CN100415125C - Method of manufacturing regenerated tobacco material - Google Patents
Method of manufacturing regenerated tobacco material Download PDFInfo
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- CN100415125C CN100415125C CNB2004800121138A CN200480012113A CN100415125C CN 100415125 C CN100415125 C CN 100415125C CN B2004800121138 A CNB2004800121138 A CN B2004800121138A CN 200480012113 A CN200480012113 A CN 200480012113A CN 100415125 C CN100415125 C CN 100415125C
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Abstract
A regenerated tobacco material is produced through extracting of natural tobacco material with an extractant solvent to thereby obtain an extract solution containing components of the natural tobacco material and an extraction residual. Regeneration tobacco web is prepared from the extraction residual. On the other hand, the extract solution is subjected to fractionation using ultrafiltration or reverse osmosis filtration, or fractionation using reverse phase partition chromatography so as to obtain a first fraction wherein desired components are enriched while undesired components are impoverished and a second fraction wherein desired components are impoverished while undesired components are enriched. An arbitrary amount of first fraction together with a reduced amount of second fraction is added to the regeneration tobacco web, thereby obtaining a regenerated tobacco material.
Description
Technical field
The present invention relates to the manufacture method of reclaimed tobacco material.
Background technology
In the tobacco-containing materials such as the leaf of natural baccy, pipe tobacco, middle bone, stem, root, contain various compositions such as nicotine, Nitrates, nitrosamines, hydro carbons, protein.From the natural baccy material, extract these compositions, as the suction flavor additive of tobacco.At this moment,, be hopeful to reduce or remove the composition of its amount, on the other hand, also be hopeful not remove or increase the composition of its amount from inhaling flavor or the consideration of other reasons.
For example,, in No. the 4th, 364,401, No. 929 and the United States Patent (USP), disclose with water system and extracted the solvent extraction tobacco-containing material, the water-based tobacco extract that obtains has been supplied with electrodialysis, separated the method for removing nitrate ion at United States Patent (USP) the 4th, 253.Can be added into as making each tobacco articles in the cellulosic tobacco-containing material that extracts residue by the extract that will remove behind this nitrate ion.
In U.S. Patent Publication US2002/0134394A1 (open WO 02/28209) corresponding to the world, disclose absorb nitrosamine such as active carbon with absorption adsorbent to handling with the extract that obtains behind the extraction solvent extraction tobacco-containing material, remove the method for nitrosamine.Can be added into by the extract that will remove this nitrosamine as making each tobacco articles in the cellulosic tobacco-containing material that extracts residue.
In No. 01/65954, the open WO in the world, disclose with the supercritical carbon dioxide treatment tobacco and extracted nitrosamine, again this extract is supplied with nitrosamine and remove operation.This nitrosamine is removed operation and is comprised the lock out operation that is undertaken by chromatography.Yet, be indefinite to chromatographic detailed mechanism, and to supply with chromatographic extract be not the water system extract.
Adopt above-mentioned electrodialytic separation to remove method, separation is removed object and is only limited to ion, no versatility.In addition, the voltage that applies during owing to electrodialysis makes extract rotten, perhaps heats the possibility height that makes extract rotten in order to improve separative efficiency.In addition, remove nitrate ion and organic principle in the dialysate that obtains, when using in certain purposes, dialysate must carry out concentration operation.In addition, in the separation method that uses adsorbent, must carry out concentration operation too.In addition, use the method for supercritical carbon dioxide, used device costliness.
Yet, the purpose of this invention is to provide a kind of from the extract that the natural baccy material obtains, adopt easier method, obtain desirable one-tenth separating/enriching and fraction and desirable composition that undesirable composition reduces reduce and the fraction of undesirable one-tenth separating/enriching, adopt one or both of these fractions again, make the method for reclaimed tobacco material.
Summary of the invention
According to the present invention, a kind of manufacture method of reclaimed tobacco material is provided, this method comprises: (a) with extracting solvent extraction natural baccy material, obtain containing the extract and the operation of extracting residue of above-mentioned natural baccy material composition, wherein, above-mentioned natural baccy material contains desirable composition and undesirable composition; (b) said extracted liquid is supplied with the progressive operation carried out with ultrafiltration or osmosis filtration method or with the progressive operation of reversed phase partition chromatography, obtain making above-mentioned desirable one-tenth separating/enriching and the above-mentioned undesirable operation that becomes the 2nd fraction of separating/enriching of the 1st fraction that above-mentioned undesirable composition reduces with making above-mentioned desirable composition minimizing; (c) use the said extracted residue, the operation of preparation reconstituted tobacco base-material (ウ エ Block); (d) above-mentioned the 2nd fraction that above-mentioned the 1st fraction is at random reduced with amount is added into the operation in the above-mentioned reconstituted tobacco base-material.
The simple declaration of accompanying drawing
Fig. 1 is used to illustrate the flow chart of making the method for reclaimed tobacco material by one embodiment of the invention.
Fig. 2 is used to illustrate the flow chart of making the method for reclaimed tobacco material by another embodiment of the invention.
The preferred plan that carries out an invention
The present invention is described in more detail below.
The present invention relates to use by extracting the extract and extraction residue that the natural baccy material obtains, make the method for reclaimed tobacco material.Adopt and extract residue manufacturing reconstituted tobacco base-material.
On the other hand, extract offers in the progressive operation of adopting ultrafiltration or osmosis filtration or reversed phase partition chromatography.The extract that obtains from the natural baccy material, from inhaling flavor or the consideration of other reasons, be hopeful to make it to measure the composition (not wishing composition) that reduces or remove, and the composition (wishing composition) of wishing not remove or make its amount increase.By progressive operation of the present invention, can obtain desired one-tenth separating/enriching and the 1st fraction and desirable composition that undesirable composition reduces reduce and the 2nd fraction of undesirable one-tenth separating/enriching.The 2nd fraction that above-mentioned the 1st fraction is at random reduced with amount is added in the above-mentioned reconstituted tobacco base-material makes desirable reclaimed tobacco material.
Fig. 1 is used to illustrate the flow chart of making the method for reclaimed tobacco material by one embodiment of the invention.In this embodiment, the progressive operation of extract adopts milipore filter or osmosis filtration film to carry out.
As shown in Figure 1, at first, natural baccy material 11 is offered extract treatment S 1 by mixing, stir natural baccy material 11 and extractant 12.
As natural baccy material 11, can use leaf, silk, middle bone, stem, root and these the mixture of tobacco.As extracting solvent, can make water, organic solvent etc.Water etc. extract solvent, both can be that alkalescence also can be acid.As extracting solvent, also can make the mixture of water and water Combination organic solvent.As organic solvent, can enumerate hydrocarbon solvents such as ethers such as alcohols, diethyl ether, cyclohexane such as ethanol etc.Can also in these organic solvents, dissolve inorganic salts such as NaOH and used.Extract treatment S 1, usually under 0～100 ℃ temperature, carried out 5 minutes～6 hours.
After extracting treatment S 1 and finishing, the extraction mixture that obtains offered by for example filtering wait the lock out operation S2 that carries out, be separated into extract 13 and extraction residue 14.
In the natural baccy material, contain slaines such as potassium, nitrate, nicotine, carbohydrate, amino acids, glucoside, amino-sugar compounds class, protein, hydro carbons (saturated hydrocarbons, unsaturated hydro carbons, arene), alcohols, ethers, aldehydes, ketone, the ester class, lactone, quinones, acids (comprising acid anhydrides), phenols, amine, pyroles, pyridines, the pyrazine class, alkaloids, polycycle nitrogen-containing compound class, nitrosamine nitroso compound classes such as (comprising the intrinsic nitrosamine of tobacco (TSNA)), amide-type, lipid, halide, sulfur-containing compound, inorganic elements etc.Handling in the extract 13 that obtains,, can contain nearly all composition of these compositions though depend on used extraction solvent types by said extracted.In these compositions, any be wish composition, any be not wish composition, though different because of the suction flavor of the reclaimed tobacco material wanting to make etc., nicotine is desirable composition at least, and nitrosamines such as nitrate, TSNAS and other amines are undesirable composition.
Extract residue 14 for extracting the insoluble composition of solvent, come down to constitute by fiber.Use this extraction residue 14, make the reconstituted tobacco base-material with common method.This reconstituted tobacco base-material can be that its part constitutes by extracting residue 14, also can be that it all constitutes by extracting residue 14.For example, can will contain the paper pulp material that extracts residue 14, copy paper with common machine hand's preface S3 and make reconstituted tobacco base-material 15.
On the other hand, from the extract 13 that lock out operation S2 obtains, delivery film lock out operation S4.Film lock out operation S4 is undertaken by ultrafiltration or osmosis filtration.The film (milipore filter, osmosis filtration film) that uses in these films separate is the perforated membrane with hole of certain certain following size, mainly with the difference of solute molecule size solute is separated classification by the size in hole.The classification molecular weight that the molecular weight that can not see through the minimum solute of film is called film.The classification molecular weight ranges of general milipore filter is 1,000～1,000,000, and the classification molecular weight ranges of osmosis filtration film is 100～1,000 scope.These films can be buied from market.For example, as milipore filter, can use バ イ オ マ Star Network ス (Biomax) 5 (classification molecular weight 5,000) that ミ リ Port ア (Milipore) society makes and PCXK cellulose (classification molecular weight 1,000,000) etc.In addition, as the osmosis filtration film, can use Na ノ マ Star Network ス (Nanomax) 95 (classification molecular weight about 100) that ミ リ Port ア (Milipore) society makes and Na ノ マ Star Network ス 50 (classification molecular weight about 400) etc.Adopt the film of ultrafiltration and osmosis filtration to separate, can be undertaken by itself known method.When carrying out these films separation, because extract 13 may reside in 0 ℃～30 ℃ low temperature, so needn't worry that the composition in the extract 13 is rotten.Also have, osmosis filtration film (reverse osmosis membrane) can effectively separate hydrated ions such as nitrate ion.
By this film lock out operation S4, natural baccy material composition with molecular weight bigger than the classification molecular weight of used film, do not see through thing fraction 16 and obtain as film, and have a natural baccy material composition of the molecular weight littler than the classification molecular weight of used film, see through thing fraction 17 and obtain as film.In other words, film does not see through thing fraction 16, see through thing fraction 17 with film and compare, the natural baccy material composition with molecular weight bigger than the classification molecular weight of used film is by enrichment, and the natural baccy material composition with molecular weight littler than the classification molecular weight of used film reduces.On the other hand, film sees through thing fraction 17 and does not compare through thing fraction 16 with film, natural baccy material composition with molecular weight littler than the classification molecular weight of used film is by enrichment, and the natural baccy material composition with molecular weight bigger than the classification molecular weight of used film reduces.Therefore, enrichment, minimizing are the relative concentration/amounts for the natural baccy material composition.
Film does not see through thing fraction 16 and/or film and sees through thing fraction 17, can supply with further processing (not shown).When this is further handled, comprising: carry out at least 1 time with above-mentioned same film lock out operation, component separation, the concentration of usefulness gas chromatography have used that the composition of adsorbent is removed etc.
Film does not see through the thing fraction and/or film sees through thing fraction (the further handled thing that comprises them), if undesirable composition then can discard, if the composition of wishing then can be directly to be inhaled flavor and mix (S5) with other compositions in order to regulate.Like this, when film does not see through thing fraction and/or film and sees through the thing fraction and mix, reduce wherein a kind of amount at least.
Add (S6) to reconstituted tobacco base-material 15 by tobacco odor absorber, obtain reclaimed tobacco material 18 preparation like this.The reclaimed tobacco material 18 that obtains so not only contains the composition from the natural baccy material, and presents the suction flavor different with the natural baccy material.Also have, when adopting different a plurality of milipore filters of classification molecular weight or reverse osmosis to cross filter membrane to carry out repeatedly above-mentioned film lock out operation, the film that obtains can not be seen through thing fraction and film and see through being added into more than 1 or 1 in the above-mentioned reconstituted tobacco base-material of thing fraction.But, when will this moment the film that obtain do not see through that thing fraction and film see through the thing fraction whole when being added in the above-mentioned reconstituted tobacco base-material, reduce these films that obtain and do not see through thing fraction and film and see through the amount of at least 1 fraction in the thing fraction and be added in the above-mentioned reconstituted tobacco base-material.
For example,, when wanting to make nitrate in the natural baccy material to reduce, water is extracted the aqueous extract of natural baccy material, supply with the film lock out operation of the osmosis filtration film that adopts classification molecular weight about 400 as the 1st example.Thus, can obtain molecular weight and surpass 400 composition (in other words by enrichment, the molecular weight that contains inorganic ions such as nitrate ion, potassium is that the composition below 400 or 400 reduces) film do not see through the thing fraction, surpass film that 400 composition is reduced (molecular weight that in other words, contains inorganic ions such as nitrate ion, potassium is the one-tenth separating/enriching 400 or 400 below) through the thing fraction with molecular weight.The film that nitrate ion reduces do not see through the thing fraction can be separately or be added in the reclaimed tobacco material that has used the said extracted residue after a spot of film mixes through the thing fraction.The cigarette of adopting this reclaimed tobacco material to make is compared with the cigarette of adopting the natural baccy material to make, and can significantly reduce the NO in the mainstream smoke
X, burning velocity also can reduce.
In addition, as the 2nd example, when water extracts the film separation of natural baccy material extraction liquid, when using the osmosis filtration film of classification molecular weight about 100, the molecular weight that can obtain containing nicotine surpass 100 composition by the film of enrichment do not see through thing fraction and molecular weight be composition 100 or 100 below by the film of enrichment through the thing fraction.Employing does not see through the thing fraction to this film and is added into the cigarette that the reclaimed tobacco material in the above-mentioned reconstituted tobacco base-material is made, and has kept tobacco smoke (ら さ), or the tobacco smoke strengthens relatively, and, because nitrate ion also reduces, so the NO in the mainstream smoke
XAlso descend.In addition, do not seen through in the thing fraction by the film of enrichment, because might contain nitrosamine such as TSNA, so before in being added into the reconstituted tobacco base-material, it is preferred that this film is not supplied to the further processing of removing nitrosamine through the thing fraction at this nicotine.As this further processing, comprise with gas chromatography and separate, remove with the absorption of nitrosamine sorbing material.Removing of this nitrosamine, the film that also can be used for above-mentioned the 1st example sees through the thing fraction.
As the 3rd example, can enumerate the example that extract is carried out classification with 2 kinds of films.Promptly, water is extracted the extract that the natural baccy material obtains, supply to the film lock out operation of the osmosis filtration film that adopts classification molecular weight 100, as the 2nd example, the film that can obtain the nitrate ion minimizing does not see through the film of thing fraction (as fraction A) and nitrate ion enrichment through the thing fraction.Secondly, the film lock out operation fraction A supplies with the milipore filter that adopts classification molecular weight about 5000 obtains film and does not see through thing fraction (as fraction B) and film through thing fraction (as fraction C).Fraction B, protein is by enrichment; Fraction C, carbohydrates such as sucrose are by enrichment.Therefore,, fraction C is mixed with a small amount of fraction A and/or fraction B and be added in the above-mentioned reconstituted tobacco base-material, prepare reclaimed tobacco material,, then can be emphasized the cigarette of sweet taste relatively if use it to make cigarette according to occasion.
Fig. 2 is the method for reclaimed tobacco material is made in explanation by another embodiment of the invention a flow chart.In Fig. 2, same symbol is used in key element, the operation same with Fig. 1.
In the scheme of Fig. 2, the progressive operation of extract is undertaken by reversed phase partition chromatography.Progressive operation by the extract that undertaken by this reversed phase partition chromatography can effectively separate nicotine and TSNA.
Present inventors notice, are extracting from the natural baccy material in the extract that obtains with water system extraction solvent, and the short-cut method as separating nicotine and TSNA is conceived to gas chromatography.As gas chromatography, it is after filling the packing material of the pore size with regulation, to make elutriant flow through chromatographic column, utilizes and depends on that the elution speed of bulk of molecule and shape is poor, separates granularity (the サ イ ズ) gas chromatography of desired composition.Yet, adopt the granularity gas chromatography, because the proterties of nicotine and TSNA is approaching, so they are difficult to separate.In addition, adopt the ion-exchange gas chromatography or along distributing gas chromatography mutually, in order to separate nicotine and the TSNA that adsorbs on the packing material, the salinity of elutriant must be adjusted pH, when only adopting the water system extract, nicotine can not separate with TSNA.
Therefore, further result of study when adopting reversed phase partition chromatography, can effectively be separated nicotine and TSNA by the water system elutriant as can be known.
In addition, in Fig. 2,, from natural baccy material 11,, can obtain extract 13 and extract residue 14 by having used the extraction treatment S 1 of extracting solvent 12 as the explanation among Fig. 1.Reconstituted tobacco base-material 15, described as the explanation among Fig. 1, can make by having used the paper S3 that copies that extracts residue 14.
From the extract 13 that lock out operation S2 obtains, supply with lock out operation S21 by reversed phase partition chromatography.This lock out operation S21 can use (methyl) acrylic resin, vinyl-based resin or silicones (シ リ カ Class Trees fat) to carry out mutually as the fixing of matrix material.Matrix material preferably has hydrophobic group, and the preferred carbon number of hydrophobic group is the alkyl below 6 or 6.Carbon number is that the alkyl below 6 or 6 is hydrophobic, but because the low reasons such as (hydrophily are high relatively) of its hydrophobicity if use the fixedly phase that comprises the matrix material with such hydrophobic group, then can be separated nicotine and TSNA more effectively.Carbon number is that the alkyl below 6 or 6 comprises methyl, ethyl, propyl group, butyl, amyl group, hexyl, phenyl.Hydrophobic group both can be used as that the modified matrix material imports, and for example, as the methyl of the metering system acid moieties that constitutes the polymethacrylic acid resin, also can be that matrix material had originally.Reversed phase partition chromatography stationary phase material with this hydrophobic group is granular form, can buy from market.
Reversed phase partition chromatography, can in the post of having filled the said fixing phase, inject tobacco extract after, use the water system eluent to carry out classification and carry out.As the water system eluent, can make water, or the mixture of water and water Combination organic solvent (for example, ethanol).Reversed phase partition chromatography can be carried out being lower than the temperature of solvent boiling point (for example, 10 ℃～90 ℃).From the fraction that the chromatographic column by this reversed phase partition chromatography flows out, recovery (for example contains obvious amount, be initial more than at least 30% or 30% of nicotine content) nicotine and the fraction 21 (containing the fraction that nicotine is removed TSNA) of having removed TSNA in fact be recovered the discarded fraction (TSNA fraction) 22 that contains the TSNA of obvious amount.As adopt the reversed phase partition chromatography of using among the present invention, and compare with above-mentioned natural baccy material, can obtain the fraction of nitrosamine to the ratio minimizing of nicotine.Particularly, compare, can obtain the slip about 90% of TSNA or about more than 90%, and the nicotine slip is lower than 60% fraction with the extract before the classification according to the present invention.When use has when comprising carbon number and being the stationary phase material of hydrophobic group of the alkyl below 6 or 6, can obtain more than the slip about 90% or 90% of TSNA, and the slip of nicotine is lower than 35% fraction.
The fraction 21 that will contain nicotine and remove TSNA is concentrated or is not concentrated, and part or all is added into (S22) in the reconstituted tobacco base-material 15 with it, thus, can obtain reclaimed tobacco material 23.The reclaimed tobacco material 23 that obtains like this contains nicotine but does not contain TSNA in fact.
Describe the present invention by various schemes above, but the present invention is not subjected to the qualification of these schemes again.Self-evident, can make up such scheme.
For example, the film that obtains according to the 1st scheme can be seen through thing fraction or film and not see through the thing fraction, supply in the progressive operation of employing reversed phase partition chromatography of the 2nd scheme.Particularly, will obtain according to the 1st scheme, nicotine and TSNA see through the thing fraction by the film of enrichment and supply in the reversed phase partition chromatography of the 2nd scheme, this film can be seen through that the thing fraction is separated into TSNA fraction and nicotine enrichment and fraction that TSNA is removed.
Below by embodiment the present invention is described, but the present invention is not limited by it again.
In addition, in following embodiment, comparative example, the NOx amount in the mainstream smoke, aromatic amine amount and TSNA amount are measured according to Canadian method No.T-110, T-102 and T-111 respectively;
Nicotine content in the mainstream smoke is measured according to ISO 103 15;
Nicotine content in the pipe tobacco is measured according to the DIN of DIN mechanism 10373;
NO in the pipe tobacco
3Amount is after the extraction of pipe tobacco water, with the NO in the extract
3Be reduced into nitrous acid with the hydrazine reducing process, carry out colorimetric assay by the diazotising method and measure (compiling health test method(s), p707, p836 with reference to Japanese medicine association);
Albumen quality in the pipe tobacco, measure (with reference to Balasubramaniam D et al. " Tobacco Protein Separation by aqueous two-phaseextraction " according to the method for Balasubramaniam etc., Journal of Chromatography A 989,119-129,2003).
In addition, carbohydrate, use Agilent 1100 LC Chromatograph as liquid chromatography, (4.6 * 250mm) as chromatographic column to use Waters High Performance Carbohydrate Column 60A 4 μ m, column temperature is set at 35 ℃, the sample injection rate is 8.0 μ L, uses acetonitrile: Purified Water=3: 1 is analyzed as mobile phase.
25 ℃ temperature,, carry out pipe tobacco and extract by the 200g pipe tobacco is mixed stirring with 875mL water.The extraction mixture that obtains is filtered, be divided into extract and extract residue.Copy paper with the extraction residue, obtain the reconstituted tobacco base-material.In addition, its weight is 100g when dry, is about half weight of former pipe tobacco.
On the other hand, in extract, add 211mL water, supply with the film lock out operation of the osmosis filtration film (the Na ノ マ Star Network ス 95 that ミ リ Port ア society makes) that adopts classification molecular weight 100, obtain film and do not see through thing fraction (246mL) and film through thing fraction (840mL).The film that obtains does not see through thing fraction and film and analyzes with the amount of sugar (fructose and glucose) through the nitric acid of thing fraction, obtains the result shown in the following table 1.Analysis result to extract also is shown in table 1.
Table 1
By the result shown in the table 1 as can be known, film do not see through the thing fraction sugar by enrichment and nitric acid reduces.On the other hand, film nitric acid enrichment through the sugar minimizing (be 0 this moment) of thing fraction.
In addition, film is not seen through thing fraction full dose (246mL) be added among the above-mentioned reconstituted tobacco base-material 100g, use the reclaimed tobacco material that obtains to make cigarette.
In addition, different therewith, fully similarly extract operation with last method, extract residue from it and similarly make the reconstituted tobacco base-material.In addition, extract is not carried out the film lock out operation, only carry out heating in vacuum and concentrate, its full dose is added in the reconstituted tobacco base-material, make cigarette with the reclaimed tobacco material that obtains.
According to the ISO method to these cigarettes with 1 the 2 seconds smoking time (1 smoking capacity 35mL), carry out smoking with Bel's type smoking section bar (プ ロ Off ア イ Le), measure the NOx amount in the mainstream smoke, the NOx amount of the unit's of calculating tar.Variously the results are shown in following table 2.
Table 2
Result as shown in table 2 does not see through the thing fraction by the film that nitric acid is reduced and is added in the reconstituted tobacco base-material as can be known, and the NOx amount in the cigarette mainstream smoke and the NOx amount of unit tar are reduced.
Embodiment 2
To with embodiment 1 in the used different pipe tobacco of pipe tobacco, the extraction of carrying out is similarly to Example 1 handled, and obtains extract and extracts residue.Copy paper with this extraction residue, obtain the reconstituted tobacco base-material.
On the other hand, (day Dong Diangongshe makes, and film lock out operation NTR-729HG) does not see through the thing fraction to the film that obtains and is added in the above-mentioned reconstituted tobacco base-material, obtains reclaimed tobacco material, and it is cut into pipe tobacco extract to be supplied with the employing reverse osmosis membrane.
In addition, fully similarly extract operation, the extraction residue that obtains is copied paper, obtain the reconstituted tobacco base-material with last method.In addition, the extract that obtains is carried out heating in vacuum concentrate, its full dose is added in this reconstituted tobacco base-material, obtain reclaimed tobacco material, it is cut into pipe tobacco.
Measure the NO in the pipe tobacco that obtains like this
3Amount and nicotine content.The results are shown in table 3.
Table 3
| Pipe tobacco | NO in the pipe tobacco 3Amount (mg/g) | Nicotine content in the pipe tobacco (mg/g) |
| Add extract | 6.17 | 7.5 |
| Add film and do not see through the thing fraction | 0.3 | 6.6 |
Result as shown in table 3 as can be known, by not seen through the thing fraction, film is not added into the reclaimed tobacco material pipe tobacco that obtains in the reconstituted tobacco base-material, compare with the reclaimed tobacco material pipe tobacco that has added the extract that does not carry out the film processing, not only the minimizing of nicotine content is suppressed, and the NO in the pipe tobacco
3Amount reduces about 95%.
Adopt above-mentioned each pipe tobacco to make cigarette, measure NO in the mainstream smoke similarly to Example 1
XAmount and nicotine content.The results are shown in table 4.
Table 4
Result as shown in table 4 adopts and has added the cigarette that film is not made through the pipe tobacco of thing fraction as can be known, compares with the cigarette that the pipe tobacco that adds the extract that does not carry out the film processing is made, though nicotine content is not inferior, and NO
3Amount significantly reduces.
Embodiment 3
To with embodiment 1 in the used different pipe tobacco of pipe tobacco, the extraction of carrying out is similarly to Example 1 handled, and obtains extract and extracts residue.To extract residue and copy paper, obtain the reconstituted tobacco base-material.
On the other hand, extract is supplied with the membrane molecule operation of adopting milipore filter (day Dong Diangongshe makes, CF30-F4-PT, classification molecular weight 50,000), the film that obtains is seen through the thing fraction resupply employing reverse osmosis membrane (day Dong Diangongshe manufacturing, film lock out operation NTR-729HG).The film that obtains is not seen through the thing fraction be added in the above-mentioned reconstituted tobacco base-material, obtain reclaimed tobacco material, it is cut into pipe tobacco.
In addition, fully similarly extract operation, and the extraction residue that will obtain copies paper, obtain the reconstituted tobacco base-material with last method.In addition, the extract that obtains is carried out heating in vacuum concentrate, its full dose is added in the reconstituted tobacco base-material, obtain reclaimed tobacco material, it is cut into pipe tobacco.
Measure the NO in the pipe tobacco that obtains like this
3Amount, nicotine content and albumen quality.The results are shown in table 5.
Table 5
| Pipe tobacco | NO in the pipe tobacco 3Amount (mg/g) | Nicotine content in the pipe tobacco (mg/g) | Albumen quality in the pipe tobacco (mg/g) |
| Add the pipe tobacco of extract | 6.17 | 7.5 | 16 |
| Add the pipe tobacco that film does not see through the thing fraction | 0.22 | 7.5 | 0 |
From result shown in the table 5 as can be known, by supplying with the osmosis filtration film through the thing fraction that sees through of milipore filter, the film that obtains not being seen through the thing fraction is added in the reconstituted tobacco base-material and obtains regenerated cut tobacco again, compare with the regenerated cut tobacco that has added the extract that does not carry out the film processing, not only the minimizing of nicotine content is suppressed, and NO in the pipe tobacco
3It is about 95% that amount reduces, and protein also almost all reduces.
Adopt above-mentioned each pipe tobacco to make cigarette, measure the NO in the mainstream smoke similarly to Example 1
3Amount and nicotine content.The results are shown in table 6.
Table 6
From result shown in the table 6 as can be known, by will not being added in the reconstituted tobacco base-material through the film that obtains through thing fraction supply osmosis filtration film of milipore filter through the thing fraction, obtain regenerated cut tobacco, cigarette (cigarette of the present invention) with this pipe tobacco making, compare with the cigarette that the pipe tobacco that adds the extract that does not carry out the film processing is made, though nicotine content is not inferior, NO in the pipe tobacco
3Amount significantly reduces.
In addition, when estimating, obtain the common evaluation of the stink reduction of cigarette of the present invention with one group of 10 people.
Embodiment 4
To with embodiment 1 in the used different pipe tobacco of pipe tobacco, the extraction of carrying out is similarly to Example 1 handled, and obtains extract and extracts residue.To extract residue and copy paper, obtain the reconstituted tobacco base-material.
In addition, extract is supplied with employing milipore filter (the バ イ オ マ Star Network ス 10 that ミ リ Port ア society makes, classification molecular weight 10,000) membrane molecule operation, the film that obtains is seen through the thing fraction resupply the film lock out operation that adopts reverse osmosis membrane (the Na ノ マ Star Network ス 95 that ミ リ Port ア society makes, classification molecular weight about 100).The film that obtains is not seen through the thing fraction be added in the above-mentioned reconstituted tobacco base-material, obtain reclaimed tobacco material, be cut to pipe tobacco, make cigarette with it.
In addition, adopt with the same fully method of said method and extract operation, and the extraction residue that will obtain copies paper, obtain the reconstituted tobacco base-material.Extract is carried out heating in vacuum concentrate, its full dose is added in this reconstituted tobacco base-material, obtain reclaimed tobacco material, be cut to pipe tobacco, make cigarette with it.
Aromatic amine amount in the mainstream smoke of the cigarette that mensuration obtains like this.The results are shown in table 7.
Table 7:
From result shown in the table 7 as can be known, by will not being added in the reconstituted tobacco base-material through the film that obtains through thing fraction supply osmosis filtration film of milipore filter through the thing fraction, obtain regenerated cut tobacco, cigarette (cigarette of the present invention) with this pipe tobacco making, compare with the cigarette that the regenerated cut tobacco that adds the extract that does not carry out the film processing is made, the aromatic amine in the mainstream smoke significantly reduces.
Embodiment 5
Under 25 ℃ of temperature,, carry out the extraction of pipe tobacco by mixing, stir with water 1000mL by tobacco leaf silk (yellow is planted the mixture with uncle's Lay cigarette kind) and the pipe tobacco 100g of middle bone silk with 1: 1 mixture of weight ratio formation.The extraction mixture that obtains is filtered, tell extract and extract residue.To extract residue and copy paper, obtain the reconstituted tobacco base-material.
In addition, with film lock out operation concentrated extracting solution, its 1mL is injected in the chromatographic column (diameter 8mm, long 300mm) of the polymethacrylic acid resin (Mitsubishi Chemical society makes, trade name HP2MG) of having filled particle diameter 200～600 μ m.To flow to chromatographic column as the water of eluent, at first classification 70mL (fraction 1), classification 8030mL (fraction 2) again.Analyze the nicotine that contains in the extract (extract is untreated) and each fraction before the classification and nitrosamine (N '-nitrosonornicotine) (NNN), the amount of 4-(methyl nitroso amino)-1-(3-pyridine radicals)-1-butanone (NNK) and N '-nitroso nicoteine (NAT).The results are shown in following table 8.Nicotine slip and TSNA slip also are shown in the table 8.
Table 8:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 1 | 2.81 | - | 0.94 | 0.04 | 0.04 | 1.02 | - |
| |
70 | 2.73 | 3％ | 0.11 | 0.00 | 0.00 | 0.11 | 89％ |
| Fraction 2 | 8030 | 0.08 | 97％ | 0.83 | 0.04 | 0.04 | 0.91 | 11％ |
As shown in table 8, the TSNA of fraction 1 has reduced about 89% than primary quantity, and NNK among the TSNA and NTA are removed fully, and nicotine only reduces 3% than primary quantity.
Therefore, discarded fraction 2, and by fraction 1 being added in the above-mentioned reconstituted tobacco base-material preparation reclaimed tobacco material.
Embodiment 6
Except that the mixing ratio that changes yellow kind and uncle's Lay cigarette kind, similarly to Example 5, preparation concentrates tobacco extract and reconstituted tobacco base-material.Concentrating in the chromatographic column (diameter 10mm, long 250mm) that tobacco extract 1mL is injected into the phenyl modified polyvinyl resin of having filled particle diameter 50～150 μ m (eastern ソ one society make trade name TOYOPEARLPhenyl 650C).To flow to chromatographic column as the water of eluent, at first classification 28mL (fraction 1), then classification 115mL (fraction 2).The nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and N '-nitroso anabasine (NAB).The results are shown in following table 9.Also show nicotine slip and TSNA slip in the table 9.
Table 9:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 1 | 3.51 | - | 0.80 | 0.20 | 0.21 | 0.21 | 1.42 | - |
| |
28 | 2.51 | 0％ | 0.13 | 0.00 | 0.00 | 0.00 | 0.13 | 91％ |
| Fraction 2 | 115 | 0.00 | 100％ | 0.68 | 0.20 | 0.21 | 0.21 | 1.30 | 9％ |
As shown in table 9, the TSNA of fraction 1 reduces about 91% than primary quantity, and the NNK among the TSNA, NAT and NAB are removed fully, and nicotine fully reduces.
Therefore, discarded fraction 2, and by fraction 1 being added in the above-mentioned reconstituted tobacco base-material preparation reclaimed tobacco material.
Embodiment 7
Except that the mixing ratio that changes yellow kind and uncle's Lay cigarette kind, similarly to Example 1, preparation concentrates tobacco extract and reconstituted tobacco base-material.Concentrating the chromatographic column (diameter 6mm, long 150mm) that tobacco extract 0.02mL is injected into the butyl modified silicone resin (YMC society makes, trade name Pack C4) of having filled average grain diameter 15 μ m.To flow to chromatographic column as the water of eluent, at first classification 600mL (fraction 1), classification 400mL (fraction 2) again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 10.Also show nicotine slip and TSNA slip in the table 10.
Table 10:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 0.02 | 2.16 | - | 2.29 | 0.56 | 1.47 | 1.47 | 5.79 | - |
| |
600 | 0.72 | 67％ | 2.29 | 0.56 | 1.47 | 1.47 | 5.79 | 0％ |
| Fraction 2 | 400 | 1.44 | 33％ | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100％ |
As shown in table 10, the TSNA of fraction 2 reduces 100%, and nicotine only reduces 33% than primary quantity.
Therefore, discarded fraction 1, and by fraction 2 being added in the above-mentioned reconstituted tobacco base-material preparation reclaimed tobacco material.
In addition, the result who obtains from embodiment 5～7 as can be known, when employing has when containing carbon number and being the stationary phase material of hydrophobic group of the alkyl below 6 or 6, can obtain the TSNA slip is more than about 90% or 90%, and the nicotine slip is lower than 35% fraction.
Embodiment 8
Except that the mixing ratio that changes yellow kind and uncle's Lay cigarette kind, similarly to Example 5, preparation concentrates tobacco extract and reconstituted tobacco base-material.Concentrating the chromatographic column (diameter 4.6mm, long 150mm) that tobacco extract 0.02mL is injected into the octyl group modified silicone resin (Aligent society makes, trade name XDB-C8) of having filled average grain diameter 5 μ m.To flow to chromatographic column as the water of eluent, at first classification 200mL (fraction 1), classification 200mL (fraction 2), classification 400mL (fraction 3) at last again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 11.Also show nicotine slip and TSNA slip in the table 11.
Table 11:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 0.02 | 1.64 | - | 2.22 | 0.77 | 2.49 | 0.04 | 5.52 | - |
| |
200 | 0.00 | 100％ | 1.83 | 0.00 | 0.00 | 0.00 | 1.83 | 67％ |
| Fraction 2 | 200 | 0.92 | 44％ | 0.39 | 0.77 | 2.49 | 0.04 | 3.69 | 33％ |
| Fraction 3 | 400 | 0.72 | 56％ | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100％ |
As shown in table 4, the TSNA of fraction 3 removes fully, and the nicotine slip is 56%.
Therefore, discarded fraction 1 and fraction 2, and by fraction 3 being added in the above-mentioned reconstituted tobacco base-material preparation reclaimed tobacco material.
Embodiment 9
Except that the mixing ratio that changes yellow kind and uncle's Lay cigarette kind, similarly to Example 1, preparation concentrates tobacco extract and reconstituted tobacco base-material.Concentrated tobacco extract 0.02mL is injected in the chromatographic column (diameter 6mm, long 150mm) of the octadecyl modified silicone resin (YMC society makes, trade name ODS-AP) of having filled average grain diameter 15 μ m.To flow to chromatographic column as the water of eluent, at first classification 400mL (fraction 1), classification 200mL (fraction 2), classification 200mL (fraction 3) at last again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 12.Also show nicotine slip and TSNA slip in the table 12.
Table 12:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 0.02 | 2.17 | - | 2.33 | 0.57 | 2.28 | 0.03 | 5.21 | - |
| |
400 | 0.37 | 83％ | 2.33 | 0.00 | 0.00 | 0.00 | 2.33 | 55％ |
| Fraction 2 | 200 | 1.03 | 53％ | 0.00 | 0.57 | 2.28 | 0.03 | 2.88 | 45％ |
| Fraction 3 | 200 | 0.76 | 65％ | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100％ |
As shown in table 12, the TSNA of fraction 3 removes fully, and the slip of nicotine is 65%.
Therefore, discarded fraction 1 and fraction 2, and by fraction 3 being added in the above-mentioned reconstituted tobacco base-material preparation reclaimed tobacco material.
Comparative example 1
Except that changing yellow mixing ratio of planting with uncle's Lay cigarette kind, similarly to Example 5, the concentrated tobacco extract 1mL for preparing be injected into filled average grain diameter 300 μ m the polystyrene type cationic ion-exchange resin (to ion Na
+, オ Le ガ ノ society makes, trade name CR-1310) chromatographic column (diameter 10mm, long 250mm).To flow to chromatographic column as the water of eluent, at first classification 100mL (fraction 1), classification 900mL (fraction 2) again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 13.Also show nicotine slip and TSNA slip in the table 13.
Table 13:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 1 | 3.09 | - | 1.04 | 0.43 | 0.33 | 0.02 | 1.82 | - |
| |
100 | 0.00 | 100％ | 0.00 | 0.00 | 0.00 | 0.02 | 0.02 | 99％ |
| Fraction 2 | 900 | 0.00 | 100％ | 0.00 | 0.43 | 0.00 | 0.00 | 0.43 | 76％ |
As shown in Table 13, any TSNA of fraction 1 and fraction 2 all obviously removes, and nicotine is removed fully.Therefore, adopt any reclaimed tobacco material that all can not get containing nicotine of fraction 1 and fraction 2.
Comparative example 2
Except that changing yellow mixing ratio of planting with uncle's Lay cigarette kind, similarly to Example 1, the concentrated tobacco extract 0.22mL for preparing be injected into filled average grain diameter 7 μ m polystyrene type anion exchange resin (to ion CH
3COO
-, Mitsubishi Chemical society makes, trade name CDR10) chromatographic column (diameter 4.6mm, long 250mm) in.To flow to chromatographic column as the water of eluent, at first classification 500mL (fraction 1), classification 950mL (fraction 2) again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 14.Also show nicotine slip and TSNA slip in the table 14.
Table 14:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | NAB (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 0.22 | 0.78 | - | 0.53 | 0.22 | 1.21 | 0.07 | 2.03 | - |
| |
50 | 0.78 | 0％ | 0.20 | 0.00 | 0.29 | 0.04 | 0.53 | 74％ |
| Fraction 2 | 950 | 0.00 | 100％ | 0.33 | 0.22 | 0.92 | 0.03 | 1.50 | 26％ |
As shown in table 14, the TSNA of fraction 1 obviously removes, and nicotine is removed fully, and in addition, the nicotine of fraction 2 is kept 100% of primary quantity, and the TSNA slip only is 26%.Therefore, adopt any of fraction 1 and fraction 2, all can not get containing the nicotine of obvious amount, do not contain the reclaimed tobacco material of TSNA simultaneously in fact.
Comparative example 3
Except that the mixing ratio that changes yellow kind and uncle's Lay cigarette kind, similarly to Example 5, the concentrated tobacco extract 0.5mL of preparation be injected into filled average grain diameter 40～60 μ m (ダ イ ソ society makes with silicones along distributing gas chromatography mutually, trade name Daisoge 12000) chromatographic column (diameter 7.5mm, long 50mm) in.To flow to chromatographic column as the water of eluent, at first classification 10mL (fraction 1), classification 10mL (fraction 2), classification 10mL (fraction 3), classification 10mL (fraction 4), classification 110mL at last more then again.Nicotine that contains in extract (extract is untreated) and each fraction before the analysis classification and the amount of NNN, NNK, NAT and NAB.The results are shown in following table 15.Also show nicotine slip and TSNA slip in the table 15.
Table 15:
| Liquid measure (mL) | Nicotine (mg) | The nicotine slip | NNN (μg) | NNK (μg) | NAT (μg) | TSNA total amount (μ g) | The TSNA slip | |
| Extract is untreated | 0.5 | 1.05 | - | 0.89 | 0.02 | 0.15 | 1.06 | - |
| |
10 | 0.12 | 89％ | 0.25 | 0.00 | 0.02 | 0.27 | 75％ |
| Fraction 2 | 10 | 0.31 | 72％ | 0.39 | 0.22 | 0.05 | 0.66 | 38％ |
| Fraction 3 | 10 | 0.19 | 82％ | 0.17 | 0.00 | 0.06 | 0.23 | 78％ |
| Fraction 4 | 10 | 0.09 | 91％ | 0.08 | 0.00 | 0.02 | 0.02 | 98％ |
| Fraction 5 | 110 | 0.35 | 67％ | 0.00 | 0.00 | 0.00 | 0.00 | 100 |
As shown in Table 15, though any TSNA of fraction 1～fraction 5 obviously is removed, and the nicotine slip reaches more than about 70% or 70%.Therefore, adopt any of fraction 1～fraction 5, all can not get containing the nicotine of obvious amount, do not contain the reclaimed tobacco material of TSNA simultaneously in fact.
Claims (10)
1. the manufacture method of a reclaimed tobacco material, wherein comprise: (a) with extracting solvent extraction natural baccy material, obtain containing the extract and the operation of extracting residue of above-mentioned natural baccy material composition, wherein, above-mentioned natural baccy material contains desirable composition and undesirable composition; (b) said extracted liquid is supplied with the progressive operation carried out with ultrafiltration or osmosis filtration method or with the progressive operation of reversed phase partition chromatography, obtain making above-mentioned desirable one-tenth separating/enriching and the above-mentioned undesirable operation that becomes the 2nd fraction of separating/enriching of the 1st fraction that above-mentioned undesirable composition reduces with making above-mentioned desirable composition minimizing; (c) use the said extracted residue, the operation of preparation reconstituted tobacco base-material; (d) above-mentioned the 2nd fraction that above-mentioned the 1st fraction is at random reduced with amount is added into the operation in the above-mentioned reconstituted tobacco base-material.
2. according to the method for record in the claim 1, wherein, adopt milipore filter or osmosis filtration film to carry out above-mentioned progressive operation, obtain film and do not see through fraction through fraction and film.
3. according to the manufacture method of putting down in writing in the claim 2, wherein, above-mentioned progressive operation adopts the different film of classification molecular weight repeatedly to carry out, and the film that obtains is not seen through thing fraction and film see through being added into more than 1 or 1 in the above-mentioned reconstituted tobacco base-material of thing fraction, wherein, this film that obtains do not see through that thing fraction and film see through the thing fraction whole when being added in the above-mentioned reconstituted tobacco base-material, reduce this film that obtains and do not see through the amount that thing fraction and film see through at least a kind of fraction in the thing fraction, be added into again in the above-mentioned reconstituted tobacco base-material.
4. according to the method for record in the claim 2, wherein, it is the fraction that nitrate ion reduces that above-mentioned film does not see through the thing fraction, and it is added in the above-mentioned reconstituted tobacco base-material.
5. according to the method for record in the claim 1, wherein, above-mentioned progressive operation is undertaken by reversed phase partition chromatography, obtains the fraction that nitrosamine reduces from said extracted liquid.
6. according to the method for putting down in writing in the claim 5, wherein, use is carried out above-mentioned reversed phase partition chromatography with (methyl) acrylic resin, vinyl-based resin or silicones mutually as the fixing of matrix material, and above-mentioned matrix material has the hydrophobic group that carbon atom quantity is the hydrocarbon below 6 or 6.
7. according to the method for record in the claim 5, it is characterized in that the extract that above-mentioned nitrosamine reduces is compared with above-mentioned natural baccy material, nitrosamine reduces the ratio of nicotine.
8. according to the method for record in the claim 2, wherein, above-mentioned film is seen through the thing fraction supply with the progressive operation of adopting reversed phase partition chromatography, see through the thing fraction from this film and obtain nicotine by enrichment and the fraction that TSNA is removed.
9. according to the method for record in the claim 8, wherein, it is the fraction that nitrate ion reduces that above-mentioned film does not see through the thing fraction, and it is added in the above-mentioned reconstituted tobacco base-material.
10. according to the method for putting down in writing in the claim 8, wherein, employing is carried out above-mentioned reversed phase partition chromatography with (methyl) acrylic resin, vinyl-based resin or silicones mutually as the fixing of matrix material, and above-mentioned matrix material has the hydrophobic group that carbon atom quantity is the hydrocarbon below 6 or 6.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003128104 | 2003-05-06 | ||
| JP128104/2003 | 2003-05-06 | ||
| JP384083/2003 | 2003-11-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004800121138A Expired - Fee Related CN100415125C (en) | 2003-05-06 | 2004-04-26 | Method of manufacturing regenerated tobacco material |
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| UA (1) | UA79698C2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106714587A (en) * | 2014-08-20 | 2017-05-24 | 菲利普莫里斯生产公司 | Methods for forming aerosol-generating substrates having a reduced amount of tobacco specific nitrosamines |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2717434T3 (en) * | 2013-03-15 | 2019-06-21 | Philip Morris Products Sa | Methods to reduce one or more tobacco-specific nitrosamines in tobacco material |
| CN103349351B (en) * | 2013-07-24 | 2016-03-09 | 江苏久吾高科技股份有限公司 | A kind of method of the papermaking-method reconstituted tobaccos based on membrane separation technique |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56148275A (en) * | 1980-03-05 | 1981-11-17 | Philip Morris Inc | Tobacco treatment |
| JPS62298167A (en) * | 1986-06-18 | 1987-12-25 | Hitachi Ltd | Semiconductor integrated circuit device |
| CN1053535A (en) * | 1990-01-25 | 1991-08-07 | 聂绪强 | New-type cigarette and manufacture method thereof |
| JPH05292935A (en) * | 1991-09-30 | 1993-11-09 | R J Reynolds Tobacco Co | Method for reconstituting tobacco |
-
2004
- 2004-04-26 CN CNB2004800121138A patent/CN100415125C/en not_active Expired - Fee Related
- 2004-04-26 UA UAA200511542A patent/UA79698C2/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56148275A (en) * | 1980-03-05 | 1981-11-17 | Philip Morris Inc | Tobacco treatment |
| JPS62298167A (en) * | 1986-06-18 | 1987-12-25 | Hitachi Ltd | Semiconductor integrated circuit device |
| CN1053535A (en) * | 1990-01-25 | 1991-08-07 | 聂绪强 | New-type cigarette and manufacture method thereof |
| JPH05292935A (en) * | 1991-09-30 | 1993-11-09 | R J Reynolds Tobacco Co | Method for reconstituting tobacco |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106714587A (en) * | 2014-08-20 | 2017-05-24 | 菲利普莫里斯生产公司 | Methods for forming aerosol-generating substrates having a reduced amount of tobacco specific nitrosamines |
| CN106714587B (en) * | 2014-08-20 | 2021-10-22 | 菲利普莫里斯生产公司 | Method for forming an aerosol-generating substrate having a reduced amount of tobacco-specific nitrosamines |
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| Publication number | Publication date |
|---|---|
| UA79698C2 (en) | 2007-07-10 |
| CN1784152A (en) | 2006-06-07 |
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