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Publication numberUS3608560 A
Publication typeGrant
Publication dateSep 28, 1971
Filing dateNov 7, 1968
Priority dateNov 7, 1968
Publication numberUS 3608560 A, US 3608560A, US-A-3608560, US3608560 A, US3608560A
InventorsBriskin Theodore S, Ward Geoffrey R
Original AssigneeSutton Res Corp
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Smokable product of oxidized cellulosic material
US 3608560 A
Abstract  available in
Previous page
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Claims  available in
Description  (OCR text may contain errors)

nited States Patent Inventors Theodore S. Briskln;

Geofirey R. Ward, both of Beverly Hills, Calif.

Nov. 7, 1968 Sept. 28, 1971 Sutton Research Corporatlon Los Angeles, Calif.

Continuation-impart of application Ser. No. 595,622, Nov. 21, 1966, Pat. No. 3,447,539, Continuation-impart of appllcation Ser. No. 674,994, Oct. 12, 1967, now abandoned.

Appl. No. Filed Patented Assignee SMOKABLE PRODUCT 0F OXllDlZED CELLULOSlC MATERIAL 5 Claims, No Drawings 11.5. C1 1131/2, 131/17,131/140 Int. Cl. A241) 15/00,

- A24d 01/18 Field ofSearch 131/2,15, 17, 140-144; 260/212 References Cited UNITED STATES PATENTS 2,536,285 1/1951 Heckel et a1 8/116 Primary Examiner-Melvin D. Rein Attorney-McDougall, Hersh, Scott& Ladd ABSTRACT: A smokable product of oxidized cellulosic material formulated to include combustible carbon in an amount within the range of 2-50 percent by weight of the oxidized cellulosic material for the improvement in the smoking characteristics of the smoking product forward thereof. The combustible carbon particles are of approximate colloidal dimensions and increase the heat of combustion of the oxycellulose. Melting of the oxycellulose is minimized with the carbon additive. Further, the carbon particles may carry a volatile additive absorbent thereon and function as a filtration means downstream from the combustion area. The carbon particles may be secured to the oxycellulose by means of a soluble carbohydrate binder.

SMOIKABLE PRODUCT F OXIDllZED CELLULOSllC MATERIAL This is a continuation-in-part of our copending applications U.S. Pat. Ser. No. 595,622, filed Nov. 21, 1966, now U.S. Pat. No. 3,447.539 and entitled Smoking Products, and US, Pat. Ser. No. 674,994, now abandoned, filed Oct. 12, 1967, and entitled Smoking Products and Process for Making Such Products.

This invention relates to a smokable product produced of oxidized cellulosic materials and to smoking products produced thereof.

As used herein, the term smokable products is meant to refer to and include filler material for use in cigarettes, cigars, pipe tobacco and the like, cigarette papers, wrappers and the like used in the preparation of cigars and cigarettes.

in the aforementioned copending applications, description is made of the preparation of a smokable product suitable for use in cigars and cigarettes and pipes wherein the smokable product is prepared of relatively pure cellulosic materials subjected to selective oxidization with liquid nitrogen dioxide to convert preferably more than 90 percent of the methylol groups in the cellulosic molecule to yield a product which can be referred to as oxycellulose. The oxidation reaction produced is further processed by removal of nitrogen oxides by vaporization and washing and by extraction with an organic solvent to remove undesirable impurities, such as oils, waxes, latexes, and aromatics which have been released as a consequence of the treatment with nitrogen dioxide.

As further described in the aforementioned copending applications, the oxidized and cleansed oxycellulose is further processed by a reduction reaction with borohydride of an alkali or alkaline earth metal, such as sodium borohydride, for reduction of nitro compounds, quinones, ketones and aldehydes which otherwise might have a tendency to impart undesirable aroma and taste to the smoking product when burned, or to reduce stability thereof during storage.

The product, before or after reduction, can be subjected to additional oxidation with a dilute solution of peroxide to eliminate further groupings that contribute undesirable aroma or taste to the product. The need for such treatments naturally varies with the initial purity of the oxycellulose.

The refined oxycellulose is then formulated with mineralizing agents, such as oxalates, glycolates, diglycolates, lactates, pivatates or tannates of the alkaline earth metals, preferably in a manner to form such salts internally of the oxycellulose fibrils. As described, internal formation can be achieved by first forming the alkaline earth metal salt of the oxycellulose and then treating with a solution of the anion to precipitate the mineralizing salt in situ in the cellulosic material.

The treated oxycellulose can be further formulated to improve burning, glow and smoking characteristics by the use of potassium, rubidium or cesium salts, such as the oxalates as described in the aforementioned copending applications and in the copending application U.S. Pat. Ser. No. 623,528, filed Mar. 16, 1967, and entitled Smoking Products and Process for their Manufacture.

Smoke generators for improving the appearance of the smoke from the product can be introduced, as by the use of fatty acids and the like, and suitable aroma can be achieved by the addition of volatilizable alkalizing material, such as ammonium oxalate, urea and the like.

It has been found that oxidized cellulosic material does not burn as vigorously as tobacco with the result that the smoka ble product often times experiences difficulty in maintaining full combustion. Such less vigorous burning may also tend to lend to thermal decomposition instead of combustion of the carbonaceous components with corresponding increase in tars and the like materials sought to be eliminated by the smokable product of this invention.

There is reason to believe that the deviation in combustion is attributable, at least in part, to the lower heat of combustion of oxidized cellulosic materials, as compared to cellulose or tobacco. The heat of combustion of cellulose is calculated to be about 4.2 kilocalories per gram, whereas the heat of combustion of fully oxidized cellulose is calculated to be about 3.2 kilocalories per gram.

Attempts have been made to increase the heat of combustion of the smoking product by decrease in the proportion of oxidized cellulosic material employed but the result has been the generation of undesirable oxygenated short chain materials which contribute undesirable odor and irritating taste during combustion.

Thus, it is an object of this invention to produce and to provide a method for producing a smokable product of oxidized cellulosic material which enjoy desirable vigorous burning characteristics during combustion whereby the smokable product is capable of the desired rate of combustion without generation of undesirable taste and odors, and it is a related object to produce and to provide a method for producing a smokable product of the type described which has improved characteristics for use as a smoking product from the standpoint of taste, odor and appearance as well as reduction in the amount of undesirable compounds released with the fumes and smoke inhaled from the smoking product.

We have found that the burning characteristics of the oxidized cellulosic material can be markedly improved and that the use of the oxidized cellulosic material, as a smokable product, is also improved by the formulation to include a substantial amount of combustible carbon in uniform distribution with the oxidized cellulosic material and preferably bonded thereto in the form of fine particles or powders of almost colloidal dimension. Benefits are derived when the carbon is present in the smokable product in an amount as little as 2 percent by weight of the oxidized cellulose up to an amount as great as 50 percent by weight of the oxidized cellulosic material. When an amount less than 2 percent by weight is employed, the carbon has negligible effect and when the carbon content exceeds the upper limit of 50 percent by weight of the oxidized cellulosic material, the carbon has deleterious effect in that it tends to muffle the combustion of the oxidized cellulose, with corresponding generation of the undesirable odor and taste. In the preferred practice of this invention, combustible carbon is employed in an amount within the range of 15-40 percent by weight of the oxidized cellulosic material.

As the combustible carbon, it is preferred to make use of various forms of activated carbon charcoal, burnt cork and the like, in finely divided or powder form or other forms of combustible carbon, preferably of the absorbent type, as used in the absorption of gases, liquids, vapors or fumes.

It will be recognized that such replacement of substantial amounts of oxidized cellulose with the carbon will operate proportionately to reduce the concentration of oxidized cellulosic material making up the smokable product, with corresponding reduction in volatile organics, such as aldehydes, acids, phenols, polycyclies and tars often generated during combustion of the oxidized cellulosic material. This, of course, constitutes a benefit derived from the presence of carbon over and above its beneficial effect on combustion or burning rate of the smokable product.

The presence of carbon in the smoking product presents a number of other beneficial effects, some of which were wholly unexpected. For example, carbon present within the amounts described contribute color to the smokable product thereby to increase its aesthetic value as well as ability to blend the smokable material with tobacco to provide a mixture characterized by reduced volatilizable byproducts from tobacco.

Most significant is the fact that the carbon particles are capable of functioning as absorbents to enable pretreatment with liquids desired to be formulated into the smoking product and to achieve uniform distribution of such liquids with the treated carbon particles. The latter operate to retain such liquids in the desired distribution in the smoking product for their most beneficial use. Thus, the carbon particles serve as a means for uniformly distributing small amounts of liquid ingredients and for retaining such liquids in unifonn distribution throughout the smokable product.

Still more significant and somewhat surprising is the ability of the carbon particles, uniformly distributed throughout the smoking product, to extract volatile organic components from the smoke and fumes and to withhold such absorbed materials while even in the hot zone generated during combustion of the smoking product. Thus, extra pyrolysis is required with more complete combustion of the absorbed volatiles with the result that less of the organic volatiles are released during combustion of the smoking product. While in the nonburning portion of the smoking product, the carbon particles function as a filter which removes and holds volatile vapors and fumes otherwise inhaled.

Another surprising result of the presence of carbon is that it helps to stop the undesirable tendency of oxycellulose to melt and coalesce during its pyrolysis and then produce bad odors. In this respect, carbon acts like calcium oxalate and, to some extent, substitutes for inorganic minerals. This allows a less coherent ash to be formulated.

The carbon particles may be formulated into the cellulose system in various ways. If the carbon particles are pasted with oxidized cellulose fibers, much of the carbon will absorb or adhere, depending upon the amount of swelling and stickiness of the fibers, which depends further upon the temperature and pH of the paste. instead, the cellulosic fibers may be impregnated with an aqueous dispersion of the carbon particles containing a binder component, such as a small amount of soluble polyuronic acid obtained by boiling oxidized cellulose in water, pectin, demethylated pectin, and the like carbohydrate binder materials.

Having described the basic concepts of this invention, illustration will now be made of the practice of the invention by reference to the following example, which is given by way of illustration and not by way of limitation.

EXAMPLE I A low ash, low lignin, high purity paper is oxidized by immersion in liquid NO at 20 C. for 5 or 6 days until caustic soda titrations show that the carboxyl content has reached an asymptotic level, which can be taken as indicating close to 100 percent conversion of the methylol groups. The paper is then removed and the N0 volatilized off by drying. The paper is then rinsed and treated with a 1 percent suspension of calcium carbonate, containing an amount of calcium sufficient when absorbed in the oxidized cellulose to give an ash level of percent to the dried product. The absorption of the calcium becomes substantially complete in -30 minutes and the material is then removed, rinsed and immersed in a 1 percent solution of oxalic acid of sufficient volume to form the oxalate of the calcium in the oxidized cellulose. After 2030 minutes, the material is removed, rinsed to remove excess acids, and passed through a wringer to remove free water. While the fibers are still swollen, the material is pasted with an aqueous slurry containing 50 percent of finely powdered activated charcoal. By using a quantity of charcoal about half that of the dry fibers, a mixture of about 35 percent charcoal 65 percent oxidized cellulose can be prepared. The slurry is formulated to contain 1 percent by weight low methoxyl pectin for adhesion and the moist pasted fibers are then dried in a stream of warm air at 50 C. To obtain a good rate of burning, 1 percent of rubidium or cesium oxalate is incorporated in the oxidized cellulose and carbon mixture. Approximately 0.5 percent of ammonium oxalate is also added, to give an alkaline smoke such that moist pH paper held in the smoke indicates a pH of 8 to 9.

By way of modification, the mineralizing or ashing ingredient in the form of calcium oxalate, can be incorporated into the eellulosic material before oxidation with liquid nitrogen dioxide. In such event, the steps of treating the oxidized cellulose with calcium carbonate and oxalic acid can be dispensed with in the above example. It is desirable to make use of such mineralizing agents as calcium, magnesium, or the like alkaline earth metal oxalates in an amount within the range of 5-40 percent by weight of the smokable product or in an amount to give 5 25 percent ash in the smoked product.

Instead oflignm, in example I, use can be made of other cellulosic materials, such as purified cellulose pulp or paper, alpha-cellulose, wood pulp, flax, hemp, straw and cellulose components derived from plants, leaves, weeds and the like.

Oxidized cellulose, formulated in the manner described, and which include suitable ash, burning accelerators and smoke modifiers, can be used alone as a smoking product, or it can be used as a diluent with tobacco for the manufacture of cigarettes with reduced tars and improved smoking characteristics.

It will be understood that changes may be made in the details of formulation and operation, without departing from the spirit of the invention, especially as defined in the following claims.

We claim:

1. A substitute smoking product adapted to be employed as combustible filler either alone or in combination with tobacco, said product being a mixture consisting essentially of an oxidized cellulose material and an incorporation of fine, absorbent combustible carbon particles approximating colloidal dimensions, said combustible carbon particles being within the range of 2-50 percent by weight of the oxidized cellulose, said combustible carbon particles functioning during combustion of the mixture in smoking to increase the heat of combustion of the oxycellulose and preclude the melting thereof, act as an absorbent for introducing a volatile additive and/or for smoke filtration downstream from the zone of combustion.

2. A substitute smokable product as claimed in claim 1 in which the combustible carbon is present in an amount with the range of 15-40 percent by weight of the oxidized cellulosic material.

3. A substitute smokable product as claimed in claim 1 in which the carbon particles are bonded to the oxidized cellulosic material with a soluble carbohydrate.

4. The substitute smoking product of claim 1 in which the oxidized cellulose is stabilized by removal of the excess nitrogen dioxide subsequent to the oxidation of the cellulose.

5. The substitute smoking product of claim 1 in which the carbon particles are adhered to the oxycellulose by coating a suspension of the said particles in a water soluble binder onto the oxycellulose and then drying same.

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US7001 *Jan 8, 1850 Improvement in curing tobacco-stems
US2114281 *May 15, 1936Apr 19, 1938Raymond P AllenTobacco and process of treating same
US2536285 *Jul 25, 1946Jan 2, 1951Champion Paper & Fibre CoProcess of making high wet strength paper
US2809904 *Nov 17, 1954Oct 15, 1957Raymar CompanySmoking product
US2915069 *Jul 13, 1954Dec 1, 1959Olin MathiesonSmoking device
US3007917 *Apr 2, 1954Nov 7, 1961Leon SimonProduction of oxycellulose material
US3012915 *Nov 21, 1957Dec 12, 1961Minerals & Chem Philipp CorpTobacco composition including comminuted solid material affixed thereto
US3106210 *Oct 8, 1958Oct 8, 1963Reynolds Metals CoSmoking tobacco
US3364200 *May 19, 1965Jan 16, 1968Johnson & JohnsonOxidized cellulose product and method for preparing the same
CA702918A *Feb 2, 1965Celanese CorpTobacco substitute
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US3729009 *Mar 22, 1971Apr 24, 1973Kimberly Clark CoSmoking product with improved flavor and method of making it
US3805803 *May 24, 1972Apr 23, 1974Brown & Williamson TobaccoReconstituted-tobacco smoking materials
US3818915 *Mar 18, 1971Jun 25, 1974Ici LtdTobacco substitute smoking material
US3885574 *Mar 18, 1971May 27, 1975Ici LtdSmoking mixture
US3934594 *Aug 1, 1974Jan 27, 1976Tamag Basel AgProcess for the manufacture of tobacco substitute
US3943942 *Jun 21, 1974Mar 16, 1976Imperial Chemical Industries LimitedSmoking mixtures
US3957060 *Nov 23, 1971May 18, 1976Brown & Williamson Tobacco CorporationTobacco treatment
US3987800 *Jul 2, 1974Oct 26, 1976Tamag Basel AgSmokable product with meerschaum particles
US3987801 *Jul 2, 1974Oct 26, 1976Tamag Basel AgSmokeable product with meerschaum particles as absorbents
US3993082 *May 5, 1975Nov 23, 1976Olin CorporationTobacco substitute
US4014348 *Jun 9, 1975Mar 29, 1977Imperial Chemical Industries LimitedSmoking mixture
US4019520 *Nov 25, 1974Apr 26, 1977Brown & Williamson Tobacco CorporationTobacco substitute containing boric oxide, boron oxyacids, and ammonium, alkali metal, or alkaline earth metal salts of boron oxyacids
US4505282 *May 10, 1983Mar 19, 1985American Brands, Inc.Innerliner wrap for smoking articles
US4793365 *Sep 14, 1984Dec 27, 1988R. J. Reynolds Tobacco CompanySmoking article
US4893639 *Jul 22, 1986Jan 16, 1990R. J. Reynolds Tobacco CompanyDensified particulate materials for smoking products and process for preparing the same
US4920990 *Nov 23, 1988May 1, 1990R. J. Reynolds Tobacco CompanyCigarette
US4942888 *Jan 18, 1989Jul 24, 1990R. J. Reynolds Tobacco CompanyCigarette
US4966171 *Jan 27, 1989Oct 30, 1990Philip Morris IncorporatedSmoking article
US4981522 *Jul 22, 1988Jan 1, 1991Philip Morris IncorporatedThermally releasable flavor source for smoking articles
US4991606 *Jul 22, 1988Feb 12, 1991Philip Morris IncorporatedSmoking article
US5060676 *Oct 26, 1987Oct 29, 1991Philip Morris IncorporatedProcess for making a carbon heat source and smoking article including the heat source and a flavor generator
US5074321 *Sep 29, 1989Dec 24, 1991R. J. Reynolds Tobacco CompanyCigarette
US5076292 *Aug 24, 1987Dec 31, 1991R. J. Reynolds Tobacco CompanySmoking article
US5076297 *Mar 14, 1986Dec 31, 1991R. J. Reynolds Tobacco CompanyMethod for preparing carbon fuel for smoking articles and product produced thereby
US5092353 *Jun 26, 1990Mar 3, 1992R. J. Reynolds Tobacco CompanyCigarette
US5101839 *Aug 15, 1990Apr 7, 1992R. J. Reynolds Tobacco CompanyCigarette and smokable filler material therefor
US5105836 *Aug 15, 1990Apr 21, 1992R. J. Reynolds Tobacco CompanyCigarette and smokable filler material therefor
US5129408 *Aug 15, 1990Jul 14, 1992R. J. Reynolds Tobacco CompanyCigarette and smokable filler material therefor
US5144967 *Oct 22, 1990Sep 8, 1992Kimberly-Clark CorporationFlavor release material
US5284166 *Oct 7, 1992Feb 8, 1994Kimberly-Clark CorporationMethod of producing brown cigarette wrapper paper
US5345951 *Aug 12, 1992Sep 13, 1994Philip Morris IncorporatedSmoking article
US5369723 *Sep 11, 1992Nov 29, 1994Philip Morris IncorporatedTobacco flavor unit for electrical smoking article comprising fibrous mat
US5388594 *Sep 10, 1993Feb 14, 1995Philip Morris IncorporatedElectrical smoking system for delivering flavors and method for making same
US5396911 *Nov 27, 1991Mar 14, 1995R. J. Reynolds Tobacco CompanySubstrate material for smoking articles
US5415186 *Apr 16, 1993May 16, 1995R. J. Reynolds Tobacco CompanySubstrates material for smoking articles
US5443560 *Dec 14, 1992Aug 22, 1995Philip Morris IncorporatedChemical heat source comprising metal nitride, metal oxide and carbon
US5505214 *Sep 11, 1992Apr 9, 1996Philip Morris IncorporatedElectrical smoking article and method for making same
US5573692 *Sep 28, 1994Nov 12, 1996Philip Morris IncorporatedPlatinum heater for electrical smoking article having ohmic contact
US5598868 *Nov 30, 1994Feb 4, 1997R. J. Reynolds Tobacco CompanyCigarette and smokable filler material therefor material for use in smoking articles
US5613504 *May 24, 1995Mar 25, 1997Philip Morris IncorporatedFlavor generating article and method for making same
US5649554 *Oct 16, 1995Jul 22, 1997Philip Morris IncorporatedElectrical lighter with a rotatable tobacco supply
US5665262 *Jan 9, 1995Sep 9, 1997Philip Morris IncorporatedTubular heater for use in an electrical smoking article
US5666976 *Jun 7, 1995Sep 16, 1997Philip Morris IncorporatedCigarette and method of manufacturing cigarette for electrical smoking system
US5666978 *Jan 30, 1995Sep 16, 1997Philip Morris IncorporatedElectrical smoking system for delivering flavors and method for making same
US5692291 *May 25, 1995Dec 2, 1997Philip Morris IncorporatedMethod of manufacturing an electrical heater
US5692525 *Apr 20, 1995Dec 2, 1997Philip Morris IncorporatedCigarette for electrical smoking system
US5708258 *May 25, 1995Jan 13, 1998Philip Morris IncorporatedElectrical smoking system
US5730158 *May 24, 1995Mar 24, 1998Philip Morris IncorporatedHeater element of an electrical smoking article and method for making same
US5750964 *Jan 29, 1997May 12, 1998Philip Morris IncorporatedElectrical heater of an electrical smoking system
US5816263 *Dec 31, 1996Oct 6, 1998Counts; Mary EllenCigarette for electrical smoking system
US5865185 *May 24, 1995Feb 2, 1999Philip Morris IncorporatedFlavor generating article
US5915387 *Dec 31, 1996Jun 29, 1999Philip Morris IncorporatedCigarette for electrical smoking system
US6026820 *Sep 12, 1997Feb 22, 2000Philip Morris IncorporatedCigarette for electrical smoking system
US8402976Apr 17, 2009Mar 26, 2013Philip Morris Usa Inc.Electrically heated smoking system
US8794231Apr 29, 2009Aug 5, 2014Philip Morris Usa Inc.Electrically heated smoking system having a liquid storage portion
US8851081Mar 15, 2013Oct 7, 2014Philip Morris Usa Inc.Electrically heated smoking system
US8997753Jan 31, 2013Apr 7, 2015Altria Client Services Inc.Electronic smoking article
US8997754Jan 31, 2013Apr 7, 2015Altria Client Services Inc.Electronic cigarette
US9004073Jan 31, 2013Apr 14, 2015Altria Client Services Inc.Electronic cigarette
US9084440Nov 26, 2010Jul 21, 2015Philip Morris Usa Inc.Electrically heated smoking system with internal or external heater
WO1994006313A1 *Sep 10, 1993Mar 31, 1994Philip Morris ProdTobacco flavor unit for electrical smoking articles
U.S. Classification131/359
International ClassificationA24B15/16, A24B15/00
Cooperative ClassificationA24B15/165
European ClassificationA24B15/16K
Legal Events
May 19, 1981ASAssignment
Effective date: 19810306
Effective date: 19810220