CN113861165A - Two-phase extraction method of nicotine - Google Patents
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- CN113861165A CN113861165A CN202111370031.2A CN202111370031A CN113861165A CN 113861165 A CN113861165 A CN 113861165A CN 202111370031 A CN202111370031 A CN 202111370031A CN 113861165 A CN113861165 A CN 113861165A
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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
Abstract
The invention discloses a two-phase extraction method of nicotine, and particularly relates to the technical field of two-phase extraction. The invention puts the tobacco powder into a distillation device, adds a proper amount of liquid after putting the tobacco powder into the distillation device, starts the distillation device, the temperature of the liquid is increased rapidly, so that the liquid is in a boiling state, the internal pressure of the distillation device is adjusted, normal hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction to realize two-phase extraction of liquefied steam, and when the liquefied steam is generated, can be immediately enriched in the oil phase to obtain the nicotine extract, so that the method only needs to add normal hexane or petroleum ether as an extraction phase, and can immediately enrich in the oil phase while generating the target nicotine, thereby realizing the timely separation and purification of the product, having more efficient reaction process, greatly reducing the generation of byproducts, and the complicated steps in extracting the nicotine are reduced, and the effect of the method in extracting the nicotine is ensured.
Description
Technical Field
The invention relates to the technical field of two-phase extraction, in particular to a two-phase extraction method of nicotine.
Background
Natural tobacco leaves typically contain 1-3% nicotine. Nicotine is commonly called nicotine, and can excite spirit, eliminate fatigue, increase thinking ability, improve work efficiency and have a certain anesthetic effect when being taken in a proper amount, which is the place where many smokers smoke. However, nicotine is toxic, and excessive intake of nicotine can damage human health, such as chronic pharyngitis, respiratory diseases, cardiovascular diseases, certain digestive diseases, headache, insomnia and other nervous system disorders. Under the current realistic situation that smoking cannot be completely quitted, the regulation and control of reducing the nicotine content in common cigarettes has become the pursuit target of the cigarette industry. In addition, in order to meet different requirements of different smokers, cigarette products with different nicotine contents are generally produced by the tobacco-making process reconstituted tobacco technology in the tobacco-making industry, so that the nicotine content in tobacco extract or extract is also required to be regulated and controlled in the production of the tobacco-making process reconstituted tobacco.
Tobacco contains various alkaloids, more than 40 of which are identified, and the content of nicotine is the most, about 95% of the alkaloids in tobacco, and 0.5-6% of the dry weight of tobacco. Nicotine has wide application in the fields of medicine and chemical industry. Pharmacological research shows that: nicotine binds to nicotinic choline in the peripheral and central nervous systems, has multiple effects on the brain, activates various neurochemical pathways, and effects on the central nerve can lead to increased arousal, attention and responsiveness, and reduced anxiety and stress responses. Certain pharmaceutically acceptable nicotine salt compounds are useful for treating certain conditions, such as muscle spasms and joint pain that are not alleviated by massage or aspirin, by topical administration of nicotine tartrate. In addition, the nicotine sulfate is a plant pesticide with high efficiency, low toxicity, no drug resistance, no residue, no toxicity and great potential for polluting land, is a green pesticide and has excellent effect on preventing and treating cotton and vegetable aphids.
Tobacco is planted in many areas in China, most qualified products in tobacco leaves harvested by tobacco growers every year are sold to tobacco companies directly, but most of tobacco stems and inferior tobacco leaves are left every year, the rest parts are not used for household fire at present due to improvement of living standard, if the tobacco stems and inferior tobacco leaves are put into a methane tank, a proper methane tank is needed, and potential safety hazards and environmental pollution are caused by field incineration. In the prior art, the residual materials can be used for extracting nicotine, namely nicotine, the nicotine is an important component of smoking cessation drugs and green environment-friendly insecticides, trace nicotine does not directly cause harm to human bodies, and the nicotine is used as an effective drug for treating senile dementia, Parkinson's disease and depression. Meanwhile, nicotine is not only in tobacco leaves, but also in fruits of various solanaceae plants, such as tomatoes, barbary wolfberry fruits and other plants, and nicotine is contained in the vegetables and medicinal materials, but the vegetables and medicinal materials are generally accepted as healthy food beneficial to human bodies, so that the world health organization popularizes 'nicotine replacement therapy' in the world in the early 90 th 20 th century to give up smoking, replaces nicotine obtained from cigarettes in the past, helps people overcome dependence on cigarettes physiologically and psychologically, increases the success chance of giving up smoking by more than 1 time, and changes waste into valuables to be the best home for the materials.
Chinese patent document (CN111620851A) discloses a method for extracting nicotine from tobacco based on a three-time extraction method, wherein the method provides that nicotine, also known as nicotine, is colorless or light yellow oily liquid, has a chemical name of 1-methyl-2- (2-pyridyl) pyrrolidine and a molecular formula of C10H14N2The molecular weight is 162.28, the boiling point is 247 deg.C, the melting point is-79 deg.C, the flash point is 95 deg.C, and the autoignition temperature is 240 deg.C. Nicotine is an important raw material for medicines, natural pesticides, spices and chemical industry, and can be used for producing safe and effective smoking cessation products, electronic cigarettes and low-toxicity and residue-free pesticides. Tobacco is the major source of nicotine. The existing extraction methods of nicotine comprise a steam distillation method, an organic solvent extraction method and the like, however, the steam distillation method has high energy consumption; the organic solvent extraction method has the disadvantages that the organic solvent with strong toxicity, such as chloroform, diethyl ether and the like, is harmful to the body of a production worker, and the purity of the obtained nicotine cannot be reached, meanwhile, the specification proposes that in the invention, the organic solvent removal mode is preferably rotary evaporation, and the specific operation mode of the rotary evaporation is not specially carried out in the inventionThe operation method known to those skilled in the art can be used with special requirements. The invention can effectively separate nicotine from tobacco through three extraction processes, and the obtained nicotine has higher yield and purity. Furthermore, the acid used in the extraction process is organic acid, so that the corrosion on metal equipment is low; the invention uses low-toxicity organic solvent to carry out the first extraction and the third extraction, which has little harm to human body and environment, but the invention still has difficulty in solving the problems of layering and organic solvent addition and removal during the extraction of nicotine in the actual operation process, so the following problems still exist in the prior nicotine extraction method and the cited comparative case method:
conventional nicotine extraction methods include steam distillation, organic solvent extraction and ion exchange resin methods. Among them, the steam distillation method is the earliest method for producing nicotine, but the obtained nicotine has low purity. In order to increase the purity, it is customary in industry to combine solvent extraction with steam distillation, i.e. to extract the starting materials with a certain amount of lye and then to distill them with steam. The main flow of the solvent extraction method comprises the following steps: alkali liquor soaking → organic solvent extraction → distillation refining, but a large amount of organic solvent is used in the treatment process, which is easy to cause environmental pollution and poor in safety. The ion exchange resin method has the defects of complex resin activation operation, large solvent consumption and complicated steps.
At present in the process of extracting nicotine, need adopt the supplementary extraction nicotine of extractant at the in-process that nicotine extracted, however after the extraction finishes, then need carry out the secondary separation or adopt follow-up separation step, distinguish nicotine impurity together, the extraction process that leads to nicotine in the in-process of actual operation effect is comparatively loaded down with trivial details, it is difficult to realize the enrichment in the oil item, separation and the purification that leads to the product need be divided into a plurality of steps and go on, very big increase the time of reaction and the loaded down with trivial details degree of extracting nicotine, simultaneously, it produces the increase to add the byproduct in the nicotine extraction easily to add multiple reactant.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a two-phase extraction method of nicotine, and the technical problems to be solved by the invention are as follows: at present at the in-process of drawing nicotine, need adopt the supplementary extraction nicotine of extractant at the in-process that nicotine was drawed, however after the extraction finishes, then need carry out the secondary separation or adopt follow-up separation step, distinguish nicotine impurity together, the extraction process that leads to nicotine in the in-process of actual operation effect is comparatively loaded down with trivial details, it is difficult to realize the enrichment in the oil item, separation and the purification that leads to the result need be divided into a plurality of steps and go on, very big increase the time of reaction and the loaded down with trivial details degree of drawing nicotine, simultaneously, add the problem that multiple reactant caused the by-product in the nicotine extraction to generate the increase easily.
In order to achieve the purpose, the invention provides the following technical scheme: a biphasic extraction process of nicotine comprising the steps of:
pretreatment: crushing the collected tobacco, crushing the tobacco stems and the tobacco leaves by a crusher, sieving for later use to obtain tobacco powder, leaching the tobacco powder, mixing the tobacco powder with water according to the proportion of 1:7, keeping the temperature of the water at 20-70 ℃ to obtain a tobacco solution, putting the tobacco solution into a vertical leaching tank, standing for 10min, taking out the tobacco solution, heating the tobacco solution, keeping the temperature at 30-70 ℃ to obtain a high-temperature tobacco solution, putting the high-temperature tobacco solution into a horizontal spiral leaching device, accelerating the leaching of the high-temperature tobacco solution, and keeping the time for 20-60 min to obtain a tobacco leaching solution.
Concentration treatment: and putting the tobacco extract into a multi-effect concentrator, controlling the vacuum degree in the multi-effect concentrator, keeping the internal vacuum degree at 0.08-0.09 MPa, and concentrating the tobacco extract by the multi-effect concentrator until the tobacco extract meets the requirements of the coating process, and stopping operation to obtain the tobacco concentrated stock solution.
Adjusting and treating stock solution:
(1) mixing tobacco and water, sequentially heating, leaching and filtering, quantitatively adding strong base stock solution, adjusting the pH value of the obtained filtrate to be more than or equal to 10, and standing for later use to obtain alkaline tobacco stock solution.
(2) Taking out the alkaline tobacco stock solution after standing, and carrying out microwave treatment on the alkaline tobacco stock solution, wherein the power of the microwave treatment is 800w-1000w, and after the alkaline tobacco stock solution is treated for 2-3 times by keeping the efficiency of 20-30 s/time, the tobacco blocks are rolled into powder to obtain the tobacco powder.
Extraction treatment:
A. putting the obtained tobacco powder into a distillation device, adding a proper amount of liquid after putting the tobacco powder into the distillation device, starting the distillation device, accelerating to increase the temperature of the liquid, so that the liquid is in a boiling state, adjusting the internal pressure of the distillation device, and keeping the boiling of the liquid on the premise of keeping the internal temperature of the distillation device lower than 100 ℃.
B. The liquid is collected by the reflux device, the steam generated by boiling is collected, n-hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction, the two-phase extraction of the liquefied steam is realized, and the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, so that the nicotine extract is obtained.
As a further scheme of the invention: the internal temperature of the multi-effect concentrator in the concentration treatment is maintained at 60-75 ℃ in the tobacco extract processing period, and the specific gravity of internal compressed liquid of the multi-effect concentrator is 30-40 Be in the tobacco extract processing period.
As a further scheme of the invention: the internal pressure of the distillation device in the step A is more than 1.333 kPa.
As a further scheme of the invention: the ratio of the liquid to the tobacco powder in the step A is 1: 5.
the invention has the beneficial effects that:
1. the invention puts the obtained tobacco powder into a distillation device, adds a proper amount of liquid after putting the tobacco powder into the distillation device, starts the distillation device, leads the liquid to be in a boiling state by accelerating the temperature rise of the liquid, adjusts the internal pressure of the distillation device, keeps the boiling of the liquid on the premise of keeping the internal temperature of the distillation device to be lower than 100 ℃, collects the steam generated by the boiling of the liquid through a reflux device, adds normal hexane or petroleum ether as an extraction phase in the process of liquefying the steam, realizes the two-phase extraction of the liquefied steam, immediately enriches the liquefied steam in an oil phase while generating the nicotine to obtain the nicotine extract, leads the method to immediately enrich in the oil phase while generating the target nicotine only by adding the normal hexane or petroleum ether as the extraction phase, thereby realizing the timely separation and purification of the product, the reaction process has more efficient effect, the generation of byproducts is greatly reduced, the complicated steps in extracting nicotine are reduced, and the effect of the method in extracting nicotine is ensured.
2. According to the invention, the tobacco powder is fed into the distillation device, the pressure inside the distillation device is correspondingly adjusted, when the temperature of the liquid inside the distillation device reaches the boiling point, the temperature of the liquid inside the distillation device is lower than 100 ℃, so that the extraction efficiency of nicotine is accelerated, meanwhile, the loss of nicotine can be avoided by adjusting the pressure, and the tobacco can be extracted by treating the tobacco in a pretreatment mode, so that the application range of the extraction method is enlarged.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a biphasic extraction process of nicotine comprising the steps of:
pretreatment: crushing the collected tobacco, crushing tobacco stems and tobacco leaves by a crusher, sieving for later use to obtain tobacco powder, leaching the tobacco powder, mixing the tobacco powder with water according to the proportion of 1:7, keeping the temperature of the water at 60 ℃ to obtain a tobacco solution, putting the tobacco solution into a vertical leaching tank, standing for 10min, taking out the tobacco solution, heating the tobacco solution, keeping the temperature at 60 ℃ to obtain a high-temperature tobacco solution, putting the high-temperature tobacco solution into a horizontal spiral leaching device, accelerating the leaching of the high-temperature tobacco solution, and keeping the temperature for 50min to obtain a tobacco leaching solution.
Concentration treatment: and putting the tobacco extract into a multi-effect concentrator, controlling the vacuum degree in the multi-effect concentrator, keeping the internal vacuum degree at 0.08-0.09 MPa, and concentrating the tobacco extract by the multi-effect concentrator until the tobacco extract meets the requirements of the coating process, and stopping operation to obtain the tobacco concentrated stock solution.
Adjusting and treating stock solution:
(1) mixing tobacco and water, sequentially heating, leaching and filtering, quantitatively adding strong base stock solution, adjusting the pH value of the obtained filtrate to be more than or equal to 10, and standing for later use to obtain alkaline tobacco stock solution.
(2) Taking out the alkaline tobacco stock solution after standing, and carrying out microwave treatment on the alkaline tobacco stock solution, wherein the power of the microwave treatment is 800w-1000w, and after the alkaline tobacco stock solution is treated for 2-3 times by keeping the efficiency of 20-30 s/time, the tobacco blocks are rolled into powder to obtain the tobacco powder.
Extraction treatment:
A. putting the obtained tobacco powder into a distillation device, adding a proper amount of liquid after putting the tobacco powder into the distillation device, starting the distillation device, accelerating to increase the temperature of the liquid, so that the liquid is in a boiling state, adjusting the internal pressure of the distillation device, and keeping the boiling of the liquid on the premise of keeping the internal temperature of the distillation device lower than 100 ℃.
B. The liquid is collected by the reflux device, the steam generated by boiling is collected, n-hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction, the two-phase extraction of the liquefied steam is realized, and the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, so that the nicotine extract is obtained.
In the concentration treatment, the internal temperature of the multi-effect concentrator is maintained at 60-75 ℃ in the tobacco extract processing period, the specific gravity of internal compressed liquid in the multi-effect concentrator is 30-40 Be in the tobacco extract processing period, the internal pressure of a distillation device in the step A is more than 1.333kPa, and the ratio of liquid to tobacco powder in the step A is 1: 5.
example 2:
this example is a two-phase extraction of nicotine, which differs from example 1 only in that it comprises the following steps:
pretreatment: crushing the collected tobacco, crushing tobacco stems and tobacco leaves by a crusher, sieving for later use to obtain tobacco powder, leaching the tobacco powder, mixing the tobacco powder with water according to the proportion of 1:7, keeping the temperature of the water at 20 ℃ to obtain a tobacco solution, putting the tobacco solution into a vertical leaching tank, standing for 10min, taking out the tobacco solution, heating the tobacco solution, keeping the temperature at 30 ℃ to obtain a high-temperature tobacco solution, putting the high-temperature tobacco solution into a horizontal spiral leaching device, accelerating the leaching of the high-temperature tobacco solution, and keeping the temperature for 60min to obtain a tobacco leaching solution.
Concentration treatment: and putting the tobacco extract into a multi-effect concentrator, controlling the vacuum degree in the multi-effect concentrator, keeping the internal vacuum degree at 0.08-0.09 MPa, and concentrating the tobacco extract by the multi-effect concentrator until the tobacco extract meets the requirements of the coating process, and stopping operation to obtain the tobacco concentrated stock solution.
Adjusting and treating stock solution:
(1) mixing tobacco and water, sequentially heating, leaching and filtering, quantitatively adding strong base stock solution, adjusting the pH value of the obtained filtrate to be more than or equal to 10, and standing for later use to obtain alkaline tobacco stock solution.
(2) Taking out the alkaline tobacco stock solution after standing, and carrying out microwave treatment on the alkaline tobacco stock solution, wherein the power of the microwave treatment is 800w-1000w, and after the alkaline tobacco stock solution is treated for 2-3 times by keeping the efficiency of 20-30 s/time, the tobacco blocks are rolled into powder to obtain the tobacco powder.
Extraction treatment:
A. putting the obtained tobacco powder into a distillation device, adding a proper amount of liquid after putting the tobacco powder into the distillation device, starting the distillation device, accelerating to increase the temperature of the liquid, so that the liquid is in a boiling state, adjusting the internal pressure of the distillation device, and keeping the boiling of the liquid on the premise of keeping the internal temperature of the distillation device lower than 100 ℃.
B. The liquid is collected by the reflux device, the steam generated by boiling is collected, n-hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction, the two-phase extraction of the liquefied steam is realized, and the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, so that the nicotine extract is obtained.
In the concentration treatment, the internal temperature of the multi-effect concentrator is maintained at 60-75 ℃ in the tobacco extract processing period, the specific gravity of internal compressed liquid in the multi-effect concentrator is 30-40 Be in the tobacco extract processing period, the internal pressure of a distillation device in the step A is more than 1.333kPa, and the ratio of liquid to tobacco powder in the step A is 1: 5.
example 3:
this example is a two-phase extraction of nicotine, which differs from example 1 only in that it comprises the following steps:
pretreatment: crushing the collected tobacco, crushing tobacco stems and tobacco leaves by a crusher, sieving for later use to obtain tobacco powder, leaching the tobacco powder, mixing the tobacco powder with water according to the proportion of 1:7, keeping the temperature of the water at 70 ℃ to obtain a tobacco solution, putting the tobacco solution into a vertical leaching tank, standing for 10min, taking out the tobacco solution, heating the tobacco solution, keeping the temperature at 70 ℃ to obtain a high-temperature tobacco solution, putting the high-temperature tobacco solution into a horizontal spiral leaching device, accelerating the leaching of the high-temperature tobacco solution, and keeping for 10min to obtain a tobacco leaching solution.
Concentration treatment: and putting the tobacco extract into a multi-effect concentrator, controlling the vacuum degree in the multi-effect concentrator, keeping the internal vacuum degree at 0.08-0.09 MPa, and concentrating the tobacco extract by the multi-effect concentrator until the tobacco extract meets the requirements of the coating process, and stopping operation to obtain the tobacco concentrated stock solution.
Adjusting and treating stock solution:
(1) mixing tobacco and water, sequentially heating, leaching and filtering, quantitatively adding strong base stock solution, adjusting the pH value of the obtained filtrate to be more than or equal to 10, and standing for later use to obtain alkaline tobacco stock solution.
(2) Taking out the alkaline tobacco stock solution after standing, and carrying out microwave treatment on the alkaline tobacco stock solution, wherein the power of the microwave treatment is 800w-1000w, and after the alkaline tobacco stock solution is treated for 2-3 times by keeping the efficiency of 20-30 s/time, the tobacco blocks are rolled into powder to obtain the tobacco powder.
Extraction treatment:
A. putting the obtained tobacco powder into a distillation device, adding a proper amount of liquid after putting the tobacco powder into the distillation device, starting the distillation device, accelerating to increase the temperature of the liquid, so that the liquid is in a boiling state, adjusting the internal pressure of the distillation device, and keeping the boiling of the liquid on the premise of keeping the internal temperature of the distillation device lower than 100 ℃.
B. The liquid is collected by the reflux device, the steam generated by boiling is collected, n-hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction, the two-phase extraction of the liquefied steam is realized, and the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, so that the nicotine extract is obtained.
In the concentration treatment, the internal temperature of the multi-effect concentrator is maintained at 60-75 ℃ in the tobacco extract processing period, the specific gravity of internal compressed liquid in the multi-effect concentrator is 30-40 Be in the tobacco extract processing period, the internal pressure of a distillation device in the step A is more than 1.333kPa, and the ratio of liquid to tobacco powder in the step A is 1: 5.
the following table is obtained according to examples 1 to 3:
| temperature of mixing | Leaching time | Leaching temperature | Tobacco extract treatment effect | |
| Example 1 | 60℃ | 50min | 60℃ | Fully leaching and uniformly mixing |
| Example 2 | 20℃ | 60min | 20℃ | Difficult uniform leaching and excessive precipitation |
| Example 3 | 70℃ | 10min | 70℃ | Reaction is advanced and not mixed uniformly |
From the comparison in the table above, it can be seen that: the method comprises the steps of adopting the temperature of 20 ℃ to stand a tobacco solution, then leaching the tobacco mixed solution at the temperature of 20 ℃ for 60min, firstly, ensuring the primary mixing efficiency of tobacco and liquid when standing still at the temperature of 20 ℃, secondly, leading nicotine in the tobacco solution to be difficult to dissolve in the liquid when leaching the tobacco through the temperature of 20 ℃, and stirring the tobacco mixed solution for 60min, wherein the time consumption is too long, tobacco powder in the tobacco solution is rapidly precipitated after the leaching is stopped, the requirement of extracting the nicotine is difficult to meet, adopting the temperature of 70 ℃ to stand the tobacco solution, then leaching the tobacco mixed solution at the temperature of 70 ℃ for 20min, firstly, the temperature of 70 ℃ can rapidly reach the requirement of mixing the tobacco solution, leading the reaction time to be advanced, easily leading the nicotine to be volatilized, and leading the stirring time of 10min to be too short, thus leading the incomplete mixing condition to occur.
The obtained tobacco powder is put into a distillation device, a proper amount of liquid is added after the tobacco powder is put into the distillation device, the distillation device is started, the temperature of the liquid is increased by accelerating, so that the liquid is in a boiling state, the internal pressure of the distillation device is adjusted, the boiling of the liquid is kept on the premise that the internal temperature of the distillation device is required to be kept lower than 100 ℃, the steam generated by the boiling of the liquid is collected by a reflux device, n-hexane or petroleum ether is added as an extraction phase in the process of liquefying the steam, the two-phase extraction of liquefied steam is realized, the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, a nicotine extract is obtained, the method only needs to add the n-hexane or petroleum ether as the extraction phase, the target nicotine is generated, the enrichment can be immediately carried out in the oil phase, the timely separation and purification of products are realized, and the reaction process has more efficient effect, the generation of byproducts is greatly reduced, the complicated steps in the extraction of nicotine are reduced, and the effect of the method in the extraction of nicotine is guaranteed.
Through throwing the tobacco bits into distillation plant and corresponding the inside pressure of adjustment distillation plant, when the temperature of the inside liquid of distillation plant reached the boiling point, the temperature of its inside liquid was less than 100 ℃ to accelerated extraction efficiency to nicotine, simultaneously, the condition that the loss can effectually be avoided to the mode that adopts the adjustment pressure, and the mode that adopts the preliminary treatment handles the tobacco and can carry out the quick extraction to the nicotine that tobacco crushed aggregates, tobacco stalk or tobacco leaf contain, thereby improved the application scope of this extraction method.
The points to be finally explained are: although the present invention has been described in detail with reference to the general description and the specific embodiments, on the basis of the present invention, the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. A method for biphasic extraction of nicotine, comprising the steps of:
pretreatment: crushing the collected tobacco, crushing tobacco stems and tobacco leaves by a crusher, sieving for later use to obtain tobacco powder, leaching the tobacco powder, mixing the tobacco powder with water according to the proportion of 1:7, keeping the temperature of the water at 20-70 ℃ to obtain a tobacco solution, putting the tobacco solution into a vertical leaching tank, standing for 10min, taking out the tobacco solution, heating the tobacco solution, keeping the temperature at 30-70 ℃ to obtain a high-temperature tobacco solution, putting the high-temperature tobacco solution into a horizontal spiral leaching device, accelerating the leaching of the high-temperature tobacco solution, and keeping the temperature for 20-60 min to obtain a tobacco leaching solution;
concentration treatment: putting the tobacco extract into a multi-effect concentrator, controlling the vacuum degree in the multi-effect concentrator, keeping the internal vacuum degree at 0.08-0.09 MPa, and concentrating the tobacco extract by the multi-effect concentrator until the tobacco extract meets the requirements of a coating process, and stopping operation to obtain a tobacco concentrated stock solution;
adjusting and treating stock solution:
(1) mixing tobacco and water, sequentially heating, leaching and filtering, quantitatively adding a strong base stock solution, adjusting the pH value of the obtained filtrate to be more than or equal to 10, and standing for later use to obtain an alkaline tobacco stock solution;
(2) taking out the alkaline tobacco stock solution after standing, and carrying out microwave treatment on the alkaline tobacco stock solution, wherein the power of the microwave treatment is 800w-1000w, and after the alkaline tobacco stock solution is treated for 2-3 times by keeping the efficiency of 20-30 s/time, the tobacco blocks are rolled into powder to obtain tobacco powder;
extraction treatment:
A. putting the obtained tobacco powder into a distillation device, adding a proper amount of liquid after putting the tobacco powder into the distillation device, starting the distillation device, enabling the liquid to be in a boiling state by accelerating the temperature rise of the liquid, and adjusting the internal pressure of the distillation device, wherein the boiling of the liquid is kept on the premise that the internal temperature of the distillation device is required to be kept lower than 100 ℃;
B. the liquid is collected by the reflux device, the steam generated by boiling is collected, n-hexane or petroleum ether is added as an extraction phase in the process of steam liquefaction, the two-phase extraction of the liquefied steam is realized, and the liquefied steam can be immediately enriched in an oil phase while the nicotine is generated, so that the nicotine extract is obtained.
2. A biphasic extraction process of nicotine according to claim 1, characterised in that: the internal temperature of the multi-effect concentrator in the concentration treatment is maintained at 60-75 ℃ in the tobacco extract processing period, and the specific gravity of internal compressed liquid of the multi-effect concentrator is 30-40 Be in the tobacco extract processing period.
3. A biphasic extraction process of nicotine according to claim 1, characterised in that: the internal pressure of the distillation device in the step A is more than 1.333 kPa.
4. A biphasic extraction process of nicotine according to claim 1, characterised in that: the ratio of the liquid to the tobacco powder in the step A is 1: 5.
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