United States Patent (19)
`Mays et al.
`
`11)
`45
`
`4,449,541
`May 22, 1984
`
`54 TOBACCO TREATMENT PROCESS
`4,054,145 10/1977 Berndt et al. ....................... 131/139
`4,148,325 4/1979 Solomon et al. ....
`... 131/134
`75 Inventors: Charles D. Mays, Lewisville; Max A.
`FOREIGN PATENT DOCUMENTS
`Wagoner; Daniel G. Williard, both of
`1065767 9/1959 Fed. Rep. of Germany.
`Winston-Salem, all of N.C.
`OTHER PUBLICATIONS
`73) Assignee: R. J. Reynolds Tobacco Company,
`ld Tob
`No. 59, (J
`78)
`Winston-Salem, N.C.
`Wor obacco, No. 59, (Jan. 1978), pp. 89-91. .
`Akehurst, B. C., Tobacco, Longman, (1968), pp.
`21 Appl. No.: 269,086
`471-474.
`(22
`Filed:
`Jun. 2, 1981
`3. Evil; Industry 4, (No. 11), (Nov.-Dec. 1973), pp.
`51) Int. Cl. ................................................
`52 U.S. Cl. ..................................... 131/302; 131/310
`0.
`58) Field of Search ............... 131/296, 300, 302, 303,
`Primary Examiner-Vincent Millin
`131/304, 305, 306, 309, 310
`Attorney, Agent, or Firm-Herbert J. Bluhm
`References Cited
`57
`ABSTRACT
`U.S. PATENT DOCUMENTS
`Cut shredded or otherwise comminuted tobacco is
`Re. 29,298 2/1977 Banks .................................. 131/144
`treated with a volatile flavoring additive in a continuous
`3,085,581 4/1963 Rosenberg ......
`... 131/144
`process wherein the additive is combined with a poly
`3,419,015 12/1968 Wochnowski.
`... 131/138
`hydric alcohol carrier and the additive/polyhydric
`: 3.1879
`------- -
`-
`- - -
`-
`/ : alcohol combination is applied to the tobacco by gas
`374,661 7/1973 W .
`7
`atomizing spray nozzle means) under controlled condi
`3,800,806 4/1974 Banks.
`131/144
`tons.
`3,817,258 6/1974 Ernow .................................. 131/31
`4,004,594 1/1977
`o a ea o saw a ow 131/303
`
`(56)
`
`-
`
`-
`
`-
`
`-
`
`-
`
`-
`
`- -
`
`27 Claims, 1 Drawing Figure
`
`
`
`FROM
`
`CONTINUOUS OACCO
`We GNG CONMEYoR
`
`
`
`
`
`Alk paeSSURE
`SUPPLY
`
`uMsCANT
`FAN/orAN
`SUPPY tank.
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 001
`
`

`

`U.S. Patent
`
`May 22, 1984
`
`4,449,541
`
`
`
`
`
`continuous Tobacco
`FRONM
`TO3 ACCO-- WEG NG conVEyota
`SUpply
`
`
`
`
`
`
`
`O3ACCO
`RANG
`CAMER
`
`UMscVANT
`FLAN/O ean
`SUpps/ ANK
`
`
`
`
`
`
`
`AR
`2RSSSURE SUPPS/
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 002
`
`

`

`TOBACCO TREATMENT PROCESS
`
`55
`
`TECHNICAL FIELD
`This invention relates to the treatment of tobacco
`with flavoring and other additives in connection with
`the manufacture of tobacco products utilizing the
`treated tobacco.
`10
`BACKGROUND ART
`The manufacture of tobacco products usually in
`volves treatment of the tobacco being processed with
`certain additives to enhance the quality and flavor char
`acteristics of the resulting products. In view of the vari
`15
`ous processing conditions to which the tobacco is sub
`jected, care must be taken so that additives applied to
`the tobacco are not adversely affected by subsequent
`processing steps. This is particularly true in the case of
`flavoring additives which are somewhat volatile be
`cause subsequent processing steps involving heat can
`result in significant losses of the volatile additives from
`the treated tobacco. Thus, tobacco flavoring additives
`which are somewhat volatile are generally applied to
`the tobacco in the form of an alcoholic solution of "top
`25
`flavors' after the tobacco has already been subjected to
`the heating and drying conditions which are used dur
`ing certain processing steps.
`In addition to the volatile "top flavor” additives,
`another category of additives having a relatively low
`30
`degree of volatility is also customarily applied to to
`bacco. This category includes materials such as sugars,
`licorice, cocoa, essential oils, fruit extracts and humec
`tants. These materials are known in the art as "casing'
`35
`materials and they are applied to the tobacco by dipping
`or spraying prior to the cutting or shredding operation.
`While the ingredients used in casing compositions may
`vary to a considerable degree, the basic components are
`the sugars and humectants. The sugars serve to import
`the smoking quality of certain tobaccos such as Burley
`which are deficient in natural sugars. The humectants
`impart elasticity to the tobacco and contribute to in
`creased stability of the flavor. It should be noted that
`water is also used in most casing compositions and can
`45
`provide improved elasticity or pliability of the tobacco.
`The elasticity due to water, however, is less permanent
`than that of humectants because water is removed from
`the cased tobacco during subsequent processing of the
`tobacco whereas the less volatile humectants are re
`50
`tained by the tobacco during the heating and drying
`steps. With regard to the specific humectants used in the
`treatment of tobacco, glycerine was the original humec
`tant used but other compounds used for this purpose
`include diethylene glycol, triethylene glycol, propylene
`glycol, butylene glycol and sorbitol.
`Apart from the question of where in the processing
`sequence, "top flavors' are applied to tobacco, the
`particular method for applying such additives is of pri
`mary concern. The method used must be capable of
`60
`applying the desired quantities of flavoring material to
`the tobacco as uniformly as possible. It is not surprising,
`therefore, that methods and apparatus for applying
`flavoring materials to tobacco have attracted consider
`able attention from those skilled in the art. For example,
`65
`recent improvements in application methods and appa
`ratus are disclosed in U.S. Pat. No. 4,054,145. The com
`plex arrangement described in that patent attests to the
`
`4,449,541
`2
`difficulties in achieving uniform application of flavoring
`additives to tobacco.
`-
`Perhaps the best known and most widely accepted
`"top flavor' applied to tobacco is menthol. Menthol is
`most often applied in the form of a dilute alcoholic
`solution using a rotating cylinder similar to that shown
`in U.S. Pat. No. 4,054,145. Alcoholic solutions of men
`thol have also been applied to tobacco in a pneumatic
`system as described in U.S. Pat. Nos. 3,548,838 and
`3,678,939. In spite of its long history of use, the applica
`tion of alcoholic solutions of menthol to tobacco is not
`without its disadvantages. The use of alcohol as a car
`rier medium for menthol and other flavoring additives is
`both expensive and hazardous. Since the alcohol is nor
`mally not recovered following its removal from the
`treated tobacco by evaporation, it is necessary to em
`ploy venting procedures that will remove most of the
`alcohol and other volatile materials from the factory
`area where the tobacco is being treated. Not only do
`such venting procedures result in losses of menthol and
`other flavoring additives from the treated tobacco, they
`also require appropriate steps to prevent the formation
`of explosive mixtures of alcohol vapors and air. Thus,
`the alcohol-based flavor application systems incur the
`cost of the alcohol as well as operation and maintenance
`of equipment for controlling and removing alcohol
`vapors released into the factory processing area.
`The deficiencies associated with the application of
`menthol dissolved in alcohol have been recognized by
`those skilled in the art and have led to the development
`of methods and apparatus for overcoming these defi
`ciencies. One such method is disclosed in U.S. Pat. No.
`3,800,806 (Reissue No. 29,298)which describes a
`method for applying menthol and other flavorants to
`tobacco by exposing the tobacco to flavorant vapors
`under controlled conditions. This method avoids the
`use of solvents or other carriers and purports to over
`come the deficiencies of prior art processes based on the
`spray application of flavorant solutions. Although the
`teachings of this patent refer to the variations in flavor
`ant application levels which can occur in prior art pro
`cesses, no data are provided which would indicate that
`consistently uniform application levels result from the
`vaporized flavorant application process disclosed. In
`deed, it is stated that the factors affecting deposition of
`the vaporized flavorant on tobacco include the concen
`tration of flavorant vapor in the process stream, the
`contact time of flavorant vapor with tobacco, tempera
`ture of the air stream in the pneumatic conduit, velocity
`of air in the conduit, tobacco feed rate and tobacco
`temperature. In order to maintain the desired concen
`tration of flavorant vapor in the process stream, it is
`necessary to withdraw samples of the pneumatic stream
`flowing through the conduit for analysis so that addi
`tional flavorant can be injected into the process stream.
`It is apparent that the number of factors that must be
`precisely controlled in the process increase processing
`costs without providing any guarantee that variation in
`flavorant application levels will not occur due to inade
`quate control over one or more process parameters.
`Thus, the method disclosed in U.S. Pat. No. 3,800,806 is
`not entirely satisfactory.
`Another attempt to solve the problem of applying
`uniform quantities of flavorants such as menthol to
`tobacco is described in U.S. Pat. No. 3,817,258 and the
`corresponding U.K. patent specification No. 1,357,057.
`This patent discloses a method and apparatus for apply
`ing a flavorant solution to a shredded tobacco stream
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 003
`
`

`

`5
`
`10
`
`15
`
`20
`
`4,449,541
`3
`just before the tobacco is made into cigarettes. The
`teachings indicate that menthol dissolved in alcohol is
`sprayed, preferably in aerosol form, onto a moving
`layer of tobacco just before the tobacco layer is depos
`ited onto a moving web of cigarette paper on a cigarette
`making machine. Although the disclosed invention has
`certain attractive features, it has proven to be somewhat
`unsatisfactory when used with present-day high speed
`cigarette making machines. Some of the invention's
`drawbacks are discussed in U.K. patent application No.
`2,030,894 published in April 1980. The net result is that
`a completely satisfactory solution to the problem of
`applying uniform levels of flavorants to tobacco in an
`economical manner continues to elude those skilled in
`the art.
`In this review of background art, it should be noted
`that a number of references teach the use of solvents
`other than alcohol for applying menthol and other fla
`vorants to tobacco. For example, U.S. Pat. No.
`3,085,581 discloses a process for spraying cigar tobacco
`with a composition containing menthol, butylene glycol
`and water. U.S. Pat. No. 4,128,101 (Example IV) dis
`closes the treatment of tobacco with a 5 percent by
`weight solution of 3-ethoxy-4-hydroxy-benzaldehyde
`25
`2,2-dimethylpropanediol acetal in propylene glycol
`although it is evident from the teachings that solvent
`systems based on ethyl alcohol are preferred. In Ger
`man Pat. No. 1,065,767, tobacco is treated with solu
`30
`tions of menthol and certain menthol esters in solvents
`such as diethylene glycol, 1,3-butylene glycol and iso
`propyl alcohol. Other references could be cited which
`teach the use of glycols as solvents for flavoring addi
`tives but such teachings are usually found in connection
`35
`with casing compositions which are based largely on
`flavorants of low volatility. In spite of the numerous
`teachings relating to the addition of flavorant additives,
`there is an apparent lack of recognition among those
`skilled in the art as to how relatively volatile flavor
`40
`additives may be applied to tobacco without the use of
`costly volatile solvents and/or apparatus for incorpo
`rating volatile flavorants into tobacco products.
`BRIEF SUMMARY OF THE INVENTION
`45
`This invention provides a method for incorporating a
`volatile flavoring additive into cut, shredded or other
`wise comminuted tobacco in connection with the manu
`facture of tobacco products.
`50
`It is a principal object of this invention to provide a
`method for applying a volatile flavoring additive to cut,
`shredded or otherwise comminuted tobacco which
`avoids the use of solvents with low boiling points as a
`carrier medium for the flavoring additive.
`55
`It is a further object of this invention to provide a
`method for continuously applying uniform amounts of a
`flavoring additive and a humectant material to a moving
`stream of cut or shredded tobacco.
`Further objects of this invention include a reduction
`in evaporative losses of a volatile flavoring additive
`from treated tobacco and an overall reduction in the
`release of potential air pollutants from the treatment of
`tobacco with a volatile flavoring additive when com
`pared with prior art methods based on flavorant carrier
`65
`solvents having low boiling points.
`Other objects and advantages of the invention will be
`apparent from the detailed description which follows.
`
`4.
`DETAILED DESCRIPTION OF THE
`INVENTION
`In the conventional processing of cured tobacco des
`tined for use in consumer products such as cigarettes
`and pipe smoking tobacco, tobacco strips (i.e., pieces of
`tobacco leaflamina having stems and midribs removed
`therefrom) are treated with casing materials before
`further processing. The casing materials are essentially
`aqueous solutions of sugars and humectants which are
`applied to the cased strips prior to or in conjunction
`with a heating treatment to seal the casing in the leaf
`and to carmelize the added sugars. The treated tobacco
`strips are cut or shredded while still moist to give parti
`cle sizes of desired dimensions and the cut or shredded
`tobacco is again heated to reduce moisture levels. The
`dried and cooled cut tobacco is normally treated with
`an alcoholic solution of relatively volatile top flavors to
`impart desired flavors notes and aroma to the tobacco.
`The alcohol is allowed to evaporate from the treated
`tobacco before the tobacco is incorporated into smok
`ing tobacco products.
`This invention is based on the discovery that the
`quantities of humectants used in the casing materials
`applied to tobacco strips can be reduced substantially
`without apparent adverse effects on the tobacco during
`the subsequent processing steps and that the quantities
`of humectants withheld from the casing materials can
`instead be used as a vehicle or carrier for the top flavors
`applied to the cut or shredded tobacco. The net result is
`that the final humectant levels applied to the tobacco
`are essentially unchanged while the alcohol previously
`used for applying the volatile flavoring additives is no
`longer needed. Not only is there a substantial economic
`benefit realized by eliminating the cost of the alcohol
`carrier for the top flavors but a source of air pollution
`(i.e., the evaporating alcohol) is also eliminated.
`The humectants which may be used in carrying out
`the process of this invention are those which are nor
`mally liquid at the processing temperatures employed.
`Those humectants which are preferred carriers include
`polyhydric alcohols such as propylene glycol, dipropyl
`ene glycol, trimethylene glycol, diethyleneglycol, trie
`thyleneglycol, glycerol, a-methylglycerol and 1,2-,
`1,3-, 1,4- and 2,3-butanediols. Propylene glycol and
`glycerol are particularly preferred as humectant/sol
`vent agents since they are already widely used as to
`bacco humectants.
`Humectants which are normally in the solid state at
`ambient temperatures (e.g., sorbitol) may also be used
`with this invention provided that the volatility of the
`flavoring additives incorporated therein and the operat
`ing temperatures employed do not lead to unacceptable
`losses of flavoring additives due to evaporation. In
`order to avoid excessively high operating temperatures,
`it is desirable to include one or more additional humec
`tants and/or water in the carrier medium with the solid
`humectant. This will ensure that the medium is main
`tained in the liquid state at operating temperatures that
`are somewhat lower than would otherwise be the case.
`A variety of flavoring additives may be applied to the
`tobacco by using a humectant as the carrier for the
`additives. Examples of flavoring additives commonly
`used in the tobacco industry are menthol, anethole,
`cinnamaldehyde, vanillin, ethyl vanillin, peppermint oil
`and spearmint oil. Other examples of tobacco flavoring
`additives may be found in a compilation published in
`World Tobacco 59, pages 89-91 (January 1978). The
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 004
`
`

`

`10
`
`15
`
`4,449,541
`5
`6
`flavoring additives preferably included in the humec
`tionally been used as flavorant carriers, it is necessary to
`tant carrier are those additives which are volatile. For
`employ spray nozzles which are capable of accommo
`the purposes of this invention, volatile flavoring addi
`dating the viscosities and relatively low flow rates in
`tives are defined as those additives which readily distil
`volved. Spray nozzles which are effective for this pur
`at atmospheric pressure without appreciable decompo
`pose include the gas- or air-atomizing type nozzles
`sition or which are volatile with steam. In contrast to
`which emit an aerosol spray that is very suitable. Such
`the volatility of the preferred additives, the sugars used
`nozzles may generate the aerosol spray by mixing the
`in casing compositions are not distillable at atmospheric
`compressed gas or air with the liquid medium either
`pressure nor are they volatile with steam.
`internally or externally to the nozzle from which the
`The composition of the flavoring additive/humectant
`liquid medium emerges. Gas-atomizing spray nozzles
`carrier system applied to the tobacco will depend on
`are also amenable to use with heated flavoring ad
`various factors including (a) the desired final humectant
`ditive/humectant carrier systems in that a heated gas
`level in the treated tobacco, (b) the desired final concen
`may be used to effect atomization of the additives. Al
`tration of flavoring additive or additives in the treated
`though other types of spray nozzles such as hydraulic
`tobacco and (c) the solubility or miscibility of the fla
`pressure type nozzles will accommodate the liquid
`voring additive(s) in the humectant carrier under the
`humectant/flavorant systems, such nozzles give less
`process conditions used. The normal use levels of hu
`satisfactory results as far as uniform distribution of the
`mectants in tobacco products are sufficiently high so
`additives throughout the tobacco mass is concerned.
`that no particular problems are encountered in achiev
`Another important consideration is the nature of the
`ing the desired concentration of flavoring additives.
`moving tobacco stream as it moves through the treating
`20
`The World Tobacco reference mentioned above, for
`zone. The tobacco stream should be sufficiently spread
`example, recommends maximum weight percentages
`out or dispersed to expose as many tobacco particles as
`(based on dry weight of tobacco) of 3.0, 10.0 and 6.0
`possible to the droplets of liquid emerging from the
`percent of 1,3-butanediol, glycerol and propylene gly
`spray nozzles. The temperature of the tobacco at the
`col, respectively. For certain flavoring additives and
`time it is contacted with the spray should be such that
`25
`appreciable loss of flavoring additives due to evapora
`humectants which are in the solid state at ambient tem
`peratures it may be necessary to heat the mixture when
`tion is avoided. This is particularly true when a heated
`preparing and applying the additive/carrier system.
`flavoring additive/humectant carrier system is being
`Depending on the degree of volatility of the particular
`applied to the tobacco. It is preferred that the tobacco
`flavoring additive(s) being applied, the additive/carrier
`be agitated as it moves through the treating zone to
`system may be heated to temperatures of 30 to 100° C.
`improve exposure of the individual particles of tobacco
`at the time of application to the tobacco in order to
`to the spray droplets. At least one spray nozzle and
`maintain a homogeneous, liquid system. It is obvious
`preferably two or more spray nozzles are located in the
`that two or more humectants may also be used in com
`treating zone. The number of nozzles, their location and
`bination to prepare the flavoring additive/humectant
`their orientation with respect to the moving stream of
`35
`carrier system. The incorporation of suitable emulsifiers
`tobacco will be largely determined by the design of the
`may also be necessary with some systems. Regardless of
`apparatus being used and the tobacco flow rate capacity
`the techniques used in preparing the flavoring ad
`of the apparatus. These factors are appreciated by those
`ditive/humectant carrier systems, it is essential that
`skilled in the art and the particular arrangement that is
`they be completely homogeneous under the application
`most suitable can be determined with a minimum of
`experimentation. For example, apparatus involving a
`conditions employed so that the additive(s) and humec
`rotating cylinder of the type disclosed in U.S. Pat. Nos.
`tant(s) can be applied to the tobacco at consistently
`uniform levels.
`3,419,015 and 4,054,145 has been found to be effective in
`When menthol is used as the flavoring additive, it is
`the practice of this invention provided that the specific
`preferred that the polyhydric alcohol selected as the
`teachings contained herein are observed. Vertically
`45
`carrier be one that is capable of dissolving appreciable
`disposed treating chambers of the general type dis
`quantities of menthol. This is particularly true where
`closed in U.S. Pat. No. 3,742,961 may also be used with
`the treated tobacco is to be used for manufacturing
`modifications in accordance with the present teachings.
`tobacco products containing relatively high levels of
`Other apparatus designs may also be adapted for use
`menthol. The use of higher menthol concentrations in
`with this invention.
`50
`the humectant carrier makes it possible to avoid exces
`The manner in which the flow rate of the liquid
`sive levels of humectant in such treated tobacco. Ac
`humectant/flavorant system to the treating zone is con
`cordingly, it is preferred that menthol concentrations in
`trolled with respect to the stream of tobacco moving
`the humectant carrier medium be at least 20 percent or,
`through the zone is crucial to the application of uniform
`more preferred, at least 35 percent or, most preferred, at
`levels of humectant/flavorant additives to the tobacco
`55
`least 50 percent by weight based on the total weight of
`being treated. Although the prior art recognizes the
`the menthol/carrier system. When propylene glycol,
`need to control carefully with respect to each other the
`for example, is used as the carrier, it is possible to em
`flow rates of the liquid and tobacco streams, the de
`ploy menthol concentrations of up to 80 percent by
`mands placed on devices for controlling the process
`weight or more in the menthol/propylene glycol sys
`streams are considerably less stringent with relatively
`dilute alcoholic solutions of flavoring additives as com
`tem.
`The manner in which the flavoring additive/humect
`pared with the humectant/flavorant systems used in the
`ant carrier system is applied to the tobacco is a very
`present invention. Since it is desirable to avoid exces
`important consideration if the additive is to be distrib
`sive levels of humectants in the treated tobacco, the
`uted uniformly throughout the tobacco. Since the hu
`present invention must achieve uniform distribution of
`65
`mectants preferred for use with this invention are rela
`flavoring additives with relatively small quantities of
`tively high boiling, viscous liquids as compared to sol
`humectants. It is preferred that the humectant/flavo
`vents such as ethanol and propanol which have tradi
`rant flow rate be regulated by a mass flow meter and
`
`30
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 005
`
`

`

`4,449,541
`8
`7
`air-atomizing spray nozzles equally spaced along a 1.3
`associated control valve means because mass flow me
`meter length of stainless steel pipe positioned within the
`ters are capable of accurate measurement even at low
`cylinder parallel to but slightly above the longitudinal
`flow rates. Mass flow meters are commercially available
`axis of the cylinder. The spray nozzles were oriented so
`and one such meter is described, for example, in U.S.
`that the spray was directed onto the tobacco as it was
`Pat. No. 4,109,524. Other types of flow meters such as
`falling from the flights attached to the inside surface of
`those based on regenerative sonics, magnetic or turbine
`the rotating cylinder. A Proctor & Schwartz continu
`flow principles may also be used provided that humec
`ous weighing conveyor was used to introduce a stream
`tant/flavorant flow rates are used which permit accu
`of cut tobacco into the rotating cylinder and a Model
`rate measurements. The continuous weighing devices
`B-12 mass flow meter available from Micro Motion
`for measuring the quantity of tobacco being introduced
`Incorporated of Boulder, Colo. was employed to mea
`into the treating zone are well known in the art and
`sure the flow rate of the flavorant solution. The flavor
`require no separate description here. It is, of course,
`ant solution flow rate was controlled by a TY78S con
`necessary to provide such weighing devices with means
`trol valve obtained from Badger Meter, Inc., of Tulsa,
`for generating signals which indicate the tobacco feed
`Okla. and the ratio controller was a Model No. 57-Z
`rate at any given instant. The tobacco feed rate signals
`pneumatic ratio controller supplied by Foxboro Instru
`and the humectant/flavorant flow rate signals are trans
`ments Company of Foxboro, Mass. The flavorant mix
`mitted to a ratio controller which compares the signals
`ture was dissolved in the solvent medium to give the
`and regulates the control valve through which the
`desired final flavorant concentration. Cut tobacco was
`humectant/flavorant stream is introduced into the treat
`introduced into the rotating cylinder at the rate of 5,900
`ing zone. Both pneumatic and electronic ratio control
`20
`kilograms per hour and the ratio controller was set to
`lers are satisfactory for this purpose.
`deliver the desired quantity of flavorant mixture per
`A better understanding of the present invention is
`kilogram of tobacco. Air pressure in the head space of
`provided by referring to the drawing which illustrates
`the flavorant supply tank was maintained at 3922 g/cm2
`in block diagrammatic form a preferred embodiment.
`(gauge) and the air pressure supplied to the air-atomiz
`Cut tobacco is continuously introduced into tobacco
`25
`ing spray nozzles in the cylinder was maintained at 844
`treating chamber 12 via continuous tobacco weighing
`g/cm2 (gauge). Treated tobacco withdrawn from the
`conveyor 11 which is provided with means for transmit
`rotating cylinder was collected in containers and al
`ting data on tobacco feed rates to ratio controller 15.
`lowed to stand at room temperature for 24 hours. Rep
`Supply tank 13 containing the humectant with a prede
`resentative samples were randomly taken from the con
`termined concentration of flavorant(s) therein is pro
`30
`tainers for flavorant analyses. The results are shown in
`vided with sufficient air pressure from supply source 16
`via pressure control valve 17 to assure adequate flow of
`Table 1 below.
`For comparison purposes experimental data were
`the humectant/flavorant fluid through flow meter 14
`also obtained for tobacco treated with alcoholic solu
`and control valve 18 to the air-atomizing spray nozzles
`tions of flavorants using an arrangement which was the
`in the tobacco treating chamber 12. Flow meter 14 is
`35
`same as that described above except that the rotating
`provided with means for transmitting fluid flow rate
`cylinder was provided with six hydraulic pressure type
`data to ratio controller 15. Ratio controller 15 is ad
`spray nozzles instead of the air-atomizing type spray
`justed to give the desired humectant/flavorant to to
`nozzles and associated air pressure supply. Also, the
`bacco flow ratio. This ratio is continuously regulated by
`flow meter used for measuring the flow rate of the
`control valve 18 which responds to signals from ratio
`40
`alcoholic solution was a 2800 series magnetic flow
`controller 15. Air pressure supply 19 and pressure con
`meter supplied by Foxboro Instruments Company of
`trol valve 20 provide air pressure to the air-atomizing
`Foxboro, Mass. The data for treatment of tobacco with
`spray nozzles in treating chamber 12.
`Using a tobacco treating arrangement similar to that
`alcoholic solutions of flavorants are also shown in Table
`depicted in the drawing, a flavorant mixture containing 45 1 below.
`TABLE 1.
`TREATMENT OF TOBACCO WITH FLAVORANTS
`Flavorant
`Grams of
`Calculated
`Concentration
`Flavorant Medium
`Flavorant
`in Medium
`Applied per Kg.
`Level in Treated
`(% by Weight)
`of Tobacco
`Tobacco (% by Wt.)
`37.8
`8.60
`0.325
`
`Solvent
`Favorant
`Used for
`Being
`Flavorant
`Monitored
`Medium
`Propylene Menthol
`Glycol
`Menthol
`Ethanol
`Propylene Menthol
`Glycol
`Menthol
`Ethanol
`Propylene Coumarin
`Glycol
`0.00054
`0.0033
`16
`0.0030
`14.30
`0.21
`Coumarin
`Ethanol
`Flavorant medium was applied through Spray Set-Up 1/4J 13 303 stainless steel air-atomizing spray nozzles obtained from Spraying Systems Company of Wheaton,
`Illinois.
`Flavorant medium was applied through Spray Set-Up 1/4J 13A 303 stainless steel air-atomizing spray nozzles obtained from Spraying Systems Company of Wheaton,
`Illinois.
`It is apparent from the data shown in Table 1 that the
`either menthol or coumarin was applied to cut cigarette
`filler tobacco. This treating arrangement employed a 65 humectant-based flavorant media can be applied to
`tobacco at desired flavorant levels and that the unifor
`conventional rotating cylinder of the type disclosed in
`mity of such flavorant levels is superior to that obtained
`U.S. Pat. No. 3,419,015. The cylinder was approxi
`with alcohol-based flavorant media. Although propy
`mately 2.4 meters in length and it was provided with six
`
`10
`
`15
`
`6.8
`37.8
`
`16.8
`0.67
`
`19.37
`8.60
`
`19.37
`448th
`
`Measured Flavorant Level
`in Treated Tobacco
`Average Level
`Samples
`Analyzed (% by Weight)
`12
`0.30
`
`Standard
`Deviation
`0.06
`
`0.325
`0.325
`
`0.325
`0.0030
`
`12
`16
`
`16
`16
`
`0.31
`0.29
`
`0.32
`0.0035
`
`0.030
`0.019
`
`0.024
`0.00025
`
`Philip Morris Products, S.A.
`Exhibit 1031
`Page 006
`
`

`

`10
`
`15
`
`EXAMPLE 2
`20
`A tobacco treating arrangement similar to that shown
`in the drawing is used to apply a solution of vanillin in
`glycerol to cut pipe smoking tobacco. A glycerol solu
`tion containing 3.0 percent by weight vanillin is sprayed
`onto a moving stream of cut tobacco through six air
`25
`atomizing spray nozzles at the rate of 25 grams of vanil
`lin/glycerol solution per kilogram of tobacco. The
`treated tobacco emerging from the tobacco treating
`chamber contains approximately 0.072 percent by
`weight vanillin uniformly distributed throughout the
`30
`tobacco mass.
`
`4,449,541
`10
`approximately 0.038 percent by weight ethyl vanillin
`lene glycol is preferred as both the humectant and as a
`uniformly distributed throughout the tobacco mass.
`carrier for the flavoring additives, other humectant/-
`flavorant combinations may be employed as described
`EXAMPLE 6
`in the following examples.
`A tobacco treating arrangement similar to that shown
`EXAMPLE 1.
`in the drawing is used to apply a solution of menthol in
`propylene glycol to cut cigarette filler tobacco. The
`A tobacco treating arrangement similar to that shown
`tobacco treating chamber comprises a vertical tower
`in the drawing is used to apply a solution of coumarin in
`having a rectangular cross section 61 cm. by 46 cm. and
`glycerol to cut cigarette filler tobacco. A glycerol solu
`provided with nine adjustable baffles measuring about
`tion containing 0.70 percent by weight coumarin is
`48 cm. by 46 cm. hingedly attached to two opposing
`sprayed onto a moving stream of cut tobacco through
`walls of the tower in alternating fashion vertically
`six air-atomizing spray nozzles at the rate of 4.30 grams
`spaced approximately 23 cm. apart. The hingedly at
`of coumarin/glycerol solution per kilogram of tobacco.
`tached baffles are adjusted to slope downwardly
`The treated tobacco emerging from the tobacco treat
`toward the center of the tower at an angle of about 31'
`ing chamber contains approximately 0.0030 percent by
`with respect to the side wall of the