Methods for extracting and isolating constituents of cellulosic material
View Patent ↗A method for extracting and isolating constituents of cellulosic matter, comprising providing cellulosic matter; contacting the cellulosic matter with a supercritical fluid; separating the supercritical fluid from the cellulosic matter, thereby forming an extract and a raffinate; and separating at least one compound present in the extraction medium by distillation.
1. A process for extracting and isolating constituents from cellulosic material, the process comprising:
contacting cellulosic material with a supercritical fluid under conditions to provide an extract;
removing insoluble material from the extract; and
fractionating the extract by distillation under depressed pressure compared to atmospheric pressure to provide one or more isolated constituents, said fractionating including a first distillation carried out under a pressure of 90-130 mbar.
2. The process as claimed in claim 1 , wherein the supercritical fluid is carbon dioxide.
3. The process as claimed in claim 2 , wherein a temperature during said contacting is around 40° C., and a pressure during said contacting is around 30 MPa.
4. The process as claimed in claim 1 , further comprising a water-removal performed after said removing.
5. The process as claimed in claim 1 , wherein said first distillation is carried out at a temperature from 80° C. to 150° C.
6. The process as claimed in claim 1 , wherein said fractionating comprises one or more further distillations.
7. The process as claimed in claim 6 , wherein a first further distillation is carried out under a pressure of between 1 mbar and 5 mbar.
8. The process as claimed in claim 6 , wherein a second further distillation is carried out under a pressure of between 1 mbar and 5 mbar.
9. The process according to claim 1 , wherein the cellulosic material is derived from one of mullein, cloves, mint, tea, Eucalyptus , camomile and tobacco.
10. The process according to claim 9 , wherein the cellulosic material is tobacco lamina.
11. The process according to claim 1 , wherein the one or more isolated constituents are substantially pure, or have a reduced level of one or more of nicotine, one or more nitrosamines, or benzo[a]pyrene in comparison to the cellulosic material from which the constituents were isolated, or from the cellulosic material from which the constituents were isolated when concentrated and/or processed to a comparable extent.
12. The process as claimed in claim 1 , wherein the one or more isolated constituents are substantially free of at least one of nicotine, one or more nitrosamines, and benzo[a]pyrene.
13. The process as claimed in claim 12 , wherein the one or more isolated constituents have at least one of levels of nitrosamines below 0.1 μg/ml, levels of nicotine below 25 mg/ml, and levels of benzo[a]pyrene below 2 ng/g.
14. The process as claimed in claim 1 , wherein the one or more isolated constituents are one or more of coumarin, pulegone, piperonal, trans-anethole, safrole, methyl eugenol and myristicin.
15. The process as claimed in claim 1 , wherein the first distillation is carried out at a temperature of between 90-120° C.
16. The process as claimed in claim 1 , wherein the first distillation is carried out at a temperature between 100° C. and 110° C.
17. The process as claimed in claim 1 , wherein said first distillation is carried out under a pressure from 100 mbar to 110 mbar.
18. The process as claimed in claim 1 , wherein said first distillation is carried out under a pressure of 100 mbar.
19. The process as claimed in claim 6 , wherein a first further distillation is carried out under a pressure of between 1 mbar and 3 mbar.
20. The process as claimed in claim 6 , wherein a first further distillation is carried out under a pressure of 2 mbar.
21. The process as claimed in claim 6 , wherein a first further distillation is carried out at an initial temperature of between 110° C. and 180° C.
22. The process as claimed in claim 6 , wherein a first further distillation is carried out at an initial temperature of between 120° C. and 160° C.
23. The process as claimed in claim 6 , wherein a first further distillation is carried out at an initial temperature of between 135° C. and 155° C.
24. The process as claimed in claim 21 , wherein the initial temperature reduces to between 110° C. and 150° C.
25. The process as claimed in claim 21 , wherein the initial temperature reduces to 140° C.
26. The process as claimed in claim 6 , wherein a second further distillation is carried out under a pressure of between 1 mbar and 3 mbar.
27. The process as claimed in claim 6 , wherein a second further distillation is carried out under a pressure of 2 mbar.
28. The process as claimed in claim 6 , wherein a second further distillation is carried out under an initial temperature of between 110° C. and 180° C.
29. The process as claimed in claim 6 , wherein a second further distillation is carried out under an initial temperature of between 120° C. and 160° C.
30. The process as claimed in claim 6 , wherein a second further distillation is carried out under an initial temperature of between 135° C. and 155° C.
31. The process as claimed in claim 28 , wherein the initial temperature reduces to between 110° C. and 140° C.
32. The process as claimed in claim 28 wherein the initial temperature reduces to 130° C.
33. A method, comprising: contacting cellulosic material with a supercritical fluid to provide an extract; removing insoluble material from the extract; and fractionating the extract by distillation under depressed pressure compared to atmospheric pressure to provide one or more isolated constituents of the cellulosic material, said fractionating including a first distillation carried out under a pressure of about 100 mbar.