CN1115751A - Extraction process of solanesol from tobacco with the nicotine extracted - Google Patents
Extraction process of solanesol from tobacco with the nicotine extracted Download PDFInfo
- Publication number
- CN1115751A CN1115751A CN 94107849 CN94107849A CN1115751A CN 1115751 A CN1115751 A CN 1115751A CN 94107849 CN94107849 CN 94107849 CN 94107849 A CN94107849 A CN 94107849A CN 1115751 A CN1115751 A CN 1115751A
- Authority
- CN
- China
- Prior art keywords
- extracting
- tobacco
- solanesol
- nicotine
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacture Of Tobacco Products (AREA)
Abstract
The tobacco with its nicotine extracted is stove-dried, crushed, extracted for several times with C5-C12 alkane as solvent. Obtained extracts are mixed and concentrated, saponified with alcohol and alkali solution, after removing water and solvent, treated with mixed ketone and alcohol liquid I and II separately, and cooled to separate pure solanesol crystal. The said process can produce high pure product.
Description
The present invention is a kind of method of extracting solanesol from the tobacco of extracting nicotine, belongs to the manufacturing and the method for purification of chemical industry intermediate.
The English name of solanesol is Solanesol, and molecular formula is H[CH
2C (CH
3) CHCH
2]
9OH, formal name used at school be 3,7,11,15,19,23,27,31,35-nine methyl-2,6,10,14,18,22,26,30,34, and-hexatriacontane nine alkene-1-alcohol, molecular weight are 631, and pure product are white powdery solid, and fusing point is 41 ℃, is synthesizing coenzyme Q
10And vitamin K
2Main intermediate, also be the important intermediate of making some anti-allergy agent, anti-ulcerative drug, hypolipidemic and anticarcinogen.People's whats such as R.L.Rowland were found (J.A.C.S.78.4680.1956) in 1956 the earliest from tobacco.United States Patent (USP) U.S.Pat No:4,013,731 has reported the method for extracting solanesol from the potato leaf; U.S.3,526,667 have reported the method for extracting solanesol from mulberry leaf; Japanese Patent (openly specially permit the clear 52-139711 1977.11.12 of communique, openly specially permit the clear 54-138510 1979.10.27 of communique (A) and openly specially permit the clear 63-190840 1988.8.8 of communique (A)) etc. to have reported with the tobacco be raw material, with pure hexane is the solanesol extracting method of solvent, and its treating process step is many, productive rate is low, and content is that 90% product at room temperature still is dope.In China, Zhang Deyu has invented the technology (application for a patent for invention prospectus CN 1056486 A) for preparing solanesol with mould cigarette or tobacco waste, and what he obtained is that content is twenties percent crude product, does not have the content of purifying aspect.Retrieval shows extracts the solanesol and the report of the technology of purifying in addition in the tobacco of all having no way of both at home and abroad having extracted nicotine.
Purpose of the present invention is used to the tobacco of extracting nicotine at what, obtains the very high content of economic worth at the pure product of the solanesol more than 90% with the simplest and the most direct method.
According to method of the present invention, at first will extract the tobacco oven dry of nicotine, make moisture below 10%, be crushed to then below the particle diameter 10mm, press tobacco leaf weight the volume of solvent is added C with 1: 3～8
5～C
12Fat alkane stirred 30～80 minutes to the temperature that is lower than below the solvent boiling point in room temperature, extracted 2～4 times, filtration, merging filtrate, concentrated, added pure alkaline solution saponification, added water after the saponification, leave standstill and discard water layer, solvent evaporated is respectively handled once with ketone and pure mixed solvent I and mixed solvent II, and crystallization and drying are separated out in cooling, can get purity and be the solid solanesol more than 90%, yield can reach about 1%.
The present invention compares its advantage at what with the past similar inventions:
1, utilizes the tobacco leaf that had extracted nicotine to obtain valuable solanesol, realized turning waste into wealth.
2, the present invention is the solanesol extracts active ingredients in the tobacco manufactured goods, and economic worth increases more than four times at least, and does not require the existing nicotine extraction process of change.
3, the solanesol that adopts of the present invention extract and purifying process all simpler than the method that has abroad adopted, and extract yield and product purity all is significantly improved, therefore the industrial production of more convenient mass-producing.
Operational flowchart of the present invention is as follows: figure (1)
Embodiment 1:
The tobacco of extracting nicotine is dried to water content below 8%, be crushed to particle diameter below 2mm.Get this broken tobacco 200 grams, add and have agitator, thermometer, in 2000 milliliters of reactors of well heater and reflux condensing tube, the reprocessing industry is tasted with discrimination 1000 milliliters of normal heptanes, be heated with stirring to mixture temperature and reach 40-60 ℃, keep this temperature to stir 60 minutes, filter, the filter quarrel adds in the reactor again, processing industry is tasted with discrimination 800 milliliters of normal heptanes, reheat stirred 60 minutes, filter, with 2000 milliliters of normal heptane leaching quarrels once, press dry, merging filtrate, under heating in water bath, be concentrated into 100 milliliters, add 100 milliliters of pure alkaline solutions (adding 2 gram sodium hydroxide in 100 milliliters of ethanol is made into) again, stir at 50 ℃ and carried out saponification in 3 hours with rotary film evaporator, add 50～100 milliliters in water after the saponification, stirred 30 minutes, static layering discards water layer, organic solvent is removed in evaporation, dope, with 60 milliliters of mixed solvent I[acetone: ethanol (V/V)=4: 1] dissolving, remove by filter insolubles, concentrating filter liquor gets the brown dope, in this dope, add 200 milliliters of mixed solvent II[acetone: ethanol (V/V)=10: 100], 50 ℃ of following heating for dissolving, cooling, isolate crystallization, cryodrying gets the yellow solid crystallization.
Embodiment 2:
To extract the tobacco leaf drying of nicotine to containing moisture below 8%, be crushed to particle diameter below 5mm, get this broken tobacco 1000 grams, 4.5 liters of processing industry product normal hexanes, with embodiment 1 device, 60 ℃ of following heated and stirred 60 minutes, filter, the filter quarrel is extracted once with 4.5 liters of normal hexanes again, merging filtrate, heating concentrates, during to remaining 500 milliliters, add 1000 milliliters of pure alkaline solutions (adding 5 gram potassium hydroxide in 100 milliliters of ethanol is made into), be heated to 50 ℃ and stirred 4 hours, add 1200 milliliters in water, to layering, discard water layer, organic solvent layer steams normal hexane with 40 gram anhydrous sodium sulfate dryings, and remaining dope is with mixed solvent I[butanone: methyl alcohol (V/V)=3: 1] and mixed solvent II[butanone: methyl alcohol (V/V)=6: 100] the method processing of pressing embodiment 1, as when adding mixed solvent II, adding decolorizing charcoal, can obtain the faint yellow xln more shallow than embodiment 1 color.
Embodiment 3:
By above-mentioned example 1 step to the tobacco of extraction nicotine not and the tobacco of extraction nicotine compare test, to be the solanesol productive rate of not carrying nicotine exceed 3% than what carry nicotine to the result.
Figure (1)
Claims (8)
1, a kind of method of from the tobacco of extracting nicotine, extracting solanesol.It is characterized in that adopting the tobacco of having extracted nicotine is raw material, through oven dry, pulverizing, with C
5～C
12Fat alkane is as solvent, extraction several, and united extraction liquid is concentrated, and adds pure alkaline solution saponification, removes and anhydrates and solvent, respectively handles once with ketone and pure mixed solvent I and mixed solvent II, and crystallization is separated out in cooling.
2, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1 is characterized in that the described Tobacco drying that extracted nicotine is to water content below 10%.
3, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1 is characterized in that it is below the 10mm that the described tobacco powder that extracted nicotine is broken to particle diameter.
4, the method for from the tobacco of extracting nicotine, extracting solanesol according to claim 1, it is characterized in that described with fat alkane when extracting solvent, the add-on of solvent is 1: 3～8 by tobacco weight to the volume ratio of solvent.
5, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1, the proportioning that it is characterized in that described pure alkaline solution are to add 2～5 gram sodium hydroxide or potassium hydroxide in 100 milliliters of alcohol.
6, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1, it is characterized in that described mixed solvent I is by ketone: the volumetric ratio of alcohol is 0.5～8: 1 preparation.
7, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1, it is characterized in that described mixed solvent II is by ketone: the volumetric ratio of alcohol is 0.5～20: 100 preparations.
8, the method for extracting solanesol from the tobacco of extracting nicotine according to claim 1 is characterized in that in the described operation steps can adding decolorizing charcoal adding mixed solvent II when handling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107849 CN1115751A (en) | 1994-07-19 | 1994-07-19 | Extraction process of solanesol from tobacco with the nicotine extracted |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107849 CN1115751A (en) | 1994-07-19 | 1994-07-19 | Extraction process of solanesol from tobacco with the nicotine extracted |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1115751A true CN1115751A (en) | 1996-01-31 |
Family
ID=5033234
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94107849 Pending CN1115751A (en) | 1994-07-19 | 1994-07-19 | Extraction process of solanesol from tobacco with the nicotine extracted |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1115751A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100417632C (en) * | 2004-08-06 | 2008-09-10 | 昆明韬辉生物工贸有限责任公司 | Method for extraction of high purity solanocupsin and synthesis of isodecyl dienol and isoprenol |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN102408312A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for separating and purifying solanesol through subsection crystallization |
| CN104606918A (en) * | 2015-01-21 | 2015-05-13 | 云南中海路德科技有限公司 | Comprehensive development and utilization method for tobacco stems in tobacco planting process |
-
1994
- 1994-07-19 CN CN 94107849 patent/CN1115751A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100417632C (en) * | 2004-08-06 | 2008-09-10 | 昆明韬辉生物工贸有限责任公司 | Method for extraction of high purity solanocupsin and synthesis of isodecyl dienol and isoprenol |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN102408312A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for separating and purifying solanesol through subsection crystallization |
| CN102408312B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for separating and purifying solanesol through subsection crystallization |
| CN104606918A (en) * | 2015-01-21 | 2015-05-13 | 云南中海路德科技有限公司 | Comprehensive development and utilization method for tobacco stems in tobacco planting process |
| CN104606918B (en) * | 2015-01-21 | 2016-02-10 | 云南中海路德科技有限公司 | The comprehensive development and utilization method of tobacco rod in tobacco leaf planting process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100497343C (en) | Method for preparing ellagic acid by pomegranate rind | |
| CN107353183A (en) | A kind of method that high-content of resveratrol is extracted from giant knotweed | |
| JPH0324084A (en) | Separation and refining of gingkoride from gingko leaves | |
| CN101016235B (en) | Method of extracting gossypol acetate from cotton seed oil niger | |
| CN102070411B (en) | Method for refining honokiol | |
| CN107337593B (en) | Preparation method of coenzyme Q10 pure product | |
| CN114380829A (en) | Pentoxifylline and synthetic method and application thereof | |
| CN106832045B (en) | A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously | |
| CN1115751A (en) | Extraction process of solanesol from tobacco with the nicotine extracted | |
| CN111018819B (en) | Preparation method of luteolin | |
| CN100418969C (en) | Process for preparing natural chlorophyll and products thereof with spearmint as raw material | |
| CN106810619A (en) | A kind of gingko episperm pectin and polypentenol extracting method | |
| CN1224022A (en) | New process for extracting tea saponin | |
| CN109771475A (en) | A method of extracting polyphenol from purple perilla seed shell | |
| CN113354526B (en) | Alkali purification method of coenzyme Q10 | |
| CN1054068C (en) | Method for preparation of puerarin | |
| CN1054788A (en) | Process for extracting grease and tea saponin by one-step leaching of cake dregs | |
| CN111848458B (en) | Process for extracting dicyandiamide in process of preparing 3-mercaptopropionic acid | |
| CN1032753C (en) | Process for preparing tea natural alkaloid-caffeine | |
| US4313880A (en) | Extractive process for preparing apigenin | |
| CN108101761B (en) | Preparation method of curcumin | |
| CN1026485C (en) | Process for preparing solanesol from mouldy tobacco or tobacco waste | |
| CN102697838A (en) | Method for extracting and separating flavone enrichment substance, saponin enrichment substance and polysaccharide from astragalus simultaneously | |
| CN112592332A (en) | Preparation process of high-purity nicotine | |
| CN1150027A (en) | Method for extracting available composition of chrysanthemum flower |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |