CN101296627A

CN101296627A - Menthol cigarette

Info

Publication number: CN101296627A
Application number: CNA2006800401833A
Authority: CN
Inventors: U·贝克; T·豪威尔; 薛立新; G·D·卡勒斯; J·A·弗尼尔
Original assignee: Philip Morris Products SA
Current assignee: Philip Morris Products SA
Priority date: 2005-09-30
Filing date: 2006-09-29
Publication date: 2008-10-29
Also published as: JP2009509524A; CO6160280A2; BRPI0616634A2; WO2007036814A3; EA013933B1; ZA200802486B; EA200800998A1; AU2006296290A1; KR20080059168A; WO2007036814A2; EP1931224A2

Abstract

Cigarettes are provided which contain a filtering system (180) and flavorants encapsulated with polyvinyl acetate (150), wherein deactivation of a sorbent by the flavorant is reduced through the encapsulation of the flavorant within the polyvinyl acetate. A preferred flavorant is menthol. The encapsulated flavorants are prepared by mixing at least one flavorant with polyvinyl acetate and a solvent, such as ethanol, and forming the encapsulated flavorants. Methods of making cigarettes and smoking the articles are also provided.

Description

Menthol cigarette

Background technology

Flavoring agent usually joins in the tobacco product to realize required sensory feel.One of common flavoring agent is a menthol.Menthol is a kind of volatile compound and tends to evaporate (volatilization) and escape from tobacco product gradually in storage process.

Various sorbent materials are used as additive in tobacco product, to remove the composition of selecting in the tobacco smoke.More common additive comprises active carbon, molecular sieve, zeolite and composition thereof.

Active carbon is useful sorbent material and has big adsorption capacity.Yet although active carbon is removed target component effectively from tobacco smoke, in the time of in they are present in tobacco product, they do not have selectivity and also absorb volatility flavoring agent, for example menthol.

Therefore; to in the tobacco product that contains sorbent material such as active carbon, molecular sieve and zeolite, providing the flavoring agent such as menthol to have interest; wherein said sorbent material is avoided volatilization, deterioration and is adsorbed agent material absorption for the protection flavoring agent, makes the form that flavoring agent can discharge gradually simultaneously when tobacco product is sucked.

Summary of the invention

A kind of cigarette is provided, and it contains the flavoring agent that useful polyvinyl acetate is sealed, and wherein utilizes heat and/or moisture, discharges flavoring agent and enter in the mainstream smoke in the smoking process from polyvinyl acetate is sealed.A kind of method of improving the cigarette sense of taste characteristic that contains adsorbent such as active carbon by the flavoring agent with the adsorbent deactivation also is provided.

A kind of filter-tip cigarette also is provided, and it comprises columniform basically plume, columniform basically filter stick, and the tipping paper that encases and connect filter tip and plume, and wherein filter stick comprises the flavoring agent of being sealed by polyvinyl acetate; Make the method for cigarette; With the method for handling mainstream tobacco smoke.

In one embodiment, provide a kind of cigarette, it comprises tobacco, filter tip, adsorbent and contains polyvinyl acetate matrix and the flavoring agent of sealing of the menthol flavoring agent of combination in this matrix.

The further embodiment method that provides manufacturing to comprise the cigarette of adsorbent within it, this method are included in to mix in the cigarette component and contain polyvinyl acetate matrix and the flavoring agent of sealing of the menthol flavoring agent of combination in this matrix.

In an embodiment again, the method that makes the main flow smoke from cigarette increase flavor is provided, this method comprises with polyvinyl acetate matrix and keeps flavoring agent (menthol), and discharges menthol when producing mainstream smoke in this matrix, and described release steps comprises and applies heat and/or moisture on matrix.

The accompanying drawing summary

Fig. 1 (a)-(c) has set forth the packaged products that exemplifies embodiment in plume.

Fig. 2 (a)-(c) has set forth according to the flavor that increases of the embodiment that exemplifies and has been with.

Fig. 3 shows according to the flavor that increases of another embodiment that exemplifies and is with.

Fig. 4 shows in the embodiment that exemplifies, and time time suction (puff-by-puff) of benzene is carried.

Fig. 5 shows in the embodiment that exemplifies, and the drawing-in type of methacrylaldehyde is carried.

Fig. 6 shows in the embodiment that exemplifies, the conveying of the suction of 1,3-butadiene.

Fig. 7 shows the menthol retention rate of the embodiment that exemplifies when changing the ratio of menthol and polyvinyl acetate.

Fig. 8 shows the menthol retention rate of the embodiment that exemplifies when changing solvent volume.

Fig. 9 shows with the loss in weight of film and compares, and compares thermogravimetric analyzer (TGA) result of the test of polyvinyl acetate-menthol film with the pure menthol that demonstrates the menthol retention rate.

It is benchmark that Figure 10 shows with the aging of solution, the retention rate of menthol.

Describe in detail

Described and contained useful polyvinyl acetate flavoring agent of sealing and the cigarette that contains the filtration system of at least a adsorbent.Also describe the method for making the flavoring agent of sealing, made the method and the method for handling from the smog of these goods of cigarette.

Term " smog goods " comprises cigarette, tobacco pipe, cigar, cigarlet and analog.

Term " mainstream smoke " comprises the aerosol that is drawn into the mouth end of smog goods by the smog goods.

Term " is sealed " and is comprised sealing with little by a kind of material and seal another kind of material, and wherein little sealing is included on the microcapsules size, promptly less than 1 micron sealing on surpass 2000 microns.For example, as used herein sealing preferably includes the matrix that forms a kind of material, wherein in the little matrix that is encapsulated in first kind of material of second kind of material.Equally, " flavoring agent of sealing " is meant and seals or little flavoring agent of sealing, preferably at the intramatrical flavoring agent of polyvinyl acetate encapsulation agent.

Any flavoring agent is suitable for adopting polyvinyl acetate to seal.Menthol is preferred flavoring agent.Other suitable flavoring agents comprise peppermint, for example peppermint and spearmint, vanillic aldehyde, chocolate, Radix Glycyrrhizae, citrus and other fruit flavoring agents, spices flavoring agent, for example Chinese cassia tree, gaultherolin, linalool, bergamot oil, geranium oil, lemon oil, ginger oil, tobacco flavoring agent and give the mainstream smoke local flavor of tobacco product and other reagent that fragranced is commonly used.In common US-A-5301693, US-A-5228461 that transfers the possession of and US-A5137036, the flavoring agent that is suitable for sealing has been discussed also, has been introduced by reference in its entirety at this.

According to an embodiment, one or more are planted flavoring agent and are incorporated in the filter tip of cigarette, and wherein employed filter tip comprises at least a adsorbent (absorbent or adsorbent) in cigarette." adsorbent " as used herein is meant absorbent or adsorbent, perhaps can serve as the material of absorbent and adsorbent simultaneously.Interaction and the interaction in its hole and passage on the adsorbent outer surface such as active carbon, molecular sieve, zeolite and other similar materials intended being included in term " absorption ".

Preferably adsorbent comprises various forms of active carbons, molecular sieve, zeolite for example, and composition thereof.The activated form of carbon has the strong physical absorption power and the absorption porosity of high volume.Can make active carbon by any suitable technique.A kind of technology is for example cocoanut shell, timber, pitch, cellulose fibre or a polymer fiber of carbonization.Preferably at high temperature, promptly under 200 ℃-800 ℃, in inert atmosphere, carry out carbonization, followed by under oxidizing condition, activating.Employed active carbon can be monoblock shape, particle, pearl, powder or fiber in cigarette.Optionally, active carbon can be incorporated into another material, for example in the paper.

Active carbon can comprise the distribution of micropore, mesopore and macropore.Term " micropore " typically refers to this material that cell size is less than or equal to about 20 dusts, and term " mesopore " typically refers to this material that cell size is about 20 dusts-500 dust.Term " macropore " is meant the cell size that 500 dusts are above.Can with respect to target remove from the assign to relative quantity of preliminary election micropore, mesopore and macropore of being chosen in the mainstream tobacco smoke.Therefore, use, can regulate cell size and distribution of pores as required for some.

Can in the filtration system of cigarette, another material as adsorbent be molecular sieve zeolites.Term as used herein " molecular sieve " is meant the loose structure of being made up of the inorganic silicic acid salt material.Zeolite has the passage or the hole of uniform molecular size size.Exist and have the many known unique zeolite structures of different size and shape passage or hole.But the absorption of these materials of size and dimension appreciable impact of passage or hole and the performance of separation characteristic aspect.Can use zeolite, in passage or hole, and/or come isolated molecule by the adsorption strength difference.Have greater than the passage of the selected composition of mainstream smoke or one or more kind zeolites of hole by use, only be small enough to those selection molecular energies that pass molecular sieve pores and enter in the cavity and by zeolite adsorption.

Micropore, mesopore and/or large pore molecular sieve can be used as adsorbent.They are selected in based on the filtration system of removing special component from mainstream smoke.The zeolite-type molecular sieves that can be used for cigarette comprises crystal aluminosilicate, silicoaluminophosphate (AIPO/SAPO) and mesoporous molecular sieve, for example MCM-41, MCM-48 and SBA-15.These are bulk material preferably.This group material contains the regularly arranged and modifiable inner activity site of uniform-dimension passage, and allows the molecule below a certain size to enter in its inner space, wishes therein optionally under the situation, makes their useful as catalysts and adsorbent.

Adsorbent can be incorporated in one or more position of cigarette.For example, adsorbent can place in the path of the free-pouring filter assemblies of tubulose, in the material of filter assemblies, and/or in the interstitial space of filter tip.Adsorbent can be in addition or alternatively is incorporated in tobacco-containing material or the cigarette coil paper.

Filter tip can and surround in the shell of this fiber at the orientation or the fiber of non-orientation and comprise adsorbent.Adsorbent can be one or more kinds in active carbon, zeolite and other molecular sieves of arranging with fibre property for example.Adsorbent mixtures can provide different filtering feature to realize the mainstream smoke composition of goal filtering.

Perhaps, adsorbent can be by at microporous fibre, for example available from HoneywellInternational of Morristown, the TRIAD of New Jersey ^TMOne or more kind sorbent materials of dipping in the microporous fibre, for example carbon, silica, zeolite and analog are formed.Fiber can be the moulding microporous fibre of planting the adsorber material granules dipping with one or more.Referring to common US-A-6584979, US-A-6772768 and the US-A-6779528 that transfers the possession of, introduce by reference in its entirety at this.

In another embodiment, fiber can be the discontinuous fiber of bunchy, and the discontinuous fiber of described bunchy preferably is orientated in filter tip on the direction that flows along the mainstream smoke by cigarette.

In the filter tip process for making, can be for example the sorbent fibers material (preferably it has total filament denier and every threads dawn number of control) of non-crimping by the stretching bunchy through preform or the shell that is shaped on the spot, form the filter stick that contains adsorbent.The filter stick that is shaped can be separated into filter stick by cutting into Len req.For example, the length of filter stick can be the about 30mm of about 5mm-.

Can adsorbent be incorporated in the cigaratte filter at one or more place, desired position.In preferred embodiments, the adsorbent part combines with free-pouring filter tip.Adsorbent can contact (promptly adjoining) with the free-pouring filter tip of arranging between free-pouring filter tip and cigarette holder filter stick, perhaps contact (promptly adjoining) with cigarette holder filter stick.The preferred diameter of adsorbent part is substantially equal to the external diameter of free-pouring filter tip, to be minimized in the by-pass flow that filters smog in the technical process.

The filter tip part that contains fiber adsorbing substance preferably has high fluffy sense and suitable bulk density and fibre length, so that produce parallel path between fiber.This structure can be removed the gas phase composition of selection effectively, for example formaldehyde and/or methacrylaldehyde, preferably in smog, remove the only particulate matter of minimum simultaneously, thereby realize selecting the remarkable decline of gas phase composition, have no significant effect the total particulate matter (TPM) in the tobacco smoke simultaneously.Preferred low bulk density and short fibre length are to realize this strainability.

The component type that employed adsorbent consumption depends on the type of gas phase composition in the tobacco smoke and wishes to remove from tobacco smoke in the preferred embodiment of cigarette.

When using adsorbent and flavoring agent in cigarette, if flavoring agent is adsorbed agent absorption, then flavoring agent can make the adsorbent deactivation.Therefore, in order to reduce the deactivation degree of adsorbent, preferably by sealing, the protection flavoring agent is avoided absorption.By sealing, therefore can reduce the interaction between adsorbent and the flavoring agent, and the adsorptivity of the flavoring agent that is caused.

The flavoring agent of sealing can be positioned at the each several part of cigarette, flavoring agent is provided in cigarette and reduces the deactivation of adsorbent.In one embodiment, Bu Fen flavoring agent can be the bead form that is positioned at smokable filler.By using bead, can be implemented in the control release of flavoring agent in the cigarette in the cyclic process of smog stream.Bead preferably includes the polyvinyl acetate of sealing at least a flavoring agent, and the heat and/or the moisture that wherein are applied in the cigarette aspiration procedure on the flavoring agent of sealing will discharge flavoring agent from encapsulation agent.Can randomly add and improve the encapsulating material characteristic or improve its stable other materials, for example filler.

In the embodiment that exemplifies, the additive of sealing bead can be provided, described bead has basically to be formed uniformly, and wherein flavoring agent is evenly distributed in the middle of the bead basically.Can in aspiration procedure, from bead, discharge fragrance by this structure in uniform mode.

In addition, by sealing flavoring agent, protected the flavoring agent of sealing to avoid being exposed under the atmosphere under the adsorbent in the surrounding air of package interior (promptly) and the cigarette such as cigarette.Therefore, the release of flavoring agent and/or migration are minimum, are exposed to up to the flavoring agent of sealing under the moisture or heat of increase.Although be not wishing to be bound by theory, but think the moisture that increases, and the temperature that increases will cause that the polyvinyl acetate matrix of sealing flavoring agent expands the polyvinyl acetate matrix, leave the path of polyvinyl acetate matrix and allow flavoring agent to escape thereby produce.

For example, the flavoring agent that the polyvinyl acetate matrix is sealed may be used on the cigaratte filter, and wherein moisture and the Re Ke from user's mouth discharges flavoring agent.As another example, between 50 ℃ to 900 ℃, perhaps the temperature between 100 ℃ to 800 ℃ (for example 25 ℃, 50 ℃, 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, more than 800 ℃) may be used on sealing on the flavoring agent, the polyvinyl acetate matrix sealed is expanded, and this expansion can cause conversely from the polyvinyl acetate matrix of sealing and discharges flavoring agent.

Therefore, can be by sealing the unconscious release or the interaction between flavoring agent and adsorbent of flavoring agent reduction flavoring agent.In addition, can realize autotelic release by the moisture level of obtainable rising in the cigarette of smoldering or the temperature of rising.Therefore, seal flavoring agent and allow in the temperature that increases and/or humidity level's process in the polyvinyl acetate matrix, particularly improved flavoring agent is carried in containing the cigarette of adsorbent.

The flavoring agent of sealing can have any required shape, comprising rule or irregularly shaped, comprising circle, square, rectangle, ellipse, other are polyhedron-shaped, cylindrical, fibrous and analogous shape.Bead can have various sizes.Preferably, bead is a maximum particle size less than about 25 microns and be more preferably less than about 1 micron microballon.By the surface agent that provides bead to increase, reducing bead size can provide the more all even control of flavoring agent to discharge.

Can have any appropriate method of the goods of desired structure, composition and size by generation, make the product of sealing.For example, can by extrude, spray-drying, coating or other suitable technology, make the product of sealing.In preferred embodiments, contain solution, dispersion or the emulsion of polyvinyl acetate, flavouring and optional flavoring agent by formation, and the dry encapsulation agent that obtains moulding, thereby the product that preparation is sealed.

Although be not wishing to be bound by theory, think that sealing flavoring agent by polyvinyl acetate is based on the fractional condensation on surface principle.Think that polyvinyl acetate forms the matrix of the surface portion with flavoring agent of sealing, the surface portion of the wherein said flavoring agent of sealing has than polyvinyl acetate wherein towards fractional condensation on surface and flavoring agent away from the ratio of the high polyvinyl acetate in the inside of fractional condensation on surface with encapsulation agent.

Preferably by mixing reinforcing agent, volatile solvent and the polyvinyl acetate that one or more plant powder or liquid form, dry then gained emulsion, remove and desolvate, and the flavoring agent that in the matrix that forms by polyvinyl acetate, bonds, thereby the flavoring agent that preparation is sealed.The product that reclaims is the flavoring agent of sealing by the polyvinyl acetate matrix, so that keep the flavoring agent and the flavoring agent that bonds in matrix.The product of sealing can be fiber, film, material all in one piece, bead, powder or particle form.

Preferred solvent comprises methyl alcohol or ethanol.Solvent is volatilization fully preferably, removes fully in product, thereby stays polyvinyl acetate and flavoring agent separately.Yet, can optionally keep solvent.

Can broadly change the ratio of each component.Based on 100 weight portion polyvinyl acetate, flavoring agent, for example the consumption of menthol can be about 1-90%, about 2-70% or about 10-50wt%.Solvent load preferably is enough to solubilising flavoring agent and polyvinyl acetate.

Preferably, by compounding in solvent, blend and/or dissolving flavoring agent and polyvinyl acetate, form the composite of flavoring agent and polyvinyl acetate.Preferably, use heat and mechanical shearing mixing flavoring agent and polyvinyl acetate.

Equally preferably, one or more are planted flavoring agents with independent phase form dissolving and be captured in the successive substrates of polyvinyl acetate.Therefore, in case be exposed under heat and/or the moisture, it is lax then can to increase the polyvinyl acetate matrix that causes by Yin Wendu and/or humidity level, reduces the barrier properties of polyvinyl acetate, thereby allows flavoring agent to discharge from matrix.

For example, the method for preparing menthol/polyvinyl acetate composite can comprise mixing such as alcohol, and for example solvent of ethanol and so on and polyvinyl acetate form solution.Next, the menthol flavoring agent can be joined in ethanol and the polyvinyl acetate solution, flavouring is provided.Next, can reduce alcohol solvent content, increase the concentration level of interior menthol of solution and polyvinyl acetate.Note, although menthol has volatility and can evaporate, but the mixture of menthol and polyvinyl acetate will reduce the evaporation of menthol in this embodiment, and this is because menthol is dispersed in the polyvinyl acetate, wherein due to the evaporation rate of this dispersion reduction menthol.Next, this mixture can be formed required form, for example fiber, film, material all in one piece, bead, powder and particle wherein can evaporate this solvent, form menthol and are encapsulated in the interior final composite of polyvinyl acetate matrix.Reduce solvent and choose wantonly, and the flavoring agent content of increase can be provided in final composite.

Notice that also in the polyvinyl acetate relative amount of menthol provides the variation of final flavoring agent content.For example, if about 37% menthol is provided, in case can expect that then when using, about 35% menthol discharges.On the other hand, for these encapsulating methods that exemplifies, the menthol level in the mixture can surpass basic level of encapsulation, and can use alternative wrapper technology.

For these simplified methods of sealing, the example that surpasses the menthol level of basic level of encapsulation is that the initial amount of menthol is higher than for example about 70% in the mixture.Under this level, the consumption of the menthol that is used to seal is thought above basic level of encapsulation, and is because find in this embodiment, encapsulated about only 23% menthol.Although be not wishing to be bound by theory, but for this simplified method, in higher level, for example 70% time, as if menthol assembled and more than a certain menthol level, in this embodiment at about 70% level place, as if menthol is not dispersed in the polyvinyl acetate matrix, thereby reduces the level of encapsulation of menthol.

Yet attention can use another method that exemplifies to seal higher menthol level.For example, if time period by keeping menthol and polyvinyl acetate in solution, to prolong, thus the aging mixture that has 70% high menthol base level as mentioned above, final release when then can be observed improved flavoring agent and sealing and use.For example, if about 3 months of the mixture of aging 70% menthol, solvent and polyvinyl acetate, then the composite that is formed by this aged solution can demonstrate improved menthol retention rate and envelop rate and finally reach the emission levels of 70% menthol in aspiration procedure.Therefore, by the aging menthol/polyvinyl acetate ester admixture that highly concentrates, can realize reaching 70% menthol emission levels.

Perhaps, attention can pass through to reduce the solvent in menthol, solvent and the polyvinyl acetate solution, rather than by aging, realizes sealing the similar results of higher level menthol.For example, can evaporate the solvent in the solution, reduce solvent.By reducing solvent, entrapped similarly high menthol level seem with the similar level of encapsulation of the menthol that carries out overaging under.For example, can seal the solvent with reduction and the menthol of high-load by polyvinyl acetate, the solution of 55% menthol for example, and can cause the menthol content of about 55% envelop rate.

Can find out and to seal flavoring agent and provide that described physical form is stable and do not suffer a loss because of volatilization, deterioration and/or the active carbon that is existed in the cigarette, zeolite or other adsorbents adsorb with various physical form.Preferably, the flavoring agent of sealing contains flavoring agent, polyvinyl acetate and optional flavoring agent, the if there is no words of other materials.

Cigarette preferably includes the flavoring agent of sealing in right amount, and described flavoring agent provides the seasoning of aequum in cigarette.In preferred embodiments, based on the gross weight of tobacco in the cigarette, cigarette comprises maximum about 20% and about 15% flavoring agent of sealing of 10%-more preferably from about.For example, the cigarette of containing the 100mg tobacco is preferably contained the flavoring agent that maximum about 20mg seal.

In preferred embodiments, the flavoring agent of sealing places at least one position in the cigarette, and described position will reach the minimum temperature at least when flavoring agent discharges in aspiration procedure from the polyvinyl acetate encapsulation agent.For example, the flavoring agent of sealing can place in the tobacco or burn with on the cigarette paper, wherein can utilize the combination of heat and moisture, discharges flavoring agent from the polyvinyl acetate encapsulation agent.

In another embodiment preferred, the flavoring agent of sealing places at least one position in the cigarette, and described position humidity in aspiration procedure increases, wherein from mainstream smoke or can be used as the relieving mechanism of flavoring agent from the moisture of smoker's mouth.For example, the flavoring agent of sealing can place from the hole in filter tip adsorbent downstream or place on one or more surface of free-pouring filter tip, and wherein the moisture from mainstream smoke can make flavoring agent discharge from encapsulation agent.

In another embodiment preferred, be injected in the plume by the flavoring agent of sealing, thereby the flavoring agent of sealing is placed plume liquid form.For example, the flavoring agent of sealing can form the liquid form of the flavoring agent of sealing, and for example hot melt or solvent base fluid body are for injection.Preferably, the liquid injection can be applied in the plume of cigarette in the heart, with wetting tobacco or fill the core of plume, provides the flavoring agent of sealing in plume.Yet injection can be any position in plume.For example, referring to Fig. 1 (a), the figure shows embodiment preferred plume 100, it has the flavoring agent of sealing 150 that injects with liquid form in the core of the plume 100 of filter tip 180 upstreams.

In another embodiment preferred, by spray or the flavoring agent of sealing of coating liquid form to smokable filler, thereby the flavoring agent of liquid envelope is placed in the tobacco filter tip.For example, the flavoring agent of sealing can form the hot melt or the solvent based sols (for example ethanol, polyvinyl acetate and menthol) of the aforesaid flavoring agent of sealing, but in this embodiment, the flavoring agent of liquid envelope is sprayed or be coated on the smokable filler.Preferably for cigarette, before forming plume 100, spray or the flavoring agent of sealing of coating is applied on the smokable filler equably, so that the flavoring agent of sealing 160 is provided in the middle of plume 100, as shown in Fig. 1 (b).

In another embodiment preferred, the flavoring agent of sealing by hybrid solid is in smokable filler, and the flavoring agent that solid is sealed places smokable filler.Preferably, in order to increase the compatibility of the flavoring agent that solid seals, chopping, pulverize or the powder of the flavoring agent sealed of machining solid to be mixed becomes chopping in other cases film, pulverizing or the particle of reduced size in other cases the compatibility of flavoring agent in filler of sealing with increase.Preferably, before making rod or among, mixing encapsulated reinforcing agent 170 and smokable filler, thus the flavoring agent 170 that allows to seal distributes in whole plume 100, shown in Fig. 1 (c).

In another embodiment, the reinforcing agent of sealing can exist by form membrane.Can provide film by applying and the dry filmogen that has flavoring agent within it, wherein flavoring agent can provide with flavoring agent of sealing in advance or the non-flavoring agent form of sealing of mixing with filmogen.Preferably, filmogen comprises the polyvinyl acetate film.In addition, preferably, flavoring agent is a menthol.

For example, the bead of the menthol that polyvinyl acetate is sealed in advance can mix with the polyvinyl acetate filmogen, and form that then can film applies this mixture to cigarette.Perhaps, the non-liquid menthol of sealing can mix with the polyvinyl acetate filmogen, can apply this mixture then with the form of film to cigarette.

Note, before mixing the menthol of sealing in advance and filmogen, the menthol of sealing in advance can pass through other adhesives, keep the polymeric material of flavoring agent, and for example polyvinyl alcohol, polyacrylate, poly-(ethylene glycol), polyglycolic acid (polyglycolic acid), pectin, polysaccharide, PLA, polyester, PEO, polyepoxide or analog are sealed in advance.

In preferred embodiments, it is maximum 20% that the polyvinyl acetate film comprises, more preferably from about the flavoring agent of about 15% weight of 10%-is for example sealed or the non-menthol of sealing, and can be applied on the assembly in the cigarette.For example, film can be applied on the filter tip surface, and the tobacco pad (mat) that is coated on unconventional cigarette is gone up or is coated on the coil paper of cigarette.In preferred embodiments, film is sealed menthol and peppermint randomly.

Preferably, as mentioned above, the flavoring agent that the film class is sealed comprises polyvinyl acetate filmogen and at least a flavoring agent of sealing.Yet, can randomly add extra other materials, the film forming characteristics of the polyvinyl acetate filmogen of sealing with improvement or improve the stability of polyvinyl acetate filmogen.In the embodiment that exemplifies, film has flavoring agent wherein and is evenly distributed in forming uniformly basically in it basically.The film encapsulating material provides and discharges stopping of flavoring agent, wherein optionally discharges the flavoring agent of effective dose.For example, the release that discharges the stream of 0.01mg/ battle array smog at least from the conventional cigarette that exemplifies is desirable, and perhaps before suction, the menthol of the about 2wt% of plume gross weight is desirable in the cigarette, release when allowing suction.

Film can be applied to one or more assembly in the cigarette with the liquid coating form, for example surround on the outside tipping paper of the tipping paper outer surface of filter tip or cigarette, then drying and forming-film.The size of desciccator diaphragm without limits.Preferably, the maximum ga(u)ge of desciccator diaphragm is about 50 microns-Yue 150 microns and more preferably the most about 75 microns.Any suitable method manufacturing film that can have the film of desired structure, composition and size by generation.For example, can pass through coating process, for example spraying, dipping process, electrostatic precipitation, printing wheel apply, photogravure, ink-jet applies and similar technology, applies film.Preparation contains emulsion, suspension or the slurry of polyvinyl acetate and flavoring agent and optional additive, and one or more that increases then that the flavor coating is applied in the cigarette that one or more selects assembly selected on surface.Preferred dry coating removes and anhydrates and/or other solvents, and forms the solid film with required size.Can carry out drying by the temperature of evaporation or reduction film, so that sclerosis and raising film are to the cohesive on selected surface.

In one embodiment, on the tipping paper outer surface that surrounds cigaratte filter, for example go up or in the smog in any adsorbent downstream flows, form the encapsulated membranes of polyvinyl acetate base film at filter rod forming paper (plug wrap).By providing film in this position, can be in aspiration procedure exposed film in from smoker's mouth, and come under the heat and moisture of the rising in the mainstream smoke.As mentioned above, heat and the moisture film that allows to seal discharge at least a portion flavoring agent from the polyvinyl acetate matrix.Therefore, by in use, in the position of moisture with rising and/or temperature levels, provide film, can be by in storage process, at polyvinyl acetate matrix IT, thereby keep flavoring agent, and from the polyvinyl acetate matrix, discharge in use.

In another embodiment, film can form the flavoring agent band on the wrapping paper externally, and wherein the flavoring agent band can be coated on the inboard or the outside of outer packaging paper.Preferably, arrange quantity, width and the position of flavoring agent band,, in the static combustion process, keep burning, but still the mainstream smoke flavoring agent is provided so that air can be diffused in the plume.For example, shown in Fig. 2 (a), the burning direction that can be parallel to plume 220 forms flavoring agent band 210, thereby when suction cigarette 200, carries flavoring agent.Shown in Fig. 2 (b) and 2 (c), flavoring agent band 210 can be positioned on the inboard or the outside of cigarette wrapper 230.Flavoring agent band 210 also can use with adsorbent 240, as shown in Figure 3.

Can by surround coating, printing, japanning on the paper of plume, spray, extrude, dip-coating or casting films, form before the plume, among and/or afterwards, form the flavoring agent band.By using the flavoring agent band, flavoring agent and any adsorbent have the interaction of reduction, thereby keep performance separately.For example, when the flavoring agent band places cigarette to go up, can in having the cigarette process of active carbon, suction provide high menthol to carry.In addition, when using the flavoring agent band and containing the cigarette of active carbon, even after long-time section adjacent one another are, active carbon and flavoring agent band can keep the performance of their desired levels.

Carbon does not interact with menthol flavoring agent band.Shown in Fig. 4-6, in the comparison of suction, with contain non-menthol, (its absorbs benzene, methacrylaldehyde and 1 to contain the contrast cigarette (" tester ") of carbon, the 3-butadiene is better than the cigarette 2R4F that contains non-carbon) compare, cigarette B and C (it also contains carbon) with menthol flavoring agent band have similar benzene, methacrylaldehyde and 1,3-butadiene adsorption rate.Shown in Fig. 4-6, contrast cigarette and flavoring agent band cigarette are all similarly being reduced benzene, methacrylaldehyde and 1,3-butadiene under the level.Just because of this, when providing menthol by the flavoring agent band, menthol does not significantly make the adsorbent deactivation in the cigarette, reduces benzene, methacrylaldehyde and 1,3-butadiene at least equally.

Preferably, the menthol in the flavoring agent band in cigarette has minimum negative effect to the adsorbent in the cigarette, and also allows to discharge in aspiration procedure high-caliber menthol.For example, as shown in table 1, in filter tip, have exemplifying in the flavoring agent band on the cigarette of carbon adsorbent material and can arrange for example menthol content of 0.18mg/ root cigarette, 0.51mg/ root cigarette and 1.36mg/ root cigarette.The result, compare with the cigarette that does not have the flavoring agent band (tester), can be in the 4th suction (embodiment A, B, C) of cigarette with flavoring agent band, realize that in aspiration procedure 0.021mg/ once aspirates, 0.058mg/ once aspirates and 0.145mg/ once aspirates menthol and methacrylaldehyde, 1,3-butadiene, acetaldehyde or benzene content seldom change.Yet, note preferably, the flavoring agent band provides the menthol flavoring agent at least about 0.01mg/ battle array smog stream, wherein the content of every gust of interior menthol flavoring agent of smog stream depends on the menthol concentration in the polyvinyl acetate filmogen, and the menthol consumption that is provided, the size and the quantity of the flavoring agent band that is promptly provided.

Table 1

In addition, the flavoring agent band can be used as the additive in the employed seam adhesive or its substitute on tipping paper.For example film can be placed on the seam of cigarette package paper, seam is provided, and the interior flavoring agent of cigarette is bonding.

In an above-mentioned embodiment, the flavoring agent of sealing can be positioned at the filter tip part of cigarette at least.In some embodiments, Bu Fen flavoring agent can be positioned at the filter tip of cigarette.For example, the flavoring agent of adsorbent and part can be positioned at the filter tip part of cigarette, and wherein flavoring agent is in the downstream of adsorbent.

Can use various filter structures to prepare cigarette.The filter structures that exemplifies that can be used for cigarette includes, but not limited to the filter tip of single filter tip, two filter tip, three filter tips or many cavitys, recessed filter tip or free-pouring filter tip.Single filter tip typically contains estron bundle or filter paper material.Two filter tips typically comprise cellulose acetate mouth side and cellulose acetate filter plug portion.In this double filter, adsorbent and the flavoring agent of sealing are preferably placed near the sucked material or the tobacco side of cigarette.Can regulate the length and the pressure drop of two parts in the double filter, the absorption of increase is provided, keep the acceptable draw resistance of cigarette simultaneously.

The triple filter tips of cigarette can comprise mouth and sucked material or tobacco side part and contain filter tip material or the mid portion of paper.The flavoring agent of adsorbent and part can be provided at mid portion.Cavity filters typically comprises two parts that separated by cavity, for example cellulose acetate-cellulose acetate, cellulose acetate-paper or paper-paper.Adsorbent preferably is provided in cavity.Recessed filter tip is included in the open cavity on the mouth side, and can mix adsorbent in the middle of filter plug material.Filter tip also can randomly be taken a breath, and/or comprises extra adsorbent, catalyst, flavoring agent or other additives that use routinely in the cigaratte filter field.

Embodiment

For high flavoring agent releasability, the flavoring agent of sealing by polyvinyl acetate that exemplifies can be formed the ratio of predetermined flavoring agent and polyvinyl acetate.It is desirable to, formation has the flavoring agent of high-load flavoring agent and the stability of composite materials of polyvinyl acetate, and sufficient flavoring agent release reagent is provided.The following embodiment of the composite of flavoring agent and polyvinyl acetate provides about the stability of flavoring agent in the polyvinyl acetate data as the function of flavoring agent concentration.

In the composite (flavoring agent of promptly sealing) that preparation exemplifies, for flavoring agent, use menthol, and use polyvinyl acetate to seal menthol.The method of the reinforcing agent that preparation is sealed comprises: 1) add 75.5g ethanol (95%) in 12.5g polyvinyl acetate bead (MW～500,000); 2) at room temperature stir this mixture about 2 hours, form clear solution; 3) add 7.5g, 15.1g, 30.1g or 15.1g menthol solid, form the solution of A, B, C and D respectively; 4) the about 6-12 of solution hour of stirring A, B, C and D, form clear solution; 5) ethanol content in the reduction solution D is from 75g to 62.5g; With 6) by curtain coating, molding, extrude, pulverize, cutting and/or rotating technics, after evaporating solvent, form film, bead, bar and fiber.

Can test the stability of menthol releasability in the formed composite, wherein stability exemplifies that under open container internal environment condition composite keeps its most of weight and along with the loss minimum of flavoring agent time lapse.On the other hand, unstability exemplifies the loss of weight and menthol smell.

As shown in table 2, in the middle of composite A, B, C, C has the highest menthol initial concentration, and B has the second high initial concentration, and next A has minimum initial menthol concentration.Yet when making A, B and C composite, B has than C or the high menthol retention rate of A.Note, with respect to the initial sample weight ratio initial menthol level and final menthol retention rate level in the table 2 so that set forth the influence of polyvinyl acetate to the menthol retention rate.By with respect to initial sample weight, calculate final menthol retention rate, can be relative to each other, and pure menthol control sample, relatively the menthol retention rate of composite A-D.Therefore table 2 loss of having set forth menthol content in the pure menthol, and compare the higher variation level of menthol retention rate in composite A-D with the pure menthol of contrast.

Menthol content in table 2. menthol/polyvinyl acetate composite

Sample	Initial menthol %/W0	The retention rate %/W0 of final menthol	Expection menthol %/W1	The menthol %/W1 that discharges
Sample	Initial menthol %/W0	The retention rate %/W0 of final menthol	Expection menthol %/W1	The menthol %/W1 that discharges	Composite A	37	38	38	35
Composite B	55	41	46	46	Composite A	37	38	38	35
Composite B	55	41	46	46	Composite C	71	＜18	＜37	23
Composite D	54	48	51	52	Composite C	71	＜18	＜37	23
Composite D	54	48	51	52	Tester (pure menthol)	100	＜8	100	-

W0: initial sample weight; W1: final sample weight.

* unsettled sample under environmental condition, error ± 2% wherein, this is because the moisture content and the error of calculation that change cause.

This further is set forth among Fig. 7, this figure compared along with time lapse, composite A, B and C, and the menthol retention rate of pure menthol (tester), wherein A and B had similar menthol retention rate after 20 days, and C and pure menthol have lower menthol retention rate.As if the menthol retention rate result of Fig. 7 illustrated that C is unstable in polyvinyl acetate, this may be because it has higher initial menthol content and causes, wherein aspect time lapse its retention rate, the behavior of composite C is similar to pure menthol.

As shown in Figure 8, ethanol reveals menthol conservation rate in time by B to the reduction water-glass of D and improves.By contrast, control sample (the pure menthol that does not add polyvinyl acetate) is than low many of the menthol conservation rate in time of B or D, also referring to Fig. 7.

Also can measure releasability (wt%), the flavoring agent performance of sealing with mensuration along with menthol time lapse.Just as shown in Figure 9, the menthol of sealing (composite B) is suitable with pure menthol (not sealing), wherein along with time lapse, they are placed under the temperature of increase (this represents to top-right temperature line and the temperature on vertical axis by Fig. 9 lower left) separately.As shown in Figure 9, use thermogravimetric analysis (TGA), as if composite B and non-encapsulated pure menthol keep similar menthol retention rate (shown in the upper left side part of Fig. 9) being lower than under about 50 ℃ temperature, but be higher than under about 50 ℃ temperature, composite B keeps its weight and is better than pure menthol.As shown in Figure 9, pure menthol is about 0wt% being lower than below 100 ℃, and composite B is kept above 0wt%, up to about 600 ℃.In addition, composite B is surpassing 50wt% above descending under 300 ℃ the temperature, and composite B drops to about 80wt% (dropping to 10wt% from about 90wt%) in weight under about 100 ℃-Yue 500 ℃ temperature, and demonstrates the release gradually (weight % is stable to descend) of menthol in about 50 ℃-Yue 200 ℃ temperature range.Therefore in composite B by sealing menthol, can be implemented in release in the bigger and higher temperature.

In addition, in another example, the sample of composite C can wear out about 3 months, to measure any variation of the aging stability that may cause.As shown in following and Figure 10, in particular for the reservation that surpasses 4 days, compare with the composite C of " fresh ", aging composite C has improved menthol retention rate.

Therefore, can under high level, mix menthol and polyvinyl acetate, and, then can keep these high menthol levels if use the interior solvent of composite of aging and/or reduction menthol and polyvinyl acetate.

Aforesaid various variation and modification are conspicuous for a person skilled in the art.This variation and modification are regarded as in the authority and scope of claims.

Claims

1. cigarette, it comprises tobacco, filter tip, adsorbent and the flavoring agent of sealing, the described flavoring agent of sealing comprises the polyvinyl acetate matrix, wherein flavoring agent combination in matrix.

2. the cigarette of claim 1, the flavoring agent of wherein sealing are positioned on the outer surface of cigaratte filter and adsorbent is positioned at the cavity of filter tip.

3. the cigarette of claim 1, the flavoring agent of wherein sealing is positioned at the plume central area of cigarette or is distributed in the middle of the plume of whole cigarette.

4. the cigarette of claim 1, the flavoring agent of wherein sealing comprises the flavoring agent band that is positioned on the wrapping paper that encases the cigarette plume.

5. the cigarette of claim 4, wherein the flavoring agent band is on the interior or outer surface of tipping paper.

6. the cigarette of claim 4, the flavoring agent of wherein sealing are positioned on the seam of tipping paper and the seam cohesive are provided.

7. the cigarette of claim 1, the flavoring agent of wherein sealing is to responsive to temperature, wherein will discharge flavoring agent in cigarette greater than 100 ℃ temperature, and wherein below 100 ℃ or under the temperature below 300 ℃, the flavoring agent that great majority are sealed keeps sealing.

8. the cigarette of claim 12, wherein when the temperature following time of a part of cigarette between 300 ℃ to 800 ℃, a part of menthol flavoring agent discharges from the polyvinyl acetate matrix.

9. the cigarette of claim 1, wherein based on 100 weight portion polyvinyl acetate, the amount of menthol flavoring agent is about 1-90%, 2-70% or 10-50% weight.

10. preparation comprises the method for the cigarette of adsorbent in its filter tip, and this method comprises:

Mix the flavoring agent of sealing, the described flavoring agent of sealing comprises the polyvinyl acetate matrix, wherein combination in the flavoring agent matrix of flavouring agent in the assembly of cigarette.

11. the method for claim 10 wherein forms the flavoring agent of sealing by following step:

Mixed alcohol and polyvinyl acetate;

Mix menthol in alcohol-polyvinyl acetate ester admixture, the consumption of menthol should be provided at the menthol flavoring agent that the tobacco smoke at least 10 μ g/ that produce in the cigarette aspiration procedure once aspirate effectively;

Reduce pure content or aging menthol-alcohol-polyvinyl acetate ester admixture in menthol-alcohol-polyvinyl acetate ester admixture; With

Form menthol-polyvinyl acetate ester fiber, film, material all in one piece, bead, powder or particle form by menthol-alcohol-polyvinyl acetate ester admixture.

12. the method for claim 10, wherein by heating and in solution mechanical shearing menthol flavoring agent and polyvinyl acetate, form the flavoring agent seal.

13. the method for claim 10 wherein by dissolving menthol flavoring agent and polyvinyl acetate in ethanol, methyl alcohol or its bond, forms the flavoring agent of sealing.

14. the method for claim 10 wherein by form the independent phase of menthol in the successive substrates of polyvinyl acetate, forms the flavoring agent of sealing.

15. the method for claim 10, wherein mixing the flavoring agent of sealing in the assembly of cigarette comprises, the flavoring agent mixture of liquid envelope is injected in the tobacco section of cigarette, the flavoring agent of liquid envelope is injected in the core of tobacco section of cigarette, on smokable filler, spray or coating liquid flavoring agent partly, and by spraying or the smokable filler of coating is formed for the plume of cigarette, the flavoring agent that the distribution liquid or solid is sealed in the middle of the plume of cigarette, the flavoring agent that solid is sealed is incorporated in the smokable filler, and by with seal the plume that smokable filler that flavoring agent mixes is formed for cigarette, perhaps place fiber in the cavity in the filter tip part of cigarette or in the smokable filler cigarette, material all in one piece, bead, the flavoring agent of powder or graininess part.

16. the method for claim 10 wherein by towards the surf zone fractional condensation on surface polyvinyl acetate of the flavoring agent sealed and the menthol surf zone away from the reinforcing agent of sealing, thereby forms the polyvinyl acetate matrix of menthol flavoring agent combination in matrix.

17. make mainstream tobacco smoke increase the method for flavor, this method comprises:

Keep flavoring agent with polyvinyl acetate matrix; With

Discharge flavoring agent from this matrix, generate mainstream tobacco smoke simultaneously, described release steps comprises and applies heat and/or moisture to matrix.

18. a smoking product, it is included in the menthol in the polyvinyl acetate matrix.