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WO2013082342A2 - Appareil et procédé d'activation de charbon à l'aide d'un four périodique à chambres multiples - Google Patents

Appareil et procédé d'activation de charbon à l'aide d'un four périodique à chambres multiples Download PDF

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Publication number
WO2013082342A2
WO2013082342A2 PCT/US2012/067170 US2012067170W WO2013082342A2 WO 2013082342 A2 WO2013082342 A2 WO 2013082342A2 US 2012067170 W US2012067170 W US 2012067170W WO 2013082342 A2 WO2013082342 A2 WO 2013082342A2
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Prior art keywords
chamber
tray
inter
door
temperature
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.)
Ceased
Application number
PCT/US2012/067170
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English (en)
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WO2013082342A3 (fr
Inventor
James G Fagan
Edward T O'MARA
Milton T SIMPSON
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Corning Inc
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Corning Inc
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Publication of WO2013082342A2 publication Critical patent/WO2013082342A2/fr
Publication of WO2013082342A3 publication Critical patent/WO2013082342A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C01B32/312—Preparation
    • C01B32/336—Preparation characterised by gaseous activating agents
    • 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
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • 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
    • C01B32/39—Apparatus for the preparation thereof

Definitions

  • the present specification generally relates to manufacture of activated carbon and, more specifically, to apparatus and methods of carbon activation using a multi-chamber periodic furnace.
  • Activated carbon is useful in the manufacture of various articles such as energy storage devices. Electrical energy storage is needed in many applications, such as electric/hybrid vehicles, portable electronic devices, and power systems. Batteries of various kinds have been used for most applications. In recent years, electrochemical double layer capacitors (EDLCs, a.k.a. ultracapacitors or supercapacitors) have emerged as an alternative to batteries in applications that require high power and long shelf and cycle life. Energy storage in an EDLC is achieved by separating and storing electrical charges in the electrochemical double layer at the interface between a solid surface and an electrolyte. Activated carbon (or active carbon) can be used in EDLCs thanks to its very large surface area, good electrical and ionic conductivity, excellent chemical stability, and low cost.
  • a method of manufacturing activated carbon material comprising: providing a multi-chamber furnace having: interior walls defining first, second, and third chambers, a first exterior door disposed at a first end of the first chamber, a first inter-chamber door separating a second end of the first chamber and a first end of the second chamber, a second inter-chamber door separating a second end of the second chamber and a first end of the third chamber, and a second exterior door disposed at a second end of the third chamber; disposing a first tray containing a first carbon activation batch mixture in the first chamber, and, in a first phase for the first tray: maintaining the first exterior door and first inter-chamber door in respective closed positions, and exposing the first tray to a first inert environment, wherein the temperature of the first inert environment is increased to a first maximum temperature between 300 and 450°C, and in some embodiments between 350 and 450 °C, then disposing the first tray
  • Liquid water may also be introduced into the third chamber, for example when lower temperatures are present in the third inert environment, e.g. below 100 °C.
  • a tray carriage conveyance system for translation of the tray into and out of chambers can help provide full, or near full, door sealing.
  • a second tray is disposed in the third chamber and, in a first phase for the second tray, the method further comprises: maintaining the second inter-chamber door and the second exterior door in respective closed positions, and exposing the second tray to a first inert environment, wherein the temperature of the first inert environment is increased to a first maximum temperature between 300 and 450°C, and in some embodiments between 350 and 450 °C; then, disposing the second tray in the second chamber and, in a second phase for the second tray, maintaining the first and second inter-chamber doors in respective closed positions, and exposing the second tray to a second inert environment wherein the temperature of the second inert environment is increased to a second maximum temperature between 600 and 1000 °C whereby the at least a portion of the first carbon activation batch mixture is converted into activated carbon; then disposing the second tray in the first chamber and, in a third phase for the second tray, maintaining the first inter- chamber door and the first exterior door in respective closed positions,
  • Liquid water may be introduced into the third chamber when lower temperatures are present in the third inert environment, e.g. below 100 °C.
  • the second tray is in the second chamber.
  • the first tray is in the first chamber
  • the second tray is in the third chamber.
  • the first and second trays occupy the second chamber simultaneously.
  • a multi-chamber furnace for manufacturing activated carbon material comprising: interior walls defining first, second, and third chambers, the interior walls in some embodiments, being metal lined, such as the interior walls defining the first and third chambers; first, second, and third inlet valves configured to provide inert gas to the first, second, and third chambers, respectively; first, second, and third heaters configured to heat the first, second, and third chambers, respectively, wherein the first and third inlet valves are capable of providing water vapor to the first and third chambers, respectively; a first exterior door disposed at a first end of the first chamber; a first inter- chamber door separating a second end of the first chamber and a first end of the second chamber; a second inter-chamber door separating a second end of the second chamber and a first end of the third chamber; and a second exterior door disposed at a second end of the third chamber; wherein the first exterior door and first inter-chamber door are capable of providing water vapor to the first and third chambers, respectively
  • FIG. 1 schematically illustrates an embodiment of a multi-chamber furnace as disclosed herein for manufacturing activated carbon material.
  • FIG. 2 schematically illustrates a cross-sectional view of one of the chambers of a multi-chamber furnace as disclosed herein.
  • FIG. 3 illustrates an embodiment of a stackable tray.
  • FIG. 4 shows a schematic side view of a tray stack comprised of a plurality of stackable trays.
  • FIG. 5 shows a schematic perspective view of the tray stack of FIG. 4.
  • FIG. 6 schematically illustrates an embodiment of a multi-chamber furnace configured to accept activation mix from either end of the furnace, i.e., a bi-directional furnace comprising a dual purpose end chamber configuration.
  • FIG. 7 schematically illustrates a top view of one embodiment of a stack configuration comprising an open space that facilitates the flow or distribution of gas or liquid throughout the tray stacks.
  • FIG. 8 schematically illustrates a top view of another embodiment of a stack configuration comprising two open spaces that facilitate the flow or distribution of gas or liquid throughout the tray stacks.
  • FIG. 9 schematically illustrates a cutaway end view of one of the furnace chambers showing a recirculation fan, heating tubes, and a tray carriage carrying at least three tray stacks.
  • FIG. 10 schematically illustrates a cutaway end view of one of the furnace chambers, the bottom of the tray carriage adapted to engage a bottom tray carriage conveyance mechanism which is part of a tray carriage conveyance system to transport the tray carriage into and out of the chamber.
  • FIG. 11 schematically illustrates a cutaway end view of one of the furnace chambers showing a side tray carriage conveyance mechanism.
  • FIGS. 12-14 schematically illustrate cutaway side views of two chambers of a furnace, showing a sequence of transport of a tray carriage through the two chambers.
  • Activated carbon can be synthesized by carbonizing a carbonaceous precursor in an inert atmosphere (e.g. N2 or Ar) at a high temperature (in this context, hundreds of degrees Celsius) followed by physical (such as by using C0 2 or steam) or chemical (such as by using KOH, K2CO3, NaOH, Na 2 C0 3 , A1C1 3 , ZnCl 2 , MgCl 2 , or H3PO4, etc.) activation.
  • Precursors include natural materials such as coals, nut shells, woods, biomass, non-lignocellulosic sources (e.g. wheat flour, cornmeal, corn starch etc.)8, and synthetic materials like polymers such as phenolic resin,9-l 1 poly( vinyl alcohol) (PVA),12 polyacrylonitrile (PAN), 10.
  • FIG. 1 schematically illustrates an embodiment of a multi-chamber furnace 5 as disclosed herein for manufacturing activated carbon material.
  • the multi-chamber furnace 5 comprises first, second, and third chambers 10, 20, 30.
  • Inlet valves 40, 50, 60 are configured to provide inert gas to the three chambers 10, 20, 30, respectively.
  • the first and third inlet valves 40, 60 are also capable of providing water vapor to the first and third chambers 10, 30, or separate additional inlet valves are configured to provide steam or water vapor to the first and third chambers 10, 30.
  • the first and third inlet valves 40, 60 may also be capable of providing liquid water to the first and third chambers 10, 30, or separate inlet valves can be configured to provide liquid water to the first and third chambers 10, 30. Water may be introduced into the second chamber for cleaning purposes when no product material is being processed and the furnace chambers are cooled to room temperature or near room
  • a first exterior door 70 is disposed at a first end 110 of the first chamber 10.
  • a first inter-chamber door 80 separates a second end 120 of the first chamber 10 and a first end 130 of the second chamber 20.
  • a second inter-chamber door 90 separates a second end 140 of the second chamber 20 and a first end 150 of the third chamber 30.
  • a second exterior door 100 is disposed at a second end 160 of the third chamber 30.
  • the first exterior door 70 and first inter-chamber door 80 are capable of being closed to substantially seal the first chamber 10.
  • the first and second inter-chamber doors 80, 90 are capable of being closed to
  • the second inter-chamber door 90 and the second exterior door 100 are capable of being closed to substantially seal the third chamber 30.
  • One or more recirculation fans can be disposed in one or more of the chambers 10, 20, 30.
  • the interior walls that define the first, second, and third chambers 10, 20, 30 may be metal lined.
  • the metal lined walls forming the chambers can provide capability for faster heating and cooling capability than that attainable with traditional refractory ceramic walls, with the added benefit of being more durable for the hydration and cleaning environments envisioned, in the processing of chemically activated carbon, for example with alkali salts.
  • Metals for such liners can include Ni, or alloys of nickel, as well as stainless steels such as 310 stainless steel or 330 stainless steel.
  • the interior walls that define the second chamber 20 may be refractory ceramic lined, where the second chamber is not exposed to excessive water (liquid, vapor, steam), for example owing to the ability to shut the first and second inter-chamber doors 80 and 90 such that a complete, or nearly complete, seal is formed around the doors, thereby sealing off the second chamber.
  • Activation mix carbon or carbon precursor material
  • FIG. 2 schematically illustrates a cross-sectional end view of one of the chambers of the multi- chamber furnace 5 as disclosed herein such as chamber 10, showing heaters 42 and
  • FIG. 1 One set of embodiments of a process disclosed herein for manufacturing activated carbon material can be described with reference to FIG. 1.
  • pre-heating of the activation mix can occur.
  • One or more trays, preferably one or more stackable trays400containing activation mix are loaded onto a tray carriage 400 , which is then moved into the first chamber 10 which serves as a preheat chamber.
  • FIG. 2 schematically shows one exemplary embodiment of a tray carriage 400 comprised of a tray rack 410 and a plurality of rollers or wheels 420 disposed on the bottom of the tray rack 410.
  • a tray stack 500 is shown disposed on top of the tray rack 410 of the tray carriage 400.
  • FIG. 3 illustrates an
  • FIG. 4 shows a schematic side view of a tray stack 500 comprised of 6 stackable trays 510, i.e. a plurality of stackable trays.
  • FIG. 5 shows a schematic perspective view of the tray stack 500 of FIG. 4. As seen in FIG.
  • one or more open spaces 560 above or near the tray liners 530 allows the tray contents to become exposed to gases or liquids during processing.
  • Gas tight chamber doors 70, 80 are closed and inert gas (such as N 2 ) is cycled through the chamber 10 at a volume exchange rate of 0.1 to 20 volume exchanges per hour. Heating can be started once the O 2 content in the first chamber 10 is less than about 1%. Heating is conducted at rates up to 400C/hr or more to a maximum
  • the temperature in the chamber 10 is held for a period of time (in some embodiments, 10 to 60 minutes) to allow equilibration and mix material dehydration and gas removal from the mix.
  • the use of gas recirculation can be employed in the chamber to improve heating rate and uniformity throughout the load.
  • Internal fan recirculation and or external gas recirculation can be employed.
  • the tray stack 510 on tray carriage 400 is passed into the second chamber 20 for a high temperature soak at a temperature of about 400C.
  • the chamber doors 80, 90 are closed, and an inert gas is fed into the chamber 20 at volume exchange rate of 0.1 to 20/hr.
  • the second chamber 20 is heated at a rate of 100 to 400C/hr to a maximum temperature of up to 850C for a 2 to 4 fir soak.
  • This second chamber 20, or high temperature heat soak chamber can be refractory insulated with a replaceable interior metal lining to minimize refractory exposure to high temperature corrosion.
  • Recirculation fans 41 can be disposed in this chamber to aid thermal uniformity, for example to achieve less than 20C maximum
  • the third chamber Prior and during transfer of the tray stack 510 to the third chamber, the third chamber is held at 400C under an inert atmosphere.
  • the chamber doors 90, 100 are closed and cooling to a temperature of less than 200 °C within the third chamber 30 commences, in some cases at about 200-400C/hr.
  • a temperature of, for example, lOOC can be targeted where the product is held at this temperature while being exposed to water vapor within a nitrogen sweep gas entering the third chamber 30.
  • the sweep gas flow rate for the third chamber 30 can be about 0.1 to 20 volume exchanges, although the rate may vary depending on whether just cooling or hydration is taking place. Hydration is allowed to occur over a long enough period of time to ensure thorough hydration in the bulk material within the trays as well as within the interior of the third furnace chamber 30 and the tray stack(s), in some cases from 1 to 10 firs. Gas recirculation can be employed in the third chamber 30 to enhance the cooling rate. Upon completion of hydration, the contents of the stacked tray(s) 510 are cooled further, with or without the presence of water vapor.
  • Liquid water may also be injected into the furnace trays 510 and third chamber 30 during this portion of the cycle to ensure more complete hydration at an appropriate temperature, e.g. less than lOOC. In some cases, cooling to less than 70C is sufficient, and in other cases, cooling to lower temperatures, such as less than 50C, may be conducted.
  • the exterior chamber door 100 is opened, and the tray carriage 400 with tray(s) 510 (or tray stack(s) 500) is removed from the third chamber 30.
  • total cycle time for this process operation can be up to 12 hours.
  • the adjoining chamber Upon completion of each cycle in a given chamber, the adjoining chamber will preferably be in the process of preparation to receive another tray carriage 400 either by heating, cooling or gas purging or conducting a process cycle on one or more tray stack(s) 500. In this way this embodiment will allow for a continuous cycling of tray stacks 500 such that a maximum number of two tray carriages 400 can be completed in one day for the maximum cycle times noted above.
  • a multi-chamber furnace 205 is configured to accept activation mix from either end of the furnace, i.e. a dual purpose end chamber configuration. That is, the first, second and third chambers 10, 20, 30 can operate in the same manner as in the first set of process embodiments for each of their individual process cycles, but in the second set of process embodiments, a tray carriage 400 can enter (and exit) the high temperature soak of the second chamber 20 from two opposite directions. Thus in some embodiments, through-put rates greater than tray carriages 400 can be processed in one day. Such configuration offers greater through-put with similar type furnace construction as the embodiment illustrated in FIG. 1, particularly if the hydration is the longest phase of the process operation.
  • the tray design such as shown in FIGS. 3-5 and stack configuration designs such as shown in FIGS. 7-8 provide for ready exposure of the material in the tray 510 for hydration via water vapor, steam or water as well as venting of gases from the process material during activation processing.
  • FIGS. 3-5 and stack configuration designs such as shown in FIGS. 7-8 provide for ready exposure of the material in the tray 510 for hydration via water vapor, steam or water as well as venting of gases from the process material during activation processing.
  • FIG. 7-8 schematically illustrate two exemplary stack configurations, respectively 600, 650, on a rack or carriage 400 with open spaces, 610, 660, respectively, which provide locations to align with piping, for example thereabove, inside a chamber once the rack 400 is fully deployed inside a chamber, for distribution of hydration media (steam, water vapor, or liquid water) en masse throughout the tray stack height, and which provide means to more uniformly distribute process gases throughout the stack 500 and the furnace chamber 10, 20, 30 effectively within a shorter period of time as the distribution will no longer rely on distribution of gases that occur solely due to overall gas volume exchanges.
  • hydration media steam, water vapor, or liquid water
  • an open space 610 is provided which is not occupied by a tray stack (an "unoccupied tray stack space") such that at least two adjacent-facing tray stacks 500 are separated by a distance of greater than the length (or a distance of greater than the width) of a tray stack 500.
  • an unoccupied tray stack space such that at least two adjacent-facing tray stacks 500 are separated by a distance of greater than the length (or a distance of greater than the width) of a tray stack 500.
  • two pairs of adjacent-facing tray stacks 500 are separated by a distance of greater than the length or width of a tray stack 500.
  • a (partial) open space can be provided which is occupied by a tray stack which is shorter than one or more of the other tray stacks on the rack at the time, such that at least portions of two adjacent-facing tray stacks are separated by a distance of greater than the length or width of a tray stack.
  • FIG. 8 schematically illustrates 14 tray stacks 500 disposed on top of a tray carriage or rack 400 and configured in such a way to provide two such openings 660.
  • These configurations can also avoid the complexity seen for commercial roller hearth systems where individual trays with lids need to be handled and hydrated in discrete groupings, incurring significant equipment capital and operational expense. The en masse hydration approach disclosed herein can avoid such costs while maintaining through-put capacity.
  • FIG. 1 schematically illustrates a cutaway end view of one of the furnace chambers to reveal a recirculation fan 44, heating tubes 42, and a tray carriage 400 disposed on the floor within the chamber, the wheels 420 of the tray carriage 400 capable of traveling across the chamber floor, wherein three tray stacks 500 on the tray carriage 400 are visible in this view.
  • FIG. 1 schematically illustrates a cutaway end view of one of the furnace chambers to reveal a recirculation fan 44, heating tubes 42, and a tray carriage 400 disposed on the floor within the chamber, the wheels 420 of the tray carriage 400 capable of traveling across the chamber floor, wherein three tray stacks 500 on the tray carriage 400 are visible in this view.
  • FIG. 10 schematically illustrates a cutaway end view of one of the furnace chambers to reveal a recirculation fan 44, heating tubes 42, and a tray carriage 400 disposed on the floor within the chamber, the wheels 42 of the tray carriage 400 capable of traveling across the chamber floor, wherein three tray stacks 500 on the tray carriage 400 are visible in this view, and the bottom of the tray carriage 400 is adapted to engage a bottom tray carriage conveyance mechanism 710 which is part of a tray carriage conveyance system 700 to transport the tray carriage 400 into and out of the chamber.
  • FIGS. 11 schematically illustrates a cutaway end view of one of the furnace chambers to reveal a recirculation fan 44, heating tubes 42, and a tray carriage 400 disposed on the floor within the chamber, the wheels 420 of the tray carriage 400 capable of traveling across the chamber floor, wherein three tray stacks 500 on the tray carriage 400 are visible in this view, and a side tray carriage conveyance mechanism 720, which is part of a tray carriage conveyance system 700 to transport the tray carriage 400 into and out of the chamber, engages the sides of the tray carriage 400 and/or the sides of the tray stacks or to transport the tray carriage into and out of the chamber.
  • FIGS. 12-14 schematically illustrate cutaway side views of two chambers of a furnace, such as first and second chambers 10, 20 showing a sequence of transport of a tray carriage 400 through the two chambers in accordance with a bottom tray carriage conveyance mechanism 710 such as the mechanism shown in FIG. 10.
  • the mechanism 710 may comprise a drive gear 712 powered by a gear motor 714 and associated shaft connection 716, the gear 712 engaging a gear rack 718 on the bottom of the tray carriage 400.
  • FIGS. 12-14 three tray stacks 500 are visible on a tray carriage 400, with 6 stackable trays 510 in each stack 500.
  • the first exterior door 70 and first inter-chamber door 80 are closed to substantially seal the first chamber 10 with the tray carriage 400 disposed inside the first chamber 10 after the tray carriage was transported into the chamber via the part of the tray carriage conveyance mechanism disposed inside the first chamber 10.
  • the first and second inter- chamber doors 80, 90 are also closed to substantially seal the second chamber 20.
  • FIG. 13 shows the first exterior door 70 and second inter-chamber door 90 remaining shut and the first inter-chamber door 80 open while the tray carriage 400 is transported from the first chamber 10 via the part of the tray carriage conveyance mechanism disposed inside the first chamber 10 and into the second chamber 20 via the part of the tray carriage conveyance mechanism disposed inside the second chamber 20.
  • FIG. 13 shows the first exterior door 70 and second inter-chamber door 90 remaining shut and the first inter-chamber door 80 open while the tray carriage 400 is transported from the first chamber 10 via the part of the tray carriage conveyance mechanism disposed inside the first chamber 10 and into the second chamber 20 via the part of the tray carriage conveyance mechanism disposed inside the second chamber 20.
  • the tray carriage conveyance system 700 is configured so as to not interfere with the sealing of the chambers, and for example does not include rollers, rails, or other parts which would prevent closure of the furnace doors or sealing of the chambers, thereby providing sealing of the respective chambers during operation. Instead, the tray carriage conveyance system 700 comprises a drive mechanism such as a gear drive or roller drive which engages the tray carriage 400 or the tray stacks 500 themselves inside the respective chambers.
  • a method of manufacturing activated carbon material comprising: providing a multi-chamber furnace having: interior walls defining first, second, and third chambers, a first exterior door disposed at a first end of the first chamber, a first inter-chamber door separating a second end of the first chamber and a first end of the second chamber, a second inter-chamber door separating a second end of the second chamber and a first end of the third chamber, and a second exterior door disposed at a second end of the third chamber; disposing a first tray or tray stack containing a first carbon activation batch mixture in the first chamber, and, in a first phase for the first tray or tray stack: maintaining the first exterior door and first inter-chamber door in respective closed positions, and exposing the first tray or tray stack to a first inert environment, wherein the temperature of the first inert environment is increased to a first maximum temperature between 300 and 450°C, and in some embodiments between 350 and 450
  • the first environment in the first phase, is held to within 50°C of the first maximum temperature for a first hold period of 10 to 360 minutes, and in some of these embodiments, 10 to 120 minutes, and in some of these embodiments, 10 to 60 minutes.
  • inert gas (N 2 ) is introduced into the first chamber at a volume exchange rate of 0.1 to 20 volume exchanges per hour.
  • the first inert environment in the first phase, is heated at a first maximum rate of between 300 and 500 °C/hr; in some of these embodiments, the first maximum rate is 400°C/hr or less, and in some embodiments the first maximum temperature is 400°C or less.
  • gas is removed from the first chamber.
  • the first carbon activation batch mixture is at least partially dehydrated.
  • the first tray stack is disposed in the first chamber for over 1 hour.
  • the method in this one aspect further comprises then disposing the first tray or tray stack in the second chamber and, in a second phase for the first tray or tray stack, maintaining the first and second inter-chamber doors in respective closed positions, and exposing the first tray or tray stack to a second inert environment wherein the temperature of the second inert environment is increased to a second maximum temperature between 600 and 1000 °C, whereby at least a portion of the first carbon activation batch mixture is converted into activated carbon.
  • the second environment in the second phase, is held to within 50°C of the second maximum temperature for a second hold period of 1 to 6 hours and, in some of these embodiments 1 to 5 hours, and in some of these embodiments 2 to 4 hours.
  • the temperature of the second environment is reduced at a rate of 400 to 800 °C/hr.
  • the temperature of the second environment is reduced to between 300 and 450°C, and in some embodiments between 350 and 450 °C.
  • inert gas (N 2 ) is introduced into the first chamber at a volume exchange rate of 0.1 to 20 volume exchanges per hour.
  • the second inert environment in the second phase, is heated after the first inter-chamber door is closed. In some embodiments, in the second phase, the second inert environment is heated at a second maximum rate of between 300 and 500 °C/hr. In some embodiments, the second maximum rate is 400°C/hr or less. In some embodiments, the second maximum temperature is 400°C or less. In some embodiments, in the second phase, gas is removed from the second chamber. In some embodiments, the first tray or tray stack is disposed in the second chamber for over 2 hours, and in some of embodiments for over 5 hours.
  • the method in this one aspect further comprises then, disposing the first tray or tray stack in the third chamber and, in a third phase for the first tray or tray stack, maintaining the second inter-chamber door and the second exterior door in respective closed positions, and exposing the first tray or tray stack to a third inert environment wherein the temperature of the third inert environment is decreased to a hydration temperature and, in a hydration period, steam or water vapor is introduced into the third chamber.
  • Liquid water may be introduced into the third chamber when lower temperatures are present in the third inert environment, e.g. below 100 °C.
  • the hydration period is between 1 and 10 hours, inclusive.
  • the water vapor is introduced along with a nitrogen sweep gas.
  • the temperature is reduced to less than 100 °C, and in some embodiments less than 70 °C, and in other embodiments less than 50 °C.
  • the second environment in the second phase, is held to within 50°C of the second maximum temperature for a second hold period of 1 to 6 hours and, in some of these embodiments 1 to 5 hours, and in some of these embodiments 2 to 4 hours.
  • the second environment is cooled at 400 to 800 °C/hr.
  • the second environment is cooled to between 300 and 450°C, and in some embodiments between 350 and 450 °C.
  • inert gas (N 2 ) is introduced into the first chamber at a volume exchange rate of 0.1 to 20 volume exchanges per hour.
  • the second inert environment is heated after the first inter-chamber door is closed.
  • the second inert environment is heated at a second maximum rate of between 300 and 500 °C/hr.
  • the second maximum rate is 400°C/hr or less.
  • the second maximum temperature is 400°C or less.
  • gas is removed from the second chamber.
  • the first carbon activation batch mixture is at least partially dehydrated.
  • the temperature of the third environment is reduced, in some embodiments to less than 70 °C, in other embodiments to less than 50 °C, in a cooling period.
  • water vapor is present in the third environment during the cooling period.
  • water vapor is not present in the third environment during the cooling period.
  • the third chamber is purged with air during a purge period.
  • the method further comprises opening the second exterior door and moving the first tray or tray stack out of the third chamber.
  • the first tray or tray stack is disposed in the third chamber for over 2 hours, and in some embodiments for over 3 hours.
  • a second tray or tray stack is disposed in the third chamber and, in a first phase for the second tray or tray stack, the method further comprises: maintaining the second inter-chamber door and the second exterior door in respective closed positions, and exposing the second tray or tray stack to a first inert environment, wherein the temperature of the first inert environment is increased to a first maximum temperature between 300 and 450°C, and in some embodiments between 350 and 450 °C; then, disposing the second tray or tray stack in the second chamber and, in a second phase for the second tray or tray stack, maintaining the first and second inter-chamber doors in respective closed positions, and exposing the second tray or tray stack to a second inert environment wherein the temperature of the second inert environment is increased to a second maximum temperature between 600 and 1000 °C whereby the at least a portion of the first carbon activation batch mixture is converted into activated carbon; then disposing the second tray or tray stack in the first chamber and, in a third phase for
  • Liquid water may be introduced into the third chamber when lower temperatures are present in the third inert environment, e.g. below 100 °C.
  • the conditions in the first, second, and third phases for the second tray or tray stack may be the same as, or substantially similar to, the conditions in the first, second, and third phases for the first tray or tray stack as described above, even though the first phase for the second tray or tray stack occurs in the third chamber, and the third phase for the second tray or tray stack occurs in the first chamber.
  • the second tray or tray stack is in the second chamber.
  • the first tray or tray stack is in the first chamber
  • the second tray or tray stack is in the third chamber.
  • the first and second trays or tray stacks occupy the second chamber
  • the apparatuses and methods disclosed herein for the manufacture of activated carbon can accommodate chemical activation using caustics such as KOH, and can help to avoid the use of rotary kilns (which require pre-calcination and drying/dehydration steps prior to treatment at activation temperatures), can help to avoid agglomeration, complexity, and cost issues associated with screw kneaders and rotary kilns, and can help to avoid the use of roller hearths.
  • the apparatuses and methods disclosed herein for chemically activating carbon, for example via alkali salts, using a tray type configuration reduces costs relative to

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  • Inorganic Chemistry (AREA)
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  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un appareil et un procédé de production de charbon actif à l'aide d'un four périodique à chambres multiples. Facultativement, le four est bidirectionnel.
PCT/US2012/067170 2011-11-30 2012-11-30 Appareil et procédé d'activation de charbon à l'aide d'un four périodique à chambres multiples Ceased WO2013082342A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201161565038P 2011-11-30 2011-11-30
US61/565,038 2011-11-30

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WO2016014460A1 (fr) * 2014-07-23 2016-01-28 Corning Incorporated Appareil et procédé de fabrication de charbon activé par des alcalis
CN111924845A (zh) * 2020-07-15 2020-11-13 山东省科学院能源研究所 一种零碳排放的快速活化法制备活性炭材料系统及方法

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