U.S. patent application number 16/227742 was filed with the patent office on 2020-06-25 for method for whitening tobacco.
The applicant listed for this patent is R.J. Reynolds Tobacco Company. Invention is credited to Michael David Davis, David Neil McClanahan.
Application Number | 20200196658 16/227742 |
Document ID | / |
Family ID | 69167870 |
Filed Date | 2020-06-25 |
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United States Patent
Application |
20200196658 |
Kind Code |
A1 |
McClanahan; David Neil ; et
al. |
June 25, 2020 |
METHOD FOR WHITENING TOBACCO
Abstract
A method of preparing a whitened tobacco material is provided,
the method including the steps of (i) extracting a tobacco material
with an aqueous solution to give a tobacco solids material and a
tobacco extract; (ii) treating the tobacco solids material with a
caustic wash to give a tobacco pulp; (iii) bleaching the tobacco
pulp with a solution including a strong base, an oxidizing agent,
or a combination thereof to give a bleached tobacco pulp; and (iv)
drying the bleached tobacco pulp to give the whitened tobacco
material. The invention also provides a smokeless tobacco product
incorporating a whitened tobacco material. The smokeless tobacco
product may be a snus-type formulation contained within a sealed
pouch.
Inventors: |
McClanahan; David Neil;
(Winston-Salem, NC) ; Davis; Michael David;
(Germanton, NC) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
R.J. Reynolds Tobacco Company |
Winston-Salem |
NC |
US |
|
|
Family ID: |
69167870 |
Appl. No.: |
16/227742 |
Filed: |
December 20, 2018 |
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A24B 15/32 20130101;
A24B 3/04 20130101; A24B 15/287 20130101; A24B 13/00 20130101; A24B
15/42 20130101; A24B 15/24 20130101 |
International
Class: |
A24B 15/42 20060101
A24B015/42; A24B 15/24 20060101 A24B015/24; A24B 3/04 20060101
A24B003/04; A24B 13/00 20060101 A24B013/00; A24B 15/32 20060101
A24B015/32 |
Claims
1. A method of preparing a whitened tobacco material for use in a
smokeless tobacco product, comprising: (i) extracting a tobacco
material with an aqueous solution to provide a tobacco solids
material and a tobacco extract; (ii) treating the tobacco solids
material with a caustic wash to provide a tobacco pulp; (iii)
bleaching the tobacco pulp with a solution comprising a strong
base, an oxidizing agent, or a combination thereof to provide a
bleached tobacco pulp; and (iv) drying the bleached tobacco pulp to
provide the whitened tobacco material.
2. The method of claim 1, further comprising milling the tobacco
material such that the milled tobacco material is able to pass
through a screen of 18 U.S. sieve size.
3. The method of claim 1, wherein in the step of treating the
tobacco solid material with a caustic wash is done at atmospheric
pressure.
4. The method of claim 1, wherein the caustic wash comprises at
least one strong base.
5. The method of claim 1, wherein the caustic wash comprises sodium
hydroxide.
6. The method of claim 1, wherein the bleached tobacco pulp is
dried to a moisture content of less than about 30 percent moisture
on a wet basis.
7. The method of claim 1, further comprising hydrolyzing the
tobacco pulp with an acid prior to step (ii).
8. The method of claim 7, wherein the acid is sulfuric acid,
hydrochloric acid, citric acid, or a combination thereof.
9. The method of claim 1, further comprising dewatering the tobacco
material using at least one of a screw press and a basket
centrifuge following steps (i), (ii) and/or step (iii).
10. The method of claim 1, wherein the bleaching step (iii)
comprises treatment with one or more of peracetic acid, sodium
hydroxide, and hydrogen peroxide.
11. The method of claim 1, wherein the bleaching step (iii) further
comprises treatment with one or more stabilizers in addition to an
oxidizing agent.
12. The method of claim 11, wherein the stabilizers are selected
from the group consisting of magnesium sulfate, sodium silicate,
and combinations thereof.
13. The method of claim 1, wherein the bleaching step (iii)
comprises treatment with a strong base and an oxidizing agent, and
wherein the molar ratio of the amount of strong base to the amount
of oxidizing agent is from about 1:1 to about 1:100.
14. The method of claim 13, wherein the molar ratio of the amount
of strong base to the amount of oxidizing agent is from about 1:5
to about 1:50.
15. The method of claim 1, further comprising neutralizing the
bleached pulp material to a pH in the range of about 5 to about 11
prior to step (iv).
16. The method of claim 1, further comprising milling the whitened
tobacco material following step (iv) to a size in the range of
approximately 5 mm to about 0.1 mm.
17. The method of claim 1, wherein the aqueous solution used to
extract the tobacco material in step (i) comprises a chelating
agent.
18. The method of claim 17, wherein the chelating agent comprises
one or more of EDTA and DTPA.
19. The method of claim 1, wherein the molar ratio of aqueous
solution to the tobacco material in the extraction step (i) is from
about 4:1 to about 16:1.
20. The method of claim 1, wherein the tobacco material comprises
lamina, stems, or a combination thereof.
21. The method of claim 1, wherein the tobacco material comprises
Rustica stems.
22. The method of claim 1, wherein the tobacco material comprises
at least about 90% by weight roots, stalks, or a combination
thereof.
23. The method of claim 1, wherein the whitened tobacco material is
characterized by an International Organization for Standardization
(ISO) brightness of at least about 60%.
24. The method of claim 1, further comprising mixing the tobacco
solids material with a wood pulp prior to step (ii).
25. The method of claim 1, further comprising incorporating the
whitened tobacco material within a smokeless tobacco product.
26. The method of claim 25, wherein the smokeless tobacco product
further comprises one or more additional components selected from
the group consisting of flavorants, fillers, binders, pH adjusters,
buffering agents, colorants, disintegration aids, antioxidants,
humectants, and preservatives.
27. A smokeless tobacco product incorporating the whitened tobacco
material prepared according to the method of claim 1.
28. The smokeless tobacco product of claim 27, comprising a
water-permeable pouch containing the whitened tobacco material.
29. The smokeless tobacco product of claim 27, further comprising
one or more additional components selected from the group
consisting of flavorants, fillers, binders, pH adjusters, buffering
agents, colorants, disintegration aids, antioxidants, humectants,
and preservatives.
Description
FIELD OF THE INVENTION
[0001] The present invention relates to products made or derived
from tobacco, or that otherwise incorporate tobacco, and are
intended for human consumption.
BACKGROUND
[0002] Cigarettes, cigars and pipes are popular smoking articles
that employ tobacco in various forms. Such smoking articles are
used by heating or burning tobacco, and aerosol (e.g., smoke) is
inhaled by the smoker. Tobacco also may be enjoyed in a so-called
"smokeless" form. Particularly popular smokeless tobacco products
are employed by inserting some form of processed tobacco or
tobacco-containing formulation into the mouth of the user.
[0003] Various types of smokeless tobacco products are known. See
for example, the types of smokeless tobacco formulations,
ingredients, and processing methodologies set forth in U.S. Pat.
No. 1,376,586 to Schwartz; U.S. Pat. No. 3,696,917 to Levi; U.S.
Pat. No. 4,513,756 to Pittman et al.; U.S. Pat. No. 4,528,993 to
Sensabaugh, Jr. et al.; U.S. Pat. No. 4,624,269 to Story et al.;
U.S. Pat. No. 4,991,599 to Tibbetts; U.S. Pat. No. 4,987,907 to
Townsend; U.S. Pat. No. 5,092,352 to Sprinkle, III et al.; U.S.
Pat. No. 5,387,416 to White et al.; U.S. Pat. No. 6,668,839 to
Williams; U.S. Pat. No. 6,834,654 to Williams; U.S. Pat. No.
6,953,040 to Atchley et al.; U.S. Pat. No. 7,032,601 to Atchley et
al.; and U.S. Pat. No. 7,694,686 to Atchley et al.; US Pat. Pub.
Nos. 2004/0020503 to Williams; 2005/0115580 to Quinter et al.;
2006/0191548 to Strickland et al.; 2007/0062549 to Holton, Jr. et
al.; 2007/0186941 to Holton, Jr. et al.; 2007/0186942 to Strickland
et al.; 2008/0029110 to Dube et al.; 2008/0029116 to Robinson et
al.; 2008/0173317 to Robinson et al.; 2008/0196730 to Engstrom et
al.; 2008/0209586 to Neilsen et al.; 2008/0305216 to Crawford et
al.; 2009/0065013 to Essen et al.; 2009/0293889 to Kumar et al.;
2010/0291245 to Gao et al; and 2011/0139164 to Mua et al.; PCT WO
04/095959 to Arnarp et al. and WO 2010/132444 to Atchley; each of
which is incorporated herein by reference.
[0004] One type of smokeless tobacco product is referred to as
"snuff." Representative types of moist snuff products, commonly
referred to as "snus," are manufactured in Europe, particularly in
Sweden, by or through companies such as Swedish Match AB, Fiedler
& Lundgren AB, Gustavus AB, Skandinavisk Tobakskompagni A/S,
and Rocker Production AB. Smokeless tobacco products available in
the U.S.A. are marketed under the tradenames CAMEL Snus, CAMEL
Orbs, CAMEL Strips and CAMEL Sticks by R. J. Reynolds Tobacco
Company; GRIZZLY moist tobacco, KODIAK moist tobacco, LEVI GARRETT
loose tobacco and TAYLOR'S PRIDE loose tobacco by American Snuff
Company, LLC; KAYAK moist snuff and CHATTANOOGA CHEW chewing
tobacco by Swisher International, Inc.; REDMAN chewing tobacco by
Pinkerton Tobacco Co. LP; COPENHAGEN moist tobacco, COPENHAGEN
Pouches, SKOAL Bandits, SKOAL Pouches, RED SEAL long cut and REVEL
Mint Tobacco Packs by U.S. Smokeless Tobacco Company; and MARLBORO
Snus and Taboka by Philip Morris USA. See also, for example,
Bryzgalov et al., 1N1800 Life Cycle Assessment, Comparative Life
Cycle Assessment of General Loose and Portion Snus (2005). In
addition, certain quality standards associated with snus
manufacture have been assembled as a so-called GothiaTek
standard.
[0005] Through the years, various treatment methods and additives
have been proposed for altering the overall character or nature of
tobacco materials utilized in tobacco compositions. For example,
additives or treatment processes are sometimes utilized in order to
alter the chemistry or sensory properties of the tobacco material,
or in the case of smokable tobacco materials, to alter the
chemistry or sensory properties of mainstream smoke generated by
smoking articles including the tobacco material. In some cases, a
heat treatment process can be used to impart a desired color or
visual character to the tobacco material, desired sensory
properties to the tobacco material, or a desired physical nature or
texture to the tobacco material.
[0006] It would be desirable in the art to provide further methods
for altering the character and nature of tobacco (and tobacco
compositions and formulations) useful in smoking articles or
smokeless tobacco products.
BRIEF SUMMARY
[0007] The present disclosure provides a method of processing a
tobacco material to modify the color of the tobacco material,
specifically to provide a tobacco material that is lightened in
color (i.e., "whitened"). The whitened tobacco material can be used
in smokeless tobacco materials to give materials adapted for oral
use with a whitened appearance.
[0008] In various embodiments of preparing a whitened tobacco
material described herein, the method can include (i) extracting a
tobacco material with an aqueous solution to provide a tobacco
solids material and a tobacco extract; (ii) treating the tobacco
solids material with a caustic wash to provide a tobacco pulp;
(iii) bleaching the tobacco pulp with a solution comprising a
strong base, an oxidizing agent, or a combination thereof to
provide a bleached tobacco pulp; and (iv) drying the bleached
tobacco pulp to provide the whitened tobacco material. In certain
embodiments, the bleached tobacco pulp can be dried to a moisture
content of less than about 30 percent moisture on a wet basis. In
various embodiments, the whitened tobacco material is characterized
by an International Organization for Standardization (ISO)
brightness of at least about 55%, at least about 60%, at least
about 65%, or at least about 70%.
[0009] In certain embodiments, the tobacco input material comprises
lamina, stems, or a combination thereof. For example, the tobacco
input material can include Rustica stems and/or Burley stems. In
some embodiments, the tobacco input material comprises at least
about 90% by weight roots, stalks, or a combination thereof.
[0010] The method can further include milling the tobacco material
before the extraction step such that the milled tobacco material is
able to pass through a screen of 18 or 16 U.S. sieve size. In some
embodiments, the method can further include hydrolyzing the tobacco
pulp with an acid prior to step (ii). The acid can be sulfuric
acid, hydrochloric acid, citric acid, or a combination thereof. In
various embodiments, the method can further comprise dewatering the
tobacco material, for example using at least one of a screw press
and a basket centrifuge, following steps (i), (ii) and/or step
(iii).
[0011] In various embodiments of the present invention, the aqueous
solution used to extract the tobacco material in step (i) can
comprise a chelating agent. For example, the aqueous solution can
include ethylenediaminetetraacetic acid (EDTA) and/or
diethylenetriamine pentaacetic acid (DTPA). In various embodiments,
the molar ratio of aqueous solution to the tobacco material in the
extraction step (i) is from about 4:1 to about 16:1.
[0012] In various embodiments, the step of treating the tobacco
solid material with a caustic wash is done at atmospheric pressure.
In some embodiments, the caustic wash comprises at least one strong
base. For example, the caustic wash can comprise sodium hydroxide.
In certain embodiments, the methods described herein can further
comprise mixing the tobacco solids material with a wood pulp prior
to step (ii). In certain embodiments, the methods described herein
can further comprise mixing the tobacco solids material with a wood
pulp after step (ii).
[0013] In some embodiments, the bleaching step (iii) comprises
treatment with a strong base and an oxidizing agent, and wherein
the molar ratio of the amount of strong base to the amount of
oxidizing agent is from about 1:1 to about 1:100, or from about 1:5
to about 1:50. In some embodiments, the bleaching step (iii)
comprises treatment with one or more of peracetic acid, sodium
hydroxide, and hydrogen peroxide. In various embodiments, the
bleaching step (iii) further comprises treatment with one or more
stabilizers in addition to an oxidizing agent. For example, the
stabilizers can be selected from the group consisting of magnesium
sulfate, sodium silicate, and combinations thereof. In certain
embodiments, the method further includes neutralizing the bleached
pulp material to a pH in the range of about 5 to about 11 prior to
step (iv).
[0014] In various embodiments, the method further includes
incorporating the whitened tobacco material within a smokeless
tobacco product. In certain embodiments, the whitened tobacco
material can be milled before incorporating the tobacco material
into a tobacco product to a size in the range of about 10 mm to
about 0.1 mm. In addition to the whitened tobacco material, the
smokeless tobacco product can further include one or more
additional components selected from the group consisting of
flavorants, fillers, binders, pH adjusters, buffering agents,
colorants, disintegration aids, antioxidants, humectants, and
preservatives.
[0015] A smokeless tobacco product incorporating the whitened
tobacco materials described herein is also provided. In some
embodiments, the smokeless tobacco product can include a
water-permeable pouch containing the whitened tobacco material. In
various embodiments, the smokeless tobacco product can further
include one or more additional components selected from the group
consisting of flavorants, fillers, binders, pH adjusters, buffering
agents, colorants, disintegration aids, antioxidants, humectants,
and preservatives.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 is a front perspective view illustrating a pouched
product according to an embodiment; and
[0017] FIG. 2 is a flow chart illustrating the general steps for
preparing a whitened tobacco material according to an
embodiment.
DETAILED DESCRIPTION
[0018] Aspects of the present disclosure now will be described more
fully hereinafter. This invention may, however, be embodied in many
different forms and should not be construed as limited to the
embodiments set forth herein; rather, these embodiments are
provided so that this disclosure will be thorough and complete, and
will fully convey the scope of the invention to those skilled in
the art. As used in this specification and the claims, the singular
forms "a," "an," and "the" include plural referents unless the
context clearly dictates otherwise. Reference to "dry weight
percent" or "dry weight basis" refers to weight on the basis of dry
ingredients (i.e., all ingredients except water).
[0019] Certain embodiments will be described with reference to FIG.
1 of the accompanying drawings, and these described embodiments
involve snus-type products having an outer pouch and containing a
whitened tobacco material within the tobacco formulation. As
explained in greater detail below, such embodiments are provided by
way of example only, and the smokeless tobacco product can include
tobacco compositions in other forms.
[0020] Referring to FIG. 1, there is shown a first embodiment of a
smokeless tobacco product 10. The tobacco product 10 includes a
moisture-permeable container in the form of a pouch 20, which
contains a solid tobacco filler material 15 comprising a whitened
tobacco material of a type described herein. The smokeless tobacco
product also may optionally comprise, in certain embodiments, a
plurality of microcapsules dispersed within the tobacco filler
material 15, the microcapsules containing a component (e.g., a
flavorant) such as described in greater detail below.
[0021] The tobacco product 10 is typically used by placing one
pouch containing the tobacco formulation in the mouth of a human
subject/user. During use, saliva in the mouth of the user causes
some of the components of the tobacco formulation to pass through
the water-permeable pouch and into the mouth of the user. The pouch
preferably is not chewed or swallowed. The user is provided with
tobacco flavor and satisfaction, and is not required to spit out
any portion of the tobacco formulation. After about 10 minutes to
about 60 minutes, typically about 15 minutes to about 45 minutes,
of use/enjoyment, substantial amounts of the tobacco formulation
and the contents of the optional microcapsules and have been
ingested by the human subject, and the pouch may be removed from
the mouth of the human subject for disposal. In certain
embodiments, the pouch materials can be designed and manufactured
such that under conditions of normal use, a significant amount of
the tobacco formulation contents permeate through the pouch
material prior to the time that the pouch undergoes loss of its
physical integrity.
[0022] The present disclosure provides a whitened tobacco
composition, smokeless tobacco products incorporating such whitened
tobacco compositions, and methods for preparing a whitened tobacco
composition and for incorporating such compositions within
smokeless tobacco products. As used herein, the term "whitened"
refers to a composition comprising a tobacco material that has been
treated to remove some degree of color therefrom. Thus, a
"whitened" tobacco material that is treated according to the
methods described herein is visually lighter in hue than an
untreated tobacco material. The whitened tobacco composition of the
invention can be used as a component of a smokeless tobacco
composition, such as loose moist snuff, loose dry snuff, chewing
tobacco, pelletized tobacco pieces, extruded or formed tobacco
strips, pieces, rods, or sticks, finely divided ground powders,
finely divided or milled agglomerates of powdered pieces and
components, flake-like pieces, molded processed tobacco pieces,
pieces of tobacco-containing gum, rolls of tape-like films, readily
water-dissolvable or water-dispersible films or strips, or
capsule-like materials.
[0023] Tobaccos used in the tobacco compositions of the invention
may vary. In certain embodiments, tobaccos that can be employed
include flue-cured or Virginia (e.g., K326), burley, sun-cured
(e.g., Indian Kurnool and Oriental tobaccos, including Katerini,
Prelip, Komotini, Xanthi and Yambol tobaccos), Maryland, dark,
dark-fired, dark air cured (e.g., Passanda, Cubano, Jatin and
Bezuki tobaccos), light air cured (e.g., North Wisconsin and Galpao
tobaccos), Indian air cured, Red Russian and Rustica tobaccos, as
well as various other rare or specialty tobaccos and various blends
of any of the foregoing tobaccos. Descriptions of various types of
tobaccos, growing practices and harvesting practices are set forth
in Tobacco Production, Chemistry and Technology, Davis et al.
(Eds.) (1999), which is incorporated herein by reference. Various
representative other types of plants from the Nicotiana species are
set forth in Goodspeed, The Genus Nicotiana, (Chonica Botanica)
(1954); U.S. Pat. No. 4,660,577 to Sensabaugh, Jr. et al.; U.S.
Pat. No. 5,387,416 to White et al. and U.S. Pat. No. 7,025,066 to
Lawson et al.; US Patent Appl. Pub. Nos. 2006/0037623 to Lawrence,
Jr. and 2008/0245377 to Marshall et al.; each of which is
incorporated herein by reference. Exemple Nicotiana species include
N. tabacum, N. rustica, N. alata, N. arentsii, N. excelsior, N.
forgetiana, N. glauca, N. glutinosa, N. gossei, N. kawakamii, N.
knightiana, N. langsdorffi, N. otophora, N. setchelli, N.
sylvestris, N. tomentosa, N. tomentosiformis, N. undulata, N. x
sanderae, N. africana, N. amplexicaulis, N. benavidesii, N.
bonariensis, N. debneyi, N. longiflora, N. maritina, N.
megalosiphon, N. occidentalis, N. paniculata, N. plumbaginifolia,
N. raimondii, N. rosulata, N. simulans, N. stocktonii, N.
suaveolens, N. umbratica, N. velutina, N. wigandioides, N. acaulis,
N. acuminata, N. attenuata, N. benthamiana, N. cavicola, N.
clevelandii, N. cordifolia, N. corymbosa, N. fragrans, N.
goodspeedii, N. linearis, N. miersii, N. nudicaulis, N.
obtusifolia, N. occidentalis subsp. Hersperis, N. pauciflora, N.
petunioides, N. quadrivalvis, N. repanda, N. rotundifolia, N.
solanifolia, and N. spegazzinii.
[0024] Nicotiana species can be derived using genetic-modification
or crossbreeding techniques (e.g., tobacco plants can be
genetically engineered or crossbred to increase or decrease
production of components, characteristics or attributes). See, for
example, the types of genetic modifications of plants set forth in
U.S. Pat. No. 5,539,093 to Fitzmaurice et al.; U.S. Pat. No.
5,668,295 to Wahab et al.; U.S. Pat. No. 5,705,624 to Fitzmaurice
et al.; U.S. Pat. No. 5,844,119 to Weigl; U.S. Pat. No. 6,730,832
to Dominguez et al.; U.S. Pat. No. 7,173,170 to Liu et al.; U.S.
Pat. No. 7,208,659 to Colliver et al. and U.S. Pat. No. 7,230,160
to Benning et al.; US Patent Appl. Pub. No. 2006/0236434 to
Conkling et al.; and PCT WO 2008/103935 to Nielsen et al. See,
also, the types of tobaccos that are set forth in U.S. Pat. No.
4,660,577 to Sensabaugh, Jr. et al.; U.S. Pat. No. 5,387,416 to
White et al.; and U.S. Pat. No. 6,730,832 to Dominguez et al., each
of which is incorporated herein by reference. Most preferably, the
tobacco materials are those that have been appropriately cured and
aged. Especially preferred techniques and conditions for curing
flue-cured tobacco are set forth in Nestor et al., Beitrage
Tabakforsch. Int., 20 (2003) 467-475 and U.S. Pat. No. 6,895,974 to
Peele, which are incorporated herein by reference. Representative
techniques and conditions for air curing tobacco are set forth in
Roton et al., Beitrage Tabakforsch. Int., 21 (2005) 305-320 and
Staaf et al., Beitrage Tabakforsch. Int., 21 (2005) 321-330, which
are incorporated herein by reference. Certain types of unusual or
rare tobaccos can be sun cured. Manners and methods for improving
the smoking quality of Oriental tobaccos are set forth in U.S. Pat.
No. 7,025,066 to Lawson et al., which is incorporated herein by
reference. Representative Oriental tobaccos include katerini,
prelip, komotini, xanthi and yambol tobaccos. Tobacco compositions
including dark air cured tobacco are set forth in US Patent Appl.
Pub. No. 2008/0245377 to Marshall et al., which is incorporated
herein by reference. See also, types of tobacco as set forth, for
example, in US Patent Appl. Pub. No. 2011/0247640 to Beeson et al.,
which is incorporated herein by reference.
[0025] The Nicotiana species can be selected for the content of
various compounds that are present therein. For example, plants can
be selected on the basis that those plants produce relatively high
quantities of one or more of the compounds desired to be isolated
therefrom. In certain embodiments, plants of the Nicotiana species
(e.g., Galpao commun tobacco) are specifically grown for their
abundance of leaf surface compounds. Tobacco plants can be grown in
greenhouses, growth chambers, or outdoors in fields, or grown
hydroponically.
[0026] Various parts or portions of the plant of the Nicotiana
species can be employed. For example, virtually all of the plant
(e.g., the whole plant) can be harvested, and employed as such.
Alternatively, various parts or pieces of the plant can be
harvested or separated for further use after harvest. For example,
the flower, leaves, stem, stalk, roots, seeds, and various
combinations thereof, can be isolated for further use or treatment.
In some embodiments, the tobacco material subjected to the
treatments set forth herein is Rustica stems in milled form.
[0027] The post-harvest processing of the plant or portion thereof
can vary. After harvest, the plant, or portion thereof, can be used
in a green form (e.g., the plant or portion thereof can be used
without being subjected to any curing process). For example, the
plant or portion thereof can be used without being subjected to
significant storage, handling or processing conditions. In certain
situations, it is advantageous for the plant or portion thereof be
used virtually immediately after harvest. Alternatively, for
example, a plant or portion thereof in green form can be
refrigerated or frozen for later use, freeze dried, subjected to
irradiation, yellowed, dried, cured (e.g., using air drying
techniques or techniques that employ application of heat), heated
or cooked (e.g., roasted, fried or boiled), or otherwise subjected
to storage or treatment for later use.
[0028] The harvested plant or portion thereof can be physically
processed. The plant or portion thereof can be separated into
individual parts or pieces (e.g., the leaves can be removed from
the stems, and/or the stems and leaves can be removed from the
stalk). The harvested plant or individual parts or pieces can be
further subdivided into parts or pieces (e.g., the leaves can be
shredded, cut, comminuted, pulverized, milled or ground into pieces
or parts that can be characterized as filler-type pieces, granules,
particulates or fine powders). The plant, or parts thereof, can be
subjected to external forces or pressure (e.g., by being pressed or
subjected to roll treatment). When carrying out such processing
conditions, the plant or portion thereof can have a moisture
content that approximates its natural moisture content (e.g., its
moisture content immediately upon harvest), a moisture content
achieved by adding moisture to the plant or portion thereof, or a
moisture content that results from the drying of the plant or
portion thereof. For example, powdered, pulverized, ground or
milled pieces of plants or portions thereof can have moisture
contents of less than about 25 weight percent, often less than
about 20 weight percent, and frequently less than about 15 weight
percent.
[0029] Tobacco compositions intended to be used in a smokeless form
such as that in FIG. 1 may incorporate a single type of tobacco
(e.g., in a so-called "straight grade" form). For example, the
tobacco within a tobacco composition may be composed solely of
flue-cured tobacco (e.g., all of the tobacco may be composed, or
derived from, either flue-cured tobacco lamina or a mixture of
flue-cured tobacco lamina and flue-cured tobacco stem). In one
embodiment, the tobacco comprises or is composed solely of
sun-cured milled Rustica stems (i.e., N. rustica stems). The
tobacco within a tobacco composition also may have a so-called
"blended" form. For example, the tobacco within a tobacco
composition of the present invention may include a mixture of parts
or pieces of flue-cured, burley (e.g., Malawi burley tobacco) and
Oriental tobaccos (e.g., as tobacco composed of, or derived from,
tobacco lamina, or a mixture of tobacco lamina and tobacco
stem).
[0030] Portions of the tobaccos within the tobacco product may have
processed forms, such as processed tobacco stems (e.g., cut-rolled
stems, cut-rolled-expanded stems or cut-puffed stems), or volume
expanded tobacco (e.g., puffed tobacco, such as dry ice expanded
tobacco (DIET)). See, for example, the tobacco expansion processes
set forth in U.S. Pat. No. 4,340,073 to de la Burde et al.; U.S.
Pat. No. 5,259,403 to Guy et al.; and U.S. Pat. No. 5,908,032 to
Poindexter, et al.; and U.S. Pat. No. 7,556,047 to Poindexter, et
al., all of which are incorporated by reference. In addition, the
tobacco product optionally may incorporate tobacco that has been
fermented. See, also, the types of tobacco processing techniques
set forth in PCT WO 05/063060 to Atchley et al., which is
incorporated herein by reference.
[0031] In certain embodiments, the starting tobacco material can
include tobacco stems. As used herein, "stem" refers to the long
thing part of a tobacco plant from which leaves or flowers grow,
and can include the leaves, lamina, and/or flowers. In some
embodiments, it can be advantageous to use stalks and/or roots of
the tobacco plant. The tobacco stalks and/or roots can be separated
into individual pieces (e.g., roots separated from stalks, and/or
root parts separated from each other, such as big root, mid root,
and small root parts) or the stalks and roots may be combined. By
"stalk" is meant the stalk that is left after the leaf (including
stem and lamina) has been removed. "Root" and various specific root
parts useful according to the present invention may be defined and
classified as described, for example, in Mauseth, Botany: An
Introduction to Plant Biology: Fourth Edition, Jones and Bartlett
Publishers (2009) and Glimn-Lacy et al., Botany Illustrated, Second
Edition, Springer (2006), which are incorporated herein by
reference. The harvested stalks and/or roots are typically cleaned,
ground, and dried to produce a material that can be described as
particulate (i.e., shredded, pulverized, ground, granulated, or
powdered). As used herein, stalks and/or roots can also refer to
stalks and/or roots that have undergone an extraction process to
remove water soluble materials. The cellulosic material (i.e.,
pulp) remaining after stalks and/or root materials undergo an
extraction process can also be useful in the present invention.
[0032] Although the tobacco material may comprise material from any
part of a plant of the Nicotiana species, in certain embodiments,
the majority of the material can comprise material obtained from
the stems, stalks and/or roots of the plant. For example, in
certain embodiments, the tobacco material comprises at least about
90%, at least about 92%, at least about 95%, or at least about 97%
by dry weight of at least one of the stem material, the stalk
material and the root material of a harvested plant of the
Nicotiana species.
[0033] The tobacco material used in the present invention is
typically provided in a shredded, ground, granulated, fine
particulate, or powder form. As illustrated at operation 100 of
FIG. 2, the tobacco whitening process described herein can include
optionally milling a tobacco material. Most preferably, the tobacco
is employed in the form of parts or pieces that have an average
particle size less than that of the parts or pieces of shredded
tobacco used in so-called "fine cut" tobacco products. Typically,
the very finely divided tobacco particles or pieces are sized to
pass through a screen of about 18 or 16 U.S. sieve size, generally
are sized to pass a screen of about 20 U.S. sieve size, often are
sized to pass through a screen of about 50 U.S. sieve size,
frequently are sized to pass through a screen of about 60 U.S.
sieve size, may even be sized to pass through a screen of 100 U.S.
sieve size, and further may be sized so as to pass through a screen
of 200 U.S. sieve size. It is noted that two scales commonly used
to classify particle sizes are the U.S. Sieve Series and Tyler
Equivalent. Sometimes these two scales are referred to as Tyler
Mesh Size or Tyler Standard Sieve Series. U.S. sieve size is
referred to in the present application. If desired, air
classification equipment may be used to ensure that small sized
tobacco particles of the desired sizes, or range of sizes, may be
collected. In one embodiment, the tobacco material is in
particulate form sized to pass through an 18 or 16 U.S. sieve size,
but not through a 60 U.S. sieve size. If desired, differently sized
pieces of granulated tobacco may be mixed together. Typically, the
very finely divided tobacco particles or pieces suitable for snus
products have a particle size greater than -8 U.S. sieve size,
often -8 to +100 U.S. sieve size, frequently -16 to +60 U.S. sieve
size. In certain embodiments, the tobacco is provided with an
average particle size of about 0.2 to about 2 mm, about 0.5 to
about 1.5 mm, about 0.2 to about 1.0 mm, or about 0.75 to about
1.25 mm (e.g., about 1 mm).
[0034] The manner by which the tobacco is provided in a finely
divided or powder type of form may vary. Preferably, tobacco parts
or pieces are comminuted, ground or pulverized into a powder type
of form using equipment and techniques for grinding, milling, or
the like. Most preferably, the tobacco is relatively dry in form
during grinding or milling, using equipment such as hammer mills,
cutter heads, air control mills, or the like. For example, tobacco
parts or pieces may be ground or milled when the moisture content
thereof is less than about 15 weight percent to less than about 5
weight percent. The tobacco material can be processed to provide it
in the desired form before and/or after being subjected to the
whitening and/or clarification processes described herein.
[0035] In some embodiments, the type of tobacco material that is
treated (i.e., subjected to the processes described herein) is
selected such that it is initially visually lighter in color than
other tobacco materials to some degree. Accordingly, one optional
step of the method described herein comprises screening various
tobacco materials and selecting one or more of the tobacco
materials based on their visual appearance (i.e., their
"lightness," or "whiteness"). Where conducted, this screening step
can, in some embodiments, comprise a visual screening wherein
certain tobacco materials (e.g., certain tobacco types) are
selected that are visually lighter in hue than other tobacco
materials. In some embodiments, the screening can be conducted by
means of an automated operation that selects certain tobacco
materials based on predetermined characteristics (e.g., having a
lightness above a given threshold value). For example, optical
instruments (e.g., spectrophotometer/spectroreflectometer) and/or
optical sorting equipment can be used for this purpose. Such
equipment is available, for example, from Autoelrepho.RTM.
Products, AZ Technology, Hunter Lab, X-Rite, SpecMetrix, and
others.
[0036] In various embodiments, the tobacco material can be treated
to extract a soluble component of the tobacco material therefrom.
As illustrated in FIG. 2, this first treatment step can comprise a
solvent extraction at operation 105 comprising contacting the
tobacco material with a solvent (e.g., water) for a time and at a
temperature sufficient to cause the extraction of one or more
components of the tobacco material into the solvent, and separating
the extract from the residual tobacco solid material. "Tobacco
solid material" as used herein is the solid, residual tobacco
material that remains after the liquid component (i.e., tobacco
extract) is removed from the material in step 105. "Tobacco
extract" as used herein refers to the isolated components of a
tobacco material that are extracted from solid tobacco pulp by a
solvent that is brought into contact with the tobacco material in
an extraction process in step 105.
[0037] Various extraction techniques of tobacco materials can be
used to provide a tobacco extract and tobacco solid material. See,
for example, the extraction processes described in US Pat. Appl.
Pub. No. 2011/0247640 to Beeson et al., which is incorporated
herein by reference. Other exemple techniques for extracting
components of tobacco are described in U.S. Pat. No. 4,144,895 to
Fiore; U.S. Pat. No. 4,150,677 to Osborne, Jr. et al.; U.S. Pat.
No. 4,267,847 to Reid; U.S. Pat. No. 4,289,147 to Wildman et al.;
U.S. Pat. No. 4,351,346 to Brummer et al.; U.S. Pat. No. 4,359,059
to Brummer et al.; U.S. Pat. No. 4,506,682 to Muller; U.S. Pat. No.
4,589,428 to Keritsis; U.S. Pat. No. 4,605,016 to Soga et al.; U.S.
Pat. No. 4,716,911 to Poulose et al.; U.S. Pat. No. 4,727,889 to
Niven, Jr. et al.; U.S. Pat. No. 4,887,618 to Bernasek et al.; U.S.
Pat. No. 4,941,484 to Clapp et al.; U.S. Pat. No. 4,967,771 to Fagg
et al.; U.S. Pat. No. 4,986,286 to Roberts et al.; U.S. Pat. No.
5,005,593 to Fagg et al.; U.S. Pat. No. 5,018,540 to Grubbs et al.;
U.S. Pat. No. 5,060,669 to White et al.; U.S. Pat. No. 5,065,775 to
Fagg; U.S. Pat. No. 5,074,319 to White et al.; U.S. Pat. No.
5,099,862 to White et al.; U.S. Pat. No. 5,121,757 to White et al.;
U.S. Pat. No. 5,131,414 to Fagg; U.S. Pat. No. 5,131,415 to Munoz
et al.; U.S. Pat. No. 5,148,819 to Fagg; U.S. Pat. No. 5,197,494 to
Kramer; U.S. Pat. No. 5,230,354 to Smith et al.; U.S. Pat. No.
5,234,008 to Fagg; U.S. Pat. No. 5,243,999 to Smith; U.S. Pat. No.
5,301,694 to Raymond et al.; U.S. Pat. No. 5,318,050 to
Gonzalez-Parra et al.; U.S. Pat. No. 5,343,879 to Teague; U.S. Pat.
No. 5,360,022 to Newton; U.S. Pat. No. 5,435,325 to Clapp et al.;
U.S. Pat. No. 5,445,169 to Brinkley et al.; U.S. Pat. No. 6,131,584
to Lauterbach; U.S. Pat. No. 6,298,859 to Kierulff et al.; U.S.
Pat. No. 6,772,767 to Mua et al.; and U.S. Pat. No. 7,337,782 to
Thompson, all of which are incorporated by reference herein. In
certain embodiments, the solvent is added to the tobacco material
and the material is soaked for a given period of time (e.g., about
1 h); the pulp is then filtered to give a tobacco solid material
and the solvent and any solubles contained therein are filtered off
to give a tobacco extract.
[0038] The solvent used for extraction of the tobacco material can
vary. For example, in some embodiments, the solvent comprises a
solvent having an aqueous character, such as distilled water and/or
tap water. In some embodiments, the solvent can have one or more
additives and may contain, for example, organic and/or inorganic
acids, bases, or salts, pH buffers, surfactants, or combinations
thereof and may comprise minor amounts of one or more organic
solvents (e.g., various alcohols, polyols, and/or humectants). In
one particular embodiment, the solvent comprises sodium hydroxide
(NaOH) (e.g., as a 5% NaOH solution in water). In other
embodiments, the solvent can comprise an organic solvent, such as
an alcohol (e.g., ethanol, isopropanol, etc.), which can be used
alone or in combination with an aqueous solvent. Typically, the
extraction comprises adding a large excess of one or more solvents
to the tobacco material so as to produce a slurry (comprising, for
example, 50-90% by weight of the solvent), although the amount of
solvent can vary. The solvent can be at room temperature or at an
elevated temperature. For example, the solvent can be heated at a
temperature of between about room temperature and about 120.degree.
C., preferably about room temperature and about 110.degree. C.
(e.g., about 100.degree. C., about 80.degree. C., about 60.degree.
C., about 40.degree. C., or about 20.degree. C.).
[0039] In some preferred embodiments, the particulate or powder
tobacco material can be combined with water to form a moist aqueous
material (e.g., in the form of a suspension or slurry) and the
resulting material is typically heated to effectuate extraction of
various compounds. The water used to form the moist material can be
pure water (e.g., tap water or deionized water) or a mixture of
water with suitable co-solvents such as certain alcohols. In
certain embodiments, the amount of water added to form the moist
material can be at least about 50 weight percent, or at least about
60 weight percent, or at least about 70 weight percent, based on
the total weight of the moist material. In some cases, the amount
of water can be described as at least about 80 weight percent or at
least about 90 weight percent.
[0040] In certain embodiments, the tobacco material can be
extracted with water and at least one chelating agent which is
capable of removing transition metals from the tobacco material.
Chelating agents are useful to remove certain metals from the
tobacco material that could cause yellowing, and thus interfere
with the whitening process. For example, the tobacco material can
be extracted with an aqueous solution comprising
ethylenediaminetetraacetic acid (EDTA). In some embodiments, the
chelating agent can comprise diethylenetriamine pentaacetic acid
(DTPA). In various embodiments, the chelating agent(s) can be
present in an amount of about 0.01 to about 1.0 dry weight percent,
about 0.05 to about 0.5 dry weight percent, or about 0.1 to about
0.2 dry weight percent, based on the total dry weight of the
tobacco material.
[0041] The amount of time for which the tobacco material remains in
contact with the solvent can vary. For example, in some
embodiments, the tobacco material is in contact with the solvent
for about thirty minutes to about six hours (e.g., about 1 hour,
about 2 hours, about 3 hours, about 4 hours, about 5 hours, or
about 6 hours), although shorter and longer time periods can be
used. The amount of time can depend, for example, on the
temperature of the solvent. For example, less time may be required
to extract the tobacco material using solvent at a higher
temperature than that required to extract the tobacco material with
room temperature or cold solvent. The extraction process provides a
tobacco solid material and a tobacco extract.
[0042] The number of extraction steps can vary. For example, in
certain embodiments, the tobacco pulp is extracted one or more
times, two or more times, three or more times, four or more times,
or five or more times. The solvent used for each extraction can
vary. For example, in one particular embodiment, one or more
extractions are conducted using hot water; and in a final
extraction, the extraction is conducted using a basic solution
(e.g., a 5% NaOH solution). After each extraction step, the tobacco
solid material is filtered and the solvent and solubles are removed
from the tobacco solid material. In certain embodiments, the
extracts obtained from each extraction can be combined and
clarified, as described in U.S. Pat. No. 9,420,825 to Beeson et
al., which is herein incorporated by reference in its entirety. In
other embodiments, some extracts are discarded, such as extracts
from later stages. In such embodiments, for example, it may be
desirable in some embodiments to use only the tobacco extract
obtained from a first extraction of a tobacco material or to
combine tobacco extracts obtained from a first and second
extraction of a tobacco material.
[0043] Following the extraction process, the tobacco pulp is
generally isolated from the tobacco extract, for example, by
filtration or centrifugation, although these methods are not
intended to be limiting. Alternatively, in some embodiments, the
tobacco pulp can be isolated from the extract by means of
distillation (e.g., steam distillation) of the tobacco mixture
(e.g., the tobacco slurry). The process of filtration can comprise
passing the liquid through one or more filter screens to remove
selected sizes of particulate matter. Screens may be, for example,
stationary, vibrating, rotary, or any combination thereof. Filters
may be, for example, press filters or pressure filters. In some
embodiments, the filtration method used can involve
microfiltration, ultrafiltration, and/or nanofiltration. A filter
aid can be employed to provide effective filtration and can
comprise any material typically used for this purpose. For example,
some common filter aids include cellulose fibers, perlite,
bentonite, diatomaceous earth, and other silaceous materials. To
remove solid components, alternative methods can also be used, for
example, centrifugation or settling/sedimentation of the components
and siphoning off of the liquid. See, for example, the processes
and products described in U.S. Pat. App. Pub. Nos. 2012/0152265 to
Dube et al. and 2012/0192880 to Dube et al., herein incorporated by
reference in their entireties. The extracted solid components can
be used as the starting tobacco material in various embodiments of
the whitening process described herein.
[0044] In various embodiments, the tobacco material can be
hydrolyzed with at least one acid, as illustrated at operation 110
of FIG. 2, for example. Steam- or water-based pre-hydrolysis of the
tobacco material prior to pulping, for example, can reduce the
amount of chemicals necessary in a bleaching operation. Any form of
hydrolysis known in the art can be used. In certain embodiments, a
salt of a weak acid or a weak base (or both) can be dissolved in
water in a hydrolysis process. In various embodiments, tobacco
materials can undergo enzymatic hydrolysis. In certain embodiments,
the tobacco material can be hydrolyzed with sulfuric acid,
hydrochloric acid, or any other mineral or organic acid.
[0045] The tobacco material will undergo a pulping process, as
illustrated at operation 115 in FIG. 2, for example. Pulps can be
produced from raw materials either mechanically or chemically. For
example, refiner mechanical pulping techniques can be used to
produce tobacco pulp. In a mechanical pulping process, raw tobacco
materials can be chipped, and then fed between refiners where the
chips are made into fibers between revolving metal disks, for
example. See, e.g., the mechanical pulping equipment and processes
disclosed in U.S. Pat. No. 4,421,595 to Huusari and U.S. Pat. No.
7,237,733 to Vikman, WO 2010/023363, CA 1074606, and CN 201268810,
all of which are herein incorporated by reference in their
entireties.
[0046] As discussed above, in some embodiments, raw tobacco
material can be pretreated (i.e., extracted) with water for several
hours before undergoing the pulping process. The weight ratio of
water to tobacco material can be approximately 10:1 to about 4:1.
Pretreating the tobacco material (e.g., stalk and/or root
materials) can soften the starting tobacco material and remove
water soluble extracts. The pretreated mixture can then be drained
to about a 20% consistency. As used herein, the term "consistency"
is defined as the percentage of solids in a mixture. This
pretreated tobacco material can then be refined at atmospheric
pressure with a plurality of passes through a machine that can chip
the stalk. See, for example, the machines discussed in U.S. Pat.
No. 3,661,192 to Nicholson et al.; U.S. Pat. No. 3,861,602 to Smith
et al.; U.S. Pat. No. 4,135,563 to Maucher; and U.S. Pat. No.
5,005,620 to Morey, each of which is incorporated by reference
herein.
[0047] In some embodiments, a chemical pulping process can be used
to pulp and delignify the tobacco biomass at operation 115. A
chemical pulping process separates lignin from cellulose fibers by
dissolving lignin in a cooking liquor such that the lignin, which
binds the cellulose fibers together, can be washed away from the
cellulose fibers without seriously degrading the cellulose fibers.
There are three main chemical pulping processes known in the art.
Soda pulping involves cooking raw material chips in a sodium
hydroxide cooking liquor. The kraft process evolved from soda
pulping and involves cooking raw material chips in a solution of
sodium hydroxide and sodium sulfide. The acidic sulfite process
involves using sulfurous acid and bisulfate ion in the cook. The
kraft process is the most commonly used method for chemical wood
pulping; however, the soda process can also be used to produce some
hardwood pulps. Any chemical pulping process, including, but not
limited to the three examples listed above, can be used to produce
a tobacco pulp from raw tobacco materials.
[0048] A cooking liquor can comprise a strong base. As used herein,
a strong base refers to a basic chemical compound (or combination
of such compounds) that is able to deprotonate very weak acids in
an acid-base reaction. For example, strong bases that can be useful
in the present invention include, but are not limited to one or
more of sodium hydroxide, potassium hydroxide, sodium carbonate,
sodium bicarbonate, potassium carbonate, potassium bicarbonate,
ammonium hydroxide, ammonium bicarbonate, and ammonium carbonate.
In some embodiments, the weight of the strong base can be greater
than about 5%, greater than about 25%, or greater than about 40% of
the weight of the tobacco input. In certain embodiments, the weight
of the strong base can be less than about 60% or less than about
50% of the weight of the tobacco input. In still further
embodiments, the weight of the strong base can be from about 5% to
about 50%, or from about 30% to about 40% of the weight of the
tobacco input. Various other chemicals and weight ratios thereof
can also be employed to chemically pulp the tobacco input in other
embodiments.
[0049] In addition to combining a tobacco input with a strong base,
chemically pulping a tobacco input can include heating the tobacco
input and the strong base. Heating the tobacco input and the strong
base can be conducted to increase the efficacy of the chemical
pulping. In this regard, an increase in either cooking temperature
or time will result in an increased reaction rate (rate of lignin
removal).
[0050] In some embodiments, the method of producing a
tobacco-derived pulp can include one or more additional operations.
See, e.g., U.S. Patent Appl. Pub. No. 2013/0276801 to Byrd Jr. et
al., herein incorporated by reference in its entirety. For example,
the tobacco input can undergo further processing steps prior to
pulping and/or the delignification method can include additional
treatment steps (e.g., drying the tobacco input, or depithing the
tobacco input). In some embodiments, these additional steps can be
conducted to remove pith (which comprises lignin) from the tobacco
input and/or tobacco pulp manually, and thus reduce the amount of
chemicals necessary to delignify the tobacco input during a
chemical pulping process, for example. Mixing water with the
tobacco pulp to form a slurry and filtering the slurry can be
conducted, for example, to remove certain materials, such as pith,
parenchyma, and tissue from the tobacco pulp. Anthraquinone can be
employed in a chemical pulping method in an attempt to provide a
higher yield by protecting carbohydrates from the strong base
during delignification, for example. Other processing steps known
in the pulping and delignification field can be employed in forming
tobacco pulp from the raw tobacco input.
[0051] In various embodiments, a wood pulp is added to the solid
tobacco materials and/or the tobacco pulp during the overall
bleaching processes described herein. It is noted that wood pulp
can be introduced into the bleaching process at any of the steps
described herein. For example, in certain embodiments, the methods
described herein can further comprise mixing the tobacco solids
material with a wood material prior to pulping such that the wood
material is also pulped. In certain embodiments, the methods
described herein can further comprise mixing the tobacco pulp with
a wood pulp after the pulping process. In some embodiments, the
wood pulp is a bleached pulp material and can be added after the
solid tobacco materials have been pulped and bleached. If
unbleached wood pulp is used, an additional caustic extraction step
may be required, or the wood pulp can need to be added to the
tobacco pulp before the step of bleaching.
[0052] In various embodiments, the wood pulp can be market
available wood pulp. In certain embodiments, the wood pulp can be a
bleached hardwood pulp. The wood pulp added to the processes
described herein can be added in an amount of about 1 to about 20
wt. %, or about 5 to about 15 wt. %, based on the total weight of
the pulp used (i.e., the total weight of tobacco pulp and wood pulp
used). In some embodiments, the wood pulp can be added in an amount
of at least about 1 wt. %, at least about 5 wt. %, or at least
about 10 wt. %, based on the total weight of the pulp used. In
certain embodiments, the wood pulp can be added in an amount of no
more than about 5 wt. %, no more than about 10 wt. %, no more than
about 15 wt. %, or no more than about 20 wt. %, based on the total
weight of the pulp used.
[0053] Tobacco pulp that has been provided and isolated following
the extraction and pulping steps can be whitened in certain
embodiments according to any means known in the art, as shown in
step 120 of FIG. 2. It is noted that in certain embodiments, a
combination of tobacco pulp and wood pulp may undergo a whitening
step or any other process step described herein; however, for
convenience, the following description refers only to tobacco pulp.
For example, whitening methods using various bleaching or oxidizing
agents and oxidation catalysts can be used. Example oxidizing
agents include peroxides (e.g., hydrogen peroxide), chlorite salts,
chlorate salts, perchlorate salts, hypochlorite salts, ozone,
ammonia, and combinations thereof. Example oxidation catalysts are
titanium dioxide, manganese dioxide, and combinations thereof.
Processes for treating tobacco with bleaching agents are discussed,
for example, in U.S. Pat. No. 787,611 to Daniels, Jr.; U.S. Pat.
No. 1,086,306 to Oelenheinz; U.S. Pat. No. 1,437,095 to Delling;
U.S. Pat. No. 1,757,477 to Rosenhoch; U.S. Pat. No. 2,122,421 to
Hawkinson; U.S. Pat. No. 2,148,147 to Baier; U.S. Pat. No.
2,170,107 to Baier; U.S. Pat. No. 2,274,649 to Baier; U.S. Pat. No.
2,770,239 to Prats et al.; U.S. Pat. No. 3,612,065 to Rosen; U.S.
Pat. No. 3,851,653 to Rosen; U.S. Pat. No. 3,889,689 to Rosen; U.S.
Pat. No. 3,943,945 to Rosen; U.S. Pat. No. 4,143,666 to Rainer;
U.S. Pat. No. 4,194,514 to Campbell; U.S. Pat. Nos. 4,366,823,
4,366,824, and 4,388,933 to Rainer et al.; U.S. Pat. No. 4,641,667
to Schmekel et al.; and U.S. Pat. No. 5,713,376 to Berger; and PCT
WO 96/31255 to Giolvas, all of which are incorporated herein by
reference. Other whitening methods using reagents such as ozone and
potassium permanganate can also be used. See, for example, U.S.
Pat. No. 3,943,940 to Minami, which is incorporated herein by
reference.
[0054] In certain embodiments of the present invention, tobacco
pulp is whitened using a caustic reagent and/or an oxidizing agent.
In some embodiments, the tobacco pulp is whitened using both a
caustic reagent and an oxidizing agent. In such embodiments, the
caustic reagent and oxidizing agent can be provided separately or
can be combined.
[0055] The caustic reagent can vary and can be, for example, any
strong base, including but not limited to, an alkaline metal
hydroxide, alkaline earth metal hydroxide, or mixture thereof. In
certain example embodiments, the caustic reagent is sodium
hydroxide or potassium hydroxide. Alternative reagents that can be
used include, but are not limited to, ammonium hydroxide, sodium
carbonate, potassium carbonate, ammonia gas, and mixtures thereof.
The caustic reagent is generally provided in solution form (e.g.,
in aqueous solution) and the concentration of the caustic reagent
in the solution can vary. Also, the amount of caustic reagent used
in the methods of the present invention can vary. For example, in
certain embodiments, the caustic reagent is provided in an amount
of between about 1% and about 50% dry weight basis (e.g., between
about 1% and about 40% or between about 1% and about 30%) by weight
of the (dry) tobacco pulp. For example, the caustic reagent can be
provided in an amount of about 2%, about 5%, about 7%, about 10%,
or about 25% by weight of the (dry) tobacco pulp. It is noted that
the quantity of caustic reagent required may, in certain
embodiments, vary as a result of the strength of the caustic
reagent. For example, more caustic reagent may, in some
embodiments, be required where the caustic reagent is a weaker
base, whereas less caustic reagent may, in some embodiments, be
required where the caustic reagent is a strong base.
[0056] The oxidizing agent (i.e., oxidant or oxidizer) can be any
substance that readily transfers oxygen atoms and/or gains
electrons in a reduction/oxidation (redox) chemical reaction.
Peroxides (e.g., hydrogen peroxide, peracetic acid) are preferred
oxidizing agents; however, any oxidizing reagent, including, but
not limited to; other oxides (including nitrous oxide, silver
oxide, chromium trioxide, chromate, dichromate, pyridinium
chlorochromate; and osmium tetroxide); oxygen (O.sub.2); ozone
(O.sub.3); fluorine (F.sub.2); chlorine (Cl.sub.2); and other
halogens; hypochlorite, chlorite, chlorate, perchlorite, and other
halogen analogues thereof; nitric acid; nitrate compounds; sulfuric
acid; persulfuric acids; hydroxyl radicals; manganate and
permanganate compounds (e.g., potassium permanganate); sodium
perborate; 2,2'-diphyridyldisulfide; and combinations thereof can
be used according to the invention. In certain preferred
embodiments, the oxidizing reagent used according to the invention
is chlorine-free. In certain embodiments, the oxidizing reagent is
provided in aqueous solution form. The amount of oxidizing agent
used in the methods of the present invention can vary. For example,
in certain embodiments, the oxidizing agent is provided in a weight
amount of about one to fifty times the weight of the (dry) tobacco
pulp. For example, in some embodiments, the oxidizing agent is
provided in a weight amount about equal to the weight of the (dry)
tobacco pulp, about 1.3 times the weight of the (dry) tobacco pulp,
about 1.5 times the weight of the (dry) tobacco pulp, about 2 times
the weight of the (dry) tobacco pulp, or about 5 times the weight
of the (dry) tobacco pulp.
[0057] In various embodiments, the bleaching process can further
include treatment with one or more stabilizers in addition to an
oxidizing agent. For example, the stabilizer can be selected from
the group consisting of magnesium sulfate, sodium silicate, and
combinations thereof. In various embodiments, the stabilizer(s) can
be present in an amount of about 0.01 to about 3.0 dry weight
percent, about 0.1 to about 2.5 dry weight percent, or about 0.5 to
about 2.0 dry weight percent, based on the total dry weight of the
tobacco material pulp.
[0058] According to the invention, the tobacco pulp is brought into
contact with the caustic reagent and/or oxidizing agent for a
period of time. The tobacco material can be brought into contact
with the caustic reagent and oxidizing reagent simultaneously, or
can be brought into contact with the caustic reagent and oxidizing
reagent separately. In one embodiment, the oxidizing reagent is
added to the tobacco material and then the caustic reagent is added
to the tobacco material such that, after addition, both reagents
are in contact with the tobacco material simultaneously. In another
embodiment, the caustic reagent is added to the tobacco material
and then the oxidizing reagent is added to the tobacco material
such that, after addition, both reagents are in contact with the
tobacco material simultaneously.
[0059] The molar ratio of the caustic reagent to oxidizing agent
can vary. In certain embodiments where the caustic reagent is NaOH
and the oxidizing agent is hydrogen peroxide, the molar ratio of
NaOH to hydrogen peroxide is from about 1:1 to about 1:100,
preferably from about 1:5 to about 1:50, and more preferably from
about 1:10 to about 1:25. In one particular embodiment, the molar
ratio of NaOH to hydrogen peroxide is between about 1:20 and about
1:25. These ratios are not limited to ratios of NaOH and hydrogen
peroxide and could also be applicable to other caustic reagent and
oxidizing agent combinations.
[0060] The time for which the tobacco material is contacted with
the caustic reagent and/or oxidizing agent can vary. For example,
in certain embodiments, the time for which the tobacco material is
contacted with the caustic reagent and/or oxidizing agent is that
amount of time sufficient to provide a tobacco pulp material with a
lightened color as compared to the untreated tobacco material. In
certain embodiments, the tobacco material is contacted with the
caustic reagent and/or oxidizing agent overnight. Normally, the
time period is a period of at least about 10 minutes, typically at
least about 20 minutes, more often at least about 30 minutes. In
certain embodiments, the time period is a period of no more than
about 10 hours, no more than about 8 hours, no more than about 6
hours, no more than about 4 hours, no more than about 2 hours, or
no more than about 1 hour.
[0061] In certain embodiments, the tobacco material can be heated
during treatment with the caustic reagent and/or oxidizing agent.
Generally, heating the tobacco material accelerates the whitening
process. Where the tobacco material is heated during treatment,
sufficient color lightening is typically achieved in less time than
in embodiments wherein the tobacco material is unheated during
treatment. The temperature and time of the heat treatment process
will vary, and generally, the length of the heat treatment will
decrease as the temperature of the heat treatment increases. In
certain embodiments, the mixture of tobacco material, caustic
reagent, and/or oxidizing agent can be heated at a temperature of
between room temperature and about 100.degree. C. (e.g., about
90.degree. C. or about 80.degree. C.). Preferably, the mixture is
heated between room temperature and about 75.degree. C. The
heating, where applicable, can be accomplished using any heating
method or apparatus known in the art. The heating can be carried
out in an enclosed vessel (e.g., one providing for a controlled
atmospheric environment, controlled atmospheric components, and a
controlled atmospheric pressure), or in a vessel that is
essentially open to ambient air. The temperature can be controlled
by using a jacketed vessel, direct steam injection into the
tobacco, bubbling hot air through the tobacco, and the like. In
certain embodiments, the heating is performed in a vessel also
capable of providing mixing of the composition, such as by stirring
or agitation. Example mixing vessels include mixers available from
Scott Equipment Company, Littleford Day, Inc., Lodige Process
Technology, and the Breddo Likwifier Division of American
Ingredients Company. Examples of vessels which provide a pressure
controlled environment include high pressure autoclaves available
from Berghof/America Inc. of Concord, California, and high pressure
reactors available from The Parr Instrument Co. (e.g., Parr Reactor
Model Nos. 4522 and 4552 described in U.S. Pat. No. 4,882,128 to
Hukvari et al.). The pressure within the mixing vessel during the
process can be atmospheric pressure or elevated pressure (e.g.,
about 10 psig to about 1,000 psig).
[0062] In other embodiments, the heating process is conducted in a
microwave oven, a convection oven, or by infrared heating.
Atmospheric air, or ambient atmosphere, is the preferred atmosphere
for carrying out the optional heating step of the present
invention. However, heating can also take place under a controlled
atmosphere, such as a generally inert atmosphere. Gases such as
nitrogen, argon and carbon dioxide can be used. Alternatively, a
hydrocarbon gas (e.g., methane, ethane or butane) or a fluorocarbon
gas also can provide at least a portion of a controlled atmosphere
in certain embodiments, depending on the choice of treatment
conditions and desired reaction products.
[0063] In certain embodiments, before drying the bleached tobacco
pulp, the bleached tobacco pulp can be treated with an acid to
neutralize the tobacco pulp after the bleaching process to a pH in
the range of about 5 to about 11 (as illustrated at operation 125
of FIG. 2, for example), such as about 6 to about 10. The bleached
tobacco pulp can be treated with sulfuric acid, hydrochloric acid,
citric acid, or any combination thereof. Other acids known in the
art can also be used to neutralize the bleached tobacco pulp.
Following treatment with an acid, the pH of the bleached tobacco
pulp can be approximately 7.
[0064] Following treatment of the tobacco pulp with the caustic
reagent and/or oxidizing reagent, the treated tobacco pulp is
generally filtered (i.e., isolated from the caustic reagent and/or
oxidizing reagent) and dried (as illustrated at operation 130 of
FIG. 2, for example) to give a whitened tobacco pulp material. In
certain embodiments, the tobacco pulp can be dried to a moisture
level of about 1-30%, about 5-20%, or about 10-15% moisture on a
wet basis.
[0065] After drying, the whitened tobacco material can optionally
be milled a size in the range of approximately about 5 mm to about
0.1 mm, or about 1 mm to about 0.1 mm. In certain embodiments, the
whitened tobacco material can be milled to a size of less than
about 10 mm, less than about 5 mm, less than about 2 mm, or less
than about 1 mm.
[0066] After drying, the whitened tobacco material can have an ISO
brightness of at least about 50%, at least about 60%, at least
about 65%, at least about 70%, at least about 75%, or at least
about 80%. In some embodiments, the whitened tobacco material
described herein can have an ISO brightness in the range of about
50% to about 90%, about 55% to about 75%, or about 60% to about
70%. ISO brightness can be measured according to ISO 3688:1999 or
ISO 2470-1:2016.
[0067] In some embodiments, the whitened tobacco pulp thus produced
can be characterized as lightened in color (e.g., "whitened") in
comparison to the untreated tobacco pulp. Visual and/or
instrumental assessments such as those previously described can be
used to verify and, if desired, quantify the degree of lightening
achieved by way of the presently described method of the invention.
Assessment of the whiteness of a material generally requires
comparison with another material. The extent of lightening can be
quantified, for example, by spectroscopic comparison with an
untreated tobacco sample (e.g., untreated tobacco pulp). White
colors are often defined with reference to the International
Commission on Illumination's (CIE's) chromaticity diagram. The
whitened tobacco pulp can, in certain embodiments, be characterized
as closer on the chromaticity diagram to pure white than untreated
tobacco pulp.
[0068] The tobacco materials discussed in the present invention can
be treated and/or processed in other ways before, after, or during
the process steps described above. For example, if desired, the
tobacco materials can be irradiated, pasteurized, or otherwise
subjected to controlled heat treatment. Such treatment processes
are detailed, for example, in US Pat. Pub. No. 2009/0025738 to Mua
et al., which is incorporated herein by reference. In certain
embodiments, tobacco materials can be treated with water and an
additive capable of inhibiting reaction of asparagine to form
acrylamide upon heating of the tobacco material (e.g., an additive
selected from the group consisting of lysine, glycine, histidine,
alanine, methionine, glutamic acid, aspartic acid, proline,
phenylalanine, valine, arginine, compositions incorporating di- and
trivalent cations, asparaginase, certain non-reducing saccharides,
certain reducing agents, phenolic compounds, certain compounds
having at least one free thiol group or functionality, oxidizing
agents, oxidation catalysts, natural plant extracts (e.g., rosemary
extract), and combinations thereof), and combinations thereof. See,
for example, the types of treatment processes described in US Pat.
Pub. Nos. 2010/0300463 and 2011/0048434 to Chen et al., and US Pat.
8,991,403 to Chen et al., which are all incorporated herein by
reference. In certain embodiments, this type of treatment is useful
where the original tobacco material is subjected to heat in the
extraction and/or distillation process previously described.
[0069] The whitened tobacco material can be incorporated within a
smokeless tobacco product according to the present invention.
Depending on the type of tobacco product being processed, the
tobacco product can include one or more additional components in
addition to the whitened tobacco material as described above. For
example, the whitened tobacco material can be processed, blended,
formulated, combined and/or mixed with other materials or
ingredients, such as other tobacco materials or flavorants,
fillers, binders, pH adjusters, buffering agents, salts,
sweeteners, colorants, oral care additives, disintegration aids,
antioxidants, humectants, and preservatives. See, for example,
those representative components, combination of components,
relative amounts of those components and ingredients relative to
tobacco, and manners and methods for employing those components,
set forth in US Pat. Pub. Nos. 2011/0315154 to Mua et al.;
2007/0062549 to Holton, Jr. et al.; 2012/0067361 to Bjorkholm et
al.; 2017/0020183 to Bjorkholm; and 2017/0112183 to Bjorkholm; and
U.S. Pat. No. 7,861,728 to Holton, Jr. et al., each of which is
incorporated herein by reference.
[0070] The relative amount of whitened tobacco material within the
smokeless tobacco product may vary. Preferably, the amount of
whitened tobacco material within the smokeless tobacco product is
at least about 10%, at least about 25%, at least about 50%, at
least about 60%, at least about 70%, at least about 80%, or at
least about 90% on a dry weight basis of the formulation. A typical
range of tobacco material within the formulation is about 10 to
about 99%, more often about 50 to about 99% by weight on a dry
basis.
[0071] The whitened tobacco material used for the manufacture of
the smokeless tobacco products of the invention preferably is
provided in a ground, granulated, fine particulate, or powdered
form. Although not strictly necessary, the whitened tobacco
material may be subjected to processing steps that provide a
further grinding for further particle size reduction. The whitening
processes of the present invention generally provide a whitened
tobacco material with a decreased amount of high molecular weight
compounds, leading to more interstitial room and thus higher
possible water content in smokeless tobacco materials produced
therefrom than those from unwhitened tobacco materials. In certain
embodiments, the smokeless tobacco products produced according to
the invention provide for faster nicotine release than products
produced from unwhitened tobacco materials.
[0072] Example flavorants that can be used are components, or
suitable combinations of those components, that act to alter the
bitterness, sweetness, sourness, or saltiness of the smokeless
tobacco product, enhance the perceived dryness or moistness of the
formulation, or the degree of tobacco taste exhibited by the
formulation. Flavorants may be natural or synthetic, and the
character of the flavors imparted thereby may be described, without
limitation, as fresh, sweet, herbal, confectionary, floral, fruity,
or spicy. Specific types of flavors include, but are not limited
to, vanilla, coffee, chocolate/cocoa, cream, mint, spearmint,
menthol, peppermint, wintergreen, eucalyptus, lavender, cardamon,
nutmeg, cinnamon, clove, cascarilla, sandalwood, honey, jasmine,
ginger, anise, sage, licorice, lemon, orange, apple, peach, lime,
cherry, strawberry, and any combinations thereof. See also,
Leffingwell et al., Tobacco Flavoring for Smoking Products, R. J.
Reynolds Tobacco Company (1972), which is incorporated herein by
reference. Flavorings also may include components that are
considered moistening, cooling or smoothening agents, such as
eucalyptus. These flavors may be provided neat (i.e., alone) or in
a composite (e.g., spearmint and menthol, or orange and cinnamon).
Representative types of components also are set forth in U.S. Pat.
No. 5,387,416 to White et al.; US Pat. App. Pub. No. 2005/0244521
to Strickland et al.; and PCT Application Pub. No. WO 05/041699 to
Quinter et al., each of which is incorporated herein by reference.
Types of flavorants include salts (e.g., sodium chloride, potassium
chloride, sodium citrate, potassium citrate, sodium acetate,
potassium acetate, and the like), natural sweeteners (e.g.,
fructose, sucrose, glucose, maltose, mannose, galactose, lactose,
and the like), artificial sweeteners (e.g., sucralose, saccharin,
aspartame, acesulfame K, neotame, and the like); and mixtures
thereof. The amount of flavorants utilized in the tobacco
composition can vary, but is typically up to about 10 dry weight
percent, and certain embodiments are characterized by a flavorant
content of at least about 1 dry weight percent, such as about 1 to
about 10 dry weight percent. Combinations of flavorants are often
used, such as about 0.1 to about 2 dry weight percent of an
artificial sweetener, about 0.5 to about 8 dry weight percent of a
salt such as sodium chloride and about 1 to about 5 dry weight
percent of an additional flavoring.
[0073] Example filler materials include vegetable fiber materials
such as sugar beet fiber materials (e.g., FIBREX.RTM. brand filler
available from International Fiber Corporation), oats or other
cereal grain (including processed or puffed grains), bran fibers,
starch, or other modified or natural cellulosic materials such as
microcrystalline cellulose. Additional specific examples include
corn starch, maltodextrin, dextrose, calcium carbonate, calcium
phosphate, lactose, manitol, xylitol, and sorbitol. The amount of
filler, where utilized in the tobacco composition, can vary, but is
typically up to about 20 dry weight percent, and certain
embodiments are characterized by a filler content of up to about 10
dry weight percent, up to about 5 dry weight percent or up to about
1 dry weight percent. Combinations of fillers can also be used.
[0074] Typical binders can be organic or inorganic, or a
combination thereof. Representative binders include povidone,
sodium carboxymethylcellulose and other modified cellulosic
materials, sodium alginate, xanthan gum, starch-based binders, gum
arabic, pectin, carrageenan, pullulan, zein, and the like. The
amount of binder utilized in the tobacco composition can vary, but
is typically up to about 30 dry weight percent, and certain
embodiments are characterized by a binder content of at least about
5 dry weight percent, such as about 5 to about 30 dry weight
percent.
[0075] Preferred pH adjusters or buffering agents provide and/or
buffer within a pH range of about 6 to about 10, and example agents
include metal hydroxides, metal carbonates, metal bicarbonates, and
mixtures thereof. Specific example materials include citric acid,
sodium hydroxide, potassium hydroxide, potassium carbonate, sodium
carbonate, and sodium bicarbonate. The amount of pH adjuster or
buffering material utilized in the tobacco composition can vary,
but is typically up to about 5 dry weight percent, and certain
embodiments can be characterized by a pH adjuster/buffer content of
less than about 0.5 dry weight percent, such as about 0.05 to about
0.2 dry weight percent. Particularly in embodiments comprising an
extract clarified by distillation, the pH may be lowered by the
addition of one or more pH adjusters (e.g., citric acid).
[0076] A colorant may be employed in amounts sufficient to provide
the desired physical attributes to the tobacco formulation. Example
colorants include various dyes and pigments, such as caramel
coloring and titanium dioxide. The amount of colorant utilized in
the tobacco composition can vary, but is typically up to about 3
dry weight percent, and certain embodiments are characterized by a
colorant content of at least about 0.1 dry weight percent, such as
about 0.5 to about 3 dry weight percent.
[0077] Example humectants include glycerin and propylene glycol.
The amount of humectant utilized in the tobacco composition can
vary, but is typically up to about 5 dry weight percent, and
certain embodiments can be characterized by a humectant content of
at least about 1 dry weight percent, such as about 2 to about 5 dry
weight percent.
[0078] Other ingredients such as preservatives (e.g., potassium
sorbate), disintegration aids (e.g., microcrystalline cellulose,
croscarmellose sodium, crospovidone, sodium starch glycolate,
pregelatinized corn starch, and the like), and/or antioxidants can
also be used. Typically, such ingredients, where used, are used in
amounts of up to about 10 dry weight percent and usually at least
about 0.1 dry weight percent, such as about 0.5 to about 10 dry
weight percent. A disintegration aid is generally employed in an
amount sufficient to provide control of desired physical attributes
of the tobacco formulation such as, for example, by providing loss
of physical integrity and dispersion of the various component
materials upon contact of the formulation with water (e.g., by
undergoing swelling upon contact with water).
[0079] As noted, in some embodiments, any of the components
described above can be added in an encapsulated form (e.g., in the
form of microcapsules), the encapsulated form a wall or barrier
structure defining an inner region and isolating the inner region
permanently or temporarily from the tobacco composition. The inner
region includes a payload of an additive either adapted for
enhancing one or more sensory characteristics of the smokeless
tobacco product, such as taste, mouthfeel, moistness,
coolness/heat, and/or fragrance, or adapted for adding an
additional functional quality to the smokeless tobacco product,
such as addition of an antioxidant or immune system enhancing
function. See, for example, the subject matter of US Pat. Appl.
Pub. No. 2009/0025738 to Mua et al., which is incorporated herein
by reference.
[0080] Representative tobacco formulations may incorporate about
80% to about 95% percent whitened tobacco material, about 0.1% to
about 5% artificial sweetener, about 0.5% to about 2% salt, about
1% to about 5% flavoring, about 1% to about 5% humectants (e.g.,
propylene glycol), and up to about 10% pH adjuster or buffering
agent (e.g., sodium bicarbonate or citric acid), based on the total
dry weight of the tobacco formulation. The particular percentages
and choice of ingredients will vary depending upon the desired
flavor, texture, and other characteristics.
[0081] The components of the tobacco composition can be brought
together in admixture using any mixing technique or equipment known
in the art. The optional components noted above, which may be in
liquid or dry solid form, can be admixed with the whitened tobacco
material in a pretreatment step prior to mixture with any remaining
components of the composition or simply mixed with the whitened
tobacco material together with all other liquid or dry ingredients.
Any mixing method that brings the tobacco composition ingredients
into intimate contact can be used. A mixing apparatus featuring an
impeller or other structure capable of agitation is typically used.
Example mixing equipment includes casing drums, conditioning
cylinders or drums, liquid spray apparatus, conical-type blenders,
ribbon blenders, mixers available as FKM130, FKM600, FKM1200,
FKM2000 and FKM3000 from Littleford Day, Inc., Plough Share types
of mixer cylinders, and the like. As such, the overall mixture of
various components with the whitened tobacco material may be
relatively uniform in nature. See also, for example, the types of
methodologies set forth in U.S. Pat. No. 4,148,325 to Solomon et
al.; U.S. Pat. No. 6,510,855 to Korte et al.; and U.S. Pat. No.
6,834,654 to Williams, each of which is incorporated herein by
reference. Manners and methods for formulating snus-type tobacco
formulations will be apparent to those skilled in the art of snus
tobacco product production.
[0082] The moisture content of the smokeless tobacco product prior
to use by a consumer of the formulation may vary. Typically, the
moisture content of the product, as present within the pouch prior
to insertion into the mouth of the user, is less than about 55
weight percent, generally is less than about 50 weight percent, and
often is less than about 45 weight percent. For certain tobacco
products, such as those incorporating snus-types of tobacco
compositions, the moisture content may exceed 20 weight percent,
and often may exceed 30 weight percent. For example, a
representative snus-type product may possess a tobacco composition
exhibiting a moisture content of about 20 weight percent to about
50 weight percent, preferably about 20 weight percent to about 40
weight percent.
[0083] The manner by which the moisture content of the formulation
is controlled may vary. For example, the formulation may be
subjected to thermal or convection heating. As a specific example,
the formulation may be oven-dried, in warmed air at temperatures of
about 40.degree. C. to about 95.degree. C., with a preferred
temperature range of about 60.degree. C. to about 80.degree. C. for
a length of time appropriate to attain the desired moisture
content. Alternatively, tobacco formulations may be moistened using
casing drums, conditioning cylinders or drums, liquid spray
apparatus, ribbon blenders, or mixers. Most preferably, moist
tobacco formulations, such as the types of tobacco formulations
employed within snus types of products, are subjected to
pasteurization or fermentation. Techniques for pasteurizing/heat
treating and/or fermenting snus types of tobacco products will be
apparent to those skilled in the art of snus product design and
manufacture.
[0084] The acidity or alkalinity of the tobacco formulation, which
is often characterized in terms of pH, can vary. Typically, the pH
of that formulation is at least about 6.5, and preferably at least
about 7.5. In some embodiments, the pH of that formulation will not
exceed about 11, or will not exceed about 9, and often will not
exceed about 8.5. A representative tobacco formulation exhibits a
pH of about 6.8 to about 8.2 (e.g., about 7.8). A representative
technique for determining the pH of a tobacco formulation involves
dispersing 5 g of that formulation in 100 ml of high performance
liquid chromatography water, and measuring the pH of the resulting
suspension/solution (e.g., with a pH meter).
[0085] In certain embodiments, the whitened tobacco material and
any other components noted above are combined within a
moisture-permeable packet or pouch that acts as a container for use
of the tobacco. The composition/construction of such packets or
pouches, such as the container pouch 20 in the embodiment
illustrated in FIG. 1, may be varied. Suitable packets, pouches or
containers of the type used for the manufacture of smokeless
tobacco products are available under the tradenames CatchDry,
Ettan, General, Granit, Goteborgs Rape, Grovsnus White, Metropol
Kaktus, Mocca Anis, Mocca Mint, Mocca Wintergreen, Kicks, Probe,
Prince, Skruf, Epok, and TreAnkrare. The tobacco formulation may be
contained in pouches and packaged, in a manner and using the types
of components used for the manufacture of conventional snus types
of products. The pouch provides a liquid-permeable container of a
type that may be considered to be similar in character to the
mesh-like type of material that is used for the construction of a
tea bag. Components of the loosely arranged, granular tobacco
formulation readily diffuse through the pouch and into the mouth of
the user.
[0086] Descriptions of various components of snus types of products
and components thereof also are set forth in US Pat. App. Pub. No.
2004/0118422 to Lundin et al., which is incorporated herein by
reference. See, also, for example, U.S. Pat. No. 4,607,479 to
Linden; U.S. Pat. No. 4,631,899 to Nielsen; U.S. Pat. No. 5,346,734
to Wydick et al.; and U.S. Pat. No. 6,162,516 to Derr, and US Pat.
Pub. No. 2005/0061339 to Hansson et al.; each of which is
incorporated herein by reference. See, also, the types of pouches
set forth in U.S. Pat. No. 5,167,244 to Kjerstad, which is
incorporated herein by reference. Snus types of products can be
manufactured using equipment such as that available as SB 51-1/T,
SBL 50 and SB 53-2/T from Merz Verpackungmaschinen GmBH. Snus
pouches can be provided as individual pouches, or a plurality of
pouches (e.g., 2, 4, 5, 10, 12, 15, 20, 25 or 30 pouches) can
connected or linked together (e.g., in an end-to-end manner) such
that a single pouch or individual portion can be readily removed
for use from a one-piece strand or matrix of pouches.
[0087] A pouch may, for example, be manufactured from materials,
and in such a manner, such that during use by the user, the pouch
undergoes a controlled dispersion or dissolution. Such pouch
materials may have the form of a mesh, screen, perforated paper,
permeable fabric, or the like. For example, pouch material
manufactured from a mesh-like form of rice paper, or perforated
rice paper, may dissolve in the mouth of the user. As a result, the
pouch and tobacco formulation each may undergo complete dispersion
within the mouth of the user during normal conditions of use, and
hence the pouch and tobacco formulation both may be ingested by the
user. Other example pouch materials may be manufactured using water
dispersible film forming materials (e.g., binding agents such as
alginates, carboxymethylcellulose, xanthan gum, pullulan, and the
like), as well as those materials in combination with materials
such as ground cellulosics (e.g., fine particle size wood pulp).
Preferred pouch materials, though water dispersible or dissolvable,
may be designed and manufactured such that under conditions of
normal use, a significant amount of the tobacco formulation
contents permeate through the pouch material prior to the time that
the pouch undergoes loss of its physical integrity. If desired,
flavoring ingredients, disintegration aids, and other desired
components, may be incorporated within, or applied to, the pouch
material. In various embodiments, a nonwoven web can be used to
form an outer water-permeable pouch which can be used to house a
composition adapted for oral use.
[0088] The amount of material contained within each pouch may vary.
In smaller embodiments, the dry weight of the material within each
pouch is at least about 50 mg to about 150 mg. For a larger
embodiment, the dry weight of the material within each pouch
preferably does not exceed about 300 mg to about 500 mg. In some
embodiments, each pouch/container may have disposed therein a
flavor agent member, as described in greater detail in U.S. Pat.
No. 7,861,728 to Holton, Jr. et al., which is incorporated herein
by reference. If desired, other components can be contained within
each pouch. For example, at least one flavored strip, piece or
sheet of flavored water dispersible or water soluble material
(e.g., a breath-freshening edible film type of material) may be
disposed within each pouch along with or without at least one
capsule. Such strips or sheets may be folded or crumpled in order
to be readily incorporated within the pouch. See, for example, the
types of materials and technologies set forth in U.S. Pat. Nos.
6,887,307 to Scott et al. and U.S. Pat. No. 6,923,981 to Leung et
al.; and The EFSA Journal (2004) 85, 1-32; which are incorporated
herein by reference.
[0089] The smokeless tobacco product can be packaged within any
suitable inner packaging material and/or outer container. See also,
for example, the various types of containers for smokeless types of
products that are set forth in U.S. Pat. No. 7,014,039 to Henson et
al.; U.S. Pat. No. 7,537,110 to Kutsch et al.; U.S. Pat. No.
7,584,843 to Kutsch et al.; D592,956 to Thiellier; D594,154 to
Patel et al.; and D625,178 to Bailey et al.; US Pat. Pub. Nos.
2008/0173317 to Robinson et al.; 2009/0014343 to Clark et al.;
2009/0014450 to Bjorkholm; 2009/0250360 to Bellamah et al.;
2009/0266837 to Gelardi et al.; 2009/0223989 to Gelardi;
2009/0230003 to Thiellier; 2010/0084424 to Gelardi; and
2010/0133140 to Bailey et al; 2010/0264157 to Bailey et al.;
2011/0168712 to Bailey et al.; and 2011/0204074 to Gelardi et al.,
which are incorporated herein by reference.
[0090] Products of the present disclosure may be packaged and
stored in much the same manner that conventional types of smokeless
tobacco products are packaged and stored. For example, a plurality
of packets or pouches may be contained in a container used to
contain smokeless tobacco products, such as a cylindrical container
sometimes referred to as a "puck". The container can be any shape,
and is not limited to cylindrical containers. Such containers may
be manufactured out of any suitable material, such as metal, molded
plastic, fiberboard, combinations thereof, etc. If desired, moist
tobacco products (e.g., products having moisture contents of more
than about 20 weight percent) may be refrigerated (e.g., at a
temperature of less than about 10.degree. C., often less than about
8.degree. C., and sometimes less than about 5.degree. C.).
Alternatively, relatively dry tobacco products (e.g., products
having moisture contents of less than about 15 weight percent)
often may be stored under a relatively wide range of
temperatures.
[0091] Various smokeless tobacco products disclosed herein are
advantageous in that they provide a composition that is
non-staining, or is staining to a lesser degree than products
comprising only unwhitened tobacco materials. These products thus
are desirable in reducing staining of teeth and clothing that may
come in contact therewith. It is noted that even the spent (used)
product is lighter in color than traditional spent (used) oral
tobacco products. Further, the products may have enhanced visual
appeal by virtue of their whitened color.
[0092] The following examples are provided to further illustrate
embodiments of the present disclosure, but should not be construed
as limiting the scope thereof. Unless otherwise noted, all parts
and percentages are by weight.
Experimental
[0093] Embodiments of the present disclosure are more fully
illustrated by the following examples, which are set forth to
illustrate aspects of the present disclosure and are not to be
construed as limiting thereof. In the following examples, g means
gram, L means liter, mL means milliliter, and Da means daltons. All
weight percentages are expressed on a dry basis, meaning excluding
water content, unless otherwise indicated.
EXAMPLE 1
[0094] A bleached tobacco material was produced using tobacco
plants as raw material. 1.1 lbs of milled N. rustica stem tobacco
material (milled to a particle size of about 18-60 US mesh was
soaked in 15.4 lbs of water and 2.4 g of EDTA for 1 hour. The
soaked tobacco material was then pressed and drained (i.e.,
dewatered) using a screw press.
[0095] The drained and pressed tobacco material was then treated
with a caustic wash. Specifically, 10 lbs of 2.5% NaOH was added to
the pressed tobacco material. The tobacco material and caustic wash
mixture was held at about 210.degree. F. (about 100.degree. C.) for
about 90 minutes. The tobacco material in the NaOH wash was then
drained and pressed to provide a tobacco pulp and residual liquid
extract.
[0096] The tobacco pulp (1.34 lbs) was then mixed with a bleaching
solution comprising 2L water, 15 grams NaOH, and 45 grams of sodium
silicate (NaSiO.sub.3). Next, 0.9 lbs of 35% hydrogen peroxide was
added to the mixture and the mixture was cooked for 60 minutes. The
cooked mixture was allowed to sit for 30 mins, and then it was
neutralized with HC1 to bring the mixture to a pH of about 9.
Finally the mixture was dried.
EXAMPLE 2
[0097] A bleached tobacco material was produced using tobacco
plants as raw material. 1.1 lbs of finely milled burley stem
tobacco material (milled to a particle size of about 18-60 US mesh)
was soaked in 15.4 lbs of water and 2.4g of EDTA for 1 hour. The
soaked tobacco material was then pressed and drained in a screw
press.
[0098] The drained and pressed tobacco material was then treated
with a caustic wash. Specifically, 10 lbs of 2.5% NaOH was added to
the pressed tobacco material. The tobacco material and caustic wash
mixture was held at about 210.degree. F. (about 100.degree. C.) for
about 90 minutes. The tobacco material in the NaOH wash was then
drained and pressed to provide a tobacco pulp and residual liquid
extract.
[0099] The bleaching was conducted by two-stage high-consistency
bleaching with peracetic acid followed by hydrogen peroxide (P).
First, the pressed tobacco pulp was mixed with a first bleaching
solution comprising 4.5 L of water and 50 g of peracetic acid for
90 minutes. The pH of the mixture after the addition of the
peracetic acid was about 5.2. 7.0 g of NaOH was added and the new
pH was about 6.8. After about 20 mins, an additional 6.0 g of NaOH
was added to the mixture and the pH was about 8.0. The final pH of
the tobacco pulp after the bleaching with the peracetic acid was
about 8.2. The pulp was then pressed and drained in a screw
press.
[0100] The tobacco pulp, bleached with peracetic acid, was then
mixed with a second bleaching solution comprising 2 L water, 15
grams NaOH, 15 grams of magnesium sulfate (MgSO.sub.4) and 45 grams
of sodium silicate (NaSiO.sub.3). Next, 0.9 lbs of 35% hydrogen
peroxide was added to the mixture and the mixture was cooked for 60
minutes.
[0101] The cooked mixture was allowed to sit for 30 mins, and then
it was neutralized with HCl to bring the mixture to a pH of about
9. Finally the mixture was dried.
EXAMPLE 3
[0102] A bleached tobacco material was produced using tobacco
plants as raw material.
[0103] The dry weight recipe of the resulting pulp, which has no
added wood pulp, is shown in Table 1 below.
TABLE-US-00001 TABLE 1 Recipe for Tobacco Pulp with No Wood Pulp
Added Material Dry Weight Percentage Range EDTA 0.01-0.5% Caustic
Soda 20-30% Citric Acid 25-35% Sodium Silicate 0.5-2% Hydrogen
Peroxide 15-20% Defoamer 0.01-0.5% Rustica Stem 25-30%
[0104] First, tobacco biomass was extracted with hot water. About
75 lbs. of milled Rustic stem was weighed out. About 600 lbs. of
hot water (about 212.degree. F.) was added to a tank. An agitator
was turned on in the tank, it was ensured that the discharge valve
on the tank was closed, and the milled Rustica stem was added to
the tank. Next, about 187.5 g of EDTA was weighed out and added to
the tank. The steam drain on the tank was opened and steam was
applied to the tank. Once the temperature of the liquid in the tank
reached about 180-215.degree. F., the contents of the tank were
mixed for 50 mins while steam was still being added to the tank.
After 50 minutes, the steam into the tank was cut off. The contents
of the tank were then mixed for an additional 10 minutes. After
mixing, the liquid in the tank was discharged and the remaining
Rustica stem was rinsed and drained using a basket centrifuge.
Alternative dewatering equipment can also be used. In particular,
it is noted that a screw press was used for recipes that included
wood pulp, while a basket centrifuge was used for recipes with no
added wood pulp.
[0105] Next, the tobacco biomass was caustically extracted. About
600 lbs. of water was added to the tank. An agitator was turned on
in the tank and it was ensured that the discharge valve on the tank
was closed. About 37.5 lbs. of sodium hydroxide powder was measured
and added to the tank. The steam drain on the tank was opened and
steam was applied to the tank. Once the temperature of the liquid
in the tank reached about 200-215.degree. F., the contents of the
tank were then held at about 212.degree. F. and mixed for about 90
mins while steam was still being added to the tank. After 90
minutes, the steam into the tank was cut off. About 50.0 lbs. of
citric acid powder was then measured and slowly added to the tank.
The contents of the tank were then mixed for an additional 10
minutes. The pH of the contents of the tank was measured and
adjusted until the pH was in the range of about 9.0 to about 10.5.
After mixing, the liquid in the tank was discharged and the
remaining tobacco cake was rinsed and drained using a basket
centrifuge. About 100 lbs. of water can be used to rinse the
residual pulp and the rinsing and dewatering steps can be repeated
if necessary.
[0106] Next, the tobacco biomass was subjected to a peroxide
bleaching process. The discharge valve of the tank is closed and
about 600 lbs. of hot water (about 180.degree. F.) was added to the
tank. The steam drain on the tank was opened and steam was applied
to the tank. The agitator for the tank was turned on. The rinsed
and dewatered tobacco cake was then added to the tank. About 22.5
lbs. of sodium hydroxide powder was measured and added to the tank.
About 7.5 lbs. of 40% sodium silicate was measured and added to the
tank. About 127.5 lbs. of 36% peroxide was measured and added to
the tank. A pump at 20 psi was run to the tank for about 1 minute
with the ball valve wide open and then flushed with about 12
gallons of water. The steam drain on the tank was opened and steam
was applied to the tank. Once the temperature of the liquid in the
tank reached about 165.degree. F., the liquid began to foam. About
30 grams (or more) of defoamer can be added as necessary to keep
the foam contained in the tank. After the temperature of the liquid
in the tank reached about 180.degree. F., the steam was turned off
and the contents of the tank were mixed for about 30-60 mins. Next,
about 34.0 lbs. of citric acid powder was measured and added to the
tank. The contents of the tank were then allowed to mix for about
10 minutes. The pH of the contents of the tank was then measured
and adjusted until the pH was in the range of about 10.0 to about
10.75. After mixing, the liquid in the tank was discharged and the
remaining tobacco cake was rinsed and drained using a screw press
and/or centrifuge. About 100 lbs. of water can be used to rinse the
residual pulp and the rinsing and dewatering steps can be repeated
if necessary. The final tobacco cake can be dried to a moisture
content of about 10-15% moisture.
EXAMPLE 4
[0107] A bleached tobacco material was produced using tobacco
plants as raw material. The dry weight recipe of the resulting
pulp, which has wood pulp added, is shown in Table 2 below.
TABLE-US-00002 TABLE 2 Recipe for Tobacco Pulp with Added Wood Pulp
Material Dry Weight Percentage Range EDTA 0.01-0.5% Caustic Soda
20-30% Citric Acid 25-35% Sodium Silicate 0.5-2% Hydrogen Peroxide
15-20% Defoamer 0.01-0.5% Rustica Stem 25-30% Wood Pulp (Bleached
Hardwood Kraft) 1-5%
[0108] The extraction and bleaching processes used above in Example
3 were also used for bleaching the tobacco biomass with the added
wood pulp. However, as noted above, a screw press was used for
dewatering/drying the pulp at various points in the process instead
of a basket centrifuge.
EXAMPLE 5
[0109] The bleached tobacco material of Example 3 (no added wood
pulp) and the bleached tobacco material of Example 4 (with added
wood pulp) was tested for ISO brightness using TAPPI standardized
test T 534.
[0110] Two samples of bleached tobacco pulp according to Example 3
(no added wood pulp) were tested and had an ISO brightness of 67.6%
and 63.8%. One sample of bleached tobacco pulp according to Example
4 (with added wood pulp) was tested and had an ISO brightness of
70.1%.
[0111] Many modifications and other embodiments will come to mind
to one skilled in the art to which this disclosure pertains having
the benefit of the teachings presented in the foregoing
description. Therefore, it is to be understood that the disclosure
is not to be limited to the specific embodiments disclosed and that
modifications and other embodiments are intended to be included
within the scope of the appended claims. Although specific terms
are employed herein, they are used in a generic and descriptive
sense only and not for purposes of limitation.
* * * * *