throbber
United States Patent (19)
`Miller
`
`IIIMINIII
`
`US00569.1270A
`11) Patent Number:
`45 Date of Patent:
`
`5,691,270
`Nov. 25, 1997
`
`54 SHAPED LIGNOCELLULOSIC-BASED
`ACTIVATED CARBON
`
`(75) Inventor: James R. Miller, Mt. Pleasant, S.C.
`73) Assignee: Westvaco Corporation, New York,
`N.Y.
`
`(21) Appl. No.: 613,270
`22 Filed:
`Mar 8, 1996
`(51) Int. Cl. ... B01.J. 20/02
`52 U.S. Cl. ............................ 502/416: 502/80; 502/423;
`502/428; 502/429; 502/174; 502/180; 502/182
`(58) Field of Search ..................................... 502/416, 423,
`502/428,429, 80, 174, 180, 182
`References Cited
`U.S. PATENT DOCUMENTS
`6/1987 McCue et al. ............................ 502/80
`4,677,086
`Primary Examiner-Glenn Caldarola
`
`(56)
`
`Assistant Examiner. In Suk Bullock
`Attorney, Agent, or Firm-Terry B. McDaniel; Daniel B.
`Reece, IV; Richard L. Schmalz
`57
`ABSTRACT
`Extruded pellets comprising a majority of activated carbon
`particles and a minority of a binder material are disclosed to
`provide improved performance when processed through
`tumbling equipment while the pellets are in their "green"
`state (i.e., pellets which are freshoff the extruder and contain
`activated carbon), binder material, and water and have not
`been subjected to any thermal processing (drying or
`calcining). The tumbling action both Smooths and densifies
`(i.e., reduces void volume within) the pellet, thereby closing
`any cracks and greatly improving appearance. Improved
`performance results from an ability to increase the weight of
`carbon pellets which can be packed into a fixed volume and
`thereby increase the volumetric working capacity of the bed
`for adsorbing/desorbing vapors. Another benefit is to greatly
`reduce the levels of dust associated with the carbon, both the
`initial dust and the dust attrition.
`8 Claims, 2 Drawing Sheets
`
`
`
`Activated Carbon POWoder
`Binder -
`Water
`
`Calcine
`
`Product
`
` MAHLE-1025
`U.S. Patent No. RE38,844
`
`

`

`U.S. Patent
`US. Patent
`
`Nov. 25, 1997
`Nov. 25, 1997
`
`Sheet 1 of 2
`Sheet 1 of 2
`
`5,691,270
`5,691,270
`
`EH
`
`
`
`.“030051mC_U_mo
`
`
`
`_.mmDmu—u.
`
`
`
`
`
`.ouzon.coEmoumfi>=o<
`
`

`

`U.S. Patent
`US. Patent
`
`Nov. 25, 1997
`Nov. 25, 1997
`
`Sheet 2 of 2
`Sheet 2 of 2
`
`5,691,270
`5,691,270
`
`?OnpOud
`“269;
`
`0528
`
`NHEDGE
`
`
`
`
`
`Loosen.coemoumfi>=o<
`
`
`

`

`1.
`1
`SHAPED LIGNOCELLULOSIC-BASED
`SHAPED LGNOCELLULOSC-BASED
`ACTIVATED CARBON
`ACTIVATED CARBON
`
`5,691,270
`5,691,270
`
`5
`
`20
`20
`
`25
`25
`
`30
`30
`
`35
`35
`
`BACKGROUND OF THE INVENTION
`BACKGROUND OF THE INVENTION
`1. Field of the Invention
`1. Field of the Invention
`This invention relates to an active carbon pellet prepared
`This invention relates to an active carbon pellet prepared
`by extruding activated lignocellulosic-based carbon with a
`by extruding activated lignocellulosic—based carbon with a
`binder material. More particularly, the invention relates to an
`binder material. More particularly, the invention relates to an
`improved active carbon pellet characterized by low pellet
`improved active carbon pellet characterized by low pellet
`void volume and low dust attrition.
`void volume and low dust attrition.
`2. Description of the Prior Art
`2. Description of the Prior Art
`Granular carbons and carbon pellets are typically used in
`Granular carbons and carbon pellets are typically used in
`columns or beds for gas and vapor systems as well for
`columns or beds for gas and vapor systems as well for
`processing a number of liquids. Such carbons have been
`processing a number of liquids. Such carbons have been
`used in canisters in automobiles through which gasoline tank
`used in canisters in automobiles through which gasoline tank
`and carburetor vapors are directed prior to release to the
`and carburetor vapors are directed prior to release to the
`environment. To qualify for this application, a carbon must
`environment. To qualify for this application, a carbon must
`possess sufficient mechanical strength to withstand the abra
`possess sufficient mechanical strength to withstand the abra-
`sion incident to continued use.
`sion incident to continued use.
`There generally is a direct correlation between the
`There generally is a direct correlation between the
`mechanical strength of the granular activated carbon product
`mechanical strength of the granular activated carbon product
`and the mechanical strength of its precursor raw material.
`and the mechanical strength of its precursor raw material.
`Thus, coal-based active carbon generally exhibits a high
`Thus, coal—based active carbon generally exhibits a high
`mechanical strength and density; whereas, lignocellulosic
`mechanical strength and density; whereas, lignocellulosic-
`based active carbons, derived from a much "softer” precur
`based active carbons, derived fi'om a much “softer” precur-
`sor relative to coal, generally exhibit low mechanical
`sor relative to coal, generally exhibit low mechanical
`strengths and densities.
`strengths and densities.
`Also, gas-adsorbing carbons should be as dense as is
`Also, gas-adsorbing carbons should be as dense as is
`consistent with high adsorption capacity so as not to require
`consistent with high adsorption capacity so as not to require
`a large space for the adsorber. The development of high
`a large space for the adsorber. The development of high
`adsorption capacity during thermal activation, however, is
`adsorption capacity during thermal activation, however, is
`accompanied by a loss of mechanical strength and density;
`accompanied by a loss of mechanical strength and density;
`therefore, some compromise is required in selecting the
`therefore, some compromise is required in selecting the
`degree to which the activation is conducted. So, with igno
`degree to which the activation is conducted. So, with ligno-
`cellulosic precursors (or, for lignocellulosic-based active
`cellulosic precursors (or, for lignocellulosic-based active
`carbons), the problem is compounded.
`carbons), the problem is compounded
`Several approaches have been taken to address the prob
`Several approaches have been taken to address the prob-
`lem of low mechanical strength and density of
`lem of low mechanical strength and density of
`lignocellulosic-based active carbons. In U.S. Pat. No. 3,864,
`lignocellulosic—based active carbons. In US. Pat. No. 3,864,
`277, Kovach emphasizes the binder additive in teaching the
`277, Kovach emphasizes the binder additive in teaching the
`phosphoric acid activation of wood, straw, or low-rank
`phosphoric acid activation of wood, straw, or low—rank
`brown coals in the presence of a carbonaceous binder
`brown coals in the presence of a carbonaceous binder
`material such as lignosulfonates and polyvinyl alcohol,
`material such as lignosulfonates and polyvinyl alcohol,
`followed by forming solid granular shaped particles from the
`followed by forming solid granular shaped particles from the
`mixture, and heat-treating at less than 650° C. to give a
`mixture, and heat-treating at less than 650° C. to give a
`granular product having a ball-pan hardness of greater than
`granular product having a ball-pan hardness of greater than
`85%. Given the teaching of Kovach and employing the
`85%. Given the teaching of Kovach and employing the
`knowledge of the relationship of precursor mechanical
`lmowledge of the relationship of precursor mechanical
`strength and density with those characteristics of the active
`strength and density with those characteristics of the active
`carbon product, MacDowall (in U.S. Pat. No. 5,162.286)
`carbon product, MacDowall (in U.S. Pat. No. 5,162,286)
`teaches increasing lignocellulosic-based active carbon den
`teaches increasing lignocellulosic-based active carbon den-
`sity by the use of young carbonaceous vegetable products
`sity by the use of young carbonaceous vegetable products
`high (>30%) in natural binding agent, such as nut shell, fruit
`high (>30%) in natural binding agent, such as nut shell, fruit
`stone, almond shell, and coconut shell, as precursors for
`stone, almond shell, and coconut shell, as precursors for
`treatment with phosphoric acid followed by carbonization.
`treatment with phosphoric acid followed by carbonization.
`A third approach, which relates to the present invention,
`A third approach, which relates to the present invention,
`is taught by McCue et al. in US Pat. No. 4,677,086. To
`is taught by McCue et al. in U.S. Pat. No. 4,677,086. To
`achieve, in a wood-based active carbon, the mechanical
`achieve, in a wood-based active carbon, the mechanical
`strength and product density approaching that achieved with
`strength and product density approaching that achieved with
`coal-based products, McCue et al. teach extruding an active
`coal-based products, McCue et a1. teach extruding an active
`wood-based carbon with bentonite clay, followed by calcin
`wood-based carbon with bentonite clay, followed by calcin-
`ing the extruded active carbon/clay pellets. This technology
`ing the extruded active carbon/clay pellets. This technology
`65
`has been the basis for the commercial products NUCHARO)
`has been the basis for the commercial products NUCHAR®
`65
`BAX-950 and NUCHARGE BAX-1100 marketed by West
`BAX-950 and NUCHAR® BAX-1100 marketed by West-
`vaco Corporation.
`vaco Corporation.
`
`45
`45
`
`50
`50
`
`55
`55
`
`60
`
`10
`10
`
`2
`2
`Carbons of suitable mechanical strength and density for
`Carbons of suitable mechanical strength and density for
`use in an evaporative emission control device (automotive
`use in an evaporative emission control device (automotive
`canister) for adsorbing gasoline vapors preferably also
`canister) for adsorbing gasoline vapors preferably also
`exhibit a butane working capacity of about 10 to about 17
`exhibit a butane working capacity of about 10 to about 17
`g/100 cc and an apparent density from about 0.25 to about
`g/100 cc and an apparent density from about 0.25 to about
`0.40 g/cc.
`0.40 g/cc.
`In addition to gas column (or, packed bed) requirements
`In addition to gas column (or, packed bed) requirements
`for high mechanical strength and high density, it is also
`for high mechanical strength and high density, it is also
`desirable to reduce the bed void volumein order to maxi-
`desirable to reduce the bed void volume in order to maxi
`mize the carbon content of the bed, and subsequently
`mize the carbon content of the bed, and subsequently
`maximize the adsorptive capacity. This is primarily deter
`maximize the adsorptive capacity. This is primarily deter-
`mined by the shape of the granular or pelleted carbon. In
`mined by the shape of the granular or pelleted carbon. In
`fact, because of the irregular shape of granular carbon, more
`fact, because of the irregular shape of granular carbon, more
`regularly shaped carbon pellets are preferred for their better
`regularly shaped carbon pellets are preferred for their better
`15 n
`"packing.” However, as a result of uneven cutting of the
`15
`packing.” However, as a result of uneven cutting of the
`extrudate to form the pellets, the pellets are, in fact, irregu
`extrudate to form the pellets, the pellets are, in fact, irregu-
`larly shaped, and fissures and cavities often appear along the
`larly shaped, and fissures and cavities often appear along the
`pellet surface. This creates two problems. The resulting
`pellet surface. This creates two problems. The resulting
`irregularities in shape prevent optimization of bed (or
`irregularities in shape prevent optimization of bed (or
`column) packing and detract from maximizing the carbon
`column) packing and detract from maximizing the carbon
`content for a given pellet volume. In addition, the surface
`content for a given pellet volume. In addition, the surface
`irregularities are often removed from the pellet due to
`irregularities are often removed from the pellet due to
`abrasion. These material losses, in addition to debris caused
`abrasion. These material losses, in addition to debris caused
`by cutting the pellets to size, present another problem: dust.
`by cutting the pellets to size, present another problem: dust.
`Typically, dusting due to abrasion, or dust attrition, may be
`Typically, dusting due to abrasion, or dust attrition, may be
`retarded or precluded by spraying a coating on the surface of
`retarded or precluded by spraying a coating on the surface of
`the pellet. Invariably, this remedy is at the expense of butane
`the pellet. Invariably, this remedy is at the expense of butane
`working capacity; thereby providing another trade-off for
`working capacity; thereby providing another trade-ofi for
`the working life of the active carbon material.
`the working life of the active carbon material.
`Besides having a product which may appear to
`Besides having a product which may appear to
`disintegrate, attrited dustin a packed bed, such as a column
`disintegrate, attrited dust in a packed bed, such as a column
`or an automotive canister, can fill the bed voids to create
`or an automotive canister, can fill the bed voids to create
`high pressure drops and impede the flow-through of vapors
`high pressure drops and impede the flow-through of vapors
`to be treated. A particular problem in the automotive appli
`to be treated. A particular problem in the automotive appli—
`cation is concern that the dust will act to interfere with
`cation is concern that the dust will act to interfere with
`various sensing devices connected to the canister to monitor
`various sensing devices connected to the canister to monitor
`performance, resulting either in false readings or in failure
`performance, resulting either in false readings or in failure
`of the sensing devices altogether.
`of the sensing devices altogether.
`Therefore, an object of this invention is to provide an
`Therefore, an object of this invention is to provide an
`improved lignocellulosic-based activated carbon pellet of a
`improved lignocellulosic-based activated carbon pellet of a
`smoother surface and more uniform shape which provides
`smoother sm‘face and more uniform shape which provides
`optimal bed packing, exhibits increased density, and is less
`optimal bed packing, exhibits increased density, and is less
`susceptible to dust attrition. An additional object of this
`susceptible to dust attrition. An additional object of this
`invention is to provide an improved method of manufacture
`invenn'on is to provide an improved method of manufacture
`of such activated carbon pellet.
`of such activated carbon pellet.
`BRIEF DESCRIPTION OF THE DRAWINGS
`BRIEF DESCRIPTION OF THE DRAWINGS
`FIG. 1 shows a block flow diagram of the invention
`FIG. 1 shows a block flow diagram of the invention
`process wherein tumbling is carried out on the green
`process wherein tumbling is carried out on the green
`extrudate, followed by drying and calcination.
`extrudate, followed by drying and calcination.
`FIG. 2 shows a block flow diagram of the invention
`FIG. 2 shows a block flow diagram of»: the invention
`process whereby tumbling is carried out on the green
`process whereby tumbling is carried out on the green
`extrudate as it is being dried, followed by calcination.
`extrudate as it is being dried, followed by calcination.
`SUMMARY OF THE INVENTION
`SUMMARY OF THE INVENTION
`The object of the invention is achieved in the discovery
`The object of the invention is achieved in the discovery
`that extruded pellets comprising a major portion of activated
`that extruded pellets comprising a major portion of activated
`carbon particles and a minor portion of inorganic or organic
`carbon particles and a minor portion of inorganic or organic
`binder provides improved performance when processed
`binder provides improved performance when processed
`through tumbling equipment while the pellets are in their
`through tumbling equipment while the pellets are in their
`"green" state. Green pellets are those which are fresh off the
`“green” state. Green pellets are those which are fi'esh off the
`extruder and contain activated carbon, binder, and moisture
`extruder and contain activated carbon, binder, and moisture
`(from 50-70% water, by weight) and have not been sub
`(from 50—70% water, by weight) and have not been sub-
`jected to any thermal processing (i.e., drying or calcining).
`jected to any thermal processing (i.e., drying or calcining).
`The tumbling action both smooths and densifies (i.e.,
`The tumbling action both smooths and densities (i.e.,
`reduces interparticle voids within) the pellet, thereby
`reduces interparticle voids within) the pellet,
`thereby
`
`

`

`3
`3
`sealing, or otherwise closing, any cracks and greatly improv
`sealing, or otherwise closing, any cracks and greatly improv—
`ing appearance. (Interestingly, debris caused by cutting the
`ing appearance. (Interestingly, debris caused by cutting the
`pellets to size is assimilated by the tumbling pellets.)
`pellets to size is assimilated by the tumbling pellets.)
`Improved performance results from an ability to increase the
`Improved performance results from an ability to increase the
`weight of carbon pellets which can be packed into a fixed
`weight of carbon pellets which can be packed into a fixed
`volume and thereby increase the volumetric working capac
`volume and thereby increase the volumetric working capac-
`ity of the bed for adsorbing/desorbing vapors. Another
`ity of the bed for adsorbing/desorbing vapors. Another
`benefit is to greatly reduce the levels of dust associated with
`benefit is to greatly reduce the levels of dust associated with
`the carbon, both the initial dust and the dust attrition.
`the carbon, both the initial dust and the dust attrition.
`DESCRIPTION OF THE PREFERRED
`DESCRIPTION OF THE PREFERRED
`EMBODIMENT(S)
`EMBODIMENT(S)
`The process steps for the alternative embodiments of the
`The process steps for the alternative embodiments of the
`invention process are set forth in the drawings. FIG. 1 shows
`invention process are set forth in the drawings. FIG. 1 shows
`that activated carbon powder (produced from grinding
`that activated carbon powder (produced from grinding
`granular lignocellulosic-based activated carbon), binder
`granular lignocellulosic-based activated carbon), binder
`material, and water are sequentially mulled, extruded,
`material, and water are sequentially mulled, extruded,
`tumbled, dried, and calcined to produce the invention active
`tumbled, dried, and calcined to produce the invention active
`carbon pellet. FIG. 2 shows the activated carbon powder,
`carbon pellet. FIG. 2 shows the activated carbon powder,
`binder material, and water to be sequentially mulled,
`binder material, and water to be sequentially mulled,
`extruded, dried while tumbling, and calcined to produce the
`extruded, dried while tumbling, and calcined to produce the
`invention active carbon pellet, The process steps are
`invention active carbon pellet. The process steps are
`described in greater detail in the Examples which follow.
`described in greater detail in the Examples which follow.
`Also, with the exception of the invention improvement, the
`Also, with the exception of the invention improvement, the
`process generally follows the teaching of U.S. Pat. No.
`process generally follows the teaching of US. Pat. No.
`4,677,086, which disclosure is incorporated herein by ref
`4,677,086, which disclosure is incorporated herein by ref-
`erence.
`eece
`Basically, the blend of activated lignocellulosic-based
`Basically,
`the blend of activated lignocellulosic-based
`carbon, binder material, and water are mixed and then fed
`carbon, binder material, and water are mixed and then fed
`through an extrusion device. The generally continuous
`through an extrusion device. The generally continuous
`extrudate is cut at consistent intervals to produce a cylin
`extrudate is cut at consistent intervals to produce a cylin-
`drical pellet, relatively uniform in length and diameter. The
`drical pellet, relatively uniform in length and diameter. The
`invention process improvement involves taking these
`invention process improvement
`involves taking these
`"green" pellets soon after they are generated and subjecting
`“green” pellets soon after they are generated and subjecting
`them to a tumbling process for a period of time sufficient to
`them to a tumbling process for a period of time suflicient to
`produce a pellet that, upon subsequent drying and/or
`produce a pellet
`that, upon subsequent drying and/or
`calcination, exhibits a pellet void fraction of less than 0.19
`calcination, exhibits a pellet void fraction of less than 0.19
`(determined as the actual pellet density divided by the base
`(determined as the actual pellet density divided by the base
`pellet density and subtracted from 1) and a dust attrition rate
`pellet density and subtracted from 1) and a dust attrition rate
`of less than 1.2 mg/100 cc/minute. In a preferred embodi
`of less than 1.2 mg/lOO cclminute. In a preferred embodi-
`ment of the invention composition, the pellet void fraction
`ment of the invention composition, the pellet void fraction
`is less than 0.17 and the dust attrition rate is 1.0 mg/lOO
`is less than 0.17 and the dust attrition rate is 1.0 mg/100
`cc/minute. In the most preferred embodiment, the pellet void
`cclminute. In the most preferred embodiment, the pellet void
`fraction is less than 0.15 and the dust attrition rate is less
`fraction is less than 0.15 and the dust attrition rate is less
`than 0.8 mg/100 cc/minute. In particular, it has been found
`than 0.8 mg/lOO cclminute. In particular, it has been found
`that the rambling step is effective to provide the improved
`that the rambling step is effective to provide the improved
`composition of the invention if it is performed in lieu of
`composition of the invention if it is performed in lieu of
`immediately drying the green pellets in additional equip
`immediately drying the green pellets in additional equip—
`ment.
`ment.
`It is envisioned that the moisture level of the green pellets
`It is envisioned that the moisture level of the green pellets
`is important in the effectiveness of the tumbling step, and
`is important in the eifectiveness of the tumbling step, and
`that a critical moisture level may exist below which densi
`that a critical moisture level may exist below which densi-
`fication and reduction of dust levels may not occur. As a
`fication and reduction of dust levels may not occur. As a
`result, in an additional embodiment of the invention, the
`result, in an additional embodiment of the invention, the
`tumbling equipment can also be used to dry the green
`tumbling equipment can also be used to dry the green
`pellets, if the dryingrate is kept to a level low enough to give
`pellets. if the drying rate is kept to a level low enough to give
`a sumcient residence time before the critical moisture level
`a sufficient residence time before the critical moisture level
`is reached. The critical moisture level is in the range of
`is reached. The critical moisture level is in the range of
`50-70% water, by weight. A preferred moisture level is
`50—70% water, by weight. A preferred moisture level is
`55-65% water, by weight. The most preferred moisture level
`55—65% water, by weight. The most preferred moisture level
`for the tumbling operation of the green pellets is 58-62%
`for the tumbling operation of the green pellets is 58—62%
`water, by weight.
`water, by weight.
`Any commercial tumbling equipment, based on the nature
`Any cormnercial tumbling equipment, based on the nature
`and volume of material to be treated and whether the process
`and volume of material to be treated and whether the process
`is to be batch or continuous, is considered suitable for use in
`is to be batch or continuous, is considered suitable for use in
`the invention process. Equipment which would be expected
`the invention process. Equipment which would be expected
`
`45
`45
`
`50
`50
`
`55
`55
`
`65
`65
`
`5,691,270
`5,691,270
`
`10
`10
`
`15
`15
`
`20
`
`25
`25
`
`30
`30
`
`35
`35
`
`4
`4
`to produce the beneficial product properties in the invention
`to produce the beneficial product properties in the invention
`composition are considered to be equivalent to the equip
`composition are considered to be equivalent to the equip-
`ment employed in the examples below. The tumbling opera
`ment employed in the examples below. The tumbling opera-
`tion may be employed for up to 30 minutes. The process is
`tion may be employed for up to 30 minutes. The process is
`considered to ofler little or no benefit once the moisture level
`considered to offer little or no benefit once the moisture level
`in the pellets is significantly reduced (<50%).
`in the pellets is significantly reduced (60%).
`The lignocellulosic material precursor to the
`The lignocellulosic material precursor to the
`lignocellulosic-based active carbon used in the invention
`lignocellulosic-based active carbon used in the invention
`process to form the invention composition is selected from
`process to form the invention composition is selected from
`the group consisting of wood chips, wood flour, sawdust,
`the group consisting of wood chips, wood flour, sawdust,
`coconut shell, nut shells, fruit pits, kernal, olive stone, and
`coconut shell, nut shells, fruit pits, kernal, olive stone, and
`almond shell.
`almond shell.
`The binder materials include bentonite clays or chemi-
`The binder materials include bentonite clays or chemi
`cally modified bentonite clays. Preferred binders are sodium
`cally modified bentonite clays. Preferred binders are sodium
`bentonite and calcium bentonite.
`bentonite and calcium bentonite.
`In the Examples to follow, the various analyses were
`In the Examples to follow, the various analyses were
`performed in measurements determining the benefits of the
`performed in measurements determining the benefits of the
`invention product and process:
`invention product and process:
`Apparent Density (AD)-ISO No. 960-050: weight of dry
`Apparent Density (AD)—ISO No. 960-050: weight of dry
`carbon per unit volume of the carbon bed;
`carbon per unit volume of the carbon bed;
`Butane Working Capacity (BWC)-ISO No. 960-080:
`Butane Working Capacity (BWC)—ISO No. 960-080:
`weight of butane purged from a sample of dried carbon after
`weight of butane purged from a sample of dried carbon after
`it had been saturated with butane per unit volume of the
`it had been saturated with butane per unit volume of the
`carbon bed;
`carbon bed;
`Dusting Attrition (DA)-ISO No. 960–380: weight of dust
`Dusting Attrition (DA)-ISO No. 960-380: weight of dust
`attrited from a 100 ml sample of carbon per unit time;
`attrited from a 100 ml sample of carbon per unit time;
`Initial Dust (ID)- same as dusting attrition: Weight of dust
`Initial Dust (ID)- same as dusting attrition: weight of dust
`initially present on a 100 ml sample of carbon prior to
`initially present on a 100 ml sample of carbon prior to
`attrition test;
`attrition test;
`Actual Pellet Density (APD); weight of dry carbon per
`Actual Pellet Density (APD); weight of dry carbon per
`unit volume of entire carbon pellet, determined using mer
`unit volume of entire carbon pellet, determined using mer—
`cury porosimetry;
`cury porosimetry;
`Base Pellet Density (BPD); weight of dry carbon per unit
`Base Pellet Density (BPD); weight of dry carbon per unit
`volume of carbon pellet including only pore space less than
`volume of carbon pellet including only pore space less than
`0.5 microns equivalent diameter, determined using mercury
`0.5 microns equivalent diameter, determined using mercury
`porosimetry;
`porosimetry;
`Bed Void Fraction (BVF): volume of space between
`Bed Void Fraction (BVF): volume of space between
`carbon pellets per unit volume of carbon bed, determined by
`carbon pellets per unit volume of carbon bed, determined by
`the equation 1-(AD/APD); and
`the equation l-(AD/APD); and
`Pellet Void Fraction (PVF) (pellet interparticle void
`Pellet Void Fraction (PVF) (pellet
`interparticle void
`fraction): volume of space within a carbon pellet including
`fraction): volume of space within a carbon pellet including
`only pore space greater than 0.5 microns equivalent diameter
`only pore space greater than 0.5 microns equivalent diameter
`per unit volume of entire carbon pellet, determined by the
`per unit volume of entire carbon pellet, determined by the
`equation 1-(APD/BPD).
`equation 1-(APD/BPD).
`The invention process and composition are further
`The invention process and composition are further
`described in the following specific examples:
`described in the following specific examples:
`EXAMPLE 1
`EXAMPLE 1.
`Ground wood—based activated carbon was mixed with
`Ground wood-based activated carbon was mixed with
`bentonite clay and water in a muller mixer. The dry basis
`bentonite clay and water in a muller mixer. The dry basis
`clay concentration was 14 wt %. The mixture was mulled
`clay concentration was 14 wt %. The mixture was mulled
`until it reached a consistency which could be extruded. It
`until it reached a consistency which could be extruded. It
`was extruded in a twin screw auger extruder through a die
`was extruded in a twin screw auger extruder through a die
`plate containing 2 mm holes and cut as it exited the die plate
`plate containing 2 mm holes and cut as it exited the die plate
`into "green” pellets ranging in length from 2-6 mm. The
`into “green” pellets ranging in length from 2—6 mm. The
`green pellets had amoisture content of approximately 55-60
`green pellets had a moisture content of approximately 55—60
`wt % (wet basis). Following extrusion, a portion of the green
`wt % (wet basis). Following extrusion, a portion of the green
`pellets was loaded into a rotating disc pan pelletizer in order
`pellets was loaded into a rotating disc pan pelletizer in order
`to tumble the pellets. The pan was angled above the hori
`to tumble the pellets. The pan was angled above the hori-
`zontal to retain the pellets and rotated at 15 rpm for 5
`zontal to retain the pellets and rotated at 15 rpm for 5
`minutes. After 5 minutes, pellets were collected from the pan
`minutes. After 5 minutes, pellets were collected from the pan
`and dried in a batch, convection oven. The portion of green
`and dried in a batch, convection oven. The portion of green
`pellets which was not tumbled was also dried in the same
`pellets which was not tumbled was also dried in the same
`oven for the same amount of time. The two batches of dried
`oven for the same amount of time. The two batches of dried
`pellets were calcined separately to 1200° F in a batch
`pellets were calcined separately to 1200° F.
`in a batch
`
`

`

`5,691,270
`5,691,270
`
`6
`6
`
`5
`5
`indirect-fired rotary furnace for 15 minutes. Following
`indirect-fired rotary furnace for 15 minutes. Following
`calcination, they were discharged and cooled separately
`calcination, they were discharged and cooled separately
`under a nitrogen purge prior to analysis.
`under a nitrogen purge prior to analysis.
`The pertinent properties of each product are shown in
`The pertinent properties of each product are shown in
`Table I. From the data, it can be seen that BWC increased
`Table I. From the data, it can be seen that BWC increased
`7.5%, apparent density increased 9.2%, initial dust was
`7.5%, apparent density increased 9.2%,
`initial dust was
`reduced by 70%, and dust attrition was reduced by 45%
`reduced by 70%, and dust attrition was reduced by 45%
`(from 2.16 to 1.19).
`(from 2.16 to 1.19).
`
`TABLE I
`
`TABLE I
`DA
`1])
`BWC
`AD
`DA
`D
`BWC
`AD
`
`(g/100 cc)
`(glee)
`(mg)
`(mg/min)
`Batch I.D.
`(g/100 cc)
`(gfcc)
`(mg)
`(mg/min)
`Batch I.D.
`095-0342
`10.7
`0.336
`58.8
`2.16
`C-95-0342
`10.7
`0.336
`58.8
`2.16
`-Not Tumbled-
`-Not Tumbled
`C-950343
`11.5
`0.367
`17.8
`1.19
`C-95.0343
`11.5
`0.367
`17.8
`1.19
`-Tumbled—
`
`-Tumbled
`
`10
`10
`
`15
`15
`
`20
`20
`
`25
`25
`
`30
`30
`
`EXAMPLE 2
`EXAMPLE 2
`Ground lignocellulosic-based activated carbon was mixed
`Ground lignocellulosic-based activated carbon was mixed
`with bentonite clay and water in a Muller mixer. The dry
`with bentonite clay and water in a Muller mixer. The dry
`basis clay concentration was 9 wt %. The mixture was
`basis clay concentration was 9 wt %. The mixture was
`mulled until it reached a consistency which could be
`mulled until it reached a consistency which could be
`extruded. It was extruded in a single screw auger extruder
`extruded. It was extruded in a single screw auger extruder
`through a die plate containing 2 mmholes and cut as it exited
`through a die plate containing 2 mmholes and cut as it exited
`the die plate into "green” pellets ranging in length from 2-6
`the die plate into “green” pellets ranging in length from 2—6
`mm. The green pellets had a moisture content of approxi
`mm. The green pellets had a moisture content of approxi-
`mately 55-60 wt % (wet basis). Following extrusion, a
`mately 55—60 wt % (wet basis). Following extrusion, a
`portion of the green pellets was taken and loaded into a 24
`portion of the green pellets was taken and loaded

This document is available on Docket Alarm but you must sign up to view it.


Or .

Accessing this document will incur an additional charge of $.

After purchase, you can access this document again without charge.

Accept $ Charge
throbber

Still Working On It

This document is taking longer than usual to download. This can happen if we need to contact the court directly to obtain the document and their servers are running slowly.

Give it another minute or two to complete, and then try the refresh button.

throbber

A few More Minutes ... Still Working

It can take up to 5 minutes for us to download a document if the court servers are running slowly.

Thank you for your continued patience.

This document could not be displayed.

We could not find this document within its docket. Please go back to the docket page and check the link. If that does not work, go back to the docket and refresh it to pull the newest information.

Your account does not support viewing this document.

You need a Paid Account to view this document. Click here to change your account type.

Your account does not support viewing this document.

Set your membership status to view this document.

With a Docket Alarm membership, you'll get a whole lot more, including:

  • Up-to-date information for this case.
  • Email alerts whenever there is an update.
  • Full text search for other cases.
  • Get email alerts whenever a new case matches your search.

Become a Member

One Moment Please

The filing “” is large (MB) and is being downloaded.

Please refresh this page in a few minutes to see if the filing has been downloaded. The filing will also be emailed to you when the download completes.

Your document is on its way!

If you do not receive the document in five minutes, contact support at support@docketalarm.com.

Sealed Document

We are unable to display this document, it may be under a court ordered seal.

If you have proper credentials to access the file, you may proceed directly to the court's system using your government issued username and password.


Access Government Site

We are redirecting you
to a mobile optimized page.





Document Unreadable or Corrupt

Refresh this Document
Go to the Docket

We are unable to display this document.

Refresh this Document
Go to the Docket