CN1091767C - Nicotine extraction process - Google Patents
Nicotine extraction process Download PDFInfo
- Publication number
- CN1091767C CN1091767C CN99105952A CN99105952A CN1091767C CN 1091767 C CN1091767 C CN 1091767C CN 99105952 A CN99105952 A CN 99105952A CN 99105952 A CN99105952 A CN 99105952A CN 1091767 C CN1091767 C CN 1091767C
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- CN
- China
- Prior art keywords
- extraction
- nicotine
- phase
- extracting
- tobacco leaf
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- 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.)
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- 238000000605 extraction Methods 0.000 title claims abstract description 48
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 27
- 229960002715 nicotine Drugs 0.000 title claims abstract description 27
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 241000208125 Nicotiana Species 0.000 claims abstract description 14
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims description 11
- 238000007670 refining Methods 0.000 claims description 11
- 239000000779 smoke Substances 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000009834 vaporization Methods 0.000 claims description 5
- 230000008016 vaporization Effects 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 4
- 238000000638 solvent extraction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000006200 vaporizer Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 240000000249 Morus alba Species 0.000 claims description 2
- 235000008708 Morus alba Nutrition 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims 1
- 238000003809 water extraction Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 5
- 239000000706 filtrate Substances 0.000 abstract description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 5
- YHBIGBYIUMCLJS-UHFFFAOYSA-N 5-fluoro-1,3-benzothiazol-2-amine Chemical compound FC1=CC=C2SC(N)=NC2=C1 YHBIGBYIUMCLJS-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- UOUKIRCMEDQIDS-UHFFFAOYSA-N ethyl acetate 3-(1-methylpyrrolidin-2-yl)pyridine Chemical compound C(C)(=O)OCC.N1=CC=CC(=C1)C1N(C)CCC1 UOUKIRCMEDQIDS-UHFFFAOYSA-N 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Manufacture Of Tobacco Products (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A new process for extracting nicotine comprises leaching tobacco leaf with hot water, and adding Ca (OH) into the leaching solution2And CO2Neutralizing, filtering, extracting the filtrate, namely refined tobacco juice, with ethyl acetate or chloroform in a packed tower, evaporating the extract phase to obtain a product containing 75-85% of free nicotine, and evaporating the raffinate phase to recover the extractant, so that the raffinate phase can be recycled as hot water for extraction. The process has the advantages of simple equipment, convenient operation, no waste water, waste gas and waste material generation, and accordance with the requirements of industrial production.
Description
The present invention relates to a kind of nicotine extraction process.
The extraction process of nicotine is a lot, as classical extraction method; Dry distillation extraction method, ion exchange extraction method, water logging organic solvent extractionprocess, these methods respectively have its relative merits, and the finished product of these technologies all are nicotine sulfate.Wherein using more is the water logging organic solvent extractionprocess, and it has advantages such as technology is reasonable, equipment is simple, but a lot of shortcomings are also arranged, and at first because its product is a nicotine sulfate, needs in the technology to use dilute sulphuric acid, thereby causes equipment corrosion; Moreover a large amount of waste water can not reuse in the technology, cause environmental pollution; The 3rd in technology because of using Na
2CO
3, make shortcomings such as production cost rising.
The objective of the invention is on the basis of water logging organic solvent extractionprocess, overcome the many shortcomings that exist in the former technology, is purpose to produce free nicotine, invents the new extraction process of a kind of nicotine.
The present invention mainly by tobacco leaf through flooding, vat liquor neutralization, filter, form with production technique such as organic solvent extraction, extraction phase evaporations, its technology comprises the steps:
A. with tobacco leaf through the hot water lixiviate, must contain the vat liquor of nicotine 1.5～2.0%;
B. the vat liquor with A step gained neutralizes, and filter with pressure filter the neutralization back, gets refining smoke succus;
C. with step B gained refining smoke succus, enter packing tower, use organic solvent extraction, get extraction phase and extracting phase;
D. step C gained extraction phase is entered evaporator evaporation, obtain the free nicotine of content 70～80%;
E. C step gained extracting phase is entered the solvent recuperation vaporizer, recovered solvent enters the extraction tower recycling, and the water behind the recovery solvent enters the recycling of tobacco leaf extracting technology.
Below narrate detailed content of the present invention:
A. the fragment of lixiviate raw tobacco through being ground into size about 0.5cm * 0.5cm-2cm * 2cm is the lixiviate materials.Mulberry Ke Shi extraction is adopted in lixiviate.Preimpregnation 8-12 hour, back continuous extraction 4-6 time, each 1-3 hour, lixiviate 12-30 hour altogether.The lixiviate water temperature remains on 30～40 ℃, presoak as in and materials.Surplus scarp contains below the nicotine 0.3% (wet basis) after the lixiviate, does him in addition and uses.
B. neutralization.In and in the reactor that tool stirs, carry out.At first in still, add presoak, be warming up to 40-60 ℃, add Ca (OH)
2Making still liquid pH is 14.Continue to be warming up to 70-80 ℃, react after 1 hour, be cooled to 40～50 ℃, in still, feed the CO of 3-4% again
2Gas reacted after 1 hour, became solidliquid mixture in the still, entered filter and filtered, and filtered liquid is refining smoke succus.
C. extraction.Extraction is carried out in packing tower, and extraction agent is ethyl acetate or chloroform, extraction temperature 30-35 ℃.Extraction agent and refining smoke succus are counter-current flow in extraction tower, increase two liquid phase contacts area by packing layer, to improve extraction efficiency.The liquid flowing ratio of extraction agent and refining smoke succus is decided to be 1: 6 (volume ratio), must be rich in the extraction phase of free nicotine at the extraction cat head, must contain the extracting phase of a small amount of extraction agent at the bottom of the tower.
D. evaporation.Evaporative process adopts natural-circulation evaporator with the extraction agent in the evaporation extraction phase, obtains containing the product of free nicotine 70～80%, vaporization temperature 80-90 ℃.Adopt the forced circulation evaporation extracting phase to be dissolved in a small amount of extraction agent in the extracting phase with recovery, the extracting phase after being evaporated has reduced environmental pollution on the one hand as lixiviate hot water, and one side has been saved diffusion water.90-95 ℃ of extracting phase vaporization temperature
Fig. 1 is a process flow diagram of the present invention.
The present invention can provide by following embodiment:
Embodiment: take by weighing and contain nicotine 4.5%, moisture 9% tobacco leaf fragment (1000kg of 1cm * 1cm) drops in the lixiviate jar, adds hot water (35 ℃) 3000kg, and the insulation lixiviate is after 10 hours, a step vat liquor 2000kg; Go into the lixiviate of 3000kg hot water in the lixiviate jar successively, each lixiviate 2 hours totally 5 times, gets two, three, four, five, six step vat liquors; After extracting 6 times, remove scarp, add new tobacco leaf, go on foot liquid lixiviates 10 hours with two of lixiviate last time, get a step vat liquor 2000kg, add three, four, five, six step vat liquor and hot water lixiviates of gained last time more successively, two, three, four, five, the six step vat liquors of getting back; Remove scarp, add new tobacco leaf, use the same method and step is carried out lixiviate.
One step liquid 2000kg of lixiviate gained contains nicotine 2.2%, is heated to 60 ℃, adds Ca (OH)
280kg, 75 ℃ of holding temperatures, stirring reaction is cooled to 40 ℃ after 1 hour, feed CO in still
280kg reacted 1 hour, filtered solidliquid mixture in the still, got filtrate (refining smoke succus) 2000kg.Refining smoke succus enters packing tower, uses ethyl acetate extraction, and the throughput ratio of cigarette juice and extraction agent is: the refining smoke succus flow: ethyl acetate flow=6: 1 (volume ratio) gets nicotine ethyl acetate solution 357kg, nicotine content 12.3% after the extraction.The nicotine ethyl acetate solution enters vaporizer, 95 ℃ of vaporization temperatures, and atmospheric evaporation must contain the concentrated solution 50.7kg of nicotine 84.5%.This concentrated solution is nicotine products.
Claims (6)
1. nicotine novel technology for extracting is characterized in that by tobacco leaf through flooding, the vat liquor neutralization, filters, and with the production technique that organic solvent extraction, extraction phase evaporation are formed, its technology comprises the steps:
A. with tobacco leaf through the hot water lixiviate, must contain the vat liquor of nicotine 1.5～2.0%;
B. the vat liquor with A step gained neutralizes, and filter with pressure filter the neutralization back, gets refining smoke succus;
C. with step B gained refining smoke succus, enter packing tower, use organic solvent extraction, get extraction phase and extracting phase;
D. step C gained extraction phase is entered evaporator evaporation, obtain the free nicotine of content 70～80%;
E. C step gained extracting phase is entered the solvent recuperation vaporizer, recovered solvent enters the extraction tower recycling, and the water behind the recovery solvent enters the recycling of tobacco leaf extracting technology.
2. nicotine extraction process as claimed in claim 1 is characterized in that the hot water extraction temperature is 30～40 ℃ in the steps A, and with mulberry Ke Shi method circulation lixiviate, preimpregnation for the first time is 8-12 hour in the circulation, and the continuous extraction tobacco leaf is 4-6 time again, each 1-3 hour.
3. nicotine extraction process as claimed in claim 1 is characterized in that among the step B, earlier vat liquor is heated to about 50 ℃, again the Ca (OH) that adds to vat liquor
2Powder is warming up to 70-80 ℃, reacts after 1 hour, to the CO that wherein feeds vat liquor weight 3～4%
2Gas reacted 1 hour, was cooled to 40～50 ℃ simultaneously, filtered neutralizer, got refining smoke succus.
4. nicotine extraction process as claimed in claim 1 is characterized in that among the step C, and packing tower is adopted in extraction, and extraction is ethyl acetate or chloroform with solvent, and temperature is 30～35 ℃.
5. nicotine extraction process as claimed in claim 1 is characterized in that among the step D, and natural-circulation evaporator is adopted in evaporation, 80～90 ℃ of vaporization temperatures, and recovered solvent is as the extraction agent among the poly-C of step, and concentrated solution is nicotine products.
6. nicotine extraction process as claimed in claim 1 is characterized in that in the step e that the vaporization temperature of extracting phase is 90～95 ℃, and recovered solvent reuses as extraction agent, and the water behind the recovery solvent enters the recycling of tobacco leaf lixiviate workshop section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99105952A CN1091767C (en) | 1999-04-23 | 1999-04-23 | Nicotine extraction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99105952A CN1091767C (en) | 1999-04-23 | 1999-04-23 | Nicotine extraction process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1234403A CN1234403A (en) | 1999-11-10 |
| CN1091767C true CN1091767C (en) | 2002-10-02 |
Family
ID=5272195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99105952A Expired - Fee Related CN1091767C (en) | 1999-04-23 | 1999-04-23 | Nicotine extraction process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1091767C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093336B (en) * | 2010-11-26 | 2013-02-13 | 武汉淡雅香科技发展股份有限公司 | Method for extracting alkaloid by utilizing waste water and sludge of tobaccos |
| CN102070285B (en) * | 2010-11-26 | 2013-01-09 | 武汉淡雅香科技发展股份有限公司 | Tobacco wastewater sludge activation and recycling method |
| CN102516226B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for distilling and refining nicotine circularly and nicotine distilling and absorbing device |
| CN102516227B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for flocculating, decolorizing, separating and purifying nicotine |
| CN102659760B (en) * | 2012-04-12 | 2013-12-18 | 湖南省健鑫生物科技有限公司 | Extraction technology of nicotine by acid process |
| CN102703218A (en) * | 2012-06-15 | 2012-10-03 | 川渝中烟工业有限责任公司 | Method for extracting neutral fragrance ingredients from tobacco leaves |
| CN109512014A (en) * | 2017-09-18 | 2019-03-26 | 湖南中烟工业有限责任公司 | A method of the extraction nicotine from tobacco |
| CN110511210A (en) * | 2019-09-12 | 2019-11-29 | 许达勇 | High purity nicotine production technology |
| CN111777591A (en) * | 2020-07-16 | 2020-10-16 | 晨光生物科技集团股份有限公司 | Method for rapidly preparing nicotine crude product |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146454A (en) * | 1995-09-29 | 1997-04-02 | 吉林市万发实业有限公司 | Technology for extracting nicotine from tobacco leaf |
-
1999
- 1999-04-23 CN CN99105952A patent/CN1091767C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146454A (en) * | 1995-09-29 | 1997-04-02 | 吉林市万发实业有限公司 | Technology for extracting nicotine from tobacco leaf |
Non-Patent Citations (1)
| Title |
|---|
| 黑龙江大学自然科学学报第12卷第1期 1995.3.1 孙志忠等，烟提取方法的研究 * |
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| Publication number | Publication date |
|---|---|
| CN1234403A (en) | 1999-11-10 |
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