Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
~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
: `
- 1- ~
53~
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
.. . . . .
~6~3~
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
- 4 -
~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
- 5 -
~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.
-- 7 --
6~S3~
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.
- 8 --
~ 3~
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
-- 10 --
:
1~6~L~3~
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
-- 11 --
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
- 13 -
.
~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
- 14 -
. . ,. ,, . . - . . . . . . ..... . . .. .. .
3~
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.
- 15 -
~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
- 16 -
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
~ ____
200 0 2510
250 11450
300 25844 48439
400 ~ 43544 g4319
500 96475 172826
- 17 -
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
- 18 -
,
~ 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
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20 -
:. .
~a~6~L53~
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.
21
S3~
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.
.
- 22 -
.~ :
~ 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-
- 24 -
-
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
.
- 25 -
. , . .: , : . - . - . . , .. .. ~ : : , , . , :. ,.,, . . : , . . , : -.. : , ,
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-
- 26 -
.
~ 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
- 27 -
~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 -
' '.
LS30
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
29 -
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
- 30 -
.- .: ~ . . . .. . ; . . .. . . . .. .
.,. :, . . , ~ ,
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
- 33
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
- 34
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~)
'
- 35 -
~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
- 36
:
~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
.
- 37 -
, ., . . ., . . . , . . ~ - . , ., , , ~ ,
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.~
- 38 -
,
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)
- 41 -
.. , - . ... ,. - - . .. - - - . . .. . . ~ .... .. - . . .. ... . .
-
~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)
- 42 -
.
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
- 43 -
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
150C 9
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
- 45 -
-
~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 -
.
