CA1061530A - TOBACCO PRODUCT CONTAINING A THERMO-GELABLE .beta.-1,3-GLUCAN-TYPE POLYSACCHARIDE - Google Patents

Abstract

Tobacco Product Containing a Thermo-gelable .beta.-1,3-glucan-type polysaccharide Abstract of the Disclosure A tobacco product, which is produced by incorporating in smoking material a thermo-gelable .beta.-1,3-glucan-type polysaccharide, either as the sole smoking material or as its partial replacement, has improved smoking characteristics such as flavor, taste and irritability, and its smoking material has improved physical properties such as thickness, wet-proof qualities, tensile strength, elongation and filling capacity.

Description

~a~6~30 ~ his invention relates to a tobacco product which comprises incorporating in smoking material a thermo-gelable ~-193-glucan-type polysaccharide, either as the sole smoking material or as its partial replacement.
It is an object o~ this inven-tion to provide a tobacco product with improved smoking characteristics.
Another objec-t is to provide an unusually superior binding agent for reconstituted tobacco, synthetic tobacco, etc. Still another object of this invention is to provide a tobacco substitute with less irritative or less unpléasant odor and with improved organoleptic properties and to produce a tobacco substitu-te having batter physical properties and improved processing characters relative to the known tobacco substitutes.
Further~ another object is to improve physical properties o~ tobacco leaves and thereby to e~fect savings in tobacco leaves~
O-ther objects will become clear hereinafter as the disclosure proceeds.
In -the context of this specification and the appended claims, the term "smoking material" means all kinds o~
smokable material including, among others, natural tobacco leaves such as burley9 '~urkish tobacco, Maryland tobacco, Virginia tobaoco, ~lue-cured tobacco and the like, tobacco originated material such as reconstituted tobacco 9 homogenized tobacco, tissue culture tobacco, etc. and non-tobacco origi-nated material intended to replace natural tobacco leaves with various vegetable leaves such as lettuce, cabbage : `
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leaves, etc., cellulose derivatives such as carboxymethyl-cellulose9 methylcellulose9 etc.9 starch derivatives such as carboxymethylstarch9 carboxyethylstarch9 etc.9 and so on9 the term "tobacco produc-t" means all kinds ol smokable products including9 among others, cigarettes9 cigars and cigarillos, fine cut tobacco9 pipe tobacco and the like, which are made from said smoking material.
The tobacco substitute means any material being used substituting for natural tobacco leaves.
As additives for smoking ma-terial3 there have been employed such casing sources as saccharide9 e.g. sucrose, glucose, sorbitol, e-Gc . 9 and glycols~ e.g. glycerin, ethylene glycol, propylene glycol, 1,3-butylene glycol, etc.
and such flavorants as various essential oils.
The effects of casing sources are said to include improvements in smoking characteristics and in physical properties such as fragility, tenæile strength, moisture retention, yield~ etc. These casing sources still have many behaviors to be further improved.
Depending upon the variety of tobacco~ there are employed 9 in addi-tion to said additives, binders or spreader such as galactomannan gum, locust bean gum, carboxymethyl-cellulose, hydroxyethylcellulose, carboxymethylstarch, sodium alginate, sodium pectinate, etc.9 either singly or as a suitable mixture.
~ hese additives are~also used in conjunction with wst-proof agents such as glyoxal9 dialdehyde starch and so on. However, the use of these addi-tives, especialIy

- 2 -la6ls30 those binders or spreader9 wet-proof agents, etcO which are conventionally employed, has been limited to the necessary minimum because they are less desirable -than tobacco leaves in terms of flavor and other smoking characteristics.
~urthermore, so far9 tobacco produc-ts in various forms, e.g.
cigarettes, cigars and fine cut tobacco9 have all been produced employing naturally cultivated tobacco leaves as the smoking material and processing them by various means.
Recently, however9 in view of the change of smokers' or of the smokers' hygiene, the market for tobacco products with light taste grows. Complying with the demandg the development of tobacco substitutes which may be substi-tuted for all or a part of natural tobacco leaves is under rapid progress.
There has been known9 as the smoking material of tobacco substitute (burning material), cellulose derivativesy e g.
carboxymethylcellulose 9 carboxyethylcellulose 9 hydroxyethyl-cellulose 9 carboxymethylhydroxyethylcellulose, methylcellulose9 ethylcellulose and hydroxypropylcellulose, starch derivatives, e.g. starch9 carboxymethylstarch and carboxyethyls-tarch9 and so on~
These burning materials still have some properties to be improved from the viewpoints of their taste on smoking and burning behavior. Thus, it has been expected among industries of manufacturing tobacco substitute that a novel burning material be provided for the substitute for known burning ma~erials.
The present inventors made an in-tensive research into the flavor and taste, physical properties, processability .. . . . .

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and other pro~erties O:L tobacco product and found that a thermo-gelable ~-193-glucan-type polysaccharide (hereinafter referred -to as the polysaccharide~, which means a thermally gelable polysaccharide compo~ed predominantly of ~-193-glycosidic units9 has an excellent binding action as well as properties to improve the smoking characteristics~ e.g.
flavor, taste, irritability9 etc.g of tobacco product and to improve the physical properties o~ smoking ma-terial, for example its firmness, tensile strength9 elongation, filling capacity~ we-t-proof qualities9 flexibility, yield etc. and has desirable burning behaviors to give less tar and less hazardous substances, ~urther that -the polysaccharide can be used as tobacco substitute sheet without employing any other binding agent and wet-proof agent. trhis invention was completed on the basis of these findings.
As the polysaccharide that is to be employed according to this invention~ there are known those of vegetable origin9 microorganism origin and so on. Although these are all advantageously employable for the method of this invention~
those originated from microorganisms are rather easily availsble ones among them. ~or instance9 -there may be mentioned the polysaccharide elaborated by microorganisms belonging to the genus Alcaligenes and the pclysaccharide produced by microorganisms belonging to the genus Agro-bacterium. More par-ticularly3 there may be mentioned the polysaccharide produced by _lcali~enes faecalis var. mVxogenes lOC3K (Agricultural ~iological ahemistry Vol,30~ page~ 196 et seq. (1966) by Harada et al.9 hereinafter re~erred to as ~6153~

polysaccharide A~, the polysaccharide produced by the mutant NTK-u (I~0-131409 ATCC 21680~ of Al~ æ faecalis var.
myxogenes lOC3K (U.S Patent 3,754,9259 U.S. ~atent 39822,250) (hereina-fter referred to as polysaccharide ~9 the polysaccha-ride produced by ~E~k~ radiobacter (IF0-13127, ATC~
6466) or lts mutant U~l9 (I~0-131269 ATCC 21679) (U.~
Patent ~,7549925, U.S~ Patent 398229250) (hereinafter referred to as Polysaccharide C) and pachyman being a main ingredient of Poria cocos (Agr. Biol. Chem. Vol. 32, No.10, P.1261 (1968))9 and the likec ~ he polysaccharide may be used in either purified or crude preparation. As the crude preparation9 there may be employed a cultured broth itself of a microorganism produ-cible ~e polysaccharide, or a material obtained by removing cells of the microorganism from the cultured broth, or any of other crude materials in the various steps of the purifi-cation process of the above.
~ he characteristics and advantages of the polysaccha-ride as it is used as additives to smoking material include the following.
An advantage is that the smoking characteristics are improved. Wnile addition of the polysaccharide to the con-ventional smoking material improves their smoking charac-teristics, the use of the pol~saccharide in lieu of the conventional additive or additives resultæ in considerably ameliorated smoking characteristics~ This is presumably because the polysaccharide yields less offensive odors and less irritant py~olyzates upon pyrolDsis and combustion and9 ~6116~53~) in addition, the afoYementioned ameliorated physical properties are apparen-bly responsible9 to a certain exten-t, for the improvements in smoking charac~teristics.
Another advantage is that the reductions in nicotine and tar cont;ents are accomplished~ These resul-ts are of necessity accomplished, partly because since the tobacco shreds in which the polysaccharide has been incorporated have an increased filling capacity, this capacity being further increased by the co-use o~ a puffing agent such as sodium bicarbonate and ammonium carbonate with the poly~
saccharide, and other improved physical characteristics, such a product is superior to ordinary tobacco shreds in firmness, assuming they are equal in packaged amount, with the result that i~ a tobacco product of a given firmness is the goal, the polysaccharide is instrumental in reducing the required amount of tobacco æhreds 9 and partly because the polysaccharide does not contain niCotine and produces a considerably less amount of tars than does the tobacco shreds.
Furthermore7 the polysaccharide is an excellent binder providing better binding and smo.king characteris-tics than do the hitherto-kno~m binders such as galactomannan gum9 locust bean gum, carboxymethylcellulose9 carboxymethylstarch9 sodium alginate9 ~odium pectinate and so on.
Currently carbo~ymethylcellulose is commonly e~ployed but this additive is undesirable in that it impartæ adhssi-vity to tobacco sheet under the wet condition in the produc-tion process as well as its unpleasant burning -~lavor.

.; ~, , , . ., . , . . - - .. , - , . . . .. .. ...... .

~ ~ 6~ S3~
In contrast, the polysaccharide is advantageous, process-wise7 in that it gives insoluble and unadhesive tobacco sheet in wa-ter9 which resul-ts in making -the pro-duction process easy and increasing yield of -the tobacco product~ In addition9 with the polysaccharide, the existing tobacco-manufacturing equipment can be utilized without modifications. When any of the aforementioned known binders is employed, it is necessary, for instance7 to use a wet~
proof agent such as glyoxal or dialdehyde starch in combina-tion with the binderO However, because the polysaccharide has both excellent binding and wet-proof properties~ a wet-proof a~ent are not neces~arily required. Although the polysaccharide may be used together with a suitable amount of any known binder~ even in -this case~ use of no wet-proof agent is necessarily required. ~astly, if the surface of a cigar wrapper and of paper, which is a material used in the manufacture of cigaret-tes and the like, is -treated with the polysaccharide 9 the surface texture is improved in smoothness and other qualities and, because of the resultant enhanced wet resistance, the dissipation of the odor, flavor and moisture fro~ the stuffer or ~iller smoking material is prevented and, accordingly, the staining of the wrapper is inhibited so that general deteriorations in the quality of tobacco product are prevented. Furthermore7 the excessive wetting of the tobacco product with saliva and the resultant discomfort of a smoker's lip touch are improved.
The method and stage of addition of the polyæaccha-ride are unlimited for practioal purposes.

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As for the manner in ~hich the polysaccharide is employed, -the powdery polysaccharicle as such may be employed or, alternatively9 lt may be previously caused to swell or made readily swellable.
The latter-mentioned condition is e~emplified by a dispersion of -the polysaccharide in water, aqueous alcohol, aqueous polyol, aqueous ammonia or -the like9 and a gelation product of the polysaccharide.
The dispersion is preferably in the concentration range of about 0~5 to 10 weight percent. The gelation product can be obtained -~or example 9 by preparing a dispersion containing O.5 to 10 weight percent of the polysaccharide, heating the dispersion under s-tirring to abou-t 55 to 78 degrees centi-grade and, theng promptly allowing it to stand and cool or, alternatively, hea-ting and allowing to stand the aforesaid dispersion at a temperature of about 65 to about 200C, preferably about 70 to about 150C~ Another alternative procedure comprises adding the polysaccharide to an aqueous -solution o~ alkali9 e~g. sodium hydroxide, potassium hydro-~ide or sodium carbonate9 of about O.lN to about ~N and9 then~ neutralizing the dispersion or adding9 ~or example, caloium hydroxide or calcium carbonate, thereto, followed by neutraliza-tion.
In these procedures, a porous gelation product can be obtained by add mg to the polysaccharide a puf~ing agent such as sodium bicarbonate and ammonium carbona-te.
The a~oremen-tioned gelation product can be processed by conventional manner into sheets or other optional shapes.

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The sheet like gelation product may be shredded into suitable size and to these shreds, further9 may be added with variou~ lavoring materials9 or the polysaccharide to which the flavoring materials were previously added may be gelled.
'~'he flavoring materials include any of those conven-tionally employable as the tobacco additive 9 i e. extracts such as tobacco extract and licorice extrac-t, menthol9 organic acid esters~ amino acids, proteins, essen-tial oils9 fruit flavors such as peach, walnut and cherry and so on.
While the amo~mt of the flavoring materials to be thus employed depends upon such fac-tors as uses, desired taste, etc., it is in general preferable to employ about 0~1 to about 10 percent baæed on the weight o~ the gelation product~
To the gelation product and the polysaccharide, further, may be added with a suitable amount of glow-promot-ing catalysts, materials to improve ash coherence and ~o on.
As glow-promoting catalysts for ensuring 1'fire-holdlng capacity", alkali metal compounds are preferred~
As material to improve the ash9 salts of ammonia, alkali metals or alkaIine earth metals can be used and o~
these salts of magnesium9 calcium or ammonium are preferred.
~ The addition of the polysacoharide may be effected either directly or in any other manner, e.g. by spraying.
The polysacoharide may be added to smoking material before, during or after proce3sing. For the manufacture o-~ sheet tobacco9 the polysaccharide may be added to a whole smoking material or, alternatively, a sheet-like , , : ~ - 9 - ~ ~

~196~53a~

gelation product of -the polysaccharide may be jointed to the sheet tobacco ~moking material. In the production of calus tobacco 9 t~le polysaccharide m~y be added before or after molding, or before or after drying and, then9 the blending may be performed. The polysaccharide may also be adcled in the course o~ manu~acture o~ pipe -tobacco and cigars9 or in such produc-ts. In the case of cigare-ttes, the poly-saccharide may also be used as coat~d on the wrapping paper for use in the making of cigarettes or as incorporated in the adhesive for fastening the paper.
~ hile the amoun-t of the polysaccharide to be -thus employed depends upon such factors as the type of tobacco products to be processed by the polysaccharide, uses, desired tastes9 etc., it is in many cases preferable to employ 0.1 to 30 percent by weight of the polysaccharide based on the weight of tobacco leaves or about 0.05 to about 25 percent by weight of the polysaccharide based on the weight of smoking material~ Particularly, it is in general pre~erable to employ about 0.1 to about 10 percent by ~eight of the poly~accharide for the purpose of the improvement of smoking characteristics, about 0.5 to about 15 percent by weight of the polysaccharide ~or the purpose of the improvement of physical properties and about 1 to about 30 percent by weight of the poly~accharide for the purpose of -the improve-ment of binding action and other properties of reconstitutea tobacco9 synthetic tobacco and so on~ which are in general mixed in other smoking~material at the rate of about 25 percent by weight based on the weight of whole smoking :

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material.
In case of the incorporation of wrapping leaves of cigars and wrapping papers of cigarettes, of tobacco ~ilters, etc., it rnay be preferable to employ about 30 to 200 grams per square meter of the polysaccharide dispersion of about 0.5 to about 10 percen-t by weight, by means of coating, spraying, etc. Furthermore, a tobacco substitu-te is produced by employing burning regulator and -the polysaccharide and is also used as a substi-tute for all or a part of smoking material.
The polysaccharide is employed as a substi-tute for all or a part of known burning materials. In this case9 it is advisable to use from 30 to 100 percent o~ polysaccharide in terms of its purified material relative to the -total amount of burning materials which may include the poly-saccharide used ~or the burning material.
As the burning regulator, there may be employed non- -burning and physiologically inactive inorganic compounds, e.g. oxide, hydro~ide, carbonate9 phosphate, sulfate, alumi-nate, silicate, aluminosilicate and so on of aIkali metals such as sodium and potassium, alkaline earth me-tals such as calcium and magnesium, and other me-tals such as zinc, alumi-nium9 iron, titanium and silicon. Further, there may be used natural inorganic compounds e.g. dolomite, bentonite, diatomaceous ear-th, magnecite9 perlite, vermiculite and asbeætos, and carbonaceous materials e.g. activated carbon.
aO far i-t has been known that, in the me-thod ~or the preparation of tobacco substitutes employing burning material and burning regulator, the objective produc-t can 5i3~

be obtained by shaping~ into sheet 9 thread or the like 9 a mixture of materials containing burnin~ material and burning regulator~ or by making burning regulator adhere to a burning material shaped into such a proper form as sheet or the like. In the method for the produc-tion of this -tobacco substitute, shaping of the burning material may be effected through availing the gelable behavior of the polysaccharide.
It may be possible to apply the manner of gelatlon of the polysaccharide E~ se which is described on page 8 9 to the means for the production of the tobacco substitute.
As examples of the practising features of this inven-tion, there may be processes of (a) spreading an aqueous slurry containing ~s polysaccharide and a burning regulator on a plate with smooth surface 9 followed by heating to be dried up and to make a sheet, (b) adding to an alkaline aqueous slurry containing the polysaccharide and a burning regulator ~t~ ~ water-soluble caloium salt, followed by shaping and thsn drying, (c) spreading an aqueous suspension containing the polysaccharide, so far kno~m burning material and burning regulator on a plate with smooth surface 9 followed by heating to be dried up and to make a sheet, (d) making into sheet or thread wet powdery particles containing the polysaccharide, burning regulator and comparatively small amount of ~Jate~ by the use of an e~truder or a roller, followed by drying up under heating, (e) shaping gel made from the polysaccharide together with an appropriate binder such as galactomannan gum, locust bean gUm9 carbogymethyl-cellulose, sodium arginate, sodium pectinate and so on~
' .

~ 6~ S3 and (f) other suitable manners.
The tobacco substitutes shaped in sheet or thread form are shredded into suitable si~e and shape in accordance with their objects in use.
The incorpora-ting ratio between the burning regulator and the combination of the burning material and the poly-saccharide is~ in the respective weight ratio, 90.10 to 1090, and preferably 70030 to 30~70~ ~urther9 to the tobacco substitute there may conveniently be added any of conveniently used additi~es such as perfumes, ma-terials to improve ash coherence, tobacco powder, nicotine (usually used in the form of sulfate or organic acid sal-ts), edible pigments and 90 on. As such perfumes, there may be tobacco extract, licorice extract, ~aint John's Bread extract~
Cacao extract, absolute honey wa~, menthol, vanilla extract~
organic acid esters, essential oils and so on. These addi--tives may be added before or after shaping of the tobacco substitute of this in~ention. r~hus, these may be added to the tobacco ~ubstitutes furnished. In the latter case9 the perfumes or the like is preferably added in the form of a suitable solutions or dilutions in an organic solvents such as ethanol.
The charac-teristics of the tobacco substi-tutes thus obtained is firstly remarkabl~ impro~ed physical properties.
Namely, the sheet -tobacco substitute composed of the polysaccha-ride does not dissolve in water and ~lves a little adhesi-vity, but shows e~cellent bindlng propertg when gelled, so that the physical properties of the tobacco substitutes of .

~L~63L530 this invention is remarkably impro~ed in firmness 7 elongation, tensile strength, and so on in comparison with so far known burning materials. This is easily understandable from the fact that there is a li-ttle bad smell and irritative pyrolg-zates on burning or on pyrolyzing 7 and from the fact that there is keen r~lationship between the abovementioned improved physical properties and improved smoking charac-teristics.
The following experimental data and working examples are intended merely to illustrate presently preferred embodi-ments of the present invention and not to restrict the scope of this invention.

Ex~eriment 1.5 g. o~ polysaccharide B was weijghed into a round-bottomed flask of 100 me. capacity, fitted with a condenser and pyrolyzed in a silicone bath maintained a-t 240-280~
for 2 hours~ The pyrolysate consisted of brownish tan po~ders, caramels and tarry components9 giving off a caramel odor, There was substantially no irritant odor like that commonly encountered upon pyrolysis of cellulose, carboxy-methylcellulose 9 galac-tomannan gum, carboxymethylcellulose 9 carboxymethylstarch and sodium alginate.

_ per_men-t 2 2 g. o~ polysaccharide B was weighed ou-t an a sufficient amount of deionized water was added to it -to make 100 m~.
~he mixture was homogenized in a mixer for 5 minu-tes~ rrhe resulting suspension was transferred onto a glass plate 5 mm . . ,. ,, . . - . . . . . . ..... . . .. .. .

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thick, r-iubjected to degassing and heated ab 100C for 5 hours to prepare a ~ilm. When igni-ted 9 the ~ilm burned with -the produc-tion of a flame and the smoke arising from it upon extinguishing had an caramel-like odor. '~his was in cont-rast with the odor irritating to the nostrils charac-terized by the lack of caramel-like odor which was e~perienced with the smoke arising upon extingushing a burning celluloce, carboxymethylcellulo.se, galactomannan gum, carboxymethyl~
starch9 or sodium algina-te, Experiment 3 The pyrolysate of the polysaccharide was analyzed with a pyrolytic gas chromatography. As controls, the pyrolysates o~ glucose9 which is the monomeric unit of the pol~rsaccharide, and cell~lose, which is the principal poly-saccharide occurring in tobacco leaves~ were also analyzed.
The conditions under which these samples ~ere pyrolyzed are as follows.
Pyrolyzer. Hit~chi Model KP-l ~lrnace temperatureO 500C
Heating time~i 20 seconds The condition~ o~ analysis of pyrolysates are as follows.
Gas chromatographic apparatus. Hitachi Model 063 Columno Dinonyl phthalate/Diasolid ~ ~(60-80 mesh~-300100i 3mm in dia~ x 3 m.
Temperature o~ column~ 8 minutes a-t 30C; thereafter~ the temperature was increased to 80C a-t the rate of 2C/
min.

~1~6~530 Carrier gasO LIelium9 30 m~./min.
Detectorq Hydrogen Ylame ioniza-tion detector The peak areas of the chromatogram oY each sample were computed by means of a digital integra-ter (Takeda Riken Model TR 22113~ The result was expressed as a percentage of the individual peak area relative to the sum total of areas of various gas components. Of the unidentified compo nents~ Xl with a large peak area is also ~hown.
~he~e results are set for-th in Table 1.

Table - __ample Percent of Pyrolyoates --____ Poly Pyrolysate \ saccharide Glucose Cellulose Acetaldehyde 7.6 8.1 15.0 Methanol 0.2 1.8 0.4 Isoprene 0.3 0.4 0.2 ~uran 2.2 1~9 4.0 Propionaldehyde lo 2 1.4 2.1 Acetone 10.7 10.1 19.9 Acrolein Xl 10.7 10.3 9.0 2-Methyl~ur~n 4.4 3.0 1~6 n-~utylaldehyde 0,8 0.9 0.9 Methyl ethyl ketone4.4 3.3 6.9 Diacetyl 3.7 3.7 4~7 Benzene 1.0 1.7 1.4 2,5-Dimethyl~uran 4.2 2.7 3.7 LS3~
~ample Percent of Pyrolyoates ~ Poly Pyrolysa-te \ saccharide Glucose Cellulose Crotonaldeh,yde2.3 2.9 4,0 Toluene 8.9 1~c2 2,8 Methane~ethane and other hydrocarbons 37-4 34.6 23.4 It is apparent from Table 1 that 9 compared with cellulose, polysaccharide B can be said to be low in acetal-dehyde, acetone and acrolein contents, and to be less irri-tating as to its pyrolysate. The results ~Eor poly~accharide A and polysaccharide ~ are substantially the same as the results obtained with polysaccharide B.
.._ ~ xperiment 4 IJnder the same conditions as those set forth in Experi-ment 3, there were obtained pyrograms of the polysaccharide and gl~lcose o~rer the pyrolytic temperature range o~ 200 to 500 degrees centigrade. The sum totals O:e peak areas are set forth in lrable 2.

Table 2 Temperature OIPeak areas pyrolysis (C) Polysaccharide Glucose ~ ____ 400 ~ 43544 g4319 1~6~30 Compared wi-th glucose 9 the polysaccharide i~ high in the tem~erature of pyroly~is and low in gaseous components~

Experim~
A blend of tobacco leaf fines of 60 g. of flue~cured tobacco~
25 g. o~ Japanese dom~stic tobacco and 15 g. of burley tobacco 9 and flavored tobacco stems (winnower debris) were comminuted to sizes not exceeding 100 mesh, ~ sheet pulp was also flavored and disintegrated in a turbo-mill~
70 g. of the blended tobacco powder was mixed with the powdered stem (winnower debris) 9 followed by the addition of 10 % (on a dry basis) of the pulp fiber as a reinforcement.
After thorough mixing, 5 C/Q each o~ sucrose and propylene glycol were added. Following the addition of 8 oiO of poly~
saccharide B, a sufficient volume of water was added to the mixture so that the water content of the mi~ture ~as about 40 CJo. The resulting wet powder was thoroughly homogenized and formed into a web on a press roll plant for tobacco sheet. The web was dried at 100C to obtain a reconstituted tobacco sheet with a moisture content of about 12 ~0.
Qn the other hand, as controls 9 the polysaccha~ide B
was replaced by (1) 4 ~ of carbo~ymethylcellulose and 4 %
o~ glyoxal, (2) 8 ~O of locu~t bean gum or (3) 4 % of sodium alginate and 4 % of glyoxal and the respective compositions were homogenized and processed in the same manner as above to prepare reconstituted tobacco samples~
Each of these samples was made into single-strand cigars and organoleptically tested twice by 10 panelists.
The total scores of two smoking tests are shown in , ~ 3 Table 3.

Tab Smoking characteristics \ Flavor Taste Irritability Sample ~
. ~
Control (1) 7 4 2 Product of this invention 13 16 la . ~
Control (2) 5 3 Product of this invention 15 17 19 Control (3) 6 4 2 Product of this invention 14 16 18 The scores on flavor and taste, respectively, mean the number o~ smokers who judged that the corresponding product was better9 the irritabilit~ score indicates the number of smokers who judged that the corresponding product was less irritant.

Experiment 6 The tobacco sheets prepared by the procedure set forth in Experiment 5 were measured for thickness, weigh-t per unit area, wet-proof timeJ tensile strength, elongation and filling capacity. The results are shown ln Table 4 .

- 19_ ' ~6~53 ~V
~ ,i a ri O ri O O O 0 r-i ~ ~ ~ ~ ~ N
r-l ~ ~ ~ ~
FT~ O bD r-l r-i rl ~i !~
ri .. ~ (~ C~ C~ N
1_~

r~ 1 r~ ~ ~ r-i O ~l O
V~ O 03 03 0~ N
f~ ~I bD~--j ~ r-j N
r~l ~ . .

~i 8 ~Q
~ ~ ~ U~ q I ~rl ~ N N N r-i ,i~ +~ _, ~i f~
h ~
N N L~
~) ~ ~ iX~ ~ CO N
~rJ ~r~ ~o 0 oo a) C~

~Q_ ~ ~ $ co ~ o C~ ~ O O O r~i ri ~
~3 O O O O
.
/ ~Ig E~ / O r ~ N ~ ~ ~
~Q 1 r j r j r i O ri E~ / r j O O O h ~-d o g g ,,~ ~
,/ ~2 V V V ~i :. .

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The procedures used for measuring the physical pro-perties of sheets are as follows.
1. Thickness lrhe thickness o~ each sheet was measured under a load of 550 g/cm2 on a thickness tes-ter (for paper) manufactured by Toyo Seiki K.K.
2. Weight per unit area (1) Usin~ a boring edge a disc 30 mm in diameter wa~ cut out from 30 sheets.
(2) All the 30 mm. samples were weighed together on an automatic scale with a sensitivity of 5 mg.
(3) The weight per unit area was calculated by means of the following equation.
1"000,000 x ~
Weight per unit area - ~~~~~ 2 ~-3.14x(15) x30 where, X is the weight (g.) of ~0 sheets . Wet~proof time (1) The sample was stored in a air conditioning room (20C, 60 ~0 RH) for 2 days.
(2) ~he conditioned sheet was punched with a 30 mm(diameter) cutter edge.
(3) A dish was filled with 150 m~ o~ water of 25C and 5 sheets, 30 mm in diameter, were placed in the dish without overlapping, For each test specimen, the tlme that had elapsed before two or more slits (throughout - the thickness) were produced was measured in minutes with a etop watch.
~he dish was given a slight vibration every 1 mi~ute.

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4. Tensile strength (1) Equipment 1) Constant ra-te of elongation apparatus (Toyo Seiki K.~.) with an integrater.
2) Sample cutter 3) Thickness gauge (2) Samples From among mois-ture controlled products (20C, 60 a~O
RE), more or less representative specimens free o~
creases, cracks or slits were selected.
In longitudinal and transverse directions, 15 sheets each were cut to a size of 70 x 15 mm~
(3) Procedure The test was performed in a chamber maintained at 20C
and 60 ~jO ~H~
Each specimen was loaded until it wa~ torn apart.
1~ Pulling speedi 10 mm/min.
2) The specimen was held taut in position~ The ef~ective length was 50 mm~
3) The thickness of each specimen was previousl~ measured.
(4) Computation and indication 1) Tensile load at break (g) The load required to break the specimen was read on the meter~
2) Ten~ile strength (g/mm2) The load required to break the specimen was expressed per unit area.

.

.~ :

~ O ~ ~3 3) Elongation ('~o) ~ he elonga-~ion at break was read on the me-ter and expressed as a percen-t of the leng-th of the specimen~

5. Filling capacity 1) The samples taken (200 g.) were stored spread in an air conditioning chamber (20C9 60 % RH) for 2 day~.
2) The conditioned samples were transversely aligned and cut to a width of 10 mm with a cutting edge.
3) The cut specimens were longitudinally aligned and shredded to a shredding width of Q.8 mm by means of a rotary shredder.
4) The conditioned samples were stored spread in a condi-tioning chamber(20C,60~oP.~1 ~or 2 days.
5~ The conditioned samples were weighed on an automatic scale with a sensitivity of 5 mg. and five sets of samples 15 g. each were taken.

6) ~y means of a instrument for the measurement of filling capacity each 15 g. specimen was tested for its bulk density (g./3~135 cm3) against a compression stress of 250 g./cm2.

7) ~or the remainder of specimen, their moisture contents were measured at two points with an Acme-type moisture tester (100C, 1 hour).

8) The mean a~erage of values of filling capacity were calculatedO

Experiment 7 With a cutting edge, 10 g~ o~ a film of poly3accharide obtained by the procedure set forth in Experiment 2 was - 2~ -~ ~ 6~ 53~

cut to a width of C~.5 to 1 mm and a length o-f 5 -to 15 mm.
The fllaments were blended with 10 gO of -tobacco shreds for commercial ci~arettes (I~ ite ~ manufactured by Japan Tobacco & Salt Public Corporation~ and, from this blend, cigarettes with a wrapping circumference of 25 mm and a length of 63 mm were fabricated using a manual test-cigarette wrapping equipmentO
Then, by the same procedure as that described above for films9 paper wrapped cigarettes were fabricated from the reconsitu-ted tobacco prepared using the polysaccharide B obtained in Experiment 5.
To each of these test cigarettes was attached an acetate filter with the same specifications as those of commercial cigarettes (Hi-~ite ~9 i.e. a length of 17 mm, a size of monofilament of 4 deniers and a total denier number of 43,000, and the tar and nicotine conten-ts of the smoke of each speci-men were measured in -the following manner.
A constant-flow automatic smoking machine was used to artificially smoke each cigarette specimen under the condi-tionsO flow rate 17.5 me./sec., smoking time 2 æec./puff7 pu~f frequency l/min. 9 and distance of combustion 5.0 cm.
The crude tar waæ trapped with an aerosol trap filter (Cambridge ~ilter CM-113) and the moisture measured by -the Earl-Fisher method was substracted from the value~ The result was taken as the tar content. After the steam diæ-tilla-tion of the crude ~ar, the nico-tine in it was determined by the absorbance method (Scientific Papers of the Central Research Institute of -the Japan Tobacco &Salt Public ~orpo--S3~

ration No.105, P.291, 1~63).
The results are set forth in Table 5O
Table 5 _ __ ~ength Weight Tar in Nicotine Sample smoke in smoke (mm) (mm/piece)(mg/piece)(mg/piece) Test cigaret,tes with 30 r/0 80 0.98~0.01 13~15 0.9-1.2 polysaccharide B
. ~
Test cigarettes with 50 %
recons-tituted 80 0.98~0.01 17 105 tobacco ba~ed on polysaccharide B
Controlo cigarettes 80 0.98~0.01 21 108 (Hi-~ite ~ 3 ....

It will be apparent from '~able 5 that in the tar and nicotine contents of smokes, the test cigarettes based on polysaccharide B are significantly less than the commercial cigarettes (Hi-~ite ~ ).

Exam~le 1 A mixture of 750 g. of the tobacco fines ~rom the tobacco manufacturing process and 250 g. of winnower debri~
was comminuted in a grinding~machine to a mesh size of 100 ~ To this powder were added 50 gO of poly~accharide B
ana 300 m~. of water -to prepare homogeneous wet granules.

The granules were ~ed to an extruder to obtaln pellets about ~ mm in dlameter and about 6 mm long. '~he pellets .

. , . .: , : . - . - . . , .. .. ~ : : , , . , :. ,.,, . . : , . . , : -.. : , , 6~530 were directly passed down over a pair of rollers -to prepare a reconstituted tobac~o consisting of sheet fragments measuring 0.1 mm in thickness, 2-3 cm in width and 5~8 cm in length. The surface speed ratio of the rollers was 1 1~3, with the surface speed of the higher-speed roller being 60 m/min. The roll temperature was 85~. The sheet scraped off with a doctor knife was in semidry condition. To adjust the moisture content of the sheet to about 12 jO~ the sheet was f'ed on a wire-net conveyer through a moisture control room. ~he resulting product was superior to the comparable product based on the sodium salt of carboxymethyl-cellulose in all the physical properties mentioned in Experi-ment 6.

xample 2 10 kg. of low-grade smoking flue-cured tobacco were crushed in a crushing machine to a size of about 10 mm2 and9 then, milled -to a powder in a mixer. ~o -this powder was added 3 kg. of polysaccharide B, followed by thorough mixing to obtain a mixed powder. To this mixed powder were added 0.55 kg. of propylene glycol9 0.65 kg. of sucrose and 26 ~. of water and the resulting homogeneous slurry was coated on a stainless steel belt which was, then, passed over a heater, whereupon the slurry became a gel. The gel was then dried to obtain a sheet tobacco with a thickness of 0.15 mm, a weight per unit area of 58 g/m2 and a moisture content of 12 ~o~
~ his sheet was superior to the comparable prior-art product based on hydro~yethylcellulose instead of poly-saccharide B in the physical propertles mentioned in Experl-.

~ 6~LS3~
ment 69 as well as in smoking characteristics~

Example 3 10 kg. of a mix-ture of fines, dust and winnower debris formed in the course of production in a tobacco plant was me-thanically milled to a powder~ to which ~ kg~ of purified a-cellulose and ~ kg. of polysaccharide B were added. The mixture was thoroughly blended to prepare a mixed powder.
To this mixed powder were added 0.5 kg. of propylene glycol~
0.5 kg. of sucrose and 13 ~. of water~ followed by thorough mixing to prepare a komogeneous wet granular product. This product was passed down over the rollers of a heat-rolling equipment maintained at a roll-surface temperature of 150C
to obtain a thin film. The film thus formed was detached with a doctor knife and transferred on a wirenet conveyer through a drying chamber and, then, a conditioning chamber to prepare a tobacco sheet with a moisture content of 15 /
This sheet product was superior to the comparable sheet based on locust bean gum instead of polysaccharide B
in smoking characteristics and in the physical properties mentioned in Experiment 6, EX~E~
To a solvent mixture of 4~ . of demineralized water and 100 g. of glycerin was added 4 g. of calcium carbonat~, followed by stirring. To this were added 1 kg~ of tobacco dust with a particle size o~ 50 to 200 ~ and 200 g. of polysaccharide B
and tke resul-ting mixture was kneaded to prepare a homoge-neous mixture. This slurry was coated on a stainless steel ~6~S3~

belt to a -thickness of about 2 mm. The slurry coating was caused to undergo gelation at 90C and, -then, dried in a hot current of air to a rnoisture content of' 10~15 Ijo~
The s-tainless steel belt was then further driven to transverse a cooling chamber9 wherehy -the sheet was cooled to 5-10C. The shee-t was detached from the belt with a doctor knife. The tensile strength of the resulting product sheet was comparable to tha-t of ordinary tobacco leaves9 it being difficult to disintegrate the sheet by crumpling in the palm.
It also had excellent smoking characteristics.

Example __ The procedure of Example 4 was repeated, excep-t that 1 kg. of tobacco dust was replaced with 200 g. of needle leaf tree pulp and 800 g. of tobacco dust to prepare a sheet product.
The tensile strength of this produc-t was almost comparable to that of ordinary leaf -tobacco9 it being difficult to disinte grate by crumpling in the palm.

Exam~
To 35 ~. of water was added 2 kg. of polysaccharide and the mix-ture was stirred well to the consistency of a slurry. To the slurry was poured 65 ~. of hot water -to prepare a suspension of 60-70C. The suspension was coated on a stainless steel belt at room temperature to a æmall thickness and allowed to undergo gelation ~n situo Over a continuous web of the wet polysaccharide B gel on the stain-less æteel belt, 40 g~/m2 of the tobacco dus-t described in Example 2 was dusted. ~hen, on the dusted surface was super-~ - 28 -' '.

imposed a separa-te wet polysaccharide B gel obtained in the same manner as Example 2, foliowed by drying and heat-sealing.
The procedure provided about 7 kg. of a tobacco sheet with a moisture content of 12 '~0. This shee-t was superior to the product based on 1 kg. of sodium alginate and 1 kg. of glyoxal instead of polysaccharide B in smoking characteristics and in the physical properties mentioned in Experiment 6.

Example 7 In 100 m~. of 1.4 70 aqueous ammonia was dissolved 4 g.
of polysaccharide A and the solution was promptly coated on a place where it was allowed to undergo gelation andy then9 dried at a temperature not exceeding 60C. When the moisture content of the film had dropped to 30 ~ or less9 4 g. of tobacco dust was evenly deposited over the surface o~ this semi-wet ~ilm. Then, the composition was heat-compressed at 150C for 5 minutes to obtain a tobacco sheet. rrhis product had excellent smoking characteristics.

Egample 8 500 m~0 o~ a 2 r/o aqueous suspen~ion of polysaccharide C was coated on a stainless s-teel belt to a thickness of about 1 mmc rrhen~ 100 g. of tobacco dust containing 3 '~ o~
powder~ polysaccharide C was dusted evenly over the polysaccha-ride C slurry coating on the stainless steel belt, followed by drying. r~he resul-ting tobacco sheet had exceptionally satisfactory smoking characteristics.

Exa~le 9 100 g~ of shredded tobacco for commercial cigarettes 1~)6~53~
(Hi-~ite ~ ) was sprayed with 5 m~. of distilled water and, then9 mixed with 2 g. o-f polysaccharide B powder. The result-ing mi~ture was placed in a dryer at 100C fcr 5 minutes and9 after spontaneous cooling9 wrapped in paper on a test cigarette-wrapplng equipmen-t to a length of 70 mm and a circumference of 25.7 mm. The resulting cigare-ttes were superior in firm-ness to the commercial cigarettes free of the polysaccharide.
These cigarettes also haA excellent smoking characteristics.

~xample 10 7.5 kg. portions of tobacco shreds for cigarettes were sprayed with 3 kg. of water and 3 yg. of a 2 ~o suspension of polysaccharide B9 respectively, whereby the tobacco shreds were impregnated with the additives. These treated tobacco shreds were dried by heated air flow in a drying chamber to adjust their moisture contentO
The resulting percent increases in bulk are as follows.

Amount required for 10 cigarette~ ncrease Untreated shreds 90 m~0 ~hreds treated with water 98 m~. +9 %

Shreds treated with polysacchariAe B 117 m~ 22 o/o The cigaret-tes obtained by wrapping -the tobacco shreds thus treated with polysaccharide B to a length o~ 76 mm and a circumference of 25,7 mm were superior to the cigarettes similarly fabricated from untreated shreds and water-trea-ted .- .: ~ . . . .. . ; . . .. . . . .. .

.,. :, . . , ~ , 6~53~

shreds, respec-tively, in terms of firmness and smoking characteristics ~xample _ 1 To a tobacco source composed of 1 kg30f sorbi-tol9 5 kg.
of sucrose9 1 ~. of tobacco extract (10 % concentration)9 2 kg. of 193-butylene glycol9 0.5 kg. of water-soluble flavor and 100 ~. of water was added 3 kg. of polysaccharide ~ and the resulting mixture was used to treat tobacco leaves at the rate of addition of 2 3 G/~ relative to the leaves in an atmos-phere of 100C for 5 minutes in a casing step of the tobacco manufacturing process. After spontaneous cooling, the tobacco was shreddedg dried and thereafter subjected to a flavoring step, a conditioning step, etc. The tobacco shreds thus treated were fabricated into cigarettes with a length of 70 mm and a circumference of 25.7 mm.
~ he resul-ting cigaret-tes were lower in specific gravity than the comparable products free of polysaccharide B, dis-playing excelIent smoking characteristics. Moreover, the tobacco of this example yielded a less amount of debris or rejects in the shredding operatlon, giving an improvement in yield.

Exam~le 12 ~ o 1 kg. of a tobacco leaf composition consisting of 30 % of flue-cured -tobacco, 10 % of burley tobacco9 30 o~v of Japanese domestic tobacco9 18 % o~ stems and 12 v,~ of rolled æheets was added a hot solution prepared~as follows~ ~huso 30 g. of a formulated flavorant made up of 30 % of gl~cerin~ 22 a~o of .

~L~61S3~

sucrose9 10 ~0 of sorbitol~ 5 ~ of licorice extract, 3 ~o of fruit extract and 30 ~0 of polysaccharide B was diluted with hot water to prepare a 20 Gjo solution.
The above procedure provided a homogeneous wet powdery product. ~his powder was processed in the same manner as ~xample 1 to obtain a tobacco product. This product displayed improvements ln smoking characteristics as well as in the physical proper-ties mentioned in Experiment 6.

Example 13 With -the addi-tion of 50 ~. of water, 100 g. of a blend of 60 ~0 of tobacco dust, 20 G/o of purified cellulose and 20 %
of polysaccharide ~ was mixed well in a mixer. The mixture was extr~ded from a manual screen-type extruder (6 r.p.m,) equipped with a plate having 8 mm. orifices and the extrudate was cut with the accessory cutter to a length of 7 mm.
The procedure provided a molded product with a moisture content of 38 %r The temperature of the composi-tion at the mixing and molding step was 20-30Co Then, the molded product was maintained under indirect heating with steam at 80C for 10 minutes, after which it was dried in a dryer with shelfs at an air-current temperature of 90C for 2 hours to prepare a tobacco molding with a mois~-ture con-tent o~ 9 ~O~ This product had excellent smoking characteristics.

The wrapper (Nambu leaves,~etc,) for ~orming the exterior layer of a cigar was coated with 50 g./square meter of a 2 ~o - ~2 -.. ~ : . - . .. . : .. . . .. .

S3~

suspension of polysaccharide B and dried in a current of air to a moisture conte~t o~ about 13 %. The cigars fabricated using this product were superior to the con~entional cigars in water-retention property, being less sticky to the lips and having excellent smoking characteristics.

Exam~le 15 To 20 g. of the pol~saccharide A were added 50 g. of powdery dolomite (CaMg(C03)2) and 30 g. of carboxymethyl-cellulose, followed by mixing sufficiently. To this mixture was added 350 m~. of water and the resulting mixture was muddled to prepare a slurry. The slurry was spreaded on a glass plate and, then, dried at 80C to prepare a sheet-like product with a weight per unit area of about 100 g/m2~ This sheet was cut to a width of about 0,8 mm and a length of about 10 mm~ to which were, then, added 1 m~O of tobacco extract (10 % concentration) and 0.3 m~. of licorice extract -to prepare tobacco substitute product.
On -the other hand, the above~mentioned procedure was repeated, except employing 20 g. of carboxymethylcellulose in place o~ 20 g. o~ the polysaccharide A, to prepare tobacco subs-titute produc-t.
The former was superior to the latter in the physical properties mentioned in Experiment 6, as well as in reducing undesirable odor arising from a smoking paper, irritant odor and specific odor or taste.
~ o -tobacco shreds for the commercial cigarettes (Hi-~ite ~J ) was added the aforementioned thredded tobacoo substi-tute product containing the polysaccharide A at the rate of 53~

20 percent by weight For an experimental use, the resul-ting mixture was prepared into cigare-ttes.
The cigare-ttes were mild in smoking flavor and tas-te and were respectively reduced at the rate of about 10 percent in tar content and abou-t 15 percent in nicotine content of smoke in comparison with the commercial cigarettes (Ei-lite~ )~

Exam~le 16 To 50 g. of -the polysaccharide A was mixed with 50 g.
of powdery dolomite.
To this mixture was added 350 m~. of water and the resulting mixture was muddled to prepare a slurry. The slurry was spreaded on a chromium plated brass plate and 7 then, dried at 80C' to prepare a sheet-like product with a weight per unit area of about 100 g/m2. This sheet was cut into a width of about 0.8 mm and a length of abou-t 10 mm9 to which are then added tobacco extract (10 ~0 concentration) and licorice extract of the same volume as example 15 to prepare tobacco substitute product 9 which was far superior to the ~obacco substitute product, prepared in the Example 15, comprising dolomite and carboxymethylcellulose in the physi~al properties mentioned in Experiment 6 as well as in reducing undesirable odor arising from a smoking papeP, irritant odor and specific odor or taste.

xample 17 Fifty grams of polysaccharide A was well mixed with 50 ~. of powdery dolomi-te, followed by addition of 350 m~.
of water to make the resulting mixture a slurry, The slurry i3~1 was spreaded on a chromium-plated brass board 9 and 9 then dried at 80C to prepare a sheet-like composition weighing about 100 g/m2. This shee-t was cut into pieces wi-th a wid-th of about 098 mm and a leng-th o~ about lO mm, ~o these pieces was added homogeneously a 50 ~0 e-thyl alcohol solu-tion contain-ing 1.0 g. of tobacco extract 9 O. 3 gO of licorice ex-tract and 0.3 g. o~ ~t~ John's Bread e~tract (manufactured and sold by Ogawa Koryo Co., ~td.) 9 the resulting mix-ture being used as a good tobacco substitute, On the other hand, to 50 g. of powdery dolomite was added 50 g. of powdery carboxymethylcellulose in place of poly-saccharide A and the mixture was processed and flavored in the same manner as above to prepare a control product.
The tobacco substitute was found to be superior to the control product in tensile strength, elongation and wet-proof qualities as shown in Table 6 and in smoking characte-ristics as shown in Table 7.

Table 6 Test Thickness Weight Wet- Tensile Elonga-tem per proof strength -tion Sampl ~ ~mm) area -time (g/m2) (min.) (g/mm) (%) Control 0,15103.0 1 127 2~8 Product of this ~ 0.1399.8 45 248 3.5 invention (The same measure methods as in Experiment 6 were emplo~ed~) ' ~6~530 Table 7 -Smoking ~ ristics Flavor Taste Irritability Sample ~

Control 8 6 Product of this invention 12 14 17 Each of these samples was tested twice by 10 panelists~
The scores on flavor and taste9respectively, mean the number of smokers who judged -that the corresponding product was be~ter9 the irri-tability score indicates the number of smokers who judged that the corresponding product was less irritant.

xample _18 Thirty grams of polysaccharide A was well mixed with 30 g. of powdery ferric oxide (Fe20~) and 40 g. of powdery carboxymethylcellulose, followed by addition of 400 m~ of water to make the resulting mixture a slurry. The slurry was spreaded on a glass plate 9 and, then dried a-t 80C to prepare a sheet-like composition weighing of about 100 g.jm2.
This sheet was cut into pieces with a width of about O,8 mm and a length of about 10 mm~ To these pieces was added homo-geneously 50 ~ ethyl alcohol solution containing 0.5 g. of tobacco extract and 0.5 g. of cocoa extract, the resulting mixture being used as a good tobacco substitute.
On the other hand~ 30 g. of powdery ~erric oxide and 70 g. o~ powdery carboxymethylcellulose are mixed and the :

~0~3~
mixture was processed and flavored in the samc manner as above solution a,s above to prepare a control product.
The tobacco subs-titute product was superior to the control product in smoking characteristics as shown in Table 8.

Smoking ~lavor Taste Irritability Sample ~

Control 7 9 Product of this invention 13 11 16 (The same test method as in ~xample 17 was employed.) Example 19 Sixty grams o~ polysaccharide A was well mi~ed with 40 gO
(A~2Q3 4SiO2H20), ~ollowed by addition of 350 m~ of water to make the resulting mixture a slurry~
The slurry was spreaded on a chromium-plated brass board, and, then dried at 80C to prepare a s~eet-like composition weighing about lOO g/m . This sheet was cut into pieces with a width of about 098 mm and a length o~ about 10 mm. To these pieces T~as added homogeneously a 50 ~o ethyl alcohol solution containing l.O g. of -tobacco extract, 0~3 g. of licorice ex-tract and 003 g. of ~t. John's Bread extract~ the resulting mixture being used as a good tobacco substitute~
On the other hand, to 40 g~ o~ powdery ben-tonite was .

, ., . . ., . . . , . . ~ - . , ., , , ~ , 53~
added 60 g. of powdery carboxymethylcellulose and -the mixture was processed and flavored in the same manner as above to prepare a control product.
rl'he tobacco substitute was superior -to the control product in smoking characteristics.

Example 20 To 60 ~. of refined and screened (opening 1 rnm pass) pulp (Needle fold bleached kraft pulp) were added 10 g o~
colloidal calcium carbonate and 30 g. of polysaccharide A9 followed by mixing. To this mixture was added 500 mQ. of water and the resulting mixture was muddled to prepare a slurry.
The slurry was spreaded on a chromium plated brass plate and, then, dried at 80C to prepare a sheet-like composition weigh-ing about 100 g,/m2~
To this sheet was added homogeneously a 50 % ethyl alcohol solution containing 1.0 g. o~ tobacco ex-trac-t 9 0.5 g.
of absolute honey wax and 0~2 g. of cocoa extract to prepare a sheet-like tobacco substitute~
On the other harld 7 60 g. of the above mentioned pulp were mixed with 10 g. of colloidal calcium carbonate and 30 g.
of carboxymethylcellulose. The resulting mixture was processed and flavored in the same manner as above to prepare a sheet-like tobacco substitute product (control).
~ The sheet-11ke tobacco substitute product was superior to the control produc-t in wet-proo~ qualities and smokin~
charao-teristics.~

, LS3~

E~ampla _ 60 g. of refined and screened (opening 1 mm pass) pulp (N.B.K.P) was impregnated with about 4 g. of a 6 v~O aqueous ammonium sulfamate solution and was heated at 200C for about 3 hours to prepare burnt black pulp powderO
To this black powder were added 10 g. of colloidal calcium carbonate, 20 g. of carboxymethylcellulose and 40 g.
of polysaccharide A7 follo~,7e~ by mixing r To this mix-ture was added 400 m~O of water and -the resulting mixture was muddled to prepare a slurry, followed by adding 1.5 g. of tobacco extract9 0~5 g. of dear tang extract (manufactured by Takasago-Koryo ~td. 9 Japan)~ 1.0 g. of fig extract (manu~actured by Hogyoku Koryo ~td., Japan) and 0.3 g~ of licorice extract.
The slurry was spreaded on a glass plate and~ then, dried at about 60C to prepare a sheet-like product weighing about 100 g/m2.
On the other hand, to the treated powdery pulp mentioned above were 10 g. of colloidal calciu~ carbonate and 60 g~ of carboxymethylcellulose. The resulting mixture was flavored and processed in -the same manner as above to prepare a product (control).
r~he sheet-like product was superior to the ^ontrol i~
smoking characteristics as shown in ~able 9 '~abla 9 _ _ Smokin~
character~ Flavor Taste Irritability \ is-tics ~amp ~

Control 4 3 8 in~ention 16 17 12 - 39 ~

~6~53~

(The same tes-t method as in Example 17 was employed), ~xample 22 -Twenty grams of powdery activated carbon for decolora--tion was well mixed wi-th 30 g. o~ p~lysaccharide B and 50 g.
of powdery carboxymethylcellulose, followed by addi-tion of 450 m~. of water -to make the resulting mixture a slurry.
The slurry was spreaded on a glass plate9 and9 then dried at 80C to prepare a sheet-like composition weighing about 100 g/m2. This sheet was cut into pieces wi-th a width o~
about 0.8 mm. and a length of about 10 mm. To these pieces was added homogeneously a 50 ~ ethyl alcohol solution contain-ing 1.0 g. of tobacco egtract, 0.3 g. of licorice extract and 0.3 g. of St. John's Bread extract, the resulting mixture being used as a good -tobacco substitute.
On the other hand, to 20 g. of powdery activated carbon for decoloration ~as added 80 g. of powdery carboxymethyl-cellulose and the mixture was processed and flavored in the same manner as above to prepare product (control)~
The tobacco substitute was superior to the control product in smoking characteristics as shown in Table 10.

I`able 10 Smoking _________characteristics ~lavor Taste Irritability Sample ~ ~ ~
Control 3 3 5 Product of this invention 17 17 15 (The same test method as in Example 17 was employed).
:
~ - 40 _ ~6~53~

_ample 23 To 30 g. of powdery dolomite were sufficiently mixed with 20 g. of ground residue obtained by evaporating 3 %
dispersion of polysaccharide A at 80C in an air bath to dryness, 20 g. of powdery polysaccharide A and 30 gO o~
powdery carboxymethylcellulose. To this mixture was 500 m~.
of water and the resulting mixture was muddled to prepare a slurry. The slurry was spreaded on a glass plate and, then, dried at 80C -to prepare a sheet-like product with a weight per unit area o~ about 100 g./m2. This sheet was cut into pieces with a width of about 0.8 mm and a length of about 10 mm, to which was homogeneously added 50 ~o ethyl alcohol con-taining 1.0 g. of tobacco extrac-t, 0.3 g. o~ licorice extract and 0.~ g. o~ St. John's Bread extract to prepare to~acco substitute product. On the other hand9 30 g. of powdery dolomite was mixed wi-th 70 g. of carboxymethylcellulose and -the mixture was processed and flavored in the same manner as above to prepare a control product.
The tobacco substitute product was superior to the control product in smokin~ characteristics as shown in Table 11.

Tabl Smoking haracteristics Flavor Taste Irritability ~ample ~
__ __ ____.
Control 8 7 5 Product of t~i~
invention 12 13 15 (The same test method as in Example 17 was employed) .. , - . ... ,. - - . .. - - - . . .. . . ~ .... .. - . . .. ... . .

-~L~6~530 Ex mple 24 20 g. of powdery activated carbon for decoloration was sufficiently mixed with 50 g. of powdery carboxymethyl-cellulose. To this mixture was added 300m~. of wa-ter and the resulting mixturs was muddled to prepare a slurry9 which was sufficiently mixed with a mixture comprising 20 g. o~ poly-saccharide A and 300 m~. of 1 % aqueous ammonia~
The resul-ting slurry was spreaded on a glass plate and, then dried at 100C -to prepare a sheet-like product with about 100 g./m2. This sheet was cut into a width of about 0.8 mm and a length of about 10 mm9 to which was, then, homo-geneously added 50 % ethyl alcohol solu-tion containing 1.0 gO
of tobacco extract, 0.3 g. of licorice ex-tract and 0.3 g of St. John's ~read extract to prepare a tobacco substitute~
On the other hand, to 20 g. of powdery activated carbon for decoloration was added 80 g. of powdery carboxymethyl-cellulose and the mixture was processed and flavored in the same manner as above to prepare a control product.
The tobacco subs-titute showed better smoking charac-teristics -than the control product as shown in Table 12 Table 12 ~moking characteristics ~lavor Taste Irritability eD.~
Control 7 7 3 Product of this 13 13 invention 17 ~The aame test method as in Example 17 was employed) .

i3~

Example 25 To 500 kg~ of culture broth~ in which concentration of polysaccharide B was about 4 /09 obtained by cul-tiva-ting the mutant NTK u (IFO 131409 ATCC 21680) of A~ Q faecalis var, m!yxogenes lOC3~ was poured 500 ~. of hot water and stirred vigorously to prepare a suspension of 60-70C. This suspen-sion was thinly coated on a stainless steel belt at room temperature and allowed to undergo gelation in situ, Over a continuous web o~ the wet polysaccharide B gel on the stainless steel bel-t, 40 g~/m2 of refined and screened (opening 1 mm pass) pulp (obtained by treatin~ 60 g, of N~
B.K.P. i~pregnated with about 4 g, of a 6 ~0 aqueous ammonium sulfamate solution a-t 200C for about 3 hours) was dusted and the obtained product was put in a heater (90C), allo~ed to gelatinize and, then, dried to prepare a shee-t-like product.

_ample 26 100 kga of culture broth9 in which concentration of polysaccharide C was about 2 ~9 obtained by cultivating A~ 3~ radiobacter (IFO 13127, ATCC 6466) was concent-rated by a centrifuge (5000 G) to prepare 450 kg. of concent-rated solu-tion containing polysaccharide C of abou-t 4 ~.
To the concentrated solution were added 20 kg. of powdery acti~ated carbon for decoloration and 50 kg. of powdery carboxymethylcellulose, followed by mixing suf~i-ciently~ to prepare a slurr,y. The slurr,y was spreaded on a stainless steel bel-t, gelatinized at 90C and, then, dried to prepare a sheet-like product9 -to which was homogeneously added a 50 % ethyl alcohol containing lo O kg. o-f tobacco 53lt3 extract, 0.5 kg. of absolute honey wax and 0.2 kg, of cocoa extract to a flavored sheet-like product.

~ 27 A 4 ~ culture broth of polysaccharide A obtained by cultivating ~ faecalis v r m~ nes lOC~K was concentrated by a centrifuge (5000 G~ to prepare 450 kg. o concentrated solution (solids about 7 8 ~jo)9 to which were added 20 kg. of powdery activated carbon for decoloration and 50 kg~ of powdery carboxymethylcellulose9 followed by mixing sufficiently, to prepare a slurry. r~he slurry was extruded from an extruder to prepare pellet-like products, which was passed down o~rer a roller at a rollsurface temperature of rrhus-obtained sheet-like fragments pieces were put in a fluid-type dryer and sprayed with a 50 % ethanol solution containing 1.0 kg. of tobacco extract, 0.3 kg. of licorice extract and 0O~ kg. of St. John's Bread ex-tract to prepare tobacco substitute.

Exam~le 28 r~O 1500 ~, of culture broth, in which concentration of polysaccharide B was about 4 ~, obtained by cultivating the mutant NTK-u (I~0 13140, ArrCc 21680) f ~ e~
faecalis v~ o~ lOC3~ was added 1500 ~ of & 4 ~0 aqueous sodium hydrogide solution to dissolve polysaccharide 3 and then, ~rom the resulting solution the cells was removed by~a centrifuge and, -then~ polysacoharide B was separated by neutralizing with a 4N-H~ solution to prepare 3280 ~. of ~ ~ 44-~6~L53~

1.75 ~/0 suspension of polysaccharide B (yieldO 95.5 %). As to the suspension, concentration by using centrifuge and dilution by adding wa-ter were repeated -to re ove soluble inorganic salts. '~he suspension was coated on a stainless steel belt, on which were9 -then~ coated the mixture comprising 100 kg. of refined and screened (opening 1 mm pass) pulp (N.
B.K.P) and 100 kg. of -the above-mentioned suspension9 followed by drying to prepare a sheet-like product~

Example 29 3280 ~ of suspension of polysaccharide B removed soluble inorganic salts in the same manner as ~xample 28 was concentrated with a centrifuge (8000 G) -to prepare 900 kg.
of 6.1 ~0 concentrated suspension of polysacchiaride B (yield 95.8 a~o)~ To 400 kg~ of t~e concentrated suspension was sufficiently mixed with 30 kg. of powdery ferric oxide (Fe203) and 40 kg. of powdery carboxymethylcellulose to prepare a slurry. The slurry was spreaded on a stainless steel belt, allowed to gelatinize at 90~C and then dried to prepare a sheet-like product. To the shee-t-like produc-t was added a 50 ~ ethanol solution containing 1 kg. of tobacco extract and 1 kg. of cocoa extract to prepare a flavored sheet-like product, Example 30 To 500 kg. of -the remaining concentrated suspension of polysaccharide ~ employed in Example 29 were added ~0 kg. of powdery Bukuryo (Poria COC09 ) and the burnt black pulp powder obtained by treating 60 kg~ of refined and screened (opening -~L~6~S30 1 mm pass) pulp impYe~1ated with 4 kg, of a 6 ,~ aqueovs ammonium sulfamate solution at 200C for abou-t 3 hours9 followed by mixing i~ufficiently to prepare a slurry. To the slurry were added 1.5 kg. of tobacco e~tract, 0~5 kg. o~
dear tang extract, loO kg. of fig extract and 0~ kg. of licorice extract. The resulting slurry was spreaded on a stainless steel belt and, then, dried at abou-t 60C to a sheet-like product. rrhe sheet-like product had no undesirable odor arising ~rom a smoking paper and excellent smoking characteristics.

Examl~le~_~
To 100 ~. of a 4 ~/o culture broth of polysaccharide A
obtained by cultivating ~ faecalis var. ~
lOC3K was added 100 ~. of a 4 % aqueous sodium hydroxide solution to dissolve polysaccharide A.
The solution was added dropwi~e through a nozzle of 1.5 mm~ in diameter into 2~-HC~ solution to prepare granules o~ polysaccharide A.
The granules were taken out and washed with water and then were passed down over a roller at a rollsurface tempera-ture of 150C to prepare sheet-like piecesc These sheet-llke pieces were put in a fluid-type d~er and sprayed with flavorants. Thus-obtained shee-t-like pieces were mild in smok~ng aroma and tastG and were suitable ~or smoking.

.

- ~6 -.

Claims (44)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS;

1. A process for producing a smoking material for a tobacco product, which comprises incorporating a thermo-gelable .beta.-1,3-glucan-type polysaccharide into the smoking material before, during or after forming it into the tobacco product.

2. The process according to claim 1, which the thermo-gelable .beta.-1,3-glucan-type polysaccharide to be incorporated is a crude prepara-tion.

3. The process according to claim 1, wherein the amount of the thermo-gelable .beta.-1,3-glucan-type polysaccharide to be incorporated is about 0.05 to about 25 percent by weight based on the weight of the smoking material.

4. The process according to claim 1, 2 or 3, wherein the incor-poration is made by spraying or coating a dispersion of about 0.5 to about 10 percent by weight of the thermo-gelable .beta.-1,3-glucan-type poly-saccharide onto the smoking material.

5. The process according to claim 1, 2 or 3, wherein the incor-poration is made by the addition of a gelation product made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the smoking material.

6. The process according to claim 1, 2 or 3, wherein the incor-poration is made by the addition of a sheet made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the smoking material.

7. The process according to claim 1, 2 or 3, wherein the incor-poration is made by the addition of shreds of a sheet made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the smoking material.

8. The process according to claim 1,2 or 3, wherein the incorporation is made by spraying or coating a dispersion of about 0.5 to 10 percent by weight of the thermo-gelable .beta.-1,3-glucan-type polysaccharide onto the wrapper of tobacco product.

9. A process for producing a tobacco substitute, which comprises incorporating burning regulator and a thermo-gelable .beta.-1,3-glucan-type polysaccharide in burning material.

10. The process according to claim 9, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide to be incorporated is a crude preparation.

11. The process according to claim 9, wherein the incorpo-rating ratio between the burning regulator and the combina-tion of the burning material and the thermo-gelable .beta.-1,3-glucan-type polysaccharide is, in the respective weight ratio, 90:10 to 10:90.

12, The process according to claim 9 or 10, wherein the amount of the thermo-gelable .beta.-1,3-glucan-type polysaccharide to be incorporated is from 30 to 100 percent by weight based on the weight of burning material.

13. The process according to claim 9 or 10 wherein the amount of the thermo-gelable .beta.-1,3-glucan-type polysaccharide to be incorporated is 100 percent by weight based on the weight of burning material.

14. The process according to claim 9, wherein the incorpo-ration is made by the addition of a gelation product made from the thermo gelable .beta.-1,3-glucan-type polysaccharide to the burning material.

15. The process according to claim 9, wherein the incorpo-ration is made by the addition of a sheet made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the burning material.

16. The process according to claim 15, wherein the incorpo-ration is made by the addition of shreds of the sheet made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the burning material.

17. The process according to claim 9, wherein the incorpo-ration is made by the addition of a thread made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the burning material.

18. The process according to claim 17, wherein the incorpo-ration is made by the addition of shreds of the thread made from the thermo-gelable .beta.-1,3-glucan-type polysaccharide to the burning material.

19. A tobacco product, which comprises smoking material and a thermo-gelable .beta.-1,3-glucan-type polysaccharide.

20. The tobacco product according to claim 19, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is a crude preparation.

21. The tobacco product according to claim 19 , wherein the amount of the thermo-gelable .beta.-1,3-glucan-type polysaccha-ride is about 0.05 to about 25 percent by weight based on the weight of the smoking material.

22. The tobacco product according to claim 19,20 or 21, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is in the form of a dispersion of about 0.5 to about 10 percent by weight.

23. The tobacco product according to claim 19, 20 or 21, wherein the thermo gelable .beta.-1,3-glucan-type polysaccharide is in the form of a dispersion of about 0.5 to about 10 percent by weight and is incorporated by spraying or coating.

24. The tobacco product according to claim 19, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is in the form of a gelation product.

25. The tobacco product according to claim 24, wherein the gelation product is a sheet.

26. The tobacco product according to claim 25, wherein the sheet is shreds of the sheet.

27. The tobacco product according to claim 19, 20 or 21, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is in the form of a gelation product containing flavorants of about 0.1 to about 10 percent based on the weight of the gelation product.

28. The tobacco product according to claim 19, 20 or 21, wherein the tobacco product is a tobacco having improved smoking characteristics comprising smoking material and about 0.1 to about 10 percent by weight of the smoking material of the thermo-gelable .beta.-1,3-glucan-type poly-saccharide.

29. The tobacco product according to claim 19, 20 or 21, wherein the tobacco product is a tobacco having improved physical properties comprising smoking material and about 0.5 to about 15 percent by weight based on the weight of the smoking material of the thermo-gelable .beta.-1,3-glucan-type polysaccharide.

30. The tobacco product according to claim 19, 20 or 21, wherein the tobacco product is a tobacco having improved binding action and properties comprising smoking material and about 1 to about 30 percent by weight based on the weight of the smoking material of the thermo-gelable .beta.-1,3-glucan-type polysaccharide.

31. The tobacco product according to claim 19, 20 or 21, wherein the tobacco product is a tobacco product incorporated in the surface of tobacco product with a dispersion of about 0.5 to about 10 percent by weight of the thermo-gelable .beta.-1,3-glucan-type polysaccharide.

32. The tobacco product according to claim 19, 20 or 21, wherein the tobacco product is a tobacco product incorporated in the surface of tobacco product with a dispersion of about 0.5 to about 10 percent by weight of the thermo-gelable .beta.-1,3-glucan-type polysaccharide, and wherein the amount of the thermo-gelable 3-1,3-glucan-type polysaccharide to be incorporated is about 30 to about 200 grams per square meter of the polysaccharide dispersion of about 0.5 to about 10 percent by weight.

33. The tobacco product according to claim 19,20 or 21, wherein the tobacco product is a tobacco produce incorporated in the surface of tobacco product with a dispersion of about 0.5 to about 10 percent by weight of the thermo-gelable .beta.-1,3-glucan-type polysaccharide, and wherein the incorporation is made by spraying or coating.

34. A tobacco substitute, which comprises burning regulator, a thermo-gelable .beta.-1,3-glucan-type polysaccharide and burning material.

35. The tobacco substitute according to claim 34, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is a crude preparation.

36. The tobacco substitute according to claim 34, wherein the amount of the thermo-gelable .beta.-1,3-glucan-type polysaccharide is from 30 to 100 percent by weight based on the weight of burning material.

37. The tobacco substitute according to claim 36, wherein the amount of the thermo-gelable .beta.-1,3-glucan-type poly-saccharide is 100 percent by weight based on the weight of burning material,

38. The tobacco substitute according to claim 34, wherein the incorporating ratio between the burning regulator and the combination of the burning material and the thermo-gelable .beta.-1,3-glucan-type polysaccharide is, in the respec-tive weight ratio, 90:10 to 10:90.

39. The tobacco substitute according to claim 38, wherein the incorporating ratio between the burning regulator and the combination of the burning material and the thermo-gelable .beta.-1,3-glucan-type polysaccharide is, in the respective weight ratio, 70:30 to 30:70.

40. The tobacco substitute according to claim 34, wherein the thermo-gelable .beta.-1,3-glucan-type polysaccharide is in the form of a gelation product.

41. The tobacco substitute according to claim 40, wherein the gelation product is a sheet,

42, The tobacco substitute according to claim 41. wherein the sheet is shreds of the sheet.

43. The tobacco substitute according to claim 40. wherein the gelation product is a thread.

44. The tobacco substitute according to claim 43, wherein the thread is shreds of the thread.