US283622A - Oscae libbeeich and hugo michaelis - Google Patents

Oscae libbeeich and hugo michaelis Download PDF

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US283622A
US283622A US283622DA US283622A US 283622 A US283622 A US 283622A US 283622D A US283622D A US 283622DA US 283622 A US283622 A US 283622A
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tobacco
nicotine
extract
hugo
michaelis
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D401/00Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
    • C07D401/02Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
    • C07D401/04Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond

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  • OSCAR LIEBREIOH AND HUGO MICHAELIS OF BERLIN, GERMANY, ASSIGNORS TO FRIEDRICH CARL GLASER, OF SAME PLACE.
  • OSCAR LIEBREIOH and Hoeo hIICHAELIS subjects of theKing of Prussia, residing at the city of Berlin, in the Kingdom of Prussia and Empire of Germany, have invented new and useful Improvements in Processes for Treating Tobacco, of which the following is a specification.
  • This invention relates to a mode of preparing an extract of tobacco, which consists in subjecting the tobacco to the action of volatile example, by chloroform,
  • a fixed dosing of the nicotine contained may be attained by treating the extract with acidulated water, as hereinafter more fully set forth.
  • the tobacco is subj ected to extraction by any substance which is volatile and which dissolves fatsas, for
  • the extracting material which after extraction is retained by the tobacco, is removed therefrom by being forced out by air, carbonic acid or other gases, or by heating and the production of a vacuum in he vessel in which the extraction is carried on, and in this way the extracting material is again obtained. From the extract thus ob tained the extracting material. is distilled off, and the last traces of the same are removed by heating, which may be done in. a vacuum.
  • the extract now contains, in addition to other,
  • the extract is for a considerable period agitated, in the presence of heat, with an alkaline reacting aqueous liquid, most suitably a solution containing about one-half per cent. of ammonia.
  • the aromatic components are taken up by the alkaline reacting liquid, while a smeary, colored, and sticky mass remains behind.
  • Coloring-matters and a part of the nicotine are also taken upby the alkaline liquid.
  • the alkaline liquid charged with the mentioned materials is separated from the waxy components by filtration or centrifugaether, ethylidenetion, or other similar process. With the alkaline liquid thus obtained the tobacco is im pregnated by sprinkling, immersion, or similar treatment. The tobacco is then dried, while the aroma, color, and the like remain behind.
  • the extract which has been freed from the extracting material is agitated with slightly acidulated water, (most suitably water containing about one-half per cent. of hy- 6p drochloric acid,) and the resulting solution in which the nicotine is contained is separated from the undissolved remaining substances by filtration or similar treatment.
  • the sediment is washed out with water.
  • Example 1 One kilogram of tobacco is subjected to extraction by about four kilo grams of ethylidenechloride, until the ex- 'tractive flowing off is no longer colored. The 9 5 tobacco thus treated is dried in order to drive out the extractive which may yet be contained therein. This drying is done in a closed vessel through which air is forced, so as to cause the ethylidene-chloride which is forced out by the air to be caught in suitable condensers and be regained for use. The ethylidone-chloride is distilled off from the extract to stand and cool, when waxy substances sepatakes place,
  • Example 2 In this example ethylidenechloride is to be used as an extracting material.
  • the proportionate quantities, as also the operation of extracting and distilling, are the same as just described. If in this case the nicotine contained in the extract is to be removed, the extract is agitated, while being warmed, with one liter of acid solution-containing about one- 'half per cent. of hydrochloric acid.
  • Example 3 In this third example is to be shown how an improvement of the tobacco can be undertaken with simultaneous dosing and after continued agitation for of the nicotine contents, and in this case chloroform is to be used, as extracting material.
  • the tobacco here used as raw material is first examined by analysis in regard to its nicotine contents, and as an example the same will be assumed as being three per cent.
  • One kilogram of extract is then subjected to extraction by about four kilograms of chloroform.
  • the extract is freed from chloroform by distillation, the precipitate is agitated, while being warmed, with one liter of acid solution containing one-half per cent. of nitric acid, and the solution is filtered.
  • the precipitate. obtained is agitated with one liter of potash lye containing onehalf per cent. of potash, and again filtered;
  • the nicotine is obtained by distillation with caustic lime. Nico are obtained, corresponding to the above named contents of this material in the tobacco, and if, for example, these contents are to be reduced to one per cent., ten grams of the nicotine obtained are added to the alkaline solution, with which latter the tobacco is uniformly impregnated and then dried, as before stated.
  • ⁇ Vhat we claim is The method of preparing an extract of tobacco, which consists in subjecting the tobacco to the action of volatile fat, resin, and wax dissolving substances, and of alkaline reacting liquids, substantially as set forth.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Tobacco Products (AREA)

Description

Ni'rsc STATES PATENT rica.
OSCAR LIEBREIOH AND HUGO MICHAELIS, OF BERLIN, GERMANY, ASSIGNORS TO FRIEDRICH CARL GLASER, OF SAME PLACE.
f PREPARING EXTRACTS OF TOBACCO.
SPECIFICATION forming part of Letters Patent No, 283,622, dated August 21, 1883.
Application filed March 17, 1883. (No specimens) To all 20. 1.0121, it may concern.-
Be it known that we, OSCAR LIEBREIOH and Hoeo hIICHAELIS, subjects of theKing of Prussia, residing at the city of Berlin, in the Kingdom of Prussia and Empire of Germany, have invented new and useful Improvements in Processes for Treating Tobacco, of which the following is a specification.
This invention relates to a mode of preparing an extract of tobacco, which consists in subjecting the tobacco to the action of volatile example, by chloroform,
bon, and thc like.
fat, resin, and wax dissolving substances and of alkaline reacting liquids, as hereinafter more fully set forth.
A fixed dosing of the nicotine contained may be attained by treating the extract with acidulated water, as hereinafter more fully set forth.
In carrying out the method the tobacco is subj ected to extraction by any substance which is volatile and which dissolves fatsas, for
chloride, ethylene-chloride, sulphide of ca- The extracting material, which after extraction is retained by the tobacco, is removed therefrom by being forced out by air, carbonic acid or other gases, or by heating and the production of a vacuum in he vessel in which the extraction is carried on, and in this way the extracting material is again obtained. From the extract thus ob tained the extracting material. is distilled off, and the last traces of the same are removed by heating, which may be done in. a vacuum.
The extract now contains, in addition to other,
ingredients, a part of the nicotine, coloringmatters, waxy and fatty components, and, joined to the latter, the aroma of the tobacco. After this the extract is for a considerable period agitated, in the presence of heat, with an alkaline reacting aqueous liquid, most suitably a solution containing about one-half per cent. of ammonia. The aromatic components are taken up by the alkaline reacting liquid, while a smeary, colored, and sticky mass remains behind. Coloring-matters and a part of the nicotine are also taken upby the alkaline liquid. The alkaline liquid charged with the mentioned materials is separated from the waxy components by filtration or centrifugaether, ethylidenetion, or other similar process. With the alkaline liquid thus obtained the tobacco is im pregnated by sprinkling, immersion, or similar treatment. The tobacco is then dried, while the aroma, color, and the like remain behind.
If a fixed amount of the nicotine contents is to be attained, the extract which has been freed from the extracting material is agitated with slightly acidulated water, (most suitably water containing about one-half per cent. of hy- 6p drochloric acid,) and the resulting solution in which the nicotine is contained is separated from the undissolved remaining substances by filtration or similar treatment. The sediment is washed out with water. By a greater or less 65 addition of acid, and by regarding the amount of nicotine already present or still remaining in the tobacco to be impregnated, the exact dosing or proportioning of the amount of nicotine required to be contained in product can be attained.
Under circumstances it may be advantageous, in place of raw tobacco, to subject tobacco in any degree of manufacture to the process described; also, the several steps of the process may be divided among the different steps of manufacture, so that, for example, the extraction may take place'after fermentation, and the addition of the extract may take place only when the manufacture is complete.
In the above-described process nothing prevents the application of sauce, which is occasionally employed to generate a certain taste in the smoking of the tobacco.
In the following it is intended, in addition 85 to the process already set forth, to describe some examples whereby the ch osen extractions, as also the materials eventually used for the acid solutions, are varied, and it is to be noticed that these variations may also be effected 0 in difibrent manners.
Example 1. One kilogram of tobacco is subjected to extraction by about four kilo grams of ethylidenechloride, until the ex- 'tractive flowing off is no longer colored. The 9 5 tobacco thus treated is dried in order to drive out the extractive which may yet be contained therein. This drying is done in a closed vessel through which air is forced, so as to cause the ethylidene-chloride which is forced out by the air to be caught in suitable condensers and be regained for use. The ethylidone-chloride is distilled off from the extract to stand and cool, when waxy substances sepatakes place,
rate. The latter are taken from the liquor, and the tobacco, treated and dried as above set forth, has uniformly poured over it the ex tract, which has been cleaned and freed from waxy substances, after which the whole is dried.
Example 2. In this example ethylidenechloride is to be used as an extracting material. The proportionate quantities, as also the operation of extracting and distilling, are the same as just described. If in this case the nicotine contained in the extract is to be removed, the extract is agitated, while being warmed, with one liter of acid solution-containing about one- 'half per cent. of hydrochloric acid.
After cooling and filtering, the precipitate, which is now freed from nicotine, is washed with water. This extract is now, as in the first example, agitated, while being warmed, with one liter of ammonia solution containing one half per cent. of ammonia, and filtered after cooling. The separation of the waxy substances again so that the tobacco which has been subjected to extraction and dried can then have uniformly poured over it the filtrate, after the same has cooled, after which the tobacco is dried. By these means the desired result is attained of a tobacco of an agreeable taste, and free from waxy, fatty, and resinous substances.
Example 3. In this third example is to be shown how an improvement of the tobacco can be undertaken with simultaneous dosing and after continued agitation for of the nicotine contents, and in this case chloroform is to be used, as extracting material. The tobacco here used as raw material is first examined by analysis in regard to its nicotine contents, and as an example the same will be assumed as being three per cent. One kilogram of extract is then subjected to extraction by about four kilograms of chloroform. In the same manner as before the tobacco is subjected to air-drying to remove the absorbed chloroform, the extract is freed from chloroform by distillation, the precipitate is agitated, while being warmed, with one liter of acid solution containing one-half per cent. of nitric acid, and the solution is filtered. The precipitate. obtained is agitated with one liter of potash lye containing onehalf per cent. of potash, and again filtered;
From the acid solution, which contains all the nicotine, the nicotine is obtained by distillation with caustic lime. nicotine are obtained, corresponding to the above named contents of this material in the tobacco, and if, for example, these contents are to be reduced to one per cent., ten grams of the nicotine obtained are added to the alkaline solution, with which latter the tobacco is uniformly impregnated and then dried, as before stated.
\Vhat we claim is The method of preparing an extract of tobacco, which consists in subjecting the tobacco to the action of volatile fat, resin, and wax dissolving substances, and of alkaline reacting liquids, substantially as set forth.
In testimony whereof we have hereunto set our hands and seals in the presence of two subscribing witnesses.
OSCAR'LIEBREICH. n s] HUGO MICHAELIS. n s] Witnesses:
MARC M. RUSSEN, O. L. THEODOR M'L' LLER.
Thirty grams of
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3428053A (en) * 1965-10-07 1969-02-18 American Tobacco Co Production of reconstituted tobacco
US3575178A (en) * 1969-03-13 1971-04-20 Reynolds Tobacco Co R A process for increasing the filling capacity of tobacco
USRE30693E (en) * 1975-03-17 1981-08-04 Reynolds Leasing Corporation Process for increasing the filling capacity of tobacco
US4967771A (en) * 1988-12-07 1990-11-06 R. J. Reynolds Tobacco Company Process for extracting tobacco
US5005593A (en) * 1988-01-27 1991-04-09 R. J. Reynolds Tobacco Company Process for providing tobacco extracts
US5018540A (en) * 1986-12-29 1991-05-28 Philip Morris Incorporated Process for removal of basic materials
US5148819A (en) * 1991-08-15 1992-09-22 R. J. Reynolds Tobacco Company Process for extracting tobacco

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3428053A (en) * 1965-10-07 1969-02-18 American Tobacco Co Production of reconstituted tobacco
US3575178A (en) * 1969-03-13 1971-04-20 Reynolds Tobacco Co R A process for increasing the filling capacity of tobacco
USRE30693E (en) * 1975-03-17 1981-08-04 Reynolds Leasing Corporation Process for increasing the filling capacity of tobacco
US5018540A (en) * 1986-12-29 1991-05-28 Philip Morris Incorporated Process for removal of basic materials
US5005593A (en) * 1988-01-27 1991-04-09 R. J. Reynolds Tobacco Company Process for providing tobacco extracts
US4967771A (en) * 1988-12-07 1990-11-06 R. J. Reynolds Tobacco Company Process for extracting tobacco
US5148819A (en) * 1991-08-15 1992-09-22 R. J. Reynolds Tobacco Company Process for extracting tobacco

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