Method for simultaneous obtaining of tobacco extract and target carbon material from waste tobacco and applications thereof
By combining deep eutectic solvent and KOH solution, the problems of low utilization rate and environmental pollution of tobacco waste were solved, and the simultaneous extraction of porous carbon, nicotine and solanesol was achieved, which improved resource utilization and reduced environmental pollution.
Patent Information
- Application Number
- CN202310892606.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-19
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2043-07-19
AI Technical Summary
Existing technologies have low utilization rates of tobacco waste, and the treatment process causes environmental pollution. They also cannot simultaneously extract porous carbon, nicotine, and solanesol, and generate waste gas and wastewater during the preparation process.
Tobacco waste is treated with a deep eutectic solvent, and porous carbon materials are prepared by heating and reacting with KOH solution. Nicotine and solanesol in the tobacco extract are then extracted by extraction and washing methods, reducing environmental pollution and improving resource utilization.
It enables the simultaneous extraction of high-value porous carbon, nicotine, and solanesol from tobacco waste, improving the utilization rate of waste tobacco, reducing resource waste and environmental pollution, and generating almost no waste gas or wastewater during the preparation process.
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Figure CN117003220B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of recycling of tobacco waste, and particularly relates to a method for synchronously obtaining tobacco extract and target carbon material from waste tobacco and application. BACKGROUND
[0002] China is a big country of tobacco in the world, and the total annual tobacco output ranks first in the world. A large amount of tobacco leaves, straws, tobacco dust and other wastes are generated in the process of tobacco leaves and processing. At present, the main treatment method for such tobacco waste is to fill in the place or burn as fertilizer, which has low utilization rate and causes serious pollution to the atmosphere and environment. However, the tobacco leaves, straws, tobacco dust and other wastes contain extractable porous carbon, nicotine, solanesol and other substances. Activated carbon is a kind of porous solid carbon material, which has a unique strong adsorption performance due to its developed void structure and large specific surface area, and is chemically stable and insoluble in water and most other solvents, so it is widely used in adsorption, separation, catalysis and other fields. Nicotine is a biologically active substance, and some studies have shown that moderate nicotine intake has potential use in the treatment of cognitive disorders (such as Alzheimer's disease) and attention deficit hyperactivity disorder (ADHD) and other diseases. In addition, nicotine also has certain anti-inflammatory effect, which can inhibit inflammatory response and activation of immune cells, and has application prospect in the treatment of some inflammatory diseases. Solanesol is a plant active chemical in tobacco leaves, which has anti-inflammatory, bactericidal, ultraviolet absorption and antioxidant functions, and is mainly used in the production of drugs (such as coenzyme Q10) and other pharmaceutical intermediates, and can also be directly used in the production process of antioxidant health care products and cosmetics; especially it is the necessary raw material of anti-aging and coenzyme Q10 which can improve cell vitality and enhance human immunity. It is no doubt that the on-site landfill or incineration treatment of tobacco leaves, straws, tobacco dust and other wastes wastes these resources.
[0003] In addition, for the utilization of tobacco leaves, straws, tobacco dust and other wastes, although the technology for preparing tobacco extract (nicotine or solanesol) and carbon material (activated carbon) from tobacco leaves, straws, tobacco dust and other wastes has been popularized, there are problems of low utilization rate of tobacco waste and environmental pollution (waste gas and wastewater generated in the preparation process), and only a single target product (activated carbon material, nicotine or solanesol) can be obtained.
[0004] Therefore, there is an urgent need for a method for synchronously obtaining tobacco extract and target carbon material from tobacco waste without environmental pollution, so as to improve the utilization rate of waste tobacco. SUMMARY
[0005] In view of the above problems existing in the prior art, the present application provides a method and application for simultaneously obtaining tobacco extract and target carbon material from waste tobacco, wherein tobacco waste is treated by a deep eutectic solvent (DES) to obtain tobacco residues and a liquid phase, and then a KOH solution is mixed with the tobacco residues and heated to prepare a biomass porous carbon material, while extracting the tobacco extract in the liquid phase to obtain nicotine, solanols and porous carbon in the target carbon material, thereby realizing high-value utilization of waste tobacco. The specific application content is as follows.
[0006] In a first aspect, the present application provides a method for simultaneously obtaining tobacco extract and target carbon material from waste tobacco, wherein the preparation method comprises the following steps:
[0007] S1. A deep eutectic solvent is added to the dried and crushed tobacco, and heated under stirring to obtain a mixture of tobacco and deep eutectic solvent;
[0008] S2. An appropriate amount of deionized water is added to the mixture, and centrifugal separation is performed to obtain tobacco residues and a first liquid phase;
[0009] S3. The KOH solution is mixed with the tobacco residues, and then heated to obtain a porous carbon, which is the target carbon material;
[0010] S4. A first extracting agent is added to the first liquid phase, and stirring is performed, and then the mixture is placed in an environment at-20℃ for static layering, and after separation, a second liquid phase and a second solid phase are obtained, and the second solid phase is dried to obtain the deep eutectic solvent;
[0011] S5. Dilute sulfuric acid is used as a washing agent to wash the second liquid phase in a separatory funnel, so that nicotine in the second liquid phase is converted into nicotine sulfate into the washing agent, and a third liquid phase containing nicotine sulfate and a fourth liquid phase from which nicotine is removed are obtained, and then anhydrous calcium chloride is added to the fourth liquid phase, and drying and rotary evaporation are performed to obtain the tobacco extract-solanols;
[0012] S6. The pH of the third liquid phase is adjusted to be greater than 10, and then a second extracting agent is added, and extraction and static layering are performed in a separatory funnel, and after separation, an organic phase containing nicotine is obtained, and the organic phase is rotary evaporated to remove the second extracting agent by using a rotary evaporator to obtain the tobacco extract-nicotine.
[0013] Alternatively, in step S1, the deep eutectic solvent is obtained by stirring and heating choline chloride and urea at a molar ratio of 1:2 to be clear and transparent at 80℃, or
[0014] choline chloride and oxalic acid at a molar ratio of 1:1 are stirred and heated to be clear and transparent at 80℃, or choline chloride and lactic acid at a molar ratio of 1:1 are stirred and heated to be clear and transparent at 80℃.
[0015] Optionally, in step S1, the mass-volume ratio of the tobacco and the deep eutectic solvent is 10 g:100 mL.
[0016] Optionally, in step S1, the heating condition is that the temperature is 80℃ and the time is 1-3h.
[0017] Optionally, in step S2, the deionized water is 100 mL.
[0018] The centrifugal condition is that the rotation speed is 3000 r / min and the time is 10 min.
[0019] Optionally, in step S3, the mass ratio of the KOH and the tobacco is 2:1.
[0020] The heating reaction condition is that the temperature increasing rate is 5℃ / min, the temperature is 500℃, the time is 60 min, then the temperature is increased to 800℃, and the time is 1-3h.
[0021] Optionally, in step S4, the first extractant is diethyl ether, chloroform, acetone or ethyl acetate.
[0022] The volume ratio of the first extractant and the first liquid phase is 5:1.
[0023] The stirring condition is that the rotation speed is 500 r / min and the time is 30 min.
[0024] The temperature condition of the drying is 60-80℃.
[0025] Optionally, in step S5, the second extractant is diethyl ether, chloroform or n-hexane.
[0026] In a second aspect, the present application provides a tobacco extract and a target carbon material obtained by the method of the first aspect.
[0027] In a third aspect, the present application provides an application of the tobacco extract and the target carbon material obtained by the method of the first aspect, wherein the porous carbon in the target carbon material is used for the preparation of an electrode material and the adsorption of heavy metal ions in an aqueous solution.
[0028] The nicotine in the tobacco extract is used as a raw material for the preparation of a health cigarette, a smoking cessation paste, an external medicine for treating joint pain or muscle spasm.
[0029] The solanesol in the tobacco extract is used as a raw material for the preparation of coenzyme Q10, vitamin K2, an anticancer synergist SDB, an antibacterial, an anti-inflammatory, a medicine for treating cardiovascular diseases and an anti-ulcer medicine.
[0030] Compared with the prior art, the present application has the following advantages:
[0031] The application provides a method for synchronously obtaining tobacco extract and target carbon material from waste tobacco.
[0032] The application also provides an application of the method for synchronously obtaining tobacco extract and target carbon material from waste tobacco. 2 The application provides the target carbon material, which has reasonable pore size distribution, is doped with nitrogen elements, has high specific surface area (the surface area is up to 1460 m
[0033] The target carbon material has high specific surface area and reasonable pore size distribution, and can be used for preparation of electrode material and adsorption of heavy metal ions in aqueous solution. BRIEF DESCRIPTION OF DRAWINGS
[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort on the basis of these drawings.
[0035] Figure 1 The application provides a method for synchronously obtaining tobacco extract and target carbon material from waste tobacco.
[0036] Figure 2 The application provides a method for synchronously obtaining tobacco extract and target carbon material from waste tobacco.
[0037] Figure 3 N2adsorption-desorption isotherm of the porous carbon in the target carbon material provided by the embodiment of the present application is shown;
[0038] Figure 4 A pore size distribution graph of the porous carbon in the target carbon material provided by the embodiment of the present application is shown. DETAILED DESCRIPTION
[0039] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. The following description of at least one exemplary embodiment is actually only illustrative, but not as any limitation on the present application and its application or use. Based on the embodiments in the present application, any person under the inspiration of the present application or combining the present application with other prior art features to obtain any product same or similar to the present application falls within the protection scope of the present application. In addition, all other embodiments obtained by the ordinary skilled in the art without carrying out creative labor fall within the protection scope of the present application.
[0040] The specific experimental steps or conditions not mentioned in the embodiments can be carried out according to the conventional experimental steps or conditions described in the prior art in the field. The reagents and other instruments not mentioned by the manufacturer are all conventional reagent products that can be obtained by purchase. In addition, the drawings are only schematic illustrations of the embodiments of the present application, and are not necessarily drawn to scale. The same reference signs in the drawings represent the same or similar parts, and thus repeated description thereof will be omitted. Some block diagrams shown in the drawings are functional entities, and do not necessarily correspond to physically or logically independent entities.
[0041] The technologies, methods and devices known to the ordinary skilled in the relevant field can not be discussed in detail, but in appropriate cases, the technologies, methods and devices should be regarded as part of the authorized description.
[0042] In the description of the present application, it should be understood that the use of the words "first", "second" and the like to qualify elements is only for the convenience of distinguishing the corresponding elements, and the above words have no special meaning unless otherwise stated, and therefore cannot be understood as limiting the protection scope of the present application.
[0043] In addition, the technical features involved in different embodiments of the present application described below can be combined with each other as long as they do not conflict with each other.
[0044] There are some reports and patents on obtaining tobacco extract or carbon materials from waste tobacco. Scientists prepare microbial fertilizer from waste tobacco leaves or residues after extracting effective components. Chinese patent CN103274784A discloses a method for producing organic fertilizer from field-treated waste tobacco leaves. The waste tobacco leaves are crushed, and then wheat straw, urea, horse manure, etc. are added for natural fermentation to prepare organic fertilizer. However, because the nicotine component has not been removed, it inhibits many microorganisms, resulting in a long preparation period, low efficiency, and low number of viable bacteria for microbial fertilizer. Chinese patent CN101050212A discloses a method for simultaneously extracting high-purity natural nicotine and solanesol from waste tobacco. This method only extracts the components in waste tobacco, and does not involve the high-value utilization of the residues after extraction.
[0045] Chinese patent CN200510010670.2 discloses a method for preparing high-specific-surface-area activated carbon from tobacco stem solid waste. The tobacco stem solid waste is crushed, dried, immersed in a KOH solution for activation, and then dried after acid washing to obtain activated carbon. Chinese patent CN111115629A discloses a method for preparing a tobacco stem activated carbon-NiCo2S4 composite electrode material. The method includes pretreatment, carbonization, and activation of the tobacco stem to obtain a tobacco stem activated carbon, i.e., a high-specific-surface-area carbon material. Chinese patent CN112713006A discloses a method for preparing a tobacco stem activated carbon-based NiCo2S4 composite electrode material. Specifically, the tobacco stem-based activated carbon electrode material is added to an aqueous solution containing Co(NO3)2·6H2O, Ni(NO3)2·6H2O, hexamethylenetetramine, and urea to prepare an electrode material with high specific capacity and specific capacity retention rate. However, in the preparation process of these electrode materials, even though the use of tobacco waste as raw material reduces production costs, a lot of waste gas and waste liquid are generated during production, and solanesol and nicotine in tobacco are not fully utilized.
[0046] Based on the above-mentioned methods for preparing tobacco extract or target carbon materials from tobacco waste, the utilization rate of tobacco waste is low, the types of products obtained are single, and porous carbon, nicotine, and solanesol in tobacco waste cannot be extracted simultaneously. Moreover, waste gas and waste water are generated during preparation, which is not friendly to the environment. To solve these problems, the present application proposes a method for treating tobacco waste with a deep eutectic solvent to obtain tobacco residues and a liquid phase, and then mixing the tobacco residues with a KOH solution and heating to prepare a biomass porous carbon material, while extracting nicotine and solanesol from the liquid phase. In this way, nicotine, solanesol, and porous carbon in the target carbon material can be obtained simultaneously, realizing the high-value utilization of waste tobacco and reducing resource waste. Moreover, almost no waste gas and waste water are generated during the entire preparation process, the deep eutectic solvent used is a green solvent and can be recycled, which is friendly to the environment. The specific implementation is as follows:
[0047] In a first aspect, the present application provides a method for simultaneously obtaining tobacco extract and target carbon material from waste tobacco, Figure 1 A flow chart of the preparation method of the tobacco extract and the target carbon material provided by the embodiment of the present application is shown in FIG. 1. Figure 1 As shown in the figure, the preparation method comprises the following steps:
[0048] S1, adding a deep eutectic solvent to the dried and crushed tobacco, and heating under stirring to obtain a mixture of tobacco and the deep eutectic solvent;
[0049] In the specific implementation of this step, the deep eutectic solvent is obtained by stirring and heating choline chloride and urea at a molar ratio of 1:2 to be clear and transparent at 80℃, or choline chloride and oxalic acid at a molar ratio of 1:1 to be clear and transparent at 80℃, or choline chloride and lactic acid at a molar ratio of 1:1 to be clear and transparent at 80℃. The mass-volume ratio of tobacco and the deep eutectic solvent is 10g:100mL. The heating condition is that the temperature is 80℃ and the time is 1-3h.
[0050] S2, adding an appropriate amount of deionized water to the mixture, and centrifuging to obtain tobacco residue and a first liquid phase;
[0051] In the specific implementation of this step, deionized water is added to the mixture, and the first liquid phase and the tobacco residue are obtained by centrifuging. The first liquid phase is removed to a beaker, and the tobacco residue is centrifuged with water. This cycle is repeated 2-3 times until the supernatant is clear and transparent after centrifugation to ensure complete centrifugation. The amount of deionized water is 100mL. The centrifugation condition is that the rotation speed is 3000r / min and the time is 10min.
[0052] S3, mixing KOH solution with the tobacco residue, and then performing a heating reaction to obtain a porous carbon, which is the target carbon material;
[0053] In the specific implementation of this step, KOH is weighed, mixed with a small amount of deionized water, heated with the tobacco residue, and then dried. After drying, it is added to a tube furnace for heating carbonization, then activated by increasing the temperature, and finally neutralized, washed, and dried with deionized water to obtain the porous carbon. The mass ratio of KOH to tobacco is 2:1. The heating reaction condition is that the temperature increasing rate is 5℃ / min, the carbonization temperature is 500℃, the time is 60min, the activation temperature is increased to 800℃, and the time is 1-3h.
[0054] S4, adding a first extraction agent to the first liquid phase, stirring, and then placing it in an environment at-20℃ for static stratification. After separation, a second liquid phase and a second solid phase are obtained. The second solid phase is dried to obtain the deep eutectic solvent;
[0055] In the implementation of the step, the first liquid phase is added with a first extractant, and stirring is performed under a magnetic stirrer to ensure uniform mixing, and then placed in a refrigerator at-20℃ for freezing, and after separation, a second liquid phase and a second solid phase are obtained, the deep eutectic aqueous solution becomes the second solid phase, and the first extractant extracted with nicotine and solanesol remains liquid as the second liquid phase. The second solid phase is dried to obtain a reusable deep eutectic solvent. The first extractant is diethyl ether, chloroform, acetone or ethyl acetate. The volume ratio of the first extractant to the first liquid phase is 5:1. The stirring condition is that the rotating speed is 500 r / min and the time is 30 min. The temperature condition for drying is 60-80℃.
[0056] S5, using dilute sulfuric acid as a washing agent to wash the second liquid phase in a separatory funnel, so that nicotine in the second liquid phase is converted into nicotine sulfate into the washing agent, and a third liquid phase containing nicotine sulfate and a fourth liquid phase from which nicotine is removed are obtained, and then anhydrous calcium chloride is added to the fourth liquid phase and dried and rotary evaporated to obtain the tobacco extract solanesol;
[0057] In the implementation of the step, the second liquid phase is washed several times with dilute sulfuric acid as a washing agent in a separatory funnel, and after standing and layering, a third liquid phase containing nicotine sulfate and a fourth liquid phase from which nicotine is removed are obtained. The third liquid phase is transferred and collected into a beaker, and after observing that there is substantially no nicotine in the fourth liquid phase, the fourth liquid phase is washed with clean water until the pH is neutral, and then anhydrous calcium chloride is added to the fourth liquid phase for drying, and then the first extractant is removed by rotary evaporation to obtain solanesol.
[0058] S6, adjusting the pH of the third liquid phase to be greater than 10, and then adding a second extractant, and extracting and layering with a separatory funnel, and after separation, obtaining an organic phase containing nicotine, and removing the second extractant from the organic phase by rotary evaporation to obtain the tobacco extract nicotine.
[0059] In the implementation of the step, the second extractant is diethyl ether, chloroform or n-hexane.
[0060] The tobacco extract and the target carbon material are obtained simultaneously through the above preparation steps, which greatly improves the utilization rate and added value of waste tobacco and reduces resource waste. And the entire preparation process almost does not produce waste gas and waste water, the deep eutectic solvent selected is a green solvent and can be recycled, which is more friendly to the environment.
[0061] In a second aspect, the present application provides a tobacco extract and a target carbon material obtained by the method of the first aspect.
[0062] In a third aspect, the application provides an application of the tobacco extract and the target carbon material obtained by the method of the first aspect, wherein the porous carbon in the target carbon material is used for preparation of an electrode material and adsorption of heavy metal ions in an aqueous solution.
[0063] The nicotine in the tobacco extract is used as a raw material for preparation of a health cigarette, a smoking cessation paste, an external medicine for treating joint pain or muscle spasm.
[0064] The solanesol in the tobacco extract is used as a raw material for preparation of a coenzyme Q10, a vitamin K2, an anticancer synergist SDB, an antibacterial, an anti-inflammatory, a medicine for treating cardiovascular diseases and an anti-ulcer medicine.
[0065] Experimental verification results show that the porous carbon in the target carbon material has a reasonable pore size distribution, is doped with nitrogen elements, has a high specific surface area (up to 1460 m 2 / g), generates a pseudo-capacitance, has a relatively high specific capacitance, has a relatively high capacitance retention rate due to the mesopores, and can be used for an electrode material of a supercapacitor and has a high specific capacitance and a high cycle stability.
[0066] In order to enable those skilled in the art to more clearly understand the application, the method for synchronously obtaining the tobacco extract and the target carbon material from the waste tobacco and the application thereof are described in detail through the following examples.
[0067] Figure 2 A preparation step flowchart of the tobacco extract and the target carbon material provided by the embodiment of the application is shown, and the following examples are prepared by referring to the flowchart.
[0068] Example 1
[0069] Step 1, choline chloride and urea with a molar ratio of 1:2 are weighed, and are stirred and heated at 80 DEG C to obtain a deep eutectic solvent (DES). The deep eutectic solvent is added to the tobacco after drying and crushing, and is stirred and heated at 80 DEG C for 3 hours to obtain a mixture of the tobacco and the deep eutectic solvent. The mass-volume ratio of the tobacco and the deep eutectic solvent is 10 g:100 mL.
[0070] Step 2, 100 mL of deionized water is added to the mixture, and is centrifuged at 3000 r / min for 10 min to obtain a first upper liquid phase and a lower tobacco residue. The first upper liquid phase is transferred to a beaker, and the lower tobacco residue is added with water and is centrifuged at 3000 r / min for 10 min, and the cycle is repeated for 3 times until the upper liquid phase is clear and transparent after centrifugation.
[0071] Step 3: Weigh KOH at twice the initial tobacco mass, add a small amount of deionized water and mix with tobacco residue, heat and dry, then add to a tube furnace, heat to 500℃ at a rate of 5℃ / min for 60 min, then heat to 800℃ for 1 hour, finally neutralize with deionized water, wash, and dry to produce porous carbon for electrode materials.
[0072] Step 4: Add diethyl ether to the first liquid phase, stir at 500 r / min for 30 min with a magnetic stirrer, and then freeze in a refrigerator at -20℃. After separation, the second liquid phase and the second solid phase are obtained. The second solid phase is dried in an oven at 60℃ to obtain a reusable deep eutectic solvent.
[0073] Step 5: Using dilute sulfuric acid as a detergent, wash the second liquid phase several times in a separatory funnel. After standing and separating the layers, obtain a third liquid phase containing nicotine sulfate and a fourth liquid phase free of nicotine. Transfer the third liquid phase to a beaker and observe it on a TLC plate until the fourth liquid phase is essentially free of nicotine. Then wash the fourth liquid phase with water to remove the sulfuric acid until the pH is neutral. Add anhydrous calcium chloride to the obtained fourth liquid phase and dry it. Then remove the ether by rotary evaporation to obtain the tobacco extract—solaneneol. This solaneneol is used as a raw material for preparing coenzyme Q10, vitamin K2, the anticancer synergist SDB, antibacterial, anti-inflammatory, cardiovascular disease treatment, and anti-ulcer drugs.
[0074] Step 6: Adjust the pH of the third liquid phase to greater than 10 with NaOH, then add chloroform, extract using a separatory funnel, allow to stand and separate, and obtain an organic phase containing nicotine. Remove the chloroform from the organic phase using a rotary evaporator to obtain the tobacco extract—nicotine. This nicotine is suitable as a raw material for the preparation of health cigarettes, smoking cessation pastes, and topical medications for treating joint pain or muscle spasms.
[0075] Figure 3 The N2 adsorption-desorption isotherm of porous carbon in the target carbon material provided in Embodiment 1 of the present invention is shown, such as Figure 3 As shown, the adsorption capacity increases sharply at relatively low pressure, and the subsequent curve is close to horizontal, with the adsorption capacity approaching a limit value. This is a typical Langmuir isotherm. The obtained N2 adsorption-desorption isotherm of the porous carbon is a type I isotherm and has a hysteresis loop, indicating that it has a wide micropore size distribution and may also have narrow mesopores.
[0076] Figure 4 The diagram shows the pore size distribution of porous carbon in the target carbon material provided in Embodiment 1 of the present invention, as follows: Figure 4 As shown, micropores refer to pores with an internal pore width of less than 2 nm, while mesopores are pores with a width between 2 and 50 nm. As can be seen from the pore size distribution diagram, the pore size distribution of the obtained porous carbon is mainly micropores, with a small amount of mesopores.
[0077] Porous carbon specific surface area data: BET specific surface area was 1459.9 m 2 / g.
[0078] Example 2
[0079] Step 1, weigh the molar ratio of 1:1 choline chloride and oxalic acid, and stir heat to a clear transparent solution at 80°C to obtain a deep eutectic solvent (DES). Add the deep eutectic solvent to the tobacco after drying and crushing, and stir heat at 80°C for 1.5h to obtain a mixture of tobacco and deep eutectic solvent. The mass-volume ratio of tobacco and deep eutectic solvent is 10g:100mL.
[0080] Step 2, add 100mL of deionized water to the mixture, centrifuge at 3000r / min for 10min to obtain the upper first liquid phase and the lower tobacco residue. Transfer the upper first liquid phase to a beaker, and continue to centrifuge the lower tobacco residue with water at 3000r / min for 10min, and repeat this cycle 3 times until the supernatant is clear and transparent after centrifugation.
[0081] Step 3, weigh 2 times the initial tobacco mass of KOH, add a small amount of deionized water to mix with the tobacco residue and heat, then dry and add to a tube furnace, heat to 500°C at a rate of 5°C / min for carbonization for 60min, then heat to 800°C for activation for 2h, finally neutralize, wash with deionized water, dry, and prepare the porous carbon for heavy metal ion adsorption.
[0082] Step 4, add ethyl acetate to the first liquid phase, stir at 500r / min for 30min under a magnetic stirrer, then freeze in a refrigerator at -20°C, separate to obtain a second liquid phase and a second solid phase, and dry the second solid phase in a 70°C oven to obtain reusable deep eutectic solvent.
[0083] Step 5, dilute sulfuric acid as a washing agent is used to wash the second liquid phase several times in a separatory funnel, and the layers are separated to obtain a third liquid phase containing nicotine sulfate and a fourth liquid phase without nicotine. Transfer the third liquid phase to a beaker, and observe the fourth liquid phase to be essentially free of nicotine, then wash the fourth liquid phase with water until the pH is neutral, then add anhydrous calcium chloride to dry, and then use a rotary evaporator to remove the ethyl acetate to obtain the tobacco extract-solanesol. The solanesol is used as a raw material for the preparation of coenzyme Q10, vitamin K2, anticancer synergist SDB, antibacterial, anti-inflammatory, cardiovascular disease treatment, and anti-ulcer drugs.
[0084] Step 6, adjust the pH of the third liquid phase to greater than 10 with NaOH, then add n-hexane, extract with a separatory funnel, and separate to obtain an organic phase containing nicotine. The n-hexane is removed from the organic phase using a rotary evaporator to obtain the tobacco extract-nicotine. The nicotine is suitable for use as a raw material for the preparation of health cigarettes, smoking cessation pastes, and external medicines for treating joint pain or muscle spasms.
[0085] The specific surface area, N2sorption-desorption isotherm, and pore size distribution of the target carbon material prepared in this example have similar trends to those of Example 1, and are not repeated here.
[0086] Example 3
[0087] Step 1, weigh choline chloride and lactic acid in a molar ratio of 1:1, and stir and heat at 80°C until a clear and transparent solution is obtained to obtain a deep eutectic solvent (DES). Add the deep eutectic solvent to the dried and crushed tobacco, and stir and heat at 80°C for 2 h to obtain a mixture of tobacco and deep eutectic solvent. The mass-volume ratio of tobacco to deep eutectic solvent is 10 g:100 mL.
[0088] Step 2, add 100 mL of deionized water to the mixture, and centrifuge at 3000 r / min for 10 min to obtain an upper first liquid phase and a lower tobacco residue. Transfer the upper first liquid phase to a beaker, and continue to centrifuge the lower tobacco residue at 3000 r / min for 10 min with water, and repeat this cycle 3 times until the upper liquid phase is clear and transparent after centrifugation.
[0089] Step 3, weigh KOH that is 2 times the mass of the initial tobacco, add a small amount of deionized water to the tobacco residue, heat and dry, then add to a tube furnace, heat to 500°C at a rate of 5°C / min, carbonize for 60 min, then heat to 800°C and activate for 2 h, finally neutralize and wash with deionized water, dry, and prepare a porous carbon for electrode material.
[0090] Step 4, add acetone to the first liquid phase, stir at 500 r / min for 30 min under a magnetic stirrer, then freeze in a refrigerator at -20°C, separate to obtain a second liquid phase and a second solid phase, dry the second solid phase in a 70°C oven to obtain reusable deep eutectic solvent.
[0091] Step 5, the second liquid phase is washed several times with dilute sulfuric acid as a washing agent in a separatory funnel, and is allowed to stand and separate into layers, to obtain a third liquid phase containing nicotine sulfate and a fourth liquid phase from which nicotine has been removed. The third liquid phase is transferred and collected in a beaker, and the fourth liquid phase is washed with clean water until the pH is neutral. The obtained fourth liquid phase is dried with anhydrous calcium chloride, and then is subjected to rotary evaporation to remove acetone, to obtain the tobacco extract-solanesol. The solanesol is used as a raw material for preparing coenzyme Q10, vitamin K2, anticancer synergist SDB, antibacterial, anti-inflammatory, cardiovascular disease treatment, and anti-ulcer drugs.
[0092] Step 6, the pH of the third liquid phase is adjusted to greater than 10 with NaOH, and then ether is added. Extraction is performed with a separatory funnel, and the mixture is allowed to stand and separate into layers. After separation, an organic phase containing nicotine is obtained. The organic phase is subjected to rotary evaporation to remove ether, to obtain the tobacco extract-nicotine. The nicotine is suitable for use as a raw material for preparing health cigarettes, a smoking cessation paste, and an external medicine for treating joint pain or muscle spasms.
[0093] The specific surface area, N2sorption-desorption isotherm, and pore size distribution graph of the target carbon material prepared in this example have similar trends to those of Example 1, and are not repeated here.
[0094] In the description of the present specification, the description of the terms "one embodiment", "some embodiments", "an example", "a specific example", or "some examples" and the like means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, a person skilled in the art can combine and combine different embodiments or examples described in the present specification.
[0095] For the method embodiments, for the sake of simple description, they are all described as a combination of a series of actions, but those skilled in the art should know that the present application is not limited by the order of the described actions, because according to the present application, certain steps can be performed in other order or simultaneously. Secondly, those skilled in the art should know that the embodiments described in the specification are all preferred embodiments, and the actions and components involved are not necessarily necessary for the present application.
[0096] The above describes in detail the method for simultaneously obtaining tobacco extract and target carbon material from waste tobacco and the application of the method. The principles and implementation manners of the application are described by using specific examples. The above description of the examples is only used to help understand the method and the core idea of the application. Meanwhile, for those skilled in the art, the specific implementation manners and application ranges can be changed according to the idea of the application. In conclusion, the content of the specification should not be understood as a limitation on the application.
Claims
1. A method for simultaneously obtaining a tobacco extract and a target carbon material from waste tobacco, the method comprising: The method comprises the following steps: S1, adding a deep eutectic solvent to the tobacco after drying and crushing, and heating under stirring to obtain a mixture of tobacco and deep eutectic solvent; S2, adding a proper amount of deionized water to the mixture and centrifuging to obtain tobacco residue and a first liquid phase; S3, mixing KOH solution with the tobacco residue and then performing a heating reaction to obtain porous carbon, which is the target carbon material; S4, adding a first extractant to the first liquid phase, stirring, and then placing in an environment at-20℃ to stand and separate into a second liquid phase and a second solid phase, drying the second solid phase to obtain the deep eutectic solvent; S5, using dilute sulfuric acid as a washing agent to wash the second liquid phase in a separatory funnel, so that nicotine in the second liquid phase is converted into nicotine sulfate into the washing agent, and then adding anhydrous calcium chloride to the fourth liquid phase and performing drying and rotary evaporation to obtain the tobacco extract-nianol; S6, adjusting the pH of the third liquid phase to be greater than 10, then adding a second extractant, and using a separatory funnel to perform extraction and standing and separation to obtain a nicotine-containing organic phase, and using a rotary evaporator to remove the second extractant from the organic phase to obtain the tobacco extract-nicotine; In step S1, the deep eutectic solvent is obtained by stirring and heating choline chloride and urea at a molar ratio of 1:2 to be clear and transparent at 80℃, or choline chloride and oxalic acid at a molar ratio of 1:1 to be clear and transparent at 80℃, or choline chloride and lactic acid at a molar ratio of 1:1 to be clear and transparent at 80℃. In step S1, the mass-volume ratio of the tobacco and the deep eutectic solvent is 10 g:100 mL. In step S1, the heating condition is that the temperature is 80℃ and the time is 1-3 h.
2. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. In step S2, the deionized water is 100 mL.
3. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. The centrifugation condition is that the rotation speed is 3000 r / min and the time is 10 min.
4. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. In step S3, the mass ratio of KOH to tobacco is 2:
1. The heating reaction condition is that the temperature rising rate is 5℃ / min, the temperature is 500℃, the time is 60 min, then the temperature is raised to 800℃, and the time is 1-3 h.
5. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. In step S4, the first extractant is diethyl ether, chloroform, acetone or ethyl acetate. The volume ratio of the first extractant to the first liquid phase is 5:
1.
6. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. The stirring condition is that the rotation speed is 500 r / min and the time is 30 min. The drying temperature condition is 60-80℃. In step S5, the second extractant is diethyl ether, chloroform or n-hexane.
8. A tobacco extract and a target carbon material obtained by the method of any one of claims 1-7.
7. The method of claim 1, wherein the tobacco extract and the target carbon material are simultaneously obtained from the waste tobacco. The porous carbon in the target carbon material is used for the preparation of electrode materials and the adsorption of heavy metal ions in aqueous solution. The nicotine in the tobacco extract is used as a raw material for the preparation of health cigarettes, smoking cessation paste, and external medicines for treating joint pain or muscle spasms.
9. Use of a tobacco extract obtained by the process according to any one of claims 1 to 7 and a target carbon material, characterized in that, The solanesol in the tobacco extract is used for preparing raw materials of coenzyme Q10, vitamin K2, anti-cancer synergist SDB, anti-bacterial, anti-inflammatory, cardiovascular disease treating and anti-ulcer drugs.
Citation Information
Patent Citations
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