EP2832244B1 - Procédé de production d'une matière pour tabac, matière pour tabac à usage oral, et produit pour tabac à usage oral - Google Patents

Procédé de production d'une matière pour tabac, matière pour tabac à usage oral, et produit pour tabac à usage oral Download PDF

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Publication number
EP2832244B1
EP2832244B1 EP13769140.8A EP13769140A EP2832244B1 EP 2832244 B1 EP2832244 B1 EP 2832244B1 EP 13769140 A EP13769140 A EP 13769140A EP 2832244 B1 EP2832244 B1 EP 2832244B1
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Prior art keywords
tobacco
ozone
starting material
water
suspension
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EP13769140.8A
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German (de)
English (en)
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EP2832244A4 (fr
EP2832244A1 (fr
Inventor
Masashi FURUKOSHI
Michinori Yokoi
Manabu Takeuchi
Hirokazu MIYAMAE
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Japan Tobacco Inc
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Japan Tobacco Inc
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts

Definitions

  • the present invention relates to a method for producing a tobacco material, a tobacco material for oral use, and a tobacco product for oral use.
  • a method comprising adding water to a tobacco starting material, heating based on tube heat, heating based on steam spraying, and drying with hot air in order to modify the tobacco material is known.
  • a saccharide or the like is added, if necessary.
  • U.S. Patent Application Publication No. 1757477 discloses a method for directly bringing a tobacco starting material into contact with an ozone gas.
  • the permeability of ozone into an object to be treated is very low.
  • the reaction in the tobacco starting material is not expected or a long treatment time is required.
  • the treatment efficiency is low. This is inefficient and the treatment cost is high.
  • U.S. Patent application 2012/0060854 discloses mixing a tobacco material with water and an additive and heating the mixture at a temperature of at least 60°C for the purpose of reducing acrylamide content.
  • An oxidizing agent such as ozone is disclosed as an example of the additive.
  • U.S. Patent application 2006/0037620 discloses bringing an aqueous tobacco extract into contact with a gas (for example ozone) to remove proteins.
  • a gas for example ozone
  • a tobacco product for oral use has attracted attention in recent years.
  • the tobacco product for oral use is produced by putting a tobacco material for oral use containing moist tobacco powder in a water-permeable pouch.
  • the tobacco product for oral use is inserted between the lip and the gum of the mouth to enjoy the taste and fragrance of the tobacco.
  • a pH regulator is added to the moist tobacco powder so as to adjust a nearly neutral region of the pH to an alkaline region.
  • preferable flavor and taste are provided.
  • the pH adjusted during the storage period is substantially maintained from the viewpoint of quality maintenance.
  • Jpn. PCT National Publication No. 2009-082331 discloses a tobacco product which contains magnesium carbonate as a pH regulator to make a tobacco material alkaline.
  • the article also discloses that an additional pH regulator may be used, in addition to magnesium carbonate.
  • an additional pH regulator may be used, in addition to magnesium carbonate.
  • sodium carbonate, phosphate or the like are described.
  • the additional pH regulator is used to rapidly adjust the pH of the tobacco material to a desired pH value (neutral or alkaline).
  • the amount of the alkaline substance to be uniquely determined is an amount required to adjust the pH of the moist tobacco powder to a desired neutral or alkaline pH value. Further, as the amount of the alkaline substance to adjust the pH of the tobacco powder to a desired pH value is relatively small, it is not possible to maintain the adjusted pH value over a long period of time. As a result, it is necessary to store the tobacco product for oral use containing the tobacco powder whose initial pH is adjusted using only the alkaline substance not at room temperature but at a low temperature (-20°C to 10°C).
  • the tobacco product for oral use containing the moist tobacco powder that is used in the mouth desirably has a pH of 9.0 or less.
  • a tobacco product for oral use in the form such that a tobacco material is wrapped with a bag-shaped pouch of non-woven fabric and the whole pouch is put into the mouth for use is known.
  • the pigment component as an ingredient in the tobacco product for oral use is eluted into the water content and attached to the pouch, color stains such as spots may be formed on the pouch.
  • the pigment component as an ingredient seeps into the pouch through the saliva and the pouch is colored.
  • Such color staining of the pouch easily gives an unpleasant impression.
  • Color stains derived from the pigment component as an ingredient impair an aesthetic appearance of the product.
  • a method comprising allowing only the pigment component in the tobacco starting material to be eluted to the extent that color staining of the pouch is not caused and removing it has been attempted.
  • the method impairs a taste component of the tobacco starting material, and thus it has been technically difficult.
  • An object of the present invention is to provide a method for producing a tobacco material in which bad habits are removed and the bleaching or the like is modified and which has a excellent storage stability over a long period of time.
  • Another object of the present invention is to provide a tobacco material for oral use having a high brightness by Hunter.
  • Still another object of the present invention is to provide a tobacco product for oral use which contains a tobacco material for oral use having a high brightness by Hunter and exhibits an aesthetic appearance during storage and after use.
  • a method for producing a tobacco material which comprises:
  • a method for producing a tobacco material which comprises:
  • a method for producing a tobacco material which comprises:
  • a tobacco material for oral use produced by the method according to any of the first to third aspects.
  • a tobacco product for oral use which contains a tobacco material for oral use having a brightness by Hunter of 35 or more.
  • the method for producing a tobacco material according to the first embodiment includes the following steps.
  • a mixed suspension of a tobacco starting material residue and an extract of a water-soluble component is prepared by immersing a tobacco starting material in water to allow the water-soluble component in the tobacco starting material to be dissolved in water.
  • Ozone is supplied to the mixed suspension to be dissolved in it.
  • the dissolved ozone is brought into contact with the mixed suspension.
  • ozone is supplied to the mixed suspension of the tobacco starting material residue and the extract of the water-soluble component to be dissolved in it, and the dissolved ozone is brought into contact with the mixed suspension so that the reaction of the mixed suspension with the ozone can efficiently proceed.
  • the substance which decomposes to release an acidic component is also referred to as "a substance decomposable to release an acidic component".
  • the substance decomposable to release an acidic component e.g., polysaccharide
  • the substance decomposable to release an acidic component may be pre-oxidized before the storage of the tobacco material and released as an acidic component.
  • the amount of the dissolved ozone to be brought into contact with the mixed suspension is adjusted, namely, the level of treatment for the tobacco starting material residue and the extract of the water-soluble component is selected so that it is possible to produce a tobacco material from which undesirable characteristics have been removed without impairing the flavor of tobacco, and the color tone resulting from the pigment component is adjusted (the whiteness is increased).
  • a tobacco material the whiteness of which is increased, for example, to a Hunter brightness of 35 or more may be used as a tobacco material for oral use.
  • a tobacco product for oral use for example, a tobacco product for oral use in the form such that a tobacco material is wrapped with a bag-shaped pouch of non-woven fabric and the whole pouch is put into the mouth for use, color staining of the pouch due to the pigment component during storage and after use is reduced. Accordingly, there can be provided a tobacco product having an improved aesthetic appearance.
  • Examples of the tobacco starting material used in Step a may include tobacco leaves and stems separated from the tobacco leaves.
  • the stems are rolled with a rolling mill and finely cut.
  • the resulting products may be used as stem shreds.
  • the type of water-soluble component in the tobacco starting material is not particularly limited.
  • examples thereof may include carbohydrates (saccharides), alkaloids, proteins, and amino acids.
  • the amount of water is preferably 5 to 20 times the amount of the tobacco starting material.
  • Water may be at normal temperature and it is preferably heated to 20 to 60°C.
  • the time for immersing the tobacco starting material in water is, for example, 10 minutes to 2 hours. In immersing the tobacco starting material in water, it is preferable that both the materials are stirred to facilitate the water-soluble component in the tobacco starting material dissolving in water.
  • the ozone is preferably dissolved in an amount of 0.5 to 500 g per 1 L of the extract in the mixed suspension.
  • the degree of reaction of the ozone with an extract of a tobacco starting material residue and a water-soluble component, that is, the degree of treatment may be selected by changing the ozone dissolution amount.
  • the step of supplying ozone (Step b) is performed by exposing the mixed suspension to ozone.
  • the ozone exposure allows the tobacco starting material residue and the extract in the mixed suspension to be in contact with not only the dissolved ozone but also the bubble ozone. As a result, it is possible to effectively react the water-soluble component in the tobacco starting material residue and the extract with the ozone.
  • the ozone bubbles In the ozone exposure, the ozone bubbles have a diameter of 0.5 to 1000 ⁇ m, more preferably a diameter of 0.5 to 100 ⁇ m.
  • the mixed suspension is stirred, circulated with a pump or both the stirring and circulating processes are performed.
  • the stirring and circulating processes allow the contact efficiency of the tobacco starting material residue and the extract in the mixed suspension with the ozone to be increased.
  • the step of supplying ozone is continuously performed so that the ozone dissolved in the mixed suspension as a reaction field is always present.
  • the mixed suspension after the ozone treatment may be dried.
  • the mixed suspension after the ozone treatment is subjected to solid liquid separation and the tobacco starting material residue as a solid is dried.
  • the separated extract may be applied by spraying so that the component of the extract is incorporated into the dry product.
  • the pH and water content of the resulting dry product are adjusted with a pH regulator to produce a target tobacco material.
  • a pH regulator for example, sodium carbonate or potassium carbonate may be used.
  • the tobacco material after adjustment of the pH and the water content preferably has a pH of 7.0 to 9.0 and a water content of 10.0 to 50.0% by mass.
  • FIG. 1 shows a flow in the method for producing a tobacco material according to the first embodiment.
  • a tobacco starting material is prepared in Step S1.
  • Step S2 Water is added to the tobacco starting material in Step S2.
  • the tobacco starting material is stirred in a state immersed in water at Step S3.
  • the water-soluble component in the tobacco starting material is eluted to form an extract.
  • Step S4 The mixed suspension of the tobacco starting material residue and the extract obtained in Step S4 is exposed to ozone (O 3 ) in Step S5, the ozone is dissolved, and the process of bringing the aforementioned into contact with the ozone dissolved in the mixed suspension is performed.
  • Step S6 The mixed suspension is dried in Step S6. Thereafter, in Step S7, the pH and water content of the dry product are adjusted to produce a tobacco material.
  • the method for producing a tobacco material according to the second embodiment includes the following steps.
  • a tobacco starting material is immersed in water to allow a water-soluble component in the tobacco starting material to be dissolved in water.
  • the tobacco starting material residue after the extraction is separated from the extract of the water-soluble component.
  • the separated tobacco starting material residue is again mixed with water to prepare a suspension.
  • Ozone is supplied to the suspension to be dissolved in it, and the dissolved ozone is brought into contact with the suspension.
  • the water-soluble component of the tobacco starting material is extracted, the tobacco starting material residue is separated from the extract, the tobacco starting material residue is again mixed with water to prepare a suspension, ozone is supplied to the suspension to be dissolved in it, and the dissolved ozone is brought into contact with the tobacco starting material residue of the suspension so that the reaction of the tobacco starting material residue (including a large amount of the substance decomposable to release an acidic component) with the ozone can efficiently proceed.
  • the substance decomposable to release an acidic component in the tobacco starting material residue can be oxidized by effectively bringing it into contact with the ozone.
  • the substance decomposable to release an acidic component may be pre-oxidized before the storage of the tobacco material and released as an acidic component.
  • the amount of the dissolved ozone is adjusted, namely, the level of treatment for the tobacco starting material residue is selected so that it is possible to produce a tobacco material from which undesirable characteristics have been removed without impairing the flavor and the color tone resulting from the pigment component is adjusted (the whiteness is increased).
  • a tobacco material the whiteness of which is increased, for example, to a Hunter brightness of 35 or more may be used as a tobacco material for oral use.
  • a tobacco product for oral use for example, a tobacco product for oral use in the form such that a tobacco material is wrapped with a bag-shaped pouch of non-woven fabric and the whole pouch is put into the mouth for use, color staining of the pouch due to the pigment component during storage and after use is reduced. Accordingly, there can be provided a tobacco product having an aesthetic appearance.
  • Examples of the tobacco starting material used in Step a may include tobacco leaves and stems separated from the tobacco leaves.
  • the stems are rolled with a rolling mill and finely cut.
  • the resulting products may be used as stem shreds.
  • a target to be subjected to the ozone treatment is the tobacco starting material residue after the separation of the extract, one containing the substance decomposable to release an acidic component (e.g., polysaccharide) in the residue after the extraction of water may be selected as the tobacco starting material.
  • an acidic component e.g., polysaccharide
  • the conditions of immersing the tobacco starting material in water are preferably set to the same conditions as the first embodiment.
  • the separation step (in Step b) may be performed using, for example, a barrier filter.
  • the ozone is preferably dissolved in an amount of 0.5 to 500 g per 1 L of the water in the mixed suspension.
  • the degree of reaction of the ozone with a tobacco starting material residue may be selected by varying the amount of ozone dissolution.
  • the step of supplying ozone (Step d) is preferably performed by exposing the mixed suspension to ozone.
  • the ozone exposure allows the tobacco starting material residue in the suspension to be in contact with not only the dissolved ozone but also the bubble ozone. Thus, it is possible to effectively react the tobacco starting material residue with the ozone.
  • the ozone bubbles In the ozone exposure, the ozone bubbles have a diameter of 0.5 to 1000 ⁇ m, more preferably a diameter of 0.5 to 100 ⁇ m.
  • the suspension is stirred, circulated with a pump or both the stirring and circulating processes are performed.
  • the stirring and circulating processes allow the contact efficiency of the tobacco starting material residue and the extract in the mixed suspension with the ozone to be increased.
  • the step of supplying ozone is continuously performed so that the ozone dissolved in the suspension as a reaction field is always present.
  • the suspension after the ozone treatment is dried.
  • the drying process is performed at 40 to 100°C so that the moisture content of the dry product is from 5.0 to 50.0% by mass.
  • the pH and water content of the resulting dry product are adjusted with a pH regulator to produce a target tobacco material.
  • a pH regulator for example, sodium carbonate or potassium carbonate may be used.
  • the tobacco material after adjustment of the pH and the water content preferably has a pH of 7.0 to 9.0 and a water content of 10.0 to 50.0% by mass.
  • the extract separated after the extraction may not be used depending on the purpose or may be sprayed to the suspension during drying so as to return it to an original state.
  • FIG. 2 shows a flow in the method for producing a tobacco material according to the second embodiment.
  • a tobacco starting material is prepared in Step S1.
  • Step S2 Water is added to the tobacco starting material in Step S2.
  • the tobacco starting material is stirred in a state immersed in water at Step S3.
  • the water-soluble component in the tobacco starting material is eluted to form an extract.
  • Step S4 The suspension after the extraction of the water-soluble component in Step S4 is subjected to solid liquid separation to obtain a tobacco starting material residue shown in Step S5 and an extract shown in Step S6.
  • Step S7 Water is added to the tobacco starting material residue in Step S7 and a suspension is prepared in Step S8.
  • the suspension is exposed to ozone (O 3 ) in Step S9, the ozone is dissolved in water, and the process of bringing the dissolved ozone into contact with the suspension is performed.
  • Step S10 The suspension is dried in Step S10. Thereafter, the pH and water content of the dry product are adjusted in Step S11 to produce a tobacco material.
  • the extract obtained in Step S6 may be returned by the spraying process during drying of the suspension of Step S10.
  • the method for producing a tobacco material according to the third embodiment includes the following steps.
  • a tobacco starting material is immersed in water to allow a water-soluble component in the tobacco starting material to be dissolved in water.
  • the tobacco starting material residue after the extraction is separated from the extract of the water-soluble component.
  • Ozone is supplied to the separated extract to be dissolved in it, and the dissolved ozone is brought into contact with the extract.
  • the tobacco starting material residue separated in Step b is dried, and the extract after the ozone treatment is applied to the tobacco starting material residue during the drying process by, for example, spraying.
  • ozone is supplied to the extract of the water-soluble component extracted from the tobacco starting material to be dissolved in it, and the dissolved ozone is brought into contact with the extract so that the reaction of the extract with the ozone can efficiently proceed.
  • the substance decomposable to release an acidic component e.g., saccharide
  • the substance decomposable to release an acidic component may be pre-oxidized before the storage of the tobacco material and released as an acidic component.
  • the extract after the ozone treatment (including the substance decomposable to release an acidic component which has been already oxidized) is applied so as to return it to the residue.
  • the substance decomposable to release an acidic component is prevented from being decomposed by aging and releasing the acidic component during the storage of the resulting tobacco material.
  • the pH adjusted during the storage can be substantially maintained.
  • a tobacco material excellent in storage stability can be produced.
  • the amount of the dissolved ozone is adjusted, namely, the level of treatment for the extract of the water-soluble component is selected so that undesirable characteristics can be removed without impairing the flavor and the color tone resulting from the pigment component of the extract can be adjusted (the whiteness is increased).
  • the extract after the ozone treatment is returned to the residue by the spraying process so that it is possible to produce a tobacco material in which the flavor is maintained, there are no undesirable characteristics, and the whiteness is increased.
  • a tobacco material of which the whiteness is increased to for example, a Hunter brightness of 35 or more may be used as a tobacco material for oral use.
  • a tobacco product for oral use for example, a tobacco product for oral use in the form such that a tobacco material is wrapped with a bag-shaped pouch of non-woven fabric and the whole pouch is put into the mouth for use, color staining of the pouch due to the pigment component during storage and after use is reduced. Accordingly, there can be provided a tobacco product having a good aesthetic appearance.
  • Examples of the tobacco starting material used in Step a may include tobacco leaves and stems separated from the tobacco leaves.
  • the stems are rolled with a rolling mill and finely cut.
  • the resulting products may be used as stem shreds.
  • a target to be subjected to the ozone treatment is the extract
  • one containing the substance decomposable to release an acidic component (e.g., saccharide) in the extract may be selected as the tobacco starting material to be subjected to the treatment.
  • the conditions in immersing the tobacco starting material in water are preferably set to the same conditions as the first embodiment.
  • the separation step (in Step b) may be performed using, for example, a barrier filter.
  • the ozone is preferably dissolved in an amount of 0.5 to 500 g per 1 L of the extract.
  • the degree of reaction of the ozone with a starting material, that is, the degree of treatment may be selected by varying the amount of ozone dissolution.
  • the step of supplying ozone (Step c) is preferably performed by exposing the extract to ozone.
  • the ozone exposure allows the extract to be in contact with not only the dissolved ozone but also the bubble ozone. Thus, it is possible to effectively react the extract with the ozone.
  • the ozone bubbles In the ozone exposure, the ozone bubbles have a diameter of 0.5 to 1000 ⁇ m, more preferably a diameter of 0.5 to 100 ⁇ m.
  • the extract is stirred, circulated with a pump or both the stirring and circulating processes are performed.
  • the stirring and circulating processes allow the contact efficiency of the extract with the ozone to be increased.
  • the step of supplying ozone is continuously performed so that the ozone dissolved in the extract as a reaction field is always present.
  • the process of drying the separated tobacco starting material residue in Step d is preferably performed at 40 to 100°C because the extract treated with the ozone during the drying process is returned by the spraying process.
  • the drying process is performed so that the moisture content of the resulting dry product is from 5.0 to 25.0% by mass.
  • Step d a partial or total amount of the extract (the extract treated with the ozone) may be applied to the tobacco starting material residue during the drying process.
  • the pH and water content of the dry product obtained in Steps a to d are adjusted with a pH regulator to produce a target tobacco material.
  • a pH regulator for example, sodium carbonate or potassium carbonate may be used.
  • the tobacco material after adjustment of the pH and the water content preferably has a pH of 7.0 to 9.0 and a water content of 10.0 to 50.0% by mass.
  • FIG. 3 shows a flow in the method for producing a tobacco material according to the third embodiment.
  • a tobacco starting material is prepared in Step S1.
  • Step S2 Water is added to the tobacco starting material in Step S2.
  • the tobacco starting material is stirred in a state immersed in water at Step S3.
  • the water-soluble component in the tobacco starting material is eluted to form an extract.
  • Step S4 The suspension after the extraction of the water-soluble component in Step S4 is subjected to solid liquid separation to obtain a tobacco starting material residue shown in Step S5 and an extract shown in Step S6.
  • the extract is exposed to ozone (O 3 ) in Step S7, the ozone is dissolved in water, and the process of bringing the dissolved ozone into contact with the extract is performed.
  • Step S8 The tobacco starting material residue after solid liquid separation in Step S8 is dried, and the extract after the ozone treatment is returned to the tobacco starting material residue during the drying process by the spraying process. Thereafter, in Step S9, the pH and water content of the dry product are adjusted to produce a tobacco material.
  • the separated tobacco starting material residue is again mixed with water to prepare a suspension.
  • Ozone is supplied to the suspension to be dissolved in it, and the dissolved ozone is brought into contact with the suspension.
  • the suspension after the ozone treatment is dried, and the extract after the ozone treatment is, for example, returned to the tobacco starting material residue dry product during drying, by, for example, the spraying process.
  • FIG. 4 shows a flow in the method for producing a tobacco starting material.
  • a tobacco starting material is prepared in Step S1.
  • Step S2 Water is added to the tobacco starting material in Step S2.
  • the tobacco starting material is stirred in a state immersed in water at Step S3.
  • the water-soluble component in the tobacco starting material is eluted to form an extract.
  • Step S4 The suspension after the extraction of the water-soluble component in Step S4 is subjected to solid liquid separation to obtain a tobacco starting material residue shown in Step S5 and an extract shown in Step S6.
  • Step S7 Water is added to the tobacco starting material residue in Step S7 and a suspension is prepared in Step S8.
  • the suspension is exposed to ozone (O 3 ) in Step S9, the ozone is dissolved in water, and the process of bringing the dissolved ozone into contact with the suspension is performed.
  • the extract obtained by solid liquid separation in Step S4 is exposed to ozone (O 3 ) in Step S11, the ozone is dissolved in water, and the process of bringing the dissolved ozone into contact with the extract is performed.
  • Step S10 the extract after the ozone treatment is returned by the spraying process. Thereafter, the pH and water content of the dry product are adjusted in Step S12 to produce a tobacco material.
  • appropriate ozone treatment may be performed depending on the properties of the tobacco starting material residue after the extraction and the properties of the extract.
  • the ozone treatment is performed on the mixed suspension of the tobacco starting material residue and the extract after the extraction.
  • the ozone effect is uniformly applied to the tobacco starting material residue and the extract.
  • a large amount of the substance decomposable to release an acidic component may be contained in the tobacco starting material residue after the extraction, depending on the kind of the tobacco starting material.
  • a large amount of the substance decomposable to release an acidic component may be contained in the extract.
  • the flavor, undesirable characteristics, and the pigment component may be weighted in either the tobacco starting material residue or the extract.
  • the tobacco starting material residue and the extract are respectively treated with the ozone so that the degree of the reaction of the tobacco starting material residue and the extract with the ozone, namely, the treatment degree can be independently and arbitrarily adjusted according to their properties.
  • the degree of the reaction of the tobacco starting material residue and the extract with the ozone namely, the treatment degree can be independently and arbitrarily adjusted according to their properties.
  • the tobacco product for oral use according to the fourth embodiment includes a tobacco material for oral use having a Hunter brightness of 35 or more.
  • a more preferred tobacco material for oral use has a Hunter brightness of 37 or more.
  • the tobacco product for oral use has, for example, a structure in which a tobacco material is wrapped with a bag-shaped pouch of non-woven fabric. As for the tobacco product for oral use, the whole pouch is put into the mouth for use.
  • the tobacco material for oral use may be obtained by the method for producing a tobacco material described in the first to third embodiments.
  • the tobacco material for oral use may be obtained by treating the tobacco starting material with an oxidant except for the ozone.
  • an oxidant for example, hydrogen peroxide may be used.
  • the tobacco product for oral use according to the fourth embodiment includes a tobacco material for oral use having a Hunter brightness of 35 or more, color staining of the pouch due to the pigment component during storage and after use is reduced and an aesthetic appearance is exhibited.
  • the moisture content of 3.0 g of a powdered tobacco material was measured using a heat drying type moisture meter (HB 43-S: manufactured by METTLER TOLEDO International Inc.).
  • water in an amount required to adjust the final moisture content of the tobacco material to 25.0% by mass
  • Sodium carbonate was added to the water in an amount of 3.0% by mass based on the dry weight of the tobacco material.
  • the total amount of the resulting sodium carbonate solution was sprayed to the tobacco starting material to produce a tobacco material having a moisture content of 25% by mass and a pH (initial value) of 8.43.
  • the stirring was continued and the exposure to ozone fine bubbles was continued for 3 hours while circulating the mixed suspension of the tobacco starting material residue and the extract with a pump.
  • the average diameter of the ozone fine bubbles was 10 ⁇ m and the exposure to ozone was carried out at 25°C and 38.0 g/hr.
  • the mixed suspension after the ozone treatment was subjected to solid-liquid separation.
  • the extract as a liquid was sprayed to the tobacco starting material residue while heating the tobacco starting material residue as a solid to 80°C.
  • the moisture content of the resulting dry product was measured. As a result, the moisture content of the dry product was 8.8% by mass.
  • the mixed suspension after the ozone treatment was subjected to solid-liquid separation.
  • the extract as a liquid was sprayed to the tobacco starting material residue while heating the tobacco starting material residue as a solid to 80°C.
  • the moisture content of the resulting dry product was measured. As a result, the moisture content of the dry product was 8.5% by mass.
  • Example 2 Four kg of a tobacco starting material with the same composition as that of Example 2 and 80 L of water were stirred and mixed for 30 minutes so as to allow the component in the tobacco starting material to be eluted (dissolved) in water. Subsequently, the stirring was continued and the exposure to ozone fine bubbles was continued for 3 hours while circulating the mixed suspension of the tobacco starting material residue and the extract with a pump. At this time, the average diameter of the ozone fine bubbles was 10 ⁇ m and the exposure to ozone was carried out at 25°C and 38.0 g/hr.
  • the mixed suspension after the ozone treatment was subjected to solid-liquid separation.
  • the extract as a liquid was sprayed to the tobacco starting material residue while heating the tobacco starting material residue as a solid to 80°C.
  • the moisture content of the resulting dry product was measured. As a result, the moisture content of the dry product was 8.5% by mass.
  • water in an amount required to adjust the final moisture content of the tobacco material to 50.0% by mass
  • Sodium carbonate was added to the water in an amount of 2.8% by mass based on the dry weight of the tobacco material.
  • the total amount of the resulting sodium carbonate solution was sprayed to the dry product to produce a tobacco material having a moisture content of 25% by mass and a pH (initial value) of 8.48.
  • Ten g of a sample was placed in a sample bag of polyethylene terephthalate (volume: about 2 L), and the inside of the bag was substituted with a nitrogen gas. Thereafter, it was allowed to stand at room temperature for about 3 hours and used as a sample gas.
  • the smell of the sample gas was measured under the following conditions using a smell identification testing device.
  • the odor contribution is a value obtained by representing the strength of the smell of the system as an odor index equivalent value.
  • the calculated value is the set threshold or less, it is represented by a minus (-) value (the lowest value: - 30) .
  • the pH during the production, the pH after storage for two months, and the pH after storage for four months were measured by the following method. The results are shown in FIG. 5 .
  • the tobacco material was placed in an atmosphere where the temperature went up and down every day (25 to 30°C).
  • the pH during storage in the tobacco materials obtained in Examples 1 to 3 can be significantly controlled as compared to that of the tobacco material obtained in Comparative Example 1. In other words, changes in the pH during storage are small.
  • the stirring was continued and the exposure to ozone fine bubbles was continued for 10 minutes, for 20 minutes, for 30 minutes, for 40 minutes, for 80 minutes, and 120 minutes while circulating the mixed suspension of the tobacco starting material residue and the extract with a pump.
  • the average diameter of the ozone fine bubbles was 45 ⁇ m and the exposure to ozone was carried out at 25°C and 6.0 g/hr.
  • the mixed suspension after the ozone treatment was subjected to solid-liquid separation.
  • the extract after the separation was concentrated.
  • the concentrated extract was sprayed to the tobacco starting material residue after the separation so as to make it return to the original state while keeping the residue at 40°C, and thus six kinds of tobacco materials were produced.
  • a tobacco material was produced in the same manner as Examples 4 to 9 except that the circulation of the mixed suspension of the tobacco starting material residue and the extract with a pump and the exposure to ozone fine bubbles were not performed.
  • a powdered tobacco material was collected and placed in a petri dish having a diameter of 12 cm until the thickness was about 2 cm.
  • the brightness, hue, and saturation were measured with a hue color difference meter (Hue color difference meter CR410, manufactured by Konica Minolta, Inc.).
  • the temperature of the mixed suspension of the tobacco starting material residue and the extract was set to 5°C, 25°C, and 80°C.
  • the exposure to ozone fine bubbles was continued for 5 hours while circulating the mixed suspension with a pump. At this time, the average diameter of the ozone fine bubbles was 45 ⁇ m and the exposure to ozone was carried out at 6.0 g/hr.
  • the mixed suspension after the ozone treatment was subjected to solid-liquid separation.
  • the extract after the separation was concentrated.
  • the concentrated extract was sprayed to the tobacco starting material residue after the separation so as to make it return to the original state while keeping the residue at 40°C, and thus three kinds of tobacco materials were produced.
  • the tobacco materials of Examples 9 and 10 in which the temperature of the mixed suspension was set to 5°C and 25°C showed a high Hunter brightness as compared to that of the tobacco material of Example 11 in which the temperature of the mixed suspension was set to 80°C. This is because the solubility of ozone is higher at the low temperature side.
  • water in an amount required to adjust the final moisture content of the tobacco material to 25.0% by mass was prepared.
  • the water was sprayed to the dry product to produce a tobacco material having a moisture content of 25.2% by mass.
  • the suspension after the ozone treatment was subjected to solid-liquid separation and only the tobacco starting material residue as a solid was collected.
  • the residue was heated and dried at 80°C.
  • the moisture content of the dry product was measured. As a result, the moisture content of the dry product was 9.4% by mass.
  • water in an amount required to adjust the final moisture content of the tobacco material to 25.0% by mass was prepared.
  • the water was sprayed to the dry product to produce a tobacco material having a moisture content of 24.7% by mass.
  • Example 13 shows a high Hunter brightness as compared to that of the tobacco material obtained in Comparative Example 3.
  • a tobacco starting material consisting of 60% by mass of laminae (18% by mass of burley and 42% by mass of rustica) and 40% by mass of stems was prepared.
  • the exposure to ozone fine bubbles was continued for 120 minutes while circulating the extract with a pump. At this time, the average diameter of the ozone fine bubbles was 45 ⁇ m and the exposure to ozone was carried out at 25°C and 6.0 g/hr. After the treatment, the ozone was concentrated to a volume of 10% or less under reduced pressure at 60°C.
  • the total amount of the extract after the ozone treatment was sprayed for drying while heating the tobacco starting material residue at 40°C (RH 60%).
  • the resulting product was allowed to stand at 22°C and 60% RH for 12 hours to produce a tobacco material having a moisture content of 14.6% by mass and a pH of 3.726.
  • Example 14 5 g of the tobacco starting material having the same composition as that of Example 14 and 400 mL of water were stirred and mixed for 30 minutes so as to allow the component in the tobacco starting material to be eluted or dissolved in water. Subsequently, the mixed suspension was filtered to be separated into an extract and a tobacco starting material residue.
  • the exposure to ozone fine bubbles was continued for 120 minutes while circulating the extract with a pump. At this time, the average diameter of the ozone fine bubbles was 45 ⁇ m and the exposure to ozone was carried out at 25°C and 6.0 g/hr. After the treatment, the ozone was concentrated to a volume of 10% or less under reduced pressure at 60°C.
  • the total amount of the extract after the ozone treatment was sprayed for drying while heating the treated residue at 40°C (RH 60%).
  • the resulting product was allowed to stand at 22°C and 60% RH for 12 hours to produce a tobacco material having a moisture content of 12.2% by mass and a pH of 3.227.
  • the tobacco material of Example 14 obtained by spraying the extract after the ozone treatment to the tobacco starting material residue after the extraction exhibits a high Hunter brightness.
  • the tobacco material of Example 15 obtained by spraying the extract after the ozone treatment to the tobacco starting material residue treated with the ozone after the extraction and drying it exhibits a high Hunter brightness as compared to that of the tobacco material of Example 14.
  • One g of the tobacco starting material having the same composition as that of Example 14 was mixed with 5% of hydrogen peroxide water to prepare a mixed suspension.
  • the suspension was allowed to stand for 12 hours, followed by filtration of the mixed suspension to obtain a residue.
  • the treated residue was dried while heating the residue at 40°C (RH 60%).
  • the resulting product was allowed to stand at 22°C and 60% RH for 12 hours to produce a tobacco material.
  • the Hunter brightness of the resulting tobacco material was measured, and it was 47.1.
  • a tobacco product for oral use which contains a tobacco material for oral use having a high Hunter brightness, and exhibits an aesthetic appearance during storage and after use.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Claims (10)

  1. Procédé de production d'une matière tabac comprenant les étapes suivantes :
    a) préparer une suspension mixte d'un résidu de matière de départ de tabac et d'un extrait de composant hydrosoluble en immergeant une matière de départ de tabac dans l'eau pour permettre au composant hydrosoluble de la matière de départ de tabac de se dissoudre dans l'eau ;
    b) mettre la suspension mixte en présence d'ozone à y dissoudre et mettre l'ozone dissous et les bulles d'ozone en contact avec la suspension mixte, dans lequel les bulles d'ozone formées par la mise en présence d'ozone ont un diamètre de 0,5 à 1000 µm.
  2. Procédé de production d'une matière tabac selon la revendication 1, dans lequel le point b) comprend le fait de mettre l'ozone dissous et les bulles d'ozone en contact avec la suspension mixte, tout en faisant circuler la suspension mixte.
  3. Procédé de production d'une matière tabac comprenant les étapes suivantes :
    a) immerger une matière de départ de tabac dans l'eau pour permettre au composant hydrosoluble de la matière de départ de tabac de se dissoudre dans l'eau ;
    b) séparer le résidu de matière de départ de tabac après extraction du composant hydrosoluble de l'extrait ;
    c) mélanger de nouveau avec de l'eau le résidu de matière de départ de tabac séparé pour préparer une suspension ; et
    d) mettre la suspension en présence d'ozone à y dissoudre et mettre l'ozone dissous et les bulles d'ozone en contact avec la suspension, dans lequel les bulles d'ozone formées par la mise en présence d'ozone ont un diamètre de 0,5 à 1000 µm.
  4. Procédé de production d'une matière tabac selon la revendication 3, dans lequel le point b) comprend le fait de mettre l'ozone dissous et les bulles d'ozone en contact avec la suspension, tout en faisant circuler la suspension.
  5. Procédé de production d'une matière tabac comprenant les étapes suivantes :
    a) immerger une matière de départ de tabac dans l'eau pour permettre au composant hydrosoluble de la matière de départ de tabac de se dissoudre dans l'eau ;
    b) séparer le résidu de matière de départ de tabac après l'extraction du composant hydrosoluble de l'extrait ;
    c) mettre l'extrait séparé en présence d'ozone à y dissoudre et mettre l'ozone dissous et les bulles d'ozone en contact avec l'extrait, dans lequel les bulles d'ozone formées par la mise en présence d'ozone ont un diamètre de 0,5 à 1000 µm ; et
    d) sécher le résidu de matière de départ de tabac et faire retourner l'extrait après le traitement à l'ozone au résidu de matière de départ de tabac au cours du processus de séchage.
  6. Procédé de production d'une matière tabac selon la revendication 5, comprenant en outre les étapes suivantes :
    mélanger de nouveau avec de l'eau le résidu de matière de départ de tabac séparé pour préparer une suspension ;
    mettre la suspension en présence d'ozone à y dissoudre et mettre l'ozone dissous et les bulles d'ozone en contact avec la suspension, dans lequel les bulles d'ozone formées par la mise en présence d'ozone ont un diamètre de 0,5 à 1000 µm ; et
    chauffer et sécher la suspension après le traitement à l'ozone et faire retourner l'extrait après le traitement à l'ozone au résidu de matière de départ de tabac au cours du processus de séchage.
  7. Procédé de production d'une matière tabac selon l'une quelconque des revendications 1 à 6, dans lequel l'apport d'ozone est réalisé en continu, de manière que l'ozone dissous dans un champ de réaction soit toujours présent.
  8. Matière tabac à usage oral qui est produit au moyen du procédé selon l'une quelconque des revendications 1 à 7.
  9. Produit de tabac à usage oral comprenant une matière tabac à usage oral qui possède une luminosité Hunter supérieure ou égale à 35 et qui est produite au moyen du procédé selon l'une quelconque des revendications 1 à 7.
  10. Produit de tabac à usage oral selon la revendication 9, dans lequel la matière tabac à usage oral est traitée avec un oxydant.
EP13769140.8A 2012-03-28 2013-03-27 Procédé de production d'une matière pour tabac, matière pour tabac à usage oral, et produit pour tabac à usage oral Active EP2832244B1 (fr)

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JP2012074878 2012-03-28
PCT/JP2013/059103 WO2013146926A1 (fr) 2012-03-28 2013-03-27 Procédé de production d'une matière pour tabac, matière pour tabac à usage oral, et produit pour tabac à usage oral

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DK (1) DK2832244T3 (fr)
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WO2015097783A1 (fr) * 2013-12-25 2015-07-02 日本たばこ産業株式会社 Procédé de production d'une substance de tabac pour applications orales et susbtance de tabac pour applications orales
CN110810884A (zh) * 2018-08-07 2020-02-21 中烟机械技术中心有限责任公司 烟草梗丝制备方法
US11712059B2 (en) * 2020-02-24 2023-08-01 Nicoventures Trading Limited Beaded tobacco material and related method of manufacture
CN111657539B (zh) * 2020-07-14 2022-06-14 上海烟草集团有限责任公司 一种烟草原料的脱色方法
WO2023089771A1 (fr) * 2021-11-19 2023-05-25 日本たばこ産業株式会社 Procédé d'analyse de distribution de nicotine dans une composition contenant de la nicotine

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US1757477A (en) 1927-07-11 1930-05-06 Rosenhoch Samuel Process and device for ozonizing tobacco
US7337782B2 (en) * 2004-08-18 2008-03-04 R.J. Reynolds Tobacco Company Process to remove protein and other biomolecules from tobacco extract or slurry
US7992575B2 (en) * 2005-02-28 2011-08-09 U.S. Smokeless Tobacco Company Use of chlorate, sulfur or ozone to reduce tobacco specific nitrosamines
WO2009015142A2 (fr) * 2007-07-23 2009-01-29 R.J.Reynolds Tobacco Company Composition de tabac sans fumée, et procédés pour traiter le tabac destiné à y être utilisé
JP2009082331A (ja) 2007-09-28 2009-04-23 Toshiba Corp 磁気共鳴イメージング装置
US8991403B2 (en) * 2009-06-02 2015-03-31 R.J. Reynolds Tobacco Company Thermal treatment process for tobacco materials
US8434496B2 (en) * 2009-06-02 2013-05-07 R. J. Reynolds Tobacco Company Thermal treatment process for tobacco materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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JPWO2013146926A1 (ja) 2015-12-14
JP5724034B2 (ja) 2015-05-27
WO2013146926A1 (fr) 2013-10-03
EP2832244A4 (fr) 2015-11-18
DK2832244T3 (da) 2019-07-15
TW201345443A (zh) 2013-11-16
EP2832244A1 (fr) 2015-02-04

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