U.S. patent number 3,613,693 [Application Number 04/844,631] was granted by the patent office on 1971-10-19 for reconstituted tobacco.
This patent grant is currently assigned to AMF Incorporated. Invention is credited to Matthew Sallee Monte.
United States Patent |
3,613,693 |
Monte |
October 19, 1971 |
RECONSTITUTED TOBACCO
Abstract
A process for manufacturing a reconstituted tobacco composition
wherein a foamed slurry is created from tobacco, a foaming agent or
adhesive and ethylhydroxyethyl cellulose having an ethoxyl D.S. of
1.2 to 1.6 and a hydroxyethyl M.S. of 0.5 to 1.2. The foamed slurry
is shaped while maintaining the temperature thereof below the
gelatin temperature of the ethylhydroxyethyl cellulose and dried to
form a shaped sheet or rod of predetermined moisture content. The
foaming agent employed may be a synthetic or natural gum or water
dispersible protein.
Inventors: |
Monte; Matthew Sallee
(Stratford, CT) |
Assignee: |
AMF Incorporated (N/A)
|
Family
ID: |
25293260 |
Appl.
No.: |
04/844,631 |
Filed: |
July 24, 1969 |
Current U.S.
Class: |
131/370;
131/355 |
Current CPC
Class: |
A24B
15/12 (20130101) |
Current International
Class: |
A24B
15/00 (20060101); A24B 15/12 (20060101); A24b
003/14 () |
Field of
Search: |
;131/17,140-144 |
References Cited
[Referenced By]
U.S. Patent Documents
|
|
|
3528434 |
September 1970 |
Halter et al. |
|
Other References
Encyclopedia of Polymer Science and Technology: Vol. 3, pub. by
Interscience Publisher's, 1965, NYC, p. 491 cited..
|
Primary Examiner: Rein; Melvin D.
Claims
What is claimed is:
1. The process of manufacturing a smokable product comprising
creating a foamed slurry from a foaming agent or adhesive, tobacco
particles, water and 0.3 percent to 2.5 percent, by weight of the
nonsolvent ingredients, of ethylhydroxyethyl cellulose with an
ethoxyl D.S. of 1.2 to 1.6 and a hydroxyethyl M.S. of 0.5 to 1.2,
shaping said foamed slurry while maintaining the temperature
thereof below the gelation temperature of said ethylhydroxyethyl
cellulose and subsequently drying said slurry to a shaped sheet or
rod form of a predetermined moisture content.
2. The process of manufacturing a smokable product comprising
creating a foamed slurry from tobacco particles, water, 0.3 percent
to 2.5 percent by weight of nonsolvent ingredients of
ethylhydroxyethyl cellulose with an ethoxyl D.S. of 1.2 to 1.6 and
a hydroxyethyl M.S. of 0.5 to 1.2 and a foaming agent in amounts
between 3 percent and 15 percent by weight of the nonsolvent
ingredients and selected from natural or synthetic hydrophylic gums
in which the natural gums are selected from carbohydrate classes
including the animal gums such as glycogen, plant gums and their
derivatives, such as cellulose ethers, cellulose esters, starches,
starch ethers, starch esters, amylose, amylopectin and their ester
and ether derivatives, locust bean gum, guar gum, gum arabic and
related seed gums and plant exudate gums, marine plant gums, such
as algins, carrageenans laminarins and agar, and microbial gums
such as the dextrans, phosphomannans such as the USDA B-1459 and
B-1428, and the gluconic acid microbial containing gums such as the
USDA Y-1409 gums, and protein classes including water dispersible
proteins such as animal proteins such as hydrolyzed keratins, egg
albumin, and vegetable proteins such as gluten, and the synthetic
gums are selected from the group consisting of polyvinyl alcohol,
polyoxyethylene and polyacrylamide shaping said foamed slurry while
maintaining the temperature thereof below the gelation temperature
of said ethylhydroxyethyl cellulose and subsequently drying said
slurry to a shaped sheet or rod form of a predetermined moisture
content.
Description
This invention relates to improved smoking products made from
foamed tobacco slurries. More particularly this invention relates
to the use of a particular grade of ethylhydroxyethyl cellulose as
a foam-stabilizing agent in foamed reconstituted tobacco
compositions and to the novel and beneficial properties that result
therefrom.
In U.S. Pat. No. 3,364,935, U.S. Pat. No. 3,404,690, U.S. Pat. No.
3,404,691 and U.S. Pat. No. 3,410,279, Moshy and Germino described
inventions to produce a foamed tobacco slurry which, when cast or
otherwise formed into a desired shape and suitably treated will
provide a smoking article with an open cellular structure. The
Moshy and Germino inventions involve processes for combining a
foaming agent, a foam-stabilizng agent and tobacco, at least one
element of said mixture being adhesive, creating a tobacco foam
slurry from said mixture, forming said slurry into a predetermined
shape and drying said shaped slurry to a preselected moisture
content to produce a stable foamed product in which tobacco
particles are spaced from each other by a gaseous media. During the
process of pumping and shaping the foamed tobacco slurry, the work
done on this slurry can cause some degree of foam breaking and
collapse. Furthermore, during the process of drying the shaped
foamed tobacco slurry, further foam disruption and collapse can
occur. Although the practice of the Moshy and Germino patents does
result in foamed tobacco products, the lack of optimum foam
stabilization characteristics using the foam-stabilizing
ingredients specified makes the production of foamed tobacco
products with exact density characteristics difficult to obtain and
control. Since the uniformity of weight, firmness and draw of
smoking articles produced by this process depends on control of the
ultimate foam density characteristics, it is apparent to those
involved in research in this area that a significantly more stable
foamed tobacco slurry is required to provide the degree of foam
density control during transfer, shaping and drying which is
necessary for a commercially acceptable process and product.
Accordingly, it is an object of this invention to provide an
improved foamed reconstituted tobacco product and an improved
process for making same.
It is a further object of this invention to provide foamed
reconstituted tobacco products which can be made to exacting
density specifications, and a process for accomplishing same.
It is still a further object of this invention to provide
reconstituted tobacco products which, because they are made by a
process which results in reproducibility of product density, will
exhibit commercially acceptable reproducibility of product weight,
compressibility and pressure drop ("draw") as well.
It is another objective of this invention to provide foamed tobacco
products with readily controllable product densities which are
achieved through the usage of a small percentage of a particular
grade of a particular water-soluble cellulosic derivative as the
foam stabilizing agent.
Additional objectives will become apparent from the description of
the invention which follows:
It should be understood throughout the discussion that this
invention contemplates manufacture of foamed reconstituted tobacco
compositions in the shape of sheet, rods, cylinders, plugs, shreds
and the range of forms associated with the production of hundreds
of different shapes of cigars. In the case of foamed reconstituted
tobacco sheet, this sheet may be made at the thickness of the
ultimate smoking article, and the smoking article may be cut from
such sheet. As an alternative, the foamed reconstituted sheet may
be manufactured thinner than the desired smoking article, and this
thinner sheet chopped or shredded and used as filler in cigars,
cigarettes or pipes.
According to the present invention, when a particular grade of
ethylhydroxyethyl cellulose, that with an ethoxyl degree of
substitution (D.S.) of 1.2 to 1.6 and a hydroxyethyl molar
substitution of 0.5 to 1.2 is incorporated as a foam stabilizing
agent in a reconstituted tobacco slurry of the type described by
Moshy and Germino at a level of at least 0.3 percent, the superior
stability of the foamed tobacco slurry during the manufacturing
operations results, as described above.
The purpose of the following three paragraphs is to explain the use
herein and in the prior art of the terms "degree of substitution"
(D.S.) and "molar substitution" (M.S.).
There are three hydroxyl groups in each anhydroglucose unit in the
cellulose molecule. D.S. is the average number of hydroxyl groups
substituted in the cellulose per anhydroglucose unit. M.S. is the
average number of moles of reactant combined with the cellulose per
anhydroglucose unit. For the alkyl, carboxyalkyl, or acyl
derivatives of cellulose, the D.S. and M.S. are the same. For the
hydroxyalkyl derivatives of cellulose, the M.S. is generally
greater than the D.S. The reason for this is that each time a
hydroxyalkyl group is introduced into the cellulose molecule, an
additional hydroxyl group is formed with itself is capable of
hydroxyalklation. As a result of this, side chains of considerable
length may form on the cellulose molecule. The M.S./D.S. ratio
represents the average length of these side chains. Thus, from the
foregoing, it will be seen that the total D.S. of a cellulose
derivative can be no higher than 3, whereas the M.S. may be
considerably higher than 3, depending on the extent to which side
chains are formed.
With a mixed ether such as ethylhydroxyethyl cellulose, the ethoxyl
content is reported as D.S. since, as noted above, the D.S. and
M.S. must be the same for this constituent. The hydroxyethyl
substituent, on the other hand, is reported as M.S. since addition
to side chains is possible in this case.
The two most widely used methods for determining M.S. are the
Zeisel-Morgan method and the terminal methyl method. The
Zeisel-Morgan method is reported beginning at page 500, vol. 18,
1946, of "Industrial and Engineering Chemistry, Analytical
Edition." The terminal methyl method is reported by Lemieux and
Purves beginning at page 485, vol. 25B, 1947, of "Canadian Journal
of Research". Some are of the opinion that perhaps the latter
method is more accurate. However, all those skilled in the art
realize that it is quite difficult to obtain a high degree of
accuracy in determining M.S. at high M.S. levels, and that the
accuracy of neither of these methods is as high as desired.
However, the D.S. and M.S. values specified herein were determined
by the most accurate methods known and, at the substitution levels
of the ethylhydroxyethyl cellulose of choice, are quite
satisfactory. The ethoxyl D.S. was determined by the terminal
methyl method and the hydroxyethyl M.S. was determined by the
Ziesel-Morgan method.
Other grades of ethylhydroxyethyl cellulose are referred to in the
prior art. The use of the normal commercial grade of
ethylhydroxyethyl cellulose as the adhesive in reconstituted
tobacco compositions is reported by Rosenberg and Schmidt in U.S.
Pat. No. 3,042,552 (July 3, 1962 ). The ethoxyl content of this
material is listed by Rosenberg and Schmidt as 17 -18 percent (D.S.
=0.8 ), and the hydroxyethyl content at about 17.3 percent (M.S.
=0.9 ). The ethylhydroxyethyl cellulose used by Rosenberg and
Schmidt is different in composition than that of the present
invention, which involves an ethoxyl degree of substitution of 1.2
to 1.6 and a hydroxyethyl molar substitution of 0.5 to 1.2 . The
differences are even greater than one might anticipate from the
substitution differentials, and are in fact differences in kind,
not just in degree. The normal ethylhydroxyethyl cellulose (EHEC)
used by Rosenberg and Schmidt will dissolve in water at
temperatures up to about 60.degree. C. The EHEC of this invention
will not dissolve in water if the temperature is over 25.degree. C.
and, for complete solubilization, the temperature should be below
15.degree. C. The Rosenberg and Schmidt EHEC will gel or
precipitate from aqueous solution when the temperature is raised to
55.degree. -70.degree. C., depending on the exact substitution; the
EHEC of the present invention will gel or precipitate from aqueous
solution when the temperature is raised to about
32.degree.-38.degree. C. The Rosenberg and Schmidt EHEC is
insoluble in methanol or ethanol or 95 percent isopropanol; the
EHEC of the present invention is completely soluble in these
solvents. In spite of the fact that both materials are
ethylhydroxyethyl celluloses, the difference in substitution
between the two grades have resulted in physical and chemical
properties for the two grades of gum that are as different from
each other as one would expect from adhesives of entirely different
classes.
The properties contributed to foam stabilization by the
incorporation of the EHEC of the present invention are also
radically different from those which are obtained using other
carbohydrate, protein or synthetic gums at similar levels in the
formulation, or even at substantially higher levels. Furthermore,
the foam stabilization properties are radially different from those
which are obtained with any other cellulose ether and even from
other grades of ethylhydroxyethyl cellulose with different levels
of substitution.
It should be noted that Moshy and Germino employed, as foaming
agents, adhesives such a animal gums, such as glycogen, plant gums
and derivatives, such as cellulose ethers, cellulose esters,
startches, starch ethers, starch esters, amylose, amylopectin and
their ester and ether derivatives, locust bean gum, guar gum, gum
arabic and related seed gums and plant exudate gums, marine plant
gums, such as algins, carrageenans, laminarins and agar, and
microbial gums such as the dextrans, phosphomannans such as USDA
B-1459 and B-1428, and the gluconic acid microbial-containing gums
such as the USDA Y-1409 gums, and water-dispersible protein classes
such as animal proteins such as hydrolyzed keratins, egg albumin,
and vegetable proteins such as gluten and synthetic gums such as
polyvinyl alcohol, polyoxyethylene and polyacrylamide.
These materials, although foamable with Moshy and Germino
compositions, were quite unstable and required the addition of a
foam-stabilizing agent initially or after foaming, or the use of a
blowing agent, in order to provide any measure of foam stability.
The foam-stabilizng agents of the Moshy patents were ionic and
nonionic surfactants consisting of the salts of the sulfate esters
of the alkylphenoxypolyoxyethylene ethanol, the salts of sulfate
compounds of the type N-methyl-N-oleoyl taurine, sorbitan esters
such a sorbitan monostearate (Span 60 ) or the monooleate (Span 80
), ethylene oxide-sorbitol condensation products, and lecithin and
lecithin derivitives. Such materials in addition to that fact that
they do not provide the desired degree of foam stability for
optimum process control, also contribute off-aromas on combustion,
even when used at low levels.
Based on the Moshy and Germino disclosures of the foam instability
when any one of their many foaming agent-adhesives are incorporated
in tobacco slurries at generally high levels to provide the proper
adhesive qualities, it was quite unexpected and novel to find that
the EHEC of this invention, a cellulose ether, should function as
an exceptional foam-stabilizing agent when used at low
concentrations in the product of only 0.3 to 2.5 percent. It is
also interesting to note that the closest material to the EHEC of
this invention, the EHEC of the Rosenberg and Schmidt patent, does
not provide such foam stability when employed in otherwise
identical formulations. The uniqueness of the EHEC of this
invention indicates that the problem of tobacco foam stabilization
to both mechanical work and heat energy is most complex and, as
yet, without theoretical prediction or explanation.
It should be noted that the foam stabilization characteristic
associated with the use of the particular EHEC of this invention is
due to the degree of substitution of the ethoxyl and hydroxyethyl
substituents, with no significant effect of the viscoity of the gum
on this property. Differences in product strength are also not
obtained when different molecular weights or viscosities of this
EHEC are employed, since at the low usage concentrations involved
in tobacco foam stabilization, the EHEC does not function as an
adhesive to any measurable extent.
In the practice of this invention, any of the processing
modifications employed in the four Moshy and Germino patents may be
employed, with ethylhydroxyethyl cellulose with an ethoxyl D.S. of
1.2 to 1.6 and a hydroxyethyl molar substitution of 0.5 to 1.2
being used at a concentration of 0.3 to 2.5 percent of the
composition (Dry basis) in place of the foam stabilizing agents
employed by Moshy and Germino. Accordingly, the stabilized tobacco
foam may be prepared by: (a) foaming the foaming agent, then adding
tobacco and the foam-stabilizing agent (the EHEC of this
invention); (b) foaming the foam stabilizing agent (the EHEC of
this invention), then adding tobacco and the foaming agent; (c)
foaming a foaming agent, foam stabilizing agent (the EHEC of this
invention) mixture, then adding tobacco; (d) foaming a mixture of
foaming agent, foam-stabilizing agent (the EHEC of this invention)
and tobacco; (e) foaming a mixture of foaming agent and tobacco,
then adding foam-stabilizing agent (the EHEC of this invention);
(f) foaming a mixture of foam-stabilizing agent (the EHEC of this
invention) and tobacco, then adding foaming agent.
It should be noted that if tobacco is treated in a manner such that
its adhesive properties are fully developed, such as in Light and
Osborne U.S. Pat. No. 661,762, then addition of one of the adhesive
foaming agent types referred to by Moshy and Germino is not
necessary. Accordingly, (f) above, for example, would involve only
foaming a mixture of foam-stabiling agent (the EHEC of this
invention) and tobacco, shaping and drying to a preselected
moisture content.
Optional additives in the formulations of this invention include
humectants or plasticizers, ash whiteners, fungicides, fibers for
reinforcement and cross-linking or insolubilizing agents for
resistance to water. Use of such additives, of course, depends on
the particular properties required in the final smoking
article.
In working with the dispersions and foamed dispersions containing
the EHEC of this invention as the foam-stabilizing agent, it must
be remembered that this material has a low thermal gelation
temperature. Care must be taken at each step of the tobacco slurry
preparation, foaming, transfer and shaping, to insure that the
thermal gelation temperature is not approached, other gelatin or
precipitation will occur and the foam stabilization property will
be lost.
The following examples are provided as further illustrations of the
inventive concept, and should not be construed as limitations on
the invention.
EXAMPLE 1
A tobacco slurry is prepared by adding, with mild agitation, 0.2
parts (dry basis) of a 3.0 percent dispersion of refined sulfite
pulp to one part (dry basis) of a 2 percent aqueous dispersion of
methylcellulose with a viscosity of 15,000 c.p.s. The pulp
dispersion and the methylcellulose dispersion are each at about
5.degree. C. before mixing, and 10.degree. C. or less after the
mild agitation. To this mixture is added, with mild agitation, 0.03
parts (dry basis) of a 2 percent solution of ethylhydroxyethyl
cellulose with an ethoxyl D.S. of 1.2 a hydroxyethyl M.S. of 0.5, a
viscosity of 15,000 c.p.s. and at a temperature of 5.degree. C.
Also, a 20 percent aqueous dispersion of minus 80 mesh Bright
tobacco leaf is added, and the completed slurry is mixed for 15
minutes, to produce a uniform dispersion at a temperature of
16.degree. C. The tobacco slurry is foamed to a density of 0.55
grams/cc., using Hobart mixer with a wire whip, and the resultant
foamed slurry is cast on a moving stainless steel belt at a
thickness such that the tobacco slurry film after drying, will
weigh 6 grams per square foot. The foamed tobacco sheet product is
24 mils thick, as compared to a conventional nonfoamed product of
the same formulation which would be only 6 -7 mils thick at 6 grams
per square foot . It may be shredded and used as a cigarette
filler.
EXAMPLE 2
A 6 percent solids dispersion of refined burley stem pulp is
prepared to a Schopper-Riegler freeness of minus 300 cc. using the
stem pulp preparative procedure described by Light and Osborne in
U.S. Pat. Ser. No. 661,762. To 6 parts (dry basis) of this tobacco
stem pulp is added, with agitation, 4 parts (dry basis) of a 20
percent dispersion of minus 120 mesh Wisconsin leaf dust and 0.25
parts of a 2 percent aqueous dispersion of ethylhydroxyethyl
cellulose with an ethoxyl D.S. of 1.6, a hydroxyethyl M.S. of 1.2
and a viscosity of 300 c.p.s. Mild agitation is continued until a
uniform dispersion is obtained, with care being taken to prevent
the slurry temperature from rising above 20.degree. C. The
resultant tobacco slurry is foamed to a density of 0.60 grams per
cc. and may be cast and dried in sheet form as in Example 1, or
extruded or molded to product, after drying, a porous
self-supporting rod or other core shapes suitable for wrapping as a
cigar.
* * * * *