FI58254C - ROOTPRODUKT OCH FOERFARANDE FOER DESS FRAMSTAELLNING - Google Patents

Description

© FINLAND - FINLAND patent publication — patentskrift 5 8254 ® K,. || 2 / I „«. CI.3 A 24 B 15/00 ® A 24 D 1/18 © Patent application - Patentansökning 3222/72 @ Application date - Ansökningsdag l6. li.72

Sjaoy @ Start date - Giltighetsdag 16.11.72 @ Released to the public - Blivit offentlig 20.05.73 @ Date of publication and date of publication—

Ansökan utlagd och utl.skriften pubi ice rad 30.09-80

National Board of Patents and Registration ® Patents granted - Patent meddelat 12.01.81

Patents and registries

Priority claimed - Begärd priority 19-11-71 29-03.72 Federal Republic of Germany-Förbunds- w republiken Tyskland (DE) P 2157370.6, P 2215 ^ 12.7 (73) Bayer Aktiengesellschaft, D-5090 Leverkusen 1, Federal Republic of Germany- Förbundsrepubliken ) (72) Theo Eicher, Dormagen, Friedemann Muller, Dormagen, Klaus-Werner Krebs, Dormagen, Federal Republic of Germany-Förbundsrepubliken Tyskland (DE) (7 ^) Oy Kolster Ab (5h) Smoking product and method of production - Rökprodukt och förfa-rande for that purpose

The invention relates to smoking articles containing combustible cellulose-based substances and other ingredients, in particular metal chelates, and to a process for their preparation.

In the manufacture of a smoking article other than pure tobacco, it is known to use both tobacco refuse or mixtures thereof with other plant materials and also a non-tobacco natural or synthetic product formed into paper pulp, film or fiber. For example, according to DE-A-1,900 E9I, smoking articles can be made from cellulose, cellulose derivatives or starch using certain inorganic fillers which, when glowed, maintain combustion. Hydrated magnesium citrate and calcium tartrate may be added to cellulose derivatives designated as flame retardants in accordance with U.S. Patent 3,161,879.

Non-tobacco smoking articles prepared by methods known to date do not have satisfactory organoleptic properties, but more or less unpleasant organoleptic properties, such as pungency and poor aromas in the main and side streams. For example, tobacco counter products that contain only a small amount of sulfur in 5S254, e.g., in the form of sulfates, show an unpleasant sulfide taste in the smoke. Tobacco counterpart products with a high cellulose content, which contain alkali, alkaline earth and iron salts commonly used in tobacco products, give a pungent and biting odor with a cellulose taste when glowed, leaving a permanent astringent effect. In addition, known non-tobacco smoking products generally prove to be organoleptically incompatible when mixed with different types of tobacco.

For example, substances which, according to the prior art, are added to improve the glow behavior, such as the use of magnesium citrate or calcium tartrate, lead to smoking products whose organoleptic properties are completely unsatisfactory. The puncture is not reduced enough. Particularly disturbing is the unpleasant taste (cellulosic taste) produced by the combustion of the cellulosic material of such combustible products and the odor of the burnt paper, which is practically not reduced at all compared to the odor and taste properties of pure cellulose. Thus, such products do not prove to be economically viable smoking products or additives in tobacco products.

Disadvantages of known non-tobacco smoking products also include poor filling volume, generally insufficient wet strength, and low mechanical strength, resulting in abundant dust formation during handling.

The invention relates to a smoking preparation which is a cellulose-based combustible substance and which optionally contains fillers and / or ammonia-releasing compounds and / or oxidants and / or polygalacturonic acids and / or proteins and / or tobacco extract, which is characterized in that it contains chelating compounds, having the general formula I

K Me R I

z x y wherein K is magnesium, calcium or manganese (II); Me is trivalent iron or aluminum and R is a chelating organic carboxylic acid residue having 2 to 8 carbon atoms having at least one hydroxyl group, keto group or other carboxyl groups in addition to the carboxyl group; x = 1 or 2 and y = 1, 2, 3 or U and z is a number indicating the number K of divalent cations, the chelate content of the smoking preparation being 0.5 to 70% by weight of the amount of combustible material.

Chelate compounds useful in the products of the invention are hereinafter referred to as chelates.

The chelates contained in the products according to the invention preferably contain magnesium or manganese (II) as a cation.

In several cases, it has proved expedient to partially replace the chelate cations with hydrogen so that the corresponding acid salts are formed. In this case, acidic chelating compounds containing a hydrogen ion are preferred.

58254

Chelating organic carboxylic acids, hereinafter referred to as "chelating agents" (see AE Martell, M. Calvin: Die Chemie der Metalschelatverbindungen, pp. + 62-517, Verlag Chemia, Weinheim 1958), are e.g. organic carboxylic acids with 2- 8 carbon atoms and which, in addition to the carboxyl group, contain at least one hydroxyl group, a keto group or other carboxyl groups.

Chelating agents can thus be, for example, dicarboxylic acids. Examples of dicarboxylic acids are oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid, fumaric acid and itaconic acid. Particularly preferred dicarboxylic acids are oxalic acid, malonic acid and succinic acid. Chelating agents may further include hydroxy acids such as hydroxymono, hydroxide and hydroxytricarboxylic acids. Examples of hydroxymonocarboxylic acids are: lactic acid, glycolic acid, β-hydroxy-propionic acid, glyceric acid and hydroxypivalic acid. Particularly preferred hydroxymonocarboxylic acids are glycolic acid and glyceric acid. Examples of hydroxide and hydroxytricarboxylic acids are hydroxymalonic acid, malic acid, 3-methylmenic acid, 2,5-dihydroxyadipic acid, 2,1 + dihydroxyadipic acid and citric acid, preferably malic acid, tartaric acid and citric acid.

Chelating agents can further be, for example, mono- and dicarboxylic acids derived from pentoses and hexoses. Examples of these are isomeric monocarboxylic acids known as "uronic acids", such as glucuronic acid, galacturonic acid and mannuronic acid, compounds known as sugar acids, such as, for example, sugar acid, manic or idose sugar, and isomeric mucic acids (galactaric acid). Further examples are ribotrioxy-glutaric acid and xylotrioxyglutaric acid derived from pentaric acids derived from pentoses. As chelating agents containing a keto group, ketocarboxylic acids having 3 to 8 carbon atoms can be used. Examples of keto-carboxylic acids are pyruvic acid, acetic acid, levulinic acid and mesoxalic acid.

Dicarboxylic acids and hydroxycarboxylic acids can be preferably used as chelating agents, in particular oxalic acid, glyceric acid, glycolic acid, malic acid, tartaric acid, galactaric acid, sugar acid and citric acid.

For example, it has proved particularly advantageous to use chelates corresponding to the general formula I in the following configurations: magnesium iron III glycolate, magnesium iron III oxalate, magnesium iron III citrate, magnesium iron III tartrate , magnesium iron III galactarate, magnesium iron III precipitate, magnesium aluminum glycolate, magnesium aluminum oxalate, magnesium aluminum citrate, magnesium aluminum tartrate, magnesium aluminum galactarate, magnesium aluminum saccharate, manganese-iron-III-glycolate, manganese-iron-IJI-oxalate, manganese-iron-III-citrate, manganese-iron-III-tartrate, manganese-iron-III-galactarate, manganese iron-III-saccharate, manganese -aluminum-glyco-11 58254 plate, manganese-aluminum oxalate, manganese-aluminum citrate, manganese-aluminum tartrate, manganese-aluminum-galactarate, manganese-aluminum-saccharate.

Chelates that can be used in the combustible products of the invention may have, for example, the composition shown in Table 1. The compounds in Table 1 correspond to the general formula I (K / Me R 7), where K represents z x y of magnesium, calcium or manganese (II) and Me is iron (III) or aluminum and R is a chelating carboxylic acid. The given values for x, y and z are in each case placed in the general formula 1 and thus the final formula is obtained as an example for said chelate.

Table I

R i y Free negative z valences

Citrate 1 2 3 3/2 "12 6 3" 13 6 3 "2 3 6 3

Tartrate 11 1 1/2 "123 3/2" 133 3/2 "2 3 1 * 2

Oxalate 12 1 1/2 "133 3/2" 11 + / 2

Glycolate 12 1 1/2 "133 3/2

Galactarate 11 1 1/2 "112 1" 123 3/2 n 133 3/2

Particularly preferred for use as chelating agents are tartaric acid, citric acid and galactaric acid.

Particularly preferred chelates are magnesium-iron-III-tartrate, magnesium-iron-III-citrate, magnesium-aluminum-tartrate, magnesium-aluminum-citrate, manganese-iron-III-galactarate, manganese-iron-III-citrate.

The chelates contained in the smoking articles of the invention may be prepared in a known manner in aqueous solution, e.g. by reacting the iron or aluminum salts of the chelating carboxylic acids in question with calcium, magnesium or manganese salts, the latter being added as hydroxides, carbonate patent 51-50 /; Hanus und Quadrat 5 58254 Z Anorg. Chem. 63, S. 31 ^ (1909) and W. Franke, Liebig Ann. Chem. 186, S. 2k8 (1931).

Combustible cellulosic substances include, for example, a cellulosic plant material, in particular tobacco, tobacco refuse such as stems, stalks or fines, pre-cooked cellulosic plant material such as hay, straw, beans or ferns, and cellulose or cellulose derivatives alone or as a mixture. As cellulose derivatives, for example, carboxymethylcellulose, hydrocaethylcellulose or methylcellulose can be used.

In addition, polymer-homologous lower molecular weight fragments of cellulose obtained from cellulose by thermal decomposition as well as cellulose derivatives prepared by chemical processes, in particular alkaline or acid oxidation, can also be added as combustible substances.

Particularly good results are obtained by using tobacco as well as paper-like webs made of tobacco waste or cellulose.

The smoking articles of the invention generally contain about 0.5 to 70% by weight of chelate based on the total weight of the combustible material used in the articles of the invention. It has proven advantageous to determine the amount of chelate from the cellulose content of the combustible material used. For example, when the proportion of cellulose in the 10% by weight of combustible material is preferably used, about 1 to 15% by weight of chelate, particularly preferably about 5 to 10% by weight of chelate, based on the total weight. When the proportion of cellulose is more than 70% by weight, 10 to 70% by weight of chelate is used in the combustible material, particularly preferably 25 to 30% by weight of chelate.

The smoking articles of the invention preferably contain a filler. By fillers is meant, under combustion conditions, tastefully inert minerals, inorganic salts and oxides, such as diatomaceous earth, silicates, mica, clay, dolomite, magnesite and chalk, or carbonates, phosphates and oxides of aluminum, iron, magnesium and calcium. Furthermore, inert fillers which decompose under combustion conditions can also be used. The release of water can be caused, on the one hand, by the high crystal water content of the filler and, on the other hand, by chemical release, e.g. from metal hydroxides. Particularly preferred fillers have been aluminum and iron hydroxides and oxyhydrates, natural silicates such as vermiculite and kaolin, precipitated silicates such as silicic acid, silica gel, silicon sol, alkaline earth and alkali metal silicates, preferably using aluminum oxyhydrates and / or silicic acid. The fillers are suitably generally added in an amount of about 1 to 70% by weight based on the total amount of combustible product, preferably about 15 to 50% by weight. In this case, it has proved particularly advantageous to add fillers in an amount of 9 to 1: 9 relative to the chelate used.

The smoking articles of the invention also preferably contain ammonia-releasing compounds under combustion conditions. Ammonium salts of inorganic acids and organic carboxylic acids as well as salts and acid amides of amino acids are used in particular as compounds releasing ammonia 6 58254 under the combustion conditions.

Among the ammonia-releasing compounds under combustion conditions, mention may be made of the inorganic acids of inorganic acids, such as carbonic acid, nitric acid, phosphoric acid and neutral ammonium salts, most preferably the airmonium salts of phosphoric acid.

Good results are also obtained with acidic and neutral ammonium salts of organic carboxylic acids with a gross carbon / oxygen ratio of 2: 1-1: 2, preferably 1: 1-1: 2. Accordingly, e.g. also ammonium salts of mono- and dicarboxylic acids derived from pentoses and hexoses, such as glucuronic acid, galacturonic acid, mannuronic acid, sugar acid and isomeric mucic acids. Ammonium tartrate and ammonium citrate are preferably used.

Particularly preferably, ammonium salts corresponding to the chelates according to the invention can be added as ammonia-releasing compounds (in which general formula I "K" means ammonium). The following ammonium chelate compounds are preferably used: Ammonium iron III glycolate, ammonium iron III oxalate, ammonium iron III citrate, ammonium iron III tartrate, ammonium iron III galactarate and ammonium iron III saccharate and ammonium aluminum glycolate, ammonium aluminum oxalate, ammonium aluminum citrate, ammonium aluminum tartrate, ammonium aluminum galactarate and ammonium aluminum saccharate.

Particularly preferred are ammonium iron III citrate, ammonium iron III tartrate and ammonium iron III galactarate, and ammonium aluminum citrate and ammonium aluminum tartrate.

It has further proved advantageous to use acid amides as ammonia-releasing compounds, for example acetamide, propionamide, succinic acid monamide and diamide, and very preferably urea. Furthermore, ammonium, magnesium or manganese II salts of amino acids can be added as ammonia-releasing agents, the amino acids preferably being glycine, serine, lysine, arginine, leucine, proline, valine, aspartic acid or glutamic acid. Magnesium and manganese glutamate are particularly preferably used as ammonia-releasing agents.

Ammonia-releasing compounds are added, for example, in amounts of 1 to 25% by weight, based on the product to be combusted, preferably 5 to 15% by weight.

It has proved expedient to dimension the amount of ammonia-releasing compounds to be increased under smoking conditions so that the acids formed during cooking are neutralized in the smoke, which can easily be checked by pH measurements in the mainstream smoke. Preferably, ammonia-releasing compounds are added in such amounts that the pH of the mainstream smoke is about 5 ~ 8, preferably 6-7.5.

The smoking articles of the invention may contain an oxidant in an amount based on the total weight of the combustible product of 0.01 to 10% by weight, preferably 1 to 5% by weight, the oxidant being understood to mean substances which improve the glow behavior of the combustible products.

As oxidizing agents, for example, salts of nitric acid, in particular alkali or alkaline earth metal nitrates, can be used. Preferred nitrates to be used are potassium and / or sodium nitrate.

It has also proved to be very particularly advantageous to use VII-manganese compounds, in particular alkali permanganates, e.g. potassium permanganate, as oxidants in the smoking products according to the invention.

The smoking articles may also contain from about 0.01 to about 10% by weight, preferably from about 0.1% to about 5% by weight, of ammonium salts of polygalacturonic acids such as pectin, alginic acid or gum arabic and / or carboxymethylcellulose from the smoking article.

Good organoleptic results are further obtained by using 0.01-5% by weight, preferably 0.1-3% by weight, based on the smoking product, of low-sulfur proteins, for example seine, hordein or gliadin, and by extraction of these proteins by alcohol, e.g. ethanol, fractional extraction. extracts. Said compounds, in addition to releasing ammonia, give smoking products a pleasant plant-like taste with a tobacco-like tinge. They can be added to smoking products over a wide range.

Preferably, about 0.1 to 50% by weight, based on the total weight of the product, of the tobacco-containing substances is added to the smoking articles. The substances contained in tobacco are those substances or groups of substances which are obtained from tobacco by known methods. The substances contained in tobacco are obtained, for example, by pressing, distillation and extraction. Preferably, the substances contained in the tobacco are obtained by extraction, in which case the extraction takes place, for example, with water or organic solvents.

The combustible material on which the smoking articles of the invention are based may be in the form of a paper-like web, sheet, film, wire or rope, whether or not cut. Paper webs, sheets, etc. can be prepared by known technical methods (cf. Ullmanns Enzyklopädie der techn. Chemie, 3. Aufl, Band 13, pages 122-130 (1962) ibid Band 17, pages 288-296 (1966).

It has proved particularly advantageous to produce the products according to the invention in the form of paper-like webs with a basis weight of 10 to 250 g / m 2, preferably 2 to 15 to 60 g / m 2 and a sheet thickness of generally 10 to 120 μm, preferably 20 to 60 μm. and particularly preferably 30-15 Jim.

The smoking articles according to the invention can be prepared, for example, in the form of a cellulose-based combustible material in the form of a paper web, sheet, film, wire or rope, cut or uncut, and the chelates used according to the invention are added as a solution, preferably in aqueous solution.

The addition can take place, for example, by immersing the combustible material in a bath formed by a solution of the chelating compounds and then drying, suitably using temperatures of about 50-120 ° C. However, the combustible material can also be sprayed or brushed with a chelate solution. Furthermore, the chelates can also be added directly to the starting mixture, from which the combustible material is formed into, for example, a paper-like web, sheet, film, wire or rope.

For example, the chelates can be added directly to a casting solution containing a combustible material. Suitably, such casting solutions may contain, in addition to any fillers, ammonia-releasing compounds, oxidizing agents and tobacco-containing substances used, about 0.1 to 20% by weight of binder.

Examples of binders which can be used are polysaccharides or their derivatives, gum arabic, starch, low-alkali carboxymethylcellulose and / or ammonium carboxymethylcellulose. If the binder is a cellulose-based combustible substance, the binder can, of course, be considered as equally effective as a combustible substance in the products according to the invention. The products according to the invention can be prepared, for example, by pouring the casting solution onto an endless strip and drying at 50-120 ° C.

For the combustible products according to the invention, paper-like webs or sheets are preferably used.

In addition to the mode of modification, the amount of chelate adhering to the film or sheet can be controlled by the structure of the film and the viscosity and concentration of the chelate solution in question. Viscosity control can be performed, e.g., by altering the concentration of the chelate solution relative to the chelate or by adding thickening agents such as, for example, low-alkali carboxymethylcellulose, hydroxyethylcellulose, pectins, acacia, alginates, galactomannan, starch and derivatives thereof. Concentrated, high viscosity solutions, for example, give a high salt content to a combustible product. _ The fillers can be mixed with the combustible material simultaneously with the chelates. However, the mixing of the fillers can also take place, either in part or in whole, in a specific process step before or after the chelation treatment. The mixing of the fillers takes place by similar technological methods as in the production of filler-containing paper-like webs, sheets or films.

Ammonia-releasing compounds can be added simultaneously with the chelates or also in a special process step before or after mixing the chelates with the combustible material. The addition takes place, for example, by spraying, dipping 955254 or brushing the combustible material with aqueous solutions of ammonia-releasing compounds and then drying.

Oxidants can be added simultaneously with the chelates both before and after mixing them with the combustible material. The addition takes place, for example, by spraying, dipping or brushing the combustible material with an aqueous, alcoholic or acetone-containing solution of the oxidant.

Ammonium salts of polygalacturonic acids as well as low-sulfur proteins or their alcoholic extracts and substances contained in tobacco may be added simultaneously with the chelates both before and after mixing with the combustible material.

In all embodiments, additives customary in tobacco processing, such as wetting agents and spices and nicotine, can still be added in the same or separate process steps.

The products according to the invention show, in comparison with the combustible material used, mixed with combustion modifiers according to the state of the art, organoleptically reduced pungency, a pleasant mild taste without astringent effect and an improved odor. For example, when the products of the invention are blended with tobacco having a cellulosic pungency, or when such tobacco is treated by the process of the invention, the aroma of such tobacco is clearly improved as the pungency is reduced. The smoking articles according to the invention have an excellent low condensation value and, in addition, have an excellent glow behavior. The smoking articles according to the invention stand out, in particular because of the smoke, which has no taste of cellulose and are thus free of organoleptically irritating ingredients.

Smoke analyzes of the smoking products according to the invention showed a significant reduction in physiologically harmful substances compared to tobacco. Thus, per cigarette containing the products of the invention, compared to a cigarette containing tobacco, it was found to have a substantially lower phenol content and a blue acid content and to obtain substantially lower condensation values. For example, the use of filler-containing cellulose films with chelates achieved a reduction of more than 90% in phenol content, about 10% in blue acid content and about 25% reduction in benzopyrene content compared to tobacco per cigarette. The amount of dry condensate could be reduced by 80-90% compared to tobacco.

The mixing of the smoking products according to the invention with the tobacco has a beneficial effect on the smoking behavior of the tobacco, in particular in that the smoke contains considerably less physiologically harmful substances than would be expected on the basis of the individual components.

By varying the chelates and additional components used, e.g., by controlling the ratio of chelating compounds to ammonia-releasing compounds, the odor and taste of smoking products can be varied. Furthermore, the tobacco-like and artificial flavor components can be largely adapted to each other. The method according to the invention thus makes it possible to vary the taste of the smoking products in the mixtures, both by means of the flavor components, whether they are synthetic or obtained from tobacco extraction, and by different tobacco grades, such as Burley, Virginia and Orient.

The use of chelates in the products according to the invention has proved to be particularly advantageous, since these compounds are generally very highly soluble in water. This makes it possible to achieve a homogeneous distribution of chelates in smoking products in a simple way in one step. Due to their low tendency to crystallize and their hygroscopic behavior, the products according to the invention are flexible and flexible and thus easy to handle. "

They have a tobacco-like feel and are comparable to natural tobacco in their formability properties, such as cutting and blending behavior.

2

By adjusting the basis weights of the carrier, for example between 15 and 60 g / m 2, the filling volume with respect to an equal amount of tobacco can be increased in a standard smoking product such as cigarette, cigar and pipe tobacco and thus a lower proportion of tobacco in tobacco blends can be achieved. This also reduces the total amount of material to be burned and eventually the amount of condensate during further combustion.

The smoking articles of the invention may be used alone or as blending components in cigarette tobacco, cigar tobacco and pipe tobacco. In addition, they can advantageously be used as cigar wrapper or layered sheets or as cigarette paper.

Examples Smoking products formed according to the following examples were made into filter cigarettes with cellulose acetate filters. The filter cigarettes were 82 mm long, 8 mm in diameter and 67 mm long. Cigarettes were smoked on average 23 mm long Nazis.

In order to characterize the filling frequency of cigarettes, their suction resistances are reported. The suction resistance was determined with an individual cigarette suction resistance measuring device, manufactured by Firma Filtrona, London. The suction resistance is expressed as pressure drop (mm H 2 O). ~

In general, filter cigarettes made from combustible products had a suction resistance of 100-125 mm H 2 O.

The amounts of condensate reported in the examples refer to dry condensate in mg / cigarette. The condensate was determined with Coresta Standard No. 10. The test cigarettes were then burned with a suction volume of 35 ml, a suction time of 2 seconds and a suction frequency of 60 seconds. The condensate formed was filtered on a Camhridge filter and weighed. The aqueous fraction was determined titrimetrically by the Karl-Fischer method and subtracted from the total condensate.

The smoking articles obtained according to the examples were evaluated for organoleptic properties as follows: 58254 a) Pungency: (++) ordinary pungency of cellulose (+) slightly pungent, especially when igniting (-) puncture hardly at all, corresponding to tobacco (...) pungency (b) Smoke flavor * (++) more concentrated, ordinary cellulose flavor, paper trolley, strongly shrinking (+) light cellulose flavor, non-shrinking (-) no cellulose flavor, slight nuisance ^ (-) mild, no taste disadvantages.

Example 1a 100 g of a paper-like film of bleached sulphate cellulose with a basis weight of 58 g / m 2 and a thickness of 60 and an ash content of 0.06 were self-sprayed with magnesium aluminum citrate, Mg 2 [Al 2 (citrate)). ], aqueous solution and dried so that the thus obtained dried film contained 20 weight chelates. The film was cut into strips of various lengths about 0.9 mm wide (cigarette butt cut) and made using commercially available cigarette paper cores with a cellulose acetate filter into cigarettes with an average suction resistance of 113 nm B 2 O.

Cigarettes showed similar glow behavior when burned without the smoking product igniting a flame. The ash was off-white and self-sustaining.

Organoleptic Reviews Pungency t (+)

Smoke battery: (-) "" Dry condensate: 7 »5 mg.

Example Ib 100 g of a paper-like film bleached with sulphate pulp

O

with a basis weight of 25 g / m 2, a thickness of 32 μm and an ash content of 0.08 fL, was sprayed with 25 aliquots of an aqueous solution of agnesia-aluminum citrate, Mg 2 [Al 2 (citrate]) and dried so that the dried film thus obtained contained 20 parts by weight. The treated film was cut into strips of various lengths about 0.9 mm wide (cigarette butt cut) and processed into cigarettes with commercially available cellulose acetate filter cartridges into cigarettes with an average suction resistance of 102 mm H 2 O. Chelate.

Cigarettes showed similar glow behavior when burned without the flammable product igniting in a flame. The ash was self-sustaining * is 58254

Organoleptic reviews Pungency: (+)

Smoke taste: (-)

Dry condensate: 5 * 0 mg.

Example le 100 g of a paper-like film cast by about 60% by weight of ground tobacco rods, 50 by weight of pressed tobacco leaf waste (fine waste and dust) and 10% by weight of ground eulfate road pulp in a known manner on a long-wire paper machine and having a basis weight was

O

70 g / m 2 and a thickness of 60 were sprayed with a solution of 25 # of agnesia-aluminum sulfate, Mg 2 [Al 2 (nitrate)] and dried so that the impregnated film contained 5% by weight of chelate. The product thus obtained was cut according to Example 1 and made into filter cigarettes with an average opening of 109 mm h 2 O.

Cigarettes showed similar annealing behavior. The main and side stream smoke was clearly rated as aromatic.

Organoleptic review:

Pungency: (-)

Smoke taste: (-)

Eondensate: 6.2 mg.

Example 2

A product corresponding to the product of Example 1a was prepared which contained magnesium citrate as an additive instead of magnesium aluminum citrate. In this case, 100 g of the paper-like film of Example 1

O

was bleached sulphate cellulose having a basis weight of 58 g / m 2, a thickness of 60 μm and an excipient containing 11.3 wt. After washing off the excess citric acid and drying, the weight gain of the film was 19 g, which corresponds to a magnesium citrate content of 22% by weight. The product thus obtained was cut according to Example 1 and made into filter cigarettes with an average opening of 102 mm HgO.

Organoleptic review:

Pungency: (++)

Smoke taste: (++)

Condensate: 9.3 mg ·

Example 3a 100 g of a paper-like film according to Example 1 was sprayed with an aqueous solution of magnesium iron III citrate, Mg 2 [Fe (citrate) 2] 2 in 13,525,429 g and dried so that the dried film contained 20 weight by weight of chelate. The product obtained in Hfi was cut into strips of about 0.9 nm in width of different lengths and made according to Example 1 into cigarettes with a suction resistance of 119 m H 2 O.

Cigarettes showed a cigarette-like incandescent behavior when burned without the combustible product igniting in a flame. The ash was brown-gray and self-sustaining.

Organoleptic Reviews Pungency t (+)

Smoke battery t (-f)

EU condensate: 4.9 mg.

Example Each 900 grams of dried and cut stalks of dry spot (Dryopteris filix-aas) were heated in a 10 liter pressure vessel with 6 liters of 9 aluminum sulphate solution for 4 hours at 109 ° C. The vegetable material thus ripened was filtered off and washed with water to a melt-free state. Today, it was fiberized in a cholester and made into a web with a long-wire paper machine with a basis weight of 68 g / a and a thickness of 60 μα. 90 g of the film thus obtained was sprayed with 10 μl of a solution of magnesium iron citrate and dried so that the chelate content of the film was 10% by weight. The product thus obtained was cut according to Example 1 and made into filter cigarettes with an average suction resistance of 120 mm HgO. The mainstream smoke of the cigarettes was mild and had a pleasant vegetable taste.

Organoleptic reviews Pungency t (-)

Smoke taste ♦ (-)

Condensates 9 * 2 mg / cigarette.

Example 3c 100 g of a paper-like film made from about 60 wt.% Of ground tobacco stalks, 30 wt. / m and a thickness of 60 was sprayed with an aqueous solution of magnesium iron III nitrate, Mg 2 [Pe (tetraate) 2] 2, and dried so that the increase in weight after drying, i.e. 9 te. a chelate content of 9 shepherd was achieved. The glow behavior of the cigarettes prepared according to Example 1 with a suction resistance of 119 nm H 2 O was uniform. The ash was brownish red and self-sustaining.

U 58254 northwest gave a light and aromatic taste roll when burned without cellulosic piety.

Organoloptic evaluation:

Pungency: (-)

Smoke battery: (-)

Condensate: 4 »4 mg / cigarette.

Example 4

The paper-like film of Example Ib was alternately immersed in saturated calcium hydroxide solution and then in 10% tartaric acid solution until, after washing and drying, the weight gain was 25.3% by weight. the film contained about 20% by weight of calcium tartrate. The well-prepared product was cut according to Example 1 (cigarette frame cutting) and made into filter cigarettes with a suction resistance of 117 ** Η ,, Ο.

The cigarettes have a stale, musty aftertaste and a clear high cellulosic pungency.

Organoloptic evaluation:

Pungency: (♦♦)

Smoke battery: (++)

Condensate: 8.4 ag / cigarette.

Example 3

The paper-like film of Example 1 was treated in an aqueous bath containing 12.6% by weight of magnesium aluminum tartrate Hgj [A14 »(tartrate)] 2, compressed between steel rollers and dried to give a weight gain of the impregnated web of 24.8%. which corresponded to a chelate-ti content of 20 wt. The recovered product was cut according to Example 1 and made into filter cigarettes with an average resistance of 113 ea HgO. The cigarettes showed a slow and steady glow behavior and formed a light self-supporting ash.

Qrganoleptic review:

Pungency: (+)

Smoke battery: (-)

Condensate: 6.8 ag / cigarette.

Example 6 100 g of a paper-like film corresponding to Example 1e was sprayed with 23 μl of a solution of manganese-iron III oxalate Mn 2 [Pe (oxalate) 2] 2 and dried so that the film thus treated contained 20% by weight of cholate. The resulting product was cut as in Example 1 and made into filter cigarettes. Suction response 123 I H ^ O. The cigarettes glowed very evenly and formed a brown Self-sustaining ash.

15 58254

Organoleptic review:

Pungency: (-)

Smoke taste: (+)

Condensates 4.2 mg / cigarette.

Example 7 100 g of the paper-like film of Example 1 were sprayed several times with a total of 250 ml of a 10 M solution of magnesium in 1-glycolate / Mg [Al (glycolate)] and dried to a chelate content of 20% by weight.

The product thus obtained was prepared as in Example 1 into filter cigarettes with a suction resistance of 122 am HgO. The cigarettes glowed evenly, forming a light white ash.

Organoleptic rating: ^ Pungency: (+)

Smoke taste: (+)

Condensate: 7 * 0 ag / cigarette.

Example 8 100 g of the paper-like film of Example 1 was sprayed with 12 aangan-iron-galactarate solution Mn 2 [Pe (galactarate) 2] 2 and dried. The film contained 15 * 5 wt.% Chelate.

The material cut according to Example 1 and made into filter cigarettes with a suction resistance of 121 aa H 2 O glowed evenly and formed gray ash.

Organoleptic review:

Pungency: (-)

Smoke taste: (+)

Condensate: 4 * 9 ag / cigarette.

Example 9

A mixture * of 50 wt% impregnated film of Example 1 and 70 wt% of an American Virginia tobacco * with a condensate of 28 ag / cigarette was made into filter cigarettes with a suction resistance of 126 am H 2 O. The flavorings and sweetness characteristic of Vlrginia tobacco were perfectly preserved in the blend when burned. The nicotine response in the airway was clearly attenuated.

Organoleptic review:

Pungency: (-)

Smoke taste: (-)

Condensate: 15 ag / cigarette.

58254 16

Example 10

Filter cigarettes with an average suction resistance of 121 mm HgO were prepared from a blend of 30 weight # films of Example 3 and 70 weight # Italian Burley tobacco with a condensate of 22 mg / cigarette. When smoked, cigarettes impart a cigar-like taste characteristic of Burley tobacco. Organoleptic review:

Pungency: (-)

Smoke taste: (-)

Condensate: 12 mg / cigarette.

Example 11

Filter cigarettes were made from a blend of 30 wt # film of Example 6 and 70 wt% of a commercially available tobacco blend »light shade (flavor type" American Blend ") * with a condensate of 13 mg / cigarette. The cigarettes had a pleasant and mild taste when smoked. Smoked ”used in the used tobacco blend, the smoke seemed to be greatly thinned. The glow behavior corresponded to the proportionality and speed of natural tobacco.

Suction response: 118 am HgO.

Organoleptic review:

Pungency: (-)

Smoke taste: (-)

Condensate: 9 * 3 mg.

Example 12

The combustible material used was tobacco »coarse" Burley "tobacco», which was characterized by a strong cigar-like tinge. This tobacco was sprayed with a solution of ammonium iron III citrate (HH 2) 2 [Fe (citrate) 2] and acidic magnesium aluminum tartrate Mg H [Al (tartrate)] in a weight ratio of 1: 1 so that the dry weight gain was 2.3% by weight, i.e. each compound was 1.23% by weight in the treated tobacco.

Compared to the starting material, the Bur-ley tobacco treated according to the invention had a reduced, but flavored, overall aromatic effect when burned. The Burley tone was completely preserved.

Review:

PietävyyB: (-)

Smoke taste: (-)

Example 13

A paper-like film with mixed (1: 1) ground tobacco stems and sulphate cellulose with a weight of four g / m 2 and a thickness of 33 yu was used as a combustible material. This material was immersed in a bath containing: 175 82 5 4 15 parts of magnesium aluminum citrate Mgj [Al (citrate), J2 6 parts of ammonium aluminum citrate (NH4) ^ [Al (citrate) g] 4 parts of aluminum hydroxide 4 parts of silicic acid 11 parts of tobacco extract And 60 parts water.

Water was compressed from the film thus obtained, and the film was dried in a stream of air at 95 ° C. This gave a weight gain of 53% by weight. From the components dissolved in the bath, the compounds were transferred to the membrane in the same concentration ratio, i.e. the membrane contained 15.6 wt .mu.m [Al (citrate) 2] 2 and 5 wt.

Compared to the product prepared without the addition of chelate, a combustible product was obtained without a size-reducing effect, it had been pungent and gave a slightly aromatic odor. When mixed with ordinary commercially available cigarette tobacco, it proved to be completely one-sided.

Review:

Pungency: (-)

Smoke taste: (-)

Examples 14-22

Addition of Chelate Complexes Cellulose Substrate As a starting material for smoking articles, paper-like films or webs are made on a paper machine with and without filler.

The films thus obtained are summarized in Table II.

j.

Table II

Film Weight per square meter Thickness Ingredients Filler $> ash annealed g / nr yum after A 45 38 Bleached - 0.07 sulphate cellulose B 16 20 ". - 0.09 C 50 52" A1 (0H) z 29 5 D 68 60 "Vermiculite- 54 ti

Films A-D were each treated in an immersion bath with an aqueous solution of the chelates together with the ammonia-releasing compound. In Examples 15, 17, 18 and 19, the bath further contained a filler and a binder. Water was squeezed out of the dipped films in a roller and the films were dried in a stream of air at 95 ° C with an endless belt.

18 58254

Table III shows Examples 14 * 22 The quality of the film used as a Tartu combustible material, the composition of the immersion bath, the addition of the dry film of the treated film (total or chelated) and the organoleptic properties and condensate content of the obtained smoking product. The amount of solids transferred to the membrane (ammonia-releasing compounds, fillers) is indicated by the weight gain, whereby the individual components are transferred to the membrane in the same weight ratio as they are present in the immersion bath. The amount of chelate transferred is given separately.

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Saiaerkki 23-23 Tobacco blends

The films of Examples 15, 16 and 18 were cut, blended into commercially available light colored cigarette tobacco and made into filter cigarettes.

Example 25

A mixture of 50% of the film of Example 15 and commercially available light colored cigarette tobacco was obtained as full-bodied, soft aroma effects without any cellulosic pungency. Due to the lower nicotine content of the total support, the reaction was impaired by inhalation of mainstream smoke.

Review:

Pungency: (-)

Smoke taste: (-)

Condensate: 15 * 6 mg Example 24

A mixture of 50 wt% film of Example 16 gave a slightly impaired aroma effect of the tobacco blend with low (-) · As for the nicotine reaction when inhaling mainstream smoke, the same effect as in Example 15 was observed.

Rating: sharpness: (-) smoke taste: (-)

Condensate: 14.1 mg Example 25

By mixing 50% by weight of the films of Example 18, the taste becomes organoleptically weaker with respect to the aroma, but the pungency is not affected by the addition. No cellulosic off-flavor was observed in mainstream or downstream smoke. The nicotine response upon inhalation of mainstream smoke was further impaired compared to Examples 25 and 24.

Rating: sharpness: (-) smoke taste: (-) ~

Condensate: 15.0 mg Examples 26-51

The films of Examples 14 * 22 were dipped according to the following Examples 26-51 into a solution of an aqueous tobacco extract containing about 50% by weight of soluble tobacco-containing substances, or sprayed with this solution so that the transferred dry matter was 50% by weight. Drying was performed with warm air at 60-100 ° C.

Example 26

A commercially available tobacco blend, flavor type "Amerl-21 58254 can Blend", was extracted with 20% of its ingredients in a cold methanol-water solution (70 v / v). This water-methanol-containing extract was further sprayed onto the smoking product prepared according to Example 17 so that the dry matter was transferred to the palno-30. The product obtained was made into filter cigarettes which, in the main stream, gave an overall aromatic impression without any pungency (Review (-)) and without a cellulose-like off-flavor (Review: (-)) by inhalation with clearly detectable nicotine reactions and the side stream was fully aromatic. The hand-made smoking product is suitable for blending in all blending ratios with tobacco grades Virginia, Burley and Orient and their blends. (Condensate: 9.8 mg).

Example 27

The film obtained according to Example 19 was treated with the same extract of tobacco-containing substances as in Example 26, so that the dry weight increase was 29% by weight. The taste of the filter cigarette product was judged to be aroma-poor and ineffective, with only pungency on ignition (Rating (-)) · The side stream smoke is aromatic and mild (Smoke rating: (-), condensate: 10.7 mg).

Example 28

The film obtained according to Example 20 was treated with the same extract of the tobacco-containing substances as in Example 26, so that the increase in dry weight was 23% by weight. Compared to Example 27, a fuller taste impression was obtained with good reactions, with no pungency (Rating: (-)) or cellulose-like off-flavor (Rating: (-)) on ignition. The smoke from the side stream is pleasantly aromatic. (Condensate: 9.0 mg).

Example 29

All the ingredients in American Virginia tobacco were completely extracted with hot water. This aqueous extract was further sprayed onto the smoking article prepared according to Example 20 to give a dry weight gain of 31,96. When these cigarettes were smoked, a genuine Virginia flavor was found which was not damaged by the film.

Rating: sharpness: (-) smoke taste: (-)

Condensate: 11.0 mg

Example 30

Italian Burley tobacco was completely extracted with cold methanol-water-Liu branch (60 vol / 40 vol).

22 5 82 5 4 This extract was further sprayed on the smoking product prepared according to Example 22 so that the weight gain was 20%. The taste impression matched the taste of a good, typical Burley tobacco and had a sweetish tinge ·. The smoking product is less pungent than the Burley tobacco used for extraction itself. The smoking product thus obtained was suitable for blending in all blending ratios with the tobacco grades Virginia, Burley and Orient and their blends.

Rating: pietäryysi (-) conversation: (-)

Probate: 11.3 mg

Example 31

The film C shown in Tsulukos II was treated with an immersion bath containing 160 g of aaonium citrate, 80 g of agesium aluminum citrate Mg 2 [Al 2 (ether)] and 280 g of the tobacco side extracts obtained by extraction of Example 19, adjusted to pH 7 with ammonia. The increase in dry weight in Cairo was then 50% and the smoking product thus obtained contained 5.1% by weight of xylate. When burning, I don't support the light, aromatic, off-flavor and pungency, it is practically compatible with the crispy impression of the gaze and the cigarette butts in all respects.

Rating: sharpness: (-) smoke: (-)

Kendenate: 9.9 mg

Example 32 To 5 parts of an aqueous solution of sodium carboxynethylcellulose / ammonium carboxymethylcellulose, 3 * 1 »aqueous solution was added: 15 parts of ground pure linters (99.8% Qf-cellulose) 15 parts of aluminum hydroxide 5 parts of alumina 2 parts of aluminum [Ps (citrate) 2] 2

The solution was rolled on a Teflon-coated metal powder using a die and dried at 130 ° C. To a Burloy blend without yielding a slight loss of aroma but no distorted aroma or pungency (-) (Condensate: 12j4 mg).

Example 33

Commercially, sara sarcus peppers were sprayed with 6 weights with a solution of nagnosium aluminum citrate Mgj [Al2 (nitrate) j] and ammonium aluminum nitrate (NE2) ^ [Al (nitrate) 2] in a ratio of 2: 1, and dried at 90 ° C. The salt intake was 9 wt. In this case, the appearance and smell of the manufactured cigarettes were improved compared to the control because the treated paper no longer had pungency or disturbing cellulose-like non-taste · Examples 34-49

Paper webs of bleached sulfate cellulose with different filler concentrations and basis weights were used as the combustible material. The composition of the starting films used as combustible material is shown in Table Γ7.

Table Y shows examples of the preparation of smoking articles by the process of the invention and the amounts of condensate formed from these articles.

Table YI shows the preparation of smoking products according to Table Y, with potassium permanganate being added as an oxidant and the amounts of condensate formed from these products.

Table IY

Film Cellulose filler Filler weight Thickness (β / · 2) / Um A Bleached sulphate- 43 * 5 wt. # 42 33 cellulose Al (0H> 3 10.2 wt.%)

SiO 2 B - "- 4416 weight # 50 62 ai (oh) 3 C -M- 40.2 weight- # 54 70 - ai (oh) 3 10.0 weight- # 8i02 - D -H- 31.1 weight - # 38 45 ai (oh) 3 12.4 weight- #

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Example 47 »

The product prepared according to Example 54 was sprayed with a 1 # solution of citrus pectin «with citrus pectin in the form of its ammonium salt» so that citrus pectin was transferred to the product 1 »3 p» ino- #.

The substance made into cigarettes showed an improved, pleasantly fresh and slightly vegetable-like smell when burned compared to the product of Example 34 with a low condensate value.

Example 47 * 30% by weight of the product of Example 47 and 70% by weight of a commercially available fine-cut tobacco blend type "american blond" were made into blended cigarettes. The taste brought by the main stream of pectin was fully compatible with the aroma of the tobacco and had a finishing effect on the aroma mixture.

Example 49

The product prepared according to Example 35 was sprayed with a 22 # solution of Selin in ~ 2 # so that the weight gain caused by the wall after drying was 1 »7 # ·

The product made into cigarettes showed improved aromatization when smoked compared to the product of Example 35 in the main and side stream smoke with the same condensate value.

Example 49

The product prepared according to Example 39 was sprayed with a 2% ethanolic solution of the wall so that the weight gain caused by the wall after drying was 1 * 5% by weight.

Compared to the product of Example 39, the product made into cigarettes showed a significant enhancement in the tobacco aroma and a finished taste with the same condensate value.

Example 30

The smoking articles of Examples 29 and 36 were blended with commercially available tobacco with a nicotine content of 0.86 μg and a condensate of 14 x 8 mg per filter tin bag according to Table VII. The table Over gives the expected and obtained condensate contents as well as the nlcotin contents for the different mixed mixtures. When calculating the expected values, the filling volume of the different mixtures was taken into account.

58254 27

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Bsimage 51 "

The film prepared according to Example 36 was sprayed with an aqueous and alcoholic solution of km / l nitrate and dried to an increase in dry weight of 1 l »·

Condensate: 3.1 mg / cigarette.

Baiaerkki 32

The film illuminated with Beiaerkin 6 was sprayed with an aqueous solution of potassium nitrate and dried so that the increase in dry weight was 2 H>.

Condensate: 2.3 mg / cigarette.

Esiaerkkl 33

The opened film of Beiaerk 38 was sprayed with an aqueous solution of potassium nitrate and dried so that the increase in dry weight was 2

Condensate: 3.2 ag / ghost.

Baiaerkki 34

The combustible material in the austerity of the paper web, which was bleached sulphate cellulose containing 43% by weight of aluminum hydroxide as a filler and having a basis weight of 30 g / a and a thickness of 38 [mu] m, was treated in an immersion bath containing 10 parts per liter of aang Fe (nitrate) 2] 2 6 parts of aaaonium iron citrate (HH ^) ^ [Fe (nitrate) 2] 3 parts of urea 12 parts of tobacco or substances obtained completely from Burley tobacco by hot water extraction with 100 parts of water so that by drying At a uniformly rising temperature of 55-95 ° C, an increase in dry weight of 34 is obtained. The smoking product thus obtained contained 7.6 wt% chelate. It was made into filter cigarettes. From the organoleptic stage, the product was judged to be tastefully neutral by a clear tobacco-active Tolmin.

Condensate: 3.1 mg / cigarette.

Baiaerkki 33

A combustible material, such as in Example 34, formed by a film of bleached sulfate cellulose containing 43 wt% aluminum hydroxide as a filler and pretreated with 2 l of aqueous potassium permanganate solution, was treated in an immersion bath containing, parts of manganese ] 2 8 parts of magnesium aluminum citrate Ng ^ [Al (citrate) 2J2 6 parts of ammonium iron galactarate MH ^ [Fe (galactarate)] 6 parts of urea 12 parts of tobacco (obtained according to Example 29) 100 parts of water f '29 S8254 so that after drying At 55-95 ° C * at a steadily rising temperature, an increase in dry weight of 41 £ was obtained. The well-obtained smoking Luoto contained 1,4,4 palno-chelate. It was made into filter cigarettes. The product was judged organoleptically to be particularly mild and tobacco-like.

Condensate: 2.8 mg / cigarette.

The product obtained according to this example was particularly well compatible with commercially available light-colored tobacco blends.

Claims (5)

3 ° 58254 A smoking article which is a cellulose-based combustible substance and which optionally contains fillers and / or ammonia-releasing compounds and / or oxidants and / or polygalacturonic acids and / or proteins and / or tobacco extracts, characterized in that it contains chelating compounds having: is the general formula IK Me RI zxy wherein K is magnesium, calcium or manganese (IIMe is trivalent iron or aluminum and R is a chelating organic carboxylic acid residue having 2 to 8 carbon atoms having at least one hydroxyl group in addition to the carboxyl group, a keto group or other carboxyl groups, x = 1 or 2 and y = 1, 2, 3 or 1 and z is a number indicating the number K of divalent cations, the chelate content of the smoking preparation being 0.5 to 70% by weight of the amount of combustible material. Smoking preparation according to Claim 1, characterized in that tartaric acid, citric acid or galactaric acid is used as the chelating carboxylic acid. Smoking preparation according to Claims 1 and 2, characterized in that the product contains magnesium-iron-III-citrate, magnesium-iron-III-tartrate, magnesium-aluminum-citrate, magnesium-aluminum-tartrate, manganese-iron-III-citrate as chelate. citrate or manganese iron III galactarate. U. A smoking preparation according to claims 1-3, characterized in that the product contains about 5-50 weight-chelating compounds, based on the total weight of the combustible substance. A process for preparing a smoking article according to claims 1 to 3, characterized in that a) a cellulose-based combustible substance and b) chelating compounds and c) optionally fillers, ammonia donors, oxidants, polygalacturonic acids, proteins, and / or tobacco extract are combined, wherein a), b) and optionally one or more of the substances of c) are mixed into an aqueous mixture to form a paper-like web 2 having a basis weight of 10-250 g / m 2 and a thickness of 10-120 μm after drying, or a dry carrier for said a) for a substance having a basis weight of 10,000 g / m 2 and a thickness of 10 to 120 pn, a solution containing the substance mentioned in b) and optionally one or more of the substances mentioned in e) is applied by brushing, spraying or immersion in a bath.