WO2017130045A1 - Sphéroïdes de charbon actif pour articles pour fumeurs - Google Patents

Sphéroïdes de charbon actif pour articles pour fumeurs Download PDF

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Publication number
WO2017130045A1
WO2017130045A1 PCT/IB2016/058080 IB2016058080W WO2017130045A1 WO 2017130045 A1 WO2017130045 A1 WO 2017130045A1 IB 2016058080 W IB2016058080 W IB 2016058080W WO 2017130045 A1 WO2017130045 A1 WO 2017130045A1
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WO
WIPO (PCT)
Prior art keywords
activated carbon
spheroid
smoking article
binder
particles
Prior art date
Application number
PCT/IB2016/058080
Other languages
English (en)
Inventor
Alberto BONICI
Laura CANO CASANOVA
Gaëtan COUDERC
Mohammed OUZZINE
Ana AMOROS PÉREZ
Maria Ángeles LILLO RÓDENAS
Ángel LINARES-SOLANO
Original Assignee
Philip Morris Products S.A.
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 Philip Morris Products S.A. filed Critical Philip Morris Products S.A.
Publication of WO2017130045A1 publication Critical patent/WO2017130045A1/fr

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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
    • A24B15/18—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
    • 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
    • A24B15/42—Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances
    • 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
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
    • 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
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/062—Use of materials for tobacco smoke filters characterised by structural features

Definitions

  • This disclosure relates to smoking articles that have filters containing activated carbon.
  • Combustible smoking articles such as cigarettes, typically have shredded tobacco, usually in cut filler form, surrounded by a paper wrapper forming a tobacco rod.
  • a cigarette is employed by a smoker by lighting one end of the cigarette and burning the tobacco rod. The smoker then receives mainstream smoke by drawing on the opposite end or mouth end of the cigarette, which typically contains a filter.
  • the filter is positioned to entrap some constituents of mainstream smoke before the mainstream smoke is delivered to a smoker.
  • a number of smoking articles in which an aerosol generating substrate, such as tobacco, is heated rather than combusted have also been proposed in the art.
  • the aerosol is generated by heating the aerosol generating substrate.
  • Known heated smoking articles include, for example, smoking articles in which an aerosol is generated by electrical heating or by the transfer of heat from a combustible fuel element or heat source to an aerosol generating substrate.
  • volatile compounds are released from the aerosol generating substrate by heat transfer from the heat source and entrained in air drawn through the smoking article. As the released compounds cool they condense to form an aerosol that is inhaled by the consumer.
  • Non-combustible smoking articles in which a nicotine-containing aerosol is generated from a tobacco material, tobacco extract, or other nicotine source, without combustion, and in some cases without heating, for example through a chemical reaction.
  • Such non-combustible smoking articles may also include a filter positioned to adsorb smoke constituents before the mainstream smoke is delivered to a user.
  • Filters in smoking articles may contain activated carbon to remove selected constituents from smoke.
  • Activated carbon granules are typically used in filters to selectively adsorb smoke constituents. However, carbon fines are generated during transport, handling and loading of the activated carbon granules. Particle breakthrough may occur in filters containing activated carbon granules due in part to the presence of the carbon fines. Activated carbon granules are typically added to filters of smoking articles via at least one extra process step, which may add complexity to the process particularly to the high-speed processes employed in cigarette manufacturing.
  • Activated carbon powder is not used in smoking articles because its size is too small to be retained by filter material such as cellulose acetate tow.
  • Extruded rods containing activated carbon and a binder have been proposed for use directly in filters of smoking articles.
  • aligning and incorporating cylindrical objects into filters during high-speed manufacturing processes may be challenging. For example, placing the rods in filters in the proper orientation without breaking or blockage of the machine may be problematic.
  • One object of aspects of present invention is to manufacture smoking articles that include filters containing activated carbon on high-speed manufacturing lines. Another object of aspects of the present invention is to simplify the manufacturing process for incorporating activated carbon in filters for smoking articles. Another object of aspects of the present invention is to produce a smoking article that includes activated carbon in the filter, where the activated carbon exhibits less particle breakthrough during smoking than currently employed activated carbon. Other objects of aspects of the present invention will be evident to those of skill in the art upon reading and understanding the present disclosure, which includes the claims that follow and accompanying drawings.
  • a smoking article comprising a smokable material and a spheroid comprising particles of activated carbon and an alkylcellulose binder.
  • the binder preferably comprises methylcellulose.
  • the particles of activated carbon have a diameter less than 0.5 mm, more preferably less than 0.2 mm.
  • the particles of activated carbon comprise activated carbon powder.
  • the spheroid is downstream of the smokable material.
  • the spheroid has a diameter in a range from 1 mm to 8 mm, preferably from 2 mm to 7 mm, and more preferably from 2.5 mm to 6 mm.
  • the spheroids comprise from about 1 % to about 15% by weight of the binder and comprise greater than about 50% by weight of the activated carbon.
  • a "smokable material” is a material that generates an aerosol deliverable to a user of a smoking article when the material is placed in a smoking article and the smoking article is properly employed by a user.
  • the method comprises (i) mixing particles of activated carbon with a binder to produce a mixture comprising from about 1 % to about 15% by weight of the binder; (ii) extruding the mixture to produce an extrudate; (iii) spheronizing the extrudate to form a spheroid having a diameter in a range from 1 mm to 8 mm; and (iv), embedding the spheroid in filter material or disposing the spheroid between first and second plugs of filter material.
  • the particles of activated carbon in the spheroid have a size of 50 U.S. mesh (about 0.3 mm) or less.
  • One or more aspects of the smoking articles and methods of the present invention may have one or more advantages relative to currently available smoking articles that include activated carbon or associated methods for manufacturing such smoking articles.
  • millimeter-sized activated carbon spheroids may be placed in filters using existing manufacturing equipment for placing capsules, such as flavor capsules, into filters of smoking articles. Unlike rods, spheroids do not need to be oriented for placement into a filter, allowing for higher speed introduction.
  • a filter of the present invention can contain a single activated carbon spheroid as opposed to multiples, thus use of filter combiners for making filters with activated carbon granules can be avoided.
  • Carbon carry over may be reduced due to the use of a single or small number of activated carbon spheroids rather than a large number of smaller particles of activated carbon according to current filter manufacturing processes.
  • spheroids of aspects of the present invention may be formed using commercially available activated carbon powder or granules and a commercially available binder. Accordingly, manufacturing costs can be kept low.
  • particle breakthrough may be reduced due to binder.
  • particle breakthrough can be reduced due to the lack of a requirement for crushing or granulation steps in the production of the activated carbon. However, crushing or granulation steps may be employed in making spheroids of the present invention.
  • Activated carbon spheroids of the present invention can also advantageously serve as a vehicle for delivery of flavorants in smoke of a smoking article.
  • the activated carbon spheroids may also act as a flow restrictor in smoking articles due to the relatively large size of the particle.
  • the activated carbon spheroids can serve to reduce the concentration of certain smoke constituents from mainstream smoke. Additional advantages of one or more aspects of smoking articles described herein will be evident to those of skill in the art upon reading and understanding the present disclosure.
  • Activated carbon can be produced from any suitable carbonaceous source material.
  • Activated carbon is a generic term used to describe a family of carbonaceous adsorbents with an extensively developed internal pore structure.
  • Activated carbon can be produced from a carbonaceous source material such as wood, lignite, coal, nuts, nut shells, coconut husk or shells, peat, pitch, polymers such as phenolic resins, cellulose fibers, polymer fibers, or the like.
  • activated carbon is produced from a vegetal source rather than a carbon fuel or petroleum-based source.
  • a "vegetal source” is a plant or part of a plant, where the plant was a living within 50 years from being converted to activated carbon; more preferably within 20 years, even more preferably within 5 years, and yet more preferably within 2 years.
  • the primary form of carbon in a vegetal source is cellulose and other related polymers of polysaccharide, as opposed to the form of carbon in a coal- or petroleum-based source which comprises mostly solid polymers of hydrocarbons.
  • the source of carbon in the activated carbon used in the invention, before carbonization comprises more polysaccharides than polymers of hydrocarbons, for example, greater than 80% or 95%.
  • Activated carbon may be produced by any suitable process such as physical activation or chemical activation.
  • the source material is developed into activated carbon by carbonization and activation with hot gases.
  • the process of carbonization includes pyrolyzing source material at high temperatures, typically in the range of about 600°C to about 900°C, in the absence of oxygen.
  • Activation includes exposing carbonized material to oxidizing atmospheres, such as steam, carbon dioxide or oxygen, at temperatures above 250°C, such as about 800°C. Temperatures for activation/oxidization typically range from about 600°C to about 1200°C, such as about 850°C.
  • Chemical activation includes impregnating raw source material with certain chemicals, such as an acid, base or salt, such as phosphoric acid, potassium hydroxide, sodium hydroxide, calcium chloride, or zinc chloride.
  • the raw materials are then carbonized at temperatures that are typically lower than physical activation carbonization.
  • temperatures for chemical activation carbonization may be in the range of from about 450°C to about 900°C. Carbonization and activation may occur simultaneously.
  • carbonaceous source material may be activated via any suitable process.
  • activation occurs in a step following carbonization.
  • carbonized particles are activated by a physical activation process.
  • temperature is increased at a rate of about 5°C per minute or about 10°C per minute until the desired temperature is achieved during carbonization.
  • the rate of temperature increase can be lower, such as about 1°C per minute, to prevent agglomeration of particles during carbonization if needed or desired.
  • the rate of temperature increase in an activation process is about 5°C per minute.
  • Pore size and surface characteristics may be varied according to well-known techniques, which can affect the efficiency with which activated carbon can remove selected smoke constituents, such as 1 ,2-propadiene, 1 ,3-butadiene, isoprene, benzene, 1 ,2-pentadiene, 1 ,3- cyclopentadiene, 2,4-hexadiene, 1 ,3-cyclohexadiene, methyl-1 ,3-cyclopentadiene, benzene, toluene, p-xylene, m-xylene, o-xylene, styrene (vinylbenzene), 1-methylpyrrole, formaldehyde, acetaldehyde, acrolein, propionaldehyde, isobutyraldehyde, 2-methyl isovaleraldehyde, acetone, methyl vinyl ketone, diacetyl, methyl ethyl ketone, methyl prop
  • the pore size distribution and surface characteristics can be readily modified by adjusting the activating atmosphere (e.g., O2, CO2 or steam) and the activation time and temperature. Further treatment, e.g. in an inert atmosphere, may be performed to modify surface oxygen content without modifying porosity.
  • the activating atmosphere e.g., O2, CO2 or steam
  • Further treatment e.g. in an inert atmosphere, may be performed to modify surface oxygen content without modifying porosity.
  • One of skill in the art may readily adjust activation parameters to achieve activated carbon particles for use in filters and smoking articles of the present invention.
  • Spheroids of the invention may be produced in any suitable manner.
  • a "spheroid" for purposes of the present invention has a diameter of about 0.5 millimeters (mm) or greater. Generally, spheroids will also have a diameter of about 10 mm of less.
  • spheroid of the present invention have a diameter in a range from about 1 mm to about 8 mm; more preferably from about 2 mm to about 7 mm; more preferably from 2.5 mm to 6 mm; and even more preferably from about 4 mm to about 5 mm.
  • Spheroids according to the present invention have a sphericity from about 0.8 to about 1 ; preferably from about 0.9 to about 1.
  • sphericity As used herein, "sphericity", ⁇ , of a particle is the ratio of the surface area of a sphere with the same volume as the particle to the surface area of the particle. Sphericity may be determined as described in International Standard ISO 9276-6:2008, "Representation of results of particle size analysis - Part 6: Descriptive and quantitative representation of particle shape and morphology," in which sphericity, ⁇ , is defined as follows:
  • the sphericity, ⁇ , of a sphere is 1. Any particle that is not a sphere will have a sphericity of less than 1.
  • Spheroids of the present invention comprise particles of activated carbon and a binder.
  • the particles of activated carbon in the spheroids comprise granular activated carbon or powdered activated carbon.
  • the particle or particles of activated carbon in the spheroids has a size of about 0.5 mm or less; more preferably about 0.2 mm or less.
  • Powdered activated carbon is particles of activated carbon that pass through an 80- mesh (0.177 mm) sieve. Accordingly, powdered activated carbon has a diameter of less than about 0.18 mm.
  • the particles of activated carbon may not be spherical. Accordingly, the use of the term “diameter” in the context of particles of activated carbon may be considered to refer to the average of the length, width and height of the particles within a population of particles. Alternatively, “diameter” can be considered to be a range based on size of sieves through which a population of particles of activated carbon may pass, with the smallest tested sieve through which the particles pass being the maximum “diameter”, and through which activated carbon particles do not pass, with the largest tested sieve through which the particles do not pass being the minimum “diameter.”
  • Granular activated carbon is particles of activated carbon having a diameter greater than powdered activated carbon, but generally less than 1 mm in size. Accordingly, granulated activated carbon typically has a diameter on average from about 0.18 mm to about 1 mm.
  • Granulated activated carbon can be categorized into size ranges based on its ability to pass through, or not pass through, sieves. For example, a 20x40 activated carbon comprises particles that will pass through a U.S. Standard Mesh Size No. 20 sieve (0.84 mm) (generally specified as 85% passing) but be retained on a U.S. Standard Mesh Size No. 40 sieve (0.42 mm) (generally specified as 95% retained).
  • the particles of activated carbon in spheroids of the present invention is activated carbon have on average a diameter of about 30 U.S. mesh (0.595 mm) or less, such as about 35 U.S. mesh (0.5 mm) or less; preferably about 40 U.S. mesh (0.4 mm) or less or about 45 U.S. mesh (0.354 mm) or less; more preferably about 50 U.S. mesh (0.297 mm) or less, about 60 U.S. mesh (0.25 mm) or less, or about 70 U.S. mesh (0.21 mm) or less.
  • the particles of activated carbon in spheroids of the present invention may have on average a diameter of 0.5 mm or less, more preferably about 0.2 mm or less.
  • the particles of activated carbon in the spheroids of the present invention comprise powdered activated carbon.
  • An activated carbon spheroid according to the present invention may comprise any suitable binder.
  • the binder does not substantially interfere with the BET surface area of the activated carbon particles. Many substances have been found to substantially reduce the BET surface area of particles of activated carbon due to, for example, plugging of the pores or blocking access to the pores of the activated carbon.
  • the binder has a solubility in water of at least about 0.5 grams per 100 milliliters at room temperature. Such water soluble binders will enhance its rates of degradation in the environment relative to non- water soluble binders, because spheroids having water soluble binders may more rapidly break apart in the presence of environmental water.
  • use of the binder results in a spheroid exhibiting suitable hardness for processing in manufacture of smoking articles and filters for smoking articles and to resist or reduce particle breakthrough.
  • use of the binder results in a spheroid exhibiting a desired bed density and weight.
  • One suitable class of binder that may be used to produce activated carbon spheroids having one or more of these desired properties is alkylcellulose.
  • a binder may comprise any suitable alkylcellulose.
  • a binder may include an alkylcellulose having a structure according to Formula I:
  • each R is independently selected from H, Ci-C 6 straight or branched chain alkyl unsubstituted or substituted with hydroxyl; and where n is an integer greater than 2. Typically n is less than 1 ,000,000, and is often less than 100,000 or less than 10,000.
  • each R is independently selected from H, C1-C3 straight or branched chain alkyl unsubstituted or substituted with hydroxyl. More preferably, each R is independently selected from H, methyl or hydroxypropyl. Even more preferably, each R is independently selected from H or methyl. At least one R is not a hydrogen.
  • Methylcellulose is a particularly preferred binder for use in accordance with the present invention.
  • Spheroids of the present invention may be formed in any suitable manner.
  • the particles of activated carbon are mixed with a binder to produce a mixture.
  • the mixture may then be extruded to produce an extrudate.
  • the extrudate may then be spheronized to form an activated carbon spheroid.
  • the mixture is a homogenous mixture that is readily extrudable. More preferably, the mixture is a homogenous paste.
  • a mixture of powdered activated carbon and granular activated carbon may be used. Generally, powdered activated carbon, which may more readily form a paste than granules, is more preferable.
  • the mixture of activated carbon and binder may include any other suitable ingredients for forming a homogenous mixture.
  • the mixture may comprise water.
  • the mixture consists of, or consists essentially of, binder, water and particles of activated carbon. The amount of other ingredients, such as water, may be varied to achieve a mixture suitable for extruding and spheronizing.
  • the resulting mixture is extruded into rods having a diameter substantially the same as the desired diameter of the spheroid to be produced.
  • the resulting rods may then be spheronized in any suitable manner such as spheronizing in a spheronizer.
  • Suitable spheronizers include spherionizers having a disc that rotates, such as rotating friction discs.
  • the resulting spheroids may comprise any suitable amount of binder.
  • the spheroids comprise from about 1 % binder by weight to about 15% binder by weight, of the combined mixture of carbon and binder, such as methylcellulose. More preferably, the spheroids comprise between about 3% and about 10% binder by weight of the combined mixture of carbon and binder, such as methylcellulose.
  • the amount of binder used does not substantially interfere with the specific surface area of the activated carbon.
  • the weight percent of binder is preferably maintained within a range that decreases the specific surface area of a resulting spheroid by the percentage methylcellulose used in the spheroid.
  • the resulting spheroids may comprise any suitable amount of activated carbon.
  • the spheroids comprise greater than about 50% activated carbon by weight, such as greater than about 75% activated carbon by weight or greater than about 85% activated carbon by weight.
  • the resulting speheroids comprise less than about 99% activated carbon by weight, such as less than about 95% by weight.
  • the resulting speheriods comprise from about 50% to about 99% activated carbon by weight, such as from about 50% to about 95% by weight.
  • the resulting spheroids for use in filters or smoking articles of the present invention preferably has a specific surface area (BET) of about 500 m 2 /g or greater.
  • the activated carbon will have a BET of about 2500 m 2 /g or less.
  • the activated carbon has a BET in a range from about 1000 m 2 /g to about 2000 m 2 /g. More preferably, the activated carbon has a BET in a range from about 1100 m 2 /g to about 1800 m /g. More preferably, the activated carbon has a BET in a range from about 1100 m 2 /g to about 1600 m 2 /g or from about 1200 m 2 /g to about 1400 m 2 /g.
  • BET may be determined using an N 2 adsorption isotherm at -196 °C obtained in a volumetric Autosorb-6B apparatus from Quantachrome generally as described in the following (i) Gregg SJ, Sing KSW. Adsorption, Surface Science and Porosity. Academic Press, New York 1982; (ii) Rouquerol F, Rouquerol J, Sing K. Adsorption by powders and porous solids. Principles, methodology and applications. Academic Press, 1999; and (iii) Linares-Solano A, Salinas-Martinez de Lecea C, Alcafiiz-Monge J, Cazorla-Amoros D. Further advances in the characterization of Microporous carbons by Physical adsorption of gases.
  • the specific surface area of a spheroid may be determined according to ISO 9277 (2010): Determination of the specific surface area of solids by gas adsorption - BET method. Methods for determining specific surface area of microporous materials (type I isotherms) provided in an annex of ISO 9277 (2010) may be particularly useful for determining specific surface area of spheroids.
  • the binder does not block the pores of the activated carbon particles in the spheroid, and the specific surface area of spheroid is not substantially different than the specific surface area of the particles that were used to manufacture the spheroid.
  • methylcellulose reduced the specific surface area in an amount proportional to the weight percent of methylcellulose in the spheroid, which indicated that methylcellulose does not block pores of the activated carbon in the spheroid.
  • the activated carbon particles for used in filters or smoking articles of the present invention preferably has a hardness suitable for processing in existing bead insertion systems.
  • the activated carbon particle has a ball-pan hardness of greater than about 95%.
  • Ball pan hardness may be measured according to ASTM D3802-10, Standard Test Method for Ball-Pan Hardness of Activated Carbon (DOI: 10.1520/D3802-10).
  • Ball-pan hardness may provide an assessment of how resistant activated carbon is to particle degradation, with activated carbon having greater ball-pan hardness tending to have increased resistance to attrition.
  • Ball pan hardness is a widely used metric for establishing a measurable characteristic of an activated carbon that is related to dusting.
  • activated carbon particles for use in filters or smoking articles of the present invention has a ball pan hardness of about 95% or greater or 97% or greater. More preferably, activated carbon particles for use in filters or smoking articles of the present invention have a ball pan hardness of about 98%. It will be understood that activated carbon for use in filters or smoking articles of the present invention will generally have a ball pan hardness of less than 100%.
  • Resulting spheroids (about 0.1 g total) may be placed in a 10 mL vial with 15 stainless steel balls (0.18 g/ball) and shaken on a sieve shaker at about 1400 revolutions per minute (rpm) for 20 minutes.
  • the resulting content of the vial (less the stainless steel balls) is sieved on a 300 micrometer sieve and the weight of the content remaining on the sieve is determined.
  • the mass of the initial spheroids and the mass remaining on top of the sieve is compared.
  • the percent of mass lost may be used as an indicator of hardness of the spheroids, with those losing more mass being softer and those loosing less mass being harder.
  • the resulting spheres loose about 3% to about 25%; more preferably from about 5% to about 20%; and even more preferably from about 7% to about 18%.
  • Resulting spheroids for use in filters or smoking articles of the present invention may have any suitable density.
  • the density of the activated carbon particle will depend in part on the density of the source material and the carbonization and activation processes employed. Density can be determined by ASTM D2854-09 (2014), Standard Test Method for Apparent Density of Activated Carbon.
  • particles of activated carbon for use in filters of smoking articles of the present invention has a density from about 0.35 g/cm 3 to about 0.65 g/cm 3 . More preferably, particles of activated carbon for use in filters of smoking articles of the present invention has a density from about 0.4 g/cm 3 to about 0.60 g/cm 3 .
  • Resulting spheroids for use in filters or smoking articles of the present invention may be of any suitable mass.
  • the mass of the spheroid will depend in part on the mass of the source material for the activated carbon, the carbonization and activation processes employed, the amount of binder used, and the like.
  • the activated carbon particles have a mass in a range from about 5 mg to about 100 mg; more preferably from about 10 mg to about 60 mg.
  • spheroids have a weight from about 30 mg to about 60 mg, have a diameter from about 2.5 mm to 6 mm, have a specific surface area (BET) from about 1100 m 2 /g to about 1600 m 2 /g, and comprise activated carbon particles having a mesh size between 60 mesh (0.25 mm) and 120 mesh (0.125 mm).
  • BET specific surface area
  • filters and smoking articles that include activated carbon spheroids of the present invention exhibit less particle breakthrough than currently available filters and smoking articles that include activated carbon.
  • filters and smoking articles that include activated carbon spheroids of the present invention preferably exhibit less particle breakthrough than filters and smoking articles that include activated carbon derived from coconut shell and having a mesh size of 30 - 70 and a BET of 1100 m 2 /g.
  • Particle breakthrough can be determined by any suitable process.
  • particle breakthrough is measured via dry puff (unlit) analysis on a filter containing activated carbon.
  • Particle breakthrough is analyzed when the filter (optionally incorporated into a smoking article) is operably coupled to a smoking machine equipped with a particle counter configured to detect particles in the size range from about 0.3 micrometers to about 10 micrometers.
  • the particle counter is a laser light scattering particle counter, such as AEROTRAK® particle counter.
  • the smoking machine is preferably configured to take 12 puffs of 55 ml_ during 2 seconds every 13 seconds per filter (optionally incorporated into a smoking article).
  • particle breakthrough results are averaged from tests of a number of filters or smoking articles, such as five or ten or more filters or smoking articles.
  • Filters and smoking articles of the present invention can include activated carbon spheroids to which one or more sensory enhancing agent is sorbed.
  • the activated carbon particle can thus serve a dual purpose of removing one or more constituents from smoke and delivering the one or more sensory enhancing agent.
  • One or more sensory enhancing agents can be coated on or sorbed to activated carbon spheroid in any suitable manner.
  • a liquid or gaseous composition that includes one or more sensory enhancing agents can be applied to the activated carbon spheroid.
  • the activated carbon spheriod can be sprayed with a liquid composition comprising one or more sensory enhancing agents.
  • the activated carbon spheroid can be dipped in, incubated in, or placed in a stream of, a liquid composition comprising one or more sensory enhancing agents.
  • the activated carbon spheroid can be placed in a stream of, or incubated in a, gaseous composition comprising one or more sensory enhancing agents.
  • the liquid composition is applied to activated carbon spheroids in a fluidized bed.
  • activated carbon spheroids can be introduced into a vessel, a fluidizing gas can also be introduced into the vessel so as to fluidize the activated carbon spheroids, and a liquid composition comprising one or more sensory agent can be introduced into the vessel while the activated carbon particles are in a fluidized state as described in, for example, International Patent Application WO 03/71886 A1 , which is hereby incorporated herein by reference in its entirety to the extent that it does not conflict with the disclosure presented herein.
  • the one or more sensory agents in the liquid composition can adsorb or absorb to the activated carbon particles in the fluidized bed.
  • a composition comprising one or more sensory enhancing agents and one or more sensory enhancing agent-holding materials is applied to an activated carbon particle.
  • the one or more sensory enhancing agent-holding materials can include a film forming material and an emulsifying agent as needed.
  • film forming agents include glucan such as pullulan, maltodextrin and hydroxypropyl cellulose.
  • U.S. Patent Application US 20140123991A1 provides details regarding some suitable methods to apply flavorants and flavorant-holding materials to activated carbon, which methods can be modified and applied to application of sensory enhancing agents to activated carbon spheroids described in the present disclosure.
  • the disclosure of US 20140123991 A1 is hereby incorporated herein by reference in its entirety to the extent that it does not conflict with the disclosure presented herein.
  • the one or more sensory enhancing agents are coated on or sorbed to the activated carbon spheroid so that the sensory enhancing agents are retained by the particle during storage and are released during smoking of a smoking article that includes the activated carbon particle.
  • European Patent Application EP 263 0 879 A1 discloses cigarettes that include activated carbon having a specific surface area between 1500 m 2 /g and 1700 m 2 /g and having menthol sorbed at a sorption rate between 80% and 92%, relative to saturation with menthol.
  • EP 263 0 879 A1 discloses that the activated carbon can retain menthol during storage and only releases menthol during passage of tobacco smoke through the menthol-sorbed activated carbon.
  • the disclosure of EP 263 0 879 A1 is hereby incorporated herein by reference in its entirety to the extent that it does not conflict with the disclosure presented herein.
  • Any suitable sensory-enhancing agent may be coated on or sorbed to an activated carbon spheroid.
  • suitable sensory enhancing agents include flavorants, freshening agents, cooling agents, and hot effect agents.
  • suitable flavorants include aromatic or fragrance molecule as conventionally used in the formulation of flavoring or fragrance compositions.
  • the flavorant is an aromatic, terpenic or sesquiterpenic hydrocarbon.
  • the flavorant may be an essential oil, alcohol, aldehyde, phenolic molecule, carboxylic acid in their various forms, aromatic acetal and ether, nitrogenous heterocycle, ketone, sulfide, disulfide and mercaptan which may be aromatic or non-aromatic.
  • flavoring agents include natural or synthetic aromas or fragrances.
  • suitable fragrances are fruity, confectionery, floral, sweet, woody fragrances.
  • suitable aromas are coconut, vanilla, coffee, chocolate, cinnamon, mint, or roasted or toasted aromas.
  • Suitable freshening agents may be, but are not limited to, menthyl succinate and derivatives thereof.
  • a suitable hot effect agent may be, but is not limited to, vanillyl ethyl ether.
  • menthol is a sensory enhancing agent that is coated on or sorbed to an activated carbon spheroid.
  • the concentration of sensory-enhancing agent coated on or sorbed to an activated carbon spheroid can be adjusted or modified to provide a desired amount of the sensory- enhancing agent.
  • one or more sweeteners are coated on or sorbed to the activated carbon spheroid.
  • the sweeteners can be applied to the particles in, for example, a solution or suspension in ethanol.
  • suitable sweeteners include, but are not limited to, sorbitol, aspartame, saccharine, NHDC, sucralose, acesulfame, and neotame.
  • One or more activated carbon spheroids may be placed in a smoking article downstream of a smokable material in any suitable manner.
  • the term "downstream" refers to relative positions of elements of the smoking article described in relation to the direction of mainstream smoke as it is drawn from a smokable material and into a user's mouth.
  • the one or more activated carbon spheroids are placed in a filter element.
  • One or more activated carbon spheroid may be placed within a void or cavity in the filter.
  • the one or more activated carbon spheroids may be placed in one or more cavity in a plug-space-plug configuration.
  • the filter may contain a plurality of filter elements into which one or more activated carbon spheroids may be placed.
  • an activated carbon particle is embedded in filter material, such as cellulose acetate tow or a polylactic acid filter.
  • filter material such as cellulose acetate tow or a polylactic acid filter.
  • the spheroid can be embedded in a filter material in a manner similar to how flavor-containing breakable capsules are incorporated into filters of cigarettes.
  • the smoking article or filter element includes only one activated carbon spheroid.
  • the diameter of the activated carbon spheroid is similar to or less than the corresponding dimensions of a filter into which the activated carbon spheroid is expected to be inserted.
  • a filter segment has a diameter from about 3.6 mm and about 6.5 mm, and the diameter of the activated carbon spheroid, has a diameter from about 2.5 mm and about 4.5 mm.
  • a filter having a diameter of about 6.1 mm may be used in a "slim cigarette" having an overall diameter of about 7.0 mm.
  • the filter segment and the activated carbon spheroid are circular in cross section, the diameter of the filter segment is from about 3.6 mm and about 5.5 mm, and the diameter of the activated carbon spheroid is from about 3.0 mm and about 3.5 mm.
  • a filter having a diameter of less than about 4.5 mm may be used in a "super slim cigarette" having an overall diameter of less than about 5.4 mm.
  • the filter segment and the activated carbon spheroid are circular in cross section, the diameter of the filter segment is from about 3.6 mm and about 4.5 mm, and the diameter of the activated carbon spheroid is from about 3.0 mm and about 3.5 mm.
  • a filter having a diameter of about 3.8 mm may be used in a "micro slim cigarette" having an overall diameter of about 4.7 mm.
  • smoking article includes cigarettes, cigars, cigarillos and other articles in which a smokable material, such as a tobacco, is lit and combusted to produce smoke.
  • a smokable material such as a tobacco
  • smoking article also includes articles in which smokable material is not combusted, such as but not limited to smoking articles that heat a smoking composition directly or indirectly, or smoking articles that use air flow or a chemical reaction, with or without a heat source, to deliver nicotine or other materials from the smokable material.
  • an aerosol produced by a smoking article is used to describe an aerosol produced by a smoking article.
  • An aerosol produced by a smoking article may be, for example, smoke produced by combustible smoking articles, such as cigarettes, or aerosols produced by non-combustible smoking articles, such as heated smoking articles or non-heated smoking articles.
  • activated carbon spheroid is a spheroid comprising particles of activated carbon and a binder.
  • FIG. 1 is a schematic perspective view of an embodiment of a partially unrolled smoking article.
  • FIGS. 2-3 are schematic longitudinal sectional views of embodiments of filters including an activated carbon particle.
  • the smoking articles and filters depicted in FIGS. 1-3 illustrate embodiments of smoking articles or components of smoking articles described above.
  • the schematic drawings are not necessarily to scale and are presented for purposes of illustration and not limitation.
  • the drawings depict one or more aspects described in this disclosure. However, it will be understood that other aspects not depicted in the drawings fall within the scope and spirit of this disclosure. Referring now to FIG. 1 , a smoking article 10, in this case a cigarette, is depicted.
  • the smoking article 10 includes a rod 20, such as a tobacco rod, and a mouth end filter 30 that includes filter material 32, such as cellulose acetate tow or polylactic acid filter material.
  • the depicted smoking article 10 includes plug wrap 60, cigarette paper 40, and tipping paper 50.
  • the plug wrap 60 circumscribes at least a portion of the filter 30.
  • the cigarette paper 40 circumscribes at least a portion of the rod 20.
  • Tipping paper 50 or other suitable wrapper circumscribes the plug wrap 60 and a portion of the cigarette paper 40 as is generally known in the art.
  • the filter 30 includes an activated carbon spheroid, which may be placed as depicted in, for example, FIG. 2 and FIG. 3.
  • FIG. 2 illustrates an embodiment where filter 30 is in a plug 32-space 33-plug 34 configuration.
  • Plug 32 is the mouth end plug and is preferably white cellulose acetate tow.
  • Activated carbon spheroid 80 is disposed in void space 33 between plugs 32 and 34.
  • FIG. 3 illustrates an embodiment where filter 30 activated carbon spheroid 80 is embedded in filter material 32.
  • One objective of the studies presented herein was to produce activated carbon spheroids having a diameter of about one millimeter or greater, having a hardness within a desired range in light of particular commercially available activated carbon granules, and having a specific surface area of from about 1100 m 2 /g to about 1800 m 2 /g.
  • suitable activated carbon and binder were needed.
  • a number of binders were tested, including organic binders and inorganic binders. Specifically, molasses, starch, methylcellulose, cements and clays were tested. Methylcellulose was selected for further study due to its high efficiency for producing very hard activated carbon spheroids through a simple and easy process.
  • Activated carbon spheroids have been successively prepared with different commercial powdered activated carbons and methyl-cellulose as a binder. All the spheroids produced achieved the desired characteristics in term of BET surface area (1100 m 2 /g and 1800 m 2 /g), having a hardness higher than the commercially available granulated activated carbon (“GAC- 0"), which served as a reference, and having selected desired porosity (microporosity and/or mesoporosity).
  • GAC- 0 commercially available granulated activated carbon
  • the spheroids were produced from a homogeneous paste consisting of a powdered activated carbon, a binder (methyl-cellulose) and water.
  • Table 1 shows the variety of activated carbons used, which have different surface areas, pore volumes, and origins.
  • the particles activated carbon, methylcellulose and water were mixed to form a paste.
  • a series of experiments were performed varying the percentage of methylcellulose added to the activated carbon (hereafter expressed at % in respect of the weight of the mixture of carbon and methylcellulose employed).
  • the amount of each component was varied to, among other things, arrive at a carbonaceous paste suitable for extrusion.
  • Methylcellulose was varied from 3% to 10%.
  • the amount of water to be added was also studied. Different samples were prepared keeping constant the activated carbon and the % methylcellulose and varying the amount of water added. Once the amount of water to be added was known, it was determined whether the manner in which the water was added affected the results. It should be noted that for a given mixture composition, the order in which the components were added had no substantial effect on the results.
  • the prepared mixtures were stirred at room temperature until a homogeneous paste was formed that had a suitable viscosity to be extruded and spheronized.
  • the pastes dried and hardened after a few minutes at room temperature.
  • Many of the resulting activated carbon spheroids were sufficiently hard and had desired textural properties as a function of the characteristics of the selected activated carbon.
  • the porosity of the activated carbon spheroids depended on the porosity of the selected particles of activated carbon. Different batches of particles of activated carbon were studied to obtain hard activated carbon spheroids with different porosities.
  • the porous texture characterization of the different activated carbons was performed as follows. Physical adsorption of gases (N 2 at -196 °C and C0 2 at 0 °C) was determined using an Autosorb 6-B apparatus (Quantachrome Corporation). Nitrogen adsorption at - 196 °C was used for determining the total volume of micropores (pore size smaller than 2 nm) applying the Dubinin-Radushkevich equation and for determining the apparent BET surface area, whereas the adsorption of CO2 at 0 °C was used to assess the narrow micropores (pore size smaller than 0.7 nm) also by application of the Dubinin-Radushkevish equation.
  • the total pore volume (VT) was determined by nitrogen adsorption volume at a relative pressure of 0.99 like and average pore size.
  • Figure 4 shows the N 2 adsorption isotherms of selected activated carbons, which cover a wide range of adsorption capacities and pore size distributions. The majority of these activated carbons are microporous, although samples D and F have a remarkable presence of mesoporosity.
  • H 3190 1.34 0.70 0.12 1.78 0.52 An insufficient amount of binder lead to activated carbon spheroids that were too soft, and a high percentage of binder accelerated the hardening step making subsequent extrusion and spheronization difficult, if not impossible. Accordingly, to prepare a suitable paste mixture, a suitable wt. % of binder should be assessed to provide a paste that may be extruded and spheronized.
  • Preliminary test revealed that powdered activated carbon having a high porosity tends to be more difficult to spheronize with a low methylcellulose %, such as 3% methylcellulose, and resulted in lower hardness than a higher methylcellulose %, such as 10% methylcellulose.
  • the amount of binder to be used depends in part on the porosity of the selected powdered carbon materials, with higher quantities of methylcellulose, such as 10%, providing suitable hardness when more microporous activated carbon was used as the raw material.
  • methylcellulose decreases the specific surface area of a resulting spheroid is merely by the percentage methylcellulose used in the spheroid, indicating that methylcellulose does not block pores of the activated carbon in the spheroid.
  • methylcellulose decreases the adsorption capacity proportionally to the wt. % of methyl cellulose used. Table 3 shows for two selected activated carbons (GAC-0 and re-activated GAC-0) and for the three different weight percentages of methylcellulose studied (3, 6 and 10 %) the BET surface area decreases proportionally with the increase of binder.
  • % decrease on the BET corresponds very well with the % on binder which confirms that the binder has no porosity and interestingly does not block the porosity of the activated carbon.
  • Table 3 shows that the adsorption capacity of the original powdered activated carbon decreases proportionally to its wt. % of binder content. This observation confirms that methylcellulose is a non-porous compound and it does not block the porosity of the activated carbon used.
  • the hardness of the activated carbon spheroids was determined as follows. Resulting spheroids (about 0.1 g total; about 30 mg per sphere) were placed in a 10 ml vial with 15 stainless steel balls (0.18 g/ball) and shaken on a sieve shaker at about 1400 revolutions per minute (rpm) for 20 minutes. The resulting content of the vial (less the stainless steel balls) was sieved on a 300 micrometer sieve and the weight of the content remaining on the sieve was determined. The mass of the initial spheroids and the mass remaining on top of the sieve was compared. The percent of mass lost was used as an indicator of hardness of the spheroids, with those losing more mass being softer and those loosing less mass being harder.
  • Figure 5 clearly shows the effect that the wt. % of methyl-cellulose have on the N 2 adsorption isotherms, and hence, on the adsorption capacity of the resulting samples.
  • Figure 5 plots, as an example, the adsorption isotherms of two samples (E and C) without binder and with 3, 6 and 10 wt. %.
  • the amount of water used to prepare the mixture was reflected in the viscosity of the paste. It was expected that too much water would lead to a paste that was too fluid, whereas using an insufficient amount of water would result in a paste that was too viscous to be extruded or spheronized. Accordingly, a suitable amount of water to use was analyzed, using the same raw material (C), the same amount of binder (10%) and different volumes of H 2 0 added (from 1.5 and 3 ml) as detailed in Table 4.
  • this method has several advantages and allows easy preparation of hard activated carbon spheroids having tailored porosity and specific surface area.
  • activated carbon spheroids should not be exposed to temperatures above about 200-250 °C prior to placing in a smoking article or filter because the
  • methylcellulose binder may decompose around 300 °C.
  • activated carbon spheroids having properties desirable for use in smoking articles or filters for smoking articles can be formed by selecting activated carbon starting material having desired properties and forming spheroids from the activated carbon material using methylcellulose as a binder.
  • Other alkylcellulose binders may also be used in binders.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)

Abstract

L'invention concerne un article pour fumeur comprenant un matériau à fumer et un sphéroïde comprenant des particules de charbon actif et un liant. Le liant comprend de préférence de l'alkylcellulose, de préférence de la méthylcellulose. De préférence, le sphéroïde comprend d'environ 1% à environ 15% en poids du liant. De préférence, les particules de charbon actif présentent un diamètre inférieur à 0,5 mm, de préférence inférieur à 0,2 mm. De préférence, les particules de charbon actif comprennent de la poudre de charbon actif. De préférence, le sphéroïde comprend plus de 50% en poids de charbon actif. Le sphéroïde est situé en aval du matériau à fumer. Le sphéroïde présente un diamètre compris dans une plage de 1 mm à 8 mm, de préférence de 2 mm à 7 mm, et de préférence encore de 2,5 mm à 6 mm.
PCT/IB2016/058080 2016-01-25 2016-12-29 Sphéroïdes de charbon actif pour articles pour fumeurs WO2017130045A1 (fr)

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CN112089093A (zh) * 2020-10-13 2020-12-18 云南养瑞科技集团有限公司 一种增香降解塑料颗粒的制备方法及应用
CN113841922A (zh) * 2021-10-09 2021-12-28 湖北中烟工业有限责任公司 一种复合香型烟用香精香料的制备方法及其应用

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EP4260715A4 (fr) * 2020-12-11 2024-08-21 Shenzhen Global Greenland New Mat Co Ltd Application de carbone sphérique dans l'adsorption de gaz de combustion d'un produit à base de tabac à chauffage sans combustion

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CN108669663A (zh) * 2018-05-31 2018-10-19 赵雪 一种加热不燃烧卷烟
CN108669663B (zh) * 2018-05-31 2024-03-29 乐美星辰(深圳)生物科技有限公司 一种加热不燃烧卷烟
CN112089093A (zh) * 2020-10-13 2020-12-18 云南养瑞科技集团有限公司 一种增香降解塑料颗粒的制备方法及应用
CN113841922A (zh) * 2021-10-09 2021-12-28 湖北中烟工业有限责任公司 一种复合香型烟用香精香料的制备方法及其应用
CN113841922B (zh) * 2021-10-09 2023-03-10 湖北中烟工业有限责任公司 一种复合香型烟用香精香料的制备方法及其应用

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