EP1781125A2 - Ultra-fine particle catalysts for carbonaceous fuel elements - Google Patents

Ultra-fine particle catalysts for carbonaceous fuel elements

Info

Publication number
EP1781125A2
EP1781125A2 EP05759387A EP05759387A EP1781125A2 EP 1781125 A2 EP1781125 A2 EP 1781125A2 EP 05759387 A EP05759387 A EP 05759387A EP 05759387 A EP05759387 A EP 05759387A EP 1781125 A2 EP1781125 A2 EP 1781125A2
Authority
EP
European Patent Office
Prior art keywords
fuel element
carbon monoxide
catalyst composition
carbon
ultrafine particles
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.)
Withdrawn
Application number
EP05759387A
Other languages
German (de)
English (en)
French (fr)
Inventor
Chandra Kumar Banerjee
Stephen Benson Sears
Sheila Lynnette Cash
Henry Hsiao Liang Chung
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.)
RJ Reynolds Tobacco Co
Original Assignee
RJ Reynolds Tobacco Co
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 RJ Reynolds Tobacco Co filed Critical RJ Reynolds Tobacco Co
Publication of EP1781125A2 publication Critical patent/EP1781125A2/en
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes
    • A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/165—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes comprising as heat source a carbon fuel or an oxidized or thermally degraded carbonaceous fuel, e.g. carbohydrates, cellulosic material
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/285—Treatment of tobacco products or tobacco substitutes by chemical substances characterised by structural features, e.g. particle shape or size
    • A24B15/286—Nanoparticles
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/287—Treatment of tobacco products or tobacco substitutes by chemical substances by inorganic substances only
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/287—Treatment of tobacco products or tobacco substitutes by chemical substances by inorganic substances only
    • A24B15/288—Catalysts or catalytic material, e.g. included in the wrapping material
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A24D1/22—Cigarettes with integrated combustible heat sources, e.g. with carbonaceous heat sources
    • 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
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/52—Gold
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/46—Flow patterns using more than one column
    • G01N30/466—Flow patterns using more than one column with separation columns in parallel
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G01N30/7206—Mass spectrometers interfaced to gas chromatograph

Definitions

  • the metal oxide and metal ultrafme particles can demonstrate activity for catalyzing chemical reactions, such as the oxidation of carbon monoxide to carbon dioxide.
  • Ultrafme particles suitable for use in catalytic compositions of the present invention comprise, but are not limited to, iron oxides (e.g. FeO, Fe 2 O 3 and Fe 3 O 4 ), gold, copper, silver, platinum, palladium, rhodium, nickel, zinc, zirconium, other transition metals, metal oxides, and mixtures thereof.
  • the ultrafine particles of the catalyst compositions can be combined with a carbonaceous material in a number of ways to produce the fuel element composition.
  • One method of combination comprises intimately mixing the carbonaceous material with the ultrafine particles.
  • Ultrafine particles in dry powder form e.g. nanopowder
  • the ultrafine particles may be mixed directly in a carbon mix along with other dry ingredients for extrusion.
  • the ultrafine particles may be suspended in a liquid and the suspension mixed with extrudate.
  • Another method of combining the ultrafine catalyst compositions with a carbonaceous material comprises forming the carbonaceous material so as to concentrate the catalytic compositions in one or more longitudinal passageways extending partially through the fuel element.
  • a mouthend piece 22 comprising a cylindrical segment of a flavored carbon filled sheet material 24 and a segment of non- woven thermoplastic fibers 26 through which the aerosol passes to the user.
  • the smoking article, or portions thereof, is overwrapped with one or more layers of cigarette papers 30-36
  • catalyst compositions comprising metal oxide and/or metal ultrafme particles are incorporated into the filter element of the smoking article as described in United States Patent Application Serial No. 10/730,962 which is hereby incorporated by reference.
  • This smoke-like aerosol can contain reduced amounts of carbon monoxide resulting from the reduced carbon monoxide production of a fuel element of the present invention upon combustion.
  • the catalyst compositions can be deposited on a porous support such as graphite or alumina wherein the porous support is placed behind the fuel in an end to end relationship.
  • the present invention provides a method for facilitating the reduction in the amount of carbon monoxide produced by a smoking article, comprising incorporating at least one catalyst composition comprising ultrafme particles of a metal oxide and/or metal into the fuel element of a smoking article.
  • the temperature of the split single injector 302 can be varied in accordance with desired analytical conditions.
  • the temperature variance of the single split injector 302 can be controlled manually by a user or can be controlled electronically with any processor- equipped device such as a computer and/or dedicated controller.
  • one of the two columns 303 is suitable for resolving the carbon monoxide content of a gaseous mixture while the other column 304 is suitable for resolving the gaseous mixture's carbon dioxide content.
  • Chromatographic columns for use in the gas chromatograph of the present apparatus are available commercially. The two chromatographic columns feed into a mass spectrometer 305.
  • Mass spectrometers suitable for use in further resolving and quantifying the carbon monoxide content and carbon dioxide content eluting from the two columns of the gas chromato graph can comprise mass analyzers comprising magnetic sector analyzers, double-focusing spectrometers, quadrupole mass filters, ion trap analyzers, and time-of- flight (TOF) analyzers.
  • TOF time-of- flight
  • the embodiments described above in addition to other embodiments can be further understood with reference to the following examples.
  • Several of the fuel elements provided in the examples below comprise percentages of BKO carbon, Guar gum, graphite, and tobacco. Combustion of all the fuel elements in the examples below provides energy used to generate aerosol from tobacco and other aerosol formers like glycerin. Combustion of the fuel elements, however, also produces carbon monoxide and carbon dioxide. Moreover, complete combustion of the fuel elements produces a maximum amount of energy and a carbon dioxide by-product. Complete combustion is demonstrated by the chemical reaction:
  • the ion chrornatogram of Figure 6 displays a complete resolution of carbon dioxide and an incomplete resolution of carbon monoxide.
  • the carbon monoxide co-eluted with nitrogen and oxygen.
  • the results of the remaining sample materials comprising tobaccos from 1R4F cigarettes and 1R4F cigarette smoke resolved on dual chromatographic columns in accordance with the present invention are illustrated in Figures 7 and 8 respectively.
  • the ion chromato grams of Figures 7 and 8 demonstrate completely and sharply resolved carbon monoxide and carbon dioxide peaks.
  • the gaseous mixture resulting from the combustion of each sample was analyzed in accordance with the method delineated in Figure 2.
  • the pyroprobe and gas chromatogram injector were set at ambient temperature.
  • a Molsieve chromatographic column was used for carbon monoxide resolution and a GS-CarbonPLOT chromatographic column was used for carbon dioxide resolution.
  • a mass spectrometer was used as a second dimension of analysis in the quantification of the carbon monoxide and carbon dioxide contents generated by the samples. It should be noted that the carbon monoxide and the carbon dioxide contents quantified were only a fraction of the carbon monoxide and carbon dioxide contents produced by the samples and that the resolved peak areas were used for quantification. Table 1 summarizes the results produced by the samples in this example.
  • the titanium oxide-gold (TiO 2 -Au) ultrafine particles of sample (4) demonstrated a carbon monoxide reduction of 52% while the eerie oxide (CeO 2 ) ultrafine particles of sample (6) resulted in approximately a 7% reduction.
  • Example 3 Eight fuel element samples were generated for analysis of (CO/CO 2 ) ratios.
  • a pyroprobe was used to heat a small quantity of each sample to 700 0 C in the presence of air for 20 seconds.
  • 700 0 C is the average temperature of a fuel element during combustion.
  • the gaseous mixture resulting from the combustion of each sample was analyzed in accordance with the method delineated in Figure 2.
  • the pyroprobe and gas chromatogram injector were set at ambient temperature.
  • a Molsieve chromatographic column was used for carbon monoxide resolution and a GS-CarbonPLOT chromatographic column was used for carbon dioxide resolution.
  • a mass spectrometer was used as a second dimension of analysis in the quantification of the carbon monoxide and carbon dioxide contents generated by the samples. It should be noted that the carbon monoxide and the carbon dioxide contents quantified were only a fraction of the carbon monoxide and carbon dioxide contents produced by the samples and that the resolved peak areas were used for quantification. Table 2 summarizes the results produced by the samples in this example.
  • the Fe 2 O 3 ultrafine particles of sample (3) reduced the carbon monoxide content of the gaseous mixture analyzed by 89.5%, which is an 11% increase over the ⁇ -Fe 2 ⁇ 3 -large particles.
  • the results of the sample testing further demonstrate the catalytic activity of ferric oxide ultrafme particles in fuel elements that comprise the additional components of Guar gum and graphite.
  • Sample (7) is an example of a fuel element containing these additional components.
  • Sample (8) comprises the components of sample (7) with the addition of 5% by weight of ferric oxide (Fe 2 O 3 ) ultrafine particles.
  • sample (5) is a fuel element containing a 5.05% tobacco content in addition to BKO Carbon 950, Guar gum, and graphite.
  • Sample (6) comprises the components of sample (5) with the addition of 5% by weight of ferric oxide (Fe 2 O 3 ) nanoparticle.
  • the ferric oxide (Fe 2 O 3 ) ultrafine particles reduced the carbon monoxide production of the fuel element of sample (6) by 15.4% in comparison with sample (5) which did not contain ferric oxide (Fe 2 O 3 ) ultrafine particles.
  • the catalytic activity of the ferric oxide (Fe 2 O 3 ) ultrafine particles in sample (6) was diminished due to the tobacco content in the fuel element composition.
  • the combustion of tobacco produces several chemical species that inhibit the catalytic behavior of the ultrafine particles. This catalytic inhibition is displayed in the 15.4% reduction of carbon monoxide production.
  • the sample were: (1) Control Carbon (BKO 950), (2) Carbon with 5% Fe 2 O 3 ultrafine particles obtained from MACH-I, Inc., (3) Carbon with 5% Al 2 O 3 ultrafine particles obtained from NEI, Inc., (4) Carbon with 5% CeO 2 ultrafine particles obtained from NEI, Inc., (5) Carbon with 5% TiO 2 ultrafine particles obtained from NEI, hie, (6) Carbon with 5% tobacco and 5% Fe 2 O 3 ultrafine particles obtained from MACH-I, Inc., and (7) Carbon with 5% tobacco (heat treated) and 5% Fe 2 O 3 ultrafine particles obtained from MACH-I, Inc.
  • a pyroprobe was used to heat a small quantity of each sample to 700 0 C in the presence of air for 20 seconds.
  • 700 0 C is the average temperature of a fuel element during combustion.
  • the gaseous mixture resulting from the combustion of each sample was analyzed in accordance with the method delineated in Figure 2.
  • the pyroprobe and gas chromatogram injector were set at ambient temperature.
  • a Molsieve chromato graphic column was used for carbon monoxide resolution and a GC-CarbonPLOT chromatographic column was used for carbon dioxide resolution.
  • a mass spectrometer was used as a second dimension of analysis in the quantification of the carbon monoxide and carbon dioxide contents generated by the samples. It should be noted that the carbon monoxide and the carbon dioxide contents quantified were only a fraction of the carbon monoxide and carbon dioxide contents produced by the samples and that the resolved peak areas were used for quantification. Table 3 summarizes the results produced by the samples in this example.
  • ferric oxide (Fe 2 O 3 ) ultrafine particles demonstrate a greater reduction in the carbon monoxide production of heated fuel elements.
  • samples (3) and (5) containing aluminum oxide (Al 2 O 3 ) and titanium oxide (TiO 2 ) ultrafine particles respectively exhibited a slight increase in carbon monoxide content.
  • a GS-CarbonPLOT column (J&W Scientific, 60 M x 0.32 mm I.D., 1.5 ⁇ m film) was used for CO 2 analysis.
  • the temperature of the CG columns was held at 35 0 C for 10 minutes, programmed to 15O 0 C at 25°C/min and held for 10 min.
  • a mass spectrometer (MS) was used to identify and quantify the resolved CO and CO 2 peaks eluting from the gas chromatograph.
  • the MS used was a Hewlett-Packard 5972 mass selective detector.
  • the mass spectrometer was operated at 70 eV in the El mode.
  • the temperature of the ion source was maintained at 18O 0 C and the mass range scanned was 20-200 atomic mass units. It should be noted that the CO and CO 2 quantities determined were only a fraction of the total CO and CO 2 content generates from the samples. Only the resolved CO and CO 2 peak areas were used for quantification. Table 4 summarizes the results produced by the samples in this example.
  • a small component of tobacco within the fuel element does not destroy the catalytic activity of the metal oxide and metal ultrafme particles an appreciable amount and is, therefore, tolerable.
  • the inclusion of a tobacco component in the fuel element of a smoking article can provide more flavor to the aerosol comprising the mainstream smoke of a smoking article.

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Chemistry (AREA)
  • Molecular Biology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • Catalysts (AREA)
  • Manufacture Of Tobacco Products (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
EP05759387A 2004-06-15 2005-06-09 Ultra-fine particle catalysts for carbonaceous fuel elements Withdrawn EP1781125A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US10/868,126 US20050274390A1 (en) 2004-06-15 2004-06-15 Ultra-fine particle catalysts for carbonaceous fuel elements
PCT/US2005/020406 WO2006002001A2 (en) 2004-06-15 2005-06-09 Ultra-fine particle catalysts for carbonaceous fuel elements

Publications (1)

Publication Number Publication Date
EP1781125A2 true EP1781125A2 (en) 2007-05-09

Family

ID=35355344

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05759387A Withdrawn EP1781125A2 (en) 2004-06-15 2005-06-09 Ultra-fine particle catalysts for carbonaceous fuel elements

Country Status (4)

Country Link
US (1) US20050274390A1 (ja)
EP (1) EP1781125A2 (ja)
JP (1) JP2008505990A (ja)
WO (1) WO2006002001A2 (ja)

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