CN1074103A - Production method of natural nicotine for cigarette - Google Patents
Production method of natural nicotine for cigarette Download PDFInfo
- Publication number
- CN1074103A CN1074103A CN 93110817 CN93110817A CN1074103A CN 1074103 A CN1074103 A CN 1074103A CN 93110817 CN93110817 CN 93110817 CN 93110817 A CN93110817 A CN 93110817A CN 1074103 A CN1074103 A CN 1074103A
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- CN
- China
- Prior art keywords
- liquid
- cigarette
- extraction
- production method
- nicotine
- 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.)
- Granted
Links
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 32
- 229960002715 nicotine Drugs 0.000 title claims abstract description 32
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000002386 leaching Methods 0.000 claims description 13
- 239000000284 extract Substances 0.000 claims description 10
- 230000002411 adverse Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 3
- 150000001350 alkyl halides Chemical class 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 2
- 238000000622 liquid--liquid extraction Methods 0.000 claims 1
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 241000208125 Nicotiana Species 0.000 abstract description 11
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 7
- 239000000654 additive Substances 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 239000003205 fragrance Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- -1 methyl hydrogen pyrroles Chemical class 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 description 1
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 235000019506 cigar Nutrition 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 125000000596 cyclohexenyl group Chemical class C1(=CCCCC1)* 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229940043353 maltol Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention provides a production method of natural nicotine for cigarette, and is characterized by that it uses tobacco powder as raw material, uses water as lixiviant to make solid-liquid countercurrent lixiviation extraction, and after the impurities are removed from the lixivium by separation, the organic solvent is used to make liquid-liquid countercurrent extraction, and after the extraction liquor is refined and the solvent is removed, the tobacco lye containing 70-90% of natural nicotine is made up. The method of the invention has the advantages of continuous operation, small solvent loss, low energy consumption, simple equipment, convenient operation and high extraction efficiency. The obtained product contains active ingredients such as tobacco strength, tobacco fragrance and the like besides nicotine, does not contain harmful impurities, and is mainly used as a cigarette additive.
Description
The present invention relates to a kind of extracting method of natural components, particularly relate to a kind of production method of natural nicotine for cigarette.
Be that the method for raw material extraction nicotine has a variety of process forms with tobacco at present, as steam distillation, its energy consumption is big, and pollution and inconvenient operation are arranged.The hot gas rule is to extract with hot-air, hot CO2 and superheated steam, and temperature is up to 155～165 ℃, the cost of equipment height, and the operating time is long.And solvent extraction is an effective method comparatively.A kind of method that tobacco extracts is provided is disclosed as Chinese patent notification number 1034479A, be that the solvent with water signature carries out leaching to tobacco-containing material under the normal temperature, get the powder extract then after the spray-drying, carry out the leaching second time with organic solution as alcohol, ether, alkyl halide etc. again, remove with vacuum distillation or thin film evaporation technology etc. and to desolvate, thereby make highly enriched tobacco extracts.All adopt the non-flowing type leaching in this method, low temperature carries out, and is generally 15-30 ℃, and discontinuous production, extraction efficiency are low.Nicotine content is low in the concentrated extract of gained, and impurity is more, should not be used for cigarette and make additive.
The object of the present invention is to provide a kind of production method that adopts the leaching extraction of solid-liquid adverse current and liquid-natural nicotine for cigarette that the liquid counter-current extraction combines.
The production method of natural nicotine for cigarette of the present invention is, with the offal is raw material, offal comprises pipe tobacco, blade slag that cigar mill and redrying field abandon and the various tobacco leaves that can not be used as the cigarette raw material, accord with Q/DJHY-02-91 raw material standard, be outward appearance do not have go mouldy, no silt particle, free from admixture, granularity 0.5～5mm, water content≤20%, nicotine content 〉=0.6%.Earlier use water-wet as the solid-liquid leaching is last, wetness degree can be pinched agglomerating being advisable with hand, and adds alkali and mix available calcium oxide, calcium hydroxide, NaOH or sodium carbonate etc.Mixed premix is placed in the lixiviation apparatus, with water is lixivant, general drinking water with pH5-6 is for well, and the extraction ratio is an offal: water=1: 2～2.5, under 50～90 ℃ of temperature, carry out solid-liquid adverse current leaching extraction, to extract water-soluble tobacco composition, pH 〉=11 of control leachate, nicotine content＞0.15%.Then lixivium is separated and remove impurity, generally adopt first natural subsidence, remove precipitation, suspension is removed in centrifugation again.Feed liquid after the separation is sent into extraction tower, makes extractant with organic solvent, carries out liquid-liquid counter-current extraction under 20-50 ℃ of temperature, requires extract to contain the nicotine amount greater than 0.4%.Wherein used organic solvent is one or more mixtures in alkyl halide, benzene series, ethers, alcohols and the ketone, as carrene, carbon tetrachloride, benzene, ethanol, acetone, ether etc.At last with extract under 50-100 ℃ of temperature, normal pressure or decompression (are generally 0.065～0.085Mpa) distillation and remove and to desolvate, add lower alcohol again, as the further purification of ethanol, obtain brown oily nicotinic liquid.Natural nicotine content 70-90% wherein, chemical analysis be the methyl hydrogen pyrroles for pyridine, molecular formula C10H14N2, all the other are indispensable smoke feature in the smoke perfume systems such as pyridine, pyrazine, pyroles; Cyclohexene class, C4-C14 carboxylate and derivative thereof etc. improve smoke and strengthen the peat-reek element of flue gas quality; Improvement, synergy and flavoring efficiency factors such as benzene a pair of horses going side by side pyrones, ethene alcohol ketone, acetophenone, maltol, Mai Xiangsu.It and traditional high purity nicotine (content 98%) and cigarette foam cream (ordering) have obvious difference, and high purity nicotine is colourless, do not contain useful impurity such as fragrant effective ingredient of cigarette and micro-essence, have the very strong stink of excitant, can not be used as cigarette additive.
The advantage of the production method of natural nicotine for cigarette of the present invention is, but continued operation, solvent loss is little, and energy consumption is low, and equipment is simple, and is easy to operate, the extraction efficiency height.Products obtained therefrom also contains effective ingredients such as cigarette strength, cigarette perfume (or spice) except that containing the alkali cigarette, do not contain harmful impurity, mainly acts on cigarette additive.
Describe the present invention in detail with embodiment below
Embodiment 1:
Get 1 ton of the raw material offal of accord with Q/DJHy-02-91 standard-required ready.Add 100 kilograms of calcium oxide and 200 kg of water, mix, with the premix lixiviation apparatus of packing into, carry out solid-liquid adverse current leaching extraction with 2 tons of water under 60 ℃ of temperature, and check that the pH value of leachate is 11, nicotine content is 0.18%.Natural subsidence is separated and is removed contamination precipitation, gets pure feed liquid.Feed liquid is sent into extraction tower under 35 ℃ of temperature, carry out liquid-liquid counter-current extraction for 1 ton with carbon tetrachloride and chloroform mixed extractant (the cooperation ratio is 3: 1), extract air-distillation under 90 ℃ of temperature removes desolvates, and purify once more with ethanol, make 4.2 kilograms of brown oily nicotinic liquids, wherein nicotine content is 75%, and performance indications meet table 1 target level of product quality.
Embodiment 2:
Get 3 tons of the raw material offals of accord with Q/DJHy-02-91 standard-required ready, add 310 kilograms of calcium hydroxides and 600 kg of water, mix, with the premix lixiviation apparatus of packing into, carry out solid-liquid adverse current leaching extraction with 6.6 tons of water under 70 ℃, and check that the pH value of leachate is 12, nicotine content is 0.23%, contamination precipitation is removed in natural subsidence, centrifugation, gets pure feed liquid.Feed liquid is sent into extraction tower, under 40 ℃ of temperature, carry out liquid-liquid counter-current extraction for 3.3 tons with ether, ethanol and benzene mixed extractant (the cooperation ratio is 1: 1: 2), extract air-distillation under 95 ℃ of temperature removes desolvates, and purify once more with ethanol, make 10.2 kilograms of brown oily nicotinic liquids, wherein nicotine content is 80%, and performance indications meet table 1 target level of product quality.
Embodiment 3:
Get 5 tons of the raw material offals of accord with Q/DJHy-02-91 standard-required ready, add 250 kilograms of NaOH and 1 ton of water, mix, with the premix lixiviation apparatus of packing into, under 80 ℃ of temperature, carry out solid-liquid adverse current leaching extraction with 10.5 tons of water, and the pH value of checking leachate is 13, and nicotine content is 0.25%.Natural subsidence, centrifugation are removed the contamination precipitation thing, get pure feed liquid.Send into extraction tower under 25 ℃ of temperature, (the cooperation ratio is 1: 1: 1: 1) 7 tons are carried out liquid-liquid counter-current extraction with ether, acetone, ethanol and benzene mixed extractant, extract distills down except that desolvating in 85 ℃ of temperature and 0.085Mpa pressure, and purify once more with ethanol, make 17.2 kilograms of brown oily nicotinic liquids, wherein nicotine content is 87%, and performance indications meet table 1 target level of product quality.
Table 1: target level of product quality
| Index name | 1 | |
| Nicotine content | 70－80 | 80－90 |
| Moisture content (%) | ≤6.0 | ≤4.0 |
| Ignition residue (%) | ≤4.0 | ≤3.0 |
| The ethanolic solution test | Qualified | |
| Methyl alcohol (%) | ≤0.04 | |
| Heavy metal (in pb) (%) | ≤0.02 | |
| Organic solvent A r (%) | ≤0.4 | |
According to Q/DJHy-01-91 nicotine products standard.
Claims (6)
1, a kind of production method of natural nicotine for cigarette, it is characterized in that with the offal being raw material, use water as lixivant, under alkali condition, carry out solid-liquid adverse current leaching extraction, the leachate that separation is removed behind the impurity carries out liquid-liquid counter-current extraction with organic solvent again, at last refining the removing of extract desolvated, make the nicotinic liquid that contains natural nicotine 70-90%.
2, the production method of natural nicotine for cigarette as claimed in claim 1 is characterized in that the temperature of solid-liquid adverse current leaching extraction is 50～90 ℃, control pH of leaching solution 〉=11.
3, the production method of natural nicotine for cigarette as claimed in claim 1, when it is characterized in that solid-liquid adverse current leaching extraction, offal is 1: 2～2.5 with the ratio of water.
4, the production method of natural nicotine for cigarette as claimed in claim 1, the temperature that it is characterized in that liquid-liquid counter-current extraction is 20-50 ℃.
5, the production method of natural nicotine for cigarette as claimed in claim 1, the organic solvent that it is characterized in that liquid-liquid extraction is one or more mixtures in alkyl halide, benzene series, ethers, alcohols and the ketone, and leachate is 1: 1～2 with the ratio of extractant.
6, the production method of natural nicotine for cigarette as claimed in claim 1, it is characterized in that refining is under 50～100 ℃ of temperature, normal pressure or removal of solvent under reduced pressure, and purify with lower alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110817A CN1037659C (en) | 1993-01-11 | 1993-01-11 | Production method of natural nicotine for cigarette |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110817A CN1037659C (en) | 1993-01-11 | 1993-01-11 | Production method of natural nicotine for cigarette |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1074103A true CN1074103A (en) | 1993-07-14 |
| CN1037659C CN1037659C (en) | 1998-03-11 |
Family
ID=4988640
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93110817A Expired - Fee Related CN1037659C (en) | 1993-01-11 | 1993-01-11 | Production method of natural nicotine for cigarette |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1037659C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104585875A (en) * | 2015-01-21 | 2015-05-06 | 中国烟草总公司郑州烟草研究院 | Method for preparing electronic cigarette liquid by tobacco stems and tobacco leaves |
| CN108704333A (en) * | 2018-04-15 | 2018-10-26 | 湖北和诺生物工程股份有限公司 | A kind of continuous flow upstream differential extraction device of nicotine |
| CN111528517A (en) * | 2020-04-30 | 2020-08-14 | 贵州黄果树金叶科技有限公司 | Extract for heating non-burning cigarette and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5148819A (en) * | 1991-08-15 | 1992-09-22 | R. J. Reynolds Tobacco Company | Process for extracting tobacco |
-
1993
- 1993-01-11 CN CN93110817A patent/CN1037659C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104585875A (en) * | 2015-01-21 | 2015-05-06 | 中国烟草总公司郑州烟草研究院 | Method for preparing electronic cigarette liquid by tobacco stems and tobacco leaves |
| CN108704333A (en) * | 2018-04-15 | 2018-10-26 | 湖北和诺生物工程股份有限公司 | A kind of continuous flow upstream differential extraction device of nicotine |
| CN111528517A (en) * | 2020-04-30 | 2020-08-14 | 贵州黄果树金叶科技有限公司 | Extract for heating non-burning cigarette and preparation method thereof |
| CN111528517B (en) * | 2020-04-30 | 2022-01-28 | 贵州黄果树金叶科技有限公司 | Extract for heating non-burning cigarette and preparation method thereof |
| CN111528517B8 (en) * | 2020-04-30 | 2022-03-29 | 贵州黄果树金叶科技有限公司 | Extract for heating non-burning cigarette and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1037659C (en) | 1998-03-11 |
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