DK147252B - SMOKE PRODUCT - Google Patents

Description

T47252

The invention relates to smokable products containing combustible materials on cellulosic basis with additional ingredients, especially with metal chelates.

In the manufacture of a smokable material other than natural tobacco, it is known to rely on both tobacco waste products or mixtures thereof with other plant materials and from natural or synthetic products made from natural or synthetic products which are processed into papery webs. foils or for fibers. Eg. For example, according to German Publication No. 1,900,941 2 147,252, smoky materials can be prepared from cellulose, cellulose derivatives or starch using certain inorganic fillers which maintain the combustion by their glow effect. Furthermore, according to U.S. Pat. No. 3,461,879, as combustion-supporting compounds, hydrated magnesium citrate and calcium tartrate can be added to certain cellulose derivatives. Swiss Patent No. 150,286 discloses solutions of tartaric acid, citric acid and sodium chloride, to which are added ferroammonium sulfate and coumarin dissolved in alcohol, which solutions in a tobacco material produce a kind of filtering effect, which according to the patent achieves an adsorption of harmful smoke substances, the purpose is thus solely to reduce the toxic effects of tobacco smoke. The present invention, on the other hand, is aimed at achieving a homogeneous distribution of specific chelate compounds on cellulosic carrier material, thereby clearly achieving a combustion controlling effect.

The smoky products which are not naturally occurring in prior art methods do not exhibit satisfactory organoleptic properties, but exhibit more or less unpleasant organoleptic properties such as sharpness and poor aroma in both the main and lateral stream. Eg. one finds an unpleasant sulphide taste in the smoke from tobacco substitute products which exhibit only a low sulfur content, e.g. in the form of sulphates. High-cellulose tobacco replacement products, which commonly contain alkali metal, alkaline earth metal and iron salts commonly used in smoking products, give a sharp and biting smoke with cellulose flavor, leaving an unfavorable astringent effect in the oral cavity. Furthermore, the known non-naturally occurring smoky products usually exhibit unsatisfactory organoleptic properties when mixed with a variety of tobacco varieties.

Eg. For example, the use of substances which in a known manner can be added to improve the glow properties, such as magnesium citrate or calcium tartrate, for smoking products whose organoleptic properties are totally unsatisfactory. An insufficient reduction in sharpness is provided. Particularly disturbing is the unpleasant taste (cellulose flavor) of the cellulose-containing material in such smoking products, as well as the smell of burnt paper, which is practically not reduced compared to the odor and taste properties of pure cellulose. Accordingly, such products have no economic significance as smoking products or as additives to smoking products.

147252 3

Furthermore, the known non-naturally occurring smoky products suffer from the following disadvantages: They have a poor filling volume, a usually unsatisfactory moisture resistance and poor mechanical strength leading to the formation of large amounts of dust during processing.

In contrast to the previously used combustible materials which are known to be mixed with combustion-modifying substances, the products of this invention upon smoking exhibit organoleptic reduced sharpness, a pleasant mild taste without astringent effect and an improved odor. Also for example. By incorporating the smokers in question into tobacco with cellulosic flavor, a clear reduction of the sharpness of the aroma of such tobacco is provided. The smoked products in question are characterized by a particularly low condensate value and also exhibit excellent glow properties. The smoked products in question are particularly distinguished by a smoke without cellulose flavor and thus do not provide any organoleptically irritating components.

There is now provided a smokable product containing a combustible material on a cellulose basis, which product is peculiar in that it contains a chelate compound of the general formula

Kz Mex Ry (I) where K means magnesium, calcium or manganese (II),

Me means trivalent iron or aluminum, R means an anion of a chelating organic carboxylic acid having 2-8 carbon atoms which, in addition to the carboxyl group, contains at least one hydroxyl or keto group or additional carboxy.1 groups, z means 1/2, 1, 3 / 2, 2 or 3, x means 1 or 2 and y means 1-4.

The chelate compounds used herein are hereinafter referred to as "chelates".

Thus, chelates are understood to mean complex salts with a chelate structure containing as cation magnesium, calcium or manganese (II) ions, and as anion a chelate complex with ferric or aluminum ions as the central atom and the chelating organic carboxylic acids as claimed in claim 1. as ligands (cf., e.g., AE Martel1, M. Calvin, Die Chemie der Metall-Chelat-Verbindungen, page 204, Verlag Chemie, Weinheim 1958).

As cations for the cheeses contained in the present products, calcium, magnesium or manganese ions, preferably magnesium or manganese ions, are used.

Chelating organic carboxylic acids, hereinafter referred to as "chelating agents" (cf. AE Martell and M. Calvin: Die Chemie der Metelchelatverbindungen (Page 462-517) Verlag Chemie, Weinheim 1958), are as mentioned above organic carboxylic acids having 2-8 carbon atoms. containing, in addition to the carboxyl group, at least one hydroxyl group, keto group or other carboxy group.

Chelating agents can thus e.g. be dicarboxylic acids. Examples of dicarboxylic acids include: oxalic, malonic, succinic, glutaric, adipic, maleic, fumaric and itaconic.

Particularly preferred dicarboxylic acids are oxalic acid, malonic acid and succinic acid. Chelating agents may also be hydroxy acids, e.g. hydroxymono, hydroxy and hydroxytricarboxylic acids. Examples of hydroxymonecarboxylic acids include: lactic acid, glycolic acid, β-hydroxypropionic acid, glycerolic acid and hydroxypivalic acid. Particularly preferred hydroxymonecarboxylic acids are: glycolic acid and glycerol acid. As hydroxy and hydroxytricarboxylic acids, for example, hydroxymalonic acid, malic acid, tartaric acid, 2-hydroxyglutaric acid, 3-hydroxyglutaric acid, 3-methyl malic acid, 2,5-dihydroxyadipic acid, 2,4-dihydroxyadipic acid and citric acid, preferably acetic acid,

Chelating agents can furthermore e.g. be the mono- and dicarboxylic acids derived from pentoses and hexoses. Examples thereof are those known as "Uronic Acids" isomeric monocarboxylic acids such as glucuronic acid, galacturonic acid and mannuronic acid, those known as sugary acid such as sugary acid, mano or idosugaric acid, as well as the isomeric mucosal acids (galactaric acids). pentoses derived pentaric acids can be mentioned ribotrioxyglutaric acid and xylotrioxyglutaric acid.Section chelates containing a keto group can be used ketocarboxylic acids having 3-8 carbon atoms such as pyruvic acid, ethyl acetate, levulinic acid and mesoxalic acid.

As chelating agents, dicarboxylic and hydroxycarboxylic acids, especially oxalic acid, glycerolic acid, glycolic acid, malic acid, tartaric acid, galactaric acid, sugar acid and citric acid are preferably used.

5 1.47262

For example, it has been found particularly advantageous to use chelates similar to the general formula (I) having the following composition: magnesium ferric glycolate, magnesium ferric oxalate, magnesium ferric citrate, magnesium ferric tartrate, magnesium ferric acid. -galactarate, magnesium ferric saccharate, magnesium aluminum glycolate, magnesium aluminum oxalate, magnesium aluminum citrate, magnesium - aluminum tartrate, magnesium aluminum galactarate, magnesium - aluminum saccharate, manganese ferric -glycolate, manganese-ferric oxalate, manganese-ferric citrate, manganese-ferric tartrate, manganese-ferric galactarate, manganese-ferric saccharate, manganese-aluminum glycolate, manganese-aluminum - oxalate, manganese-aluminum citrate, manganese-aluminum tartrate, manganese-aluminum-galotarate, and manganese-aluminum-saccharate.

The chelates used in the smoking products of the invention may e.g. have the composition listed in Table I. The compounds listed in Table I correspond to the general formula (i) (K_ / Me R 7) in which K means magnesium, calcium or manganese (II), or λ y ~ and Me means iron (III) or aluminum, and R is the chelating carboxylic acid. The given values of x, y and z are inserted into the general formula (i) and thus give the sum formula for the chelates summarized as examples.

Table I

R x y free negative z valences_______ Λι 1 ... - ... 1 .1 - - 11 '1

Citrate 1 2 3 · ^ / 2

Citrate 12 6 5

Citrate 1 5 6 5

Citrate 25 6 5

Tartrate 11 1 1/2

Tartrate 12 5 3/2

Tartrate 1 5 5 5/2

Tartrate 25 4 2

Oxalate 12 1 1/2

Oxalate I5 5 5/2

Oxalate 14 4 2

Glycolate 1 2 1. 1.2

Glycolate 1 3 3 3/2

Galactarate 11 1 1/2

Galactarate 11 2 1

Galactarate 12 3 3/2

Galactarate__1__3__5_3 / 2__ 147252 6 Particularly preferred chelating agents are tartaric / citric acid and galactaric acid.

Particularly preferred chelates are magnesium ferric tartrate, magnesium ferric citrate, magnesium aluminum tartrate, magnesium aluminum citrate, manganese ferric galactarate and manganese ferric citrate.

The chelates contained in the subject smokers may be prepared in aqueous solution in known manner, e.g. by reacting ferric or aluminum salts of the chelating carboxylic acids concerned with calcium, magnesium or manganese salts, the latter being added as hydroxides, carbonates or salts of the corresponding chelating carboxylic acids (cf. German Patent No. 514,504, Hanus and Square Z, Anorg. Chem. 63, p. 314 (1909) and W. Pranke, Liebig Ann. Chem. 486, p. 248 (19 ^ 1)).

Combustible materials on a cellulose basis are e.g. cellulose-containing plant material, especially tobacco, tobacco waste products, e.g. stems, ribs or crumbs, loose cellulosic plant material such as hay, straw, lupines or ferns, and cellulose or cellular substances or cellulose derivatives mixed or unmixed. As cellulose derivatives, for example, use carboxymethyl cellulose, hydroxyethyl cellulose or methyl cellulose.

Further, as combustible materials, the polymer homologous lower molecular weight cellulose fragments formed by cellulose, as well as the cellulose derivatives produced by chemical processes, especially by alkaline or acid oxidation, can be used.

Particularly good results are obtained from the use of tobacco as well as from paper-like webs of tobacco waste products or from cellulose or cellular substances.

The smokable products of the invention usually contain from 0.5 to 70% by weight, preferably 5-50% by weight, of chelate, based on the total weight of the combustible material used in the smokable product of the invention. It has been found advantageous to adjust the amount of chelate to the cellulose content of the combustible material used. At a share of approx. 10% by weight of cellulose in the combustible material is used e.g. preferably 1-15% by weight chelate, based on total weight, especially 5-10% by weight. At a proportion of more than 70% by weight of cellulose in the combustible material, 10-70% by weight of chelate, based on total weight, is used, in particular 25-50% by weight.

7 147252

In a preferred embodiment of the invention, the smoked products contain a filler. By fillers is meant, under the smoking conditions, tastefully inert mineral materials, inorganic salts and oxides such as silica, silicates, mica, clay soils, dolomite, magnesite and chalk, e.g. carbonates, phosphates and oxides of aluminum, iron, magnesium and calcium. Inert fillers can also be used which dispense water under the smoking conditions. The water splitting may either be due to a high content of crystal water in the filler, or also due to chemical decomposition, e.g. from metal hydroxides. Particularly advantageous fillers are aluminum and iron hydroxides and oxide hydrates, natural silicates such as vermiculite and kaolin, precipitated silicates such as silicic acid, silica gel, silica sol, alkaline earth metal and alkali metal silicates, especially aluminum and / or silicic acid hydrates. The fillers are usually used in amounts of 1-70% by weight, based on the total weight of the smokable product, preferably 15-50% by weight. It has been found particularly advantageous to use the fillers in a ratio of 9: 1-1: 9 to the chelate used.

In another preferred embodiment of the invention, the smokable products contain compounds which dispense ammonia under the smoking conditions. As such compounds, in particular, ammonium salts of inorganic acids and organic carboxylic acids as well as salts of amino acids and acid amides can be used.

Particularly preferred compounds which cleave ammonia under the smoking conditions are acidic and neutral ammonium salts of inorganic acids, such as oreboxylic acid, nitric acid and phosphoric acid, especially ammonium salts of phosphoric acid.

Good results are also obtained with acidic and neutral ammonium salts of organic carboxylic acids having a carbon / oxygen ratio in the sum formula of from 2: 1 to 1: 2, preferably from 1: 1 to 1: 2.

Examples include the ammonium salts of monocarboxylic acids, such as formic acid and acetic acid, of dicarboxylic acids, such as oxalic acid, malonic acid and succinic acid, of hydroxymono, hydroxy and hydroxytricarboxylic acids such as glycolic acid, lactic acid, lactic acid, 3-hydroxypropionic acid, 3-hydroxypropionic acid, as well as ammonium salts of the mono- and dicarboxylic acids derived from pentoses and hexoses, such as glucuronic acid, galacturonic acid, mannuronic acid, sugar acid and the isomeric mucosal acids.

Preferably ammonium tartrate and ammonium citrate are used.

With particular advantage, as ammonia decomposing compounds, the corresponding ammonium salts of the ehelates used according to the invention can be used, where "κ" in the general formula (I) means ammonium. Preferably, the following ammonium ehelate compounds are used: ammonium ferric glycolate, ammonium ferric oxalate, ammonium ferric citrate, ammonium ferric tarrate, ammonium ferric galactarate and ammonium ferric saccharate, and ammonium-aluminum-glyeolate, ammonium-aluminum oxalate, ammonium-aluminum-citrate, ammonium-aluminum-tartrate, ammonium-aluminum-galactate and ammonium-aluminum-saccharate.

Particularly preferred are ammonium ferric citrate, ammonium ferric tartrate and ammonium ferric galactarate as well as ammonium aluminum citrate and ammonium aluminum tartrate.

Furthermore, it has been found advantageous to use acid amides as ammonia decomposing compounds. Examples are: aeetamide, propionamide, succinic monoamide and diamide. Particularly preferred is urea.

Further, as ammonia-cleaving compounds, ammonium, magnesium or manganese (II) salts of amino acids can be used, with amino acids being preferably used as glycine, serine, lysine, arginine, leucine, proline, valine, aspartic acid or glutamic acid. Particularly preferred are magnesium and manganese glutamate.

The ammonia decomposing compounds are used e.g. in quantities of from approx. 1 to 25% by weight, based on the smoked product, preferably 5-15% by weight.

It has been found appropriate to use the ammonia-scavenging compounds under the smoking conditions in such an amount that the acids formed in the smoke are neutralized, which can be easily controlled by pH measurements in the main stream smoke. The ammonia decomposing compounds are preferably added in such amounts that a pH of the main stream smoke is adjusted from 5 to 8, preferably from 6 to 7.5.

In a particularly preferred embodiment of the invention, the smoker products contain an oxidizing agent in an amount of 0.01-7, preferably 1-5% by weight, based on the total weight of the smoker product. Oxidizing agent is understood to mean substances which improve the glow conditions of the smoked product.

As an oxidizing agent, for example, use salts of nitric acid, especially alkali metal or alkaline earth metal nitrates. Particularly preferred nitrates are potassium and / or sodium nitrate.

It has been found particularly advantageous to use compounds of heptavalent manganese, especially alkali metal permanganates, such as potassium permanganate, as the oxidizing agent in the smokable products of the invention.

9 147252

In another particularly preferred embodiment, the smokable products contain 0.01-10% by weight, preferably 0.1-5% by weight (based on the smoky product) ammonium salts of poly-galacturonic acids such as pectin, alginic acid or gum arabic and / or ammonium salts of carboxymethylcellulose.

In addition, good organoleptic properties are also obtained using 0.01-5% by weight, preferably 0.1-3% by weight, based on the smoky product, low sulfur protein, for example zein, hordein or gliadin, and by fractional extraction with alcohol, eg. by extraction with ethanol, extracts obtained from these protein substances. The compounds mentioned provide, in addition to the ammonia cleavage, a pleasant plant-like taste with a tobacco-like character in the smoky products. The smoky products produced in this embodiment are aromatic in acceptable terms in any tobacco blend.

In another preferred embodiment, the smoked products contain 0.1-50% by weight of tobacco ingredients, based on the total weight of the smoked product. By tobacco constituents is meant substances or groups of substances that are commonly extracted from tobacco. Tobacco constituents can e.g. extracted by extraction, distillation and extraction. Preferably, tobacco constituents extracted by extraction are used. be made with water or organic solvents.

The combustible material used in the smoking products in question may be in the form of a paper-like web, a fiber web, a foil, a wire or a string which may be cut or uncut.

The papery webs and fiber webs can be made in known manner (cf. Ullmann's Enzyklopådie der techru. Chemie, 3rd ed., Vol. 13, pages 122-130 (1962), ibid vol. 17, pp. 288-296 (1966)).

It has been found particularly advantageous to produce the present products in the form of paper-like webs having a sheet weight of 10--250 g / m 2, preferably 15-60 g / m 2, with leaf thicknesses usually in the range of from approx. 10 to 120 µ, preferably 20 to 60 µ, especially preferably 30 to 45 µ.

The manufacture of the smoked products in question can e.g. so that the combustible material on a cellulose basis is in the form of a papery web, a fiber web, a foil, a wire or a string which may be cut or uncut, on which the chelates used according to the invention are present. is placed in a solution, preferably an aqueous solution. The application can e.g. This is done by immersing the combustible material in a bath with the solution of the chelate compounds with subsequent drying, where temperatures of from approx. 50 to 120 ° C. However, the combustible material can also be sprayed or sprayed with the solution of the chelates. The chelates may also be added directly to the starting mixture from which the combustible material, e.g. in the form of paper-like webs, a fiber web, a foil, a thread or a string are made.

The chelates may e.g. is added directly to a solution containing the combustible material. Such solutions, in addition to optionally used fillers, ammonia scavenging compounds, oxidizing agents and tobacco constituents, may advantageously contain approx.

0.1 to 20% by weight of a binder. As a binder, for example, use polysaccharides or derivatives thereof, gum arabic, starch, low alkali metal earboxymethyl cellulose and / or ammonium carboxymethyl cellulose. Of course, if the binder is a combustible material on a cellulose basis, the binder may partially take over the function of combustible material in the products in question.

The products in question may e.g. is prepared by pouring the solution onto an endless band with subsequent drying at 50-120 ° C.

Preferably, paper-like webs or fiber webs are used for the smoking products of the invention.

Chelate uptake through the film or fiber web can, in addition to processing parameters, be regulated by the structure of the film or by the viscosity and concentration of the solution of the chelate in question. The setting of the viscosity can e.g. is provided by changing the concentration of the chelate solution or by adding thickeners, e.g. low alkali metal earboxymethyl cellulose, hydroxyethyl cellulose, pectin, gum arabic, alginates, galactomanan, starch and derivatives thereof. Concentrated high viscous solutions, for example, for a large absorption of salts in the smoky product.

The fillers used in a preferred embodiment of the invention can be incorporated into the combustible material simultaneously with the ehelates. However, the incorporation of the fillers may also take place in whole or in part in a special step before or after the treatment with the ehelates. The incorporation of the fillers may be accomplished using known technological methods for producing filler-containing paper-like webs, fiber webs or foils.

11 147252

The ammonia decomposing compounds used in a preferred embodiment of the invention may be applied simultaneously with the chelates or in a particular step before or after the incorporation of the chelates into the combustible material. The application takes place e.g. by spraying, immersing or coating the combustible material with aqueous solutions of the ammonia decomposing compounds with subsequent drying.

The oxidizing agents used in a preferred embodiment may be applied simultaneously with the chelates, or they may be applied before or after the incorporation of the chelates into the combustible material. The application takes place e.g. by spraying, immersing or coating the combustible material with a solution of the oxidizing agent in water, alcohol or acetone.

The ammonium salts of polygalacturonic acids used as well as the sulfur-low protein or alcoholic extracts thereof and the above-mentioned tobacco constituents may be applied to the combustible material simultaneously with the chelates, or they may be applied before or after incorporation of the chelates. These substances are preferably incorporated simultaneously with or after the incorporation of the chelates into the smoky material.

Furthermore, in all embodiments, the additives common in tobacco processing can be added in the same or in separate steps, e.g. means for maintaining moisture, "Plavor" and nicetin.

Of course, in the preparation of the smokable products of the invention, any combination of the preferred embodiments can be made.

Smoke analyzes of the smokers in question show a marked reduction in certain physiologically harmful substances compared to tobacco. Thus, a significantly lower phenol and hydrogenyanide acid content per cigarette for cigarettes containing the products in question, as compared to a cigarette with untreated tobacco. In addition, significantly lower condensate values are found. By using filler-containing cellulose films with chelates as opposed to tobacco, a reduction in the phenol content of more than 90%, a reduction of the hydrogen cyanide acid content of approx. and a reduction of the benzpyrene content of approx.

25%. The amount of dry condensate can be reduced, 80-90% compared to tobacco.

"U7252 12

Mixing of the smoked products in question has a beneficial effect on the burning properties of tobacco. This is mainly due to the fact that there is a greater reduction of the physiologically harmful substances in the smoke than would be expected from the individual components of these admixtures.

By varying the chelates as well as the additional components used in the preferred embodiments, e.g. by matching the amount of chelate compounds with the ammonia decomposing compounds under the smoking conditions, the odor and taste of the smokable products may vary. also set a tasteful neutrality. Furthermore, a far-reaching adaptation to tobacco naturally occurring as well as artificial flavor components can be provided.

It is also possible to match the smoky products both to the aroma components, whether synthetic or extracted from tobacco, and to various tobacco varieties such as Burley, Virginia and Orient. In each case, one can reproducibly provide an unchanged, harmonic taste impression with respect to tobacco flavor.

Use of the chelates contained in the products in question is found to be particularly advantageous, since these compounds are usually very well soluble in water. This makes it possible to provide a homogeneous distribution of the chelates in the smoky products in a simple manner and in one operation. Due to the low crystallization tendency and the hygroscopic behavior, the products produced are flexible and elastic, ie. extremely well-processed.

They have a tobacco-like character and are comparable to natural tobacco in terms of their processing properties, e.g. behavior by cutting and mixing. By adjusting the carrier's flat weight to e.g. between 15 and 60 g / m, one can increase the filling volume compared to an equal amount of tobacco for a given smoking article, e.g. cigarette, cigar, or pipe tobacco, and thus tobacco admixtures will have a poorer weighting for the smoking item. This also reduces the total substance to be smoked, and finally also the amount of condensate when smoking.

The smoked products in question are used unmixed or as blend components in cigarette tobacco, cigar tobacco and pipe tobacco. In addition, they can be conveniently used as a cigar cover sheet or cover as cigarette paper.

13 147252

examples

The smoky products formed according to the examples below are processed into filter cigarettes with cellulose acetate filter. The filter cigarettes have a length of 82 mm, a diameter of 8 mm and a string length of 67 mm. The cigarettes are smoked to a medium shutter length of 23 mm.

To characterize the filling density of the cigarettes, the tensile resistance is indicated. The tensile resistance is determined by means of a single-cigarette tensile resistance meter from Filtrona, London, where the pressure drop is measured in "mm HgO".

Usually, the filtered cigarettes manufactured containing the smoked products have tensile resistances between 100 and 125 mm HgO.

The amounts of condensate indicated in the examples mean dry condensate in mg per ml. cigarette. The condensate is measured according to Coresta Standard No. 10. This smokes the sample cigarettes with a tensile volume of 35 mm, a tensile duration of 2 seconds and a tensile frequency of 60 seconds.

The condensate formed comes out on a Cambridge filter and is weighed out. The water fraction is determined titrimetrically by the Karl-Fischer method and subtracted from the total condensate.

The organoleptic properties of the smoky products prepared in the Examples are assessed as follows: a) Sharpness: (++) common cellulose sharpness, (+) slight sharpness, especially with odor (-) almost no sharpness, corresponding to tobacco material (-) without sharpness (b) smoke taste: (++) strong, common cellulose flavor, burnt paper, highly astringent, (+) light cellulose taste, non-astringent, (-) no cellulose taste, little taste influence, (-) mild, no taste influence.

Example laid 100 g of a papery film of bleached sulphate cellulose having a surface weight of 58 g / m and a thickness of 60 μ and an ash content of. $ 0.06 is sprayed with a 25% aqueous solution of magnesium-aluminum - citrate Mg 2 / Algicrate) ^^ and dried so that the resulting dried film contains 20% by weight of chelate. The film is cut into strips with a width of approx. 0.9 mm and of different lengths (cigarette cut) and processed using commercially available cigarette paper wrappers with cellulose acetate filter for cigarettes with an average tensile resistance of 113 mm HgO.

14 147252

When smoking, the cigarettes exhibit uniform glow properties and no flame of the smoky product is detected. The ash is greyish white and self-supporting.

Organoleptic assessment:

Sharpness: (+) Smoke flavor: (-) Dry condensate: 7.3 mg

Example 1b 100 g of a papery film of bleached sulfate cellulose with

ISLAND

a surface weight of 25 g / m, a thickness of 32 µ, and an ash content of 0.08 $ is sprayed with a 25 $ aqueous solution of magnesium aluminum - citrate Mg - ^ / Algf citrate), dried (7 ° S) so that the resulting dried film contains 20% by weight of chelate. The treated film is cut into strips with a width of approx. 0.9 mm and of different lengths (cigarette cut) and processed using commercially available cigarette paper wrappers with cellulose acetate filter for cigarettes with an average tensile resistance of 102 mm H 2 O.

The cigarettes exhibit uniform glow properties during smoking and no flaming of the smoky product. The ash is self-supporting.

Organoleptic assessment:

sharpness; (+) Taste of smoke: (-) Dry condensate: 5.0 mg

Example 1c 100 g of a paper-like foil made from approx. 60% by weight of ground tobacco ribs, 30% by weight of tobacco leaf waste (crumble and dust) and 10% by weight of non-ground sulphate cellulose, which is commonly produced on a long-wire paper machine and has a surface weight of 70 g / m2 and a thickness of 60 μ, is sprayed with a 25% solution of magnesium aluminum citrate Mg 2 [Al 2 (citrate) and dried so that the impregnated film contains 5% chelate. The product thus prepared is cut as described in Example 1 and processed into filter cigarettes with an average tensile resistance of 109 mm H2 O.

The cigarettes exhibit uniform glow properties. The main and side stream smoke is judged to be clearly aromatic.

15 147252

Organoleptic assessment:

Sharpness: (-) Smoke Taste: (-)

Condensate: 6.2 mg

Example 2 (Comparative Example)

A product is prepared similar to that described in Example 1a which contains, as an additive, magnesium citrate instead of magnesium-aluminum citrate. The preparation is carried out by dipping 100 g of a papery film of Example 1 consisting of bleached sulphate cellulose having a surface weight of 58 g / m 2 and a thickness of 60 µ and containing 11.5 wt.% Magnesium carbonate as filler. citric acid solution at 50 ° C to contain magnesium citrate formed in the product. After washing out excess citric acid and drying, the weight gain of the film amounts to 19 g, corresponding to a magnesium citrate content of 22% by weight. The product thus prepared is cut as described in Example 1 and processed into filter cigarettes with an average tensile resistance of 102 mm H2 O.

Organoleptic assessment:

Sharpness: (++) Smoke Taste: (++)

Condensate: 9.5 mg / cig.

Example 5a 100 g of a papery film of Example 1 is sprayed with a 25 $ aqueous solution of magnesium ferric citrate Mg 2 / Fe (citrate and dried so that the dried film contains 20% by weight of chelate. The product thus formed is cut in strips of about 0.9 mm in width and of different length and processed as described in Example 1 for cigarettes having a tensile resistance of 115 mm HgO.

The cigarettes exhibit tobacco-like glow properties during smoking, and it does not flame up the smoky product. The ash is brown-gray and self-supporting.

Organoleptic assessment:

Sharpness: (+) Smoke flavor: (+) Dry condensate: 4.5 mg 16 147252

Example 3b 500 g of dried and cut stalks of Dryopteris filix mas are heated in a 10 liter pressure vessel with 6 liters of a 5% aluminum sulfate solution for 4 hours at 105 ° C. The plant material thus collected is filtered off and washed sulfate-free with water. The fibers are then separated into a Dutch liner, and the material is processed on a longwire paper machine into a web having a surface weight of 68 g / m 2 and a thickness of 6θ µ. 90 g of the film thus produced is sprayed with a 10 $ magnesium iron citrate solution and dried, so that the content of the film of chelate is 10% by weight. The product thus formed is cut as described in Example 1 and processed into filter cigarettes with a tensile resistance of an average of 120 mm H2 O. The cigarettes have a mild mainstream smoke and a pleasant plant-like taste.

Organoleptic assessment:

Sharpness: (-) Smoke Taste: (-)

Condensate: 5.2 mg / cig.

Example 3c 100 g of a paper-like foil prepared from approx.

6% by weight of ground tobacco ribs, 50% by weight of tobacco waste (crumble and dust) and 10% by weight of non-ground sulphate cellulose prepared in a known manner on a paper machine with long wire, which

ISLAND

has a surface weight of 70 g / m and a thickness of 60 µ, is sprayed with a 5 $ aqueous solution of magnesium ferric citrate Mg - ^ / Fe (citrate) 2 ~ / ^ and dried so that the weight gain after drying amounts to $ 5, i.e. a chelate content of 5% by weight is obtained. The cigarettes prepared in the manner described in Example 1 which exhibit a tensile resistance of 115 mm HgO exhibit uniform glow properties.

The ash is brownish-red and self-supporting.

When smoking, the product exhibits a light and aromatic taste impression without cellulose sharpness.

Organoleptic assessment:

Sharpness: (-) Smoke Taste: (-)

Condensate: 4.4 mg / eq.

Example 4 (Comparative Example)

A papery film of Example 1b is dipped alternately in a saturated calcium hydroxide solution and then in a tartaric acid solution, then washed out and dried until the weight gain is 25.3% by weight, so that the film contains approx. 20% by weight of calcium tartrate. The product thus prepared is cut as described in Example 1 (cigarette fine section) and processed into filter cigarettes with a tensile resistance of 117 mm H2 O.

The cigarettes have a depressing, musty aftertaste and a distinctly sharp cellulose sharpness.

Organoleptic assessment:

Sharpness: (++) Smoke flavor: f ++)

Condensate: 8.4 mg / cig.

Example 5

A papery film of Example 1 is treated in an aqueous dipping bath containing 12.6% by weight of magnesium aluminum tartrate Mg 2 / Al (tartrate) 72, imprinted between steel rollers and dried, so that the impregnated web exhibits a weight gain of 24.8 #, corresponding to a chelate content of 20% by weight. The product thus prepared is cut as described in Example 1 and processed into filter cigarettes having an average tensile resistance of 115 mm H2 O. The cigarettes exhibit slow and constant glow properties and form a light self-supporting ash

Organoleptic assessment:

Sharpness: · (+) Smoke Taste: · f.-)

Condensate: 6.8 mg / cig.

Example 6 100 g of a papery film similar to Example 1a is sprayed with a 25 # manganese ferric oxalate solution Mn 2 / Pe (oxalate) 2/2 and dried so that the film thus treated contains 20% by weight of chelate . The resulting product is cut as described in Example 1 and processed into filter cigarettes. Tensile resistance 123 mm HgO. The cigarettes have very regular glow properties and form a brown self-supporting ash.

Organoleptic assessment:

Sharpness: (-) Taste of Smoke: (+)

Condensate: 4.2 mg / cig.

18 147252

Example 7 100 g of a paper-like film of Example 1 is repeatedly sprayed with a total of 250 ml of a 10% magnesium-aluminum-glyoolate solution Mg 2 / Al (glycolate) 72 and dried, so that the chelate content is 20% by weight.

The product thus prepared is processed into filter cigarettes as described in Example 1. Draw resistance 122 mm HgO. The cigarettes have uniform creamer properties and form a light white ash.

Grganoleptic rating:

Sharpness: (+) Smoke Taste: (+)

Condensate: 7 * 0 mg / cig.

Example 8 100 g of a papery film of Example 1 is sprayed with a 12 $ manganese-iron galactarate solution Mn - ^ / Fe (galactarate) ^^ and dried. The film contains 19 * 5% by weight of target wood.

The material, as in Example 1, cut and for filter cigarettes with a tensile resistance of 121 mm HgO, has uniform glow properties and forms a brown-gray ash.

Organoleptic assessment:

Sharpness: (-) Taste of Smoke: (+)

Condensate: 4.9 mg / cig.

Example 9

A mixture of 30% by weight of the impregnated film described in Examples 1 and 70% by weight of a US virginate tobacco having a condensate of 28 mg / cig. is processed into filter cigarettes with a tensile resistance of 126 mm HgO. The flavors and the sweetness characteristic of the virginia tray are completely preserved by smoking the mixture. The nicotine response to the respiratory tract is clearly impaired. Organoleptic assessment:

Sharpness: (-) Smoke Taste: (-)

Condensate: 15 mg / cig.

19 147252

Example 10

A mixture of 30% by weight of the film described in Examples 3 and 70% by weight of an Italian burley tobacco with a condensate of 22 mg / cig. processed into filter cigarettes with an average tensile resistance of 121 mm HgO. When smoking, the cigarettes give the characteristic, cigar-like taste of full burley tobacco. Organoleptic assessment:

Sharpness: (-) Smoke Taste: (-)

Condensate: 12 mg / cig.

Example 11

A blend of 30% by weight of the foil described in Examples 6 and 70% by weight of a commercially available light blend tobacco (flavor type: American blend) with a condensate of 15 mg / cig. processed into filter cigarettes. When smoking, the cigarettes have a pleasant and mild taste. In contrast to the tobacco mixture used, the smoke appears strongly diluted. The glow properties are similar to that of natural tobacco in terms of regularity and speed.

Wood cinema tooth: 118 mm H20 Organoleptic rating:

Sharpness: (-) Smoke Taste: (-)

Condensate: 90 mg

Example 12

As combustible material is used tobacco which is characterized as raw "Burley" with strong cigar-like character. This tobacco is so sprayed with a solution of ammonium ferric citrate (NH4) / Fe (citrate) 2_7 and acidic magnesium aluminum tartrate Mg H / Al (tart) 7 in a 1: 1 weight ratio that the dry matter absorption is 2.5% by weight, i.e. both compounds are present in the treated tobacco material in an amount of 1.25% by weight.

20 147252 In contrast to the material used, the Burley tobacco thus treated exhibits a faint, though spicy-aromatic overall impression in terms of sharpness. The Burley character is completely preserved.

Rating: Sharpness: (-) Smoke Taste: (-)

Example 13

As a combustible material, a papery film of a mixture (1: 1) of ground tobacco ribs and sulphate cellulose having a p surface weight of 45 g / m and a thickness of 55 μ is used. This material is treated in a dipping bath containing 15 parts of magnesium aluminum etrate Mg 2 / K1 (citrate

6 parts of ammonium aluminum citrate (NH4) / Kl (citrate) g_Z

4 parts aluminum hydroxide 4 parts silicic acid 11 parts tobacco extract and 60 parts water.

The film thus treated is pressed and dried at a flow of air at 95 ° C. This results in a 55% weight gain. The dissolved components of the dipping bath are incorporated into the film in the same mutual concentration ratio, ie. the film contains 15.6% by weight

Mg3 [Al (citrate) 2] 2 and 5% by weight (NH4) 3 [A1 (citrate) 2].

In contrast to a product made without the addition of chelate, the resulting smoky product has no astringent effect, exhibits no sharpness and gives a slightly aromatic odor.

Mixed with commercially available cigarette tobacco types, this proves completely acceptable.

Rating: Sharpness: (-) Smoke Taste: (-)

Examples 14 - 22 Chelate Complexes on Cellulose Paths 21 147252

As a starting material for the smokable products, paper-like sheets or webs are made with or without filler on a paper machine. The films thus prepared are compiled in Table II.

Table II

Foil Flatweight Thickness Components Filler $ ash

ISLAND

g / m µ annealing A 45 38 bleached sul- - 0.07 barrel cellulose B 16 20 "- 0.09 c 50 52" ai (oh) 5 29 D 68 60 "Vermieulite ^ 4

The films A-D are prepared in a dipping bath consisting of the aqueous solution of chelate together with an ammonia decomposing compound during the smoking. In Examples 15, 17> 18 and 19, a filler and binder are additionally used in the dipping bath. The immersed foil is pressed through a rolling chair and dried in an air stream at 95 ° C on an endless tape.

Table III lists Examples 14-22 for the nature of the film used as a combustible material, the composition of the dipping bath, the dry weight growth of the treated film (total and chelate growth), and the assessment of the organoleptic properties of the smoked product formed and the condensate value. The amount of solids absorbed by the foil (ammonia decomposing compounds, fillers) is shown by the weight gain, with the individual components being absorbed into the foil in the same weight ratio present in the dipping bath. The amount of chelates recorded is stated separately.

22 147252 i 1

G

Φ O c- rn vo m β * 4 ·> »I ·> 0 ¢ 0 tn G \ CO CT \ vo i * i cq S _________.___- φ i cq di rH Η Φ 60 ^ - ^ ^ ^ ^ ^ (1) H CQ CO + 1 · 1 Η Φ OE ^^

S OH CQ

ISLAND.--------

Ό I

Φ ft ^

B ^^ I

co Ό i i i i ϋ Φ ^^ ui -d cd -p -p co

CQ H O IS- H O

CB <D ·> ·> ·> ·> 'Hg, £ i o in o \ o * o cm cu cvj φ d ------- d φ

60B H

cdB CO VO =! -P o -P ·> ·> ft-P O C3 \ in Ό M3 0 cq b oj oj rc \ in 'h s φ cd 3 ro

1 H-P o H

CD φ · Η H H I Φ Ό Ό Η I 60 S X! 60 CO>

d E CO I H> H

HH 60 Odd O CO -P

cq h 60 co m ε ω_

| _j / -S

H B d Η ° Φ O- C *

-p -p id W

H CQ Η l 60 O 60 O

CD Ό H v_x | -

X! H \ O O

CO> a 60 inH O H

B CM <_ CM <; ; h i i ε ε

Η H d d B ΒΕΙ -P

CO Φ Η H O O d d CO

a-σ d G -p -P h co d

CQ d ^ O O CQ CQ d -P -P

co h d ε ε d d g ε d dX2 φ ε ε η η ε d co

60 B d -P CO -P CO -P d d Ε Η -P

d ϋο · Η co co d did ^

H CO B H 60 d 60 d H H

d Η \ -P -P 60 60 & οε-ρ Γ <,

-P d Φ 60 O d Od d co SJ

S O Ό— 'O ¢ 0 O c0 O O ^ -Hd ^ ·

CQ E d H-P H-P in moOcfl-PM

d ε φ φ s CD et-P CQ _______-_ 1 ^ h c0 I ΚΛ ΓΝ Γν i cm cq E-P ^ i I i I Φ d co -P ε-P CM E-P CU 'd I -p

CQ H d cO d CO'- 'd cO "-' 60 E cO

-P CQ -P d Hd-p Hd-P cod d

(D CD H-P CQ-PCO CQ -P CO EH -P

Ό ^ dOH CD H d Φ H d G d

03 d 60 H o d O-P d O P -pH OJ

xj cd cod ^ 6οε · π 6οεπ dS -p CD-P-P EHCM cod «$ 0 d O ^

ft CO H d Η E Hs— 'E H N— CQ Η -P H

ft Η H 60H l <d.H d, H CO CO 1- = 0,!> s Φ \ E \ l bOHk, bOHUe - 60 1 d Si Q X! 60 o d rn gSj SSJ §p fi o · - · OH 60 od n od A Odd CVJC0S OH 60 O H 60 CSVH CO 60

--- H CO g__OJ CO S__H CQ P S

H ® ft G "" ^ wd - = o- <mc vo - b- pq id <8 H ^ _x H ^ Hw H wm c- 23 147252 β tu <x) in oo m ro ^ · 1 · C + j "vt · oo p · mt" 0 GD> 0) W m ε ra______

pH

G i i P i ε h o tj> -—- - -

'Θ. P 0] G I ^ I I

ό g o ε i i i i + G O H W - - ^ w w M ------ &

P

G Ό I - -> - -Τ 'λ: o) iiiii ___to rd —__ ^ __ ^ __ ^ __ ^ _ φ: p -PG, _ DJ Η in P ro H o GKGP' '', · ih xi oo Vo "ro vo

Μ O H

0) G β Ή Dl44 H

never o G

4J4J4JO 'S · o - CO

p4 <a O co r4 ^ σι i-i

O & 4 H

<0 Ή

! 4 P

_ 3 I II O

+) 1 Η +> -Η -Η -Η -H 44 dj Φ1Ι4 tjigi Di g, β _

di ϋτΙΗ J id S i g m 6 i l + J

+) ca \ o 3 i4 3 co β p β ^ J4 -P -P D> P Dl G O tSMlJO β o m ε ~ 8} —- β

^ G

H 44 P Γ0 ro H O G - - '° 5 H +1 + J ® B &

ω -P Di O Dl O

P Ti Η - I w I I +}

G P \ O O G

Λ> 1 Di O P inH β G ft - 04 <<N <Dl H - = ------ ® I I> 4

Ή P I I I> L G

44 ^^ 3 44 β 3

Dl β - O P -Η -P O Ή -P 1 ·

Di G -P P 44 01 fi β -ρω. β Dl β ρ 43 g ω goo ω g ο β -HiHM-μββ g I β β, i "Γ1 β Αί Ο -ri -η D14J ε ε · Η D1-P 8, Μ 4J G 44 ρ p GG nS ni Ρ GGG 4J $ 4 ί «· Η \ ρεε 4J -p β ε ε g ©

Dl β G D> β θ 'G Di G ns Dip + J

β O'fl '' D1D1-P P P Di Di + 4 -P

G Ε β βθ44 o 44 β o p P

g S dl (D o o H o-H o -Η o o h onS G

S <+1 oi mm D 04 u 01 o in h Di ρ -P 4J

nS ____- ____44 di ω 04 04 04 04 · -

0] 1—1 I 1—1 I 1—1 I 1—1 ro -P

-p ε 04 S 44 04 g 44 04 g 04 I 44 ^ β

(D β— 3 ιί ^ 3 id β 8ns-P G

> β -P44 -HP4J Ή P 44 -H4J PPG O

G ω 44 G ω-PG Dl -P G D14JG -H-PP o

Λ G G Ρ G -Ρ Ρ G -Ρ Ρ G G Ρ ω-Ρ-Ρ P

G β P -P βϋ-Ρ β O -P β P 44 G O -Ρ a

ft ^ Di-P-P Di 8 -P tT »g -H Di-P -P β ε t) 4J

ft P G-PO G 3 AND β U G-Ρϋ D> β - Di> 1 G g O - g -P - g -Ρ - g U "G -P 04 R) Q4J4J IG βΗ βΗ IG 8 β Η> G -PD> -P ft Di-P ri! Di-P <! D> -P ft -P <η η p1—1 ε1 1 ε 1 1 ρ 1 1 Di ε 1 1 -ρ G \ up οβοο οβοο up β ro

β Di 0GD1 ο Η Di OrPDi nlGDi 0HD1 4J

O - P 44 SI H G S -PGSI P 44 SI VOGSI ω ____ fti -----> G 1-1

P -P -P

ft rp 1 · 1 ^ '- E4

ωο openq oiU 'oCJ PU 04Q

44ί 44 P'- '1 — I' 04 - 04— 04— a ft —___ J___

Examples 23 - 25: Tobacco Blends 24 ΐ47252

The cut sheets from Examples 15 * 16 and 18 are mixed with a commercial grade light cigarette tobacco and processed into filter cigarettes.

Example 23

A 30 $ blend of the foil described in Example 15 with a commercial grade light cigarette tobacco gives a round, soft aroma impression without any sharpness of cellulose. Due to the lower content of the total mixture, only the reaction of inhalation of the main stream smoke is impaired.

Rating: Sharpness: (-) Condensate: 13.6 mg Smoke flavor: (-)

Example 24

A 30 wt.% Blend of the film described in Example 16 gives a slight attenuated flavor impression of the low residue (-) tobacco blend. As for the nicotine reaction by inhalation of the mainstream smoke, the same effect as described in Example 13 is obtained.

Rating: Sharpness: (-) Condensate: 14.1 mg Smoke flavor: (-)

Example 25

A 30% by weight blend of the film described in Example 18 is organoleptically weaker in terms of aroma, but is completely inert in sharpness.

No cellulose-like offset is found in either the main stream or the sidestream smoke. The nicotine reaction by inhalation of the mainstream smoke is further attenuated compared with Examples 23 and 24.

Rating: Sharpness: (-) Smoke Taste: (-)

Condensate: 15 * 0 mg

Examples 26-31 25 147252

Films of Examples 14-22 are dipped or sprayed as described in Examples 26-31 in or with a solution of aqueous tobacco extract containing approx. 30% by weight of soluble tobacco constituents, so that the uptake of dry matter is up to 50% by weight. The drying is carried out by means of hot air at a temperature of 60-100 ° C.

Example 26 $ 20 of the ingredients in a flavored "american blend" flavored tobacco mixture is extracted with a cold methanol / water solution (70 volume / 30 volume). This water-methanol extract is sprayed onto the smoky product described in Example 17, so that a dry solids uptake of 30% by weight is obtained.The resulting product is processed as a filter cigarette. recognizable nicotine reaction and a fully aromatic sidestream, the smoked product thus produced is acceptable in any blend relationship with the Virginia, Burley and Orient tobacco varieties and mixtures thereof (Condensate: 9.8 mg).

Example 27

The film prepared in Example 19 is treated with the same extract of tobacco ingredients as in Example 26 to provide an increase in dry weight of 29% by weight. The taste impression of the product processed as a filter cigarette is judged to be low in flavor and inert, with only a slight sharpness (rating: (-)) found in smoking. The sidestream smoke is aromatic and mild. (Smoke flavor rating: (-), condensate: 10.7 mg).

Example 28

The film prepared in Example 20 is treated with the same extract of tobacco ingredients as in Example 26 to provide a dry weight gain of 25% by weight. Contrary to Example 27, a fuller taste impression is found with good reaction, with no sharpness in smoking (rating: (-)), nor is any cellulose taste (rating: (-)) found. The sidestream smoke is pleasantly aromatic. : 9 * 0 mg).

Example 29 26 147252

The ingredients in American virginia tobacco are completely extracted with warm water. This aqueous extract is sprayed onto the product of Example 20 so that the dry matter addition amounts to $ 31. When smoking this tobacco, unadulterated typical virginia flavor is found whose spicy taste is not affected by the foil. Rating: Sharpness: (-) Condensate: 11.0 mg Smoke flavor: (-)

Example 30

By extraction with a cold methanol / water solution (60 volume / 40 volume), the soluble constituents from Italian Burley Tobacco are completely extracted. This extract is sprayed on the smoky product prepared in Example 22 so that the weight gain is $ 20. The taste impression is similar to a good, characteristic Burleyt tobacco with a sweet character. The smoky product exhibits less sharpness than the Burley tobacco used for extraction. The smoked product thus produced is acceptable in any blend relationship with the Virginia, Burley and Orient tobacco varieties as well as their blends.

Rating: Sharpness: (-) Condensate: 11.3 mg Smoke flavor: (-)

Example 31

The film C listed in Table II is treated in a dipping bath containing 160 g of ammonium citrate, 80 g of magnesium aluminum citrate Mg 2 [Al 2 (citrate) and 280 g of the tobacco ingredient mentioned in Example 29 extracted by extraction with water. The pH of the dipping bath is set to 7 with ammonia. The growth in the dry weight of the film is thereby 50%, the smoked product thus produced containing 5.1% by weight of chelate. When smoking, the product gives a light, aromatic, for taste and sharpness practically free smoke impression. Mixtures with conventional tobacco varieties in any ratio are acceptable. Rating: Sharpness: (-) Condensate: 9.9 mg Smoke flavor: (-) 27 147262

Example 52

To a 5 $ aqueous solution of sodium carboxymethyl cellulose / ammonium carboxymethyl cellulose (5: 1) is added: 15 parts ground, pure linters (99 * 8 $ a-cellulose) 15 parts aluminum hydroxide 5 parts magnesium aluminum citrate Mg 2 / Kl (citrate) 2_72 5 parts magnesium iron citrate Mg 2 / Fe (citrate) 2_72

The solution is poured onto a Teflon-coated metal strip by means of a pressure dispenser and dried at 150 ° C. The manufactured

ISLAND

foil has a weight of 15 g / m. A 50% by weight blend of this product with a Virginia / Burley blend (weight ratio 5: 1), unlike the Virginia / Burley blend without the product, exhibits slight aroma impairment, but no flavor distortion and no sharpness (-). (Condensate: 12.4 mg).

Example 55

A one-part thread of cigarette paper is sprayed with a 6% by weight solution of magnesium aluminum citrate Mg 2 / Al 2 (citrate) yj and ammonium aluminum citrate (NH 2 Salt absorption is 9% by weight. The taste and smell of the cigarettes produced here are better expressed than the use of untreated cigarette paper, as the treated paper no longer shows any sharpness and does not give rise to any disruptive cellulose flavor.

Example - 49

As combustible material, paper webs of bleached sulfate cell material with different filler contents and with different surface weight are used. The composition of the starting foils used as combustible material is given in Table IV.

Table V lists examples of the preparation of smokable products according to the invention as well as the amounts of condensate formed from these products.

Table VI lists the preparation of smokable products according to Table V, which further contains potassium permanganate as the oxidizing agent, as well as the amounts of condensate formed from these products.

28 147252

Table IV

Foil Cellulose Fillers Surface weight Thickness material g / m2 µ A bleached 43.5 weight percent 42 55 sulphate cent cellulose Al (OH) z lose 10.2 vs ^ t percent SiO 2 B "44.6 weight percent 50 62

cent Al (OH

C. ”40.2 weight pro- 54 70 cents

Al (OH), 10.0 weight percent SiO 2 D "31, 1 weight percent 38 45 cents

Al (OH), 12.4 weight percent SiO 2 E 16.1 weight percent 32 40 cents

Al (OH) + F 18 weight percent 35 cents

Al! OR.) ^ 29 147252

-P

ø 03 d

(D CO IH H KV VO OO

Ό · * * * v ·.

£ K> KV - = t - = | - Ό - = 1- O g1 s ε 0) -P -P _ 03 cO VO σ \ KV O l> - o

CdrH · »· * · * ·» ·> · *

lp ø O COCJV ^ l-OO KV

ifr 4h η HH CVJ

CD P O S <D \ bOR H „

ø R ø OJ OO ^ t-VOLO O

P O P ·> · <·. ·> ·> ·> Ap o o vo κ vd is = *

OfflB Ol Η H OJ Ol - = 1- Ό

S

• cO CD>

-------- ------------_________ ....... - - "» H

i_ H +3

c «^ SI

h? h h? h ^ s g

1 OJ I cvl P 'O

OJ -— 'OJ ^ CO CJ t3. — S P ^ -P P (Die ^ p ø p co -p ni i; s P 0 P CO P -H! *! D 0 P P P P O COjx! P P · Η P H W co

• P · Η O · Η O <D P «0 O

t> H o ^ o ^ ife øao \ -—- (D w 0 hJ R p H bO {D Ifø,, <D KV <µ P | ^ ^

(OP ^ PS bO K 03bOH

Rø KV · = Κ bO SS M øp

Ό bO K S

ø s s +1 co ø rq o ^ P 0 P, Ω, Ω ø P 0 P ø O tp a øp pppp p · * ø a p ρ0 · ηρ & ο 1¾ p p h s o P p ø d s

Ό · Η P O 0 d O 0 bO -H O

O · Ρ P d P P d P H P * P

<P dC3 0 p d PP PH PP

0 Pd P 0rH T-3 0.p0 3S._y øp P Ό bfl S · ι-3 'O Ώ Pø bO T-3 0 -PPl-pt-pfS B d SRS "®. Pd ε-o oKVKVKVdRdHdodH pp. pds ip s · ρ o · ρ m · ρ p · ρ a ø md -pdod * · * ra p ra ø d ra dop ^ p ra.pp.p ra ra ra ø ra ø dodo Ώ Row 8 ødwd ^! ^ i ^! dddbos.psd island

m do do ø 0 0 bO Ή bO 0 S P B ø bO

d bOB-PB øPøBødØ> P.p

0 0 S P B · Η · Ρ * H S d B d'O

s s o d o oooot nut S bbbooovokvcviojih o æ ø oooooooojitvhh op CQ COKVOJOJ 03 03 03 H p a ό _ ^ ________ ______ - _____ .....— Il · »I - 1 1 -P I—] bp d

cd M cB

PH> R Η Ό • H 0 ØH> • p0 <c pq o p h 1¾ ø H o Open O 0 Hø H P · 0 d bo d ________------- '3S. £ • P> H Od a fe p 03 jbd kv ltv vo ih oo σν ρή KVKVKVKV KV i * 5 m _______ * 30 147262 Ρ

CO

raw

G

Φ CVI Ον O0 r & * »· \ · \ · ν · ι *» ** * »G ιΗΗ H i — I KV OJ CViCVl 0 tn« 6 ____L___ S i

G P

• ri I bQ

H P 8 cd S5> a g · «- 'cd

m bOO -P

G G h G co o vo o o reh HH

φ d o ø i '· »·>> *> ·. ·.

H S Xi O OJ KV DJ KV kv OJ 0) 01

H G X5 O

O Φ £ G

pH Prri Pt i ra i G Φ bo o

O TS Ί3 O <M

ft cd G

XJ φ bO 10

φ I 02 G O

P .3- HH «H O G fl O Ό ® p cd G φ ra G G g φ ra s ω · ®.φΐΰΜ amw G h-pxi«.

Cd id I -ri ftH φ -P

X! Φ Φ G o cd, a _ Φ h G ra Ό i ra tn

ft fto "Q. cd -» carry a) O

ft H-P H XJ O id G,

> 5 O Φ ft I GCDG & P

H -G id o o ^ t- SH -PG

[> p CO-PO y ft Η H

cd ι-l t> \ HG S co G

H G η φ -a co S bO bO O ra ra Φ cd p S G ra ^ G h id ra ^ s.

X! & 0 cora h g id h co G G G> id -P G G Η Φ ft Εηφ ΦΦ φ bo ra co <d H o

g p G Ρ Η · Η Ό. > ft I

Η Φ ftG H G S · =! -

Φ Hra H G ft G Φ o O

ft \ φ S O cd O Φ bO id G

ε bO G Φ id> Φ EG S

G G G G H ft K

• h o Φ G H-P o ra G «! t — i r-i ra φ cd φ ρ φ "s. bo ^ tiri cd bO Φ HH G'H - = d" - = t id H bo bo S O G-cd Φ Ό

cd G Φ G <D cd G ft bOG Η H

ft * h ή * h G cd G cd Φ Φ cd bO G H G G -P X! G H> ft ft g go g φ φ φ ^ sl g εε & 0 H TS, ft ISLbO Ρ X! ft O. G ΦΦ G g -P p -o ft φ ra ra η P φ G1aGra «cdSidid G 8 GO G Φ G Φ Φ ft ΦΦ U ra Φ Φ ΦΗ ft.η G G„ „

ft hpG pH ra h G G φ SS

«Cd h ft t> 5 ft o» cd o'a'SLH o o ft p φ ra φ ft ft ft p biH ra ra 1 bO O G ra Η H H G Φ Η Φ ft. λ λ η · η s ^ i-ιη vo vo t> - oo practice

ΡΗΦ KV KV KV KV KV KV KV KV

m o ra S h id φ φ G ft 1¾ cd H _ • ft cd ra oh cm kv - = t in vo vo id - = d * - = f- - = d ·

W

Example 47a 31 147252 On the product prepared according to example 34, a solution of citrus pectin in the form of the ammonium salt is sprayed onto it, so that the dry uptake of citrus pectin is 1.3% by weight.

The cigarette processed material exhibits an improved and pleasant fresh and slightly plant-like taste when compared to the product of Example 34. The condensate value is the same.

EXAMPLE 47b 30% by weight of the product of Examples 47a and 70% by weight of a commercially available "american blend" flavored tobacco blend is mixed and processed into cigarettes.

Example 48 On the product of Example 35, a 2 $ ethanolic solution of zein is sprayed so that the weight gain after drying is 1.7 $ zein.

The cigarette processed product exhibits improved aromatization of the main and side stream smoke compared to the product of Example 35. The condensate value is the same.

Example 49 On the product of Example 39, a 2 $ ethanolic solution of zein is sprayed so that the weight gain after drying is 1 * 5% by weight of zein.

The cigarette processed product exhibits a strong intensification of the tobacco flavor and a rounding of the taste impression compared to the product of Example 39 · The condensate value is the same.

32 147252

Example 50

Of the smokable products of Examples 29 and 6, the mixtures listed in Table VII are prepared with a commercial tobacco mixture whose niootine content is 0.86 mg and whose condensate is 14.8 mg per ml. filter cigarette. Table VII lists the condensate content to be expected for the various mixtures and the condensate content found. In addition, the nicotine content is indicated. When calculating the expected values, the fill volume of the various mixtures is taken into account.

147252 33 ti Μ • Η Ρ Ή Ρ φ Ο LTlCOt- OV VO - = 4 ΟΌ \ 4 W Η ΙΛ ΟΙ ri ο ΰ bo ·> ·> · »*. ·> ·.

• Η 3 Η ΟΟΟ ΟΟΟ ί3 «η ^

-Ρ · fiUlM

• Η 3 · Η 0J 0 \ 0J Η 4 ΙΜ Ρ bO Ο VO m CV1 VO - = 4 CV1 Ο φ \ ·> ·>> 1 ·> ·> ·>

Oi ^ ibD ΟΟΟ ΟΟΟ • Μ Φ Η Ϊ3 Ρ - • Ρ £ ΰ 03 ti -ρ φφ CTV = + = 4 O t— 00 · * · »· * · * · ν * Ν β {3„ Ον t— - = 4 Ο \ 0 η Ο ti g1 Η W <Ρ 6 _

-Ρ I

Η CO 3 I Ο (Μ 4 η ίο® ο ·> οο σ \ ·> * · <ί> S3 S-ι CVI ·> ·> η C0 4 φ + a η oo tn η Η Ό

Φ ti Η -Ρ II II I! II II II

γΩ Ο φ 60 ΦϋΌ-Η m Η = 4 S ΙΛ tn Εη ΰΗ · »·» · * · »· * ·> -Ρ C0 φ Η (Μ (Μ Ο Η Η 03 Μ G>» + + + + + + hO (ΰ _ φρ-ρ tt-tn in vo o \

Ih Orlil * ·> ·> · »·> * φ-ρφρ ovom ot-m

pq— / fl Ό r-t H

-P

3 Φ o o h, y p ooo ooo cd bO 00VQ = 4 CO VO - = 4 Ρ ίΒ o> E-i · - '

P P

Μ -M

3 3 Ό Ό r-s

OP OP

u ov ti 3 vo ti acu o amo o o p · o p · o Meet bO 03 3 • Ηϋ a ooo τΐϋ a ooo

Η φ P CVI - = 4 VO HOP CV1 - = 4 VO

Φ bO CD bO

bO 0 SB bO «5 fB

> 3 ti>> 3 U>

Pi + iw 147252

Example 51 34

The film prepared according to Example 36 is sprayed with a water / alcohol solution of potassium nitrate and dried. The spray is such that the increase in dry weight is $ 1.

Condensate: 3.1 mg / cig.

Example 52

The film of Example 36 is sprayed with an aqueous potassium nitrate solution and dried. The spray is such that the increase in dry weight is $ 2.

Condensate: 2.5 mg / eq.

Example 53

The film prepared according to Example 38 is sprayed with an aqueous potassium nitrate solution and dried. The spray is such that the increase in dry weight is $ 2.

Condensate: 3.2 mg / cig.

Example 54

A combustible material in the form of a paper web of bleached sulfate cellulose with a content of 45% by weight of aluminum hydroxide as

. ISLAND

filler and a surface weight of 50 g / m and a thickness of 38 μ are treated in a dipping bath containing 10 parts manganese iron citrate Mn 2 / Fe (citrate) 2_72 6 parts ammonium iron citrate (NH /) ^ / Fe (citrate 5 parts urea 12 parts tobacco content) extracted by complete extraction of hot water Burleytobacco 100 parts water.

The treatment is carried out so as to provide an increase in dry weight of $ 34 after drying at 55-95 ° C at constant rising temperature. The smoked product thus obtained contains 7.6% by weight of chelate. It is processed into filter cigarettes. Organoleptically, the product is judged to be tastefully neutral with clear tobacco flavor.

Condensate: 3.1 mg / cig.

Example 55

A combustible material analogous to that described in Example 54 consisting of a film of bleached sulfate cellulose with 45% by weight aluminum hydroxide as filler pretreated with a 2 $ aqueous potassium permanganate solution is treated in a dipping bath containing 8 parts of manganese galactarate Mn 2 / FeCgalact 8 parts magnesium aluminum etrate Mg 2

The treatment is carried out so as to provide an increase in dry weight of $ 4 after drying at 55-95 ° C with constantly increasing temperature. The smoked product thus produced contains 11.4% by weight of chelate. It is processed into filter cigarettes. The product is considered organoleptic as particularly mild and tobacco-like. Condensate: 2.8 mg / cig.

The product described in this example is extremely acceptable blended with a light-commercial commercial blend.