simple unheated stirred tank is first used. Drying takes place in a separate drying oven. The final thermal aftertreatment continues to take place in an activation furnace, wherein the activated carbon to be treated or impregnated is transferred to the respectively subsequent device after completion of the respective process step.
  • a corresponding comparative activated carbon C results.
  • a further comparative activated carbon is prepared, wherein the procedure is as described above under Example 3.) in separate or separate devices.
  • the impregnated activated carbon is removed from the drying oven and transferred to a separate washing device in addition to the process procedure according to Example 3.) in such a way as in Example 2.) described washing process in the separate washing device is performed.
  • the washed activated carbon is transferred again after removal of the washing medium in the drying oven and subjected to drying.
  • a comparison of the procedures described previously in Examples 1) to 4) shows that the method according to Example 3 with the implementation in separate or separate devices in comparison to the inventive method according to Example 1) with a 75% increased energy input associated goes; In addition, the time required compared to Example 1) is increased by 55%.
  • a corresponding comparison of the process described in Example 4) with the additional washing step for the process according to Example 2) according to the invention also shows that the process according to Example 4) is accompanied by an energy input increased by more than 92%; In addition, the time required compared to example 2) is increased by more than 65%.
  • Further comparison of the activated carbon A obtained according to the method in Example 1) with that according to the method Activated carbon B obtained according to Example 2) shows that activated carbon B has less impurities and in particular less incrustations on the surface of the particles, activated carbon B being also superior to activated carbon D according to Example 4) in this respect.
  • activated carbon D has better surface properties than activated carbon C according to Example 3
  • the properties in question are at best only slightly improved in comparison with the activated carbon A according to the invention, despite the washing step carried out in addition.
  • activated carbon C by far the most impurities or encrustations.
  • the present embodiments and investigations show overall that within the scope of the present invention an efficient process is provided with a relevant impregnating device, which leads to a significant increase in efficiency compared with the respective comparative examples with simultaneous improvement of the obtained impregnated activated carbon.
  • I storage unit (receiving / storing impregnating agent)

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un procédé d'imprégnation d'un charbon actif, en particulier pour conférer à un charbon actif une activé réactionnelle et/ou catalytique, ainsi qu'une installation de production et plus précisément un dispositif d'imprégnation permettant la mise en oeuvre (5) de ce procédé.
EP16781321.1A 2015-12-22 2016-10-04 Dispositif et procédé de modification de matières solides poreuses Pending EP3393646A1 (fr)

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DE102015016686 2015-12-22
DE102016101213.0A DE102016101213A1 (de) 2015-12-22 2016-01-25 Vorrichtung und Verfahren zur Modifizierung poröser Feststoffe
PCT/EP2016/073623 WO2017108219A1 (fr) 2015-12-22 2016-10-04 Dispositif et procédé de modification de matières solides poreuses

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CN107486148B (zh) * 2017-08-01 2020-03-31 上海纳米技术及应用国家工程研究中心有限公司 一种铌改性活性炭制备方法及其产品和应用
WO2020010106A1 (fr) * 2018-07-02 2020-01-09 Marion Process Solutions, Inc. Mélangeur conique
CN109336108B (zh) * 2018-11-30 2020-07-31 七道水（厦门）环保科技有限公司 一种净水活性炭及其制备方法
CN112705272A (zh) * 2019-10-25 2021-04-27 中国石油化工股份有限公司 催化剂浸渍塔、浸渍设备和浸渍方法
CN111185112A (zh) * 2020-01-15 2020-05-22 常熟市环境试验设备有限公司 一种具有加热效果的搅拌装置
CN115385334B (zh) * 2022-09-12 2024-04-26 南京正森环保科技有限公司 一种活性炭加工方法

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DE102016101213A1 (de) 2017-06-22
WO2017108219A1 (fr) 2017-06-29

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