U.S. patent number 3,557,801 [Application Number 04/810,404] was granted by the patent office on 1971-01-26 for cigarette smoke filter material.
This patent grant is currently assigned to Celanese Corporation. Invention is credited to Saunders E. Jamison.
United States Patent |
3,557,801 |
Jamison |
January 26, 1971 |
CIGARETTE SMOKE FILTER MATERIAL
Abstract
A cigarette filter plug is disclosed which is made from
filaments characterized by alternating regions of large and small
diameter prepared by dry spinning a solution of cellulose ester
containing a plasticizer and solid solvent adsorbent particles and
then passing the resultant filaments over a hot surface. The solid
particles found suitable may be activated charcoal, other types of
activated carbon, silica gel, alumina or clay.
Inventors: |
Jamison; Saunders E. (Summit,
NJ) |
Assignee: |
Celanese Corporation (New York,
NY)
|
Family
ID: |
27051928 |
Appl.
No.: |
04/810,404 |
Filed: |
September 16, 1968 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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495895 |
Oct 14, 1965 |
3422176 |
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Current U.S.
Class: |
131/342;
57/206 |
Current CPC
Class: |
A24D
3/10 (20130101); A24D 3/16 (20130101); D01D
5/20 (20130101) |
Current International
Class: |
A24D
3/10 (20060101); A24D 3/00 (20060101); A24D
3/16 (20060101); D01D 5/00 (20060101); D01D
5/20 (20060101); A24f 007/04 () |
Field of
Search: |
;161/170,173,174,175,177,179,180 ;131/261,266,267,268,269,10 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
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749,340 |
|
Apr 1954 |
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EN |
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941,082 |
|
Jul 1962 |
|
EN |
|
Primary Examiner: Rein; Melvin D.
Parent Case Text
This application is a divisional application of Ser. No. 495,895,
filed Oct. 14, 1965, now U.S. Pat. No. 3,422,176.
Claims
I claim:
1. A tobacco smoke filter plug comprising a collection of filaments
of a denier per filament of about 3 to 10, having spaced
alternating regions of large and small diameters, said large
diameters being from about 0.05 to 50 microns, said filaments
comprising an essentially uniform mixture of a solution spinnable
thermoplastic filamentary material, solvent adsorbent solid
particles selected from the group consisting of particles of
activated charcoal, activated carbon, silica gel, alumina and clay
and a plasticizer.
2. The filaments of claim 1 in which the thermoplastic filamentary
material comprises a cellulose ester of an organic acid.
3. The filaments of claim 1 in which the thermoplastic filamentary
material comprises cellulose acetate.
4. The filaments of claim 1 in which the adsorbent solid particles
comprise activated charcoal.
Description
This invention relates to a filter material. More particularly, the
invention relates to a collection, tow or bundle of thermoplastic
filaments suitable for use as a tobacco smoke filter rod.
Among the wide variety of materials which have been recommended as
tobacco smoke filters, one type in particular is ideally suited for
this purpose from a manufacturing standpoint. This type is a
continuous crimped tow material, preferably a continuous crimped
cellulose acetate textile tow. One reason for the widespread use of
cellulose acetate is the ease and rapidity at which it can be
processed into firm or rigid filter rods on equipment known to the
cigarette industry. Thus, for example, a continuous crimped
cellulose acetate tow of 5,000 to 50,000 filaments, depending on
the thickness of the spun fibers, can be bloomed out, sprayed with
a nonvolatile liquid plasticizer type of bonding agent, recompacted
and pulled through a rod-forming and paper-wrapping device to
produce 90 mm. filter rods at the rate of several hundred per
minute. Such rods become quite firm on standing for a period of
time.
Although continuous crimped textile tow is a useful filter material
from a processing standpoint as explained above, it has a certain
disadvantage from the standpoint of its ability to remove the tiny
nicotine and tar particles from cigarette smoke. This aspect is the
somewhat parallel relationship and surface smoothness of many of
the filaments or fibers which constitute the filtering element. As
a result, a certain amount of the nicotine and tar particles are
capable of passing between the substantially longitudinally aligned
smooth fibers without touching them. These particles, therefore,
are not trapped. One method which has been suggested for
circumventing this difficulty is to use a very fine denier fiber in
the preparation of the tow. This would mean that it would require a
considerably larger number of fibers in the tow to fill the filter
to the desired circumference of a cigarette, thus giving a higher
surface area and a much smaller space between the parallel fibers.
Such an approach, however, gives a filter tip which may have a
higher pressure drop (high resistance to the passage of air through
the filter).
Another method which has been suggested for producing a textile tow
type of filter, which is highly effective for the removal of
nicotine and tar particles and yet does not produce an excessively
high pressure drop, is to dust the tow with certain harmless
powders such as starch powders or powders of cellulose or cellulose
derivatives at some point along the assembly which processes it
into a filter. The dusting produces an irregular surface on the
substantially parallel fibers. The particles of the powdered
additive function as bumps or protrusions which extend into the
spaces between the fibers in the finished filter rod. These
protrusions make the path of the smoke particles through the filter
more difficult and part of the nicotine and tar particles which
might channel through the filter are impinged on these
protrusions.
Still another method which has been suggested for overcoming the
above problem is to incorporate crystallizable types of compounds
into the fiber-forming polymeric substance, which is spun into
fibers in the conventional manner. When these fibers are formed,
the crystallizable compounds gradually exude to the surface of the
fibers whereupon they crystallize forming rough irregular
protrusions on the fiber surface.
While the addition of protrusions on the fiber surface either by
dusting or by crystallization improves filtration of the tobacco
smoke, there are still certain disadvantages associated with the
production of these tows. For example, the dusting technique
requires the use of additional dusting equipment, forces the use of
special precautions to prevent dust explosions and also presents
problems in restricting the dust to the dusting area. The
crystallization technique usually requires the addition of
expensive crystallizable materials, and also generally necessitates
an additional curing time for the solids to exude to the surface of
the fiber and crystallize.
Accordingly, the primary object of the present invention is to
provide a filter having integral protruberances on the fibers
thereof.
Another object is to provide a filter plug which is highly
effective for removing aerosol particles from tobacco smoke without
incurring the disadvantages mentioned above.
An additional object is to provide a new fiber, for use in a filter
plug, having alternating regions of large and small diameters
without having to dust or crystallize particles on the surface of
the fiber.
The fibers of the present invention are formed by a a usual,
employing a dope comprising a solution spinnable thermoplastic
filamentary material dissolved in a suitable organic solvent,
solvent absorbent solid particles and a plasticizer is spun into
filaments in a conventional spinning device. After the spun
filaments or fibers are formed, and while they still contain a
substantial amount of solvent, the fibers are passed over a heated
stationary or moving surface, such as a plate or roller, to
evaporate substantially all of the solvent from the fibers. Prior
to passage over the heated surface the spun fibers are of a usual,
substantially uniform diameter. However, after passage over the
heated surface and evaporation of the solvent, the filaments have
spaced, alternating regions of large and small diameters. In fact,
the fibers appear to have beads positioned along the length
thereof. The required number of "beaded" fibers are combined into a
tow, which may be subsequently used as an aerosol filter element,
and particularly a tobacco smoke filter plug.
It is important to note that the above fluctuating regions on the
filament surface are not caused by bonding or crystallization of
extraneous particles on the surface of the filaments. On the
contrary, the beads appear to be swollen cavities within portions
of the fiber material itself with the solid particles being
uniformly dispersed throughout the filament. By producing the
homogeneous beaded fiber there is no need to worry about the beads
sifting out of the cigarette filter as sometimes happens when
extraneously added particles are bonded or crystallized on the
fiber surface.
While it is not certain, it is believed that the beaded effect is
caused by the discharge of the absorbed solvent as a fiber passes
over the heated surface. For this reason, it is important that the
fibers be passed over the hot surface, sometimes hereinafter
referred to as a hot shoe, while they still contain a substantial
amount of solvent. Further, it is important that the solids present
in the dope be capable of absorbing the organic solvent. Hence, the
solids are referred to as solvent adsorbent solid particles. In
addition, the solids must not be soluble in the materials contained
in the spinning solution so that they can retain their adsorptive
characteristic.
The fibers may be formed of any solution spinnable thermoplastic
filamentary material. The term "solution spinnable" is meant to
include the various polymeric substances which are soluble in
organic solvents, e.g., cellulose derivatives such as cellulose
acetate and triacetate, polymers of acrylonitrile, vinyl chloride,
vinyl esters and ethers, and the like. The preferred fiber forming
materials are cellulose esters of organic acids, and particularly
cellulose acetate, the acetyl value of which can range from about
50 to 62.5 percent by weight calculated as acetic acid.
The thermoplastic filamentary material and the plasticizer are
usually present in the spinning solution or dope in a combined
concentration ranging from about 10 to 35 percent by weight of the
spinning solution, and preferably from about 15 to 30 percent.
The presence of a plasticizer in the spinning solution is very
important. Passage of the fiber over the hot surface causes
intermittent expansion of the fiber. Because of the presence of the
plasticizer, the swollen fiber areas or beads do not burst. The
plasticizer may be any of the ones normally used with the aforesaid
thermoplastic materials in the conventional filament spinning
processes. With cellulose acetate the preferred plasticizers
include swelling agents such as glycerol triacetate (triacetin),
triethyl citrate, dimethoxy-ethyl phthalate, dimethyl phthalate,
methyl phthalyl ethyl glycolate, o-phenyl phenyl-(bis) phenyl
phosphate, and the like. The preferred plasticizers when using
cellulose acetate as the thermoplastic filamentary material are
dimethyl phthalate and triacetin. The plasticizer may be added to
the spinning solution in a concentration ranging from about 15 to
25 percent by weight of the thermoplastic filamentary material
present therein, and preferably from about 18 to 22 percent, i.e.,
in an amount sufficient to prevent rupture or bursting of the fiber
surface on sudden thermal discharge of the adsorbed solvent.
Any of the volatile organic solvents normally used with the
above-mentioned filamentary materials during the spinning process
are suitable for use. For example, solvents such as acetone,
methylene chloride, dioxane, dimethyl formamide, methanol and the
like, either alone or in combination, may be used. When the
filamentary material is secondary cellulose acetate the preferred
solvent is acetone or a mixture comprising a major proportion,
e.g., 70 to 95 percent methylene chloride and a minor proportion,
e.g., 5 to 30 percent methanol. The latter mixture is also
preferred when cellulose triacetate is the filamentary material.
The solvent is normally present in a concentration ranging from
about 65 to 90 percent by weight of the spinning solution, and
preferably from about 70 to 85 percent. Desirably, the solvent
should comprise at least one component which is rather strongly
adsorbed by the solids present in the spinning solution under the
conditions of filament formation.
As previously indicated, the primary purpose of the nonsoluble,
adsorbent solids is to extend the presence of a substantial amount
of the solvent in the spun fibers until they pass over the hot shoe
when the volatile solvent relatively suddenly evaporates upon
contact of the fiber with the shoe.
The particle size of the nonsoluble, adsorbent solids should be
small enough so as not to interfere significantly with the
continuity of the supporting filamentary material or fiber
structure being formed. Preferably, the diameter of the individual
solid particles must be such that they comprise from about 10 to 20
percent of the diameter of the eventual filament in which they
become occluded. Normally, the solids range in diameter from about
0.01 to 5 microns, and preferably from about 0.05 to 1 micron.
Suitable solids which are nonsoluble in the spinning solution
materials and which may be used in the present invention are
charcoal, preferably activated charcoal, or other types of
activated carbon, silica gel, alumina, and clay.
When cellulose acetate is the filamentary material and acetone or a
mixture of methylene chloride and methanol is the solvent a
preferred nonsoluble solid is activated charcoal. The nonsoluble
solids may be present in the spinning solution in an amount ranging
from about 1.5 to 3 percent by weight of the spinning solution, and
preferably from about 2 to 2.5 percent. Generally, the solids
comprise from about 5 to 10 percent by volume of the eventual fiber
in which they are occluded. Because of the need to produce a
continuous fiber structure, the amount and the diameter of the
solids, within the above mentioned ranges, will be related to the
fiber area or fineness of the product spun fiber, i.e., the
capacity of the solid particles to disrupt the fiber structure is
inversely related to the fiber area.
As previously mentioned, it is important to realize that the solids
do not gravitate or flow to the surface or any particular region of
the spun fibers, but are present uniformly throughout the fiber
material. The spun fiber is an essentially uniform mixture of
solids, filamentary material and plasticizer.
For a better and more complete understanding of the present
invention, its objects and advantages, reference should be had to
the following detailed description and to the accompanying drawings
in which:
FIG. 1 is a schematic elevational view showing an exemplary
spinning system suitable for use in making the filter fiber
material of the present invention;
FIG. 2 is a sketch of an individual beaded filament produced by the
disclosed process; and
FIG. 3 is a highly magnified longitudinal view of a filter plug or
element comprising a collection of the beaded filaments produced by
the said process.
Referring to FIG. 1 there is shown schematically a spinning cabinet
2 with a spinneret 4 located at its upper end and a multiplicity of
filaments 6 moving downwardly from the spinneret 4.
A spinning solution comprising the aforementioned components, e.g.,
cellulose acetate, a solvent mixture of 90 percent methylene
chloride and 10 percent methanol, activated charcoal particles and
dimethyl phthalate plasticizer, is introduced by means not shown
into the spinneret 4. The solution is spun under conventional
conditions for solution spinning, for example, a temperature in the
range of from about 30 to 50.degree. C., and an extrusion rate in
the range of from about 25 to 150 meters per minute, and preferably
40 to 60 meters per minute.
The spun filaments 6 pass downwardly through the spinning cabinet 2
at the same rate at which they were extruded. The temperature in
the spinning cabinet may be in the range of from about 20 to
100.degree. C., and preferably 30 to 50.degree. C.
The spun filaments are removed from the cabinet 2 and while still
containing solvent in the range of from about 10 to 50 percent by
weight of the filaments, are passed over a pair of conventional
skew rolls 8. The spun filaments are then passed over a hot shoe
10, which has been heated to a temperature above the evaporation
temperature of the solvent and below the charring temperature of
the filamentary material. Normally the hot shoe 10 is maintained at
a temperature in the range of from about 175 to 205.degree. C., and
preferably 180 to 190.degree. C. The hot surface or hot shoe 10 may
be heated in any convenient manner, e.g., an electrically heated
shoe may be used. As illustrated in FIG. 1, the hot shoe 10 is
connected to a conventional temperature control box 12. The heated
surface is preferably of cylindrical shape, however, a flat surface
may also be used. The hot shoe may be stationary or moving, such as
a heated rotating roller.
As previously mentioned, it is important that the filaments be
contacted with the hot shoe while still containing a substantial
amount of solvent. This condition is facilitated by proper control
of the spinning cabinet temperatures within the above mentioned
ranges and by the speed of withdrawal of the filaments from the
cabinet. The speed of travel of the filaments is normally
controlled by the pair of skew rolls 8 and a conventional take up
bobbin, not shown on the drawing. The optimum cabinet temperature
and filament withdrawal speed will also depend on the type of
filamentary material, type and amount of solids and type and amount
of solvent. However, a few simple preliminary runs with the desired
spinning solution will quickly determine the best conditions to
achieve the desired beaded filaments.
Returning to the hot shoe 10, the solvent-laden filaments are
passed over the shoe so as to cause substantially all of the
solvent to evaporate therefrom. Generally, contacting the filaments
with the hot shoe for a period of time in the range of from about
one-fiftieth to one-twentieth of a second will achieve the desired
results.
As a result of contact with the hot shoe, the filaments recovered
therefrom consist of alternating regions of large and small
diameters, the individual filaments having a weight within the
range of from about 3 to 10 denier. More specifically, the
filaments have the appearance of a fiber containing beads more or
less uniformly spaced thereon as illustrated in FIG. 2 of the
drawings.
The filaments prior to contact with the heated surface may have any
shape conventionally found in spun fibers. Normally, the spun
fibers have substantially bulbous cross sections, such as result
from dry spinning through circular orifices.
The filaments are passed from the hot shoe 10 without any stretch
of the filaments occurring and are collected on a take up bobbin in
the conventional manner, The desired amount of beaded filaments are
collected and subsequently processed in conventional filter plug
making equipment to produce the product filter plugs, as
illustrated by FIG. 3 of the drawings.
The beaded filamentary material of this invention may be used for
filtration of any aerosol particles, however, the preferred use is
as tobacco smoke filter plugs. In addition, the beaded fibers may
be used in textiles due to optical and tactual features of the
fiber structure or to its insulating or adsorptive properties.
The following example is given by way of illustrating the process
of the present invention:
EXAMPLE
A slurry of the following composition was agitated for 5 days on a
ball mill:
fifteen parts by weight of activated charcoal (Darko KB), having a
surface area of 1589 square meters per gram and a pore volume of
2,077 milliliters per gram;
two parts by weight of secondary cellulose acetate flake;
one hundred thirty-one parts by weight of methylene chloride;
two parts by weight of methanol.
A mixture was prepared of 118 grams of the above slurry, plus 111
grams of secondary cellulose acetate flake, 6.8 grams methanol, 296
grams methylene chloride, and 24 grams dimethyl phthalate. This
mixture was agitated by tumbling overnight and then extruded
through a stainless steel spinneret of five holes, 0.042 mm. in
diameter. The filaments were conveyed while still solvent-laden at
fifty meters per minute over a hot shoe at a temperature of 182 to
185.degree. C., from which they were taken up without stretch. The
filaments obtained were 6 denier per filament and had essentially
the shape illustrated in FIG. 2 of the drawings.
Firm hand-rolled filter plugs were made of these fibers and
required only 0.115 grams of fiber per each 17 millimeter plug,
which is no more than is required to form firm commercial plugs or
tips that are presently in use. The filter plug is illustrated by
FIG. 3 of the drawings.
The principle, preferred construction, and mode of operation of the
fibers of the invention have been explained and what is now
considered to be its best embodiment has been described in the
foregoing specification. However, it should be understood that the
invention which is intended to be protected herein may be practiced
otherwise than as specifically illustrated and described without
departing from the scope of the appended claims.
* * * * *