DE2313191A1 - SMOKE MIXTURE - Google Patents

Description

PATEHTANWÄLTE DR.-ING. H. FINCKE
DIPL. -ING. H. BOHR
DIPL.-ING. S. STAEGER

8 MUNICH 5
MÜLLERSTRASSE 31

Folder 23130 - Dr. K. March 16, 1973

Case Dt 24864

Imperial Chemical Industries Ltd. ■ London, Great Britain

Smoke mixture

Priority: 16. 3- 1972 - Great Britain

The invention relates to smoke mixtures. ο

Because of the popular belief that smoking Tobacco, especially in the form of cigarettes, can cause lung cancer and bronchial ailments attention to the creation of smoke generators Substrates as tobacco substitutes that produce less tar and harmful substances than tobacco. Examples of such a touch producing substrates are cellulose, oxidized cellulose and especially heat-treated cellulose, as they are

ORIOINAL INSPECTED

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for example by the process of GB-PS 1,113,979.

Unfortunately, the belly of such a tobacco ' set the taste of tobacco. In order to achieve an acceptable touch it is therefore necessary to use either the first To mix tsbak or a suitable flavor material to find. Mixtures with tobacco produce a whiff, the health hazards of which are proportional to the tobacco content.

If desired, a tobacco substitute can be made with the dried and pickled leaves of the Nicotiana Rustics plant species. be mixed. This plant species contains a very high proportion of nicotine, for example up to 14% by weight . Unlike ITicotiana Tobaccum, this type of plant has not found a complete acceptance as a basis for smoking materials, due to the extremely strong and unpleasant taste of the smoke obtained with it. However, smaller amounts can be tolerated in admixture with tobacco substitute, which itself produces a neutral smoke. In this way it is possible to produce mixtures which present less health hazards than edible similar mixtures containing tobacco. However, it is desirable to reduce the health hazards of smoking as much as possible, and for this reason the amount of tobacco or other nicotine-containing plant species in smoking mixtures should be reduced as far as possible or even to mill.

According to the invention, a smoke mixture is now proposed, which contains a tobacco substitute mixed with an extracted material which has been treated by treatment liicotiana Hustica with a solvent that dissolves jficotine has been received.

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- ⁷ Y-

The term "tobacco substitute" means any solid material that, although not derived from tobacco, is the same The way tobacco can be smoked. The tobacco substitute can, for example, have a carbohydrate jump, like it for example in GB-P3s 1 055 4-73 and 1 14-3 5CC and in U.S. Patent No. 3,106 2C9. Examples of this are cellulose, oxidized cellulose and lettuce leaves. Cellulose ethers can also be used.

The tobacco substitute is advantageously a thermally degraded carbohydrate, which is produced, for example, by subjecting a carbohydrate (in particular cellulose) to a catalyzed degradation process above 100 ^° C. (for example 100 to 250 ^° C., as described in GB-PS 1,113,979 is subjected to until the weight of the degraded carbohydrate is less than 90 wt .-% of the original carbohydrate. A similar substance can be obtained by the process of GB-PS 1 289 354, namely by an acid or a base catalyzed condensation of a compound of the formula

R ¹ CCCH ₂ CH ₂ COR ² (I)

1 2
wherein R and R, which may be the same or different, each represent a hydrogen atom or an alkyl, hydroxyalkyl or formyl group, or a precursor of such a compound (I).

Iiicotin resolution solvents which can be used for the extraction of liicotiana Rustica, in particular lower aliphatic alcohols having boiling points up to 120 ⁰ C. Specific examples are methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol and t-butanol .

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The extraction can be carried out by known techniques, for example using a Soxhlet device. It is preferred, however, _/ tion technique to perform a hot extraction, for example by äe.3. you fill a permeable sack with dried and crushed Nicotiana Rustica, hang the sack in the Ι ^ .κρί of a boiling solvent, and condense

after solvent from a reflux condenserj down through the

Lets the sack and its contents flow through.

The amount of the extract material in the smoke mixtures according to the invention can be, for example, 1 to 25% by weight of the amount of the tobacco substitute. For the best taste effect, amounts of 4 to 9% are preferred.

The smoke mixtures according to the invention can thereby be produced that one mixes the tobacco substitute and the extract material in an appropriate manner. It can too Still other ingredients for smoke mixes can be incorporated to achieve the desired physical properties and to achieve burning properties. For example, glow-influencing catalysts,, agents to improve the cohesion and color of the ashes, nicotine, other flavoring agents, medicines, humectants or film-forming gowns are added. Possibly tobacco can also be incorporated.

It is preferred, however, that the smoke mixtures are processed into a sheet which contains a film-forming agent, such as natural rubber or pectin or a cellulose ether, in particular carboxymethyl cellulose or a salt thereof. For the production of such foils, the 3estsnd-

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parts of the mixture. preferably together with the tobacco substitute in a finely divided fora, with a sufficient Amount of water mixed to make a slurry, which is then poured onto a surface and dried.

It may be useful to incorporate part of the solution into such a slurry, which is obtained directly by treating Nicotiana Rustica with a solvent. Optionally, however, all or part of the solvent can be recovered and replaced with water to produce a solution / suspension which can then be incorporated into the slurry. This way, better results are sometimes obtained in the film making process and potential fire hazards are eliminated. ■■ '■. j

- t

A sheet material made from the slurry can be crushed to produce a material in a form suitable for puffing. Venn tobacco is incorporated into the smoke mixture, then it can be ground tobacco, which before pouring into 'the Slurry is introduced. Alternatively, shredded tobacco can be mixed with the shredded film.

Surprisingly, it has been shown that despite the unpleasant taste of the smoke from Nicotiana Rustica even smoke mixtures according to the invention have an acceptable And are generally preferred by smokers to comparable mixtures that do not contain extract

material contained by '

Rustica obtained with a nicotine dissolving solvent has been..

Treatment of Nicotiana

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ORIGINAL INSPECTED

However, certain mixtures of tobacco substitutes with the extract material can produce smoke with an undesirable note. By mixing such mixtures with Tsbrik, these notes can be masked. A preferred Kr.uchgemisch consists of a mixture of a Tabakerc-.tzes having 1 to ^{Λ Λ%} (preferably 4 to 9%) of its weight of a Zxtraktmaterials which has been obtained by treating with a nicotine Nicotiena Hustica dissolving solvent, together with 65 up to 90%, based on the weight of the mixture, of tobacco, especially Virginia tobacco pickled in a fireplace. ■ -

The mentioned notes in the according to the invention. Puff mixtures produced smoke originate from the fact that the extract material does not have an ideal balance between Has nicotine and flavoring agents. It is hiring Another feature of the invention, from the Extraktmaterisl Separate fractions, which are neither the largest part of nicotine or most of the flavoring agents, and these fractions with a tobacco substitute combine in proportions such that a product with an acceptable puff taste is obtained, j

In order to separate the fractions mentioned, a solution can be used of the extract material, preferably in an alcoholic one Solvent, with an absorbent solid in; Brought into contact to absorb the nicotine, whereupon the nicotine is separated from the said solid and the flavoring agent from the liquid phase can be obtained.

The extract can be mixed with the absorbent solid, followed by filtration, or passed through through a packed column of the solid already moistened with the liquid according to a Technology that will be used in the areas of

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Chromatography and ion exchange is common. Specific Solids "that can be used" are absorbent solids that, when exposed to water under Forming a 1% suspension are mixed, one Result in liquid with a pH of 2.5 to 6.5. In particular, acid clays and cation exchanges are preferred of value.

Specific Examples "of Acid Clays Used are activated bentonites and contorillonites. Fulmont 3OCC, an activated acidic clay, is special Value. When this substance is mixed with water to form a 1% suspension it gives a liquid with a pH of 6.0.

Specific examples of cation exchange resins used are those commercially available under Chew Zeo-carb £ 225 (H) and Aaberlite IHC 5CH are. '

In a preferred way of carrying out the method, the treatment with the absorbent is carried out in such a way that at least 5C% by weight of the extracted material remain in the solution. The amount of solid and the time and temperature of treatment necessary to achieve these goals will of course depend on the particular solid selected and on the type of treatment used, ie whether the extract is stirred with the solid or through a column of the festival ^! · The substance is allowed to flow. ''<

The resulting flavor-rich material in the solution can be used directly for flavoring tobacco oil used to achieve a touch that is largely free of the tart unpleasant feces that

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by a similar aromatization with the untreated one Extract material from Nicotiana Rustica is obtained, and according to commercial needs or individual tastes, other flavor-inducing Components can be present as desired, such as tobacco,

Nicotine and other basic material produced by the Solid matter absorbed can be recovered therefrom by a known technique such as Elution with a solvent (sometimes a stronger solvent than that in the original extract) or by steam distillation of the solid Make alkaline, for example with sodium hydroxide.

The nicotine-rich material obtained in this way can be used to fortify tobacco or tobacco substitutes. Optionally it can be in tobacco or; Tobacco substitutes can be incorporated together with flavorings or with; ■ a flavor- rich material, ■ '_ ■ which is also made from Nicotiana Rustica in the above. . | _

written way has been received. ^: .

It is particularly advantageous _{to use such a tobacco substitute:} to use which is described in more detail in one of the following patent publications:, Γ.

GB-FS 1 299 296 - Tobacco substitute with usable fuel.:.

speed containing a large amount · filler i '.

DT-OS 2 113 971 - tobacco substitute containing protein I, DT-OS 2 113 970 - tobacco substitute containing protein and isoprenoid ,

contains

DT-OS 2 113 969 - Tobacco substitutes, the protein and phenylethyl alcohol or contains phenylacetic acid

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The invention is explained in more detail by the following examples, in which the parts and percentages are by weight

are pressed.

The taste determinations of the cigarettes mentioned in the examples were carried out by one of the following methods, each with a group of people throwing their cigarettes! smoked and people gave their comments.

In the first method, a group of smokers was herange- '* ■■ attracted, particularly in terms of their high consistent Geschaacksempfindlichkeit and long experience in

Testing the taste of tobacco cigarettes were selected. j

This group was called the Expert Group and consisted of j

from a small number of 5 to B people. .

The second method involved a much larger number of group.

determinations carried out (minimum number 22; minimum number of people 11), whereby the preference for one cigarette over another was determined. The procedure worked on a statistical basis, so that the certainty ^ that a preference was given, with a percentage safety factor could be asked. This group was called "statistical i

Preferred group ¹¹ is designated. ■■ "■ |

At s piel 1.

————————

2.8 parts of glycerin, 0.8 parts / citric acid and 1 part of potassium citrate were dissolved in 20 parts of distilled water and the resulting solution was added to a stirred solution of 2 parts of sodium carboxymethyl cellulose in 30 parts of hot distilled water. For this solution 9 parts of a material which was obtained by heating of U-cellulose impregnated with ammonium sulfamate for 4 hours at 2pG ^c C

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and the 0.74 part casein (fat-free) had been added, 2 parts calcium carbonate and 20 parts of a concentrated solution obtained by Soxhlet extraction from Nicotiana Rustica with ethanol and containing 1.68 parts of extract material was added. The resulting slurry was stirred until homogeneous (approximately 1 hour). -

The slurry was cast on glass plates because "a film having a basis weight of 48 to 52 g / m" was obtained. The film was crushed. The cigarettes made from this shredded material were smoked by a group of experts of four who were unanimously of the opinion that there was a cigarette tobacco taste, whereas they found that it was not present in cigarettes with a similar composition, excluding the extract of liicotiana Rustica had been made. However, some of the somewhat unpleasant notes of liicotiana rustica that a fireplace-pickled tobacco does not have were noted. ^;

Example 2 ■ j

1.1 parts of glycerin was dissolved in 20 parts of distilled water, and this solution became 1.6 parts of sodium carboxycethyl cellulose in 80 parts of distilled water was added and the mixture was stirred. Then! 6.9 Parts magnesium carbonate (magnesite), 4.1 parts calciumr carbonate, 0.2 parts of casein (fat-free), 5.1 parts of an ice material obtained by heating o ^ cellulose in the presence of ammonium sulfamate, and 1.0 part Extract material added, the latter by a; Soxhlet extraction of Nicotiana Rustica with ethanol! had been obtained, and this material ·. again in 20 I. Parts of ethanol had been dissolved.

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The resulting slurry was stirred for at least 1 hour and then poured onto glass plates to make a film from which, when dried, the ethanol is evaporated evaporated. It became a sheet with a green weight obtained from 48 to 52 g / m.

The film was shredded and made into a mixture comprising 40 parts of this shredded product and 60 parts Contained parts of a Virginia tobacco pickled in the fireplace. Cigarettes made from this mix were mixed with those made from a 4G: 60 tobacco mix with a comminuted product that contained no extract material but was otherwise similar, compared.

The cigarettes were compared by the statistical preference group, and the group presented a preference for those cigarettes that contained the Rustica tobacco extract, with a safety factor of 78%.

Example 5

1.6 parts glycerol and 0.4 parts of ammonium sulfate were dissolved in 20 parts of distilled ^water], and this solution was 3 parts * magnesite, 3entonit 0.9 parts to a mixture of 70 parts of distilled water, 5, 3.0 parts Cslciumcarbonat and 1.7 parts of extract material added with the extract material was obtained by treating IJicotiana Rustica with ethanol and this material was but partly suspended in iO parts of water mainly in solution. The mixture was stirred and 2.2 parts of sodium carboxymethyl cellulose and 4.9 parts of a material prepared by heating o ^ cellulose in the presence of ammonium sulfamate were added. Stirring was continued for at least 1 hour. The resulting slurry was poured onto glass plates,

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"to produce a film that, after drying, has a basis weight from 4-8 to 52 g / m.

The film was shredded and processed into a mixture, that is 50 parts of this crushed product and 50 parts contained a 'Virginia' tobacco pickled in the fireplace. Cigarettes from this mixture became with .einem such a 50:50 tobacco mixture compared in which the comminuted product contained no extract material but was otherwise identical.

The cigarettes were rated by a statistical preference group compared. The group placed a preference for the cigarettes with 96% certainty that the Hustica tobacco extract contained.

Example 4-, ■

A sheet material was produced in an identical manner as in Example 3, except that 2.5 parts of the extract material were used instead of the 1.7 parts were used and the amount of the other ingredients reduced proportionally became. A similar test of. Cigarettes

from 5O: 5O tobacco mixtures showed in this case that the preference for the extract-containing cigarettes was destroyed by increasing the extract.

Example 5 , " ^:

1000 g dried Nicoti & na ground in a ball mill Rustica with a moisture content of 7 »9i & were in extracted a Soxleth apparatus with 3000 ml of ethanol for 32 hours. Analysis of equal portions of the extract showed that all of the nicotine had been extracted, and that 36.3% of the dry weight of Nicotiana Rustica gone into solution

Treatment of the above ethanol extract by stirring at room temperature with Fulmont 300C and then filtering the mixture gave filtrates containing 4 to "■ ',} <> of the original nicotine of the extract and 31 to 4θ; ό of the original solids, depending on the A taste test of such a filtrate, which contained 11% of the original nicotine and 33% of the original solids, was carried out by using it in place of the entire extract in a puff mixture prepared according to Example 1. A 10% concentration of the solids produced a smoke with no deleterious notes and a taste of good chimney-pickled tobacco. A similar chimney-pickled tobacco taste was obtained at 4.7% solids concentration. At 2.5% concentration A small but definite taste of a tobacco pickled in the fireplace was found on solids, but was: this effect is smaller than with the concentration of 4-, 7 # - L

All of the nicotine retained on the solid residue after filtration was recovered by steam distillation of a slurry of the solid in 30% (w / w) aqueous sodium hydroxide at 140 to 160 ^° C. and collecting the distillate in ½ sulfuric acid. The nicotine was suitable for incorporation into smoking mixtures and did not produce any harmful taste notes. ■;

Example 6 ;

Fulmont * 725C, an activated acidic clay that when mixed with water to form a 1% suspension gives a liquid with a pH of 5, was used in the treatment of ethanol extracts from Nicotiana Rustica in

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the same way as the Pulmont 300C in Example 5 was used. Bas filtrate from the treatment, which is 2.9% of the original Nicotine and 27.9% of the original solids was flavored in the same manner at 4.7% solids concentration examined. It was found that smoke was obtained which was identical to that of the filtrate from the Fulmont 3CGG treatment was largely identical.

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Claims (1)

Claims η Puff mixture, characterized in that it contains a tobacco substitute mixed with an extract material obtained by treating Nicotiana Rustica with a nicotine-dissolving solvent. 2. Smoking mixture according to claim 1, characterized in that the tobacco substitute made of cellulose, a cellulose ether, oxidized cellulose or lettuce leaves. 3. Puff mixture according to claim 1, characterized in that that the tobacco substitute is a thermally broken down carbohydrate. 4-. Puff mixture according to Claim 3, characterized in that the tobacco substitute consists of a thermally degraded carbohydrate which has been produced by subjecting the carbohydrate to a catalyzed breakdown above GG ⁰ G until the weight of the broken down carbohydrate is less than 90 Gew "- # of the original coal-j hydrate was * 5. smoke mixture according to claim 3 or 4, characterized in that that the tobacco substitute consists of thermally degraded cellulose. "■:! 6. Smoking mixture according to one of the preceding claims', characterized in that the extract material has been obtained in that Nicotiana Rustica with; : «- ' ^! '■' ■ - ■ ■■ ·; 1 i \ j a lower aliphatic alcohol with a boiling point; 'ΐ is treated ^{up to 120 0 C.} U. 309838/1049 ^; · ■ - 16 - 7. smoke mixture according to one of the preceding claims, characterized in that the amount of extract material Is 1 to 25% by weight of the tobacco substitute. S. breath mixture according to claim?, Characterized in that the amount of extract material is 4 to 9 Gev .- ^ b of tobacco substitutes. 9 smoking mixture according to one of the preceding claims, characterized in that it is processed into the form of a sheet containing a film-forming agent has been. 10. Smoke mixture according to one of the preceding claims characterized in that it contains tobacco. ^ i. Smoke mixture, characterized in that there is a Mixture of a tobacco substitute between ί to -11 $ its weight of an extract material obtained by treating Hicotiana Rustica with a nicotine-dissolving solvent with 65 to 9G% of their weight is tobacco. I " 12 * Smoke composition according to claim 11 * characterized gekennzeien- net as £ the tobacco substitutes of 4- to S% of its weight of 2X ~ tract material is mixed. _:: 13. Process for the preparation of a smoke mixture; characterized in that one Nicotlana Sustica with a: Nicotine-dissolving solvent treated, separating the extracted material into fractions, on the one hand the largest part containing nicotine and, on the other hand, the flavoring agent1, and that these fractions are combined with a tobacco substitute in such proportions that a product with an acceptable Rauchgeschaack is obtained. . M: 14. 'The method according to claim 1'3, characterized in that that the separation into fractions is effected by -l: d, ai: msn 309838/1049 da3 extracted material with an absorbent solid treated to absorb most of the nicotine on it, then the nicotine-rich fraction from the solid and a flavor-rich fraction are preceded . wins from the liquid phase. ! 15. The method according to claim 14, characterized in that that the absorbent solid is such, deribei Mix with water to form a 1% suspension results in a liquid with a pH of 2.5 to 6.5. j 16. The method according to claim 15 »characterized in that that the absorbent solid is an acidic clay or a cation exchange resin. ; 17. The method according to any one of claims 14 bisji6, characterized in that the treatment with the absorbent solid is carried out so that at least 50 wt .-% of the extracted material remain in the solution. woim «« «ut. ^ \ i H. ! hf (-. S && t > 309138/1049