Comprehensive treatment method of waste tobacco leaves and dyeing fragrant line for cigarettes
By treating waste tobacco leaves with plasma and dyeing cotton fibers, combined with alcohol extraction and distillation techniques, the problem of low recycling rate of waste tobacco leaves has been solved, and the extraction of high-purity neophytadiene and the preparation of dyed flavoring threads for cigarettes have been achieved.
Patent Information
- Application Number
- CN202511129060.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-13
- Publication Date
- 2025-11-25
AI Technical Summary
Existing technologies result in low recycling rates, low extraction rates and product purity of waste tobacco leaves, and high operating costs, leading to resource waste and environmental pollution.
Waste tobacco leaves were pulverized by plasma treatment, and tobacco extract was extracted by reflux with an ethanol aqueous solution. The extract was then adsorbed and dyed using cotton fiber yarn. Combined with anhydrous ethanol extraction and steam distillation, colored flavoring thread for cigarettes and neophytadiene were prepared.
It improved the comprehensive utilization rate of waste tobacco leaves, enhanced the dyeing effect of yarn and the purity of new phytadiene, simplified the operation process, and reduced costs.
Smart Images
Figure CN121003319A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of tobacco resource utilization technology, and in particular to a comprehensive treatment method for waste tobacco leaves and a dyeing flavoring thread for cigarettes. Background Technology
[0002] The tobacco processing industry generates millions of tons of waste tobacco leaves annually, including tobacco dust, low-grade tobacco leaves, and unsold tobacco products. Currently, these waste tobacco leaves are mainly disposed of through landfill or incineration, which not only causes heavy metal pollution in the soil and greenhouse gas emissions but also results in a serious waste of resources. Among related technologies, there are processes for re-extracting certain components from waste tobacco leaves; however, these methods generally suffer from low extraction rates, low product purity, and high operating costs. Therefore, improving the reuse rate of waste tobacco leaves has become an urgent need for the industry. Summary of the Invention
[0003] To address or partially address the problems existing in related technologies, this invention provides a comprehensive treatment method for waste tobacco leaves and a dyed flavoring thread for cigarettes.
[0004] This invention provides a comprehensive treatment method for waste tobacco leaves, comprising: Step a) After crushing the waste tobacco leaves, they are subjected to plasma treatment to obtain pretreated waste tobacco leaf powder; Step b) The waste tobacco powder is refluxed and extracted using an aqueous ethanol solution, and the extract is concentrated to obtain a first tobacco extract; Step c) Dilute the first tobacco extract with water to obtain a diluted extract solution; immerse cotton fiber yarn pretreated with metal salt mordant in the diluted extract solution for adsorption dyeing; obtain dyed cigarette thread after adsorption dyeing; collect the remaining diluted extract solution after adsorption dyeing, concentrate it, and obtain a second tobacco extract. Step d) Using anhydrous ethanol as a solvent, the second tobacco extract is extracted with alcohol. After extraction, the extract is filtered and the filtrate is concentrated under reduced pressure to obtain tobacco pure oil. Step e) The tobacco purified oil is subjected to steam distillation to collect the organic fraction and obtain neophytadiene.
[0005] Furthermore, in step a), the plasma treatment power is 100~500W and the treatment time is 1~10min.
[0006] Furthermore, in step b), the mass-to-volume ratio of waste tobacco powder to ethanol aqueous solution is 1g:5~20L, and the extraction temperature is 75~85℃.
[0007] Further, in step c), the cotton fiber yarn pretreated with the metal salt mordant is: cotton fiber yarn pre-impregnated with potassium aluminum sulfate solution.
[0008] Furthermore, in step c), the ratio of the first tobacco extract diluted with water is 1g:5~50L.
[0009] Furthermore, in step c), the staining adsorption temperature is 60~100℃ and the time is 0.5-2h.
[0010] Furthermore, in step d), the ratio of the second tobacco extract to anhydrous ethanol is 1g:5~20L.
[0011] Further, in step d), the filtering specifically involves: Immediately after alcohol extraction, the first filtration was performed to obtain the intermediate filtrate. The intermediate filtrate is frozen and then subjected to a second filtration to obtain the filtrate.
[0012] Furthermore, in step d), the temperature for vacuum concentration is 40~50℃.
[0013] The present invention also provides a dyed flavoring thread for cigarettes, which is prepared according to any one of the methods described above.
[0014] The comprehensive treatment method for waste tobacco leaves provided by this invention can include the following beneficial effects: 1) Before extracting the extract, the waste tobacco leaves are first pulverized by plasma bombardment to loosen the cellulose-lignin structure. This makes it easier for the ethanol solvent to penetrate during the subsequent extraction process, thus increasing the extract yield. At the same time, it can also enhance pigment release and is more conducive to increasing the dissolution of dye precursors such as chlorophyll and carotenoids, thereby improving the yarn dyeing effect.
[0015] 2) Before preparing tobacco pure oil, cotton fiber yarn is used to dye and adsorb tobacco extract. On the one hand, natural pigments in the extract (such as chlorophyll and carotenoids) are adsorbed onto the yarn, thus giving the yarn a specific color. At the same time, some polar aroma components are also adsorbed onto the yarn, thus giving the yarn its aroma characteristics, thereby preparing dyed scented yarn. On the other hand, polar impurities in the extract (such as polyphenols and alkaloids) are adsorbed by the yarn, while non-polar neophytadienes and their precursors remain in the solution. This achieves preliminary impurity removal from the extract, reduces the impact of these polar components on the subsequent extraction of neophytadienes, and improves the purity of the extracted neophytadienes.
[0016] 3) The method provided by this invention is simple to operate, does not involve high-cost raw materials or equipment, and can simultaneously achieve yarn dyeing and extraction of new phytodiene. The extracted new phytodiene has high purity, thereby realizing the comprehensive utilization of waste tobacco leaves with high utilization rate.
[0017] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit the invention. Attached Figure Description
[0018] The above and other objects, features and advantages of the present invention will become more apparent from the more detailed description of exemplary embodiments of the invention in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same parts.
[0019] Figure 1 This is the 1H NMR spectrum of the organic fraction prepared in Example 1 of this invention; Figure 2 This is the carbon NMR spectrum of the organic fraction prepared in Example 1 of this invention; Figure 3 This is a chromatogram of the novel phytadiene prepared in Example 1 of the present invention; Figure 4 This is the mass spectrum of the novel phytadiene prepared in Example 1 of this invention; Figure 5 This is a K / S curve diagram of the preparation of dyed flavoring thread for cigarettes according to an embodiment of the present invention; Figure 6 This is a K / S curve diagram of the cigarette dyeing fragrance thread prepared in Example 1 and the comparative example of the present invention. Detailed Implementation
[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0021] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular forms “a,” “the,” and “the” used in this invention and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise. It should also be understood that the term “and / or” as used herein refers to and includes any or all possible combinations of one or more of the associated listed items.
[0022] It should be understood that although the terms "first," "second," "third," etc., may be used in this invention to describe various information, this information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another. For example, without departing from the scope of this invention, first information may also be referred to as second information, and similarly, second information may also be referred to as first information. Thus, features defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.
[0023] Regarding the question of how to improve the utilization rate of waste tobacco leaves, the inventors of this application first considered using them as raw materials to extract neophytadiene, specifically: Under the trend of reducing harm and tar in the tobacco industry, improving the aroma quality of cigarettes has become a key direction for enterprises' technological breakthroughs. As natural aroma sources, endogenous aroma substances in tobacco exhibit unique advantages in enhancing and preserving cigarette aroma due to their high compatibility with tobacco itself. These substances are both inherent aroma components of tobacco and aroma precursors; through scientific formulation and addition, they can significantly enhance the aroma concentration and optimize the taste experience, thereby comprehensively improving the sensory quality of cigarettes. Terpenoids are an important aroma component system in tobacco, among which neophytadiene, a diterpene, is particularly prominent. This compound is a colorless, odorless, oily liquid with excellent photostability and low volatility. It is not only the most abundant aroma precursor in tobacco but also a key factor determining the quality of tobacco leaves. Therefore, developing its extraction and purification technology has significant scientific research value and application prospects for promoting the high-quality development of the tobacco industry. Tobacco leaves are the most important natural source of neophytadiene. For fresh tobacco leaves, neophytadiene is obtained by steam distillation combined with rectification. For virgin tobacco leaves, neophytadiene is extracted by supercritical CO2 extraction, ultrasound-assisted extraction and other methods. For waste tobacco leaves, neophytadiene is extracted by ethanol extraction combined with silica gel column chromatography and other steps.
[0024] Therefore, the inventors of this application considered using waste tobacco leaves as raw materials to extract neophytadiene. Through research, the inventors discovered that existing extraction methods either produce low-purity products or are cumbersome, complex, and costly. To improve product purity while reducing operational complexity, the inventors conducted a series of studies and unexpectedly discovered that using cotton fiber yarn to dye the extract simultaneously achieves preliminary impurity removal, significantly reducing the difficulty of subsequent extraction processes and resulting in high-purity neophytadiene. However, this method suffers from low extract yield, affecting the resource utilization rate of waste tobacco leaves. Further research by the inventors revealed that plasma treatment of waste tobacco leaves before preparing tobacco extract not only enhances pigment release and subsequent dyeing effects but also increases the yield of tobacco extract.
[0025] Based on the above, embodiments of the present invention provide a comprehensive treatment method for waste tobacco leaves, which includes the following steps: Step a) After crushing the waste tobacco leaves, they are subjected to plasma treatment to obtain pretreated waste tobacco leaf powder; Step b) The waste tobacco powder is refluxed and extracted using an aqueous ethanol solution, and the extract is concentrated to obtain a first tobacco extract; Step c) Dilute the first tobacco extract with water to obtain a diluted extract solution; immerse cotton fiber yarn pretreated with metal salt mordant in the diluted extract solution for adsorption dyeing; obtain dyed cigarette thread after adsorption dyeing; collect the remaining diluted extract solution after adsorption dyeing, concentrate it, and obtain a second tobacco extract. Step d) Using anhydrous ethanol as a solvent, the second tobacco extract is extracted with alcohol. After extraction, the extract is filtered and the filtrate is concentrated under reduced pressure to obtain tobacco pure oil. Step e) The tobacco purified oil is subjected to steam distillation to collect the organic fraction and obtain neophytadiene.
[0026] Plasma treatment is a non-thermodynamic dry modification technology that uses ionized gas (such as air or nitrogen) to generate high-energy particles (electrons, ions, and free radicals) to bombard the surface of materials at room temperature and pressure. In this embodiment, plasma treatment is used in the pretreatment of waste tobacco leaves. Its effects are: plasma bombardment of the pulverized tobacco leaves loosens the cellulose-lignin structure, making it easier for the ethanol solvent to penetrate during subsequent extraction; it enhances pigment release, which is more conducive to increasing the dissolution of dye precursors such as chlorophyll and carotenoids; it improves the extract yield, laying the foundation for subsequent enrichment of new phytadienes; during plasma treatment, high-energy particles preferentially decompose large molecular impurities such as starch and pectin, reducing the burden on subsequent filtration; and plasma treatment is a room-temperature treatment method, which can protect heat-sensitive components. As a preferred embodiment, the plasma treatment power is preferably 100~500W, and the treatment time is preferably 1~10min. More preferably, the plasma treatment power is preferably 200~400W, and the treatment time is preferably 2~4min.
[0027] Step b) is the step of extracting tobacco extract from the waste tobacco powder after plasma treatment. The purpose of using an ethanol-water solution for reflux extraction in this step is to dissolve polar components (such as chlorophyll derivatives and browning pigments) and weakly polar components (such as neophytadiene precursors and ester aroma compounds) in the tobacco powder. Due to the plasma treatment in the preceding steps, the extraction rate in this step is significantly improved. Using reflux extraction avoids the introduction of other solvents and reduces the difficulty of subsequent purification. The mass-to-volume ratio of waste tobacco powder to ethanol-water solution is 1g:5~20L, and the extraction temperature is 75~85℃. More preferably, the mass-to-volume ratio of waste tobacco powder to ethanol-water solution is 1g:10~20L, and the extraction temperature is 80℃. The concentration of the ethanol-water solution is preferably 80-90%.
[0028] In step c), the cotton fiber yarn pretreated with the metal salt mordant is preferably cotton fiber yarn pre-impregnated with potassium aluminum sulfate solution. Using potassium aluminum sulfate as a metal salt mordant improves the dyeing effect through the following mechanism: Al 3+ It forms a complex with the hydroxyl groups of cotton fibers (cellulose), increasing the positive charge on the fiber surface; it attracts negatively charged pigment molecules (such as chlorophyll derivatives) in the extract, enhancing dye adsorption. After mordating, the dye forms covalent bonds with the fiber, reducing dye loss during the washing process after dyeing. The preferred concentration of potassium aluminum sulfate solution is 1-3%, and the preferred immersion time is 1-2 hours.
[0029] The purpose of immersing cotton fiber yarn in the diluted extract for dyeing and adsorption in this step is twofold: Firstly, natural pigments (such as chlorophyll and carotenoids) in the extract are adsorbed onto the yarn, thereby giving the yarn a specific color (such as a yellow-green color with a wavelength of 440 nm). At the same time, some polar fragrance components are also adsorbed onto the yarn, thereby giving the yarn a fragrance characteristic, thus preparing dyed scented yarn. Secondly, polar impurities (such as polyphenols and alkaloids) in the extract are adsorbed by the yarn, while non-polar neophytadienes and their precursors remain in the solution. This achieves preliminary impurity removal from the extract, reduces the impact of these polar components on the subsequent extraction of neophytadienes, and improves the purity of the extracted neophytadienes.
[0030] In this step, the ratio of the first tobacco extract diluted with water is 1g:5~50L, more preferably 1g:10~25L. The preferred temperature for dyeing and adsorption is 60~100℃, and the preferred time is 0.5-2h. More preferably, the temperature is 70~90℃, and the time is 1-2h. After dyeing and adsorption are completed, the cotton fiber yarn is washed with water and dried to obtain dyed flavoring thread for cigarettes. The diluted extract after dyeing and adsorption needs to be recycled and reused as a raw material for extracting neophytadiene. At this time, the diluted extract has undergone preliminary impurity removal due to the adsorption of cotton fiber yarn. In this step, in order to improve the subsequent extraction efficiency, the remaining diluted extract after adsorption and dyeing is concentrated to obtain the second tobacco extract.
[0031] Step d) is the step of extracting the second tobacco extract with alcohol to obtain tobacco pure oil. Anhydrous ethanol is used as the solvent for the alcohol extraction. Anhydrous ethanol can efficiently dissolve neophytadiene; simultaneously, the polysaccharides, proteins, and other macromolecules in the second tobacco extract have low solubility in anhydrous ethanol and dissolve as precipitates, which are then separated during subsequent filtration. In the alcohol extraction step, the ratio of the second tobacco extract to anhydrous ethanol is 1g:5~20L, more preferably 1g:10~20L. To improve the extraction efficiency, the alcohol extraction is preferably carried out under water bath heating conditions. Preferably, the water bath heating temperature is 50~60℃ and the extraction time is 0.5~1h; most preferably, the water bath heating temperature is 60℃ and the extraction time is 1h.
[0032] After alcohol extraction, filtration is performed to remove impurities such as wax and protein. Preferably, filtration is performed immediately after alcohol extraction, i.e., while the liquid is still hot, to prevent the wax from solidifying and clogging the filter paper. For further impurity removal, it is preferable to perform freezing followed by filtration after the aforementioned filtration. The freezing process induces the crystallization of impurities such as long-chain fatty acids and sterols. Specifically, the preferred filtration method is as follows: a first filtration is performed immediately after alcohol extraction to obtain an intermediate filtrate; the intermediate filtrate is then frozen and subjected to a second filtration to obtain a final filtrate. The freezing temperature is preferably -40 to -50°C, and the freezing time is preferably 10-12 hours. The filtration is then concentrated under reduced pressure to remove the solvent ethanol while preventing the oxidation of neophytadiene. The preferred temperature for reduced pressure concentration is 40-50°C. The concentration time under reduced pressure can be 10-30 minutes after concentration until no liquid drips. More preferably, the temperature for reduced pressure concentration is 45°C, and the concentration time is 20 minutes after concentration until no liquid drips.
[0033] After obtaining the tobacco purified oil, steam distillation is performed according to step e) to obtain the neophytadiene component. The neophytadiene component obtained according to the method provided in this embodiment has high purity, exceeding 94.2%.
[0034] Another embodiment of the present invention provides a dyed flavoring thread for cigarettes, which is prepared according to the method of the foregoing embodiment.
[0035] The comprehensive treatment method for waste tobacco leaves provided in this invention has the following advantages: 1) Before extracting the extract, the waste tobacco leaves are first pulverized by plasma bombardment to loosen the cellulose-lignin structure. This makes it easier for the ethanol solvent to penetrate during the subsequent extraction process, thus increasing the extract yield. At the same time, it can also enhance pigment release and is more conducive to increasing the dissolution of dye precursors such as chlorophyll and carotenoids, thereby improving the yarn dyeing effect.
[0036] 2) Before preparing tobacco pure oil, cotton fiber yarn is used to dye and adsorb tobacco extract. On the one hand, natural pigments in the extract (such as chlorophyll and carotenoids) are adsorbed onto the yarn, thus giving the yarn a specific color. At the same time, some polar aroma components are also adsorbed onto the yarn, thus giving the yarn its aroma characteristics, thereby preparing dyed scented yarn. On the other hand, polar impurities in the extract (such as polyphenols and alkaloids) are adsorbed by the yarn, while non-polar neophytadienes and their precursors remain in the solution. This achieves preliminary impurity removal from the extract, reduces the impact of these polar components on the subsequent extraction of neophytadienes, and improves the purity of the extracted neophytadienes.
[0037] 3) The method provided by this invention is simple to operate, does not involve high-cost raw materials or equipment, and can simultaneously achieve yarn dyeing and extraction of new phytodiene. The extracted new phytodiene has high purity, thereby realizing the comprehensive utilization of waste tobacco leaves with high utilization rate.
[0038] The technical solution of the present invention will be further described below with reference to specific embodiments: Example 1 (1) The waste tobacco leaves are crushed and treated under a plasma with a power of 200W for 4 min. An ethanol aqueous solution (ethanol concentration of 90%, the same in the following examples) is added according to the ratio of tobacco to solvent 1g:10L. The mixture is extracted by reflux at 80℃, and then the waste residue is filtered off. The extract is concentrated to obtain the first tobacco extract.
[0039] (2) Dilute the first tobacco extract with water at a ratio of 1g:10L. Add the cotton fiber yarn that has been soaked in 2% potassium aluminum sulfate for 1 hour to the above extract dilution solution at a bath ratio of 1g:50L. Dye and adsorb at 90℃ for 1 hour, wash with water, and dry to obtain dyed fragrance thread for cigarettes.
[0040] (3) Concentrate the diluted residual extract after dyeing to obtain the second tobacco extract; add the second tobacco extract to an Erlenmeyer flask, and add anhydrous ethanol at a ratio of 1g:10L for the second tobacco extract to the solvent. Heat in a water bath at 60°C for 1 hour, filter while hot to remove insoluble matter, collect the filtrate in a narrow-mouthed bottle, freeze, and filter again to remove insoluble matter. The freezing temperature is -40°C and the freezing time is 12 hours (the freezing conditions are the same in the following examples); concentrate under reduced pressure at 45°C until no liquid drips, and continue to concentrate under reduced pressure for 20 minutes to obtain the tobacco pure oil.
[0041] (4) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0042] The 1H NMR spectrum and 1C NMR spectrum of the organic fraction prepared in this embodiment are shown below. Figure 1 and Figure 2 As shown, by Figure 1 and Figure 2 It can be seen that the organic fraction is neophytadiene. The chromatogram and mass spectrum of the neophytadiene prepared in this example are shown below. Figure 3 and Figure 4 As shown, by Figure 3 and Figure 4 It can be seen that the purity of the new phytadiene extracted in this embodiment is high.
[0043] Example 2 (1) The waste tobacco leaves are crushed and treated under plasma at 300W power for 3 min. An ethanol aqueous solution is added according to the ratio of tobacco to solvent 1g:15L. The mixture is refluxed at 80℃ for a certain time, the waste residue is filtered off, and the extract is concentrated to obtain the first tobacco extract.
[0044] (2) Dilute the first tobacco extract with water at a ratio of 1g:12L. Add the cotton fiber yarn that has been soaked in 2% potassium aluminum sulfate for 1 hour to the above extract dilution solution at a bath ratio of 1g:30L. Dye and adsorb at 90℃ for 1 hour, wash with water, and dry to obtain dyed fragrance thread for cigarettes.
[0045] (3) Concentrate the diluted residual extract after dyeing to obtain the second tobacco extract; add the second tobacco extract to an Erlenmeyer flask, and add anhydrous ethanol at a ratio of 1g:15L for the second tobacco extract to the solvent. Heat in a water bath at 60℃ for 1 hour, filter while hot to remove insoluble matter, collect the filtrate in a narrow-mouthed bottle, freeze, filter again to remove insoluble matter, concentrate under reduced pressure at 45℃ until no liquid drips, and continue to concentrate under reduced pressure for 20 minutes to obtain the tobacco pure oil.
[0046] (4) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0047] Example 3 (1) The waste tobacco leaves are crushed and treated under a plasma with a power of 400W for 2 min. An ethanol aqueous solution is added according to the ratio of tobacco to solvent 1g:20L. The mixture is refluxed at 80℃ for a certain time, the waste residue is filtered off, and the extract is concentrated to obtain the first tobacco extract.
[0048] (2) Dilute the first tobacco extract with water at a ratio of 1g:20L. Add the cotton fiber yarn that has been soaked in 2% potassium aluminum sulfate for 1 hour to the above extract dilution solution at a bath ratio of 1g:40L. Dye and adsorb at 90℃ for 1 hour, wash with water, and dry to obtain dyed fragrance thread for cigarettes.
[0049] (3) Concentrate the diluted residual extract after dyeing to obtain the second tobacco extract; add the second tobacco extract to an Erlenmeyer flask, and add anhydrous ethanol at a ratio of 1g:15L for the second tobacco extract to the solvent. Heat in a water bath at 60℃ for 1 hour, filter while hot to remove insoluble matter, collect the filtrate in a narrow-mouthed bottle, freeze, filter again to remove insoluble matter, concentrate under reduced pressure at 45℃ until no liquid drips, and continue to concentrate under reduced pressure for 20 minutes to obtain the tobacco pure oil.
[0050] (4) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0051] Example 4 (1) The waste tobacco leaves are crushed and treated under a plasma with a power of 300W for 2 min. An ethanol aqueous solution is added according to the ratio of tobacco to solvent 1g:20L. The mixture is refluxed at 80℃ for a certain time, the waste residue is filtered off, and the extract is concentrated to obtain the first tobacco extract.
[0052] (2) Dilute the first tobacco extract with water at a ratio of 1g:25L. Add the cotton fiber yarn that has been soaked in 2% potassium aluminum sulfate for 1 hour to the above extract dilution solution at a bath ratio of 1g:45L. Dye and adsorb at 80℃ for 1 hour, wash with water, and dry to obtain dyed fragrance thread for cigarettes.
[0053] (3) Concentrate the diluted residual extract after dyeing to obtain the second tobacco extract; add the second tobacco extract to an Erlenmeyer flask, and add anhydrous ethanol at a ratio of second tobacco extract to solvent of 1:20. Heat in a water bath at 60°C for 1 hour, filter while hot to remove insoluble matter, collect the filtrate in a narrow-mouthed bottle, freeze and filter again to remove insoluble matter, concentrate under reduced pressure at 45°C until no liquid drips, continue for 20 minutes to obtain tobacco pure oil.
[0054] (4) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0055] Example 5 (1) The waste tobacco leaves are crushed and treated under a plasma with a power of 200W for 5 min. An ethanol aqueous solution is added according to the ratio of tobacco to solvent 1g:15L. The mixture is refluxed at 80℃ for a certain time, the waste residue is filtered off, and the extract is concentrated to obtain the first tobacco extract.
[0056] (2) Dilute the first tobacco extract with water at a ratio of 1g:15L. Add the cotton fiber yarn that has been soaked in 2% potassium aluminum sulfate for 1 hour to the above extract dilution solution at a bath ratio of 1g:35L. Dye and adsorb at 70℃ for 1 hour, wash with water, and dry to obtain dyed fragrance thread for cigarettes.
[0057] (3) Concentrate the diluted residual extract after dyeing to obtain the second tobacco extract; add the second tobacco extract to an Erlenmeyer flask, and add anhydrous ethanol at a ratio of second tobacco extract to solvent of 1:20. Heat in a water bath at 60°C for 1 hour, filter while hot to remove insoluble matter, collect the filtrate in a narrow-mouthed bottle, freeze and filter again to remove insoluble matter, concentrate under reduced pressure at 45°C until no liquid drips, continue for 20 minutes to obtain tobacco pure oil.
[0058] (4) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0059] The K / S curve of step (2) in the above embodiments for preparing the dyed flavoring thread for cigarettes is shown in the figure below. Figure 5 As shown, the yield of the first tobacco extract obtained in step (1) (extract yield), the yield of the tobacco pure oil obtained in step (2) (pure oil yield), the K / S value of the dyed flavoring thread for cigarettes in step (2) (yarn K / S value), and the purity of the new phytadiene obtained in step (4) in the above embodiments were calculated, and the results are listed in Table 1: Table 1. Extract yield, net oil yield, yarn K / S value, and neophytadiene purity for Examples 1-5
[0060] Comparative Example 1 (1) Same as Example 1.
[0061] (2) Place the first tobacco extract into an Erlenmeyer flask and add anhydrous ethanol at a ratio of 1g:10L for the first tobacco extract to the solvent. Heat in a water bath at 60°C for 1 hour, filter while hot to remove insoluble matter, collect the filtrate into a narrow-mouthed bottle, freeze, filter again to remove insoluble matter, concentrate under reduced pressure at 45°C until no liquid drips, and continue to concentrate under reduced pressure for 20 minutes to obtain the tobacco pure oil.
[0062] (3) The above-mentioned tobacco pure oil is subjected to steam distillation to obtain an organic fraction, which is neophytadiene.
[0063] Comparative Example 2 (1) The waste tobacco leaves are crushed and added to an ethanol aqueous solution at a ratio of 1g:10L of tobacco to solvent. The mixture is then refluxed at 80°C for extraction. The waste residue is then filtered off and the extract is concentrated to obtain the first tobacco extract.
[0064] (2)~(4) Same as Example 1.
[0065] The yield of the first tobacco extract obtained in step (1) (extract yield), the yield of the tobacco pure oil obtained in step (2) (pure oil yield), the K / S value of the dyed flavoring thread for cigarettes in step (2) (yarn K / S value), and the purity of the finally obtained neophytadiene were calculated in the above comparative example. The results are listed in Table 2: Table 2. Extract yield, net oil yield, yarn K / S value, and new phytadiene purity of Example 1 and Comparative Examples 1-2
[0066] The K / S curves of the cigarette dyeing threads prepared in step (2) of Example 1 and Comparative Example are shown below. Figure 6 As shown.
[0067] From Table 1, Table 2 and Figure 6 It can be known that: 1. The new phytadiene prepared in this embodiment has high purity, which is higher than 80.4% and 93.8% of Comparative Examples 1 and 2, respectively, and can reach 98.7%.
[0068] 2. In Comparative Example 1, the tobacco extract was not dyed and adsorbed using cotton fiber yarn, and the final purity of neophytadiene was significantly reduced, proving that the dyeing of cotton fiber yarn absorbed the polar substances in the tobacco extract, thereby increasing its purity.
[0069] 3. In Comparative Example 2, the waste tobacco leaves were not treated with plasma, and the extraction rate of the extract and the dyeing effect of the yarn were significantly reduced, proving that plasma can improve the extraction rate and the content of colored substances in the extract.
[0070] The various embodiments of the present invention have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principles, practical application, or improvement of the technology in the market, or to enable others skilled in the art to understand the embodiments disclosed herein.
Claims
1. A comprehensive treatment method for waste tobacco leaves, characterized in that, include: Step a) After crushing the waste tobacco leaves, they are subjected to plasma treatment to obtain pretreated waste tobacco leaf powder; Step b) The waste tobacco powder is refluxed and extracted using an aqueous ethanol solution, and the extract is concentrated to obtain a first tobacco extract; Step c) Dilute the first tobacco extract with water to obtain a diluted extract solution; immerse the cotton fiber yarn pretreated with metal salt mordant in the diluted extract solution for adsorption dyeing; after adsorption dyeing, obtain dyed fragrance thread for cigarettes; Collect the remaining diluted extract after adsorption and staining, and concentrate it to obtain the second tobacco extract; Step d) Using anhydrous ethanol as a solvent, the second tobacco extract is extracted with alcohol. After extraction, the extract is filtered and the filtrate is concentrated under reduced pressure to obtain tobacco pure oil. Step e) The tobacco purified oil is subjected to steam distillation to collect the organic fraction and obtain neophytadiene.
2. The comprehensive processing method according to claim 1, characterized in that, In step a), the plasma treatment power is 100~500W and the treatment time is 1~10min.
3. The comprehensive processing method according to claim 1, characterized in that, In step b), the mass-to-volume ratio of waste tobacco powder to ethanol aqueous solution is 1g:5~20L, and the extraction temperature is 75~85℃.
4. The comprehensive processing method according to claim 1, characterized in that, In step c), the cotton fiber yarn pretreated with the metal salt mordant is: cotton fiber yarn pre-impregnated with potassium aluminum sulfate solution.
5. The comprehensive processing method according to claim 1, characterized in that, In step c), the ratio of the first tobacco extract diluted with water is 1g:5~50L.
6. The comprehensive processing method according to claim 1, characterized in that, In step c), the staining adsorption temperature is 60~100℃ and the time is 0.5-2h.
7. The comprehensive processing method according to claim 1, characterized in that, In step d), the ratio of the second tobacco extract to anhydrous ethanol is 1g:5~20L.
8. The comprehensive processing method according to claim 1, characterized in that, In step d), the filtering specifically involves: Immediately after alcohol extraction, the first filtration was performed to obtain the intermediate filtrate. The intermediate filtrate is frozen and then subjected to a second filtration to obtain the filtrate.
9. The comprehensive processing method according to claim 1, characterized in that, In step d), the temperature for vacuum concentration is 40~50℃.
10. A type of dyed flavoring thread for cigarettes, characterized in that, It is prepared according to the method described in any one of claims 1-9.