US3880172A - Smoking mixtures - Google Patents

Smoking mixtures Download PDF

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Publication number
US3880172A
US3880172A US332112A US33211273A US3880172A US 3880172 A US3880172 A US 3880172A US 332112 A US332112 A US 332112A US 33211273 A US33211273 A US 33211273A US 3880172 A US3880172 A US 3880172A
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Prior art keywords
tobacco
smoking
percent
weight
parts
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Expired - Lifetime
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US332112A
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English (en)
Inventor
Robert Craig Anderson
John Cormack Lovie
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Imperial Group PLC
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Imperial Chemical Industries Ltd
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Assigned to IMPERIAL GROUP PLC, A COMPANY OF UNITED KINGDOM reassignment IMPERIAL GROUP PLC, A COMPANY OF UNITED KINGDOM ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: IMPERIAL CHEMICAL INDUSTRIES PLC
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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes
    • A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes

Definitions

  • ABSTRACT A smoking mixture comprising a tobacco-substitute in admixture with extract material obtained by treating Nicotiana Rustica with a nicotine-dissolving solvent.
  • tobacco substitutes can be mixed with the dried and cured leaves from the plant genus Nicotiana Rustica.
  • This genus contains very high proportions of nicotine, for example up to 14 percent by weight and unlike Nicotiana Tobaccum it has not proved generally acceptable as the basis of smoking materials owing to the extremely strong and unpalatable flavour of its smoke. Small proportions may be tolerated however in admixture with tobacco substitutes which themselves produce a neutral smoke and in this way it may be possible to produce mixtures with less health hazard than palatably similar mixtures containing tobacco. It is desirable, however, to reduce the health hazard from smoking as far as possible and for this reason the amount of tobacco or other nicotine-containing plant genus in smoking mixtures should be minimised or reduced to zero if possible.
  • a smoking mixture comprises a tobacco-substitute in admixture with extract material obtained by treating Nicotiana Rustica with a nicotine-dissolving solvent.
  • tobacco substitute means any solid substance which, though not of tobacco origin can be smoked in the same way as tobacco.
  • tobacco substitutes may be for example of carbohydrate origin, e.g., those described in British Pat. Nos. 1,055,473 and 1,143,500 and U.S. Pat. No. 3,106,209 namely cellulose, oxidised cellulose and lettuce leaves. Cellulose ethers may also be used.
  • the tobacco-substitute may be a thermally degraded carbohydrate, made for example by subjecting carbohydrate (particularly cellulose) to a catalysed degradation process at above 100 (e.g., 100 to 250C as in our UK Pat. No. 1,113,979) until the weight of degraded carbohydrate is less than 90 percent of the weight of the original carbohydrate.
  • carbohydrate particularly cellulose
  • a catalysed degradation process at above 100 (e.g., 100 to 250C as in our UK Pat. No. 1,113,979) until the weight of degraded carbohydrate is less than 90 percent of the weight of the original carbohydrate.
  • a similar substance is obtainable as described in our British Pat. No. 1,289,354 by acid or base catalysed condensation of a compound of the formula RCOCH CH COR wherein R and R which may be the same or different,
  • Nicotine-dissolving solvents which may be used for extracting the Nicotiana Rustica are more particularly lower aliphatic alcohols having boiling points up to C. Specific examples are methanol, ethanol, npropanol, isopropanol, n-butanol, iso-butanol and butanol. 1
  • the extraction may be carried out by known techniques, for example by the use of apparatus of the Soxhlet type, but it is preferable to employ a hot extraction technique, for example, by filling a permeable bag with dried and crushed Nicotiana Rustica, suspending this in vapour from boiling solvent and allowing condensed solvent from a reflux condenser to pass into and downwardly tnrough the bag and its contents.
  • a hot extraction technique for example, by filling a permeable bag with dried and crushed Nicotiana Rustica, suspending this in vapour from boiling solvent and allowing condensed solvent from a reflux condenser to pass into and downwardly tnrough the bag and its contents.
  • the amount of extract material in the smoking mixtures of the invention may be, for example from 1 to 25 percent by weight of the amount of the tobacco substitute, but for best flavour effect the preferred amount is from .4 to 9 percent.
  • Smoking mixtures of the invention may be made by mixing of the tobacco substitute and the extract material in any convenient manner.
  • Other known ingredients of smoking mixtures may be included to impart desired physical properties and burning characteristics.
  • the smoking mixtures may incorporate glow-controlling catalysts, materials to improve ash coherence and colour, nicotine, other flavourants, medicaments, humectants or film-forming agents. If desired tobacco may also be incorporated.
  • the smoking mixtures of the invention are fabricated in sheet form, containing a film forming agent, for example a natural gum or pectin or a cellulose ether, especially carboxymethyl cellulose or a salt thereof.
  • a film forming agent for example a natural gum or pectin or a cellulose ether, especially carboxymethyl cellulose or a salt thereof.
  • the ingredients of the mixture preferably with the tobacco substitute in a finely dividedform, may be mixed with a sufficient quantity of water to produce a slurry which is then cast on to a surface and dried.
  • Sheet material produced from the slurry may be shredded to provide material in a form suitable for smoking.
  • tobacco When tobacco is incorporated in the smoking mixture it may be as comminuted tobacco, which may be incorporated in the slurry before casting. Alternatively tobacco shred may be blended with the shredded sheet.
  • the smoking mixtures of the invention give palatably acceptable smokes and are generally preferred by smokers to comparable mixtures which do not contain any of the extract material obtained by treating Nicotiana'Rustica with a nicotine-dissolving solvent.
  • a preferred smoking mixture comprises a mixture of a tobacco substitute with from 1 to 11 percent (especially 4 to 9 percent) of its weight of extract material obtained by treating Nicotinia Rustica with a nicotine-dissolving solvent, said mixture being blended with from 65 to 90 percent of its weight of tobacco, particularly flue-cured Virginia tobacco.
  • a solution of the extract material preferably in an alcoholic solvent, may be contacted with a sorbent solid to absorb thereupon most of the nicotine, and thereafter nicotine may be recovered from the said solid and flavourants from the liquid phase.
  • the extract may be contacted with sorbent solid by mixing followed by filtration, or by allowing it to flow through a packed column of the solid already moistened with liquid in the technique already familiar in the fields of chromatography or ion-exchange.
  • Specific solids which may be used are absorbent solids which, when mixed with water to form a 1 percent suspension, give a liquor of pH 2.5 to 6.5. More particularly acid clays and cation exchange resins are of value.
  • acid clays which may be used are activated bentonites and montmorillonites. Fulmont 300C, an activated acid clay is of especial value. This substance, when mixed with water to form a l percent suspension, gives a liquor of pH 6.4.
  • cation exchange resins which may be used are those commercially available under the names Z'eo-carb K225 (H) and Amberlite IRC 50H.
  • the treatment with sorbent solid is carried out so as to leave at least 50 percent by weight of the extracted material in the solution.
  • the amount of solid, and the time and temperature of the treatment necessary to achieve this will of course depend upon the particular solid chosen, and the type of treatment used, i.e., whether the extract is stirred with the solid or allowed to flow through a column of solid.
  • the resultant flavourant-rich material in the solution may be used directly to flavour tobacco substitutes to produce smokes which are substantially without the harsh off-notes produced by flavouring in similar manner with the untreated extract material from Nicotiana Rustica according to particular commerical requirements or even individual tastes.
  • Other flavour producing ingredients may be present as desired, including tobacco.
  • Nicotine and other basic material absorbed by the solid can be recovered from it by known techniques, for example by elution with a solvent (sometimes a more powerful solvent than that present in the original extract) or by steam distillation from the solid after basification e.g. with sodium hydroxide.
  • a solvent sometimes a more powerful solvent than that present in the original extract
  • steam distillation from the solid after basification e.g. with sodium hydroxide.
  • Nicotine-rich material recovered in this way may be used to fortify tobacco or tobacco substitutes and if desired may be incorporated therewith together with flavourants or flavourant-rich material also obtained from Nicotiana Rustica in the above described manner.
  • 1,299,296 tobacco substitutes of acceptable burning rates containing large amounts of filler 13862/70 tobacco substitute containing protein 13861/70 tobacco substitutes containing protein and isoprenoid 13865/70 tobacco substitute containing protein and phenylethylalcohol or phenylacetic acid.
  • the first procedure used a group of smokers especially selected for their high consistent flavour sensitivity and long experience in testing the flavour of tobacco cigarettes.
  • This group called the Expert Panel, consisted of a small number of the order of 3-6 people.
  • the second procedure required a much larger number of panel assessments (minimum number 22; minimum panel size 1 l) and measured a preference for one cigarette against another.
  • the method was devised on a statistical basis such that the certainty that a preference existed could be stated as a percentage confidence. This panel was called the Statistical Preference Panel.
  • EXAMPLE 1 2.8 parts of glycerol, 0.8 parts of citric acid and 1 part of potassium citrate were dissolved in 20 parts distilled water and the resultant solution added to a stirred solution of 2 parts of sodium carboxymethyl cellulose in 80 parts hot distilled water. To this solution was added 9 parts of a material made by heating a-cellulose impregnated with ammonium sulphamate for 4 hours at 200C and to which had been added 0.74 parts of 'casein (fat free), 2 parts of calcium carbonate and 20 parts of a concentrated solution obtained by Soxhlet extracting Nicotiana Rustica with ethanol and containing 1.68 parts of extract material. The resulting slurry was stirred till homogeneous (approximately 1 hour).
  • the slurry was cast on glass plates to give a film of 48-52 grams/square metre basis weight and shredded.
  • the cigarettes made from this shred were smoked by an expert panel of four smokers who were unanimously of the opinion that a cigarette tobacco flavour was present, whereas this was found to be absent from cigarettes of similar composition but with the exclusion of the Nicotiana Rustica extract. However, some off-notes characteristic of Nicotiana Rustica but foreign to fluecured tobacco were detected.
  • EXAMPLE 2 1.1 parts of glycerol were dissolved in 20 parts distilled water and this solution added to 1.6 parts of sodium carboxymethyl cellulose in 80 parts of distilled water and the mixture stirred. 6.9 parts of magnesium carbonate (magnesite), 4.1 parts of calcium carbonate, 0.2 parts of casein (fat free), 51 parts of a material prepared by heating a-cellulose in the presence of ammonium sulphamate and 1.0 parts of extract material obtained by Soxhlet extracting Nicotiana Rustica with ethanol, this material being redissolved in 20 parts of ethanol.
  • the resultant slurry was stirred for at least one hour then cast on glass plates to give a film which on drying removed the ethanol by evaporation and gave a sheet of basis weight 48-52 grams/square metre.
  • the sheet was shredded and made up into a blend containing 40 parts of this shred and 60 parts of fluecured Virginian tobacco. Cigarettes from this blend were compared with those of a 40:60 tobacco blend from shred containing no extract material but otherwise identical.
  • the cigarettes were compared using a statistical preference panel test and the panel stated a preference for the cigarettes containing the Rustica tobacco extract, with 78 percent confidence.
  • EXAMPLE 3 1.6 parts of glycerol and 0.4 parts ammonium sulphate were dissolved in 20 parts of distilled water and this solution was added to a mixture of 70 parts of distilled water, 5.3 parts of magnesite, 0.9 parts of bentonite, 3.0 parts of calcium carbonate, 1.7 parts of extract material obtained by treating Nicotiana Rustica with ethanol, this material being mainly in solution but partly in suspension in parts of distilled water. This mixture was stirred and to it was added 2.2 parts of sodium carboxymethyl cellulose and 4.9 parts of a material prepared by heating a-cellulose in the presence of ammonium sulphamate. Stirring was continued for at least one hour. The resulting slurry was cast on glass plates to give a film which, on drying, had a basis weight of 48-52 grams/square metre.
  • the sheet was shredded and made up into a blend containing 50 parts of this shred and 50 parts of fluecured Virginian tobacco. Cigarettes from this blend were compared with those of a 50:50 tobacco blend from shred containing no extract material but otherwise identical.
  • the cigarettes were compared using a statistical preference panel test and the panel stated a preference for the cigarettes containing the Rustica tobacco extract with 96 percent confidence.
  • EXAMPLE 4 Sheet material was prepared identical with that described in Example 3 except that 2.5 parts of the extract material was used instead of 1.7 parts and the amounts of the other ingredients were scaled down proportionately. A similar panel assessment of cigarettes from 50:50 tobacco blends in this case showed that the preference for the extract-containing cigarette had been destroyed by increasing the amount of this extract.
  • EXAMPLE 5 Dried ball-milled Nicotiana Rustica (1,000 g) of moisture content 7.9 percent extracted in a Soxhlet apparatus with ethanol (3,000 ml) for 32 hours. Analysis of an aliquot portion of extract showed that all the nicotine had been extracted and 36.3 percent of the dry weight of the Nicotiana Rustica had passed into solution.
  • Fulmont 725C an activated acid clay which, when mixed with water to form a 1 percent suspension, gives a liquor of pH 5, was used in the treatment of ethanol extracts of Nicotiana Rustica in the same way as Fulmont 300C described in Example 5.
  • the filtrate from the reaction containing 2.9 percent of the original nicotine and 27.9 percent of the total original solids was flavour assessed in the same manner at 4.7 percent concentration of solids and was found to give a smoke essentially similar to that from the filtrate from the Fulmont 300C treatment.
  • a smoking mixture comprising a mixture of a tobacco substitute with from 1 to 11 percent of its weight of extracted material obtained by treating Nicotiana Rustica with a nicotine-dissolving solvent and removing the solvent so that the extracted material is wholly free from any toxic solvent that may be used for said extraction, said mixture being blended with from 65 to percent of its weight of tobacco and said tobacco substitute comprising a thermally degraded carbohydrate prepared by subjecting carbohydrate to a catalyzed degradation at about C until the weight of degraded carbohydrate is less than 90 percent of the weight of the orignal carbohydrate.
  • a smoking mixture according to claim 1 wherein the tobacco substitute comprises cellulose, a cellulose ether, oxidised cellulose or lettuce leaves.
  • a smoking mixture according to claim 1 fabricated in sheet form containing a film-forming agent.
  • a smoking mixture according to claim 1 incorporating tobacco.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)
US332112A 1972-03-16 1973-02-13 Smoking mixtures Expired - Lifetime US3880172A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB1235772A GB1362613A (en) 1972-03-16 1972-03-16 Smoking mixtures

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US3880172A true US3880172A (en) 1975-04-29

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Application Number Title Priority Date Filing Date
US332112A Expired - Lifetime US3880172A (en) 1972-03-16 1973-02-13 Smoking mixtures

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US (1) US3880172A (enrdf_load_stackoverflow)
JP (1) JPS49499A (enrdf_load_stackoverflow)
BE (1) BE796486A (enrdf_load_stackoverflow)
CA (1) CA992422A (enrdf_load_stackoverflow)
DE (1) DE2313191A1 (enrdf_load_stackoverflow)
FR (1) FR2176440A5 (enrdf_load_stackoverflow)
GB (1) GB1362613A (enrdf_load_stackoverflow)
IE (1) IE37276B1 (enrdf_load_stackoverflow)
IT (1) IT1048113B (enrdf_load_stackoverflow)
LU (1) LU67217A1 (enrdf_load_stackoverflow)
NL (1) NL7303613A (enrdf_load_stackoverflow)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4793365A (en) * 1984-09-14 1988-12-27 R. J. Reynolds Tobacco Company Smoking article
US5005593A (en) * 1988-01-27 1991-04-09 R. J. Reynolds Tobacco Company Process for providing tobacco extracts
CN110353300A (zh) * 2019-04-16 2019-10-22 深圳雾芯科技有限公司 用于气溶胶装置的树脂香脂分离调配物及其制备方法
US20210153543A1 (en) * 2017-05-15 2021-05-27 British American Tobacco (Investments) Limited Method of making a tobacco extract
WO2021127162A1 (en) * 2019-12-20 2021-06-24 Juul Labs, Inc. Hydrated ionic clay and tobacco material compositions
US11766067B2 (en) 2017-05-15 2023-09-26 Nicoventures Trading Limited Ground tobacco composition
US12075810B2 (en) 2017-05-15 2024-09-03 Nicoventures Trading Limited Method of making a tobacco extract
US12369617B2 (en) 2019-12-19 2025-07-29 Juul Labs, Inc. Metal oxide-based gel nicotine compositions
US12389934B2 (en) 2019-12-19 2025-08-19 Juul Labs, Inc. Organic-based nicotine gel compositions

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5379055A (en) * 1976-12-21 1978-07-13 Kanebo Ltd Production of instant dry meat
US4256126A (en) * 1978-08-02 1981-03-17 Philip Morris Incorporated Smokable material and its method of preparation
US4256123A (en) * 1978-08-02 1981-03-17 Philip Morris Incorporated Smokable material containing thermally degraded tobacco by-products and its method of preparation
US4244381A (en) * 1978-08-02 1981-01-13 Philip Morris Incorporated Upgraded tobacco stem material and its method of preparation
JPS5639765A (en) * 1979-09-04 1981-04-15 Natl Food:Kk Formed and frozen meat block, and its preparation
WO2002037989A1 (fr) * 2000-11-07 2002-05-16 Environmental Technology Licensing Ltd. Tabac a forte teneur en nicotine et procede de production dudit tabac
RU2432864C1 (ru) * 2010-12-10 2011-11-10 Олег Иванович Квасенков Способ производства некурительного изделия из махорки

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US802487A (en) * 1903-12-28 1905-10-24 Karl Wimmer Treatment of tobacco for the removal of nicotin.
US3046997A (en) * 1960-09-27 1962-07-31 Philip Morris Inc Selective alkaloid extraction
US3258015A (en) * 1964-02-04 1966-06-28 Battelle Memorial Institute Smoking device
US3390685A (en) * 1965-03-11 1968-07-02 Eresta Warenhandelsgmbh Process for extracting substances from plant particles
US3529602A (en) * 1969-02-27 1970-09-22 Philip Morris Inc Tobacco substitute sheet material
US3545448A (en) * 1966-05-19 1970-12-08 Ici Ltd Process for making a modified carbohydrate material for smoking mixtures and the material made thereby
US3638660A (en) * 1968-09-10 1972-02-01 Howard J Davis Method for making a tobacco substitute composition

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US802487A (en) * 1903-12-28 1905-10-24 Karl Wimmer Treatment of tobacco for the removal of nicotin.
US3046997A (en) * 1960-09-27 1962-07-31 Philip Morris Inc Selective alkaloid extraction
US3258015A (en) * 1964-02-04 1966-06-28 Battelle Memorial Institute Smoking device
US3390685A (en) * 1965-03-11 1968-07-02 Eresta Warenhandelsgmbh Process for extracting substances from plant particles
US3545448A (en) * 1966-05-19 1970-12-08 Ici Ltd Process for making a modified carbohydrate material for smoking mixtures and the material made thereby
US3638660A (en) * 1968-09-10 1972-02-01 Howard J Davis Method for making a tobacco substitute composition
US3529602A (en) * 1969-02-27 1970-09-22 Philip Morris Inc Tobacco substitute sheet material

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5076292A (en) * 1984-09-14 1991-12-31 R. J. Reynolds Tobacco Company Smoking article
US4793365A (en) * 1984-09-14 1988-12-27 R. J. Reynolds Tobacco Company Smoking article
US5005593A (en) * 1988-01-27 1991-04-09 R. J. Reynolds Tobacco Company Process for providing tobacco extracts
US12075810B2 (en) 2017-05-15 2024-09-03 Nicoventures Trading Limited Method of making a tobacco extract
US20210153543A1 (en) * 2017-05-15 2021-05-27 British American Tobacco (Investments) Limited Method of making a tobacco extract
US12426620B2 (en) 2017-05-15 2025-09-30 Nicoventures Trading Limited Ground tobacco composition
US12329189B2 (en) * 2017-05-15 2025-06-17 Nicoventures Trading Limited Method of making a tobacco extract
US11766067B2 (en) 2017-05-15 2023-09-26 Nicoventures Trading Limited Ground tobacco composition
CN110353300A (zh) * 2019-04-16 2019-10-22 深圳雾芯科技有限公司 用于气溶胶装置的树脂香脂分离调配物及其制备方法
CN110353300B (zh) * 2019-04-16 2022-03-01 深圳雾芯科技有限公司 用于气溶胶装置的树脂香脂分离调配物及其制备方法
US12369617B2 (en) 2019-12-19 2025-07-29 Juul Labs, Inc. Metal oxide-based gel nicotine compositions
US12389934B2 (en) 2019-12-19 2025-08-19 Juul Labs, Inc. Organic-based nicotine gel compositions
WO2021127162A1 (en) * 2019-12-20 2021-06-24 Juul Labs, Inc. Hydrated ionic clay and tobacco material compositions

Also Published As

Publication number Publication date
DE2313191A1 (de) 1973-09-20
NL7303613A (enrdf_load_stackoverflow) 1973-09-18
LU67217A1 (enrdf_load_stackoverflow) 1973-05-22
IT1048113B (it) 1980-11-20
JPS49499A (enrdf_load_stackoverflow) 1974-01-05
FR2176440A5 (enrdf_load_stackoverflow) 1973-10-26
CA992422A (en) 1976-07-06
IE37276L (en) 1973-09-16
BE796486A (fr) 1973-09-10
GB1362613A (en) 1974-08-07
IE37276B1 (en) 1977-06-22

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Owner name: IMPERIAL GROUP PLC, A COMPANY OF UNITED KINGDOM

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:IMPERIAL CHEMICAL INDUSTRIES PLC;REEL/FRAME:004599/0794

Effective date: 19860603