U.S. patent number 3,584,631 [Application Number 04/872,792] was granted by the patent office on 1971-06-15 for reconstituted tobacco composition.
This patent grant is currently assigned to AMF Incorporated. Invention is credited to Howard M. Halter, Otto K. Schmidt.
United States Patent |
3,584,631 |
Halter , et al. |
June 15, 1971 |
RECONSTITUTED TOBACCO COMPOSITION
Abstract
A reconstituted tobacco sheet is disclosed in which finally
divided tobacco is combined with an adhesive consisting essentially
of ethyl cellulose with an ethoxyl content of 45.5 percent to 46.8
percent and a viscosity at a 5 percent concentration of at least
5,000 cps at 25.degree. C. The product produced is characterized by
a substantial amount of wet strength and can be plasticized with
conventional glycol humectants.
Inventors: |
Halter; Howard M. (Norwalk,
CT), Schmidt; Otto K. (Windsor, CT) |
Assignee: |
AMF Incorporated (N/A)
|
Family
ID: |
25360302 |
Appl.
No.: |
04/872,792 |
Filed: |
August 25, 1969 |
Related U.S. Patent Documents
|
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
|
688663 |
Dec 7, 1967 |
3500833 |
|
|
|
Current U.S.
Class: |
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: |
;131/14R,17 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Rein; Melvin D.
Parent Case Text
This is a Divisional Application of Ser. No. 688,663, filed Dec. 7,
1967, now U.S. Pat. No. 3,500,833.
Claims
What we claim is:
1. A smoking composition comprising finely divided tobacco and
adhesive therefor consisting essentially of ethyl cellulose with an
ethoxyl content of 45.5 percent to 46.8 percent and a viscosity at
a 5 percent concentration of at least 5,000 cps at 25.degree.
C.
2. The composition of claim 1 in which said ethyl-cellulose
adhesive has a viscosity at a 2 percent concentration of not more
than about 10,000 cps at 25.degree. C.
3. The composition of claim 1 in which said ethyl-cellulose
adhesive comprises 2--7 percent of the final smoking
composition.
4. The composition of claim 1 comprising additionally a glycol
humpectant.
Description
This invention relates to the preparation of reconstituted tobacco
products characterized by resistance to degradation by moisture.
More particularly, it relates to tobacco products containing a
particular grade of water-insoluble adhesive material.
In recent years, tobacco manufacture from finely divided tobacco
and adhesives has assumed substantial commercial importance.
Products have been made which include sheets, shreds and other
shaped articles. In general, these products have either had a very
substantial resistance to disintegration in the presence of
moisture or else have had hardly any such resistance. Effectively,
the water-soluble tobacco products have suffered when exposed to
the action of saliva and various treatment solutions used in the
application of flavors and the like.
Two basic types of water-insoluble tobacco products are possible.
Most water-insoluble products used commercially today are made from
combinations of tobacco, water-soluble adhesives and insolubilizing
or crosslinking agents which react with or crosslink the
hydrophilic hydroxyl groups on the water-soluble adhesives to
render the products water insoluble. Some of these water-insoluble
products, while generally satisfactory, particularly when first
manufactured, have tended under some storage conditions to lose
much of their water insolubility. This loss of water insolubility
is related to hydrolysis of insolubilizing crosslinks caused in
some cases by instability of these linkages to high moisture
conditions, at which such products are frequently stored, or to
ammoniacal vapors created by continuing fermentation of the filler
tobacco in smoking articles such as cigars. Virtually all of such
wet-strength tobacco products will lose at least a portion of their
wet strength at some combination of conditions involving moisture
content, temperature, pH and time.
A second basic class of water-insoluble tobacco products achieves
its insolubility through the use of water-insoluble,
organic-solvent-soluble adhesives. Such products may be made from
nonaqueous suspensions of tobacco particles in a viscous dispersion
of the adhesive in a suitable organic solvent. In principle, one
would expect that such tobacco products would enjoy a dominant
position commercially, since they avoid the problems of stability
of wet strength associated with crosslinked aqueous adhesive
systems. However, such is not the case.
It has been found that water-insoluble adhesives which are
sufficiently hydrophobic to produce tobacco products with the
requisite water resistance result in distinctive, nontobacco,
objectionable aromas on combustion, which render the resultant
products unacceptable commercially. Water-insoluble,
organic-solvent soluble adhesives in this category include
cellulosic derivatives with hydrophobic substituents such as ethyl
or benzyl groups. The problem is increased by the fact that the
hydrophobic adhesives generally require unusual plasticizers in
order to give the resultant tobacco sheet the elongation and
pliability required for satisfactory performance on automatic
machinery. These plasticizers, such as the polyester types used to
plasticize tobacco sheets with hydrophobic adhesives described by
Hotelling et al. in U.S. Pats. Nos. 2,984,244, 2,976,873 and
2,957,478, contribute nontobacco objectionable aromas on
combustion. The combination of such plasticizers with hydrophobic
adhesives in tobacco products results in products whose combustion
aroma is unacceptable commercially. Accordingly, the only tobacco
products including water-insoluble adhesives which are in
commercial use are cellulosic types with a substantial degree of
methyl substitution. Since the methyl group is decidely less
hydrophobic than the ethyl group, highly substituted
methylcellulose is compatible with conventional glycol humectants.
However, the drawback of such adhesives is that, although soluble,
they are extremely water sensitive, and they invariably result in
products with only minimal wet strength.
It is an object of this invention to provide tobacco products
characterized by a substantial amount of wet strength.
It is a further objective of this invention to provide a
wet-strength tobacco product utilizing a particular grade of a
hydrophobic adhesive.
It is another objective of this invention to provide tobacco
products with substantial amounts of wet strength made with a
hydrophobic adhesive that can be plasticized with conventional
glycol humectants normally employed in tobacco manufacture.
It is also an objective of this invention to provide wet-strength
tobacco products with commercially-acceptable taste and aroma
properties including a particular grade of a hydrophobic
adhesive.
Additional objectives will become apparent from the description of
the invention which follows.
While the invention will be described in connection with tobacco
sheet, the adhesive of the present invention may likewise be
advantageously used with tobacco in other shapes such as rods,
cylinders, plugs shreds, and the like. Accordingly, it will be
understood that the invention contemplates also tobacco manufacture
of this kind.
Ethylcellulose, a water-insoluble hydrophobic adhesive, has been
considered as a potentially useful adhesive for reconstituted
tobacco products for many years. It is mentioned in this regard in
several patents, including U.S. Pats. Nos. 2,957,478, 3,062,688 and
2,797,689. Frankenburg, in U.S. Pat. 2,797,689, recognized that the
combustion aroma of ethylcellulose and other hydrophobic adhesives
was unacceptable in tobacco products, and attempted to overcome
this problem through the use of siliceous catalysts. Detert et al.
in U.S. Pat. No. 3,062,688, discloses a tobacco product employing
highly methylated methylcellulose as the adhesive, to which he adds
sufficient ethylcellulose or acetylcellulose to provide some degree
of water resistance. This is a "compromise"-type product, since
products containing highly methylated methylcellulose as adhesive
are stated by Detert to be capable of taking up a very high content
of pulverized tobacco which has a desirable effect with respect to
taste and burn, and also has desirable mechanical properties which
allow it to be worked by machine or hand, but suffer because of a
lack of wet strength. On the other hand, tobacco sheets made with
hydrophobic adhesives such as acetylcellulose or ethylcellulose had
good wet strength, but would not take high tobacco loadings and
would not handle satisfactorily on machines or by hand. It is
obvious that by blending ethylcellulose with highly methylated
methylcellulose that the resultant wet strength is less than would
be obtained with ethylcellulose alone, and the tobacco loading,
taste and burn and machine workability properties are poorer than
would be obtained with highly methylated methylcellulose alone.
Hotelling et al. in U.S. Pats. Nos. 2,984,244, 2,976,873 and
2,957,478 obtains good wet strength in his tobacco products by
using medium ethoxy 100 cps ethylcellulose as the sole adhesive,
and also obtains good machine workability by his discovery that
certain polyester types will plasticize tobacco sheets with
ethylcellulose adhesives. However, it is stated in U.S. Pats. Nos.
2,957,478 and 2,984,244 that such products can only be made at
tobacco contents up to 85 percent, at which point the decrease in
tensile strength and elongation makes the product marginal. The
ethylcellulose content, even in the product with 85 percent tobacco
content, is still about 12 percent, and is even higher in the lower
tobacco content products. This combination of high ethylcellulose
content and the presence of polyester plasticizers, both materials
having unusual, nontobaccolike burn aromas, results in products
which we have found to be unacceptable in commercial smoking
articles.
In the present invention, the disadvantages associated with the use
of ethylcellulose as a tobacco adhesive in the prior art have been
overcome through the use of a particular grade of ethylcellulose
having an ethoxyl content of 45.5--46.8 percent (degree of
substitution of 2.28 to 2.38 ethoxyl groups per anhydroglucose
unit) and a viscosity of at least 5,000 cps. The viscosity is for a
5 percent concentration of ethylcellulose by weight in 80.20
toluene: ethanol by weight at 25.degree. C., as measured with a
Brookfield viscometer.
Use of this particular grade of ethylcellulose has several unusual
and as yet unexplainable results. First, the tobacco loading which
the ethylcellulose can bind to produce tobacco products which still
exhibit the type of properties required for good machine
workability is increased two to six fold with this grade of
ethylcellulose, allowing preparation of tobacco products containing
2--7 percent ethylcellulose in place of the 12--20 percent levels
required previously. Second, use of this particular grade of
ethylcellulose in tobacco formulations at the 2--7 percent level
unpredictably allows plasticization with standard glycol-type
humectants to produce tobacco sheet products with 15--35 percent
wet elongation and with the requisite strength and pliability for
satisfactory workability on tobacco machinery. Accordingly, the
need for the polyester plasticizers described by Hotelling et al.
is eliminated. Overall, the combination of low ethylcellulose
content, high tobacco content, and the use of conventional glycol
humectants, all made possible by the use of this particular grade
of ethylcellulose, results in wet-strength tobacco products which
closely resemble natural tobacco in taste and aroma and are
accordingly of significant commercial value.
The properties of ethylcellulose are known to be dependent on the
degree of substitution (ethoxyl content) and on the molecular
weight, which in most cases can be measured by viscosity. The
degree of substitution of ethylcellulose affects the softening
point, hardness, water absorption, solubility in ethanol and
solubility in 80.20 toluene: ethanol. On the other hand, there are
certain other properties such as tensile strength, elongation and
flexibility which are not greatly affected by the degree of
substitution, but which depend largely upon the degree of
polymerization or molecular weight. For pure (unloaded)
ethylcellulose films, the tensile strength and elongation increase
as the molecular weight or viscosity increases. However, there is a
marked leveling off of the curves for tensile strength and
elongation versus viscosity grade between the 50 and 100 cps types.
This means that very little additional tensile strength or
elongation can be gained by using higher viscosity types than about
100 cps ethylcellulose. Such higher viscosity grades are used for
applications where increased viscosity is desirable, since
improvements in film properties do not result.
With a knowledge of the factors and relationships involved in the
properties of pure ethylcellulose films as background, it was
unexpected to find that one particular grade of ethylcellulose,
that with 45.5 to 46.8 percent ethoxyl and at a 5 percent
concentration a viscosity of at least 5000 cps, results in a
completely different effect when highly loaded with ground tobacco.
This grade of ethylcellulose, when loaded with tobacco, results in
films which have substantially greater tensile strength than
comparable formulations made with all other grades of
ethylcellulose. Equally unexpected is the finding that
tobacco-loaded films of this grade of ethylcellulose are readily
plasticized with conventional glycol humectants for tobacco, such
as triethylene glycol, propylene glycol or glycerine, to produce
products with 15--35 percent wet elongation. When other grades of
ethylcellulose are plasticized with such humectants in tobacco
formulations, wet elongations of 10 percent or less invariably
result.
Any of the solvents which dissolve ethylcellulose with a degree of
substitution of 45.5--46.8 percent ethoxyl may be employed in the
manufacture of tobacco products according to this invention. Such
solvents include methanol, ethanol, methylene chloride,
toluene-ethanol mixtures and isopropanol-water mixtures containing
from 88 percent to 97 percent isopropanol. The best solvents for
this grade of ethylcellulose are 80:20 toluene: methanol or 80:20
toluene: ethanol (weight/weight), and use of either of these
solvent mixtures results in tobacco products with maximum tensile
strength and elongation properties.
The procedure involved in the manufacture of tobacco products
involves dispersion of the ethylcellulose adhesive in the solvent
for ethylcellulose, followed by the addition of tobacco dust. The
viscosity of the resultant dispersion should be at least sufficient
to prevent separation or settling of the tobacco dust. Generally, a
minimum of 3,000 cps viscosity for the resultant dispersion, as
measured by a Brookfield viscometer, is required to prevent
separation. Other additives such as humectants or plasticizers,
fibers, fungicides, ash additives such as silicious earth or color
additives may be incorporated into the tobacco suspension prior to
shaping. If tobacco sheet is to be prepared, the resultant tobacco
slurry may be cast or otherwise applied to a moving belt at a
thickness which, on drying, will result in the desired tobacco film
thickness. Depending on the solvent employed and its volatility,
the shaped tobacco slurry may be air dried or dried at elevated
temperatures, such as by steam-air mixtures or warm or hot air
impinging on the underside of the belt. The drying temperature
should be kept below the boiling point of the solvent employed, or
bubbling of the solvent and disruption of the resultant film occur.
For toluene: methanol 80/20, weight/weight) solvent systems, drying
at temperatures of about 50.degree. C. results in both good film
properties and sufficiently rapid drying rates. The organic
solvents evaporated from the tobacco products are recoverable by
conventional processes and can be reused. The shaping of the
resultant slurry may be made by any one of the well known methods
now in use in the art. A suitable method and apparatus for the
casting of the slurry into a sheet may, for example, be found in
the following U.S. Pats. Nos. to R. C. Osborne et al. 3,250,315 and
3,294,554 and in the U.S. Pat. No. 3,145,716 issued to R. C. Gertz
et al.
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 sample of ethylcellulose with an ethoxyl content of 46.8 percent
and at a 5 percent concentration a viscosity in 80/20
toluene/ethanol of 5,400 cps at 25.degree. C. was used in this
example. The Brookfield viscometer is used to measure viscosity.
The first step in the preparation of a tobacco slurry is the
preparation of a 2 percent solids dispersion of one part of this
ethylcellulose in 80/20 toluene/ethanol (weight/weight), with
agitation being continued until dispersion is complete. To the
resulting dispersion is added, with agitation, 0.2 parts
triethylene glycol, 30 parts of tobacco ground to minus 80 mesh
U.S. Standard sieve size, and sufficient additional 80/20
toluene/ethanol solvent to produce a final total solids of 25
percent in the tobacco slurry. The resultant uniform tobacco
dispersion is cast on a moving stainless steel belt at a thickness
such that the final dried film will weigh approximately 9 grams per
square foot. The cast tobacco slurry film is dried with warm
(45.degree. C.) water impinging on the underside of the belt. The
dried tobacco film is remoistened to 20 percent moisture to
facilitate doctoring from the belt. The resulting product is
particularly suitable for use as a cigarette or cigar filler,
depending on the particular type of tobacco employed. The product
handles well on machinery required for such applications, and, due
to the low ethylcellulose content, has taste and aroma qualities
comparable to natural tobacco.
Example 2
A sample of ethylcellulose with an ethoxyl content of 45.5 percent
and at a 2 percent concentration a viscosity in 80/20
toluene/ethanol of 10,000 cps at 25.degree. C. was employed in this
example. A 1.2 percent solids dispersion of one part of this
ethylcellulose in 80/20 toluene/methanol (weight/weight) was
prepared, using agitation sufficient to insure complete dispersion.
To the resulting dispersion was added 0.5 parts glycerine, 0.2
parts diatomaceous earth and 14 parts of Wisconsin tobacco ground
to minus 120 mesh U.S. Standard sieve size. Agitation is continued
until a uniform dispersion is obtained. The resulting tobacco
slurry is cast on an endless moving stainless steel belt at a
thickness such that, after drying, a tobacco sheet weighing
3.0--3.5 grams/ft.sup.2 will be obtained. The cast tobacco-slurry
film is dried at 50.degree. C. with a suitable steam-air mixture
impinging on the underside of the belt. The dried tobacco
composition is remoistened to 30 percent moisture content to
facilitate doctoring from the belt. The product was found to be
particularly suitable for use as a cigar wrapper, by virtue of its
tensile strength, elongation and pliability. The average
properties, as measured on a Scott Tester after equilibration at 80
percent Relative Humidity and 72.degree. F. for 24 hours, were as
follows: L-6* a 2 percent concentration was taken since it was
found that the material was too viscous at a 5 percent
concentration for accurate measurement in the Brookfield
viscometer.
Sheet Weight: 3.24 grams/ft.sup.2
Percent Moisture: 18.7 percent
Tensile Strength, Equilibrated: 280 grams/inch
Tensile Strength, Wet: 200 grams/inch
Elongation, Equilibrated: 17 percent
Elongation, Wet: 32 percent
The tobacco composition of this invention has many useful
applications and smoking articles such as cigars, cigarettes, pipe
tobacco as well as chewing tobacco made in whole or in part from
this material, are within the contemplation of the invention. As
sheet material it may be fed from rolls to automatic machines, for
example, cigar machines, for use as a binder or wrapper. It may
also be shredded for filler in pipes, cigarettes, and cigars. It
may be mixed with shredded whole tobacco or used alone. It may
serve as an outside wrapper for cigars or cigarettes and has the
advantage of uniformity in appearance and in physical properties as
well as uniformly blended flavor.
While the invention has been described in its preferred embodiment,
it will be understood that the invention is not limited to the
specific details set out for purposes of illustration and that
those skilled in the art may make various changes in these details
within the scope of the claims without departing from the spirit of
the invention.
* * * * *