Note: Descriptions are shown in the official language in which they were submitted.
Various processes have been proposed for expanding tobacco.
For example, tobacco has been contacted with a gas under some-
what greater than atmospheric pressure, followed by a release
of the pressure, whereby the tobacco cells are expanded to in- ¦
crease the volume of the treated tobacco. Other methods
- which have been employed or suggested have included the treat-
ment of tobacco with various liquids, such as water or re-
latively volatile organic liquids, to impregnate the tobacco
with the same, after which the liquids are driven off to ex-
pand the tobacco. Additional methods which ha~e been suggested
have included the treatment of tobacco with solid materials
which, when heated, decompose to produce gases which serve to
expand the tobacco. Other methods include the treatment of
tobacco with gas-containing liquids, such as carbon dioxide-
containing water, under pressure to incorpora~e the gas in the
tobacco and when the tobacco impregnated therewith is heated
or the pressure thereon is reduced to thereby expand the
tobacco. Additional techniques have been developed for expand-
ing tobacco which involve the treatment of tobacco with gases
which react to form solid chemical reaction products within
the tobacco, which solid reaction products may then decompose
by heat to produce gases within the tobacco which cause expan-
sion of the tobacco upon their release. More specifically: ¦
A patent ~o Wilford J. Hawkins, U.S. Pstent 1,789,435,granted in 1931, describes a method and apparatus for expand-
ing the volume of tobacco in order to make up the loss of
-1- '~
. ,
'
p~
weight caused in curing tobacco leaf. To accomplish this
object, the cured and conditioned tobacco is contacted with a
gas, which may be air, carbon dioxide or steam under about 20
pounds o pressure and the pressure is then relieved, whereby
the tobacco tends to e~pand. The patent states that the
volume of the tobacco may, by that process, be increased to
the extent of about 5 - 15%.
An alien property custodian document No. 304,214 to
Joachim Bohme, dated 1943, indicates ~hat tobacco can be ex-
panded using a high-frequency generator but that there are
limitations to the degree of expansion which can be achieved
without affecting the quality of the tobacco.
A patent to Frank J. Sowa, U.S. Patent 2,596,183, granted
in 1952, sets forth a method for increasing the volume of
shredded tobacco by adding additional water to the tobacco to
cause the tobacco to swell and thereafter heating the moisture
conta~ning tobacco, whereby the moisture evaporates and the
resulting moisture vapor causes expansion of the tobacco.
A series of patents to Roger de la Burde, U.S. Patents
3,409,022, 3,409,023, 3,409,027 and 3,409,028, granted in
1968, relate to various processes for enhancing the utility
af tobacco stems for use in smoking products by subjecting the ,
stems to expansion operations utilizing various types of heat
treatment or microwave energy.
A patent to John D. Hind, U.S. Patent 3,425,425, granted
in 1969, which is assigned to the same assignee as the
assignee of the present ~nvention, relates to the use of
--2--
~` 4
carbohydrate, , .mpr~-e the puffing of tobacco stems. In
that process, tobacco stems are soaked in an aqueous solution
of carbohydrates and then heated to puff the stems. The car-
bohydrate solution may also contain organic acids and/or
certain salts which are used to improve the flavor and
smoking qualities of the stems.
~ pufilication in the "Tobacco Reporter" of November 1969
by P. S. Meyer describes and summarizes tobacco puffing or ex-
pansion procedures or investigations for expanding and manipu-
10 lating tobacco for purposes of reducing costs and also as the
means for reducing the "tar" content by reduction in the de-
livery of smoke. Mention is made in this publication of
puffing tobacco by different procedures including the use of
halogenated hydrocarbons, low pressure or vacuum operation,
or high pressure steam treatment that causes leaf expansion
from inside the cell when outside pressure is suddenly released.
Mention is also made in this publication of freeze-drying
tobacco which can also be employed to obtain an increase in
volu~e.
Since the above-mentioned "Tobacco Reporter" article
was published, a number of tobacco expansion techniques, in-
cluding some of the techniques described in the article, have
been described in patents and/or published patent applications.
For example, U.S. Patent 3,524,452 to Glenn P. Moser et al and
U.S. Patent 3,524,451 to James D. Frederickson, both issued in
1970, relate to the expansion of tobacco using a volatile
organic liquid, such as a halogenated hydrocarbon.
-- 3 --
, ~ :
U.S. Patent 3~734,104 to William M. Buchanan et al.
which is assigned to the sam2 assignee as the assignee of the
- present invention, issued in 1973, relates to a particular
: '
process for the expansion of tobacco stems.
` U.S. Patent 3,710,802 to William H. Johnson, issued in
1973 and British Specification 1,293,735 to American Brands, I
Inc., published in 1972, both relate to freeze-drying methods
for expanding tobacco.
South African applications 70/8291 and 70/8282 to R. J.
Reynolds Tobacco Company, both filed in 1970, relate to
; tobacco expansion employing chemical compounds which decompose
to form a gas or with inert solutions of a gas under pressure
to maintain the gas in solution until it impregnates the
tobacco
A patent to Robert G. Armstrong, U.S. Patent 3,771,533,
issued in 1973, which is assigned to the same assignee as the
assignee of the present invention, involves a treatment of
tobacco with carbon dioxide a~d ammonia gases, whereby the
tobacco is saturated with these gases and ammonium carbonate
is formed in situ. The ammonium carbonate is thereafter de-
composed by heat to release the gases within the tobacco
cells and to cause expansion of the tobacco.
Despite all of the above-described advances in the art,
no completely satisfactory process has been found. The dif-
ficulty with the various earlier suggestions for expanding
tobacco is that, in many cases, the volume is only slightly
or at best only moderately increased~ For example, freeze-
_4_
drying operations have the disadvantages of requiring elabor-
ate and expensive equipment and very substantial operating
costs. ~ith respect to the teaching of using heat energy,
infrared or radiant microwave energy to expand tobacco stems,
the difficulty is that while stems respond to these heating
- procedures, tobacco leaf has not generally been found to re-
spond effectively to this type of process.
The use of special expanding agents, for example, halo-
genated hydrocarbons, such as are mentioned in the Meyer pub- .
lication for expanding tobacco, is also not completely satis-
factory, because some of the materials employed are not al-
ways desired as additives Furthermore, the introduction, in
considerable concentration, of materials which are foreign to
tobacco presents the problem of removing the expsnsion agent
after the treatment has been completed in order to avoid
affecting aroma and other properties of the smoke due to ex-
traneous substances used or de~eloped from the combustion of
the treated tobacco.
The use of carbonated water has also not been found to
be effective.
While the method employing ammonia and carbon dioxide
gases is an improvement over the earlier described methods,
~t is not completely satisfactory under some circumstances
in that undesired deposition of salts can result during the
process.
Carbon dioxide has been used in the food industry as a
coolant and, more recently, has been suggested as an extractant
for food flavors. It has also been described in German Offen-
legungsschrift 2,142,205 (Anmeldetag: 23 August 1971) for use,
in either gaseous or liquid form, to extract aromatic materials
from tobacco However, there has been no suggestion, in con-
; nection with these uses, of the use of gaseous carbon dioxide
for the expansion of these materials.
A process employing liquid carbon dioxide has been foundto overcome many of the disadvantages of the above-mentioned
prior art processes. The expansion of tobacco, using liquid
carbon dioxide is described in Belgian Patent 821,568, which
corresponds to Canadian Patent No. 1,013,640 to de la
Burde and Aument (two of the present co-inventors) and
assigned to the same assignee as the present application and
in Belgian Patent 825,133 to Airco, Inc. This process m~y
be described as a process for expanding tobacco comprising
the steps of (1) contacting the tobacco with liqui~ carbon
dioxide to impregnate the tobacco with the liquid carbon
dioxide, (2) subjecting the liquid carbon dioxide-impregnated
tobacco to conditions such that the liquid carbon dioxide is
converted to solid carbon dioxide and (3) thereafter subjecting
the solid carbon dioxide-containing tobacco to conditions
whereby the solid carbon dioxide is vaporized to cause ex-
pansion of the tobacco.
In our earlier work with gaseous CO2, st pressures of
about 100 psia, we had found that only minute amounts of
carbon dioxide gas could be incorporated in the tobacco and
held there sufficiently long for the tobacco to be heated
-6- 1
and expanded. Thus, we found no substantial improvement over
the prior art and gaseous CO2 was believed to be much less
effective as an expanding agent than the liquid carbon
dioxide employed in the expansion process of the above-mentioned
Canadian Patent No. 1,013,640. We have now
found that gaseous carbon dioxide can be introduced into
tobacco in a manner whereby the gaseous carbon dioxide remains
in the tobacco in an amount of one per cent or more to form a
product which can then be expanded. Unexpectedly superior
results and advantages can be achieved by employing gaseous
C2 in the manner set forth in the present specification. The
pxesent process may be described as follows: A process for
expanding tobacco to achieve at least about 50 per cent
increase in cylinder volume, comprising the steps of
(l) impregnating tobacco with gaseous carbon dioxide under a
pxessure of at least about 250 psig and at sufficient tempera-
ture that substantially all of the carbon dioxide is maintain-
ed in gaseous form, (2) decreasing the pressure on the carbon
dioxide~impregnated tobacco and (3) heating the impregnated
tohacco under conditions effective to liberate the carbon
dioxide therein so as to cause expansion of the tobacco. The
present invention also relates to an improvement in that
process and have found that gaseous carbon dioxide can be in-
troduced into tobacco in a manner whereby the gaseous carbon
dioxide remains in the tobacco in an amount as high as three
per cent or more to form a product which can then be expanded.
Unexpectedly superior results and advantages can be achieved
:
by employing gaseous CO2 in the manner set forth in the
present specification.
This divisional application provides a process for
expanding tobacco to achieve at least about 50 per cent
increase in cylinder volume, comprising the steps of (1)
impregnating tobacco with gaseous carbon dioxide under a
pressure of at least about 250 psig for 1/4 to 30 minutes, and
at a temperature not lower than -23C., so that substantially
all of the carbon dioxide is maintained in gaseous form to
10 incorporate in the tobacco at least 1 part of carbon dioxide
per 100 parts of tobacco, (2) decreasing the pressure on the
carbon dioxide-impregnated tobacco and (3) heating the
impregnated tobacco under conditions effective to liberate
the carbon dioxide therein so as to cause expansion of the
tobacco.
A novel tobacco product comprises tobacco contain-
ing gaseous carbon dioxide in an amount of at least 1 part
of gaseous carbon dioxide per 100 parts of tobacco~ The
product, when rapidly heated is converted to expanded tobacco.
An improved process for the expansion of tobacco is also
provided which employs carbon dioxide as the expansion agent.
Tobacco, generally having a moisture content of from about
5 to about 35% by weight, is placed in a pressure vessel or
similar confinable space. Carbon dioxide gas may be passed
through to flush the vessel. Carbon dioxide pressure is then
increased and brought to a valve of from about 250 pounds
per square inch gauge (psig) to about 1057 psig or even higher,
and preferably to about 400 to 800 psig. The tobacco
: /
-- 8 --
A
I
.5~
is maintained under such a pressure under conditions whereby
the carbon dioxide is substantially gaseous for from
about l/4 to about 30 minutes, to impregnate the tobacco
with carbon dioxide. The pressure is then reduced in a
period of from l to 800 seconds, preferably 10 to 120
seconds, preferably to atmospheric pressure, to produce a
product comprising tobacco containing at least 1% by weight
of gaseous carbon dioxide, based on the weight of tobacco.
The resulting gaseous carbon dioxide-containing tobacco may
then be heated in the same vessel but is preferably rapidly
transferred, preferably within a few minutes, to a separate
zone where it is subjected to conditions of temperature
and pressure, as by rapid heating in
- 8(a) -
5 i~
':
: a gas at 100 to 370C and at or near atmospheric pressure for
a period of from about 1 second to about 10 minutes, to ex-
pand the tobacco.
-An improvement on the above-described invention wherein
the tobacco/CO2 system is cooled during or after pressurization, L
as by circulation of a cooling agent through the jacket of the
chamber, to a temperature close to the saturation temperature
of carbon dioxide but not lower than -23C. As an alternative
:to using a cooling jacket in the improved process CO2 gas can
be caused to flow through the system by venting a portion of
the C02 gas either during or following pressurization, pre-
ferably while maintaining an infeed of CO2 gas such that there
is not a loss in the system pressure due to the venting. With
cooling, the resulting conditions are such that the carbon
dioxide at the prevailing temperature and pressure remains sub-
stantially in the gaseous state, but further such that the
carbon dioxide, upon rapid reduction of pressure upon the sys-
tem, is converted partially to a condensed state within the
tobacco. Such conditions may be defined as such that the
enthalpy of the carbon dioxide is kept at a value which isless than about 140 BTU per lbm. By this means a signifi-
cantly greater residue of carbon dioxide remains in the tobacco
at the beginning of the expansion step, than is the case with-
out the cooling before pressure release, wherein the carbon
dioxide, at higher enthalpy, remains primarily in the gas phase
throughout. A further method of reducing the enthalpy of the
system thereby causing an increased retention of carbon dioxide
g
involves admission of additional quantities of CO2 gas during
venting thereby causing additional sweeping of CO2 gas to flow
through the system. _
In connection with the present in~ention, if desired,
the retention of carbon dioxide in the tobacco can be increased -
by pre-cooling or pre-freezing the tobacco prior to the impreg-
nation cycle to cause a reduction in the system enthalpy. A
still further method of increasing the retention of carbon
dioxide in the tobacco involves "pre-snowing" the tobacco with
finely divided solid carbon dioxide (dry ice) prior to the im-
pregnation cycle which accomplishes both a pre-cooling of the
tobacco and serves as an additional source for providing
carbon dioxide to the tobacco; applied in proper amounts of
from about 5-50% by weight of the tobacco, at least a portion
of the dry ice will be incorporated into the tobacco during
the pressurization cycle and by varying the amo~nt of dry ice
applied, a method of increasing and controlling the amount of
carbon dioxide retained by the tobacco becomes possible. When
such methods are involved, the tobacco~CO2 system ~ay be main-
tained for 1/4 to 30 minutes during the impregnation step,where the pressure is at least 250 psig, to impregnate the
tobacco with carbon dioxide. The pressure is then reduced~ in
a period of 1 to 800 seconds, preferably 10 to 120 seconds and
preferably but not necessarily to atmospheric pressure. The
tobacco is then rapidly transferred to a zone where it is
fiubjected to conditions of temperature and pressure, as by
rapid heating in a gas at 100 to 370C and at or near atmos-
pheric pressure for one second to 10 minutes to expand the tobacc
.
--10--
This invention relates broadly to an improved process
for expanding tobacco employing a readily-available, relative-
ly inexpensive, non-combustible, inoffensive, and non-toxic
expansion agent and more particularly, to the production of
an expanded tobacco product of substantially reduced density
and increased filling power. The improved process employs
carbon dioxide as the expansion agent. In general, the pro-
cess comprises placing tobacco, preferably having a moisture
content of from about 5 to about 35%, by weight, in a vessel
or similar confinable space; the vessel or space may then be
flushed with gaseous C02 to remove most of the associated air,
although this is not essential to the invention. The vessel
- is closed except for an inlet port, and carbon dioxide gas
is introduced and the pressure increased, by continued gas in-
-` troduction cr heating or both, under conditions whereby the C02
in the vessel remains primarily in the gas state to a final
pressure of at least 250 psig, preferably 400 to 800 psig.
The required temperature to maintain the CO2 in a substantially
gaseous state at a given pressure may be determined readily by
one familiar with the use of phase diagrams or critical tables.
Nhile pressures as high as gO~ psig might be economically em-
ployed, and a pressure of about 1057 would be acceptable,
there is no known upper lim~t to the useful impregnation pres-
sure range other than that imposed by the capabilities of the
equipment available. However, operation below the critical
temperature is preferred for ease of control. The tobacco
may be maintained under these impregnating conditions from
--11--
about l/4 to 3G minutes, the longer times being in general
applicable to lower pressure operation. Reference to the
pressure~enthalpy diagram for CO2 as set forth in Figure l of
the drawing will be of help in selecting desired conditions.
After the impregnation step, the gas pressure is reduced by
venting. The final pressure may be atmospheric or some pres-
sure near that to be employed in the expansion step, but pre-
ferably the former. The time of pressure reduction is from
l to about 800 seconds. The gaseous carbon dioxide-containing
tobacco is then transferred to a zone where it is subjected to
conditions whereby the carbon dioxide is removed to expand
the tobacco. The transfer of the carbon dioxide-containing
tobacco to the heating or expansion zone shou]d preferably be
effected within as sho~t a time as possible, preferably within
about five minutes, and most preferably within about two
minutes. As an alternative to rapid transfer, if desired,
the carbon dioxide-containing tobacco may be stored in an
insulated bulker or chilled or otherwise maintained in a re-
latively cool condition. The heating or expansion step prefer-
ably involves exposing the carbon dioxide-containing tobacco
to rapid heating at a temperature of about lO0 to 370C for a
period of time of from about l second to lO minutes and sub-
stantially atmospheric pressure.
In accordance with improvement in the present invention,
the impregnation step is modified, as will be set forth in de-
tail later in this specification. After the impregnation step,
the gas pressure is reduced by venting. The final pressure may
- 12 -
-
be atmospheric or some pressure near that to be employed
in the expansion step, but preferably the former. The time
of pressure reduction is from 1 to about 800 seconds. The
gaseous carbon dioxide-containing tobacco is then transferred
to a zone where it is subjected to conditions whereby the
carbon dioxide is removed to expand the tobacco. The transfer
of the carbon dioxide-containing tobacco to the heating or
expansion zone should preferably be effected within as short
a time as possible, preferably within about five minutes, and
most preferably within about two minutes. As an alternative
to rapid transfer, if desired, the carbon dioxide-containing
tobacco may be stored in an insulated bulker or chilled or
otherwise maintained in a relatively cool condition. The heat-
ing or expansion step preferably involves exposing the carbon
dio~ide-containing tobacco to rapid heating at a temperature
of about 100 to 370~C for a period of tLme of from about
1 second to 10 minutes and substantially atmospheric pressure.
To cæ ~ out the process of the invention, one may treat
either whole cured tobacco leaf, tobacco ~n cut or chopped
form, or selected parts of tobacco, such as tobacco stems or
may be reconstituted tobacco. In comminuted form~ the
tobacco to be treated may have a particle size of from about
10 to about 100 mesh, but is preferably not smaller than
about 30 mesh,
The tobacco may contain the natural moisture content
of tobacco and may contain from about 5 to about 35Z by weight
moisture. Ie is preferred, however, for best results that the
--13-
tobacco have at least about 8% moisture (by weight) and no
more than about 22% (by weight) moisture. As used herein,
% moisture may be considered equivalent to oven volatiles
(OV) since not more than about 0.9% of the tobacco weight is
volatiles other than water. The procedure for determining
oven volatiles is set forth later in this specification.
The tobacco will generally be placed in a pressure
vessel which will be m~re fully described hereinafter. For
example, it m~y be placed in a wire cage or on a platform
positioned within the vessel.
The tobacco-containing pressure vessel may be then
purged with carbon dioxide gas. The benefits of purging are
the removal of gases that might interfere with a carbon dio-
xide recovery process and/or that might interfere with full
penetration of the gaseous carbon dioxide. As an alternative
to purging with carbon dioxide gas, the vessel may be evacuated
prior to introduction of the carbon dioxide gas.
Either with or without a preliminary purging or evacua-
tion of the vessel, carbon dioxide gas is fed to the vessel
under conditions whereby the carbon dioxide gas pressure in
the vessel is increased under conditions whereby the tobacco
~n the vessel is preferably at a temæerature of from about
-10 to about 60~C, and the pressure in the veSsel is above
about 250 psig, preferably about 400 to 80~ psig. The tobacco
is maintained under conditions whereby the carbon dioxide is
at a pressure above about 250 psig and is under conditions
above and to the right of the saturated vapor line of Figure 1
~L4-
of the drawing from a period of from about 15 seconds to
about 30 minutes. The pressure is then reduce~d over a period
of from 1 to about 800 seconds, preferably 10 to 120 seconds,
such that the temperature at no point drops below the satura-
; tion temperature for carbon dioxide at the simultaneous pres-
sure, and the tobacco is brought to a temperature below about
10C, and atmospheric pressure or the pressure at which the
expansion step is to be carried out.
In the improvement on this invention, the tobacco/C02
system during the impregnation step is cooled, as for example,
by circulation of a refrigerant through the jacket of the
vessel containing the system, to reduce the enthalpy of the
carbon dioxide below sbout 140 BTU/lbm, preferably while the
pressure is maintained relatively constant by admission of
additional carbon dioxide gas The cooling is limited so that
the carbon dioxide is not condensed to any significant degree
and is not cooled to a temperature lower than -23C The
system is maintained under these impregnating conditions from
about 1/4 to 30 minutes, the longer times being in general
applicable to lower pressure operation. Reference to the afore-
mentioned phase diagram or critical tables for carbon dioxide
will be of help in selecting desired conditions. The pressure-
temperature relationship is preferably maintained to keep the
carbon dioxide gas at or near the saturation point. It is be-
lieved that when the conditions are close to or at saturation,
the absorption/adsorption characteristics of gaseous ~2 are
greatly enhanced. This results in improved retention of
- - -15-
:
gaseous C02. The final pressure, when the pressure is reduced,
may be atmospheric or some pressure near th~t to be employed
in the e:;pansion step, but is preferably atmospheric. The time
of pressure reduction may be from about 1 to about 800 seconds.
It has been found that after the impregnation step,
under conditions where the cooling of the improved process is
~ot employed, a product will be formed having at least one
'! part of carbon dioxlde gas per one hundred parts of tobacco.
By this is meant that at least one part of carbon dioxide gas,
1~ per one hundred parts of tobacco, will be associated with the
tobacco in some mannerS chemically and/or physically, for
example by being absorbed by the tobacco. The product may have
as high as three parts or more of gaseous carbon dioxide when
the process is so conducted. This has been found to occur in
the absence of added adsorbents or the ~ike. Adsorbents,
absorbents or the like may be present; however, it is preferred
that they not be present since the process is effective without
them and they might introduce undesired elements into the smoke
or might not release the carbon dioxide in a totally effective
manner. It has been found that after the impregnation step,
the tobacco may contain even greater amounts of carbon dioxide,
as high as 3 parts (per hundred of tobacco) or more. The
pressure-temperature relationship is preferably maintained to
keep the gas at or near the saturation point. It is believed
that when the conditions are close to or at saturation, the ab-
sorptiontadsorption characteristics of gaseous C02 are greatly
~nhanced. This results in improved retention of gaseous C02.
-16-
' . :
The final pressure, when pressure is reduced, may be atm~s-
- pheric or some pressure near that to be employed in the eY~pan-
si~n step, but is pre~erably atmospheric. The time of pressure
reduction may be from about 1 to about 80~ seconds.
We have found that after the impregnation step, under
conditions where the cooling of the improvement in the present
invention is employed, a product will be formed which may have
as high as three parts or more of gaseous carbon dioxide, per
one hundred parts of tobacco. By this is meant that at least
three parts of carbon dio~ide gas, per one hundred parts of
tobacco, will be associated with the tobacco in some manner,
chemically ~nd/or physically, for example, by being absorbed
by the tobacco. I have found this to occur in t~e absence of
added adsorbents or the like. Adsorbents, absorbents or the
like may be present; h~ever, it is preferred that they not be
present since the process is efective without them and they
might introduce undesired elements into the smoke or might
not release the carbon dioxide in a totally effective manner.
The tobacco, after the impregnation step, may then be
transported to a zone where it is subjected to conditions such
that the carbon dioxide is removed and the tobacco is expanded,
preferably by exposure to rapid heating at 100 to 370C for 1
second to 10 minutes and substantially atmospheric pressure.
A description of the improvement on the presently claimed
process will be described below, said improvement relating
specifically to the impregnation step.
To carry out the improvement on the present process, one
may treat either whole cured tobacco Leaf~ tobacco in cut or
-17-
'
,
chopped form, or selected parts of tobacco, such as tobacco
stems or may be reconstituted tobacco. In comminu~ed form,
the tobacco to be treated may have a particle size of fr~m
about 10 to about 100 mesh but is preferably not smaller t
than about 30 mesh.
The tobacco may contain the natural moisture content of
tobacco and may contain from about 5 to abou~ 35% by weight
moisture. It is preferred, however, for best results that
the tobacco have at least about 8% moisture (by weight) and
10 no more than about 22% (by weight) moisture. As used herein,
% moisture may be considered equivalent to oven volatiles (OV~
since not more than about 0.9% of tobacco weight is volatile
other than water. Oven volatiles determination is a simple
measurement of weight loss on exposure in a circulating air
oven for 3 hours at 100C.
The tobacco will generally be placed in a pressure vessel
which will be more fully described hereinafter. For example,
it may be placed in a wire cage or on a platform positioned
within the vessel.
The tobacco-containing pressure vessel may be then purged
with carbon dioxide gas, The benefits of purging are the re-
moval of gases that might interfere with a carbon dioxide re-
covery process and/or that might interfere with full penetra-
tion of the gaseous carbon dioxide. As an alternative to
purging with carbon dioxide gas, the vessel may be evacuated
prior to introduction of the carbon dioxide gas.
The carbon dioxide which is employed in the process of
this invention will generally be obtained from a storage ~essel
-18- 1
' ~
where it is maintained at a pressure of from about 215 to 305
psig and temperatures of from -29 to -16C. The carbon dioxide
may be introduced into the pressure vessel at 215 to 320 psig
and -29 to -14C, but is preferably brought, by suitable means,
to a temperature above -23C~ and a pressure above 250 psig
before being introduced into the pressure vessel.
Either with or without a preliminary purging or evacua-
tion of the vessel, carbon dioxide gas is fed to the vessel
under conditions whereby the carbon dioxide gas pressure in
the vessel is increased under conditions whereby the tobacco in -
the vessel is at a temperature of from about -10 to about 60C
and the pressure in the vessel is above about 250 psig, pre-
ferably about 400 to 800 psig. The tobacco/C02 system is
; cooled in such a way that the C02 enthalpy is brought below
about 140 BTU/lbm but the gas is preferably not condensed to
any significant degree, while the pressure is, preerably, held
substantially constant by admission of additional gas, and the
system is maintained at these conditions from about 15 seconds
to about 30 minutes. The pressure is then reduced over a period
of from about 1 to about 800 seconds, whereby the tobacco is
brought to a temperature below 10C, and atmospheric pressure or
the pressure at which the expansion step is to be carried out.
The resulting carbon dioxide-treated tobacco may then be
rapidly transported, as described earlier in this specification
to a zone where it is exposed to expansion conditions by sub-
~ecting it to heat or the equivalent in order to remove the
carbon dioxide from the tobacco. This may comprise the use of
--19--
. ... I
hot surraces, or a stream of hot air, a mixture of gases and
steam, or exposure to other energy sources, such as microwave
energy or infrared radiation. It has been found that the use
of a gas composition comprising at least 50~tO (by weight) of
steam, an~ preferably above 80% (by weight) of steam, provides
particularly satisfactory results. A convenient means of ex- i
panding t~e carbon dioxide-containing tobacco i~ to place it or
to entrain it in a stream of heated gas, such as superheated
steam or to place it in a turbulent air stream maintained, for
example, at a temperature of from about 150to about 260C (as
low as 100C and as high as 370C) for a period of about 1
second to 10 minutes, The impregnated tobacco may also be
heated by being placed on a moving belt and exposed to ~nfrared
heating by exposure in a cyclone dryer, by contact in a tower
with superheated steam or a mixture of steam and air or the
like. Any such contacting steps should not raise the tempera-
ture of the atmosphere with which the tobacco is in contact
to above about 370C and should preferably be from at about
100 to about 300C, most preferably 150 to 260C when con-
ducted at atmospheric pressure.
As is well known in the processing of any organic matter,
dverheating can cause damage, first to colour, such as undue
darkening and, finally, to the extent of charring. The nec-
essary and sufficient temperature and exposure time for ex-
pansion without such damage is a function of these two variables
as well as the state of subdivision of the tobacco. Thus, to
avoid und2sirable damage in the heating step, the impregnated
-20-
~L3~ 9
tobacco should not be exposed to the higher temperature levels,
e.g., 370C, longer than 1 to 2 seconds.
- One method for causing the expansion of the tobacco
cells is to use the radiation methods described in either
U.S. Patents 3,409,022 or 3,409,027. In this operation, the
tobacco never attains a temperature above about 140C, being
cooled by the rapid evolution of gases. The presence of
steam during heating assists in obtaining optimum results.
Another system, usually preferred, is to use a
dispersion dryer, for example, one that is supplied either
with steam alone or in combination with air. An example of
such a dryer is a Proctor & Schwartz PB dispersion dryer,
usually called hereafter a tower. The temperature in the
dryer may range from about 120 to 370C with contact time in
the dryer of about 1 to 10 seconds. In general, a 1 to 6
second contact time is utilized when the hot gas temperature
is 260 to 315C or somewhat higher. As stated before,
other known types of heating means may be used as long as
they are capable of causing the impregnated tobacco to expand
without excessive darkening. The presence of a steam
atmosphere of 20% or more of the total hot gas compo~ition
aids in obtaining the best expansion; a high proportion
(e.g., over 80% volume) of steam is preferred.
The present invention may be further understood by
referring to the drawings. In the drawings:
Fig. 1 is a standard phase diagram plotting
pressure of CO2 (in p.s.i.a.) vs temperature (in F) of the
tobacco bed
- 21 -
for the carbon dioxide-tobacco system, with line I-II-III
drawn thereon as an illustration of the system involved here.
Fig. 2 is a standard pressure enthalpy diagram, with
line I-IV drawn thereon to further illustrate the present
invention.
Fig. 3 is a standard pressure enthalpy diagram, with
line I-IV drawn thereon to illustra~e the process of the
present invention.
As a general illustration of the practice of this inven-
tion, reference may be made to Fig. 1. The conditions may,for example, be such as are represented by line I-II-III on
Fig, 1. For example, the tobacco, at about 12% OV in the form
of cut bright filler, is placed in a pressure vessel capable
of handling the desired pressure, for example, capable of
handling a pressure of 1057 psig The vessel may be similar
to the impregnation vessel de~cribed in Canadian Patent
No. 1,013,640, but, in distinction to that apparatus, need have
no means for the handling of liquid C02 The vessel may be
flushed with gaseous C02 or may be evacuated and is pressured
with gaseous C02 to bring the contents to a condition (at II)
where the pressure is greater than 250 psig and the temperature
is not less than -23C. The pressure is then released (to III).
The conditions of the entire sequence (as shown by line I-II-III3
are such that the carbon dioxide is maintained below and to
the right of the saturated vapor line on Fig. 1.
- In one form of the invention, as may be seen fro~ Fig. 2,
the enthalpy of the C02 is greater than about 140 BTUtlbm and
-22-
~i~ ~
the C02 is present in gaseous form. The vess~l may be main-
tained at these conditions for l/4 to 30 minutes, as illus-
trated by line I-III. The pressure may then be reduced
rapidly, preferably within 10 to 12~ seconds, preferably to
atmospheric pressure, as illustrated by line III-I~ in Fig. 2.
The impregnated tobacco then is transferred (preferably
but not necessarily directly) to a rapid heating zone or
vessel such as the heating vessel described in Canadian
Patent No. 1, 013, 640 mentioned above or as descrlbed earlier in
this specification, for example, an expansion tower, micro-
` wave chamber, or the like,
The temperature at which the impregnated tobacco is main-
tained prior to the expansion or rapid heating step will
largely govern how long the C02 remains in the tobacco in
sufficient quantity to cause the desired expansion. If there
is little insulation or means to keep the temperature down,
the transfer should be rapid~ preferably less than a few
minutes. An insulated "bulking" container is preferred to
accomplish the transfer; Supplementary cooling may also be
provided as, for example, by applying crushed or powdered dry
ice or by spraying liquid nitrogen on the impregnated tobacco.
The rapid heating causes expansion of the tobacco at a
temperature where the tobacco is pliable and elastic and the
tobacco can be expanded without fracture to an approximation
of its green leaf state. A significant and useful degree of
expansion is realized.
Referring to the Fig. 3, an illustration of the present
-23-
invention is shown Tobacco at about 12% OV in the form of
cut bright filler is placed in a pressure vessel. The vessel
may be similar to the impregnation vessel described in
Canadian Patent ~o. 1,013,640 but, in distinction to that
apparatus, need have no means for the handling o liquid CO2.
The vessel may be flushed with gaseous CO2 or may be evacuated
and is pressured with CO2 to bring the contents to a condition
wherein the pressure is greater than 250 psia and the tempera-
ture is not less than -23C, and the enthalpy is at or above
140 BTU/lbm as shown by line I-II in the drawing. The enthalpy
of the C02 is then reduced by cooling below about 140 BTU/lbm
(but at conditions of temperature and pressure such that the
C2 is present primarily as gas) as shown by line II-III. The
vessel is maintained at these conditions for 1/4 to 30 minutes.
The pressure is then reduced rapidly, preferably within 10 to
120 seconds, for example, to atmospheric pressure, as illus-
trated by line III-IV.
The impregnated tobacco then is transferred (preferably
but not necessarily directly) to a rapid heating zone or
vessel such as the heating vessel described in Canadian
Patent No. 1,~13,640, mentioned above, or as described earlier
ih this specification, for example, an expansion tower, ~icro-
wave chamber, or the like, The rapid heating causes expansion
of the tobacco at a temperature where the tobacco is pliable
and elastic and the tobacco can be expanded without fracture
to an approximation of its green leaf state. A significant
and useful degree of expansion is realized.
-24-
f
The temperature at which the impregnated tobacco is
maintained prior to the expansion or rapid heating step will
largely govern ho~ long the C02 re~ains in the tobacco in
sufficient quan~ity to cause the desired expansion, If there
is little insulation or means to kee2 the temperature down,
the transfer should be rapid, preferably less than a few
minutes. An insulated "bulking" container is preferred to
accomplish the transfer. Supplementary cooling may also be
provided as, for example, by applying crushed or powdered dry
ice or by spraying liquid nitrogen on the impregnated tobacco.
The following examples are illustrative:
EXAMPLE 1
A l-pound sample of commercial cased bright tobacco
filler at 12.5% OV was placed in an autoclave-type pressure
vessel and was pressurized to 800 psig with C02 gas obtained
from a C02 supply tank which was maintained at a C02 pressure
at least slightly above the desired impregnation pressure.
The impregnator system temperature was maintained above 30C
during the pressure cycle by supplying extra heat to the
system,when necessary,to prevent any forma~ion of liquid or
solid C02 during the entire processing cycle. After a 15-
oinute contact ~ime, the pressure and temperature conditions
of the C02 gas in the impregnator were found to correspond to
an enthalpy value of about 142 BTU/lb of C02 gas. The pressure
was released by venting in about 30 seconds after which the
tobacco temperature was found to be 2.2C. The impregnated
sample had a weight gain of 2.0% which is a~tributable to
-25- ~
the gaseous C02 contained therein. The l~.precnated material
was then, within about 5 minutes t~me, exposed to heating in
a 3-inch dia~e~er tobacco expansion tower by contact with
superheated steam at 288C and a velocity of 140 ft/sec for
about 4 seconds. The product exiting the expansion tower ~ad
an OV of 2.1%. The product was equilibrated at standard con- _
ditions of 23.9C and 60% RH for about 18 hours. The filling
power of the equilibrated product was measured by the s~andard-
- ized cylinder volume (CV) test described later in this specifi-
cation as 74 cc/10 g nt 11.2~ ov. This gave a corrected CV
(CCV) value at 11% OV of 76 cc/10 g. An unexpanded control
was found to have a cylinder volume of 36 cc/10 g. The sample
after processing, therefore, had a 111% increase in filling
power as measured by the CV method.
EXAMPLE 2
A series of bright tobacco samples were treated as in
Example 1 under conditions where gaseous C02 and substantially
no liquid or solid C02 would be formed. The tobacco feed OV
was varied from 9% to 14.6%. The conditions of each test and
the test results are shown ~n Table I. Where no value is shown
in the Table for a variable, the value is as in Example 1.
Table I
Filler Expansion with Gaseous C02
Te~st ~ 1 2 3
Tobacco Feed OV 9.0% 10 3Z 14.6%
Impregnation Pressure, psig 800 800 800
C2 Temperature Prior to Vent,C 31.7 31.7 32.2
C2 Enthalpy Prior to vent~BTu/lb. 143 143 143
Tobacco Temp. after Venting, DC -20.0 -22.8 ~2.8
% C2 Retention on Tobacco 2.9 2.4 1.5
Product OV after Expansion 1.7~ 1.8% 3.2%
Reordered Product CV 62 94 74
Reordered Product OV 11.6 10.3 11.3
Corrected CV at 11% OV 66 88 76
% Increase in ~illing Po;~er 83 144 111
-~h-
EXA~LE 3
A series of bright tobacco samples were treated as in
Example 1 under conditions whPre gaseous C02 and substantially
no liquid or solid C02 would b~ formed. The hold time was
varied. The conditions and test results are shown in Table II.
Nhere no value is shown in the Table for a variable, the
value is as in Example 1.
Table II
Filler Expansion with Gaseous C02
Test # 3 4 5
Tobacco Feed OV 14~2% 14~4% 15~3~/o
Impregnation Pressure, psig800 800 800
Hold Time, Minutes 1 2 2~
C2 Temperature prior to Vent, C 58~9 30~0 35~6
C2 Enthalpy prior to Vent,BTU/lb. 160 142 144
Tobacco Temp. after Venting, C 8~3 -5~6 4~4
% C2 Retention on Tobacco 2.0 2.6 1.5
Product OV after Expansion2~2% 2~0 3~8
Reordered Product CV 71~2 74~ 0 76 ~2
Reordered Product ~V 11.1 11.6 11.6
Corrected CV at 11% OV 72 78 80
% Increase in Filling Power100 117 122
Example 4
` A series of bright tobacco samples were treated as in
Example 1 at conditions where no liquid or sol~d C02 would be
expected to be formed. The impregnation pressure was varied.
The test results are shown in Table III. Where no value is
shown in the Table for a variable, the value is as in Exa~ple
-27-
Table III
F ler Ex~ansion with Gaseous C02
Test # 6 7 8 9 10 11
--
Tobacco Feed OV 14.5 13.6 10.3 16.1 13.2 13.3
Impregnation Pres-
sure, psig 300 400 500 600 700 800
Hold Time, Minutes 15 15 15 25 15 15
C2 Temperature prior
to Vent~ ~C -11.7 NA 20.620.6 19.4 53.g
C02 Enthalpy p~ior
-to Vent, BTU/lb. 143 NA 150 145 142 155
Tobacco Temp. after
Venting, C -13.9 NA 3.3-5.6 -16.7 20.6
Product OV after
Expansion 2.2 1.9 2.1 2.1 3.4 2.7
Reordered Product CV 69 66 59 75 74 60
Reordered Product ~V 10.7 11.5 11.7 11.4 11.5 11.6
Corrected CV at 11%
OV 66 69 64 79 77 65
Increase in Filling
Power 83 92 78 119 114 81
EXAMPLE 5
A l-pound sample of commercial cased bright tobacco
filler at 11.1% CV was placed in an FS-3 pressure vessel and
pr~essurized to 8~0 psig with C02 gas as in the procedure of
Example 1. The impregnation xystem temperature was cooled
by circulating a cooling solution through a jacket surrounding
the impregnation vessel until the C02 gas in the impregnator
was cooled to near its saturation temperature. After a 15-
minute contact time, the pressure and temperature conditions
-28- !
of the C02 gas in the impregnator were found to correspond to
an enthalpy value of about 130 BTU/lb. of C02 gas. Although
so~e C02 condensation probably occurred within the vessel, the
C2 was present primarily as a gas. The pressure was released
by venting in about 30 seconds after which the tobacco tempera- b
ture was found to be -37.8C, The impregnated sample had a
weight gain of about 3.5% attributable to C02. This impregnated
material was then heated as in Example 1. The product exiting
the expansion tower had an OV of 1.9~. The equilibrated pro-
duct had a CV of 90.6 at an OV of 10.8%. This corresponds to
- a CCV of 89 or an increase in filling power of 147Z over the
unexpanded control t36 cc/10 g).
EXAMPLE 6
A series of bright tobacco samples were treated as in
Example 5 at conditions where the C02 gas would be cooled to
near saturation prior to pressure release at three different
pressures. The conditions and test results sre shown in Table
IV. Where no value is shown in the Table for a variable, the
value is as in Example 1.
Table IV
Filler Expansion with Gaseous C02
Test ~ _ 13 14_
Tobacco Feed OV 9.5% 10.8 12.1
Impregnation Pressure, psig 800 600 S00 t
Hold Time, Minutes 15 15 20
C2 Temperature prior to Vent, C 19.4 7.2 2.2
C2 Enthalpy prior to Vent,BTU/lb. 129 139 139
Tobacco Temp. after Venting, ~C -38.9 -27.8 -18.3
-29- 1
Test # 12 13 14
% C2 Retention on Tobacco 3.7 2,6 2,4
Product OV a_ter Expansion 1.3% 1.4 1.9
Reordered Proauct GV 89 88 71
Reordered Product OV 10.5 10.9 11.9
Corrected CV ~t 11% OV 85 87 78
% Increase in Filling Power 136 142 117
EXAMPLE 7
The procedure of Example 5 was repeated using cased
burley tobacco. The equilibrated expanded product was found
to have a CV of 92.4 at 10.1~ OV or an increase of about 100%
over the unexpanded control.
EXAMPLE 8
The procedure of Example 5 was repeated using a tobacco
blend as normally used in cigarette manufacture. The product
, was found to have a CV of 78.1 at 11.1% oV or an increase of
about 105% over the unexpanded control.
- EXAMPLE 9
A l-pound sample of cased bright tobacco was processed
as in Example 1 and found to have a CCV of 81. This product
was blended at 25% with conventional tobacco blend. Cigarettes
were smoked and found to have a desirable taste and aroma;
firmness of the tobacco rod was acceptable.
EXAMPLE 10
A 13-pound sample of cased bright tobacco was processed
as in Example 5. The product was found to have a CCV of 78.
EXAMPIJE 11
A 5-pound sample of cased bright tobacco was impregnated
as in Example 5 but was then subjected to heating in a static
bed using 149C steam for a 5-minute exposure. The equilibrated
product was found to have a CV of 85.
30-
EXAMPLE 12
A series of runs was conducted following the process
of Example 5 and the runs were found to give cylinder volume
results of 80, 80, 80, 79, 84, 78, 79, 78 and 79,respectively.
This gives an average CV of 80 for the 9 trials or an increase
in filling power of 121$ over the untreated control.
EXAMPLE 13
A series of 3 runs was conducted according to the pro-
cess of Example 5, except that the feed tobacco was pre-chilled
to a temperature just below -20C before the tobacco was con-
tacted with the pressurized CO2 gas. The reordered product
CV results under these circumstances were fcund to be 92, 92
and 87, respectively. This gave an average increase in filling
power of 151% over the untreated control.
EXAMPLE 14
Two series of runs were conduct~d in a manner similar
2Q to Example 1. However, conditions were as indicated in Table
V with a ten-minute hold period and the tower conditions were:
3-inch tower at 600F, with 100% steam. Series #2 was run
under similar conditions to Series #1.
The results of both series of these runs are given in
Table V together with the results for an unexpanded control
sample and for a control sample which was expanded, without
any CO2 treatment:
- 31 -
Table V
Series #1 Series i~2
/O Reordered %Reordered
Press. (psig)OV CV/OV CCV OV CV/OV CCV
Control 11.836.8/12.6 - - - ~ t
Exp.control - - - 1.964.6/10.9
250 2.572.8/10.8 71.2 1.573.8/10.8 72.3 I
300 2.876.3/10.8 74.9 1.281.4/10.7 78.9
325 2.677.2/10.8 75.9 1.279.6/10.7 77.5
1~ 350 2.378.4/11.0 78.4 1.277.3/11.2 78.5
; 375 2.480.6/11.1 81.0 1.478.7/11.1 79.6 '
400 2.678.5/11.2 79.9 1.482.0/11.1 85.6
800 2.892.0/11.2 93.3 1.597.6/11.1 98.0
It ~ill be seen that pressures of 250 psig through 8~0
psig provided excellent expansion, compared with the controls.
The following experiments were also conducted:
Experiment 1
The impregnation procedure of Example 11 was repeated
but the impregnated material was simply allowed to warm to room
temperature and was not subjected to tower expansion. The re-
sulting product showed no gain, and perhaps a slight loss, in
CV compared to the untreated control.
Experiment 2 .
A comparison run of gaseous vs. liquid C02 impregnation
was conducted in the following manner.
1. Liquid C02--Three pounds of cased commercial bright
~obacco filler (OV of 12.7%) was impregnated with liquid C02
at 8~0 psig, cooled to 19.6C, and held for 15 minutes. There-
a~ter the excess liquid was drained and the pressure was re-
leased. A 23C/o gain in weîght WâS attributed to C02 pic~up.
-3~-
:~`
The material was somewhat clumped together because of the
large a~ount of retained C02.
2. Gaseous C02--Three pounds of cased commercial
bright tobacco filler (OV oE 13.3%) was pressurized with
gaseous C02 at 800 psig and 19.6~C for 15 minutes. Thereafter
the pressure was released. a 3% gain in weight was attributed
to C02 pickup. The material was free-flowing and easy to
handle.
Both samples were processed in a 4-inch diameter
tobac~o expansion tower and the samples were equilibrated and
measured for cylinder volume. The samples which utilized the
liquid impregnation was found to have a CCV o~ 79 and the com-
parable sample impregnated with C02 gas ~as found to have a
CCV of 82.
Experiment 3
A series of trials was conducted over an impregnation
pressure range of 20, 40, 60, 80, 100, 200, 300, 400, 600 and
- 800 psig, employing 10-minute contact time, following the
pattern of Example 1, with expansion iQ the tower with a steam
temperature of 316C. These samples were run, together with
an unexpanded control and with a control which was not con-
tacted with C02 with the conditions and the results set forth
in Table VI:
Table VI
Reordered
pressure (ps~ OV% CV OV CCV
Control 13.6 30.8 13.3 33.2
Exp. control 2.9 49.3 12.2 50.1
2.9 55.7 11.8 57.2
~-33- j
Reordered
Pressure (psi~) OV% CV OV CCV
2.4 54.3 11.9 56.3
2.0 57.7 11.6 58.2
2.5 57.7 11.7 58.7
100 2.6 55.7 11.7 56 7
200 2.3 56.4 11.7 57 4
3~0 2.7 55.0 11.8 56 .5
400 1.9 65.9 1~.5 68.9
600 1.8 75.9 11.6 80 7
800 1.8 84.4 11.5 88 4
Table VI illustrates that some expansion may be obtain-
ed at lower pressures, but pressures of about 400 psig may be
necessary to achieve product objectives. It will be seen,
however, from Example 14, that a pressure of 250 psig can be
effective to produce a satisfactory degree of expansion.
The terms "cylinder volume" and "corrected cylinder
volume" are units for measuring the degree of expansion of
tobacco. The term "oven-volatiles content" or "oven volatiles"
is a unit for measuring moisture content (or percentage of
moisture) in tobacco. As used throughout this application,
the values employed, in connection with these terms, are
determined as follows:
Cylinder Volume (CV~
.
Tobacco filler weighing 10.000 g is placed in a 3.358-cm
diameter cylinder and compressed by a 1875-g piston 3.335-cm in
diameter for 5 minutes. The resulting volume of filler is
reported as cylinder volume. This test is carried out ~t
standard environmental conditions of 23.9C and 60~ RH; con-
ventionally unless other-Jise stated, the sample is pre-condition-
ed in this environment for 18 hours.
, . . .
--34--
, . I
' , '
.
Corrected CYlinder Volu~e (CCV)
The CV value may be adjusted to some specified oven-
volatile content in orde~ to facilitate comparisons.
CV = CV + F (OV - OVs) where OVs is the specified OV
and F is a correction fac~or (volume per %) predetermined for
the particular type of tobacco filler being dealt with
- Oven-Volatiles Content ~
The sample of tobacco filler is weighed before and
after exposure for 3 hours in a circulating air oven controlled
1~ at 100C. The weight loss as percentage of initial weight is
oven-volatiles content.
For bright tobacco employed in the present applica-
tion, the value of F in the calculation of CCV is 7.6 on
average for gaseous C02 expanded tobacco.
Unless otherwise indicated, all percentages used here-
in are by weight.
'
3~-
. I ,
t
