us United States c2) Patent Application Publica Nauryzbaey et al. (54) METHOD FOR EXTRACTION OF NICOTINE FROM TOBACCO RAW MATERIAL (75) Inventors: Michall Kassymovieh, Nauryzbuev. Almaty (KZ): Datei Yurievieh Korulkin, Almaty (KZ); Serikbol T fe Shalghymbaev. Almaty (KZ); Timur Michallovich Nauryzbuey Almaty (KZ) Correspondence Address: DEFILLO & ASSOCIATES, INC. P.O. Box 14104 Clearwater, FL 33766 (US) (21) Appl.Nos 12012070 (2) Filed Jan. 31,2008, G0) Forcign Application Priority Data Jun, 5.2007 (KZ) 20070762.1 'US 200803023741 iON (10) Pub. No.: US 2008/0302377 Al (43) Pub, Date Dec. 11, 2008 ication Classification (1) Inve ADB 1526 US.CL (2006.01), 1317298 ABSTRACT The invention relates to methods of nicotine extraction fom tobacco, caporal and tobaceo crumb. The proposed method for extraction of nicotine from tobaoco, caporal and tobacco crumb implies continuous extraction from raw material with lowboiling solvents st vapor phase Followed by solvent stripper and recurrence for futher rouse in the process. The technological advantages are the opportunity to use both primary raw material and production wastes, shorter time equired for extraction, eost reduction and process simpli tation for extraction of nicotine, eduction of concomitant Substances in the target produc, and no need in using acids These advantages are achieved by the proposed extraction sethod with low-boiling organic solvents what results ia Tower consumption of chemicals, lower temperature, shorter time reine forthe process and additional purification ofthe target product and eliminates needs for high pressure to be ‘ed in technological process.US 2008/0302377 Al METHOD FOR EXTRACTION OF NICOTINE (OM TOBACCO RAW MATERIAL, (CROSS REFERENCE TO RELATED APPLICATION [0001] This is a conventional application based on KZ Pateat Application No, 200770762.1y filed Jun. 5, 2007, TECHNICAL FIELD OF THE INVENTION [0002] | Theinvention relates to methods of nicotine extrc- tion ftom tobaeeo, eaporal and tobacco ezumb, BACKGROUND OF THE INVENTION 10003] There is a known method for extraction of nicotine Jom lobacco with earbon dioxide, nitrous exile, aepon,sul- Sur hexafluoride [US. Pat. No. 4,153,063, May 8, 1979], The ‘extraction i performed at temperatures 80-70” C. and pres ures up to 1,500 atm. (preferably 70-350 atm.) then tem- perature and pressure are set lower and nicotine is extracted from the gas flows using sorbents 10004} -Forexample, for kzoftobacco with adjusted water ‘content of 15% ta 25%! 10005] CO, 70° C:; 300 atm; the gassobacco weight iti is between 4.91 and 6.31: 0006} CO, $0° C.; 1.000 aim: the gas:tobaceo weight ratios between 7:1 and 9:1; 0007] "Argon, 20° C.; 320 atm: the gasstohaceo weight ratio is betweun 35:1 and 4.51: [0008] SF, 70°C: 300 atm; the gastobaceo weight ratio is between 6: and LO 10009] Disadvantages ofthis method are: 0010] Soase hardly avaiable gases, in particular, sulfur hhoxalluride, argon and nitrous oxide are required; [0011] Supercritical pressure [0012] Tn this method, there are indications that it is pos- sible o uilize halogenhydroearbons, but the conditions are not specified 10013] There is a known method for extraction of nicotine from tobacco and exporal with nicotine istiation by team {allowed by precipitation with phosphowungstic acid: foreach 2 g of tobaceo, it is required 34-36 g of sodium chloride, 14.15 ml of SH sodium hydroxide water solution, 8 ml of 5.6% of pereipient’s solution (phosphotungstic seid) [SU Patent No. 728831, publ. No. 15, 1980} 10014) Disadvantages of this method are that itis need a Special instalation for distillation of quite complex desiga ‘andusing expensive phosphotungstic acd for precipitation this acid conventionally used for qualitative analysis at ‘dentiication of alkaloids, but i not paniculaely specific for nicotine [Shmuk, A. A, The Chemisty and Technology of ‘Tobaceo, Pishchepromizalat, Moscow, 1953, p. 225] [0015] There is a known method for extraction of nicotine from tobacco using organic solvents hardly. miscible or immiscible with water and consequent treatment of the ‘extracts by the acid-water solution, [0016] In this method for each Kilogram of tobacco, itis required 25.200 | of solvent per hour. Dichlormethane, ben- zl, cyclohexane, disopropyl ether, 1,]1-tichloroethane, trichloroehylene,12-dichlorvethane, tetrachloride ethylene are used as solvents [CA Patent No, 809968, 1969.04.08} 10017] For example, tobacco is treated by alow of organic solvent bardly miseible or immiscible with water and then ‘extraction from the solvent is performed by aeid-water solu Dee. 11, 2008 tion, In onder to assure uniform extraction and achieve economy of the method, extraction of tobaeco with organic solvent ad extraction fom solvent with acid-water solution fare relized in continuous process at counter Now of the wo eeds. At that, the contact time foe tobacco and organic sol- ‘ent comprises 45-180 min using w solvent to tobacco ratio of 25-200 of solvent per 1 ky af tobacco per hour, Acid-water solution is removed at nicotine content from 5% to 25%: removed solution is replaced with the appropriate quantity of clean acid-water solution and extracted tobacco is contin ously removed with residual organic solvent in it (in the ‘amouat of 5-4 per { kyo tobacea) then organic solvent is ‘evaporated and regenera [018] Disadvantages ofthis method include: [0019] large consumption of solvents (25-200 1, ie. the Faw materialextractant weight ratio is benwecn I:1Oand 1: 100; 0020} "extraction with organic solvent is performed in stages, at pH-2.0 and 2.Sby acid treatment of theextract, (using chlorine-bydrogen dei, sulphuri acid or ortho- phosphorie acid) 0021] the above-mentioned acids may cause corrosion ‘of the equipment SUMMARY OF THE INVENTION [0022] An objectof de invention isto provide a method for extraction of nicotine from tobacoo and caporal as well as {rom waste products (from a tobacco crumb) [0023] Another object ofthe invention isto provide a pos- sibility for processing of primary raw materials and produe- ‘ion wastes, a shorter, less expensive and technologically simple nicotine extraction, lower contents of accompanying substances in the target product and elimination of usage of acids [0024] ‘Theseobjectsare achieved by the method forextrac- ‘ion of nicotine from tobaceo raw material using extraction treatment of raw material by means of organic solvent and subsequent solvent stripping. but unlike the previously ‘known methods, there are used the low-boiling solvents (pe- ‘roleum ether, chloroform, methylenechloride) at the ra materialsolvent weight ratio of about 1:3; tobacco, capora, and tobseeo crumb (production waste) are used as the 8 ‘material, and extraction of nicotine i earred ou fr around $ bin vapor phase DETAILED DESCRIPTION OF PREFERRED EMBODIMENT OF THE INVENTION 0025}. Te proposed method makes it possible to reduce the ratio of raw material to solvent, to e-use the solveat stripper at extraction, eliminates need! for high pressure, high {emperature acids used in extraction, thatimprovesquality of nicotine, reduces equipment corrosion an, tur, decreases production cost [0026) The present invention makes it possible: 0027] to use easly accessible ow-boiling extractants; [0028] tocanry out theone-satecontinnovs process du ing 5S hours with temperatures not exceeding 70” C. and subsequent concentration of extracts at boiling tempera tures of extoctans (petroleum ether —T,,-40-70" C., chloroform —Th.-6S"C., methylenechloride Tj 40” C. at 760 mm Hg) 0025} to use any tobacco raw material, tobacco waste ‘and any extraction performance at normal pressure: [0030] to reduce the aw materiaextracant weigh! ratio tolUS 2008/0302377 Al [0031] A mass of 100 g of crushed tobacco raw material was inserted into the paper caridge of a Soxhlet extraction apparatus; 300 ml of petroleum ether was placed in a ask (theraw materialsolveat weight ratio :3) and was eflusedat 40-65" C. 10032] "The percent extraction of nicotine atthe extraction time of 2h, 3h, 4h. § hand 6 h were respectively 725%, 80.79%, 86.6%, 89.2%, and 90.5% Example 2 10033] A mass of 100 g of crushed tobacco raw material was inserted into the paper earteidge of a Soxhlet extraction apparatus; 300 ml of petroleum ether was placed in a Bask (dheraw materiasolvent weight ratio 1:3) and wasrefluxedt 60-65" C. 10034] "The percent extraction of nicotine atthe extraction time of 2h, 3h, 4h. § hand 6 h were respectively 66.4%, T1196, 78.5%, 83.5%, and 84.2% Pxample 3 10035] A mass of 100 g of crushed tobacco raw material ‘was inserted info the paper cartridge of a Soxhlet extraction apparatus; 300 ml of petroleum ether was placed in a ask (the raw materiaksolvent weight ratio 1:3) and was refluxed at 40°C. [0036] The percent extraction of nicotine atthe extraction time of 2h, 3h, 4h, Sh, and 6h were wespectively 68.9%, 75.396, 84.2%, 86.8%, and 87.6% Dee. 11, 2008 [0037] Therefore, the advantages of the proposed method include [0038] wider range of nicotine-contaning raw materials for commercial processing: 0039] cheaper extraction process due to utilization of cheaper extmcants and absence of expensive pment, of gis extraction at high pressure, of expensive and fenviroamentally hazardous acids (phosphotungstic, hydrochloric, orthophosphori or sulphurie seid) 0040] "lower concentrations of aecessory agents in the target product. 1. A method for extactng nivotine from a tobaee0 raw ‘material sing an extraction treatment ofthe raw material by ‘cans ofan organic solvent and subsequent solvent stripping ‘which comprises using as solvent a lo-boiling sven, the ‘AW mteria-solvent weiht rato being about 13; and eaery~ ing out the extraction of nicotine for around 5 h in vapor phase. 2. The method aovording to claim 1 ia which said low- boiling solvent is selected from the group consisting of pteo- Jem ether, chloroform, and methylenechloride and mixtures thereat: '3. The method according to clams 1 in which suid robaceo aw material is selected from the group consisting of tobacco, eapora, and tobaevo crumb. 4. The method according to claim 2 in which sid tobacco iw materials selocted from the group consisting oftohacc, eaporl, and tobaceo era