CN110511210A - High purity nicotine production technology - Google Patents
High purity nicotine production technology Download PDFInfo
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- CN110511210A CN110511210A CN201910864778.XA CN201910864778A CN110511210A CN 110511210 A CN110511210 A CN 110511210A CN 201910864778 A CN201910864778 A CN 201910864778A CN 110511210 A CN110511210 A CN 110511210A
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
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Abstract
The present invention provides high purity nicotine production technology, comprising the following steps: impregnates tobacco into the water, filters, tobacco soak is obtained, as liquid to be distilled；Adjust liquid pH >=11 to be distilled, heating 2.5~3.5h of distillation is absorbed between 108~110 DEG C with acid, and it controls and receives liquid pH≤3, it distills in liquid to original volume 1/10, boiling point is more than 110 DEG C, stops distillation, releasing remains in paste in distiller, distillate is heated to boiling point, original volume 1/10 is evaporated to, obtains concentrate；The volume ratio of tune pH >=11 after concentrate is cooling, addition extractant, extractant and concentrate is 1:4~6, and stratification after extraction obtains water phase and organic phase after separation；It is organic be added to molecular sieve, active carbon is refined, the organic solution after must refining after filtering；Organic solution after purification is evaporated under reduced pressure, control temperature is no more than 101 DEG C, and nicotine products are made.Nicotine products purity, high income is made in the present invention, and remains micro geranyl acetone, improves the quality of later period harmless cigarette production.
Description
Technical field
The present invention relates to nicotine technical fields, in particular to high purity nicotine production technology.
Background technique
Nicotine is also referred to as nicotine, is a kind of colorless and transparent oily volatility stimulation liquid.Nicotine is the master of smoker
It is accustomed to source.Nicotine 7.5s in sucking cigarette smoke can arrive the brain of intelligent, and smoker is made to feel a kind of soft pleased
Fast feeling.
The main component of tobacco has tar, carbon monoxide, alkaloid, amine, phenols, alkane, aldehydes, nitrogen oxides, puts
Penetrating property substance, organic agricultural chemicals and other more than 4000 kinds of substances being harmful to the human body, there are many biological actions for they, can be to human body
Cause various harm.
Smoking population is huge, and smoking causes various countries' most attention with health problem, and tar reduction, harm reduction become being total to for tobacco business
Same target, utmostly reduces harm of smoking.Therefore it is badly in need of a kind of nicotine production technology, the nicotine content in product is improved,
The content of tar and other harmful substances matter utmostly reduces.
Summary of the invention
For mirror with this, the present invention proposes high purity nicotine production technology, and nicotine purity is high is made, up to 99.7% or more, and
And product yield is high.
The technical scheme of the present invention is realized as follows:
High purity nicotine production technology, comprising the following steps:
S1, immersion: tobacco is impregnated into the water, and filtering obtains tobacco soak, as liquid to be distilled；
S2, distillation: adjusting liquid pH >=11 to be distilled, and 2.5~3.5h of heating distillation uses acid solution between 108~110 DEG C
It absorbs, and controls and receive liquid pH≤3, distill in liquid to original volume 1/10, boiling point is more than 110 DEG C, stops distillation, releases residual
Distillate is heated to boiling point by the paste in distiller, is evaporated to original volume 1/10, is obtained concentrate；
S3, extraction: adjusting pH >=11 after concentrate is cooling, is added extractant, the volume ratio of extractant and concentrate be 1:4~
6, stratification after extraction obtains water phase and organic phase after separation；
S4, purification: it is organic be added to molecular sieve, active carbon is refined, the organic solution after must refining after filtering；
S5, concentration: the organic solution after purification is evaporated under reduced pressure, and control temperature is no more than 101 DEG C, and nicotine is made and produces
Product.
Preferably, in S1 step, the soaking temperature is 50~60 DEG C, and the soaking time is 20~28h.
Preferably, in S1 step, the weight ratio of the tobacco and water is 1:8~12；
Preferably, in S1 step, tobacco is crushed as pipe tobacco shape before impregnating.
Preferably, in S2 step, the acid solution is at least one of hydrochloric acid, acetic acid.
Preferably, in S3 step, the extractant is at least one of chloroform, ether, isopropanol, ethyl acetate.
Preferably, immersion water of the step S3 water phase as S1 step is taken.
Preferably, it takes step S3 organic phase as liquid to be distilled, repeats S2-S3 distillation, extraction step 2~4 times.
Preferably, in S3 step, the extractant by chloroform, isopropanol and ethyl acetate be by volume 1:0.3~
0.5:0.1~0.3 is mixed to prepare.
Preferably, in S4 step, the specific steps of the purification are as follows: molecular sieve is first added in organic phase and is soaked in 30~40 DEG C
Steep 1~2h, active carbon is added in 45~55 DEG C of immersion 0.3~0.5h in filtering in filtrate, organic molten after must refining after filtering
Liquid.
Preferably, in S4 step, the mass ratio of the organic phase and molecular sieve, active carbon is 1:0.8~2:0.2~0.6.
Preferably, in S4 step, the active carbon is ZnO modified activated carbon.
Preferably, the molecular sieve is that 2~3:5~8 is mixed by SBA-15 molecular sieve and MCM-41 molecular sieve in mass ratio.
Preferably, in S1 step, soaking temperature is 60 DEG C, and soaking time is that for 24 hours, the weight ratio of tobacco and water is 1:10；
In S2 step, heating distillation 3h；In S3 step, the volume ratio of the extractant and concentrate is 1:5.
Compared with prior art, the beneficial effects of the present invention are:
(1) use nicotine production technology of the invention, by tobacco it is soaking-distillation-extraction-purification-concentration technology, be made
Nicotine products, nicotine purity, high income, and micro geranyl acetone is remained, the quality of later period harmless cigarette production is improved,
Titian is assisted to post-production harmless cigarette simultaneously, and low energy consumption.
(2) present invention sufficiently improves tobacco immersion using crushing before impregnating water consumption, soaking temperature and time and immersion
Nicotine content in liquid improves nicotine and the geranyl acetone rate of recovery.
(3) present invention distillation under the conditions of pH >=11, which combines, is absorbed under specific temperature using acid, and is concentrated, larger to mention
High product nicotine and geranyl acetone yield and nicotine purity.
(4) process for refining of the present invention is used, the content of nicotine and geranyl acetone in product is further increased.
(5) present invention uses a certain amount of extractant under the conditions of pH >=11, improves effect of extracting；Using extraction of the invention
Agent is taken, the loss and dosage for effectively reducing extractant further increase effect of extracting using the extractant of compounding.
(6) present invention, which is used as to impregnate before distillation using water phase after extraction, uses water, further recycles water resource, and further
Recycle nicotine and geranyl acetone.
(7) organic phase repeats distillation, extraction step after present invention extraction, further increases the purity of nicotine in product, reaches
To 99% or more.
Specific embodiment
In order to be best understood from the technology of the present invention content, specific embodiment is provided below, the present invention is described further.
Experimental method used in the embodiment of the present invention is conventional method unless otherwise specified.
Material used in the embodiment of the present invention, reagent etc., are commercially available unless otherwise specified.
Embodiment 1
High purity nicotine production technology, comprising the following steps:
S1, immersion: tobacco being crushed as pipe tobacco shape, is put into 50 DEG C of water and impregnates 28h, and the weight ratio of tobacco and water is 1:8,
Filtering, obtains tobacco soak, as liquid to be distilled；
S2, distillation: adjusting liquid pH >=11 to be distilled, heating distillation 2.5h, between 108~110 DEG C, with absorption by Hydrochloric Acid,
And control and receive liquid pH≤3, it distills in liquid to original volume 1/10, boiling point is more than 110 DEG C, stops distillation, and releasing remains in steaming
Paste in device is evaporated, distillate is heated to boiling point, original volume 1/10 is evaporated to, obtains concentrate；
S3, extraction: adjusting pH >=11 after concentrate is cooling, and ether is added as extractant, the volume of extractant and concentrate
Than for 1:4, stratification after extraction obtains water phase and organic phase after separation；
S4, purification: molecular sieve is first added in 30 DEG C of immersion 2h in organic phase, active carbon is added in 45 in filtering in filtrate
DEG C impregnate 0.5h, the organic phase and molecular sieve, active carbon mass ratio be 1:0.8:0.6, the active carbon, which is that ZnO is modified, lives
Property charcoal, the molecular sieve by SBA-15 molecular sieve and MCM-41 molecular sieve be in mass ratio 2:5 mix, after must being refined after filtering
Organic solution；
S5, concentration: the organic solution after purification is evaporated under reduced pressure, and control temperature is no more than 101 DEG C, is removed remaining
Nicotine products are made in organic solution and other volatile components.
Embodiment 2
High purity nicotine production technology, comprising the following steps:
S1, immersion: tobacco being crushed as pipe tobacco shape, is put into 60 DEG C of water and impregnates 20h, and the weight ratio of tobacco and water is 1:
12, filtering obtains tobacco soak, as liquid to be distilled；
S2, distillation: adjusting liquid pH >=11 to be distilled, and heating distillation 3.5h is absorbed between 108~110 DEG C with acetic acid,
And control and receive liquid pH≤3, it distills in liquid to original volume 1/10, boiling point is more than 110 DEG C, stops distillation, and releasing remains in steaming
Paste in device is evaporated, distillate is heated to boiling point, original volume 1/10 is evaporated to, obtains concentrate；
S3, extraction: adjusting pH >=11 after concentrate is cooling, and isopropanol is added as extractant, the body of extractant and concentrate
Product is than for 1:6, stratification after extraction obtains water phase and organic phase after separation；
S4, purification: molecular sieve is first added in 40 DEG C of immersion 1h in organic phase, active carbon is added in 55 in filtering in filtrate
DEG C impregnate 0.3h, the organic phase and molecular sieve, active carbon mass ratio be 1:2:0.2, the active carbon is ZnO modified active
Charcoal, the molecular sieve are that 3:8 is mixed by SBA-15 molecular sieve and MCM-41 molecular sieve in mass ratio, having after must refining after filtering
Machine solution；
S5, concentration: the organic solution after purification is evaporated under reduced pressure, and control temperature is no more than 101 DEG C, is removed remaining
Nicotine products are made in organic solution and other volatile components.
Embodiment 3
High purity nicotine production technology, comprising the following steps:
S1, immersion: tobacco being crushed as pipe tobacco shape, is put into 60 DEG C of water and impregnates for 24 hours, and the weight ratio of tobacco and water is 1:
10, filtering obtains tobacco soak, as liquid to be distilled；
S2, distillation: adjusting liquid pH >=11 to be distilled, heating distillation 3h, between 108~110 DEG C, with absorption by Hydrochloric Acid, and
Liquid pH≤3 are received in control, are distilled in liquid to original volume 1/10, and boiling point is more than 110 DEG C, stop distillation, and releasing remains in distillation
Distillate is heated to boiling point by paste in device, is evaporated to original volume 1/10, is obtained concentrate；
S3, extraction: adjusting pH >=11 after concentrate is cooling, and chloroform is added as extractant, the volume of extractant and concentrate
Than for 1:5, stratification after extraction obtains water phase and organic phase after separation；
S4, purification: being first added molecular sieve in 38 DEG C of immersion 1.5h in organic phase, filtering, be added in filtrate active carbon in
53 DEG C of immersion 0.4h, the organic phase and molecular sieve, active carbon mass ratio be 1:1.2:0.5, the active carbon be ZnO modification
Active carbon；The molecular sieve is 2:7 mixing by SBA-15 molecular sieve and MCM-41 molecular sieve in mass ratio, after must refining after filtering
Organic solution；
S5, concentration: the organic solution after purification is evaporated under reduced pressure, and control temperature is no more than 101 DEG C, is removed remaining
Nicotine products are made in organic solution and other volatile components.
Embodiment 4
The present embodiment is distinguished with embodiment 3 to be, the immersion water phase for the S4 step that water is embodiment 3 of S1 step；And
And take the organic phase of step S3 as liquid to be distilled, repeat S2-S3 distillation, extraction step 3 times.
Embodiment 5
The present embodiment is that the extractant is by volume by chloroform, isopropanol and ethyl acetate with the difference of embodiment 3
1:0.4:0.2 being mixed to prepare.
Embodiment 6
The present embodiment is with the difference of embodiment 3, and in S4 step, the active carbon is ZnO modified activated carbon；The molecule
Sieving is SBA-15 molecular sieve, and the mass ratio of the organic phase and molecular sieve, active carbon is 1:1:1, and molecule is added in normal temperature condition
Sieve, active carbon impregnate 2h.
Comparative example 1
This comparative example is with the difference of embodiment 3, does not carry out the distillation procedure of S2 step, tobacco soak is directly carried out
Extraction.
Comparative example 2
This comparative example is with the difference of embodiment 3, does not carry out the purification operations of S4 step, and organic phase extracted is direct
It is evaporated under reduced pressure.
Comparative example 3
This comparative example is with the difference of embodiment 3, and in S2 step, adjusting pH is 10.
Comparative example 4
This comparative example is with the difference of embodiment 3, and in S2 step, heating distillation time is 4h.
Comparative example 5
This comparative example is with the difference of embodiment 3, in S2 step, absorbs between 120~130 DEG C, then with acid solution.
Comparative example 6
This comparative example is that in S2 step, acid solution replaces with water with the difference of embodiment 3.
Comparative example 7
The difference of this comparative example and embodiment 3 is, in S2 step, when liquid is distilled to original volume 2/10, boiling point does not surpass
110 DEG C are crossed, distillation is stopped.
Comparative example 8
This comparative example is with the difference of embodiment 3, and in S2 step, distillate is heated to boiling point, is evaporated to original volume 2/
10, obtain concentrate.
Comparative example 9
This comparative example is with the difference of embodiment 3, and in S3 step, adjusting pH is 10.
Comparative example 10
This comparative example is with the difference of embodiment 3, and in S3 step, the volume ratio of extractant and concentrate is 1:3.
Nicotine products are made in above-described embodiment and comparative example production technology, detect nicotine products yield, nicotine content
And geranyl acetone content:
Nicotine products yield=nicotine products quality/tobacco material quality * 100%；
Nicotine quality/nicotine products quality * 100% in nicotine content=nicotine products；
Geranyl acetone nicotine quality/nicotine products quality * 100% in geranyl acetone content=nicotine products；
As a result as follows:
The above results show that nicotine purity is high is made using 1~6 nicotine production technology of the embodiment of the present invention, reachable
99.7%, and nicotine products high income, and a small amount of geranyl acetone is remained, improve the product of later period harmless cigarette production
Matter, while Titian is assisted to post-production harmless cigarette.Wherein, the present invention is used using water phase after extraction as preceding impregnate of distillation
Organic phase repeats distillation, extraction step after water, and extraction, further recycles water resource, sufficiently recycles nicotine and geranyl third
Ketone further increases the nicotine purity of product.The extractant compounded using the present invention further increases effect of extracting, improves and produces
Product nicotine purity and nicotine and geranyl acetone yield.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. high purity nicotine production technology, which comprises the following steps:
S1, immersion: tobacco is impregnated into the water, and filtering obtains tobacco soak, as liquid to be distilled；
S2, distillation: adjusting liquid pH >=11 to be distilled, and 2.5~3.5h of heating distillation is absorbed between 108~110 DEG C with acid solution,
And control and receive liquid pH≤3, it distills in liquid to original volume 1/10, boiling point is more than 110 DEG C, stops distillation, and releasing remains in steaming
Paste in device is evaporated, distillate is heated to boiling point, original volume 1/10 is evaporated to, obtains concentrate；
S3, extraction: the volume ratio of tune pH >=11 after concentrate is cooling, addition extractant, extractant and concentrate is 1:4~6, extraction
Rear stratification is taken, water phase and organic phase are obtained after separation；
S4, purification: it is organic be added to molecular sieve, active carbon is refined, the organic solution after must refining after filtering；
S5, concentration: the organic solution after purification is evaporated under reduced pressure, and control temperature is no more than 101 DEG C, and nicotine products are made.
2. high purity nicotine production technology according to claim 1, which is characterized in that in S1 step, the soaking temperature
It is 50~60 DEG C, the soaking time is 20~28h.
3. high purity nicotine production technology according to claim 1 or 2, which is characterized in that in S1 step, the tobacco with
The weight ratio of water is 1:8~12；Tobacco is crushed as pipe tobacco shape before impregnating.
4. high purity nicotine production technology according to claim 1, which is characterized in that in S2 step, the acid solution is salt
At least one of acid, acetic acid.
5. high purity nicotine production technology according to claim 1, which is characterized in that in S3 step, the extractant is
At least one of chloroform, ether, isopropanol, ethyl acetate.
6. high purity nicotine production technology according to claim 1, which is characterized in that take step S3 water phase as S1 step
Immersion water；It takes step S3 organic phase as liquid to be distilled, repeats S2-S3 distillation, extraction step 2~4 times.
7. high purity nicotine production technology according to claim 1, which is characterized in that in S3 step, the extractant by
Chloroform, isopropanol and ethyl acetate are that 1:0.3~0.5:0.1~0.3 is mixed to prepare by volume.
8. high purity nicotine production technology according to claim 1, which is characterized in that in S4 step, the tool of the purification
Body step are as follows: molecular sieve is first added in 30~40 DEG C of 1~2h of immersion in organic phase, active carbon is added in 45 in filtering in filtrate
~55 DEG C of 0.3~0.5h of immersion, the organic solution after must being refined after filtering.
9. high purity nicotine production technology according to claim 1, which is characterized in that in S4 step, the organic phase and
Molecular sieve, active carbon mass ratio be 1:0.8~2:0.2~0.6.
10. described in any item high purity nicotine production technologies according to claim 1~9, which is characterized in that in S4 step, institute
Stating active carbon is ZnO modified activated carbon；The molecular sieve is 2~3 by SBA-15 molecular sieve and MCM-41 molecular sieve in mass ratio:
5~8 mixing.
Priority Applications (1)
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| CN201910864778.XA CN110511210A (en) | 2019-09-12 | 2019-09-12 | High purity nicotine production technology |
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|---|---|---|---|
| CN201910864778.XA CN110511210A (en) | 2019-09-12 | 2019-09-12 | High purity nicotine production technology |
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| CN110511210A true CN110511210A (en) | 2019-11-29 |
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ID=68630810
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605382A (en) * | 2020-12-04 | 2022-06-10 | 上海烟草集团有限责任公司 | Nicotine and preparation method thereof |
| CN115028618A (en) * | 2022-07-19 | 2022-09-09 | 江西农业大学 | Method for preparing high-purity nicotine |
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| CN115028618B (en) * | 2022-07-19 | 2024-03-01 | 江西农业大学 | Method for preparing nicotine |
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