CN112321564A - Extraction process of nicotine in waste tobacco leaves - Google Patents
Extraction process of nicotine in waste tobacco leaves Download PDFInfo
- Publication number
- CN112321564A CN112321564A CN202011244635.8A CN202011244635A CN112321564A CN 112321564 A CN112321564 A CN 112321564A CN 202011244635 A CN202011244635 A CN 202011244635A CN 112321564 A CN112321564 A CN 112321564A
- Authority
- CN
- China
- Prior art keywords
- extraction
- nicotine
- waste tobacco
- tobacco leaves
- drying
- 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
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 36
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229960002715 nicotine Drugs 0.000 title claims abstract description 36
- 238000000605 extraction Methods 0.000 title claims abstract description 31
- 241000208125 Nicotiana Species 0.000 title claims abstract description 28
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 28
- 239000002699 waste material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 9
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000001256 steam distillation Methods 0.000 abstract description 5
- 238000000638 solvent extraction Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 241000282414 Homo sapiens Species 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010034010 Parkinsonism Diseases 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000658 coextraction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic 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
- C07D401/02—Heterocyclic 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
- C07D401/04—Heterocyclic 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses an extraction process of nicotine in waste tobacco leaves, which adopts supercritical CO2The extraction agent is used for carrying out supercritical extraction on waste tobacco leaf raw material particles after drying, crushing, granulating and drying the particles to obtain the nicotine extract. The extraction step of nicotine in the process is simple, the waste tobacco raw materials only need to be dried, crushed, granulated and the like, and the process is suitable for industrial and large-scale production processes. Compared with a steam distillation method, a solvent extraction method and a subcritical extraction combined separation distillation extraction technology, the method has the advantages that the raw materials are granulated and then dried in advance, the ethanol solvent brought in during granulation is removed, and no solvent residue is ensured in the extract without other operations; and the process route in the invention has no harm to the environment, operators and even the extract, is more green and safe, and is more in line with the pursuit of human beings.
Description
Technical Field
The invention relates to the technical field of natural product extraction and separation, in particular to a process for extracting nicotine from waste tobacco leaves.
Background
Nicotine is a major alkaloid in tobacco and is a colorless or pale yellow oily liquid. The natural nicotine has wide application, and can be used as residue-free and pollution-free high-efficiency pesticide for edible crops such as grains, oil plants, vegetables, fruits and the like, biological crops and the like. The use of nicotine in medicine is increasingly recognized. Studies have found that non-smokers have a much higher prevalence in patients with alzheimer's disease and parkinson's syndrome than smokers, suggesting that nicotine has a potential pharmacodynamic effect that has not yet been developed.
The traditional nicotine extraction methods include steam distillation, organic solvent extraction, subcritical extraction and ion resin exchange. The steam distillation method is the earliest method for producing nicotine, the content of nicotine produced by the method is low, and the industrial production is usually carried out by combining a solvent extraction method and the steam distillation method so as to obtain high-purity nicotine, but the use of more organic solvents not only can cause adverse effects on the environment, but also has the risk of solvent residue in the obtained nicotine product.
Disclosure of Invention
The invention aims to provide an extraction process of high-purity nicotine in waste tobacco leaves, which adopts simple operation steps to obtain a product with high nicotine purity.
The technical scheme of the invention is realized as follows:
a process for extracting nicotine from waste tobacco leaf by supercritical CO extraction2The extraction agent is used for carrying out supercritical extraction on waste tobacco leaf raw material particles after drying, crushing, granulating and drying the particles to obtain the nicotine extract.
Wherein the drying temperature before the waste tobacco leaves are crushed is 90-105 ℃, and the drying time is 1.5-3 h; and (2) wetting the crushed material by adding a 95% alcohol solution with the mass of 20-40% of the raw material, then granulating by using a 10-20 mesh screen, drying the granulated waste tobacco leaf particles in a constant-temperature oven at 45-70 ℃, and then performing supercritical extraction under the conditions that the extraction temperature is 45-60 ℃, the extraction pressure is 32-40 MPa, the separation temperature is 40-55 ℃ and the separation pressure is 6-8 MPa.
The invention has the beneficial effects that: the extraction process of nicotine is simple, the waste tobacco raw materials only need to be dried, crushed, granulated and the like, and the method is suitable for industrial and large-scale production processes. Compared with a steam distillation method, a solvent extraction method and a subcritical extraction combined separation distillation extraction technology, the method has the advantages that firstly, the raw materials are dried in advance after being granulated, the ethanol solvent brought in during granulation is removed, no solvent residue is ensured in the extract, and other operations are not needed; the content of nicotine in the extract obtained by the method is high, separation and purification operations can be omitted, and the production cost is greatly saved; finally, the process route in the invention is harmless to the environment, operators and even the extract, and is more green and safe.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the following examples.
Example 1:
the waste tobacco leaves are dried at the temperature of 95 ℃ for 3 hours, crushed, added with 95 percent ethanol with the mass of 20 percent of that of the raw materials for granulation, dried at the temperature of 50 ℃ to remove the ethanol, and subjected to supercritical extraction at the extraction pressure of 32MPa, the extraction temperature of 45 ℃, the separation pressure of 6.8MPa and the separation temperature of 45 ℃, the extraction rate of nicotine in the waste tobacco leaves is 91.74 percent, and the purity of the nicotine in the obtained extract is 54.65 percent.
Example 2:
drying the waste tobacco leaves at 100 ℃ for 2h, adding 95% ethanol with the mass of 30% of the raw materials after crushing, granulating, drying at 60 ℃ to remove ethanol, performing supercritical extraction at the extraction pressure of 35MPa, the extraction temperature of 50 ℃, the separation pressure of 7MPa and the separation temperature of 52 ℃, wherein the extraction rate of nicotine in the waste tobacco leaves is 92.48%, and the purity of nicotine in the obtained extract is 55.77%.
Example 3:
the waste tobacco leaves are dried at the temperature of 105 ℃ for 1.5h, crushed, added with 95% ethanol with the mass of 35% of the raw materials for granulation, dried and removed of ethanol at the temperature of 65 ℃, and subjected to supercritical extraction at the extraction pressure of 38MPa, the extraction temperature of 53 ℃, the separation pressure of 7MPa and the separation temperature of 55 ℃, the extraction rate of nicotine in the waste tobacco leaves is 92.37%, and the purity of nicotine in the obtained extract is 54.98%.
Example 4:
the waste tobacco leaves are dried at the temperature of 105 ℃ for 1.5h, crushed, added with 95 percent ethanol with the mass of 40 percent of that of the raw materials for granulation, dried at the temperature of 70 ℃ to remove the ethanol, and subjected to supercritical extraction at the extraction pressure of 40MPa, the extraction temperature of 55 ℃, the separation pressure of 7MPa and the separation temperature of 55 ℃, the extraction rate of nicotine in the waste tobacco leaves is 91.94 percent, and the purity of the nicotine in the obtained extract is 55.84 percent.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (6)
1. A process for extracting nicotine from waste tobacco leaves is characterized by comprising the following steps: by supercritical CO2The extraction agent is used for carrying out supercritical extraction on waste tobacco leaf raw material particles after drying, crushing, granulating and drying the particles to obtain the nicotine extract.
2. The process for extracting nicotine from waste tobacco leaves as claimed in claim 1, wherein: the drying temperature before crushing is 90-105 ℃, and the drying time is 1.5-3 h.
3. The process for extracting nicotine from waste tobacco leaves as claimed in claim 1, wherein: and in the granulation, 95% alcohol solution is added to wet the crushed materials, and then granulation is carried out by using a 10-20-mesh screen.
4. The process for extracting nicotine from waste tobacco leaves as claimed in claim 3, wherein: the addition amount of 95% alcohol during granulation is 20-40%.
5. The process for extracting nicotine from waste tobacco leaves as claimed in claim 1, wherein: and drying the particles in a constant-temperature oven at the temperature of 45-70 ℃.
6. The process for extracting nicotine from waste tobacco leaves as claimed in claim 1, wherein: the supercritical extraction temperature is 45-60 ℃, the extraction pressure is 32-40 MPa, the separation temperature is 40-55 ℃, and the separation pressure is 6-8 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011244635.8A CN112321564A (en) | 2020-11-10 | 2020-11-10 | Extraction process of nicotine in waste tobacco leaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011244635.8A CN112321564A (en) | 2020-11-10 | 2020-11-10 | Extraction process of nicotine in waste tobacco leaves |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112321564A true CN112321564A (en) | 2021-02-05 |
Family
ID=74316526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011244635.8A Pending CN112321564A (en) | 2020-11-10 | 2020-11-10 | Extraction process of nicotine in waste tobacco leaves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112321564A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020165392A1 (en) * | 2000-02-25 | 2002-11-07 | Kim Jin Woong | Method of preparing alkaloids using supercritical fluids from plants |
| CN104311534A (en) * | 2014-06-10 | 2015-01-28 | 苏州泽达兴邦医药科技有限公司 | Method for separating and purifying nicotine by supercritical-molecular distillation combined technology |
| CN104725351A (en) * | 2015-02-15 | 2015-06-24 | 洛阳市甘霖生物技术有限公司 | Method of extracting high-purity nicotine from waste tobacco |
| CN105011354A (en) * | 2015-05-06 | 2015-11-04 | 济南九州富得香料有限责任公司 | Method for supercritical CO2 extraction of upper-tobacco leaves of tobaccos, extract and application |
| CN106749172A (en) * | 2016-11-22 | 2017-05-31 | 中国烟草总公司郑州烟草研究院 | A kind of method that utilization subcritical abstraction molecular clock GC-MS purifies nicotine |
| CN110437203A (en) * | 2019-07-15 | 2019-11-12 | 湖南鑫文天生物科技有限公司 | Scale Continuous Countercurrent Extraction and supercritical carbon dioxide extracting nicotine group technology |
-
2020
- 2020-11-10 CN CN202011244635.8A patent/CN112321564A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020165392A1 (en) * | 2000-02-25 | 2002-11-07 | Kim Jin Woong | Method of preparing alkaloids using supercritical fluids from plants |
| CN104311534A (en) * | 2014-06-10 | 2015-01-28 | 苏州泽达兴邦医药科技有限公司 | Method for separating and purifying nicotine by supercritical-molecular distillation combined technology |
| CN104725351A (en) * | 2015-02-15 | 2015-06-24 | 洛阳市甘霖生物技术有限公司 | Method of extracting high-purity nicotine from waste tobacco |
| CN105011354A (en) * | 2015-05-06 | 2015-11-04 | 济南九州富得香料有限责任公司 | Method for supercritical CO2 extraction of upper-tobacco leaves of tobaccos, extract and application |
| CN106749172A (en) * | 2016-11-22 | 2017-05-31 | 中国烟草总公司郑州烟草研究院 | A kind of method that utilization subcritical abstraction molecular clock GC-MS purifies nicotine |
| CN110437203A (en) * | 2019-07-15 | 2019-11-12 | 湖南鑫文天生物科技有限公司 | Scale Continuous Countercurrent Extraction and supercritical carbon dioxide extracting nicotine group technology |
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|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210205 |
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| RJ01 | Rejection of invention patent application after publication |