U.S. patent number 3,561,451 [Application Number 04/639,032] was granted by the patent office on 1971-02-09 for process of manufacturing reconstituted tobacco of light color.
This patent grant is currently assigned to American Machine and Foundry Company. Invention is credited to Joseph Fiore, Harry Jacin.
United States Patent |
3,561,451 |
Jacin , et al. |
February 9, 1971 |
PROCESS OF MANUFACTURING RECONSTITUTED TOBACCO OF LIGHT COLOR
Abstract
A process of treating tobacco in the manufacture of
reconstituted tobacco is disclosed wherein the color of the
finished reconstituted product is lightened by the removal of basic
polyphenols present in the starting batch. The process involves
washing the tobacco with water to form an aqueous extract thereof,
separating the extract and treating it with absorbent agents such
as activated alumina or polyamids to remove the basic polyphenols
and finally reincorporating the extract minus the removed
polyphenols into the fibrous tobacco mass.
Inventors: |
Jacin; Harry (Norwalk, CT),
Fiore; Joseph (Fairfield, CT) |
Assignee: |
American Machine and Foundry
Company (N/A)
|
Family
ID: |
24562448 |
Appl.
No.: |
04/639,032 |
Filed: |
May 17, 1967 |
Current U.S.
Class: |
131/297;
131/370 |
Current CPC
Class: |
A24B
15/12 (20130101) |
Current International
Class: |
A24B
15/00 (20060101); A24B 15/12 (20060101); A24b
003/14 (); A24b 015/08 () |
Field of
Search: |
;131/15,17,140--144 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Rein; Melvin D.
Claims
We claim:
1. The method of removing basic polyphenols from tobacco which
comprises treating tobacco with water to create an aqueous solution
in which the water soluble components of tobacco including basic
polyphenols are extracted from the fibrous components thereof,
separating the said aqueous solution containing the
basic-polyphenols from the extracted tobacco, removing a material
portion of said basic-polyphenols from the extract solution by
passing said solution into contact with an adsorbent material
selected from the group consisting of activated alumina and
polyamids, separating the solution from the adsorbent material, and
finally combining the said extract solution from which the
basic-polyphenols have been removed with the fibrous extracted
tobacco so as to form an aqueous tobacco mixture which includes
extracted water soluble components of the original tobacco minus a
material amount of the basic-polyphenols originally therein.
Description
The present invention relates to a method for the preparation of
reconstituted tobacco sheet and more particularly to an improved
process for preparing light colored reconstituted tobacco sheet,
despite the use of heat as a processing aid at any step of the
process.
The commercial method for the manufacture of reconstituted tobacco
sheet requires the application of heat at some stage in the
processing e.g. either in the preparative stages and/or in the
drying. It is known that the color of the finished tobacco product
darkens because of the heating; the level of darkening being a
function of temperature and heating time. As a rule, it is
desirable to produce a light colored tobacco sheet and various
steps are taken to achieve this goal, for example, the addition of
dyes or coloring chemicals, the addition of color masking agents
("whiteners") such as titanium dioxide or Dicalite, or control of
temperature and heating time. These steps are never completely
satisfactory because of the limitations under which they can be
applied. In the case of the addition of dying, coloring and masking
chemicals, the introduction of extraneous material can be
undesirable, especially if excessive amounts are needed to produce
the desired results. Excessive use of dyes can produce "leaching"
problems while excessive use of "whiteners" can result in sheets
which are greyish in appearance or lack proper physical structure.
In the case of controlled temperature and heating time, undesirable
limits are put upon the manufacturing procedures. The invention
herein revealed makes it possible to produce a light colored,
reconstituted tobacco sheet without the resort to dyes for color
preservation and without any undue limitations on the temperature
and heating time used in the process. This is achieved by
selectively removing from the tobacco the agents responsible for
the darkening of the tobacco on heating.
In the preparation of additive reconstituted tobacco, tobacco, such
as stems, field scrap, cuttings, whole leaf and the like, is
preferably uniformly comminuted and formed into tobacco sheet
suitable for later machine processing. On the other hand, in the
preparation of all-tobacco reconstituted sheet or in reconstituted
sheets wherein a more efficient utilization of the natural gums of
the tobacco is desired, the tobacco is usually ground to
colloid-forming size particles by a wet process or refining.
However, the large amount of energy and time required for the
preparation of these colloid-forming size tobacco particles has
limited its use for the preparation of reconstituted sheets.
To reduce the energy expended and time involved to comminute the
tobacco particles in the wet process, it is desirable to cook the
tobacco prior to refining. This cooking operation reduces the
refining time and simultaneously improves the physical properties
of the finished product. However, the cooking causes darkening of
the tobacco and hence darkens the sheets made from this cooked
tobacco material, thereby making such sheets unacceptable in a
number of manufactured tobacco products.
Many attempts have been made heretofore to produce reconstituted
tobacco sheets using heat at some stage in the processing without
the adverse darkening of the tobacco, using various techniques and
methods, but, in general, such attempts have met with only limited
commercial success. For example, it has been known in the art, that
washing the tobacco products with water prior to treatment,
replacing the washings with fresh water and then cooking the washed
tobacco gives a relatively acceptable product with respect to
color. However, it is unsatisfactory from an economic standpoint,
since the discarded washings contain a large quantity of useful
tobacco product.
The present invention provides a solution to this longstanding
problem, and results in a great reduction in energy and time
required to obtain good quality reconstituted tobacco sheets of
acceptable color.
A further object of the present invention is to provide a method
for producing a light colored reconstituted tobacco sheet despite
the use of heat as a processing aid.
A still further object of the present invention is to remove
polyphenols from the tobacco prior to exposure of the tobacco-water
mixture to heat in the preparation of the reconstituted tobacco
sheet without resort to dyes and color chemical additives to the
tobacco.
Another object of the present invention is to remove from the
tobacco prior to exposure of the tobacco-water mixture to heat,
only the agents causing the darkening of the tobacco and leaving
all other valuable material in the tobacco, without adding anything
to the tobacco, so as to provide a light colored tobacco sheet.
Still another object of the present invention is to provide a
method for accomplishing all of the above, which can be used in
processing large quantities of tobacco resulting in a reconstituted
sheet of tobacco having an acceptable color and to do so in an
economical and easily controlable method.
Other objects and advantages of the present invention will be
apparent from the further reading of the specification and of the
appended claims.
Tobacco as defined for this invention includes any type of tobacco
suitable for the manufacture of reconstituted tobacco sheet, such
as stem, veins, scrap and waste tobacco, cuttings and the like, as
well as whole leaf or portions thereof.
In general, the method of the present invention discloses a method
of removing from the tobacco washings the agents responsible for
the darkening of the tobacco when it is exposed to heat. The
treated washings are then returned to the tobacco being processed,
and the product prepared in a conventional manner to provide a
reconstituted tobacco sheet of good physical properties without
detriment to the sheet color.
It has long been commonly believed that the agents responsible for
the darkening of the tobacco on cooking were the carbohydrates and
the amino acids, which react during the heating to form dark
colored compounds, the process being called the "Maillard"
reaction. We have discovered that neither the carbohydrates nor the
amino acids darken the tobacco significantly on heating, but that
polyphenols contained in the tobacco, especially the
basic-polyphenols, do cause a significant darkening of the tobacco
upon exposure to heating. This phenomenon is also pH dependent.
A series of tests were run to isolate and determine the agents
which caused tobacco darkening upon heating. The following
procedure illustrates how the polyphenols were identified as the
agents which cause tobacco darkening during heating. A sample of
"Bright" stem dust weighing 10 g. was mixed with 90 ml. of
distilled water. The slurry was filtered on a Buchner funnel using
Whatman No. 1 filter paper. The filter cake and filtrate were
retained. The filter cake was subsequently mixed with 90 ml. of a
predetermined liquid and the slurry transferred to a vessel, such
as a mason jar, which was sealed and placed in a pressure cooker,
where it was heated at 250.degree. F. at 15 p.s.i. for 2 hours.
Upon cooling, three sheets having a thickness of about 0.25--0.30
mm. were cast from the slurry on 20 cm. x 20 cm. glass plates. The
sheets were dried in an oven at 110--115.degree. C. for about
15--20 minutes and the color of each sheet was read in a Gardner
automatic color difference meter, Model AC-2 A, Series 200.
Readings were made by placing the plate over the Gardner aperture
with the tobacco side facing the aperture. A number of readings
were taken at different points on each plate so as to obtain an
overall average.
The test results in table 1 were obtained with various additives in
the predetermined liquid and serve to illustrate that polyphenols
are the agents causing the darkening of the tobacco on exposure to
heat. Water-washed Bright stem dust was used in all cases, unless
otherwise indicated. The weight of the washed tobacco in each
sample was 7 g. dry weight and this was suspended in 90 ml. of
liquid prior to heating. ##SPC1## ##SPC2## continued The polyphenol
fractions shown in table I were obtained as follows: 90 ml. of a
tobacco-water extract, prepared as described above, was mixed with
20 ml. of a 10 percent lead acetate solution, and the formed
precipitate was removed by centrifugation. This precipitate
comprised the acidic polyphenol fraction.
Adding more lead acetate solution to the supernatant caused no more
precipitation. An alkaline reagent, such as ammonium hydroxide
(NH.sub.4OH) was added to the supernatant until the pH was about
8.5--9. The formed precipitate, which was collected by
centrifugation, constituted the basic polyphenol fraction.
As seen from the experimental results shown in table I, the basic
polyphenols make a sheet darker than even the negative control (Rd
readings 12.4 and 16.4, respectively). Furthermore, it is seen that
while acidifying the basic polyphenols improves the color, it is
still far below the positive control (Rd readings of 17.2 and 24.9,
respectively). These results show that the sugars and amino acids
do not affect the sheet color and similarly neither does the lead
acetate solution used to precipitate the polyphenols.
Processes for the neutralization or removal of the polyphenol from
tobacco with the addition of chemical substances are fully
disclosed and described in our copending application, Ser. No.
639,066 filed even date herewith. The present disclosure confines
itself to the removal of polyphenols without chemical
substances.
In order to extract the basic polyphenols from the tobacco without
adding any chemical additive to the reconstituted tobacco sheet,
the tobacco water washings can be treated with adsorbent material,
which adds nothing to the extract, but selectively removes the
darkening agent or agents by adsorption. For example, tobacco water
washings are passed through a column containing a selected
adsorbent material, such as activated alumina. The adsorbent
removes the darkening material, but leaves the other valuable
tobacco constituents unchanged in the extract. The treated extract
is then recombined with the original washed tobacco and the
combination is processed into reconstituted tobacco sheet, which
retains its commercially acceptable light color with no
additives.
In accordance with the present invention, untreated tobacco, such
as broken leaves, cuttings, stemmings, various fragments or waste,
field scrap, is subjected to a water extraction operation so as to
separate the water-soluble constituents.
The water-soluble constituents of the tobacco or extract are
separated from the insoluble portion by any convenient process,
such as draining, pressing, or centrifuging. The aqueous extract
contains various water-soluble materials, including polyphenols.
This aqueous extract can then be passed through a column containing
an adsorbent material, such as activated alumina. Continuous
operation in a column can be effected by placing the adsorbent
material and passing the aqueous extract continuously through a
column. The adsorbent material removes the color-forming bodies,
but leaves the other valuable tobacco constituents unchanged in the
column effluent. The effluent is then recombined with the original
washed tobacco and the combination is processed in a conventional
form and a light colored reconstituted tobacco sheet is produced.
The extracted coloring materials can be eluted from the adsorbent
so that it can be reused as desired.
The following examples are set forth to demonstrate the method of
this invention.
A glass column (25 cm. x 3 cm.) was filled with a slurry of 100 gm.
of activated alumina (8--14 mesh) in water. The water was allowed
to drain and the column was washed repeatedly with about 500--1000
ml. fresh water. A water extract of tobacco dust obtained by the
method described previously was passed over the column at a flow
rate such that effluent was collected at 0.5 ml. per minute. The
column was then washed with water until the washings were
colorless. The combined water washings and collected effluent were
then concentrated to 100 ml. under vacuum in a flash evaporator
using a temperature range of 36--38.degree. C. The solids content
in the concentrate, as well as in the original water tobacco
extract were determined and the recovery of material from the
column calculated from these values. The test results are presented
in table 2. ##SPC3##
The figures in table 2 show that the solids recovery is 73--75
percent for Bright stem extracts and 89--91 percent for Penn. stem
extracts.
The material not removed from the column by water washing was
eluted off by passing 2 normal formic acid through the column.
Fractions were collected at a rate of 0.5 ml. per minute. The
eluted samples were very dark in color. The 2 normal formic acid
removed all the adsorbed material leaving the activated alumina
free of color. The alumina was washed with water until free of
acid, dried in the oven (130--140.degree. C.) overnight and used
again.
The formic acid was removed from the eluate (i.e., the
basic-polyphenols) by evaporation under vacuum in a flash
evaporator. The remaining dark brown material was made up to a 100
ml. volume with water and tested for carbohydrates by a thin layer
chromatography method, such as described in the Journal of
Chromatography 18, 170--174 (1965 ). Samples of the effluent
concentrate from the column previously referred to as well as the
original tobacco-water extract were also examined for
carbohydrates. The results showed that practically all of the
carbohydrates found in the original tobacco-water extract were
recovered in the concentrated effluent while only significant
amounts were found in the formic acid eluate.
It should be noted that the material, which could not be removed
from the column by water could be eluted off by other suitable
solvents, such as 50 percent ethanol containing 2 normal HCl or by
2 normal HCl solution. Advantageously, formic acid is preferred,
since it is easily removed by evaporation under vacuum. This makes
it possible to recover the solids from the formic acid eluate and
their subsequent utilization in the color experiments. In an
operation where these solids are of no consequence, their removal
from the alumina would be carried out more economically with a 2
normal HCl solution.
The effluent concentrates were made up to volume and recombined
with the washed tobacco. The slurries were treated in a manner as
described above. The obtained sheets were examined in a Gardner
colorimeter, and the results are presented in table 3. ##SPC4##
The figures in table 3 show that the effluent concentrate from the
adsorbent column is similar in its color properties to the positive
control, while the formic acid eluate, after removing the formic
acid and adjusting to volume with water, is similar to the negative
control. This is particularly apparent in the Rd values.
Adsorbents, other than activated alumina, were examined.
Regenerated alumina worked as well as unused alumina. Polyamide and
silica gel also gave satisfactory results.
Other adsorbent materials could be used, such as magnesol, silicic
acid or adsorption alumina, and the like. However, these materials
are fine meshed and pack easily in the columns, so as to reduce
flow through the columns. A pressure source would be necessary to
obtain satisfactory flow through columns using these adsorbent
materials. It is understood that the preferred adsorbents need not
be used in a column. They can also be employed effectively in
slurry-type removal polyphenols.
By the practice of the present invention, there is produced a
reconstituted tobacco sheet using heat, which contains all the
desirable portions of the original tobacco, and which is lighter in
color than sheets made of untreated tobacco.
Various changes and modifications may be made in practicing this
invention without departing from the spirit and scope thereof, and
therefore, the invention is not to be limited, except as defined in
the appended claims.
* * * * *