CA1158516A - Smoking articles and method of making such articles - Google Patents
Smoking articles and method of making such articlesInfo
- Publication number
- CA1158516A CA1158516A CA000377146A CA377146A CA1158516A CA 1158516 A CA1158516 A CA 1158516A CA 000377146 A CA000377146 A CA 000377146A CA 377146 A CA377146 A CA 377146A CA 1158516 A CA1158516 A CA 1158516A
- Authority
- CA
- Canada
- Prior art keywords
- tobacco
- accordance
- mass
- mixture
- passage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24C—MACHINES FOR MAKING CIGARS OR CIGARETTES
- A24C5/00—Making cigarettes; Making tipping materials for, or attaching filters or mouthpieces to, cigars or cigarettes
-
- 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
- A24D1/14—Tobacco cartridges for pipes
Landscapes
- Manufacture Of Tobacco Products (AREA)
Abstract
ABSTRACT
SMOKING ARTICLES AND METHOD OF MAKING SUCH ARTICLES
A smoking article (15) comprises a coherent mass (9) of combustible tobacco-containing material having at least one passage extending through it between two spaced openings in the surface of the mass, the tobacco mass having such porosity as to support combustion when ignited and such density and porosity as to substantially occlude gas flow therethrough. The article preferably has at least one air-permeable plug (5,6) of readily ignitable material blocking the passage at one or both ends. The tobacco-containing mass may include non-tobacco filler particles, such as carbon or clays, and the plug may contain a flavorant. The articles may be made by shaping a mixture of combustible tobacco material with a volatile liquid, for example a mixture of water and ethanol, under pressure into a discrete coherent mass, preferably by extrusion, forming a passage through the mass, and drying the mass to a porosity and density such as to substantially occlude gas flow therethrough but to support combustion when ignited.
SMOKING ARTICLES AND METHOD OF MAKING SUCH ARTICLES
A smoking article (15) comprises a coherent mass (9) of combustible tobacco-containing material having at least one passage extending through it between two spaced openings in the surface of the mass, the tobacco mass having such porosity as to support combustion when ignited and such density and porosity as to substantially occlude gas flow therethrough. The article preferably has at least one air-permeable plug (5,6) of readily ignitable material blocking the passage at one or both ends. The tobacco-containing mass may include non-tobacco filler particles, such as carbon or clays, and the plug may contain a flavorant. The articles may be made by shaping a mixture of combustible tobacco material with a volatile liquid, for example a mixture of water and ethanol, under pressure into a discrete coherent mass, preferably by extrusion, forming a passage through the mass, and drying the mass to a porosity and density such as to substantially occlude gas flow therethrough but to support combustion when ignited.
Description
S..~
SMOKING ARTlCLES AND METHOD OF MAKlNG SUCH ARTICLES
" .
Background of the Invention The present invention relates to smoking articles, particularly srnoking articles having distinctive physical properties, and it fur1her reia1es5 to a method of producing smoking articles so that such properties may be adjusted, thereby controlling their combustion behavior so as to achieve reduced tar delivery during smoking.
The guantity of combustion products produced by a burning bed of combystible material, such as tobacco or nontobacco smo!~ing materials, l0 is primarily dependent on certain physical properties of the burning ,, material. Th ? physical properties which influence the quantity of combus-tion products include the surface area of material available for combustion, i the density and porosity of the material, the volume of air available for f. ~ combustion, the velocity at which air is made available for combustion, thelS temperature at which the material combusts and the composition of the ~, combustible rnaterial.
A primary cause of tar production during combustion in a conventional smokina article, such as a cigarette, cigar or pipe, is pyrolysis.
, . Pyrolysis moy be defined as the thermal evolution of tars anci gases by heat ,.. .
-, ''~;
j ., , ~ , , , ,, ~ . . . ..
:,- ~ . .
!
produced from the combustion of- a carbonaceous incandescent coal~ As pyrolysis reduces smoking rnaterial to its carbonaceous skeleton, the car bonaceous remains, in turn, combust and provide heat for further pyrolysis of fresh material located adjacent to the combusting material.
Smoking materials used in conventional smoking articles are generally in the form Gf shredded tobacco leaf, shredded ræconstituted tobacco sheet, tobacco stems and combinations thereof and, as a result, such materials present a relatively large surface area for pyrolysis. In smoking a conventional smoki,,g article, moreover, gases drawn by a puff through the incandescent coal are heated. The heated gases pass through noncombusted tobacco adjc7cent to the coal and pyrolysis occurs. Thus, in conventional products pyrolysis occurs not only due to the heat of conduc-tion and radiation from the coal, but also due to the heat transferred by such heated gases to noncombus1ed tobacco adjacent the coal.
The present invention provides tobacco-containing smoking articles wherein control of combustion and pyrolysis processes is effected by adjusting properties, such as porosity, surface area and density of the tobacco-containing mass. 13y thus controlling the pyrolysis and combustion processes, ga~ phase and tar delivery by the articles of the present invention is concomitantly controlled.
Additionally, in conventional smoking articles of the above-mentioned type, substantial heat dissipation occurs in regions immediately adjacent the coal"hereby reducing the temperature of combustion gases as they progress down the article to tl-e point where they no longer can be used to effect thermal release of flavorants downstream of the coal. It has been observed that such heat reduction is significantly less for the articles of the present invention, thereby permitting downstream thermal flavorant release.
Summary o_the Invention - ¦ 30 This invention provides tobacco-containing smoking articles; j whrrein tar delivery during combustion is controlled by adjusting the density, porosity, surface area and/or composition of the article. The smoking articles comprise a coherent mass of combustible tobacco material, having at least one through passage extending from a first opening in the 35 surface of said mass to a second opening remote from tl7e first, said tobacco .; , I
mass being of a density and porosity such as to substanfially occlude gas flow therethrough, while further being of a porosity sufficient to support i combustion of said rnass when ignited.
In making such articles, a combustible tobacco material in S particulate form is mixed with one or more other ingredients including a liquid, the mixture being subjected to additional processing to produce a shaped coherent mass having a through passage therein. Shaping is effec1ed by application of pressure to the mixture to form the coheren, mass;
subsequently the formed or shuped mass is dried.
I û The articles may be formed by extrusion of a homogeneous mixture of tobacco material containing both water and a volatile organic liquid which is compatible with the tobacco, said mixture having a solids content of 55 to 75 weight percent, and drying the resuiting extrudate. The mixture for purposes of extrusion preferably contains comminuted tobacco of a mesh size less than about 3û mesh. Nontobacco filler particles, as well as burn additives and/or flavorants, may be included in the tobacco mass.
In a further aspect of the invention, improved characteristics are realized by further processing of the dried coherent mass, such furthe;
- processing including rewetting of the mass and subsequent redrying.
In a preferred embodiment, the smoking article of the invention . has a passage extending axially through a mass of cylindrical shape, the cross-sectional area of said passage most preferably being larger than that of the mass. It is also preferred to have an easily ignitable air permeable ~' i plùg disposed in passage blocking position in at least one end of the passage.
25 An additional plug or plugs of the same or different material may be included, at least at the outlet end, and may optionally contain flavorants which are thermally released.
When provided in conjunction with tl~e preferred extrusion process, it is preferable that the ignitable plug be extruded concurrently with the coherent mass.
Brief Description of the Drawinqs FIGURE I depicts in section a smoking article in accordance ', with the present invention, having a conventional filter attached thereto by ' ~ means of tipping paper.
FIGURE Ib is an end view of the smoking article of FIGURE 1.
.. .. -- --"
' ' `
:., r : FIGURE 2 shows in section a smoking article similar to FIGURE I having a plug positioned at both the mouth end and the ignition - end of said article.
FIGURE 3 is a sectional view of an alternative embodiment of 5 the invenfion in the form of a cigar-like smoking article having thickened walls, and fitted with a mouthpiece.
FIGURE 4 is a sectional view through a still further embodiment in the form of a smoking article comprising a preformed body of smoking material having multiple channels therethrough, and disposed in the bowl of 10 a pipe.
FIGURE S shows a smoking article sirnilar to FIGURE 4, in which the entire pipe bowl is preformed from combustible material.
: FIGURE 6 shows a f low diagram of steps involved in themanufacture of Q smoking articie in accordance with certain method aspects 15 of the present invention.
s FIGURE 7 Sho~Ns in schematic fashion extrusion equiprnerlt for performiny an extrusion step in accordance with a particular method of the invention.
" FIGURE ~ shows a die head for the extrusion equipment of ' 20 FIGURE 7.
General Description of the Invention ' In accordance with the present invention, tobacco-containing smoking articles formed from a coherent mass having at least one passage therethrou~h are provided. Delivery of tar and gas phase constituents is 25 controlled by adjusting the density, surface area and porosity of the combusting portion of the mass. By decreasing the surface area and porosity of the mass available for combustion, while increasing its density, it is possible to minimize the tar delivery by the smoking articles of the invention.
, 30 More particularly, the smoking articles of the present invention can be produced from a coherent mass of combustible tobacco-containing I material wherein the surface area of the m~ss available for the production " of tar may be considerably lower than that of a conventional smoking product in current usage. Moreover, the density of the mass in the instant - 35 smoking article may be significantly greater than that generally observed in ,~ .
.
conventional srnoking products, while the porosity of the mass is substan-- tially less. The resulting smoking articleohas substantially reduced tar and gas phase delivery relative to conventional smoking products.
By reducing porosity and surface area and increasing density of - 5 the material being burned, the smoking articles of the invention produce a reduced quantity of pyrolysis products per puff. Since 1he density, porosity - and geometry of the smoking articles of the invention control the volume of air and the velocity at which it is drawn over and through a burning coal during a puff and inhibit access of heated gases to unburned tobacco lO material, control of the pyrolysis and combustion processes in the pres~nt smoking articles is possible. r:urthermore, the 1emperature of the air passing throogh the passage of smoking articles of the invention can be maintained at a high enough level to effect thermal release of flavorants downstream of the burning coal thereby providing means for iow tar, fully i5 flavored srnoke delivery. The present smoking articles are thus advan-tageous in that shape, density and porosity of the mass will lower tar delivery naturally without the addition of chemicals that alter combustion ,...................................................................... .
;. and in certain instances adversely affect the subjective qualities of the tobacco, while permitting distillation of flavorants.
In the practice of the invention, a combustible tobacco-containing material is formed into a coherent mass having at least one ~ passage extending from a first opening in the surface of the mass to a ,. second opening remote from the first. Both the density and porosity of the formed n ass are such that puff induced air flow through the smoking article 25 is preferentially through the passage; that is, the density and porosity of the mass are such that gas flow longitudinally through the mass itself is substantially occluded. Porosity, however, must be high enough to support combustion and preferably sufficient to support static, nonpuff aided, combusl ion.
3û In a preferred embodiment of the invention, the mass is formed Tnto a cylinder having at least one passage axially therethrough. This j passage permits the dense smoking material to be puffed, aids in the control of volume nnd velocity of air which passes through the coal, reduces the coal volume and serves as an air conduit whereby the smoke generated 35 during combust;on is diluted by air when drawn upon by the smoker. This .
:
obviates the necessity of highh/ diluted, ventilated filters frequently employed in conventional low delivery sm~king articles.
The tobacco-containing material employed to form the coherent mass may comprise high quality, highly flavorful tobacco, such as bright, burley, Oriental or mixtures thereof, preferably in comminuted form. Other tobacco ma~erials, such as reconstituted tobaccos and prepyroiyzed fobaccos may also comprise ali or part of the tobacco-containing materials.
In a particularly preferred embodiment, the smoking article is made in the form of a hollow cylinder. Most preferably the wall thickness ;~ 10 of the coherent mass is such that the cross-sectional surface area of the mass is less than the corresponding cross-sectional area of the passage. In " such a smokin~ article, it is desirable to provide at least one plug for ~1 insertion in passage blocking position. The plug may be positioned at the end or ends of the smoking article and/or may be disposed at intermediate " . 15 positions in the passage.- Such plugs may serve either to aid ignition or as baffles to prevent flash heating through the tube due to suction on ignition or in the event of relighting. Additionally, one or more of the plugs may , contain flavorant materials. Plug material must be air permeable and, at ieast at one end, should be readily ignitable. Plugs preferably consist of comminuted tobacco material prepared in a similar manner to the coherent , mass.
Flavorant additions to the plugs (or for incorporation in the coherent mass) may be made during the preparation of either the tobacco-;S containing malerial, the plug material or both. Typical tobacco flavorants may be incorporated at any stage of processing, but it is general ly convenient to do so during mixing. Tobacco extracts may also be incor-porated at this point as part of the liquid ingredient. Extracts of Burley tobacco prepared according to methods described in U.S. Patents 4,131,117 and 4,131,118 may be used. Other tobacco extracts or slurries prepared by processes which release the pectinaceous binder material contained therein . may be employed similarly as part of the liquid ingredients in the production of the smoking articles. Descriptions of processes for releasing the natural ~:1 tobacco pectins may be found in U.S. Patent 3,353,541 or 3,420,421 to Hind.
The smoking articles of the present invention do not require an outer wrapper ot the tyye used in makir,g conventional cigalettes. However, '' ~ .
,.
~: .
~ ~ .
.. . ..
' ., :
it will be appreciated that an outer wrapping of cigarette paper or the like, - such as a coating rnaterial, or pigments il~corporated directly in the smoking - ' article, may be used to achieve the desired appearance.
,i In accordance with the method aspects of the present invention, S tobacco articles are formed by first mixing a quantity of tobacco-containing material with water and with a volatile organic liquid to provide a tobacco mixture suitable for subsequent processiny, i.e., shaping to provide a shaped - mass in any one of a number of discrete forms. Generally the tobacco materials to be mixed will have a moisture content in the range of about 5 to 15% OV, and preferably lû% OV. As used herein, the term OV (oven volatiles) represents the moisture content of tobacco determined as percent oven volatiles. OV is determined by placing a weighed sample of tobacco in an air-circulatina overi and maintaining the sample in the oven at a temperature of lû0C for a period of 3 hours after which the sample is again ~? 15 weighed. The difference in the two weight values, expressed as a percen-tage of the original weight, is defined as OV.
Prior to mixing, the tobacco may be comminuted to a desired particle size. Conventional means, such as a ball mill, a plate or disc-type ; ~ colloidal mi!l or blendor, may be used to effect comminution. The time ~0 required to accomplish this will, of course, depend on the original size of' tobacco components to be comminuted and to some extent on the type of tobaoco used as well as the moisture content thereof.
Mixing of the tobacco with the liquid ingredients may be effected with conventional equipment. For example, conventior,al Hobart ,, ~5 mixers equipped with a flat paddle or beater-type blade, ribbon-type mixers and the like or any other mixer that will effect homogenization or even distribution of liquid to tobacco is suitable.
In the mixing operation the addition of liquid ingredients to the tobacco particles may be simultaneous or the water may be added first followed by addition of the volatile agent. Mixing generally is accomplished at room lemperature and generally is effected in a closed container to prevent premature volatilization of the organic liquid. The time necessary to achieve even distribution of the liquid and tobacco particles depends to a J great extent on particle size as well as the ~ype of liquid combination used.
., , ' , ~ ~ ' Generully 15 minutes to several hours is sufficient to obtain the desired distribution of liquid.
Although it is usually desirable to prepare such mixture using both water and a volatile organic liquid in order to control porosity and 5 density of the coherent mass, it is possible to use only water in preparing the mixture, especially in cases where forming of the mixture is done by . , .
means of extrusion under conditions which can be variecl sufficiently to accomplish the desired results. Even so, one disadvantage is that the use of a sufficient quantity of water alone tends to make the density of the I û resulting mass too great as a practical matter. As noted elsewhere in greater detail, however, rewetting and redrying after forming the coherent mass ordinarily can be used to control its ultimate porosity as long as -ihe starting mixture can be extruded or otherwise formed acceptably into the . desired configuration.
ISThe volatile Grganic liquid of the mixture serves to improve the density and porosity characteristics of the final smoking article, possibly due to rapid vaporization during drying. The oryanic liquids which may be employed are preferably those haviny a higher vapor pressure than water ,i and include only those liquids which are compatible with tobacco products.
2û For purposes of this application, liquids are compatible with tobacco if theydo not appreciab!y react with tobacco constituents and, in addition, will mix '~,sufficiently with the tobacco material so as to avoid separation during the , Iarticle forming operation. Further, it is preferable to employ liquids which,when mixed with tobacco produc1s, do not adversely affect the aromatic or 25 subjective qualities thereof on smoking. Preferred liquids inclucle those which may easily be removed by evaporation under relath/c-ly nondrastic heating or drying conditions and which upon evaporation leave no appre-ciable residue. Among the suitable organic liquids are straight or branched-chain hydrocarbons of about S to 8 carbon atoms, such as the pentanes, 3û hexanes and heptanes. Straight or branched-chain alcohols selected from I
to 8 carbon atoms and including methanol, ethanol, propanol, isopropanol, butanol and the like are also suitable for use. Moreover, the "Freon" liquids including trichloromonofluoromethane and dichlorodifluoromethane may be used. Selected ketones, e.g., methyl ethyl ketone, ethers, halohydrocarbons 35 and the like, may be used in some instances. The selected liquid rnay be .
.
~ _9_ :.
used alone or, in some instances, a combination of two or more agents may be used depending on the type of smoking article being produced.
~ The ratio of total water in the mixture to volatile oryanic liquid will depend to some extent on the type and mesh of tobacco and the specific ~;~ 5 liquid being used but generally will be in the range of about 6 parts water to f~.~ I part organic liquid to about 1:1 ratio of each. Where less than -60 mesh tobacco is employed in accordance with the preferred forming practice ', discussed hereinbelow, a ratio of about 2 parts water to I part organic liquid ;,' is preferred.
~: 10 It may also be desirable to add filler materials to the aqueous : tobacco mixture. Filler materials can include calcium carbonate, selected carbon materials, diatornaceous earth, attapulgite and the like. Up 1o about ~, 40 to 50% of the solids in the mixture may comprise such fillers without ~i ~ requiring addition of binders. If desired, burn additives may also be added to the mixture to adjust burn properties.
* While it is preferable to avoid adding an extraneous binder and to rely instead on naturai binder substances of the tobacco, in order to achieve minimum tar delivery upon smoking, it will be recognized that the mechani-cal strength of such smoking articles may be increased through the use of . 20 qdditional binder materials provided that doing so is consistent with the delivery objectives of a particular product.
; When al I the desired ingredients have been added, and an homogeneous-mixture is obtained, the thus prepared mixture is ready for further processing to produce smoking articles. By this further processing, the tobacco mixture is formed into a shaped article comprised of a coherent tobacco mass whose density and porosity are sufficient to occlude gas flow ; therethrough and whose density is sufficient to support combustion of the mass when ignited. The tobacco mass is further provided with at least one ' passage extending therethrough from a first opening on the mass surface to 3û a second opening remote from the first opening. Providing of such passage as used herein means providing the same during the shaping operation or during operations subsequent thereto, or during both shaping and such subsequent operations.
In accordance with the im~ention, the article shaping operation includes pressure treatment of the mixture to transform the mixture into a :, .
!
,, :, . ' ' , '-, '', . ' , ...
. . . ~ ..
,, ':, ' `
,: -10-coherent or self-supporting tobacco mass and subsequent drying of the mass.
The pressure treatment will generally require application of pressure to the tobacco mixture in a confined space und, preferably, results in a coherent mass hQving the desired through passage. An alternate procedure woutd be 5 to form the mass without the passage and to subsequently create the - passage after the pressure treating operation, or after drying, by a material removal operation such as, for example, boring or drilling.
The pressure treatment can be effected by any one of a number of conventional techniques adapted to provide sufficient pressure to the tobacco mixture to cause release of the tobacco material's naturai binding agents, thereby resulting in a cohesive mass. The pressure forming operation thus enables self-supporting articles to be produced without the need to add extraneous binders to the tobacco mixture.
While pressure treatments such as moldin~ can be used lo implement the invention, a preferable treating technique is extrusion. In general, extrusion conditions will depend upon the type of extruder used (ram, screw, etc.), the particular composition of the tobacco mixture and the desired shape, density and porosity conditions for the resultant extru-date.
Conventional screw extruders or higher pressure producing ram extruders may be employed, with the die heads of these extruders preferably having the desired shape of the smoking articles to be produced. These extruders may be operated at selected pressures and with selected cooling of one or more sections of the extruder barrel to promote production of the desired extrudate. An extruder found suitable is a Wayne plastics extruder equipped with a 1:1 screw adapted to rotate at I to 120rpms. Such an extruder, due to its 1:1 screw, does a minimum of work on the tobacco mixture, while providing pressure sufficient to release the natural binding agents of the tobacco and thereby resu!t in a cohesive product. With screw extruders of this type, extrudate pressures at the end of the extruder barrel (i.e., melt pressures) of up to 25ûû psig are useabie, with pressures of up to 120û psig being preferable. Extrudate temperatures at such barrel end (i.e., melt temperatures) of less than about 40C also are useable and can be developed by maintaining the screw barrel temperature in the range of about 20 to 25C.
" ~
-:
Preferable tobacco mixture conditions for extrusion are a - tobacco particle size of below about .30 mesh and a 10bacco content sufficient to produce a mixture having a solids content in the range of about 55 to 75 weight percent solids, and preferably about 60 to 70 percent solids.
As above indicated, the shape of the desired smoking articles controls the extruder die head construction Preferable smoking articles are of hollow cylindrical shape and, more preferably, are cylindrical tubes - having a wall thickness such that the cross-sectional area of lhe mass is less than the corresponding cross-sectional area of the passaae. Die heGds lO having a suitably adapted annular extrusion passage are thus employed to achieve this construction. A particular extruder for realizing hollow cylinders is the aforementioned Wayne extruder. Thus, for example, thin-walled tobacco tubes having a high density and low porosity and which burn with coal temperatures in the range of 585C to 785C may be produced with 15 suitably modified extruders of this type. Additionally, when using such extruders it is customary to introduce air flow into the inner part of the formed tube to prevent collapse thereof.
Forming part of the article pressure trea1ing operation may be a severing or separating operation vhich results in the production of individual , ,, 20 coherent masses corresponding to individual smoking articles. Such an operation is necessary if pressure treatment is not itself on an individual article basis. In the case of the above-described preferred extrusion practice, wherein the extrudate `Nill typically be a single cohesive con-tinuous length mass exiting from the extruder die, it is desirable to perform . 25 a cutting operation at the die exit, thereby to form individual units of length corresponding to that of the desired smoking articles. Where articles of preselected length are desired, the cutting operation is synchronized with the rate of extrudate output to provide the required length.
The aforesaid operation of providing ir1dividual units also may be 30 effected subsequent to the drying of the extrudate if severing of the dried extrudate is found to be a more acceptable practice.
~' Drying the resultant pressure-formed coherent mass may be accomplished either by simple evaporation at ambient environment, e.g., room temperature, or by application of heat. Typically, at a room 35 temperature of from about 7û 1o 75F, typical drying times might range from about 12 to 24 hours. Heat application might be at a temperature of about 100~C. This can be done by conventional heating means such as a Freas oven ~forced air oven) over a period of time from about 15 minutes to I hour. Heating can also be accomplished more rapidly by microwave 5 application in which case the time of application will depend upon the power used. A1 power levels about about 150 watts, drying times of about 2 minutes have been found acceptable. Such rapid drying may be employed to enhance the static burn properties of the resultant smoking article.
Following the drying operation, the dried articles may be further 10 processed as by affixing the articles to suitable mouthpieces which may or may not include filters fo result in the completed smoking article construc-tion.
While the method of the invention as described above has been found to provide suitable smoking articles, a further aspect of the invention 15 is to provide further processing of the pressure-formed coherent mass subseauent to the initial drying operation. Such further processing enables changing of the porosity of the dried mass, whereby improved combustion characteristics of the resultant smoking product result. This further processing comprises rewetting the dried mass and subsequent redrying.
20 Rewetting may be carried out by spraying or immersion of the dried mass.
Suitable rewetting has been carried out by immersing the mass in a bath of liguid, preferably water, for a time sufficient to obtain the desired change in porosity. In general, rewetting conditions will depend upon initial porosity, tobacco particie size and the type of organic fiuid used. Suitable 25 rewetting conditions to realize desired porosity changes can be determined through empirical procedures. Subsequent redrying after the rewetting is preferably carried out in accordance with the initial drying procedure discussed hereinabove.
In a further aspect of the method of the invention, the method is 30 further modified to allow for disposition of a readily ignitable air permeable plug in the through passage of the pressure-formed coherent mass. Other plugs may be placed at one or more positions along the passage and in blocking relation thereto. In a preferred practice of the present invention wherein cylindrical tubular smoking articles are formed, it is desirable to 35 situate such plugs at opposite ends of the tubular passage.
Usually only one or two such plugs will be needed, especially at one end for lighting the smoking article. Consequently, the typical embodiments have a hollow passageway that is laraely unrestricted. It will be appreciated, however, that such passageway may be filled partly or ; 5 wholly with an innocuous filler materiql which either is non-cambustible or does not contribute excessively to the production of tar upon smoking.
Plug rnaterial rnay take various forms and may contain flavor-ants releaseablc upon heating. Plug material preferably comprises com-minuted tobacco prepared in the same manner as the coherent mass forming the smoking article. Plugs can, therefore, be formed using a procedure analogous to that outlined above for making the coherent mass, with pressure treatment modified as may be necessary to produce plugs of the desired configuration and sui1able for insertion in the coherent mass in passage blocking relation. Air permeability for the plugs may be realized IS either through the inherent porosity of the plug material or by through orifices prov-.ded in the plug during or after plug formation.
While plugs might be formed independently of the coherent mass and inserted in the mass subsequent to its formation or subsequent to drying, in a preferred practice the plugs are formed and situated in the mass passage simultaneoùsly or concurrently with mass formation. In yet a f~rrther preferred practice, this is accomplished in the pre~erred extrusion procedure by co-extruding the plug with the mass in suitably timed relationship so as to obtain plugs of desired size at desired passage blocking positions and in intimate contact with the inner mass wall.
~escription of the Preferred Embodiments The srnoking article of the present invention can be made in various forms particularly those which are conveniently extruded, although other article shaping methods can be employed to that end. With reference now to FIGURE 1, the smoking article I0 comprises an elongated coherent mass 9 shaped in this embodiment as a tubular rod having a through passage 2 extending end to end thereof. While the tubular mass 9 serves in and of itself as a smoking article, it is possible tsee FIGURE 2) to fit a filter 3 at the smoking end and join same to the mass 9 with tipping paper 4 in conventional manner. As seen in FIGURE Ib, the passage 2 and the mass 9 have circular configuration but it will be appreciated that other ... . . .
. -: : :' '' , , . : , sectional geometrics could be employed, for example, hexagonal, etc. The mass 9 rnay correspond generally in length and circumference to that of conventional sized cigarette tobacco cylinders. Depending upon the par-ticular delivery characteristics to be produced with the article upon smoking 5 of same, the cross-sectional area of the mass relative to the passage will be varied.
The srnoking article 15 shown in FIGURE 2 is fitted at the ignition end with a passage blocking plug 5 of air permeable combustible material. In addition to functioning as qn ignition device, the plug 5 lO func1ions to prevent flash heating through 1he passage when lighting the smoking article. Additional plugs, for example, the plus 6 shown adjacent the filter component 3 can be provided and may serve to embody flavorant materials in the smoking article. If desired, plugs could also be disposed at one or more locations intermediate the ends of the smoking article to serve 15 as either flavorant carriers or ignition means, or both.
In accordance with the present invention, the smoking article can be provided in the familiar shapes of other types of smoking articles, as for example, in the fashion and approximate dimensions of a cigar 16 as shown in FIGURE 3. In such article 16, the walls 7 of the tubular mass will 2û be of greater thickness relative to the size of the article and as compared with the FIGURE 2 smoking article. In addition to ignition and flavorant :~ plugs 5 and ~, the article can be fitted with a mouthpiece !7, which in turn itself can serve to embody flavor releasing elements or filter means 8.
FIGURES 4 and 5 illustrate the manner of providing a smoking 25 article either for utilization in a conventional smoking pipe or as a pipe shaped component as such. The smoking article 3û shown in FIGURE 4 is formed as a relatively truncated rnass l9 shaped and sized for reception in the bowl of pipe 18, with the mass being provided with one or more through passages 2 extending from top to bottom thereof. FIGURE 5 shows the 30 manner in which a coherent mass 20 is shaped in the form of a smoking pipe bowl and, like the FIGURE 4 mass, has one or more passages 2 and is fitted with a side opening as at 21 for reception of a pipe stem 28 having a filter 40 as does pipe 18.
FIGURE 6 illustrates schematicaily a preferred embodiment of 35 the invention wherein tobacco is comminuted, mixed with water and a J, ~ Y'~
volatile organic liquid and then subjected to a pressure treatment, prefer-ably extrusion, to produce a coherent tobacco mass. The tobacco mass is dried at room temperature or by application of heat. Further processing of the coherent 1obacco mass to alter the porosity thereof is achieved by a S rewettiny step followed by a drying step.
FIGURE 7 shows schematically extrusion e~uipment for provid-ing the aforesaid co-extrusion of a tubular coherent mass and plugs in accordance with the method of the invention, the die head construction being shown in greater detail in FIGURE 8. Turning to FIGURE 7, a tobacco mixture as above-described for forming the coherent mass or body of the smoking article is supplied to an automatic hopper feeder 71. The hopper 71 applies a continuous force to the tobacco mixture via a rotating blade which extends into a material receiving port of a screw extruder 72 driven by a drive 73. The tobacco mixture is force fed to the extruder 72 and the extrudate developed in the extruder is forced into a cornmon die head 74 ; where it is formed into a tubular coherent mass 100 at the die head exit.
Air also is supplied to the die head 74 from a source 75 and is conveyed by a line 76 to the die head exit interiorly of the tubular mass 100 to prevent collapse thereof as the mass is being formed.
; 20 Plug malerial of similar composition to the mass material issupplied to a hopper feeder 81 having a construction analogous to that of hopper feeder 71. The plug material is fed by hopper 81 to a plug screw extruder 82 which is driven by a drive 83. Extrudate passes from the extruder 83 through the valve 84 into the common die head 74 where it is made available interiorly of and joined to the inner wall of the tubular mass lûO.
Control synchronization circuit 91 effects control of the continued pre~sure applied to the pluy extrudate in passing to the head 74.
This control is synchronized with the issuance of the tube 100. Circuit 91 :! 30 maintains the valve 84 closed and the drive 83 stopped for a predetermined period of time corresponding to the delivery of a preselected length of tube.
~fter such time the valve 84 is opened and the drive 83 restarted, causing pressyre to be applied to the plug ex,rudate and, as a result, common -j delivery of plug and tube. This condition lasts for a second predetermined ' 35 period of time corresponding to the common delivery of a preselected length , , : ,, .
`~ of tube and plug, after which the valve is again closed and the drive 83 is agnin stopped. Repeated control of the v~lve 94 and drive 83 thus results in the tube lOû being continuously extruded with plugs 101 of determined ler.gth being disposed at determined space positions therein and in passnge 5 blocking relationship thereto.
Control synchronization circuit 9! also cortrols the direction of rotation of the blades of the hoppers 81 and 71. This direction is changed - periodically by the circuit 91 to ensure proper delivery of tobacco mixture to the respective screw extruders.
Also shown in FIGURE 7 is a cutting assembly 92 at the die head exit which also is synchronously opera,ed by the control circuit 91 to cut the tube lOû into individucll coherent mass units. Such cutting operation can be synchronized to occur immediately before disposition of a plug 101, whereby each unit will contain a single plug at the forward passage thereof.
15 Preferably, however, the- cutting assembly is controlled to effect cutting sothat units are produced having plugs at both ends. This is realized by controlling the plug extruder operation 10 issue plug material of desired length and by correspondingly controlling the cutting assembly to sever the tube 100 at positions along the length of each extruded plug.
FIGURE 8 illustrates the common die head 74 of FIGURE 7 in greater detail. As illustrated die head 74 includes an outer casing or support assembly 110 comprised of a central hollow cylindrical body 111 to whose opposite ends are attached by screws (not shown) support rings 112 and 113.
A central recessed section 114 of the body 111 cooperates with a facing central recessed section 115 of the ring 112 to suppor1 a first holiow mandrel 116. Inner conical surface 117 of mandrel 116 extends to a short cylindricol guide surface 118, the latter surface l 18 terminating at the end of ring 112 to define an exit orifice 119.
J A further hollow mandrel 121 is supported by ring 113 and by a hollow retainer element 122 held between the latter ring and body I 11. The mandrel 121 extends the length of the assembly 110 and the mandrel outer surface 123 is spaced from the respective inner surfaces 128 and 117 of body 111 ar;ri mandrel 116. These surfaces (123, 128, 117) define an annular passage 124 for receipt of the tubular mass extrudate from the extruder 73.
Surface 1 Z3 is topered inw~rdly in the region of the surfoce 117, both " "
; - surfaces cooperatir,g to provide an exit annular passage 125 of radial i~- expanse corresponding to the thickness of the tubular mass to be formed and of outer diameter commensurate with the guide surface 118.
A central bore 126 extends the length of mandrel 121 and f 5 receives plug extrudate from the extruder 82. Bore 126 at the end of 4,~ mandrel 121 is of expanse substantially equal to that of the inner diameter of the exit passage 125, whereby plug extrudate of such expanse is delivered to the end of the exit passage. Air line 76 passes throuah the bore 126 and delivers air to the region adjacent the passage 125 and the exit port 119 to prevent collapse of the tube lûû as it is being extruded.
In operation, pressure applied to the tubular mass extrudate via the extruder 73 forces the extrudate into the passage 124 and thence to the exit annular passage 125. The extrudate departs the passage 125 as the thin walled tubular coherent mass lûû, the latter mass being guided by cylin-drical surface 118 to exit port 119. With no pressure applied to the plug extrudate by the extruder 82, the lubular mass lOû exits without plug material and passes through a constriction ring 127 attached to the ' mandrel 116.
Upon pressure being applied to the plug extrudate by the extruder 82, the extrudate is forced through the central bore 126 ancl supplied to the end of the annular passage 125 where it is received inleriorly of and in contact with the inner wall of the simultaneously formed tubular mass 100. As pressure continues to be applied to the plug extrudate, the plug extrudate and the tubular mass together pass through exit port 119 into the central orifice 129 of the rina 127. The latter orifice tapers inwardly and thereafter outwardly, the inward taper ending at a radial expanse which is less than the outer diameter of the tubular mass. Upon reaching the end of the inward taper, the forward end of the tubular mass is inwardly constricted forcing its wall into cohesiye engagement v~/ith the forward end 3û of the plug extrudate. At this time, the pressure applied to the plug extruda1e terminates, and the tubular mass which continues to be extruded and is now joined to the plug extrudate breaks from the plug extrudate a plug lûl which continues to move with the tube through the orifice 129.
The portion of the tube coextensive with the plug is thereupon continuously 3~ constricted over further incremental areas, thereby cohesively joining the "
" . .
'.
` plug to the fube wall over the entire plug length. In this way the tube and plug are joined without excessive drag being placed on the tubular mass, - whereby thickening of the tube wall is prevented during the joining operat ion.
S It should be noted that cohesive joining of the plug 101 and the tubular mass 100 can be effected in other ways such as, for example, by expanding the plug by known methods so it cohesively joins to the mass wall.
As noted above, air-permeability of the plugs 101 call be brougl,t about in the plug forming operation and it is contemplated that the die head 10 of FIGURE 8 can be modified to provide through orifices in the plugs as they are being extruded. This can be accomplished by the placement of spaced thin solid rods 131 in the bore 126, such rods extending from a point in the bore to beyond the annular passage 125 These rods might be held by a ring 133 which can be placed between sections of the mandrel 121, thereby 15 placing the rods in their desired position in the bore 1~6.
Density of the rods formed in the hereinbelow examples was determined according to the following formula:
Density (g/cc) = n x [~02D~ ~ ¦l2D~ ] X rrOOd Ween;q9thht 20 wherein OD is the outer diameter of the rod in centimeters, ID is the inner diameter of the rod in centimeters and the length and weight of the rod are in centimeters and grams respectively.
Pressure drop (aP) was measured by blocking an open extruded tube at one end while inserting the other end in a pressure drop instrument 25 (P.D.I.). The ~P recorded is inversely proportional to the air flow through i the walls of the tube.
The following examples are illustrative of the invention.
Example I
Bright tobacco having an approximate moisture content of 30 11.6% OV was ground in a Fritsch-Pulverisette grinder. The ground tobacco was passed through a 6û-mesh screen to remove coarse particles and the fraction having a sieve size of 6û or smaller (-60 mesh) was selected for i fur ~her processing.
J
i - ' r --19-To 22~9 9 of the -60 mesh tobacco having a moisture content of 11.06% OV, was added 48.0 ml of 95% ethanol and 47.1 9 water. This mixture was stirred for approximately 20 minutes in a Hobart mixer (Model N-SQ) equipped with a conventional "B"-flat beater blade.
The tobacco mixture having a solids content of 64.5% by weight was then extruded to form tubes having a wall thickness of û.5 mm. A
Wayne Plastics 1" extruder with 1:1 compression ratio screw, 3 zone automatic heat, and 3 zone automatic fan cooling, straight tubing die having an 8 mm outer diameter (OD) and 7 mm inner diameter (ID) and 3 HP
lû variable speed ~û to 60 rpm) drive was employed ta effect extrusion. Zones I through 3 were maintained at room temperature. The maximum die head pressure was 1500 psig. Although these extrusion conditions were favorable for smal I runs, for longer, continuous runs it was necessary to cool the barrel to preven7 skin formation on the rod.
Some of the extruded tobacco tubes were dried in an Apollo l~llicrowave oven for S minutes at maximum power. After drying, the tubes were ignited and maintained a static burn.
Extruded tubes were also allowed to dry at room tempera1ure overnight. These tubes were then cut into 85 mm lengths having an average measured weight of 12.70 mg/mm and a calculated density of 1.078 g/cc.
Four of these tubes were allowed to static burn, and the averaae burn time was determined and found to be 4.8 mm/minute. Other room temperature dried tubes were smoked automatically under controlled laboratory condi-tions. TPM and tar delivery were measured using standard analytical techniqves of the tobacco industry. l he average TPM/puff was û.35 rng and the average tar/puff was 0.28 mg.
Example 2 677.7 g of bright tobacco (-60 mesh~ 17avir,g a moisture content of 1 1.56% OV was combined with 144 ml 95% ethanol and 138 9 water. The mixture was stirred in a Hobart mixer for 30 minutes, covered and left at ambient temperature for l.S hours. The percent solids prior to extrusion was 65.82~.
lhe equipment and conditions for extrusion were the same as i those of Example 1. The die pressure during the collection of samples was 35 approxima~el~ 500 psig, and ?he maximum melt temperature ot 1he extru-~ . ~
date at the die head was 110F. The extruded tubes had an outer diameter of 8 mm ar-ld an inner diqmeter of 7 mm and a wall thickness of 0.5 mm.
The tubes were allowed to dry overnight at room temperature.
Representative samples were cut to 85 mm lengths, having an average weight of 12.64 mg/mm. The calculated density was 1.073 g/cc. The static , burn was determined as in Example I and found to be 3.52 mm/min. TPM
and tar delivery/puff, also determined as in Example 1, were found to be 0.26 mg and 0.16 mg respectively.
- In addition, the smoke from the third puff of four tobacco tubes was collected and their gas phase constituents measured using conventional ~as chromatography techniques. The qverage gas concentrations of the third puff of the four samples was as follows:
SMOKING ARTlCLES AND METHOD OF MAKlNG SUCH ARTICLES
" .
Background of the Invention The present invention relates to smoking articles, particularly srnoking articles having distinctive physical properties, and it fur1her reia1es5 to a method of producing smoking articles so that such properties may be adjusted, thereby controlling their combustion behavior so as to achieve reduced tar delivery during smoking.
The guantity of combustion products produced by a burning bed of combystible material, such as tobacco or nontobacco smo!~ing materials, l0 is primarily dependent on certain physical properties of the burning ,, material. Th ? physical properties which influence the quantity of combus-tion products include the surface area of material available for combustion, i the density and porosity of the material, the volume of air available for f. ~ combustion, the velocity at which air is made available for combustion, thelS temperature at which the material combusts and the composition of the ~, combustible rnaterial.
A primary cause of tar production during combustion in a conventional smokina article, such as a cigarette, cigar or pipe, is pyrolysis.
, . Pyrolysis moy be defined as the thermal evolution of tars anci gases by heat ,.. .
-, ''~;
j ., , ~ , , , ,, ~ . . . ..
:,- ~ . .
!
produced from the combustion of- a carbonaceous incandescent coal~ As pyrolysis reduces smoking rnaterial to its carbonaceous skeleton, the car bonaceous remains, in turn, combust and provide heat for further pyrolysis of fresh material located adjacent to the combusting material.
Smoking materials used in conventional smoking articles are generally in the form Gf shredded tobacco leaf, shredded ræconstituted tobacco sheet, tobacco stems and combinations thereof and, as a result, such materials present a relatively large surface area for pyrolysis. In smoking a conventional smoki,,g article, moreover, gases drawn by a puff through the incandescent coal are heated. The heated gases pass through noncombusted tobacco adjc7cent to the coal and pyrolysis occurs. Thus, in conventional products pyrolysis occurs not only due to the heat of conduc-tion and radiation from the coal, but also due to the heat transferred by such heated gases to noncombus1ed tobacco adjacent the coal.
The present invention provides tobacco-containing smoking articles wherein control of combustion and pyrolysis processes is effected by adjusting properties, such as porosity, surface area and density of the tobacco-containing mass. 13y thus controlling the pyrolysis and combustion processes, ga~ phase and tar delivery by the articles of the present invention is concomitantly controlled.
Additionally, in conventional smoking articles of the above-mentioned type, substantial heat dissipation occurs in regions immediately adjacent the coal"hereby reducing the temperature of combustion gases as they progress down the article to tl-e point where they no longer can be used to effect thermal release of flavorants downstream of the coal. It has been observed that such heat reduction is significantly less for the articles of the present invention, thereby permitting downstream thermal flavorant release.
Summary o_the Invention - ¦ 30 This invention provides tobacco-containing smoking articles; j whrrein tar delivery during combustion is controlled by adjusting the density, porosity, surface area and/or composition of the article. The smoking articles comprise a coherent mass of combustible tobacco material, having at least one through passage extending from a first opening in the 35 surface of said mass to a second opening remote from tl7e first, said tobacco .; , I
mass being of a density and porosity such as to substanfially occlude gas flow therethrough, while further being of a porosity sufficient to support i combustion of said rnass when ignited.
In making such articles, a combustible tobacco material in S particulate form is mixed with one or more other ingredients including a liquid, the mixture being subjected to additional processing to produce a shaped coherent mass having a through passage therein. Shaping is effec1ed by application of pressure to the mixture to form the coheren, mass;
subsequently the formed or shuped mass is dried.
I û The articles may be formed by extrusion of a homogeneous mixture of tobacco material containing both water and a volatile organic liquid which is compatible with the tobacco, said mixture having a solids content of 55 to 75 weight percent, and drying the resuiting extrudate. The mixture for purposes of extrusion preferably contains comminuted tobacco of a mesh size less than about 3û mesh. Nontobacco filler particles, as well as burn additives and/or flavorants, may be included in the tobacco mass.
In a further aspect of the invention, improved characteristics are realized by further processing of the dried coherent mass, such furthe;
- processing including rewetting of the mass and subsequent redrying.
In a preferred embodiment, the smoking article of the invention . has a passage extending axially through a mass of cylindrical shape, the cross-sectional area of said passage most preferably being larger than that of the mass. It is also preferred to have an easily ignitable air permeable ~' i plùg disposed in passage blocking position in at least one end of the passage.
25 An additional plug or plugs of the same or different material may be included, at least at the outlet end, and may optionally contain flavorants which are thermally released.
When provided in conjunction with tl~e preferred extrusion process, it is preferable that the ignitable plug be extruded concurrently with the coherent mass.
Brief Description of the Drawinqs FIGURE I depicts in section a smoking article in accordance ', with the present invention, having a conventional filter attached thereto by ' ~ means of tipping paper.
FIGURE Ib is an end view of the smoking article of FIGURE 1.
.. .. -- --"
' ' `
:., r : FIGURE 2 shows in section a smoking article similar to FIGURE I having a plug positioned at both the mouth end and the ignition - end of said article.
FIGURE 3 is a sectional view of an alternative embodiment of 5 the invenfion in the form of a cigar-like smoking article having thickened walls, and fitted with a mouthpiece.
FIGURE 4 is a sectional view through a still further embodiment in the form of a smoking article comprising a preformed body of smoking material having multiple channels therethrough, and disposed in the bowl of 10 a pipe.
FIGURE S shows a smoking article sirnilar to FIGURE 4, in which the entire pipe bowl is preformed from combustible material.
: FIGURE 6 shows a f low diagram of steps involved in themanufacture of Q smoking articie in accordance with certain method aspects 15 of the present invention.
s FIGURE 7 Sho~Ns in schematic fashion extrusion equiprnerlt for performiny an extrusion step in accordance with a particular method of the invention.
" FIGURE ~ shows a die head for the extrusion equipment of ' 20 FIGURE 7.
General Description of the Invention ' In accordance with the present invention, tobacco-containing smoking articles formed from a coherent mass having at least one passage therethrou~h are provided. Delivery of tar and gas phase constituents is 25 controlled by adjusting the density, surface area and porosity of the combusting portion of the mass. By decreasing the surface area and porosity of the mass available for combustion, while increasing its density, it is possible to minimize the tar delivery by the smoking articles of the invention.
, 30 More particularly, the smoking articles of the present invention can be produced from a coherent mass of combustible tobacco-containing I material wherein the surface area of the m~ss available for the production " of tar may be considerably lower than that of a conventional smoking product in current usage. Moreover, the density of the mass in the instant - 35 smoking article may be significantly greater than that generally observed in ,~ .
.
conventional srnoking products, while the porosity of the mass is substan-- tially less. The resulting smoking articleohas substantially reduced tar and gas phase delivery relative to conventional smoking products.
By reducing porosity and surface area and increasing density of - 5 the material being burned, the smoking articles of the invention produce a reduced quantity of pyrolysis products per puff. Since 1he density, porosity - and geometry of the smoking articles of the invention control the volume of air and the velocity at which it is drawn over and through a burning coal during a puff and inhibit access of heated gases to unburned tobacco lO material, control of the pyrolysis and combustion processes in the pres~nt smoking articles is possible. r:urthermore, the 1emperature of the air passing throogh the passage of smoking articles of the invention can be maintained at a high enough level to effect thermal release of flavorants downstream of the burning coal thereby providing means for iow tar, fully i5 flavored srnoke delivery. The present smoking articles are thus advan-tageous in that shape, density and porosity of the mass will lower tar delivery naturally without the addition of chemicals that alter combustion ,...................................................................... .
;. and in certain instances adversely affect the subjective qualities of the tobacco, while permitting distillation of flavorants.
In the practice of the invention, a combustible tobacco-containing material is formed into a coherent mass having at least one ~ passage extending from a first opening in the surface of the mass to a ,. second opening remote from the first. Both the density and porosity of the formed n ass are such that puff induced air flow through the smoking article 25 is preferentially through the passage; that is, the density and porosity of the mass are such that gas flow longitudinally through the mass itself is substantially occluded. Porosity, however, must be high enough to support combustion and preferably sufficient to support static, nonpuff aided, combusl ion.
3û In a preferred embodiment of the invention, the mass is formed Tnto a cylinder having at least one passage axially therethrough. This j passage permits the dense smoking material to be puffed, aids in the control of volume nnd velocity of air which passes through the coal, reduces the coal volume and serves as an air conduit whereby the smoke generated 35 during combust;on is diluted by air when drawn upon by the smoker. This .
:
obviates the necessity of highh/ diluted, ventilated filters frequently employed in conventional low delivery sm~king articles.
The tobacco-containing material employed to form the coherent mass may comprise high quality, highly flavorful tobacco, such as bright, burley, Oriental or mixtures thereof, preferably in comminuted form. Other tobacco ma~erials, such as reconstituted tobaccos and prepyroiyzed fobaccos may also comprise ali or part of the tobacco-containing materials.
In a particularly preferred embodiment, the smoking article is made in the form of a hollow cylinder. Most preferably the wall thickness ;~ 10 of the coherent mass is such that the cross-sectional surface area of the mass is less than the corresponding cross-sectional area of the passage. In " such a smokin~ article, it is desirable to provide at least one plug for ~1 insertion in passage blocking position. The plug may be positioned at the end or ends of the smoking article and/or may be disposed at intermediate " . 15 positions in the passage.- Such plugs may serve either to aid ignition or as baffles to prevent flash heating through the tube due to suction on ignition or in the event of relighting. Additionally, one or more of the plugs may , contain flavorant materials. Plug material must be air permeable and, at ieast at one end, should be readily ignitable. Plugs preferably consist of comminuted tobacco material prepared in a similar manner to the coherent , mass.
Flavorant additions to the plugs (or for incorporation in the coherent mass) may be made during the preparation of either the tobacco-;S containing malerial, the plug material or both. Typical tobacco flavorants may be incorporated at any stage of processing, but it is general ly convenient to do so during mixing. Tobacco extracts may also be incor-porated at this point as part of the liquid ingredient. Extracts of Burley tobacco prepared according to methods described in U.S. Patents 4,131,117 and 4,131,118 may be used. Other tobacco extracts or slurries prepared by processes which release the pectinaceous binder material contained therein . may be employed similarly as part of the liquid ingredients in the production of the smoking articles. Descriptions of processes for releasing the natural ~:1 tobacco pectins may be found in U.S. Patent 3,353,541 or 3,420,421 to Hind.
The smoking articles of the present invention do not require an outer wrapper ot the tyye used in makir,g conventional cigalettes. However, '' ~ .
,.
~: .
~ ~ .
.. . ..
' ., :
it will be appreciated that an outer wrapping of cigarette paper or the like, - such as a coating rnaterial, or pigments il~corporated directly in the smoking - ' article, may be used to achieve the desired appearance.
,i In accordance with the method aspects of the present invention, S tobacco articles are formed by first mixing a quantity of tobacco-containing material with water and with a volatile organic liquid to provide a tobacco mixture suitable for subsequent processiny, i.e., shaping to provide a shaped - mass in any one of a number of discrete forms. Generally the tobacco materials to be mixed will have a moisture content in the range of about 5 to 15% OV, and preferably lû% OV. As used herein, the term OV (oven volatiles) represents the moisture content of tobacco determined as percent oven volatiles. OV is determined by placing a weighed sample of tobacco in an air-circulatina overi and maintaining the sample in the oven at a temperature of lû0C for a period of 3 hours after which the sample is again ~? 15 weighed. The difference in the two weight values, expressed as a percen-tage of the original weight, is defined as OV.
Prior to mixing, the tobacco may be comminuted to a desired particle size. Conventional means, such as a ball mill, a plate or disc-type ; ~ colloidal mi!l or blendor, may be used to effect comminution. The time ~0 required to accomplish this will, of course, depend on the original size of' tobacco components to be comminuted and to some extent on the type of tobaoco used as well as the moisture content thereof.
Mixing of the tobacco with the liquid ingredients may be effected with conventional equipment. For example, conventior,al Hobart ,, ~5 mixers equipped with a flat paddle or beater-type blade, ribbon-type mixers and the like or any other mixer that will effect homogenization or even distribution of liquid to tobacco is suitable.
In the mixing operation the addition of liquid ingredients to the tobacco particles may be simultaneous or the water may be added first followed by addition of the volatile agent. Mixing generally is accomplished at room lemperature and generally is effected in a closed container to prevent premature volatilization of the organic liquid. The time necessary to achieve even distribution of the liquid and tobacco particles depends to a J great extent on particle size as well as the ~ype of liquid combination used.
., , ' , ~ ~ ' Generully 15 minutes to several hours is sufficient to obtain the desired distribution of liquid.
Although it is usually desirable to prepare such mixture using both water and a volatile organic liquid in order to control porosity and 5 density of the coherent mass, it is possible to use only water in preparing the mixture, especially in cases where forming of the mixture is done by . , .
means of extrusion under conditions which can be variecl sufficiently to accomplish the desired results. Even so, one disadvantage is that the use of a sufficient quantity of water alone tends to make the density of the I û resulting mass too great as a practical matter. As noted elsewhere in greater detail, however, rewetting and redrying after forming the coherent mass ordinarily can be used to control its ultimate porosity as long as -ihe starting mixture can be extruded or otherwise formed acceptably into the . desired configuration.
ISThe volatile Grganic liquid of the mixture serves to improve the density and porosity characteristics of the final smoking article, possibly due to rapid vaporization during drying. The oryanic liquids which may be employed are preferably those haviny a higher vapor pressure than water ,i and include only those liquids which are compatible with tobacco products.
2û For purposes of this application, liquids are compatible with tobacco if theydo not appreciab!y react with tobacco constituents and, in addition, will mix '~,sufficiently with the tobacco material so as to avoid separation during the , Iarticle forming operation. Further, it is preferable to employ liquids which,when mixed with tobacco produc1s, do not adversely affect the aromatic or 25 subjective qualities thereof on smoking. Preferred liquids inclucle those which may easily be removed by evaporation under relath/c-ly nondrastic heating or drying conditions and which upon evaporation leave no appre-ciable residue. Among the suitable organic liquids are straight or branched-chain hydrocarbons of about S to 8 carbon atoms, such as the pentanes, 3û hexanes and heptanes. Straight or branched-chain alcohols selected from I
to 8 carbon atoms and including methanol, ethanol, propanol, isopropanol, butanol and the like are also suitable for use. Moreover, the "Freon" liquids including trichloromonofluoromethane and dichlorodifluoromethane may be used. Selected ketones, e.g., methyl ethyl ketone, ethers, halohydrocarbons 35 and the like, may be used in some instances. The selected liquid rnay be .
.
~ _9_ :.
used alone or, in some instances, a combination of two or more agents may be used depending on the type of smoking article being produced.
~ The ratio of total water in the mixture to volatile oryanic liquid will depend to some extent on the type and mesh of tobacco and the specific ~;~ 5 liquid being used but generally will be in the range of about 6 parts water to f~.~ I part organic liquid to about 1:1 ratio of each. Where less than -60 mesh tobacco is employed in accordance with the preferred forming practice ', discussed hereinbelow, a ratio of about 2 parts water to I part organic liquid ;,' is preferred.
~: 10 It may also be desirable to add filler materials to the aqueous : tobacco mixture. Filler materials can include calcium carbonate, selected carbon materials, diatornaceous earth, attapulgite and the like. Up 1o about ~, 40 to 50% of the solids in the mixture may comprise such fillers without ~i ~ requiring addition of binders. If desired, burn additives may also be added to the mixture to adjust burn properties.
* While it is preferable to avoid adding an extraneous binder and to rely instead on naturai binder substances of the tobacco, in order to achieve minimum tar delivery upon smoking, it will be recognized that the mechani-cal strength of such smoking articles may be increased through the use of . 20 qdditional binder materials provided that doing so is consistent with the delivery objectives of a particular product.
; When al I the desired ingredients have been added, and an homogeneous-mixture is obtained, the thus prepared mixture is ready for further processing to produce smoking articles. By this further processing, the tobacco mixture is formed into a shaped article comprised of a coherent tobacco mass whose density and porosity are sufficient to occlude gas flow ; therethrough and whose density is sufficient to support combustion of the mass when ignited. The tobacco mass is further provided with at least one ' passage extending therethrough from a first opening on the mass surface to 3û a second opening remote from the first opening. Providing of such passage as used herein means providing the same during the shaping operation or during operations subsequent thereto, or during both shaping and such subsequent operations.
In accordance with the im~ention, the article shaping operation includes pressure treatment of the mixture to transform the mixture into a :, .
!
,, :, . ' ' , '-, '', . ' , ...
. . . ~ ..
,, ':, ' `
,: -10-coherent or self-supporting tobacco mass and subsequent drying of the mass.
The pressure treatment will generally require application of pressure to the tobacco mixture in a confined space und, preferably, results in a coherent mass hQving the desired through passage. An alternate procedure woutd be 5 to form the mass without the passage and to subsequently create the - passage after the pressure treating operation, or after drying, by a material removal operation such as, for example, boring or drilling.
The pressure treatment can be effected by any one of a number of conventional techniques adapted to provide sufficient pressure to the tobacco mixture to cause release of the tobacco material's naturai binding agents, thereby resulting in a cohesive mass. The pressure forming operation thus enables self-supporting articles to be produced without the need to add extraneous binders to the tobacco mixture.
While pressure treatments such as moldin~ can be used lo implement the invention, a preferable treating technique is extrusion. In general, extrusion conditions will depend upon the type of extruder used (ram, screw, etc.), the particular composition of the tobacco mixture and the desired shape, density and porosity conditions for the resultant extru-date.
Conventional screw extruders or higher pressure producing ram extruders may be employed, with the die heads of these extruders preferably having the desired shape of the smoking articles to be produced. These extruders may be operated at selected pressures and with selected cooling of one or more sections of the extruder barrel to promote production of the desired extrudate. An extruder found suitable is a Wayne plastics extruder equipped with a 1:1 screw adapted to rotate at I to 120rpms. Such an extruder, due to its 1:1 screw, does a minimum of work on the tobacco mixture, while providing pressure sufficient to release the natural binding agents of the tobacco and thereby resu!t in a cohesive product. With screw extruders of this type, extrudate pressures at the end of the extruder barrel (i.e., melt pressures) of up to 25ûû psig are useabie, with pressures of up to 120û psig being preferable. Extrudate temperatures at such barrel end (i.e., melt temperatures) of less than about 40C also are useable and can be developed by maintaining the screw barrel temperature in the range of about 20 to 25C.
" ~
-:
Preferable tobacco mixture conditions for extrusion are a - tobacco particle size of below about .30 mesh and a 10bacco content sufficient to produce a mixture having a solids content in the range of about 55 to 75 weight percent solids, and preferably about 60 to 70 percent solids.
As above indicated, the shape of the desired smoking articles controls the extruder die head construction Preferable smoking articles are of hollow cylindrical shape and, more preferably, are cylindrical tubes - having a wall thickness such that the cross-sectional area of lhe mass is less than the corresponding cross-sectional area of the passaae. Die heGds lO having a suitably adapted annular extrusion passage are thus employed to achieve this construction. A particular extruder for realizing hollow cylinders is the aforementioned Wayne extruder. Thus, for example, thin-walled tobacco tubes having a high density and low porosity and which burn with coal temperatures in the range of 585C to 785C may be produced with 15 suitably modified extruders of this type. Additionally, when using such extruders it is customary to introduce air flow into the inner part of the formed tube to prevent collapse thereof.
Forming part of the article pressure trea1ing operation may be a severing or separating operation vhich results in the production of individual , ,, 20 coherent masses corresponding to individual smoking articles. Such an operation is necessary if pressure treatment is not itself on an individual article basis. In the case of the above-described preferred extrusion practice, wherein the extrudate `Nill typically be a single cohesive con-tinuous length mass exiting from the extruder die, it is desirable to perform . 25 a cutting operation at the die exit, thereby to form individual units of length corresponding to that of the desired smoking articles. Where articles of preselected length are desired, the cutting operation is synchronized with the rate of extrudate output to provide the required length.
The aforesaid operation of providing ir1dividual units also may be 30 effected subsequent to the drying of the extrudate if severing of the dried extrudate is found to be a more acceptable practice.
~' Drying the resultant pressure-formed coherent mass may be accomplished either by simple evaporation at ambient environment, e.g., room temperature, or by application of heat. Typically, at a room 35 temperature of from about 7û 1o 75F, typical drying times might range from about 12 to 24 hours. Heat application might be at a temperature of about 100~C. This can be done by conventional heating means such as a Freas oven ~forced air oven) over a period of time from about 15 minutes to I hour. Heating can also be accomplished more rapidly by microwave 5 application in which case the time of application will depend upon the power used. A1 power levels about about 150 watts, drying times of about 2 minutes have been found acceptable. Such rapid drying may be employed to enhance the static burn properties of the resultant smoking article.
Following the drying operation, the dried articles may be further 10 processed as by affixing the articles to suitable mouthpieces which may or may not include filters fo result in the completed smoking article construc-tion.
While the method of the invention as described above has been found to provide suitable smoking articles, a further aspect of the invention 15 is to provide further processing of the pressure-formed coherent mass subseauent to the initial drying operation. Such further processing enables changing of the porosity of the dried mass, whereby improved combustion characteristics of the resultant smoking product result. This further processing comprises rewetting the dried mass and subsequent redrying.
20 Rewetting may be carried out by spraying or immersion of the dried mass.
Suitable rewetting has been carried out by immersing the mass in a bath of liguid, preferably water, for a time sufficient to obtain the desired change in porosity. In general, rewetting conditions will depend upon initial porosity, tobacco particie size and the type of organic fiuid used. Suitable 25 rewetting conditions to realize desired porosity changes can be determined through empirical procedures. Subsequent redrying after the rewetting is preferably carried out in accordance with the initial drying procedure discussed hereinabove.
In a further aspect of the method of the invention, the method is 30 further modified to allow for disposition of a readily ignitable air permeable plug in the through passage of the pressure-formed coherent mass. Other plugs may be placed at one or more positions along the passage and in blocking relation thereto. In a preferred practice of the present invention wherein cylindrical tubular smoking articles are formed, it is desirable to 35 situate such plugs at opposite ends of the tubular passage.
Usually only one or two such plugs will be needed, especially at one end for lighting the smoking article. Consequently, the typical embodiments have a hollow passageway that is laraely unrestricted. It will be appreciated, however, that such passageway may be filled partly or ; 5 wholly with an innocuous filler materiql which either is non-cambustible or does not contribute excessively to the production of tar upon smoking.
Plug rnaterial rnay take various forms and may contain flavor-ants releaseablc upon heating. Plug material preferably comprises com-minuted tobacco prepared in the same manner as the coherent mass forming the smoking article. Plugs can, therefore, be formed using a procedure analogous to that outlined above for making the coherent mass, with pressure treatment modified as may be necessary to produce plugs of the desired configuration and sui1able for insertion in the coherent mass in passage blocking relation. Air permeability for the plugs may be realized IS either through the inherent porosity of the plug material or by through orifices prov-.ded in the plug during or after plug formation.
While plugs might be formed independently of the coherent mass and inserted in the mass subsequent to its formation or subsequent to drying, in a preferred practice the plugs are formed and situated in the mass passage simultaneoùsly or concurrently with mass formation. In yet a f~rrther preferred practice, this is accomplished in the pre~erred extrusion procedure by co-extruding the plug with the mass in suitably timed relationship so as to obtain plugs of desired size at desired passage blocking positions and in intimate contact with the inner mass wall.
~escription of the Preferred Embodiments The srnoking article of the present invention can be made in various forms particularly those which are conveniently extruded, although other article shaping methods can be employed to that end. With reference now to FIGURE 1, the smoking article I0 comprises an elongated coherent mass 9 shaped in this embodiment as a tubular rod having a through passage 2 extending end to end thereof. While the tubular mass 9 serves in and of itself as a smoking article, it is possible tsee FIGURE 2) to fit a filter 3 at the smoking end and join same to the mass 9 with tipping paper 4 in conventional manner. As seen in FIGURE Ib, the passage 2 and the mass 9 have circular configuration but it will be appreciated that other ... . . .
. -: : :' '' , , . : , sectional geometrics could be employed, for example, hexagonal, etc. The mass 9 rnay correspond generally in length and circumference to that of conventional sized cigarette tobacco cylinders. Depending upon the par-ticular delivery characteristics to be produced with the article upon smoking 5 of same, the cross-sectional area of the mass relative to the passage will be varied.
The srnoking article 15 shown in FIGURE 2 is fitted at the ignition end with a passage blocking plug 5 of air permeable combustible material. In addition to functioning as qn ignition device, the plug 5 lO func1ions to prevent flash heating through 1he passage when lighting the smoking article. Additional plugs, for example, the plus 6 shown adjacent the filter component 3 can be provided and may serve to embody flavorant materials in the smoking article. If desired, plugs could also be disposed at one or more locations intermediate the ends of the smoking article to serve 15 as either flavorant carriers or ignition means, or both.
In accordance with the present invention, the smoking article can be provided in the familiar shapes of other types of smoking articles, as for example, in the fashion and approximate dimensions of a cigar 16 as shown in FIGURE 3. In such article 16, the walls 7 of the tubular mass will 2û be of greater thickness relative to the size of the article and as compared with the FIGURE 2 smoking article. In addition to ignition and flavorant :~ plugs 5 and ~, the article can be fitted with a mouthpiece !7, which in turn itself can serve to embody flavor releasing elements or filter means 8.
FIGURES 4 and 5 illustrate the manner of providing a smoking 25 article either for utilization in a conventional smoking pipe or as a pipe shaped component as such. The smoking article 3û shown in FIGURE 4 is formed as a relatively truncated rnass l9 shaped and sized for reception in the bowl of pipe 18, with the mass being provided with one or more through passages 2 extending from top to bottom thereof. FIGURE 5 shows the 30 manner in which a coherent mass 20 is shaped in the form of a smoking pipe bowl and, like the FIGURE 4 mass, has one or more passages 2 and is fitted with a side opening as at 21 for reception of a pipe stem 28 having a filter 40 as does pipe 18.
FIGURE 6 illustrates schematicaily a preferred embodiment of 35 the invention wherein tobacco is comminuted, mixed with water and a J, ~ Y'~
volatile organic liquid and then subjected to a pressure treatment, prefer-ably extrusion, to produce a coherent tobacco mass. The tobacco mass is dried at room temperature or by application of heat. Further processing of the coherent 1obacco mass to alter the porosity thereof is achieved by a S rewettiny step followed by a drying step.
FIGURE 7 shows schematically extrusion e~uipment for provid-ing the aforesaid co-extrusion of a tubular coherent mass and plugs in accordance with the method of the invention, the die head construction being shown in greater detail in FIGURE 8. Turning to FIGURE 7, a tobacco mixture as above-described for forming the coherent mass or body of the smoking article is supplied to an automatic hopper feeder 71. The hopper 71 applies a continuous force to the tobacco mixture via a rotating blade which extends into a material receiving port of a screw extruder 72 driven by a drive 73. The tobacco mixture is force fed to the extruder 72 and the extrudate developed in the extruder is forced into a cornmon die head 74 ; where it is formed into a tubular coherent mass 100 at the die head exit.
Air also is supplied to the die head 74 from a source 75 and is conveyed by a line 76 to the die head exit interiorly of the tubular mass 100 to prevent collapse thereof as the mass is being formed.
; 20 Plug malerial of similar composition to the mass material issupplied to a hopper feeder 81 having a construction analogous to that of hopper feeder 71. The plug material is fed by hopper 81 to a plug screw extruder 82 which is driven by a drive 83. Extrudate passes from the extruder 83 through the valve 84 into the common die head 74 where it is made available interiorly of and joined to the inner wall of the tubular mass lûO.
Control synchronization circuit 91 effects control of the continued pre~sure applied to the pluy extrudate in passing to the head 74.
This control is synchronized with the issuance of the tube 100. Circuit 91 :! 30 maintains the valve 84 closed and the drive 83 stopped for a predetermined period of time corresponding to the delivery of a preselected length of tube.
~fter such time the valve 84 is opened and the drive 83 restarted, causing pressyre to be applied to the plug ex,rudate and, as a result, common -j delivery of plug and tube. This condition lasts for a second predetermined ' 35 period of time corresponding to the common delivery of a preselected length , , : ,, .
`~ of tube and plug, after which the valve is again closed and the drive 83 is agnin stopped. Repeated control of the v~lve 94 and drive 83 thus results in the tube lOû being continuously extruded with plugs 101 of determined ler.gth being disposed at determined space positions therein and in passnge 5 blocking relationship thereto.
Control synchronization circuit 9! also cortrols the direction of rotation of the blades of the hoppers 81 and 71. This direction is changed - periodically by the circuit 91 to ensure proper delivery of tobacco mixture to the respective screw extruders.
Also shown in FIGURE 7 is a cutting assembly 92 at the die head exit which also is synchronously opera,ed by the control circuit 91 to cut the tube lOû into individucll coherent mass units. Such cutting operation can be synchronized to occur immediately before disposition of a plug 101, whereby each unit will contain a single plug at the forward passage thereof.
15 Preferably, however, the- cutting assembly is controlled to effect cutting sothat units are produced having plugs at both ends. This is realized by controlling the plug extruder operation 10 issue plug material of desired length and by correspondingly controlling the cutting assembly to sever the tube 100 at positions along the length of each extruded plug.
FIGURE 8 illustrates the common die head 74 of FIGURE 7 in greater detail. As illustrated die head 74 includes an outer casing or support assembly 110 comprised of a central hollow cylindrical body 111 to whose opposite ends are attached by screws (not shown) support rings 112 and 113.
A central recessed section 114 of the body 111 cooperates with a facing central recessed section 115 of the ring 112 to suppor1 a first holiow mandrel 116. Inner conical surface 117 of mandrel 116 extends to a short cylindricol guide surface 118, the latter surface l 18 terminating at the end of ring 112 to define an exit orifice 119.
J A further hollow mandrel 121 is supported by ring 113 and by a hollow retainer element 122 held between the latter ring and body I 11. The mandrel 121 extends the length of the assembly 110 and the mandrel outer surface 123 is spaced from the respective inner surfaces 128 and 117 of body 111 ar;ri mandrel 116. These surfaces (123, 128, 117) define an annular passage 124 for receipt of the tubular mass extrudate from the extruder 73.
Surface 1 Z3 is topered inw~rdly in the region of the surfoce 117, both " "
; - surfaces cooperatir,g to provide an exit annular passage 125 of radial i~- expanse corresponding to the thickness of the tubular mass to be formed and of outer diameter commensurate with the guide surface 118.
A central bore 126 extends the length of mandrel 121 and f 5 receives plug extrudate from the extruder 82. Bore 126 at the end of 4,~ mandrel 121 is of expanse substantially equal to that of the inner diameter of the exit passage 125, whereby plug extrudate of such expanse is delivered to the end of the exit passage. Air line 76 passes throuah the bore 126 and delivers air to the region adjacent the passage 125 and the exit port 119 to prevent collapse of the tube lûû as it is being extruded.
In operation, pressure applied to the tubular mass extrudate via the extruder 73 forces the extrudate into the passage 124 and thence to the exit annular passage 125. The extrudate departs the passage 125 as the thin walled tubular coherent mass lûû, the latter mass being guided by cylin-drical surface 118 to exit port 119. With no pressure applied to the plug extrudate by the extruder 82, the lubular mass lOû exits without plug material and passes through a constriction ring 127 attached to the ' mandrel 116.
Upon pressure being applied to the plug extrudate by the extruder 82, the extrudate is forced through the central bore 126 ancl supplied to the end of the annular passage 125 where it is received inleriorly of and in contact with the inner wall of the simultaneously formed tubular mass 100. As pressure continues to be applied to the plug extrudate, the plug extrudate and the tubular mass together pass through exit port 119 into the central orifice 129 of the rina 127. The latter orifice tapers inwardly and thereafter outwardly, the inward taper ending at a radial expanse which is less than the outer diameter of the tubular mass. Upon reaching the end of the inward taper, the forward end of the tubular mass is inwardly constricted forcing its wall into cohesiye engagement v~/ith the forward end 3û of the plug extrudate. At this time, the pressure applied to the plug extruda1e terminates, and the tubular mass which continues to be extruded and is now joined to the plug extrudate breaks from the plug extrudate a plug lûl which continues to move with the tube through the orifice 129.
The portion of the tube coextensive with the plug is thereupon continuously 3~ constricted over further incremental areas, thereby cohesively joining the "
" . .
'.
` plug to the fube wall over the entire plug length. In this way the tube and plug are joined without excessive drag being placed on the tubular mass, - whereby thickening of the tube wall is prevented during the joining operat ion.
S It should be noted that cohesive joining of the plug 101 and the tubular mass 100 can be effected in other ways such as, for example, by expanding the plug by known methods so it cohesively joins to the mass wall.
As noted above, air-permeability of the plugs 101 call be brougl,t about in the plug forming operation and it is contemplated that the die head 10 of FIGURE 8 can be modified to provide through orifices in the plugs as they are being extruded. This can be accomplished by the placement of spaced thin solid rods 131 in the bore 126, such rods extending from a point in the bore to beyond the annular passage 125 These rods might be held by a ring 133 which can be placed between sections of the mandrel 121, thereby 15 placing the rods in their desired position in the bore 1~6.
Density of the rods formed in the hereinbelow examples was determined according to the following formula:
Density (g/cc) = n x [~02D~ ~ ¦l2D~ ] X rrOOd Ween;q9thht 20 wherein OD is the outer diameter of the rod in centimeters, ID is the inner diameter of the rod in centimeters and the length and weight of the rod are in centimeters and grams respectively.
Pressure drop (aP) was measured by blocking an open extruded tube at one end while inserting the other end in a pressure drop instrument 25 (P.D.I.). The ~P recorded is inversely proportional to the air flow through i the walls of the tube.
The following examples are illustrative of the invention.
Example I
Bright tobacco having an approximate moisture content of 30 11.6% OV was ground in a Fritsch-Pulverisette grinder. The ground tobacco was passed through a 6û-mesh screen to remove coarse particles and the fraction having a sieve size of 6û or smaller (-60 mesh) was selected for i fur ~her processing.
J
i - ' r --19-To 22~9 9 of the -60 mesh tobacco having a moisture content of 11.06% OV, was added 48.0 ml of 95% ethanol and 47.1 9 water. This mixture was stirred for approximately 20 minutes in a Hobart mixer (Model N-SQ) equipped with a conventional "B"-flat beater blade.
The tobacco mixture having a solids content of 64.5% by weight was then extruded to form tubes having a wall thickness of û.5 mm. A
Wayne Plastics 1" extruder with 1:1 compression ratio screw, 3 zone automatic heat, and 3 zone automatic fan cooling, straight tubing die having an 8 mm outer diameter (OD) and 7 mm inner diameter (ID) and 3 HP
lû variable speed ~û to 60 rpm) drive was employed ta effect extrusion. Zones I through 3 were maintained at room temperature. The maximum die head pressure was 1500 psig. Although these extrusion conditions were favorable for smal I runs, for longer, continuous runs it was necessary to cool the barrel to preven7 skin formation on the rod.
Some of the extruded tobacco tubes were dried in an Apollo l~llicrowave oven for S minutes at maximum power. After drying, the tubes were ignited and maintained a static burn.
Extruded tubes were also allowed to dry at room tempera1ure overnight. These tubes were then cut into 85 mm lengths having an average measured weight of 12.70 mg/mm and a calculated density of 1.078 g/cc.
Four of these tubes were allowed to static burn, and the averaae burn time was determined and found to be 4.8 mm/minute. Other room temperature dried tubes were smoked automatically under controlled laboratory condi-tions. TPM and tar delivery were measured using standard analytical techniqves of the tobacco industry. l he average TPM/puff was û.35 rng and the average tar/puff was 0.28 mg.
Example 2 677.7 g of bright tobacco (-60 mesh~ 17avir,g a moisture content of 1 1.56% OV was combined with 144 ml 95% ethanol and 138 9 water. The mixture was stirred in a Hobart mixer for 30 minutes, covered and left at ambient temperature for l.S hours. The percent solids prior to extrusion was 65.82~.
lhe equipment and conditions for extrusion were the same as i those of Example 1. The die pressure during the collection of samples was 35 approxima~el~ 500 psig, and ?he maximum melt temperature ot 1he extru-~ . ~
date at the die head was 110F. The extruded tubes had an outer diameter of 8 mm ar-ld an inner diqmeter of 7 mm and a wall thickness of 0.5 mm.
The tubes were allowed to dry overnight at room temperature.
Representative samples were cut to 85 mm lengths, having an average weight of 12.64 mg/mm. The calculated density was 1.073 g/cc. The static , burn was determined as in Example I and found to be 3.52 mm/min. TPM
and tar delivery/puff, also determined as in Example 1, were found to be 0.26 mg and 0.16 mg respectively.
- In addition, the smoke from the third puff of four tobacco tubes was collected and their gas phase constituents measured using conventional ~as chromatography techniques. The qverage gas concentrations of the third puff of the four samples was as follows:
2 - 9.61 mg/tube third puff CO - 0.07 mg/tube third puff C2 - 1.11 mg/tube third puff Finally, average pressure drop (~P) of five representative 85 mm tubes was found to be 1.56 inches of H2O.
Example 3 564.7 g bright tobacco (-60 mesh) having a moisture content of 11.5% OV was combined with 120 ml of 95% ethanol and 115.3 9 water in the same manner as described in Example 2. The mixture was stirred for 25 minutes and thereafter was allowed to stand covered overnight. Prior to extrusion, the mixture had a solids content of 65.05%.
The die of the extruder was modified to extrude a tobacco tube having an outer diameter of 8 mm and an inner diameter of 5 mm.
Employing the equipment of Example 1, the extrusion conditions were as fol lows:
,j .i -2 1 -Extrusion Conditions __ . . . _ . .
:.. PSIG Head _ Ss~ Time Pressure h'lelt rF
.... ___ .. _ .___ 0 minutes 0 75 5 minutes 550 85 10 minutes 450 98 - 15 minutes 375 105 20 minutes 375 106 25 minutes 375 109 30 minutes 375 I 10 - 34 minutes 350 ,' _ The extruded tubes were dried overnight at room temperature.
Representative examples of tubes extruded between the time interval of 6 to 10 minutes were coded A and additional tubes extruded between approxi-15 mately 23 and 28 minutes were coded B.
: Representative tobacco tubes were analyzed and the results are tabulated in Table I below.
' ,: .
,,~
. ~
: .
t ,, ' . .
-: -22~
E ~ ICL o o E Q ~ o o --I E = ~ _ o I CL E o u~
U ~. o, o.
E ~ ~ ~ ~
_ 'i - ~ E ~
Example 4 443.21 9 burley tobacco (-60 mesh) having a moisture content of 9.75% OV was stirred in a Hobart mixer with 96 ml of 95% ethanol and 100.8 9 water for approximately 25 minutes. The mixture had a solids content of 64.5% prior to extrusion.
Burley tobacco tubes having an outer diameter of 8 mm and an inner diameter of 6.5 mm were extruded using the Wayne plastics extruder perviously described and under the same conditions as in Example 2 with the exception that the gearing on the extruder was changed fo increase the range of rotation of the screw from 0 to 120 rpm. During extrusion at 120 rpm, the maximum head pressure was 25ûû psig and the maximum melt temperature was 151F. Tobacco tubes were successfully extruded. See also Example 11.
Example 5 440.8 9 of Oriental tobacco (-60 mesh) having a moisture content of 9.25% OV was combined with 96 ml 95% ethanol and lû3.2 y water. The mixture was stirred for 25 minutes and extruded using the same extrusion conditions and equipment as in Example 4. The maximum head pressure was 600 to 70û psig and maximum melt temperature was 110F. The tobacco tubes exiting the extruder die were found to be slightly sticky and were more flexible than either bright or burley tobaccos. With rea~ard to static burn, see Example 11.
' Example 6 A blended tobacco tube was prepared using the fallowing ingre-dients: 220.1 y bright tobacco at 9.12%0V, llû.8g ~urley tobacco at 9.75% OV, 110.8 9 Oriental tobacco at 9.25% OV, 96.0 ml 95% etllanol and 102.û g water. All starting tobacco materials were -6û mesh.
The dry tobacco materials.were blended in .he Hobart mixer and the alcohol and water were added. After 25 minutes of mixiny, the material was extruded as previously described in Example 4. The maximum head pressure was 95û psig and the maximum melt temperature was 112E.
The blended extruded tobacco tubes exiting the die appeared to . be more flexible than a tube of all bright tobacco tube but less flexible than o tube of al burley or all OrientQI tobrcco.
-2~--: Example 7 An all bright iobacco tube. was extruded using the same procedure and die as in Example 4. The ingredients employed were 440.1 9 bright tobacco (-60 mesh) at 9.12% OV, 96.0 ml 95% ethanol and 103.9 9 5 water.
During extrusion, the maximum head pressure reached 1400 psig and the maximum melt temperature was 116F.
ExnmrJle ~
The following tobacco constituents were blended in a Hobart 10 mixer:
220.1 g bright tobacco (-60 mesh) at 9.12% OV
110.8 g burley tobacco (-60 mesh) at 9.75,~ OV
110.2 g Oriental tobacco (-6û mesh) at 9.25% OV
To the tobacco mixture was added in an alternating manner 15 102.9 g water and 26.0ml of a cigarette flavorant solution in 70 ml of e~hanol After all the solutions were added, the total mixture was stirred for an additional 25 minutes.
The tobacco rnixture having a total solids content of 64.5% was then extruded using the Wayne Plastics 1" extruder. Zones I through 3 there 20 maintained at room temperature during extrusion. The maximum head pressure v~as 95û psig and the maximum melt temperature was 127F. The extruded tubes, having an outer diameter of 8 mm and an inner diameter of 6.5 mm, appeared to be very pliable as they exited the die. See also Example 11, especially Table 3.
Example 9 In a manner similar to Example 8, the following ingredients were combined and mixed in a Hobart mixer:
22~1.1 9 bright tobacco (-6û mesh) at 9.12% OV
110.8 g burley tobacco (-60 mesh) at 9.75% OV
110.2 g Oriental tobacco (-6û mesh) at 9.25% OV
10.0 9 mixed sugar solution 96.0 ml 95,~ ethanol 92.9 9 water The water and ethanol were mixed and added to the tobacco 35 materials in an alternating manner with the sugar solution. Mixing ,, .
', " ~
continued for 25 minutes after all ingredients were added. The percent solids was 64.5%
Tobacco tubes were extruded in the same manner as that of Example 8. During extrusion, the maximum head pressure was 90û psig and the maximum melt temperature was 126F.
The extruded tubes were dried in an oven at 10ûC overnight.
Sample tubes lighted immediately after rernoval from the oven would maintain a static burn. Tubes which had been dried in the oven and then equilibrated in ambient air at room temperature would also static burn, - lû although some tended to go out cnd required relighting.
Example 1() The following ingredients were combined and mixed in a Hobart mixer:
286. 1 y bright tobacco (-60 mesh) at 9.12% OV
110.8 9 burley tobacco (-6û mesh) at 9.75% ~V
44.1 9 Oriental tobacco (-60 mesh) at 9.25% OV
'~ 10.û 9 mixed sugar solution 13.0 ml flavorant solution (humectant and flavorants) 92.2 ml 95% ethanol 106 .4 y water The materials we!e blended for approximately 25 minutes following addition of all ingredients. The percent solids was 64.5%.
Extrusion of tobacco tubes having an 8 mm outer diameter and 6.5 mm inner diameter was conducted under the cond;tions described in Example 8. The 25 maximum head pressure noted was 700 psiy and the maximum melt tempera-ture was 1 26F.
Selected representative tubes were dried overnight in an oven at 100''C. The d. ied tubes successfully burned. Tubes that had been dried and equilibrated at ambient room temperature would also static burn. It was 30 noted on burning that a distinctive cigar aroma was produced by the tobacco tube.
Example I I
Representative extruded tubes from Examples 4 through 7 were dried in an oven at 1 0ûC overnight. One-half of the tubes were lit 35 immediately after removal from the oven to determine whether a static vj burn could be rnaintained. The remaining half were equilibrated in ambient air at room temperature overnight and then tested for static burn. The results are set forth in Table 2.
Table 2 _ 5Exomple Dried Dried and Equilibrated _ 4 Burned Burned No Static Burn No Static Burn 6 Burned Burned 7 Burned Burned , _ lû As to the second item in Table 2, however, when the extruded tubes of Exmple 5 (and a comparison specimen from Example 8) were - subjected to the water treatment described below, it was found thatsubstantially improved combustion properties were obtained.
Extruded tubes were cut to a 1ength of lOû mm and were then 15 submerged in water so that a length of 50 mm per tube became wet. The tubes were dtied in a microwave oven and conventional cellulose acetate filters were attached to the untreated end of each tube. The static burn rate and length of tube which burned were determined. The results are tabulated below in Table 3.
Table 3 .
Time Submerged Static Burn Sample Seconds Rate Length Burned Example 5 30 no burn __ Example 5 45 no burn __ 25Example 5 6û û.75 10 mm Example 5 90 1.81 50 mm Examplc 8 30 2.58 50 mm Example 13 433.1 9 of bright tobacco (-oO rn2sh) having 7.46% OV was 30 combined with 96 9 of 95% methanol and 11().9 9 water. The material was mixed in a Hobrrt mixer for 25 minutes rt room tempc~rture.
. , , ' ':
.
The tobacco mixture, having approximately 62.5"/1) solids, was extruded using a Wayne plastic extrud~r equipped with an 8 mm outer diameter and 7 mm inner diameter tubing die. Extrusion conditions were same as those employed in Example 4. The pressure in the extruder 5 increased to 1,20û psi as the first tubes were collected and when the extrusion was terminated 17 minutes later, the pressure was recorded at I ,ûûO ps i .
The hollow, extruded tubes were dried overnight at room tem-perature. The outer walls of the tubes appeared to be very smooth and 10 dense. Attempts to static burn the tubes were unsuccessful.
,f, Extruded tubes, I ûû mm in length, prepared as above were immersed in water to a depth of Sû mm for varying periods of time. The tubes were thereupon dried in a microwave oven for 2 minutes. The pressure drop of each tube was determined prior to and after water 15 treatment and redrying; The results are shown in Table 4. See also Example 19.
Table 4 ., Pressure [)rop - Inches of H O
Time Submerged 2 Seconds - ~ef~re After 60.99 60.54 60.5û 57.71 60.62 52.07 60.57 16.48 60.71 10.21 ,~ ' 25 30 60.05 5.70 ,, The results indicate that rewetting and redrying signif icantly modify the tube wall thereby decreasing the pressure drop.
F~ample 14 In a rnanner similar to Example 13, the following materials were 30 combined and mixed in the Hobart mixer to form a mixture having 62.5%
solids which was extruded using the Wayne plastics extruder:
, .
324.8 9 bright tobacco (-60 mesh) at 7.65% VV
72.0 9 95% n-propyl alcohol 83 . 2 g water The initial material that exited the extruder appeared to be 5 quite dry. Extrusion continued for approximately 15 minutes; production of tubiny was s!ower than normally observed. The extruded hollow tubes were dried overnight at room temperature. The tubes, when ignited, would static burn.
Example 15 In a manner similar to Example 13, the following ingredients were combined and mixed to form a mixture having 62.5% solids which WQS
extruded using the Wayne plastics extruder:
- 324.8 g bright tobacco (-60 mesh) at 7.64% OV
72.0 g 95% isopropyl alcohol 83.0 gwater The pressure in the extruder rose to 1,300 psi during extrusion.
The extruded hollow tubes had good mechanical properties. After drying overnight at room temperature, the tubes were tested for static burn. The tubes would not maintain static burn under normal testing conditions.
However, see Example 19 with regard to subsequent treatmen~.
ExQmple 16 In a manner siMilar to Example 13, the following materials were combined, mixed 25 minutes and then extruded:
324.8 9 bright tobacco (-60 mesh) at 7.64% ()V
72.0 g 95% tert-butyl alcohol 83 . 2 9 water i~ During extrusion the pressure varied between I lûû and 1475 psig.
The hollow tubes extruded appeared to have poor mechanical properties when wet. The solvent tended to evaporate rapidly on exiting the die and the tubes turned lighter in color as the solvent evaporated. After drying overnight, the extruded tubes were tested for static burn. After burning for approximately 2 minutes, the tube went out. However, see Example 19 with regard to subsequent treatment.
,' .
' ' ~, ' ' ~ I 1~"' . . .
iS~
.
: Example 17 . , f Usina~ the procedure of Examr)le 13, the following rnaterials were combined and mixed to form a 62.5% solid mi~ture which was extruded:
324.8 g bright tobacco (-60 mesh) at 7.64% OV
72.0 9 95% methylene chloride 83. 2 9 water During extrusion the pressure rose to about 1,500 psi. The mechanical properties of the extruded hollow tubes were excellent. The tubes exhibited a high degree of plasticity and could be stretched without lû rupturil-g. I engths greater tllan I meter could be extruded successfully.
The dried tubes would not maintain static burn. However, see Example 19 - with regard to subsequent treatment.
Examp!e 1~
- Using the procedure of Example 13, the following materials were combined and mixed to- form a mixture having 62.5% solids which was extruded:
332.2 g bright tobacco (-60 mesh) at 9.7% OV
34.2 9 methylene chloride 36 . 0 g ethanol 77 . 0 g water On extrusion, the tubes exhibited some plasticity; however, it was not as great as observed when rnethylene chloride was used as the major solvent. Static burn was achieved by subsequent treatment as noted in the following example.
Example 19 ., Representative tubes prepared in Examples 13, 15, 16, 17 and 18 were cut to a length of 10û mm. The tubes were immersed in water for 30seconds in such c manner that exactly 50 mm of each tube came in contact with the water. The tubes were dried for 2 minutes in CEM
30 Corporation Model AVC-MP microwave oven at maximum power. Conven-tional cellulose acetate filters were attached to the untreated end of each tube after drying. The tubes were secured by the filter end and the water treated end was ignited. The static burn rate was based on the time required to burn the 50 mm water treated portion of the tube. The results 35 are tabulated below in Table 5.
. .
"
.. . .. .
!
- . ~ -.~ , , Table 5 .
_ ~ _ . -- _ Static Burn Rate -- Example Solvent and Tobacco mmlmin.
13 Methyl Alcohol 1.85 Isopropyl Alcohol 3.64 16 Tert-Butyl Alcohol 2.13 17 Methylene Chloride 0.68 18 Methylene Chlorid.e-Ethanol 2.42 _ 'The tube immersed for 30 seconds would not static burn. After immersion for 45 seconds, the tube burned for 8 minutes 5 seconds and wenf out. After ~, relighting the tube burned for an additional 6 minutes 35 seconds. Total length burned was 10 mm.
The results indicate that when dried extruded tobacco tubes are 15 subjected to a water treatment, the tube wall is modified in such a manner that combustion properties of the tube are improved.
, Examp!e 20 The following ingredients were combined and mixed in a Hobart , i mixer for approximately 25 minutes:
154.05 9 bright tobacco (-60 mesh) at 9.15% OV
61.53 9 PCB* carbon (-40 +60 mesh) at 2.48% OV
~ 48.0 ml 95% ethanol 56.4 9 water , *PCB = Pittsburgh' Coal Carbon -40 +60 mesh , 1 25 The tobacco-carbon mixture having 64.5% solids was dark but appeared to have the same consistency as previous mixtures used.
Using extrusion conditions from Example 8, tobacco-carbon ' I tubes were produced wherein the outer diameter was 8 mm and the inner diameter was 6.5 mm. During extrusion the maximum head pressure was 30 2000 psig and the maximum melt temperature was 106F.
",1 After drying overnight, the tobacco-carbon tubes would maintain ,j a static burn.
~" Example 21 ' I Tobacco-carbon tubes wherein carbon represent'ed approximately s 35 40% of the to~al solids in the formulation were prepared using ~he following , ingredients:
', "
,, , ' : ~
r~
206.7 9 bright tobacco (-60 mesh) at 9.12% OV
130 . 3 g PCB carbon (-60 + 140 mesh) 75.1 ml 95% ethanol 88.7 9 water (64.5% solids) Tobacco-carbon tubes were extruded wherein the outer diameter . was 8 mm and the inner diameter was 5 mm. The Wayne plastics extruder was modified to include a low restriction spider to improve fiow properties.
The extruder conditions were as follows:
Zone I - 100F
I û Zone 2 - I 50F
Zone 3 - 200F
Die - 250F
Screw speed 120 rpm During extrusion the head pressure built up to about 600 psig cmd this was fol lowed by rapid extrusion of hibe product. As the pressure dropped, tube production ceased; however, with pressure build up, product was again cxtruded.
Samples of extruded tubes were dried overnight and tested for static burn. ~11 samples maintained a static burn.
Examp!e 22 The following ingredients were combined and mixed in a Hobart mixer:
154.û 9 bright tobacco (-60 mesh) at 9.12% OV
60.0 9 calcium carbonate at O.û6% OV (-5û mesh) 48.û ml 95% ethanol 57.9 g water (64.5% solids) After mixing for 25 minutes, tobacco tubes were extruded using the conditions described in Example 8. The maximum head pressure reached lOûO psig during extrusion. The extruded tubes appeared to have a diameter slightly larger than 8 mm. This may be due to expansion caused by the carbonate salt.
, Example 23 ; Bright tobaccoj 222.3 9, -60 mesh at lû.û9% OV, was combined with 84.8 9 of water and mixed in a Hobart mixer for I hour and 20 minutes.
.' I .
, ,~ .
. ' ~
, - .
L~
, Fifty g of ammonium carbonate at 20% OV was added and the mixture was stirred for lû minutes.
The material was extruded using the Wayne plastic extruder under the following conditions:
~one I - 30C
Zone 2 - 50~C
Zone 3 - 70~C
Vie - lû0~C
Feed cooling water on Straight tubing die (8 mm outer diameter, 7 mm inner diameter) No die head pressure was observed; the die temperature was reduced to 90C during extrusion.
c A representative example of the extruded tubesS cut to a 85 mm ; 15 length, was equilibrated overnight to 60RH in a humidity cabinet. On ignition wi1h a gas flame, the hollow tube maintained a $tatic burn for over 6 minutes. A 2û mm section of the tubc had a burn rate of ; 0.185 mm/second.
E)comple 24 2û0.2 9 bright tobacco (-40 +60 mesh) at lû.0% OV and iSû.0 g tobacco slurry containing diammonium phosphate and having 18.0% solids v content ~the slurry being of a type prepared according to U.S. Patent
Example 3 564.7 g bright tobacco (-60 mesh) having a moisture content of 11.5% OV was combined with 120 ml of 95% ethanol and 115.3 9 water in the same manner as described in Example 2. The mixture was stirred for 25 minutes and thereafter was allowed to stand covered overnight. Prior to extrusion, the mixture had a solids content of 65.05%.
The die of the extruder was modified to extrude a tobacco tube having an outer diameter of 8 mm and an inner diameter of 5 mm.
Employing the equipment of Example 1, the extrusion conditions were as fol lows:
,j .i -2 1 -Extrusion Conditions __ . . . _ . .
:.. PSIG Head _ Ss~ Time Pressure h'lelt rF
.... ___ .. _ .___ 0 minutes 0 75 5 minutes 550 85 10 minutes 450 98 - 15 minutes 375 105 20 minutes 375 106 25 minutes 375 109 30 minutes 375 I 10 - 34 minutes 350 ,' _ The extruded tubes were dried overnight at room temperature.
Representative examples of tubes extruded between the time interval of 6 to 10 minutes were coded A and additional tubes extruded between approxi-15 mately 23 and 28 minutes were coded B.
: Representative tobacco tubes were analyzed and the results are tabulated in Table I below.
' ,: .
,,~
. ~
: .
t ,, ' . .
-: -22~
E ~ ICL o o E Q ~ o o --I E = ~ _ o I CL E o u~
U ~. o, o.
E ~ ~ ~ ~
_ 'i - ~ E ~
Example 4 443.21 9 burley tobacco (-60 mesh) having a moisture content of 9.75% OV was stirred in a Hobart mixer with 96 ml of 95% ethanol and 100.8 9 water for approximately 25 minutes. The mixture had a solids content of 64.5% prior to extrusion.
Burley tobacco tubes having an outer diameter of 8 mm and an inner diameter of 6.5 mm were extruded using the Wayne plastics extruder perviously described and under the same conditions as in Example 2 with the exception that the gearing on the extruder was changed fo increase the range of rotation of the screw from 0 to 120 rpm. During extrusion at 120 rpm, the maximum head pressure was 25ûû psig and the maximum melt temperature was 151F. Tobacco tubes were successfully extruded. See also Example 11.
Example 5 440.8 9 of Oriental tobacco (-60 mesh) having a moisture content of 9.25% OV was combined with 96 ml 95% ethanol and lû3.2 y water. The mixture was stirred for 25 minutes and extruded using the same extrusion conditions and equipment as in Example 4. The maximum head pressure was 600 to 70û psig and maximum melt temperature was 110F. The tobacco tubes exiting the extruder die were found to be slightly sticky and were more flexible than either bright or burley tobaccos. With rea~ard to static burn, see Example 11.
' Example 6 A blended tobacco tube was prepared using the fallowing ingre-dients: 220.1 y bright tobacco at 9.12%0V, llû.8g ~urley tobacco at 9.75% OV, 110.8 9 Oriental tobacco at 9.25% OV, 96.0 ml 95% etllanol and 102.û g water. All starting tobacco materials were -6û mesh.
The dry tobacco materials.were blended in .he Hobart mixer and the alcohol and water were added. After 25 minutes of mixiny, the material was extruded as previously described in Example 4. The maximum head pressure was 95û psig and the maximum melt temperature was 112E.
The blended extruded tobacco tubes exiting the die appeared to . be more flexible than a tube of all bright tobacco tube but less flexible than o tube of al burley or all OrientQI tobrcco.
-2~--: Example 7 An all bright iobacco tube. was extruded using the same procedure and die as in Example 4. The ingredients employed were 440.1 9 bright tobacco (-60 mesh) at 9.12% OV, 96.0 ml 95% ethanol and 103.9 9 5 water.
During extrusion, the maximum head pressure reached 1400 psig and the maximum melt temperature was 116F.
ExnmrJle ~
The following tobacco constituents were blended in a Hobart 10 mixer:
220.1 g bright tobacco (-60 mesh) at 9.12% OV
110.8 g burley tobacco (-60 mesh) at 9.75,~ OV
110.2 g Oriental tobacco (-6û mesh) at 9.25% OV
To the tobacco mixture was added in an alternating manner 15 102.9 g water and 26.0ml of a cigarette flavorant solution in 70 ml of e~hanol After all the solutions were added, the total mixture was stirred for an additional 25 minutes.
The tobacco rnixture having a total solids content of 64.5% was then extruded using the Wayne Plastics 1" extruder. Zones I through 3 there 20 maintained at room temperature during extrusion. The maximum head pressure v~as 95û psig and the maximum melt temperature was 127F. The extruded tubes, having an outer diameter of 8 mm and an inner diameter of 6.5 mm, appeared to be very pliable as they exited the die. See also Example 11, especially Table 3.
Example 9 In a manner similar to Example 8, the following ingredients were combined and mixed in a Hobart mixer:
22~1.1 9 bright tobacco (-6û mesh) at 9.12% OV
110.8 g burley tobacco (-60 mesh) at 9.75% OV
110.2 g Oriental tobacco (-6û mesh) at 9.25% OV
10.0 9 mixed sugar solution 96.0 ml 95,~ ethanol 92.9 9 water The water and ethanol were mixed and added to the tobacco 35 materials in an alternating manner with the sugar solution. Mixing ,, .
', " ~
continued for 25 minutes after all ingredients were added. The percent solids was 64.5%
Tobacco tubes were extruded in the same manner as that of Example 8. During extrusion, the maximum head pressure was 90û psig and the maximum melt temperature was 126F.
The extruded tubes were dried in an oven at 10ûC overnight.
Sample tubes lighted immediately after rernoval from the oven would maintain a static burn. Tubes which had been dried in the oven and then equilibrated in ambient air at room temperature would also static burn, - lû although some tended to go out cnd required relighting.
Example 1() The following ingredients were combined and mixed in a Hobart mixer:
286. 1 y bright tobacco (-60 mesh) at 9.12% OV
110.8 9 burley tobacco (-6û mesh) at 9.75% ~V
44.1 9 Oriental tobacco (-60 mesh) at 9.25% OV
'~ 10.û 9 mixed sugar solution 13.0 ml flavorant solution (humectant and flavorants) 92.2 ml 95% ethanol 106 .4 y water The materials we!e blended for approximately 25 minutes following addition of all ingredients. The percent solids was 64.5%.
Extrusion of tobacco tubes having an 8 mm outer diameter and 6.5 mm inner diameter was conducted under the cond;tions described in Example 8. The 25 maximum head pressure noted was 700 psiy and the maximum melt tempera-ture was 1 26F.
Selected representative tubes were dried overnight in an oven at 100''C. The d. ied tubes successfully burned. Tubes that had been dried and equilibrated at ambient room temperature would also static burn. It was 30 noted on burning that a distinctive cigar aroma was produced by the tobacco tube.
Example I I
Representative extruded tubes from Examples 4 through 7 were dried in an oven at 1 0ûC overnight. One-half of the tubes were lit 35 immediately after removal from the oven to determine whether a static vj burn could be rnaintained. The remaining half were equilibrated in ambient air at room temperature overnight and then tested for static burn. The results are set forth in Table 2.
Table 2 _ 5Exomple Dried Dried and Equilibrated _ 4 Burned Burned No Static Burn No Static Burn 6 Burned Burned 7 Burned Burned , _ lû As to the second item in Table 2, however, when the extruded tubes of Exmple 5 (and a comparison specimen from Example 8) were - subjected to the water treatment described below, it was found thatsubstantially improved combustion properties were obtained.
Extruded tubes were cut to a 1ength of lOû mm and were then 15 submerged in water so that a length of 50 mm per tube became wet. The tubes were dtied in a microwave oven and conventional cellulose acetate filters were attached to the untreated end of each tube. The static burn rate and length of tube which burned were determined. The results are tabulated below in Table 3.
Table 3 .
Time Submerged Static Burn Sample Seconds Rate Length Burned Example 5 30 no burn __ Example 5 45 no burn __ 25Example 5 6û û.75 10 mm Example 5 90 1.81 50 mm Examplc 8 30 2.58 50 mm Example 13 433.1 9 of bright tobacco (-oO rn2sh) having 7.46% OV was 30 combined with 96 9 of 95% methanol and 11().9 9 water. The material was mixed in a Hobrrt mixer for 25 minutes rt room tempc~rture.
. , , ' ':
.
The tobacco mixture, having approximately 62.5"/1) solids, was extruded using a Wayne plastic extrud~r equipped with an 8 mm outer diameter and 7 mm inner diameter tubing die. Extrusion conditions were same as those employed in Example 4. The pressure in the extruder 5 increased to 1,20û psi as the first tubes were collected and when the extrusion was terminated 17 minutes later, the pressure was recorded at I ,ûûO ps i .
The hollow, extruded tubes were dried overnight at room tem-perature. The outer walls of the tubes appeared to be very smooth and 10 dense. Attempts to static burn the tubes were unsuccessful.
,f, Extruded tubes, I ûû mm in length, prepared as above were immersed in water to a depth of Sû mm for varying periods of time. The tubes were thereupon dried in a microwave oven for 2 minutes. The pressure drop of each tube was determined prior to and after water 15 treatment and redrying; The results are shown in Table 4. See also Example 19.
Table 4 ., Pressure [)rop - Inches of H O
Time Submerged 2 Seconds - ~ef~re After 60.99 60.54 60.5û 57.71 60.62 52.07 60.57 16.48 60.71 10.21 ,~ ' 25 30 60.05 5.70 ,, The results indicate that rewetting and redrying signif icantly modify the tube wall thereby decreasing the pressure drop.
F~ample 14 In a rnanner similar to Example 13, the following materials were 30 combined and mixed in the Hobart mixer to form a mixture having 62.5%
solids which was extruded using the Wayne plastics extruder:
, .
324.8 9 bright tobacco (-60 mesh) at 7.65% VV
72.0 9 95% n-propyl alcohol 83 . 2 g water The initial material that exited the extruder appeared to be 5 quite dry. Extrusion continued for approximately 15 minutes; production of tubiny was s!ower than normally observed. The extruded hollow tubes were dried overnight at room temperature. The tubes, when ignited, would static burn.
Example 15 In a manner similar to Example 13, the following ingredients were combined and mixed to form a mixture having 62.5% solids which WQS
extruded using the Wayne plastics extruder:
- 324.8 g bright tobacco (-60 mesh) at 7.64% OV
72.0 g 95% isopropyl alcohol 83.0 gwater The pressure in the extruder rose to 1,300 psi during extrusion.
The extruded hollow tubes had good mechanical properties. After drying overnight at room temperature, the tubes were tested for static burn. The tubes would not maintain static burn under normal testing conditions.
However, see Example 19 with regard to subsequent treatmen~.
ExQmple 16 In a manner siMilar to Example 13, the following materials were combined, mixed 25 minutes and then extruded:
324.8 9 bright tobacco (-60 mesh) at 7.64% ()V
72.0 g 95% tert-butyl alcohol 83 . 2 9 water i~ During extrusion the pressure varied between I lûû and 1475 psig.
The hollow tubes extruded appeared to have poor mechanical properties when wet. The solvent tended to evaporate rapidly on exiting the die and the tubes turned lighter in color as the solvent evaporated. After drying overnight, the extruded tubes were tested for static burn. After burning for approximately 2 minutes, the tube went out. However, see Example 19 with regard to subsequent treatment.
,' .
' ' ~, ' ' ~ I 1~"' . . .
iS~
.
: Example 17 . , f Usina~ the procedure of Examr)le 13, the following rnaterials were combined and mixed to form a 62.5% solid mi~ture which was extruded:
324.8 g bright tobacco (-60 mesh) at 7.64% OV
72.0 9 95% methylene chloride 83. 2 9 water During extrusion the pressure rose to about 1,500 psi. The mechanical properties of the extruded hollow tubes were excellent. The tubes exhibited a high degree of plasticity and could be stretched without lû rupturil-g. I engths greater tllan I meter could be extruded successfully.
The dried tubes would not maintain static burn. However, see Example 19 - with regard to subsequent treatment.
Examp!e 1~
- Using the procedure of Example 13, the following materials were combined and mixed to- form a mixture having 62.5% solids which was extruded:
332.2 g bright tobacco (-60 mesh) at 9.7% OV
34.2 9 methylene chloride 36 . 0 g ethanol 77 . 0 g water On extrusion, the tubes exhibited some plasticity; however, it was not as great as observed when rnethylene chloride was used as the major solvent. Static burn was achieved by subsequent treatment as noted in the following example.
Example 19 ., Representative tubes prepared in Examples 13, 15, 16, 17 and 18 were cut to a length of 10û mm. The tubes were immersed in water for 30seconds in such c manner that exactly 50 mm of each tube came in contact with the water. The tubes were dried for 2 minutes in CEM
30 Corporation Model AVC-MP microwave oven at maximum power. Conven-tional cellulose acetate filters were attached to the untreated end of each tube after drying. The tubes were secured by the filter end and the water treated end was ignited. The static burn rate was based on the time required to burn the 50 mm water treated portion of the tube. The results 35 are tabulated below in Table 5.
. .
"
.. . .. .
!
- . ~ -.~ , , Table 5 .
_ ~ _ . -- _ Static Burn Rate -- Example Solvent and Tobacco mmlmin.
13 Methyl Alcohol 1.85 Isopropyl Alcohol 3.64 16 Tert-Butyl Alcohol 2.13 17 Methylene Chloride 0.68 18 Methylene Chlorid.e-Ethanol 2.42 _ 'The tube immersed for 30 seconds would not static burn. After immersion for 45 seconds, the tube burned for 8 minutes 5 seconds and wenf out. After ~, relighting the tube burned for an additional 6 minutes 35 seconds. Total length burned was 10 mm.
The results indicate that when dried extruded tobacco tubes are 15 subjected to a water treatment, the tube wall is modified in such a manner that combustion properties of the tube are improved.
, Examp!e 20 The following ingredients were combined and mixed in a Hobart , i mixer for approximately 25 minutes:
154.05 9 bright tobacco (-60 mesh) at 9.15% OV
61.53 9 PCB* carbon (-40 +60 mesh) at 2.48% OV
~ 48.0 ml 95% ethanol 56.4 9 water , *PCB = Pittsburgh' Coal Carbon -40 +60 mesh , 1 25 The tobacco-carbon mixture having 64.5% solids was dark but appeared to have the same consistency as previous mixtures used.
Using extrusion conditions from Example 8, tobacco-carbon ' I tubes were produced wherein the outer diameter was 8 mm and the inner diameter was 6.5 mm. During extrusion the maximum head pressure was 30 2000 psig and the maximum melt temperature was 106F.
",1 After drying overnight, the tobacco-carbon tubes would maintain ,j a static burn.
~" Example 21 ' I Tobacco-carbon tubes wherein carbon represent'ed approximately s 35 40% of the to~al solids in the formulation were prepared using ~he following , ingredients:
', "
,, , ' : ~
r~
206.7 9 bright tobacco (-60 mesh) at 9.12% OV
130 . 3 g PCB carbon (-60 + 140 mesh) 75.1 ml 95% ethanol 88.7 9 water (64.5% solids) Tobacco-carbon tubes were extruded wherein the outer diameter . was 8 mm and the inner diameter was 5 mm. The Wayne plastics extruder was modified to include a low restriction spider to improve fiow properties.
The extruder conditions were as follows:
Zone I - 100F
I û Zone 2 - I 50F
Zone 3 - 200F
Die - 250F
Screw speed 120 rpm During extrusion the head pressure built up to about 600 psig cmd this was fol lowed by rapid extrusion of hibe product. As the pressure dropped, tube production ceased; however, with pressure build up, product was again cxtruded.
Samples of extruded tubes were dried overnight and tested for static burn. ~11 samples maintained a static burn.
Examp!e 22 The following ingredients were combined and mixed in a Hobart mixer:
154.û 9 bright tobacco (-60 mesh) at 9.12% OV
60.0 9 calcium carbonate at O.û6% OV (-5û mesh) 48.û ml 95% ethanol 57.9 g water (64.5% solids) After mixing for 25 minutes, tobacco tubes were extruded using the conditions described in Example 8. The maximum head pressure reached lOûO psig during extrusion. The extruded tubes appeared to have a diameter slightly larger than 8 mm. This may be due to expansion caused by the carbonate salt.
, Example 23 ; Bright tobaccoj 222.3 9, -60 mesh at lû.û9% OV, was combined with 84.8 9 of water and mixed in a Hobart mixer for I hour and 20 minutes.
.' I .
, ,~ .
. ' ~
, - .
L~
, Fifty g of ammonium carbonate at 20% OV was added and the mixture was stirred for lû minutes.
The material was extruded using the Wayne plastic extruder under the following conditions:
~one I - 30C
Zone 2 - 50~C
Zone 3 - 70~C
Vie - lû0~C
Feed cooling water on Straight tubing die (8 mm outer diameter, 7 mm inner diameter) No die head pressure was observed; the die temperature was reduced to 90C during extrusion.
c A representative example of the extruded tubesS cut to a 85 mm ; 15 length, was equilibrated overnight to 60RH in a humidity cabinet. On ignition wi1h a gas flame, the hollow tube maintained a $tatic burn for over 6 minutes. A 2û mm section of the tubc had a burn rate of ; 0.185 mm/second.
E)comple 24 2û0.2 9 bright tobacco (-40 +60 mesh) at lû.0% OV and iSû.0 g tobacco slurry containing diammonium phosphate and having 18.0% solids v content ~the slurry being of a type prepared according to U.S. Patent
3,353,541) were blended in a Hobart mixer for 2 hours to give a mixture having approxmateh~ 59.12% solids.
The material, which tended to form small balls, was successfully extruded using the ~Nayne plastics extruder. All three zones and the die were initially at room temperature and no coolin~ was used during extrusion.
Screw speed was between 30 to 60 rpm; head pressure was 70û psig.
Extrusion was stopped and fhe die temperature was raised to 100C. Additional tubes having 8 mm outer diameter and 7 mm inner diameter were successfully extruded.
Upon ignition with a gas flame, a sample of the latter tubes static burned for approximately 3 minutes, 20 seconds.
,'" I ' , j !
s: I
j!
s ~, '', ' ` :
, .
, b Example?5 222.3 g of bright tobacco (-40 mesh) having a moisture content of 10.05% OV was cornbined with 111.0 g water. The mixture was stirred in a Hobart mixer for 1.5 hours.
The tobacco mixture having a solids content of 60% by weight was then fed into the hopper of the extruder described in Example I and an attempt was made to extrude 8 mm O.D. x 7 mm l.D. hollow tobacco tubes.
The initial temperatures controller settings were as follows:
Zone I - 30C
Zone 2 - 5ûC
Zone 3 - 7ûC
Die - I OûC
Hopper cooling water on Tobacco tubes were extruded under these conditions. Steam was 15 noted to exit the die during extrusion. The temperature of Zone 3 was then raised to 100C. Tobacco tubes were extruded under these c~nditions and more steam was noted to exit the die than at the 7ûC setting.
The temper(lture of the die was then raised to 14ûC. Tobacco tubes were extruded under these conditions. Steam was noted to exit the 2û die and the exterior surface of the extruded tubes was more irregular (not smooth) than under previous conditions. None of the samples extruded under the above extrusion conditions would maintain static burning, suggesting the need for post-treatment or other means for controlling porosity.
Example 26 112.5 9 of bright tobacco (-40 +6û mesh) having a moisture content of 1 1.06% OV was combined with 61.33 9 water and 17.0 g 95%
ethanol. The mixture was stirred in a Hobart mixer for 1.25 hours. 112.5 9 of bright tobacco (-20 +4û mesh) having a moisture content of I I.û6% OV
was then added to the mixture and stirred for àn additional 15 minutes. The 30 tobacco mixture having a solids content of 65.9% by weight was then fed into the extruder hopper in an attempt to extrude 8 mm O.D. x 7 mm l.D.
hollow tobacco tubes.
Thc extruder temperature controls were set as follows:
, , .
,. . .. ..
,': ` :' ':
Zone I - ambient Zone 2 - ambient Zone 3 - ambient Die - off Hopper cooling water off Ambient temperature settings were obtained by positioning the controller setting to such a position that the controller supplied neither heat nor cooling. The temperature was 21C.
Hollow tobacco tubes were extruded, placed on paper towels and allowed to dry in room air overnight. The tubes would maintain static burn when dried.
Example 27 1092.2 9 of bright tobacco (-60 mesh) having a moisture content of 8.44% was combined with 268.3 9 water and 189.9 9 95% ethanol. The mixture was stirred in a Hobart mixer for 35 minutes.
The tobacco mixture having a solids content of 64.5% by weight was then divided into two parts. Approximate!y 3/4 of the mixture was fed into a Wayne Machine and Die Company table top extruder with a l-inch barrel. The extruder was supplied with four automatic temperature controls, three zones on the barrel and one on the die, water cooled hopper f4~ feed, cooling fans mounted on the barrel, a 1:1 extrusion screw, and a û to 10,000 psi Gentron No. GT-90 pressure gauge. One-fourth of the the mixture was placed in the hopper feeder of a Wayne plastics extruder Model No. 2417. The Model No. 2417 extruder was modified to take a I inch water 25 cooled barrel, a I inch 1:1 extrusion screw, and an automatic hopper feeder.
It was mated to the extruder referred to above via a modif ied Wayne - I Machine & Die Company cross-head die.
The Model No. 2417 extruder was then operated in such a manner ¦ as to sequentially extrude the tobacco mixture into the open passage of , 30 coextruded hollow tobacco tubes which were being extruded by the extruder described above. The sequential extrusion of the tobacco mixture into the 8 mm O.D. x 7 mm l.D. tubes resulted in a succession of plugs, approxi-mately 5 mm in length, located at approximately 70 mm intervals along the ', longitudinal axis of the hollow tubes. The extrusion conditions of the hollow - I 35 tubes were as follows:
,'1 .
", , ;
Zone I - 50C
Zone 2 - 70C
Zone 3 - 9ûC
Die - 200C
S Hopper cooling water on Used cross-head die and coextrusion Some samples from this extrusion were placed in a CEM Model AUC-MP microwave oven and dried at 1/2 power for five minutes. The samples so dried would maintain static burn.
Additional samples of extrudate were allowed to air dry on a paper towel overnight. These samples were then cut into smokable lengths by cutting the tube samples at the midpoint of each plug resulting in samples 75 mm in length with lobacco plugs of 2.5 mm thickness, located at each end. Several small holes were then drilled longitudinalhy through the pluggerJ ends of the samp!es using number 80 and number 69 drill bits to enûble the sarnples to be puffed on by a smoker. Cellulose acetate filters approxirnately 20 mm in length were then attached to one end of the sarnples with cellophane tape.
These samples would not maintain static burn. The samples were then dipped into water for 2 seconds and allowed to dry in room air overnight. After drying, the samples would maintain static burn and could be smoked.
" Example 28 327.2 9 of bright tobacco (-60 mesh) having a moisture content of 8.44% OV was combined with 81.67 9 water, 57.4 9 95% ethanol and 3.03 g tert butyl-p-menthanecarboxamide. The mixture was stirred in a Hobart mixer for 25 minutes.
The tobacco mixture having a solids content of 64.5% by weight was then divided into two parts and extruded under similar conditions as - 30 described in Example 27.
Plugged tube samples extruded in this manner were dried in a microwqve for five minutes at one-half power (181.4 watts). These samples would maintain static burn.
Smokable samples were produced from air dried extrudate by the same procedure used in E:<ample 27. These samples wouid not nc~intain static burn but would burn sufficiently so that they could be lit and smoked in a normal munner. A menthol-like cooling was detected when these ; samples were srnoked.
~ele 29 338.8 9 of bright tobacco (-60 mesh) having a moisture content of 11.46% OV was combined with 69.2 9 water and 56.8 g 95% ethanol. The mixture was stirred in a Hobart mixer for 35 minutes.
The tobacco mixture haviny a solid content or 64.5% was fed - into the extruder referred to in Example 26 and ô mm O.D. x 7 mm l.D.
10 hollow tobacco tubes were extruded under similqr conditions (~s described in Example 26.
Samples of the extrudate were placed on paper towels and allowed to dry in room air overnight.
Some samples collected during the time interval of 5.5 to 7.0 ,' 15 minutes of extrusion were selected for analysis. The results of the analysis were as fol lows:
Sample weight 12.96 mg/mm Wall density (calculated) I . lûû g/cc a P (85 mm) 3.94 inches H2O
20 Static burn rate 23.46 mm/min , TPM/puff .16 mg Tar/puff ~ 10 rmg ~; Third puff CO delivery .03 mg - E~comple 30 451.8 9 of bright tobacco having a moisture content of 11.46% OV was combined with 92.2 g water and 75.7 9 95% ethanol. The ~, mixture was stirred in a Hobart mixer for 25 minutes.
The tobacco mixture having a solids content of 6~.5% by weight was then fed into the Wayne l\/lachine and Die Company table top extruder ; i 30 referred to in Example 27. The die of the extruder was modified to extrude 8 mm O.D. x 6 mm l.D. hollow tubes. The extrusion conditions were the same as Example 26.
The extruded tobacco tubes were placed on paper towels to dry overnight ir, room air.
', 1 Extrudate samples collected during the time interval of 5.5 to 7.5 minutes of extrusion were selected for analysis. The results of the analysis were as follows:
Sample weight 19.87 mg/mm Wall density .904 g/cc A P (85 mm) 6 . 77 inches H2O
Static burn rate 31.20 mm/min TPM/puff .21 mg Tar/puff .1 7 mg Third puff CO delivery .06 mg ."
.'' ' ' .
, .
The material, which tended to form small balls, was successfully extruded using the ~Nayne plastics extruder. All three zones and the die were initially at room temperature and no coolin~ was used during extrusion.
Screw speed was between 30 to 60 rpm; head pressure was 70û psig.
Extrusion was stopped and fhe die temperature was raised to 100C. Additional tubes having 8 mm outer diameter and 7 mm inner diameter were successfully extruded.
Upon ignition with a gas flame, a sample of the latter tubes static burned for approximately 3 minutes, 20 seconds.
,'" I ' , j !
s: I
j!
s ~, '', ' ` :
, .
, b Example?5 222.3 g of bright tobacco (-40 mesh) having a moisture content of 10.05% OV was cornbined with 111.0 g water. The mixture was stirred in a Hobart mixer for 1.5 hours.
The tobacco mixture having a solids content of 60% by weight was then fed into the hopper of the extruder described in Example I and an attempt was made to extrude 8 mm O.D. x 7 mm l.D. hollow tobacco tubes.
The initial temperatures controller settings were as follows:
Zone I - 30C
Zone 2 - 5ûC
Zone 3 - 7ûC
Die - I OûC
Hopper cooling water on Tobacco tubes were extruded under these conditions. Steam was 15 noted to exit the die during extrusion. The temperature of Zone 3 was then raised to 100C. Tobacco tubes were extruded under these c~nditions and more steam was noted to exit the die than at the 7ûC setting.
The temper(lture of the die was then raised to 14ûC. Tobacco tubes were extruded under these conditions. Steam was noted to exit the 2û die and the exterior surface of the extruded tubes was more irregular (not smooth) than under previous conditions. None of the samples extruded under the above extrusion conditions would maintain static burning, suggesting the need for post-treatment or other means for controlling porosity.
Example 26 112.5 9 of bright tobacco (-40 +6û mesh) having a moisture content of 1 1.06% OV was combined with 61.33 9 water and 17.0 g 95%
ethanol. The mixture was stirred in a Hobart mixer for 1.25 hours. 112.5 9 of bright tobacco (-20 +4û mesh) having a moisture content of I I.û6% OV
was then added to the mixture and stirred for àn additional 15 minutes. The 30 tobacco mixture having a solids content of 65.9% by weight was then fed into the extruder hopper in an attempt to extrude 8 mm O.D. x 7 mm l.D.
hollow tobacco tubes.
Thc extruder temperature controls were set as follows:
, , .
,. . .. ..
,': ` :' ':
Zone I - ambient Zone 2 - ambient Zone 3 - ambient Die - off Hopper cooling water off Ambient temperature settings were obtained by positioning the controller setting to such a position that the controller supplied neither heat nor cooling. The temperature was 21C.
Hollow tobacco tubes were extruded, placed on paper towels and allowed to dry in room air overnight. The tubes would maintain static burn when dried.
Example 27 1092.2 9 of bright tobacco (-60 mesh) having a moisture content of 8.44% was combined with 268.3 9 water and 189.9 9 95% ethanol. The mixture was stirred in a Hobart mixer for 35 minutes.
The tobacco mixture having a solids content of 64.5% by weight was then divided into two parts. Approximate!y 3/4 of the mixture was fed into a Wayne Machine and Die Company table top extruder with a l-inch barrel. The extruder was supplied with four automatic temperature controls, three zones on the barrel and one on the die, water cooled hopper f4~ feed, cooling fans mounted on the barrel, a 1:1 extrusion screw, and a û to 10,000 psi Gentron No. GT-90 pressure gauge. One-fourth of the the mixture was placed in the hopper feeder of a Wayne plastics extruder Model No. 2417. The Model No. 2417 extruder was modified to take a I inch water 25 cooled barrel, a I inch 1:1 extrusion screw, and an automatic hopper feeder.
It was mated to the extruder referred to above via a modif ied Wayne - I Machine & Die Company cross-head die.
The Model No. 2417 extruder was then operated in such a manner ¦ as to sequentially extrude the tobacco mixture into the open passage of , 30 coextruded hollow tobacco tubes which were being extruded by the extruder described above. The sequential extrusion of the tobacco mixture into the 8 mm O.D. x 7 mm l.D. tubes resulted in a succession of plugs, approxi-mately 5 mm in length, located at approximately 70 mm intervals along the ', longitudinal axis of the hollow tubes. The extrusion conditions of the hollow - I 35 tubes were as follows:
,'1 .
", , ;
Zone I - 50C
Zone 2 - 70C
Zone 3 - 9ûC
Die - 200C
S Hopper cooling water on Used cross-head die and coextrusion Some samples from this extrusion were placed in a CEM Model AUC-MP microwave oven and dried at 1/2 power for five minutes. The samples so dried would maintain static burn.
Additional samples of extrudate were allowed to air dry on a paper towel overnight. These samples were then cut into smokable lengths by cutting the tube samples at the midpoint of each plug resulting in samples 75 mm in length with lobacco plugs of 2.5 mm thickness, located at each end. Several small holes were then drilled longitudinalhy through the pluggerJ ends of the samp!es using number 80 and number 69 drill bits to enûble the sarnples to be puffed on by a smoker. Cellulose acetate filters approxirnately 20 mm in length were then attached to one end of the sarnples with cellophane tape.
These samples would not maintain static burn. The samples were then dipped into water for 2 seconds and allowed to dry in room air overnight. After drying, the samples would maintain static burn and could be smoked.
" Example 28 327.2 9 of bright tobacco (-60 mesh) having a moisture content of 8.44% OV was combined with 81.67 9 water, 57.4 9 95% ethanol and 3.03 g tert butyl-p-menthanecarboxamide. The mixture was stirred in a Hobart mixer for 25 minutes.
The tobacco mixture having a solids content of 64.5% by weight was then divided into two parts and extruded under similar conditions as - 30 described in Example 27.
Plugged tube samples extruded in this manner were dried in a microwqve for five minutes at one-half power (181.4 watts). These samples would maintain static burn.
Smokable samples were produced from air dried extrudate by the same procedure used in E:<ample 27. These samples wouid not nc~intain static burn but would burn sufficiently so that they could be lit and smoked in a normal munner. A menthol-like cooling was detected when these ; samples were srnoked.
~ele 29 338.8 9 of bright tobacco (-60 mesh) having a moisture content of 11.46% OV was combined with 69.2 9 water and 56.8 g 95% ethanol. The mixture was stirred in a Hobart mixer for 35 minutes.
The tobacco mixture haviny a solid content or 64.5% was fed - into the extruder referred to in Example 26 and ô mm O.D. x 7 mm l.D.
10 hollow tobacco tubes were extruded under similqr conditions (~s described in Example 26.
Samples of the extrudate were placed on paper towels and allowed to dry in room air overnight.
Some samples collected during the time interval of 5.5 to 7.0 ,' 15 minutes of extrusion were selected for analysis. The results of the analysis were as fol lows:
Sample weight 12.96 mg/mm Wall density (calculated) I . lûû g/cc a P (85 mm) 3.94 inches H2O
20 Static burn rate 23.46 mm/min , TPM/puff .16 mg Tar/puff ~ 10 rmg ~; Third puff CO delivery .03 mg - E~comple 30 451.8 9 of bright tobacco having a moisture content of 11.46% OV was combined with 92.2 g water and 75.7 9 95% ethanol. The ~, mixture was stirred in a Hobart mixer for 25 minutes.
The tobacco mixture having a solids content of 6~.5% by weight was then fed into the Wayne l\/lachine and Die Company table top extruder ; i 30 referred to in Example 27. The die of the extruder was modified to extrude 8 mm O.D. x 6 mm l.D. hollow tubes. The extrusion conditions were the same as Example 26.
The extruded tobacco tubes were placed on paper towels to dry overnight ir, room air.
', 1 Extrudate samples collected during the time interval of 5.5 to 7.5 minutes of extrusion were selected for analysis. The results of the analysis were as follows:
Sample weight 19.87 mg/mm Wall density .904 g/cc A P (85 mm) 6 . 77 inches H2O
Static burn rate 31.20 mm/min TPM/puff .21 mg Tar/puff .1 7 mg Third puff CO delivery .06 mg ."
.'' ' ' .
, .
Claims (72)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A method of producing smoking articles comprising:
mixing combustible tobacco material with one or more other ingredients including a liquid to provide a tobacco mixture;
shaping the mixture under pressure into a discrete coherent mass;
providing a passage through said mass;
and drying said shaped mass, the mixture com-position being selected and the shaping pressure and drying being controlled to impart to said shaped mass a porosity and density such as to substantially occlude gas flow there-through and a porosity sufficient to support combustion of said shaped mass when ignited.
mixing combustible tobacco material with one or more other ingredients including a liquid to provide a tobacco mixture;
shaping the mixture under pressure into a discrete coherent mass;
providing a passage through said mass;
and drying said shaped mass, the mixture com-position being selected and the shaping pressure and drying being controlled to impart to said shaped mass a porosity and density such as to substantially occlude gas flow there-through and a porosity sufficient to support combustion of said shaped mass when ignited.
2. A method in accordance with claim 1 wherein:
said through passage is provided during the shaping operation.
said through passage is provided during the shaping operation.
3. A method in accordance with claim 1 wherein:
said through passage is provided subsequent to the shaping operation.
said through passage is provided subsequent to the shaping operation.
4. A method in accordance with claim 1 wherein:
said liquid is water and said one or more other ingredients further include a volatile organic liquid.
said liquid is water and said one or more other ingredients further include a volatile organic liquid.
5. A method in accordance with claim 1 wherein:
said mixture is shaped into a coherent mass by extrusion.
said mixture is shaped into a coherent mass by extrusion.
6. A method in accordance with claim 1 wherein:
the tobacco mixture has a solids content of about 55 to 75 weight percent solids.
the tobacco mixture has a solids content of about 55 to 75 weight percent solids.
7. A method in accordance with claim 1 wherein:
said one or more other ingredients are non-binder materials.
said one or more other ingredients are non-binder materials.
8. A method in accordance with claim 1 wherein:
said tobacco material in comminuted.
said tobacco material in comminuted.
9. A method in accordance with claim 1 wherein:
said tobacco material is comminuted;
said liquid is water and said one or more other ingredients are non-binder materials and include a volatile organic liquid;
said tobacco mixture has a solids content of about 55 to 75 weight percent solids; and said mixture is shaped into a coherent mass by extrusion.
said tobacco material is comminuted;
said liquid is water and said one or more other ingredients are non-binder materials and include a volatile organic liquid;
said tobacco mixture has a solids content of about 55 to 75 weight percent solids; and said mixture is shaped into a coherent mass by extrusion.
10. A method in accordance with claim 6 or 9 wherein:
the tobacco mixture has a solids content of about 60 to 70 weight percent solids.
the tobacco mixture has a solids content of about 60 to 70 weight percent solids.
11. A method in accordance with claim 8 or 9 wherein:
said tobacco material has a mesh size of less than about 30 mesh.
said tobacco material has a mesh size of less than about 30 mesh.
12. A method in accordance with claim 8 or 9 wherein:
the tobacco material has a mesh size of less than about 60 mesh.
the tobacco material has a mesh size of less than about 60 mesh.
13. A method in accordance with claim 4 or 9 wherein:
said volatile liquid is a low molecular weight alcohol compatible with tobacco.
said volatile liquid is a low molecular weight alcohol compatible with tobacco.
14. A method in accordance with claim 4 or 9 wherein:
said volatile liquid is ethanol.
said volatile liquid is ethanol.
15. A method in accordance with claim 4 or 9 wherein:
the ratio of organic liquid to water is between 1:6 to 1:1.
the ratio of organic liquid to water is between 1:6 to 1:1.
16. A method in accordance with claim 4 or 9 wherein:
the ratio of organic liquid to water is between 1:2 to 1:1.
the ratio of organic liquid to water is between 1:2 to 1:1.
17. A method in accordance with claim 1 or 9 wherein:
said one or more other ingredients further include non-tobacco filler particles.
said one or more other ingredients further include non-tobacco filler particles.
18. A method in accordance with claim 1 or 9 wherein:
the filler particles are selected from the group consisting of carbon, calcium carbonate, diatomaceous earth and attapulgite.
the filler particles are selected from the group consisting of carbon, calcium carbonate, diatomaceous earth and attapulgite.
19. A method in accordance with claim 1 or 9 wherein:
the filler particles are up to about 50 percent of the solid content of said mixture.
the filler particles are up to about 50 percent of the solid content of said mixture.
20. A method in accordance with claim 1 or 9 wherein:
said one or more other ingredients include burn additives.
said one or more other ingredients include burn additives.
21. A method in accordance with claim 1 or 9 wherein:
said one or more other ingredients include fla-vorants.
said one or more other ingredients include fla-vorants.
22. A method in accordance with claim 1 or 9 wherein:
mixing is carried out for a time sufficient to obtain a substantially homogenous mixture of said tobacco material and said one or more other ingredients.
mixing is carried out for a time sufficient to obtain a substantially homogenous mixture of said tobacco material and said one or more other ingredients.
23. A method in accordance with claim 1 or 9 wherein:
mixing is carried out for a time of about 15 minutes to several hours.
mixing is carried out for a time of about 15 minutes to several hours.
24. A method in accordance with claim 4 or 9 wherein:
mixing includes placing said tobacco material and one or more other ingredients into a closed environment to prevent volatilization of said organic liquid.
mixing includes placing said tobacco material and one or more other ingredients into a closed environment to prevent volatilization of said organic liquid.
25. A method in accordance with claim 1 or 9 wherein:
drying is effected by subjecting said shaped mass to heat.
drying is effected by subjecting said shaped mass to heat.
26. A method in accordance with claim 1 wherein:
drying is effected by applying hot air to said shaped mass.
drying is effected by applying hot air to said shaped mass.
27. A method in accordance with claim 26 wherein:
the air is heated at a temperature of about 100°C
and drying is effected for a period of about 15 minutes to 1 hour.
the air is heated at a temperature of about 100°C
and drying is effected for a period of about 15 minutes to 1 hour.
28. A method in accordance with claim 1 wherein:
drying is effected by subjecting said shaped mass to microwave energy.
drying is effected by subjecting said shaped mass to microwave energy.
29. A method in accordance with claim 28 wherein:
said microwave energy is at a preselected power level and is applied for a preselected time.
said microwave energy is at a preselected power level and is applied for a preselected time.
30. A method in accordance with claim 1 wherein:
drying is effected by subjecting said shaped mass to ambient atmosphere.
drying is effected by subjecting said shaped mass to ambient atmosphere.
31. A method in accordance with claim 30 wherein:
said ambient atmosphere has a temperature within the range of 70 to 75°F and said shaped mass is subjected to said atmosphere for a period of time in the range of 12 to 24 hours.
said ambient atmosphere has a temperature within the range of 70 to 75°F and said shaped mass is subjected to said atmosphere for a period of time in the range of 12 to 24 hours.
32. A method in accordance with claim 1 further comprising:
rewetting said dried mass;
and redrying said rewetted mass.
rewetting said dried mass;
and redrying said rewetted mass.
33. A method in accordance with claim 32 wherein:
rewetting is carried out for a period of time sufficient to obtain a desired porosity for said mass.
rewetting is carried out for a period of time sufficient to obtain a desired porosity for said mass.
34. A method in accordance with claim 5 ox 9 wherein:
extrusion is carried out in such manner that a minimum working of the tobacco mixture occurs while suffi-cient pressure is applied thereto to release the natural.
binding agents of the tobacco material contained therein.
extrusion is carried out in such manner that a minimum working of the tobacco mixture occurs while suffi-cient pressure is applied thereto to release the natural.
binding agents of the tobacco material contained therein.
35. A method in accordance with claim 5 or 9 further comprising:
force feeding said tobacco mixture to the ex-trusion mechanism.
force feeding said tobacco mixture to the ex-trusion mechanism.
36. A method in accordance with claim 5 or 9 wherein:
extrusion is carried out with a screw extrusion operation.
extrusion is carried out with a screw extrusion operation.
37. A method in accordance with claim 5 or 9 wherein.
the extrusion operation is effected with an extruder having a 1:1 screw.
the extrusion operation is effected with an extruder having a 1:1 screw.
38. A method in accordance with claim 5 wherein:
the extrusion of said tobacco mixture is at a melt pressure equal to or less than 2500 psi.
the extrusion of said tobacco mixture is at a melt pressure equal to or less than 2500 psi.
39. A method in accordance with claim 38 wherein:
the extrusion of said tobacco mixture is at a melt pressure equal to or less than 1200 psi.
.
the extrusion of said tobacco mixture is at a melt pressure equal to or less than 1200 psi.
.
40. A method in accordance with claim 39 wherein:
the temperature of said tobacco mixture during the extrusion operation is at or below a melt temperature of 40°C.
the temperature of said tobacco mixture during the extrusion operation is at or below a melt temperature of 40°C.
41. A method in accordance with claim 5 or 9 wherein:
the extrusion of said tobacco mixture is carried out with a ram extrusion operation.
the extrusion of said tobacco mixture is carried out with a ram extrusion operation.
42. A method in accordance with claim 5 or 9 wherein:
the extrusion operation is carried out such as to produce a substantially cylindrically shaped mass.
the extrusion operation is carried out such as to produce a substantially cylindrically shaped mass.
43. A method in accordance with claim 5 wherein:
said passage extends along the axis of said cylindrically shaped mass.
said passage extends along the axis of said cylindrically shaped mass.
44. A method in accordance with claim 43 wherein:
the cross-sectional area of said shaped mass normal to said axis is less than the cross-sectional area of said passage normal to said axis.
the cross-sectional area of said shaped mass normal to said axis is less than the cross-sectional area of said passage normal to said axis.
45. A method in accordance with claim 44 wherein:
said passage is defined by an inner surface of said shaped mass.
said passage is defined by an inner surface of said shaped mass.
46. A method in accordance with claim 1 or 9 further comprising the step of:
inserting one or more porous readily ignitable plugs into the passage of said mass.
inserting one or more porous readily ignitable plugs into the passage of said mass.
47. A method in accordance with claim 1 or 9 wherein:
at least one of said plugs contains a flavorant.
at least one of said plugs contains a flavorant.
48. A method in accordance with claim 5 or 9 further comprising:
inserting one or more porous readily ignitable plugs into said passage by extruding plug material into said passage.
inserting one or more porous readily ignitable plugs into said passage by extruding plug material into said passage.
49 A. method in accordance with claim 5 wherein:
the extrusion of said tobacco mixture and of said plug material occurs concurrently.
the extrusion of said tobacco mixture and of said plug material occurs concurrently.
50. A method in accordance with claim 49 wherein:
the extrusion of said plug material is carried out intermittently.
the extrusion of said plug material is carried out intermittently.
51. A method in accordance with claim 50 further compri-sing: l cutting said mass transverse to said axis at positions at which said plug material is located in said passage.
52. A method in accordance with claim 51 wherein:
said cutting is through said plug material.
said cutting is through said plug material.
53. A method in accordance with claim 51 wherein:
said cutting occurs concurrently with said ex-truding of said tobacco mixture.
said cutting occurs concurrently with said ex-truding of said tobacco mixture.
54. A method in accordance with claim 53 wherein:
said cutting is synchronized with the extrusion of said tobacco mixture to provide sections of said mass having preselected length and having plug material therein of preselected expanse.
said cutting is synchronized with the extrusion of said tobacco mixture to provide sections of said mass having preselected length and having plug material therein of preselected expanse.
55. A method in accordance with 49 further comprising:
applying force to the wall of said extruded tobacco mixture to cohesively join said tobacco mixture to said extruded plug material.
applying force to the wall of said extruded tobacco mixture to cohesively join said tobacco mixture to said extruded plug material.
56. A method in accordance with claim 49 further compri-sing:
allowing the plug material to expand and cohesively join itself to the wall of said extruded tobacco mixture.
allowing the plug material to expand and cohesively join itself to the wall of said extruded tobacco mixture.
44 ?7. A method in accordance with claim 8 or 9 further comprising:
comminuting said tobacco material prior to mixing said tobacco material.
comminuting said tobacco material prior to mixing said tobacco material.
58. Smoking article comprising a coherent mass of combustible tobacco-containing material, said mass having at least one through passage extending from a first opening in the surface of said mass to a second opening remote from the first, said tobacco mass having a porosity such as to support combustion of said mass when ignited, said tobacco mass further being of a density and porosity such as to substantially occlude gas flow therethrough, thereby providing that puff induced air flow through the smoking article is through the passage.
59. The smoking article of Claim 58 which further comprises a first air permeable plug of readily ignitable material disposed in passage blocking position at one end of said passage.
60. The smoking article of Claim 59 which further com-prises a second air permeable plug of readily ignitable material disposed in passage blocking position remote from said first air permeable plug.
61. The smoking article of Claim 60 wherein the said second plug is at the other end of said passage.
62. The smoking article of Claim 58 wherein the smoking article has a passage extending axially through a mass having a cylindrical shape.
63. The smoking article of Claim 62 wherein the cross-sectional surface area of the passage is greater than the corresponding surface area of the mass.
64. The smoking article of Claim 58wherein the coherent mass of tobacco material comprises extruded comminuted tobacco.
65. The smoking article of Claim 58 formed by extrud-ing a binder-free mixture or comminuted tobacco, water and a volatile organic liquid compatible with the tobacco, said mixture having a solids content of 55 to 75 weight percent and drying the resulting extrudate.
66. The smoking article of Claim 65wherein the comminuted tobacco is less than 30 mesh.
67. The smoking article of Claim 65wherein the organic liquid is a low molecular weight alcohol compatible with tobacco.
68. The smoking article of Claim 65wherein the organic liquid is ethanol.
69. The smoking article of Claim 68 wherein the ratio of alcohol to water is between 1: 6 and 1:1.
70. The smoking article of Claim 58wherein the tobacco-containing material further comprises combustible filler particles.
71. The smoking article of Claim 70 wherein the filler particles are selected from the group consisting of carbon, calcium carbonate, diatomaceous earth and attapulgite.
72. The smoking article of Claim 58 wherein the tobacco-containing material further comprises burn additives.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/148,124 US4391285A (en) | 1980-05-09 | 1980-05-09 | Smoking article |
| US148,124 | 1980-05-09 | ||
| US17131480A | 1980-07-23 | 1980-07-23 | |
| US171,314 | 1993-12-20 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1158516A true CA1158516A (en) | 1983-12-13 |
Family
ID=26845542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000377146A Expired CA1158516A (en) | 1980-05-09 | 1981-05-08 | Smoking articles and method of making such articles |
Country Status (10)
| Country | Link |
|---|---|
| AU (1) | AU544119B2 (en) |
| BR (1) | BR8102890A (en) |
| CA (1) | CA1158516A (en) |
| CH (1) | CH653530A5 (en) |
| DE (1) | DE3118472A1 (en) |
| FR (1) | FR2481892B1 (en) |
| GB (1) | GB2078087B (en) |
| IT (1) | IT1144345B (en) |
| NL (1) | NL8102299A (en) |
| PH (1) | PH18230A (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8329501D0 (en) * | 1983-11-04 | 1983-12-07 | British American Tobacco Co | Smoking articles |
| US4754767A (en) * | 1986-11-21 | 1988-07-05 | R. J. Reynolds Tobacco Company | Tobacco material processing |
| DE3835948A1 (en) * | 1987-10-23 | 1989-05-03 | Friedrich Wienold | Smoking material |
| GB8914508D0 (en) * | 1989-06-23 | 1989-08-09 | British American Tobacco Co | Improvements relating to the making of smoking articles |
| DE4117307C1 (en) * | 1991-05-27 | 1992-06-04 | B.A.T. Cigarettenfabriken Gmbh, 2000 Hamburg, De | |
| AU3202895A (en) * | 1994-07-28 | 1996-02-22 | Lorillard Tobacco Company | Hollow smokable article |
| EP2120614B1 (en) * | 2006-12-28 | 2013-03-06 | Philip Morris Products S.A. | Various embodiments for producing a tobacco rod with a hollow passageway extending therethrough |
| EP3626085A1 (en) | 2018-09-24 | 2020-03-25 | Imperial Tobacco Ventures Limited | Method for producing a tubular tobacco product, tubular tobacco product, aerosol-forming stick, aerosol-generating device |
| EP3626084A1 (en) | 2018-09-24 | 2020-03-25 | Imperial Tobacco Ventures Limited | Method for producing a tubular tobacco product, tubular tobacco product, aerosol-forming stick, aerosol-generating device |
| EP4070672A4 (en) * | 2019-10-11 | 2024-07-24 | Ccobato Shenzhen Tech Co Ltd | Heat-not-burn vapor generating body and preparation method therefor, tobacco product and vapor generating body |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH275420A (en) * | 1949-09-23 | 1951-05-31 | Soehne Burger | Process for the production of tobacco products such as pillar and cigarillos, and device for carrying out the process. |
| US3364935A (en) * | 1961-08-11 | 1968-01-23 | American Mach & Foundry | Tobacco product and process for making same |
| US3223090A (en) * | 1963-09-11 | 1965-12-14 | Brown & Williamson Tobacco | Reconstituted tobacco products and method of making same |
| US3349776A (en) * | 1964-12-04 | 1967-10-31 | Bell | Low-temperature cigarette |
| US3516417A (en) * | 1968-04-05 | 1970-06-23 | Clayton Small Moses | Method of smoking and means therefor |
| US3774622A (en) * | 1971-11-16 | 1973-11-27 | K Steigerwald | Device,particularly a cigarette,for smoking a cord of smokable material |
| DE2421652C3 (en) * | 1974-05-04 | 1984-01-19 | Eduard Gerlach GmbH Chemische Fabrik, 4990 Lübbecke | Process for the production of tobacco foils and plant for carrying out the process |
| LU73096A1 (en) * | 1975-07-29 | 1977-03-24 | ||
| DE2611647A1 (en) * | 1976-03-19 | 1977-09-22 | Henkel & Cie Gmbh | PROCESS FOR MANUFACTURING TOBACCO FILM |
| DE2620298A1 (en) * | 1976-05-07 | 1977-11-17 | Brasec Gmbh Chemisch Physikali | Cigarette having reduced harmful effects on smoker - has paper or metal tube with specified porosity extending through tobacco |
| US4144894A (en) * | 1977-06-29 | 1979-03-20 | Amf Incorporated | Reconstituted tobacco composition and process for manufacturing same |
-
1981
- 1981-05-08 AU AU70282/81A patent/AU544119B2/en not_active Ceased
- 1981-05-08 GB GB8114158A patent/GB2078087B/en not_active Expired
- 1981-05-08 PH PH25603A patent/PH18230A/en unknown
- 1981-05-08 FR FR8109194A patent/FR2481892B1/en not_active Expired
- 1981-05-08 CA CA000377146A patent/CA1158516A/en not_active Expired
- 1981-05-08 IT IT67621/81A patent/IT1144345B/en active
- 1981-05-08 BR BR8102890A patent/BR8102890A/en unknown
- 1981-05-09 DE DE19813118472 patent/DE3118472A1/en not_active Withdrawn
- 1981-05-11 CH CH3040/81A patent/CH653530A5/en not_active IP Right Cessation
- 1981-05-11 NL NL8102299A patent/NL8102299A/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| AU7028281A (en) | 1981-11-12 |
| FR2481892A1 (en) | 1981-11-13 |
| FR2481892B1 (en) | 1985-07-05 |
| PH18230A (en) | 1985-05-03 |
| DE3118472A1 (en) | 1982-02-04 |
| IT1144345B (en) | 1986-10-29 |
| IT8167621A0 (en) | 1981-05-08 |
| GB2078087A (en) | 1982-01-06 |
| GB2078087B (en) | 1984-06-27 |
| BR8102890A (en) | 1982-02-02 |
| NL8102299A (en) | 1981-12-01 |
| CH653530A5 (en) | 1986-01-15 |
| AU544119B2 (en) | 1985-05-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4347855A (en) | Method of making smoking articles | |
| US4391285A (en) | Smoking article | |
| DE3882740T2 (en) | Smoking articles. | |
| US5129409A (en) | Extruded cigarette | |
| DE69015833T2 (en) | Smoking articles. | |
| US5178167A (en) | Carbonaceous composition for fuel elements of smoking articles and method of modifying the burning characteristics thereof | |
| US4989620A (en) | Method and apparatus for coating extruded tobacco-containing material | |
| US5690127A (en) | Hollow cigarette | |
| US4625737A (en) | Foamed, extruded, tobacco-containing smoking article and method of making the same | |
| EP0117355B1 (en) | Process for making a carbon heat source and smoking article including the heat source and a flavor generator | |
| DE68921383T2 (en) | Carbonaceous heat source. | |
| US5829453A (en) | Low-density tobacco filler and a method of making low-density tobacco filler and smoking articles therefrom | |
| DE68925243T2 (en) | Smoking articles | |
| SU1836038A3 (en) | Smoking article | |
| US4874000A (en) | Method and apparatus for drying and cooling extruded tobacco-containing material | |
| US5240016A (en) | Thermally releasable gel-based flavor source for smoking articles | |
| DE69029309T2 (en) | Cigarette and its smokable filler | |
| DE69518247T2 (en) | SMOKING ITEMS | |
| EP0568107A2 (en) | Method and apparatus for forming a rod for use in the manufacture of smoking articles | |
| WO2000028842A1 (en) | System for supplying an inhalable aerosol | |
| CA1158516A (en) | Smoking articles and method of making such articles | |
| DD295080A5 (en) | DEVICE FOR PRODUCING TOBACCO-LIKE AEROSOLS | |
| WO2000028844A1 (en) | System for supplying an inhalable aerosol | |
| US5433224A (en) | Smoking articles | |
| CA1247970A (en) | Foamed, extruded tobacco-containing smoking articles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |