U.S. patent number 3,800,808 [Application Number 05/202,148] was granted by the patent office on 1974-04-02 for tobacco smoke filter.
This patent grant is currently assigned to Brown & Williamson Tobacco Corporation. Invention is credited to James R. Hammersmith, Martin Lance Reynolds.
United States Patent |
3,800,808 |
Reynolds , et al. |
April 2, 1974 |
TOBACCO SMOKE FILTER
Abstract
An improved tobacco smoke filter is provided for cigarettes and
the like formed of a bed or rod of shreds of a porous cellulose
ester material having a low packing density and an increased
surface area which is readily accessible to the smoke aerosol for
deposition of smoke particles. The filter draw resistance comprises
a pressure drop at or below 2.5 inches of water. The cellulose
ester material in shred form has a surface area of from about 0.6
to 3.0 square meters per gram, a mean pore diameter of from about 2
to 20 microns, and a porosity of between 65 percent and 90 percent.
The width and thickness of the shreds should be between about
0.25-2.0 mm and 0.025-0.25 mm, respectively. The shreds are formed
by casting a dope of the cellulose ester dissolved in solvent and
plasticizer in which starch and saline solution are present. The
cast sheet is washed to remove the salt and enzymatically treated
to remove the starch and thus form the porous structure.
Inventors: |
Reynolds; Martin Lance
(Anchorage, KY), Hammersmith; James R. (Jeffersonville,
IN) |
Assignee: |
Brown & Williamson Tobacco
Corporation (Louisville, KY)
|
Family
ID: |
22748677 |
Appl.
No.: |
05/202,148 |
Filed: |
November 26, 1971 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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33621 |
May 1, 1970 |
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849384 |
Aug 12, 1969 |
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Current U.S.
Class: |
131/343 |
Current CPC
Class: |
A24D
3/10 (20130101) |
Current International
Class: |
A24D
3/00 (20060101); A24D 3/10 (20060101); A24d
001/04 () |
Field of
Search: |
;131/261-269,10 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Rein; Melvin D.
Attorney, Agent or Firm: Finnegan, Henderson, Farabow &
Garrett
Parent Case Text
CROSS REFERENCE TO RELATED APPLICATION
This application is a Continuation-in-Part of our United States
patent application Ser. No. 33,621 filed May 1, 1970, now abandoned
which was a Continuation-in-Part of our United States patent
application Ser. No. 849,384 filed Aug. 12, 1969, entitled "Tobacco
Smoke Filter," now abandoned.
Claims
Having thus described the invention, what is claimed is:
1. A tobacco smoke filter comprising:
a section formed of dried shreds of porous cellulose ester selected
from the group consisting of cellulose acetate, cellulose
propionate, and cellulose butyrate,
said shreds having a width of about 0.25 to 2.0 mm. and a thickness
of about 0.025 and 0.25 mm., a porosity greater than 65 percent and
up to about 90 percent, a filtration efficiency of at least 65
percent up to about 71 percent, and
a surface area of between 0.6 and 3.0 square meters per gram,
said shreds being made by forming a dope of cellulose ester
dissolved in solvent and plasticizer and in which there is starch
and saline solution whereby a sheet cast from said dope is
shredded, washed to remove the salt, and enzymatically treated to
remove said starch to form porous shreds, a ratio of said starch to
said cellulose ester being above 2:1 and up to 4:1.
2. The invention in accordance with claim 1 wherein the bulk
density of said materials is from about 0.05 to 0.40 grams per
cubic centimeter.
3. The invention of claim 1 wherein said constituent shreds are
characterized by a mean width of about 1.0 mm and a mean thickness
of 0.03 mm.
4. The invention in accordance with claim 1 wherein said porous
constituent shreds are bonded to one another at random points.
Description
BACKGROUND OF THE INVENTION
The reduction in tar delivery which can be achieved with
conventional cigarette filters is limited by the necessity of
maintaining an acceptable cigarette pressure drop while, at the
same time, maintaining the quality of the smoke. A continuing
search has been made both within, and outside, the tabacco industry
for more efficient cigarette filters.
Heretofore attempts to incorporate porous materials into cigarette
filters to increase the filter's efficiency have met with only
limited success in that they have not proven highly efficient in
tar removal at acceptable pressure drops. Such prior art filter
materials include, for example, activated charcoal in granular
form, as a self-sustaining bonded rod or incorporated on fibers or
web material, activated alumina, silica gel and various types of
synthetic resins in granular form.
SUMMARY OF THE INVENTION
It is the principal object of the present invention to provide an
improved cigarette filter cellulose ester material capable of
filtering a smoke aerosol at acceptable pressure drops of at or
below 2.5 inches of water with a high degree of efficiency so as to
remove at least 60% of the tar from the aerosol without adversely
affecting the tobacco flavor.
Another object is to provide such a cellulose ester material which
can be produced at a sufficiently low cost so as to enable the same
to be competitive with existing filter materials.
These and other beneficial objects and advantages are attained in
accordance with the present invention by providing a filter
constituent formed of porous cellulose ester shreds have a surface
area between 0.6 and 3.0 square meters per gram, a porosity of
between 65 percent and 90 percent and a mean pore diameter of from
about 2 to 20 microns. The width and thickness of the shreds should
preferably be between about 0.25-2.0 mm and 0.025-0.25 mm,
respectively. The individual filter shreds are packed in abutting
proximity with one another to form a bed or a rod so as to provide
a tortuous path for the smoke aersol.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawing:
FIG. 1 is a cross-sectional view of a cigarette provided with a
filter incorporating the porous material of the present
invention.
FIG. 2, which is a view similar to FIG. 1, depicts a cigarette
filter employing the porous material of the present invention with
a conventional mouthpiece.
FIG. 3 is a scanning electron microscope photograph at 500X
magnification showing the porous nature of the material.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1 a cigarette 10 is provided with a filter 12 utilizing the
porous cellulose ester shreds of the present invention. The
cigarette includes a tobacco rod 14 comprising tobacco material 16
contained within a paper tube 18 to which the filter 12 is secured.
The filter 12 contains the porous cellulose ester shreds 20
contained within a wrap 22. An outer wrap 24, which may be formed
of paper or cork, overlies the entire filter and extends somewhat
beyond the tabacco rod-filter interface. If desired, the shreds may
be bonded to one another at random points with a conventional
plasticizer such as, for example, triethylene glycol.
The porous cellulose ester shreds 20 are formed having physical
characteristics defined by a surface area of between about 0.6
square meters per gram and about 3.0 square meters per gram, a
porosity of between 65 percent and 90 percent, and a mean pore
diameter of from about 2 to 20 microns. It is preferred, however,
that the surface area range from about 1 to 3 sq. meters per gram.
The porosity of the cellulose ester material is the percentage of
the total volume occupied by voids contained within each particle
related to the total volume of the particle. The approximate
relationship between pore volume, pore diameter, and surface area
is defined by the following equation (assuming cylindrical
pores):
Volume of Pores (in cc/gm)/Surface area (cm.sup.2 /gm) = 0.25 Pore
Diameter (in cm)
The lengths of the individual shreds should be at least 0.5 mm and
should vary from about 0.5 mm to 20 mm; the width of the individual
shreds should vary from about 0.25 mm to 2 mm; and the thickness of
the individual shreds should vary from about 0.025 to 0.25 mm. Good
results were obtained using porous shreds of cellulose acetate
having a mean thickness of 0.03 mm and a mean width of 1.0 mm. The
cross-sectional configuration of the individual shreds is not
critical, although ribbon-shaped shreds are preferred.
The filter efficiency and draw resistance of the filter bed is
also, of course, related to the bulk density of shreds within the
bed and in this connection the shred bulk density should lie
between 0.05 and 0.40 grams per cc and preferably between 0.09 and
0.30 grams per cc to provide pressure drops across the filter
section of approximately 2 to 2.5 inches of water. The shreds are
packed into abutting proximity with one another and, thus, unlike
granular filter material, have a high degree of
self-cohesiveness.
Various cellulose esters may also be employed, as, for example,
porous cellulose propionate, porous cellulose butyrate or the like.
Porous cellulose acetate is the preferred cellulose ester because
consumers have become accustomed to the taste of smoke drawn
through a cellulose acetate filter.
FIG. 2 depicts a cigarette 32 provided with a filter 34 formed of a
shredded porous cellulose ester 36 in accordance with an alternate
embodiment of the present invention. The filter 34 comprises two
sections, tobacco section 35 formed of shredded porous cellulose
ester 36 abutting the tobacco rod 14 and mouthpiece section 37. The
mouthpiece section may be made from conventional fibrous material
such as cellulose acetate tow. The porous material 36 of the
tobacco section 35 of the filter possesses the same physical
characteristics set forth previously.
FIG. 3 illustrates pictorially the porous nature of the shredded
material which here is cellulose acetate. The photograph is at 500X
magnification.
Porous materials in accordance with the present invention may be
manufactured from cellulose esters by encasing a starch with the
ester, swelling the starch and then removing the starch by
enzymatic and/or chemical hydrolysis or by solubilizing the starch
by cooking in water and draining off the solution. This process
provides porous cellulose esters having the desired surface area
and mean pore diameter. The porous cellulose esters are made as
shreds of the desired width and thickness and, thus, may be formed
into filter elements by employing standard cigarette making
machinery.
For a better description and understanding of the method for making
synthetic porous cellulose esters having the characteristics of the
invention herein, the following examples are provided. In each
example, the starch utilized was one which, upon swelling, produced
a pore of from 2 to 20 microns. Since the swelling rates of the
starches utilized was of the order of 100 percent, the initial
starch particle size was from 1 to 10 microns. Also, in each of the
following examples, the enzyme used was an alpha-amylase of
bacterial origin commercially available under the trade name TENASE
from Miles Laboratories. The "parts" of the examples are parts by
weight.
EXAMPLE I
One hundred parts of cellulose acetate were dissolved in a solution
of 800 parts acetone and 20 parts plasticizer (6 parts triethylene
glycol diacetate, 5 parts polyethylene having a molecular weight of
600), this amount being 20 percent of the cellulose acetate weight.
The resulting dope was stirred for 30-40 minutes until all the
cellulose acetate had been dissolved. A warm salt solution of about
80.degree. C. comprising 30 parts sodium chloride and 90 parts
water was slowly mixed into the dope before blending in 300 parts
corn starch. The resulting mixture was stirred for about one hour,
after which the mixture was rolled into a sheet at thickness 80-85
percent of that desired for the final product.
The dried sheet was cut into shreds about 29 cuts per inch, using a
guillotine cutter similar to the type employed for making tobacco
shreds from the tobacco leaf. The irregular, flaked and powdered
material was separated from the shredded material by screening. The
shredded material, 1 part by weight, was suspended in 4 parts of
0.02 molar calcium chloride, and the resulting slurry adjusted to
pH 7 with sodium hydroxide to approximately 0.02M. The slurry was
heated in a pressurized vessel at about 120.degree. C. and 15 psi
for about 30 minutes to expand the starch and to rupture the pore
walls. The slurry was then cooled to 88.degree.-95.degree. C. Since
the slurry was previously adjusted for enzymatic conditions, 0.003
parts of a concentrated alpha-amylose (TENASE - Miles Laboratories)
solution was added for solubilization of the starch. To effect
solubilization of the starch, the temperature was maintained at
between 88.degree. and 92.degree. C. with occasional agitation.
Solubilization of the starch was substantially completed after 50
to 60 minutes. The solubles were drained from the shredded material
which was then thoroughly washed with hot tap water, then spread
out to dry under ambient conditions. The dry shredded porous
cellulose acetate was air fluffed and screened to break up roped
material and long strands. The mean shred size obtained after
selectively sieving the dry material was found to be 0.88 mm in
width and 0.0305 mm in thickness. The surface area was found to be
about 1.2 M.sup.2 /gm with a porosity of about 80 percent.
Sufficient shreds were packed into a filter tube 25 mm long and
24.8 mm in circumference to provide a bulk density of about 0.122
gms/cm.sup.3 and a pressure drop of 2.3 inches. The filter removed
71 percent of the tar when attached to a conventional
cigarette.
EXAMPLE II
The relationship between pore volume, surface area and pore size
has been previously discussed. Thus, with the mean pore diameter
ranging between 8 to 12 microns the effect of the total volume and
the surface area may be examined where starch to acetate ratio in
the preparation of the porous cellulose acetate shreds are fixed in
1:1, 2:1, 3:1, and 4:1 ratios as set forth in Table I below:
TABLE I
Average Starch/Acetate Surface Filtration Ratio Used in Porosity
Area Efficiency Preparation % M.sup.2 /g % 1/1 53 0.3 33 2/1 66 0.6
50 3/1 82 1.2 68 4/1 90 2.7 70
The filters employing the materials indicated in the table above
were all 25 mm in length and packed with sufficient porous shreds
to provide a pressure drop of 2.4 inches.
From the examples presented herein with regard to the porous
cellulose acetate shreds, other cellulose ester materials such as
cellulose propionate or cellulose butyrate may be employed in place
of the porous cellulose acetate ester of the examples herein.
To compare the teachings of the prior art and the advances made by
the applicants herein, applicants' porous cellulose ester made in
accordance with this invention is compared with the teachings of
the prior art as set forth in U.S. Pat. No. 3,364,938 granted to
Mumpower II, et al, Jan. 23, 1968. This patent discloses
microporous polyolefin floc type of powder which is applied to the
surface of crimped cellulose acetate filaments which is then formed
into a filter element for cigarettes.
Applicants examined the results set forth in Examples 1-4 of U.S.
Pat. No. 3,364,938. All of the filters described therein were 17 mm
in length. Applicants then prepared filtered cigarettes employing
porous cellulose acetate shreds having a filter element 25 mm in
length.
The comparative characteristics of the filter material, the filter
pressure drop and efficiency are set forth in the Tables II and
III:
TABLE II (U.S. Pat. No. 3,364,938)
Floc Filter Ex. Material.sup.a Size.sup.b c 1 21PE:5/10,000 20-50
2.7 53 2 17PE:3/12,000 40-70 3.0 55 3 15PE:5/9,000 80-120 2.7 50 4
25PP:5/10,000 20-50 2.6 55 Notes a. 21PE:5/10,000 describes filter
containing 21% polyethylene floc dusted onto 5 denier/filament
cellulose acetate tow containing 10,000 filaments. PP is
polypropylene. b. Floc size refers to standard sieve series mesh
numbers c. Efficiency % of the filter for removing tar
TABLE III (Porous Cellulose Acetate Shreds)
Average Ex. Shred Size.sup.a (mm) Filter P.D." Efficiency 1
1.4.times.0.08 2.4 70 2 0.6.times.0.13 2.5 65 3 0.6.times.0.035 2.3
71 4 0.9.times.0.03 2.3 71 a. Shreds were 0.5 to 2.5 centimeters in
length
As can clearly be seen from reviewing the data in Tables II and
III, the filtration efficiency of the material of the present
invention is about 40 percent higher than that of the material of
the prior art. Surprisingly, the significant increase in efficiency
is obtained with a pressure drop which is lower than that of the
prior art. Thus, the efficiency increase is obtained with no loss
in drawability.
In order to properly compare the intrinsic performance of the two
different filter types, it is necessary to calculate the filtration
coefficients which allow for differences in length and pressure
drop. By using the equation
log (1 - E/100) = -.mu. PL
Where E = Filter efficiency percent
P = filter pressure drop, inches w.g.
= Filter length, cm, the coefficient .mu. which describes the
inherent filtering capability of the material is obtained.
From the formula above the filtration coefficients were calculated
for Examples 1 through 4 inclusive for U.S. Pat. No. 3,364,938 and
applicants' Examples 1 through 4 inclusive.
TABLE IV
(Comparison of filtration coefficients, .mu.)
U.S. Pat. No. Porous Cellulose Example 3,364,938 Acetate Shreds 1
0.072 0.087 2 0.068 0.073 3 0.066 0.094 4 0.079 0.094 Average 0.071
0.085
Thus, for a filter 21 mm in length, which is the average of the
filter in U.S. Pat. No. 3,364,938 and the one employed in this
disclosure, the filtration efficiency would be significantly
greater using material of the present invention.
Not only do filters made in accordance with the present invention
provide an increase in efficiency, but the desirable taste
qualities are retained. Additionally, this increase in efficiency
is obtained with no increase in pressure drop. In fact, the
pressure drop is described while obtaining this increase in
efficiency. This is surprising in view of the prior art attempts to
increase efficiency which have generally resulted in an increase in
the pressure drop.
The shredded shape and bulk density characteristics also afford a
high degree of self-cohesiveness. Therefore, it is apparent that
variations and changes will be obvious to one skilled in the art
after a reading of the present disclosure. Such variations and
changes are meant to be included within the scope of the invention
as delineated by the following appended claims.
* * * * *