WO2005104771A2 - Particule a charge aromatique elevee et procede d'elaboration - Google Patents

Particule a charge aromatique elevee et procede d'elaboration Download PDF

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Publication number
WO2005104771A2
WO2005104771A2 PCT/US2005/014548 US2005014548W WO2005104771A2 WO 2005104771 A2 WO2005104771 A2 WO 2005104771A2 US 2005014548 W US2005014548 W US 2005014548W WO 2005104771 A2 WO2005104771 A2 WO 2005104771A2
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WO
WIPO (PCT)
Prior art keywords
particle
oil
flavor
particles
ethyl
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Application number
PCT/US2005/014548
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English (en)
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WO2005104771A3 (fr
Inventor
Deborah Kennison
Original Assignee
Chr. Hansen A/S
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Application filed by Chr. Hansen A/S filed Critical Chr. Hansen A/S
Publication of WO2005104771A2 publication Critical patent/WO2005104771A2/fr
Publication of WO2005104771A3 publication Critical patent/WO2005104771A3/fr

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Classifications

    • 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
    • A24D1/002—Cigars; Cigarettes with additives, e.g. for flavouring
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
    • 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
    • A24B15/281—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
    • A24B15/282—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by indirect addition of the chemical substances, e.g. in the wrapper, in the case
    • 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
    • A24B15/281—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
    • A24B15/283—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by encapsulation of the chemical substances

Definitions

  • the present invention relates to high flavor load particles and to methods of preparing same.
  • the invention also relates to methods of using such particles to flavor tobacco products, including cigarettes and other conventional smoking articles.
  • Flavoring agents that are added to tobacco products, including cigarettes, are typically subjected to combustion as the tobacco burns. The combustion of such agents can result in the formation of harmful substances, at least some of which are considered carcinogenic.
  • flavoring agents are first added to the tobacco leaf by spraying dilute solutions of the flavoring agents directly onto the cut leaf, or by applying liquid or dry flavoring agents during the reconstituted sheeting process.
  • the amount of dry or liquid flavoring agent applied directly to reconstituted sheet filler or directly to the leaf can be as high as 4-5% of the cigarette filler weight.
  • the reconstituted sheeting consists of sheeted stem, seeds, and/or roots from the- tobacco plant; waste dust resulting from cigarette manufacture and collected from the production plant floor can also be included.
  • Reconstituted sheet can comprise 10-20% of the cigarette rod weight.
  • Liquid flavoring agents are also sometimes sprayed onto the filter cellulose of cigarettes and are delivered with the steam that is entrained through the cigarette rod. Only small amounts of the flavoring agents can be applied, otherwise they will interfere with the smoke taste and perception in the mouth. Spray-dried flavoring agents have been attempted but it has been found that they are susceptible to migration through the filter, with the potential to be inhaled into the lungs.
  • the present invention relates to an improved approach to delivering flavor to tobacco products, such as cigarettes and other conventional smoking • articles (e.g., cigars and cigarillos) .
  • the invention provides, for example, a "safer" traditional cigarette that results in reduced harm to the lungs of the smoker while imparting enhanced flavor impact.
  • spheronized particles embedded with flavoring agent (s) are positioned in the tobacco product, such as a cigarette, such that they do not undergo combustion, thereby avoiding production of harmful pyrolysis products.
  • the instant particles can be positioned in the filter cavity of a traditional cigarette between the tobacco rod and the cellulose filter. The particles are of sufficient size and durability that they do not become dislodged.
  • the present invention relates to high flavor load spherical particles (advantageously, symmetrically spherical) comprising a matrix material (e.g., a porous matrix material) that can absorb many times its weight in fluid, and at least one flavoring agent and/or excipient and/or aerosolizing agent.
  • a matrix material e.g., a porous matrix material
  • the instant particles make it possible for the tobacco industry to provide to the public a "safer" traditional cigarette that delivers flavors and/or excipients in a non-pyrolized form.
  • the invention includes the spherical particles, as well as intermediates in the process of producing such particles, including a semi-dry dough or paste resulting from mixing of the matrix material with the flavoring agent and/or excipient.
  • the invention also includes a method of preparing the spherical particles, for example, a method in which a low pressure extrudate is converted into spherical granules through a spheronization process.
  • the invention further includes a cigarette-type smoking article comprising the particles of the invention. Release of flavor from the particles is obtained through non-pyrolysis steam entrainment .
  • FIGURE 1 is a flow chart of the process of making the particles of the invention.
  • FIGURE 2 is a longitudinal cross section of an exemplary embodiment of the invention.
  • the present invention relates to particles (e.g., spherical particles) comprising a matrix (e.g., a porous matrix) and at least one material (e.g., a flavoring agent) embedded (“loaded") therein.
  • the particles are suitable for use in the tobacco industry, particularly, in the production of cigarettes and other conventional smoking articles (e.g., cigars, cigarillos, etc).
  • the matrix of the spherical particles of the invention can comprise cellulose, modified cellulose, or other carbohydrate (such as natural or synthetic gum, pectin or starch) , natural or synthetic protein (for example, gelatin), or other material (e.g., low dextrose equivalent carbohydrate (e.g., corn, rice or hydrolyzed cereal (grain) solids) ) (or mixtures thereof) that, preferably, can absorb many times its weight in fluid (advantageously, about two to five times) .
  • the matrix is cellulose as it has good particle integrity, it is insoluble in water, it is compatible with tobacco regulatory practice and appears on the tobacco 599 list. More preferably, the matrix is microcrystalline cellulose.
  • the matrix is loaded with a flavoring agent (e.g., vanillin, cocoa, licorice, menthol or other synthetic or natural material within the FEMA GRAS list permissible within tobacco additive law and that appears on the tobacco 599 list) and/or a substance that promotes aerosolization, such as glycerin, or other polyol (e.g., propylene glycol or triethylene glycol) .
  • a flavoring agent e.g., vanillin, cocoa, licorice, menthol or other synthetic or natural material within the FEMA GRAS list permissible within tobacco additive law and that appears on the tobacco 599 list
  • a substance that promotes aerosolization such as glycerin, or other polyol (e.g., propylene glycol or triethylene glycol)
  • the amount of absorbed aerosolization promoting agent can be 1% to 40%, preferably 10%-35%, more preferably 28% - 30% w/w of the particle.
  • the particles can also comprise one
  • diatomaceous earth shown to absorb fat and oil based compounds such as botanical tar
  • silica or silicates shown to absorb water and oil based compounds
  • the particles of the invention can further comprise a thin coating that protects the loaded matrix during storage.
  • the coating can range from about 2.5% of the weight of the particle to about 15% of the weight of the particle.
  • One such coating comprises, for example, hydroxypropyl methyl cellulose or carboxymethyl cellulose.
  • the particles of the invention can also comprise a coating (e.g., a polymer coating, for example, a Food Grade edible polymer permissible within the tobacco regulation (i.e., the tobacco 599 list) that serves to sustain release of the flavoring agent and/or other material embedded in the matrix. Coatings of about 2.5% to about 15% of particle weight can be used.
  • the particles of the invention are preferably symmetrical and from about 0.3 millimeters (mm) to about 10 mm in diameter, more preferably about 0.3 mm to about 1.5 mm and still more preferably about 0.7 mm to about 1.2 mm in diameter.
  • a US sieve size 14 should accommodate about 95% of 0.7 mm particles.
  • Particles of the invention can be prepared using, for example, a process that includes the production of a low-pressure extrudate that is converted into spherical granules through a spheronization process.
  • particles can be prepared by the following process: i) Mixing dry matrix and material to be loaded (e.g., liquid flavoring agent or solution (advantageously aqueous, however, hydrophobic solutions can be used) of flavoring agent and/or aerosolizing agent) in, for example, a planetary mixer - advantageously, the material to be loaded does not exceed 75% W/W of the resulting composition and the matrix is not less than 25% W/W of the resulting composition.
  • the composition is mixed until a malleable dough-like paste is formed and all liquid has been uniformly absorbed onto the matrix.
  • material to be loaded e.g., liquid flavoring agent or solution (advantageously aqueous, however, hydrophobic solutions can be used) of flavoring agent and/or aerosolizing agent) in, for example, a planetary mixer - advantageously, the material to be loaded does not exceed 75% W/W of the resulting composition and the matrix is not less than 25% W/W of the resulting composition.
  • the composition is mixed until
  • a die press channel for the extruder is selected based on the desired size of the finished spheres (typically, the diameter of the die press channel ranges from 0.1 mm- 10.0 mm, 0.7 mm being preferred) .
  • the size selected defines the cross-section of the extrudate rods produced.
  • Other parameters to be determined include the temperature of the cooling jacket shaft around the extruder screw, the roller speed and the gear speed, and the pressure at the dieface (optimum conditions will be depend, for example, on the extruder used and material extruded) .
  • step (i) The dough-like paste resulting from step (i) can then be introduced (manually or automatically) into the extruder selected of step (ii) (which is preferably a low-pressure extruder in which the temperatures at the dieface surface are lower, which minimizes volatile flavoring agents absorbed in the dough from flashing off, as would be the case in a high pressure extruder.
  • Introduction (feed) of the dough-like paste into the input shaft can be performed in batches (Batch Mode) or continuously (Continuous Mode) , or a Batch-Continuous method can be used. Feed and output rates are determined by the roller, which is a shaft within the extruder that pulls the dough into the screws so that the screws can push the dough through the dieface.
  • the extruder can be single, twin or axial twin screw and can be designed for gravity feed and low pressure extrusion.
  • the extrudate resulting from step (iii) has a rod shape and the rods can be collected and transferred (manually or by machine) directly into the spheronizing unit.
  • the rods can be gravity fed into the spheronization chamber and are allowed to fall onto the spinning friction plate.
  • the spinning rate of the friction plate is, advantageously, about 80 RPM.
  • the friction plate propels the particles against the jacketed walls of the unit by centrifugal force, whereby the rods are broken into smaller segments . Centrifugal and gravitational forces create a mechanically fluidized ring of these smaller segments or particles.
  • step (iv) The semi-moist uniform spheres resulting from step (iv) can be discharged into a fluid bed dryer and dried to the desired moisture content, which typically ranges from 2-8%.
  • the spheres can also be thin film coated if desired.
  • Extruders suitable for use in the preset method include those made by, for example, LCI, 4409-C Chesapeake Drive, P.O. Box 16348, Charlotte, N.C.
  • Spheronizing units suitable for use include those made by, for example, LCI, Hosokawa Bepex, and Caleva.
  • Particles prepared using the above-described method are substantially uniform in size and weight and typically larger (for example, about 60-80 mesh) than particles resulting from traditional spray-drying processes (100-120 mesh). These characteristics have advantages when machine filling is used in the preparation of the ultimate smoking article. The ability to control particle size makes it possible to deposit an exact number of particles, uniform in size and shape.
  • a single particle having a large diameter can also be used (for example, a single pellet large enough (about 5 mm) to occupy a space in a traditional cigarette between the filter and the tobacco) .
  • the smooth surface of particles produced by the spheronization process allows any coating to be uniformly applied.
  • the mixing and extrusion steps of the process of the invention in contrast to the traditional spray- drying process, result in the production of particles that are also uniform with respect to concentration of the material (e.g., flavoring agent) embedded within the matrix.
  • the particle preparation methods described herein result in high yields, losses of other than moisture are minimal.
  • recoveries of about 98% of cellulose and non-water soluble components such as, for example, propylene glycol, glycerin, botanical matter, and FEMA (Flavor Extract Manufacturers Association) GRAS (Generally Accepted As Safe) chemicals
  • the present method is non-dusting for production application in comparison with traditional methods. Even a layman with a visual check can easily determine a reduced dusting, because a reduced dusting results when the product of the invention is shaken or moved, in comparison with that of the traditional method.
  • the particles of the invention can be present, for example, in a traditional cigarette between the tobacco rod and the cellulose filter. The number of particles used can vary, for example, with the particle size.
  • the particles occupy about 3 mm to about 10 mm of the overall length of the cigarette.
  • the particles can be loaded into the cigarette mechanically.
  • a smokable article e.g., a cigarette, that embodies the instant invention.
  • the cigarette generally indicated 10, comprises a cylindrical rod 12 containing smokable material 14 (e.g., tobacco) wrapped in at least one layer of a circumscribing outer wrapping material 16 (e.g., paper) , and a filter element 18.
  • smokable material 14 e.g., tobacco
  • a circumscribing outer wrapping material 16 e.g., paper
  • the flavoring agent (s) is/are released from the particles by a indirect heating method within a filter system wherein steam from the burning tobacco stick is pulled through the filter. The moisture causes the particle matrix (e.g., cellulose) to swell. The flavoring agent is then displaced from the particle and mixes with the moist steam and is entrained through the filter system. As the flavoring agent (s) are not combusted, pyrolysis products, such as tar, hydrocarbons and nitrosamines, are not produced.
  • the primary function of the instant particles is to serve as a delivery for non-combusted flavoring agents within, for example, a cigarette filter system.
  • the particles particularly particles that include additives such as charcoal, diatomaceous earth, silica, silicates and/or cyclodextrins, can act as a filtration device for harmful compounds contained in, for example, cigarette smoke. Certain aspects of the present invention are described in greater detail in the non-limiting Examples that follow.
  • Particles of the invention can be prepared using the process that follows :
  • a hydrophilic flavor agent is applied to a dry matrix comprising of microcrystalline cellulose at a 50/50 w/w ratio to form a dough-like paste .
  • the dough resulting from step 1 is fed, automatically or manually, into a low-pressure extruder and extruded through a die face grid screen with a preferred grid size of 0.5mm- 1.0mm, which defines the cross section of the particle rod.
  • the extruder can be single or twin screw or axial twin screw, which is designed for gravity feed and low pressure extrusion or jacketed cooling of the extruder shaft.
  • the unit has the capacity to extrude rods down -to 0.3mm with rod integrity.
  • the rods resulting from step 2 are delivered, manually or by machine, to a spheronizing unit.
  • the spheronizer comprises a vertical cylinder with a discharge shaft or port, a circular multi baffled "friction" plate (e.g., lmm-5mm disk) and a variable speed drive train
  • the rods are fed into the spinning friction plate chamber at 80 RPM for 1.5-3 minutes.
  • the friction plate propels the rods against the inside wall of the unit by centrifugal force and, as a result, the rods are broken into smaller segments. Centrifugal and gravitational forces create a mechanically fluidized ring of particles. Collisions with the wall, the baffled friction plate and other particles, results in plastic deformation of each granule, which gives rise to the creation of a uniform spherical shape.
  • the time the particles spend in this unit is referred to as the "resonance time" or the spheronization time, and it equals the time it takes to form spheres from the total volume of extrudate rods . 5.
  • the semi-moist spheres resulting from step 4 are then dried in a belt fluid bed system until the desired moisture content is achieved. 6.
  • the semi-moist spheres are finally thin film coated.
  • Described below is a process to deliver flavor post rod filler in a cavity beneath a cigarette filter. Theoretically, cellulose will swell, discharging flavor into entrained air flow.
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 1, Acetic Acid ⁇ 100, Acetophenone ⁇ 10, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 1, Benzoin Resinoid ⁇ 50, Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 10, Bornyl Acetate ⁇ 1, Butyric Acid ⁇ 1, Cardamon Seed Oil ⁇ 1, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 1, Chamomile Flower Oil Hungarian ⁇ 5, Chamomile Flower Oil Roman ⁇ 5, Cinnamic Aldehyde ⁇ 50, Cinnamic Alcohol ⁇ 1, Citral ⁇ 1, Citric Acid ⁇ 1, D,L Citronellal ⁇ 1, Clary Sage Oil ⁇ 5, Cocoa and Cocoa extracts ⁇ 100, Coffee Extract ⁇ 50, Cognac oil Green ⁇ 1,
  • the process comprises the following steps:
  • E) collect damp extrudate rods and deposit into a Maumerizing/Spheronizing centrifugal unit - parameters are: 2.0 mm disk plate at a speed of 1200 rpm for a resonance time of 3 minutes; and F) dry in Glatt Fluid Bed Dryer ( ⁇ 90°C) target moisture is ⁇ 20%.
  • the resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade.
  • the cigarette can be lit in a conventional manner and flavor delivery evaluated.
  • Described below is a process to deliver higher flavor load post rod filler in a cavity beneath the filter. As above, the cellulose will swell, discharging flavor into entrained air flow.
  • Tobacco Type (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 0.5, Acetic Acid ⁇ 100, Acetophenone ⁇ 2.5, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.5, Benzoin Resinoid ⁇ 25, Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 0.5, Bornyl Acetate ⁇ 0.5, Butyric Acid ⁇ 0.5, Cardamon Seed Oil ⁇ 0.5, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.5, Chamomile Flower Oil Hungarian ⁇ 2.5 , Chamomile Flower Oil Roman ⁇ 2.5, Cinnamic Aldehyde ⁇ 25, Cinnamic Alcohol ⁇ 0.5, Citral ⁇ 0.5, Citric Acid ⁇ 0.5, D,L Citronellal ⁇ 0.5, Clary Sage Oil ⁇ 2.5, Cocoa and Cocoa extracts ⁇ 100,
  • Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (45.55 %W/W wet basis, 79.78 % load dry basis), iii) Deionized water (45.45 %W/W wet basis)
  • Described below is a process to deliver ultra high flavor load post rod filler in a cavity beneath the filter. Again, cellulose will swell, discharging flavor into entrained air flow.
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 0.25 Acetic Acid ⁇ 100, Acetophenone ⁇ 2.5, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.25, Benzoin Resinoid- ⁇ 12.5 , Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 2.5 , Bornyl Acetate ⁇ 0.25 Butyric Acid ⁇ 0.25, Cardamon Seed Oil ⁇ 0.25, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.25, Chamomile Flower Oil Hungarian ⁇ 1.25, Chamomile Flower Oil Roman ⁇ 1.25, Cinnamic Aldehyde ⁇ 12.5, Cinnamic Alcohol ⁇ 0.25, Citral ⁇ 0.25, Citric Acid ⁇ 0.25, D,L Citronellal ⁇ 0.25, Clary Sage Oil ⁇ 0.25, Cocoa and Cocoa extracts
  • the process comprises the same steps used in Examples 2 and 3.
  • the resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.07 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade.
  • the cigarette can be lit in a conventional manner and flavor delivery evaluated. In this procedure, flavor seemed to leach out of spheres, and this flavor load may be too high and should be optimized.
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 0.25 Acetic Acid ⁇ 100, Acetophenone ⁇ 2.5, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.25, Benzoin Resinoid ⁇ 12.5 , Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 2.5 , Bornyl Acetate ⁇ 0.25 Butyric Acid ⁇ 0.25, Cardamon Seed Oil ⁇ 0.25, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.25, Chamomile Flower Oil Hungarian ⁇ 1.25, Chamomile Flower Oil Roman ⁇ 1.25, Cinnamic Aldehyde ⁇ 12.5, Cinnamic Alcohol ⁇ 0.25, Citral ⁇ 0.25, Citric Acid ⁇ 0.25, D,L Citronellal ⁇ 0.25, Clary Sage Oil ⁇ 0.25, Cocoa and Cocoa extracts
  • the process comprises the steps used above in Examples 2-4.
  • the resulting spheres can be introduced into a cigarette rod as described in Example 4 and flavor delivery evaluated. This loading was optimal for a partially hydrophylic compound.
  • Described below is a process to deliver higher flavor load post rod filler in a cavity beneath the filter.
  • This flavor contains high essential oil levels and the formula is optimized accordingly.
  • Cellulose can be expected to swell, discharging flavor into entrained air flow.
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 0.5, Acetic Acid ⁇ 100, Acetophenone ⁇ 2.5 , Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.5, Benzoin Resinoid ⁇ 25, Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 0.5, Bornyl Acetate ⁇ 0.5, Butyric Acid ⁇ 0.5, Cardamon Seed Oil ⁇ 0.5, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.5, Chamomile Flower Oil Hungarian ⁇ 2.5, Chamomile Flower Oil Roman ⁇ 2.5, Cinnamic Aldehyde ⁇ 25, Cinnamic Alcohol ⁇ 0.5, Citral ⁇ 0.5, Citric Acid ⁇ 0.5, D,L Citronellal ⁇ 0.5, Clary Sage Oil ⁇ 2.5, Cocoa and Cocoa extracts ⁇ 100
  • Microcrystalline cellulose (Avicel PH101) (FMC Corp.) (48.78 %W/W wet basis, 80.00 load dry basis), iii) Deionized water (41.46 %W/W wet basis) .
  • the process comprises the following steps:
  • Menthol is not completely soluble and will polymerize on the surface of the spheres, not embedding completely within the matrix. This is optimum loading for menthol delivery. As noted above, cellulose will swell, discharging menthol into entrained air aerosol air flow.
  • the process comprises the following steps: A) preblend Avicel, activated charcoal and diatomaceous earth in a V-Blender until uniform; Al) add flavor to the above mixture in a planetary mixer, while mixing;
  • Menthol is not completely soluble and will polymerize on the surface of the spheres, not embedding completely within the matrix. This is optimum loading for menthol delivery. Theoretically, cellulose will swell, discharging menthol into entrained air aerosol air flow. After observation of spheres upon storage, some polymerizaton occurred, indicating further optimization of the level, ⁇ -cyclodextrin was added to the matrix for covalent bonding of menthol.
  • the process comprises the following steps: A) mix Avicel and cyclodextrin in a V-Blender until visually uniform; B) add menthol solution and blend until visually uniform;
  • Described below is a process to deliver high flavor load post rod filler in a cavity beneath the filter.
  • This flavor contains both flavor with menthol and the formula is optimized accordingly. Again, theoretically, cellulose will swell discharging flavor into entrained air flow.
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall - flavoring preparation: Acetanisole ⁇ 0.5, Acetic Acid ⁇ 100,- Acetophenone ⁇ 2.5, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.5, Benzoin Resinoid ⁇ 25, Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 0.5, Bornyl Acetate ⁇ 0.5 , Butyric Acid ⁇ 0.5, Cardamon Seed Oil ⁇ 0.5, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.5, Chamomile Flower Oil Hungarian ⁇ 2.5 , Chamomile Flower Oil Roman ⁇ 2.5, Cinnamic Aldehyde ⁇ 25, Cinnamic Alcohol ⁇ 0.5, Citral ⁇ 0.5, Citric Acid ⁇ 0.5, D,L Citronellal ⁇ 0.5, Clary Sage Oil ⁇ 2.5 , Cocoa and Cocoa
  • Oil soluble flavors will only partially embedded (fully bind) within the matrix and can form oily deposits on the surface of the sphere releasing flavor upon storage. This is optimum loading for oil based flavor delivery. As pointed out above, theoretically, cellulose will swell discharging menthol into entrained air aerosol air flow. After observation of spheres upon storage, some polymerization occurs, indicating that hydrophobic complexation is needed to bind the flavor to the matrix. ⁇ -cyclodextrin is added to the matrix for covalent bonding of oil soluble raw materials .
  • Tobacco Type flavor (composed of FEMA GRAS materials, the flavor can be a mix consisting of the following at the limits not to exceed the described maximum all described in percentage of the overall flavoring preparation: Acetanisole ⁇ 0.25 Acetic Acid ⁇ 100, Acetophenone ⁇ 2.5, Ammonium Hydroxide ⁇ 100, Benzaldehyde ⁇ 0.25, Benzoin Resinoid ⁇ 12.5, Benzyl Alcohol ⁇ 100, Bergamot Oil ⁇ 2.5 , Bornyl Acetate ⁇ 0.25 Butyric Acid ⁇ 0.25, Cardamon Seed Oil ⁇ 0.25, Carob Bean Extract ⁇ 100, Celery Seed Oil ⁇ 0.25, Chamomile Flower Oil Hungarian ⁇ 1.25, Chamomile Flower Oil Roman ⁇ 1.25, Cinnamic Aldehyde ⁇ 12.5, Cinnamic Alcohol ⁇ 0.25, Citral ⁇ 0.25, Citric Acid ⁇ 0.25, D,L Citronellal ⁇ 0.25, Clary Sage Oil ⁇ 0.25, Cocoa and Cocoa extracts ⁇ 100
  • the process comprises the following steps: A) mix Avicel and cyclodextrin in a V-Blender until visually uniform; B) add flavor and blend until visually uniform;
  • Described below is a process to deliver placebo spheres for machine filling capabilities. No flavor is contained in this product. It is a space holder within the cavity.
  • the process comprises the following steps:
  • the resulting spheres can be introduced into a cigarette rod by removing the filter with needle-nosed forceps and placing 0.05-0.10 grams of spheres, evenly distributed, above the cigarette rod filler. A 2 mm gap is left and the filter is replaced in the tipping. The 2 mm filter extension protruding from tipping can be removed with a razor blade.
  • the cigarette can be lit in a conventional manner and flavor delivery evaluated. All of the formulations above can be polymer coated concurrent with drying or post dried. The coating can contain an additional 2-5% of flavoring. Referenced below is an example of coating preparation and application to the spheres .
  • Described below is a process to prepare coating and a method of coating the spheres .
  • Dri-Klear-091 fine granulation hydroxypropyl methyl cellulose (100.00% Solids) (Chr. Hansen) (10.00 %W/W wet basis, 10.00 % load dry basis), ii) Deionized water (0% solids) (90.00 %W/W wet basis) .
  • the process comprises the following steps:
  • Dri- Clear hydroxypropyl methyl cellulose (FMC)

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Fats And Perfumes (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

L'invention concerne des particules à charge aromatique élevée et des procédés d'élaboration correspondants. On décrit aussi des procédés d'utilisation pour les produits du tabac, y compris les cigarettes et d'autres articles de tabac classiques.
PCT/US2005/014548 2004-04-27 2005-04-27 Particule a charge aromatique elevee et procede d'elaboration WO2005104771A2 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
US56552204P 2004-04-27 2004-04-27
US60/565,522 2004-04-27
US59224404P 2004-07-30 2004-07-30
US60/592,244 2004-07-30
EP04103681 2004-07-30
EP04103681.5 2004-07-30
US11/114,234 US20050241656A1 (en) 2004-04-27 2005-04-26 High flavor load particle and method of preparing same
US11/114,234 2005-04-26

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WO2005104771A2 true WO2005104771A2 (fr) 2005-11-10
WO2005104771A3 WO2005104771A3 (fr) 2009-04-09

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WO2017130045A1 (fr) * 2016-01-25 2017-08-03 Philip Morris Products S.A. Sphéroïdes de charbon actif pour articles pour fumeurs

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CA2606527C (fr) 2005-04-29 2013-09-10 Philip Morris Products S.A. Produit a base de tabac avec poche
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US8377215B2 (en) 2008-12-18 2013-02-19 Philip Morris Usa Inc. Moist botanical pouch processing
US9167835B2 (en) 2008-12-30 2015-10-27 Philip Morris Usa Inc. Dissolvable films impregnated with encapsulated tobacco, tea, coffee, botanicals, and flavors for oral products
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CN105520192B (zh) * 2016-02-03 2018-11-09 云南中烟工业有限责任公司 一种卷烟滤嘴添加剂的制备方法及应用
JP6371928B1 (ja) * 2018-02-23 2018-08-08 株式会社 東亜産業 電子タバコ用充填物およびそれを用いた電子タバコカートリッジ
GB201817860D0 (en) * 2018-11-01 2018-12-19 Nicoventures Trading Ltd Aerosolised formulation
CN110179151B (zh) * 2019-07-11 2021-10-22 中国烟草总公司郑州烟草研究院 一种烘烤中烟叶初始含水率的估算方法、鲜烟叶的烘烤方法、数学模型及其构建方法
CN112094692B (zh) * 2020-09-17 2023-01-06 湖北中烟工业有限责任公司 一种琥珀香型卷烟香精及其应用
CN112806603A (zh) * 2021-02-02 2021-05-18 云南中烟工业有限责任公司 一种避免结团的加热不燃烧发烟颗粒混合物
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JP2012115205A (ja) * 2010-11-30 2012-06-21 Ogawa & Co Ltd 粉末香味料及びその製造方法
WO2017130045A1 (fr) * 2016-01-25 2017-08-03 Philip Morris Products S.A. Sphéroïdes de charbon actif pour articles pour fumeurs

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US20050241656A1 (en) 2005-11-03
WO2005104771A3 (fr) 2009-04-09

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