Process for the extraction of nicotine from tobacco

• US 4,153,063 A
• Filed: 08/23/1973
• Issued: 05/08/1979
• Est. Priority Date: 09/02/1970
• Status: Expired due to Term

• Current Assignee: Studiengesellschaft Kohle MBH
• Original Assignee: Studiengesellschaft Kohle MBH
• Inventors: Hubert, Peter, Vitzthum, Otto, Roselius, Wilhelm
• Primary Examiner(s): Michell, Robert W.
• Assistant Examiner(s): Millin, V.
• Application Number:
  US05/390,967
• Time in Patent Office: 2,084 Days
• Field of Search: 131/17, 131/143, 131/144, 131/135, 131/140 C, 260/291
• US Class Current: 131/297
• CPC Class Codes: A24B 15/24 by extraction; Tobacco extracts
• CPC Class Codes: B01D 11/0203 with a supercritical fluid

Abstract

Process for extracting nicotine is disclosed in which tobacco is exposed to an extracting solvent in either liquid or gaseous state at temperatures below about 100° C. and at high pressures. The aroma generating substances can be removed by conducting the extraction with the tobacco in dry condition. Thereafter the tobacco can be moistened, and on further contacting the nicotine is removed. The aroma generating substances can then be recombined with nicotine free tobacco.

Claims

1. A process for the selective aroma preserving extraction of nicotine from tobacco with normally gaseous solvents characterized in that the tobacco is extracted with the said solvent in the presence of at least 10% by weight of moisture based on the weight of the tobacco either in the liquid state at a pressure of from about 65 to 300 atmospheres or in the supercritical state at a temperature from the critical temperature of the solvent to about 100°

C. at a pressure of from about 70 to 1500 atmospheres.

2. A process as in claim 1 wherein the moisture content of the tobacco is up to about 25% by weight.

3. A process as in claim 1 wherein the extraction solvent is CO₂.

4. A process as in claim 1 wherein the extraction solvent is Ar.

5. A process as in claim 1 wherein the extraction solvent is SF₆.

6. A process as in claim 1 wherein the extraction solvent is a lower halogenated carbon.

7. Process as claimed in claim 1, wherein the extraction solvent is N₂ O.

8. A process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous, nicotine extraction solvent in the super-critical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a neglibible amount of nicotine;

(b) separating the aroma constituents from the nicotine extraction agent;

(c) wetting the dry tobacco to a water content of from about 10% to 25% by traversing it with a water wet, nomrally gaseous, nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract substantially all of the remaining nicotine content from the wet tobacco;

(d) taking up the precipitated aroma constituents with a dry, normally gaseous solvent in the supercritical state at a temperature of from the critical temperature to about 100°

at a pressure of from about 70 to 1500 atmospheres to form an extract; and

(e) redepositing the aroma constituents from the extract produced in step (e), in and on tobacco from which aroma constituents and nicotine have been removed.

9. A process as in claim 8 carried out in a continuous manner.

10. A process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a negligible amount of nicotine;

(b) allowing the solvent to expand into a second vessel with cooling to convert it to a subcritical liquid and to precipitate the aroma constituents and nicotine;

(c) converting the subcritical liquid from Step B to a supercritical gas by heating it to a temperature of from the critical temperature to about 100°

C. and increasing the pressure to from about 70 to 1500 atmospheres;

(d) wetting the heated, compressed, supercritical gas by passage through water and traversing it through the extraction vessel to increase the water content of the tobacco up to about 20% to 25% and extract the nicotine content of the tobacco;

(e) taking up the precipitated aroma constituents with a dry, normally gaseous solvent in the supercritical state at a temperature of from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to form an extract; and

(f) redepositing the aroma constituents from the extract in and on the previously dried tobacco by expanding and cooling the extract in the extraction vessel containing the tobacco.

11. A process as in claim 10 carried out in a continuous manner.

12. A continuous process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous, nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a negligible amount of nicotine;

(b) allowing the solvent to expand into a second vessel with cooling to convert it to a subcritical liquid and to precipitate the aroma constituents and nicotine;

(c) converting the subcritical liquid from Step B to a supercritical gas by heating it to a temperature of from the critical temperature to about 100°

C. and increasing the pressure to from about 70 to 1500 atmospheres and returning the heated, compressed supercritical gas to the extraction vessel;

(d) repeating steps (a), (b) and (c) to remove the desired quantities of aroma producing constituents from the tobacco, and thereafter passing the supercritical gas through an aqueous sulfuric solution to wet it and to absorb the nicotine;

(e) traversing the wet, supercritical gas through the tobacco in the extraction vessel to increase its moisture content up to about 20% to 25% and extract the nicotine content of the tobacco;

(f) thereafter drying the tobacco and the wet, supercritical gas by decreasing the temperature of the gas while continuing the cycle it through the extraction vessel and the sulfuric acid solution to deposit the water from the gas into the solution;

(g) taking up the aroma producing constituents precipitated in step (b) by contact with the dry, supercritical gas from step (f) to form an aroma constituents containing extract; and

(h) redepositing the aroma constituents from the extract in and on the tobacco by expanding and cooling the extract in the extraction vessel containing the tobacco.

13. A process as in claim 12 wherein the supercritical gas from Step D passes through water before traversing the extraction vessel in Step E.

14. A continuous process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous, nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a negligible amount of nicotine;

(b) allowing the solvent to expand into a second vessel with cooling to convert it to a subcritical liquid and to precipitate the aroma constituents and nicotine;

(c) converting the subcritical liquid from step (b) to a supercritical gas by heating it to a temperature of from the critical temperature to about 100°

C. and increasing the pressure to from about 70 to 1500 atmospheres and returning the heated, compressed, supercritical gas to the extraction vessel;

(d) repeating steps (a), (b) and (c) to remove the desired quantities of aroma producing constituents from the tobacco and thereafter traversing the supercritical gas through water to wet it;

(e) traversing the wet, supercritical gas through the tobacco in the extraction vessel to increase its moisture content up to about 20% to 25% and extract the nicotine content of the tobacco;

(f) traversing the wet, supercritical gas containing the nicotine through an absorbent column containing an absorbent for the nicotine;

(g) thereafter drying the tobacco and the wet supercritical gas by decreasing the temperature of the gas to condense the water content thereof;

(h) taking up the aroma producing constituents precipitated in step (b) by contact with the dry, supercritical gas from step (f) to form an aroma constituents containing extract; and

(i) redepositing the aroma constituents from the extract in and on the tobacco by expanding and cooling the extract in the extraction vessel containing the tobacco.

15. A process as in claim 14 wherein the absorbent is aluminum oxide, silica gel, active carbon, an ion exchange resin, impregnated kieselguhr or a molecular filter.

16. A continuous process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous, nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a negligible amount of nicotine;

(b) allowing the solvent to expand into a second vessel with cooling to covert it to a subcritical liquid and to precipitate the aroma constituents and nicotine;

(c) converting the subcritical liquid from step (b) to a supercritical gas by heating it to a temperature of from the critical temperature to about 100°

C. and increasing the pressure to from about 70 to 1500 atmospheres and returning the heated, compressed supercritical gas to the extraction vessel;

(d) repeating steps (a), (b), and (c) to remove the desired quantities of aroma producing constituents from the tobacco, and thereafter passing the supercritical gas through an aqueous sulfuric acid solution to wet it and to absorb the nicotine;

(e) traversing the wet, supercritical gas through the tobacco in the extraction vessel to increase its moisture content up to about 20% to 25% and extract the nicotine content of the tobacco;

(f) drying the tobacco;

(g) thereafter drying the wet, supercritical gas by decreasing the temperature of the gas while continuing to cycle it through the extraction vessel and the sulfuric acid solution to deposit the water from the gas into the solution;

(h) taking up the aroma producing constituents precipitated in step (b) by contact with the dry, supercritical gas from step (f) to form an aroma constituents containing extract; and

(i) redepositing the aroma constituents from the extract in and on the tobacco by expanding and cooling the extract in the extraction vessel containing the tobacco.

17. A continuous process for reducing the nicotine content of tobacco comprising the steps of:

(a) traversing an extraction vessel containing dry tobacco with a stream of dry, normally gaseous nicotine extraction solvent in the supercritical state at a temperature from the critical temperature to about 100°

C. at a pressure of from about 70 to 1500 atmospheres to extract the aroma constituents of the tobacco together with a negligible amount of nicotine;

(b) allowing the solvent to expand into a second vessel with cooling to convert it to a subcritical liquid and to precipitate the aroma constituents and nicotine;

(c) converting the subcritical liquid from step (b) to a supercritical gas by heating it to a temperature of from the critical temperature to about 100°

C. and increasing the pressure to from about 70 to 1500 atmospheres and returning the heated, compressed, supercritical gas to the extraction vessel;

(d) repeating steps (a), (b), and (c) to remove the desired quantities of aroma producing constituents from the tobacco and thereafter traversing the supercritical gas through water to wet it;

(e) traversing the wet, supercritical gas through the tobacco in the extraction vessel to increase its moisture content up to about 20% to 25% and extract the nicotine content of the tobacco;

(f) traversing the wet, supercritical gas containing the nicotine through an absorbent column containing an absorbent for the nicotine;

(g) drying the tobacco;

(h) thereafter drying the wet supercritical gas by decreasing the temperature of the gas to condense the water content thereof;

(i) taking up the aroma producing constituents precipitated in step (b) by contact with the dry supercritical gas from step (f) to form an aroma constituents containing extract; and

(j) redepositing the aroma constituents from the extract in and on the tobacco by expanding and cooling the extract in the extraction vessel containing the tobacco.

18. A process for the selective aroma preserving extraction of nicotine from tobacco with normally gaseous nicotine solvent characterized in that the tobacco is extracted with the said solvent either in the presence of at least 10% by weight of moisture based on the weight of the tobacco in the liquid state at a pressure of from about 65 to 300 atmospheres or in the supercritical state.

19. Process according to claim 18, the solvent being above the critical temperature and above the critical pressure.

20. Process according to claim 19, the tobacco having a moisture content of 10-25% by weight.

21. Process according to claim 19, the tobacco being wet.

22. Process of claim 18, wherein the solvent is in said liquid state.

23. Process of claim 22, wherein the solvent is CO₂.

24. Process of claim 22, wherein the solvent is SF₆.

25. Process of claim 22, wherein the solvent is lower halogenated hydrocarbon.

26. Process of claim 22, wherein the extraction solvent is N₂ O.

27. Process of claim 18, wherein the solvent is in supercritical state.

28. Process of claim 27, wherein the solvent is CO₂.

29. Process of claim 27, wherein the solvent is Ar.

30. Process of claim 27, wherein the solvent is SF₆.

31. Process of claim 27, wherein the solvent is lower halogenated solvent.

32. Process of claim 27, wherein the extraction solvent is N₂ O.