Method for extracting nicotine-free tar from cigarette butts

Abstract

The invention discloses a method for extracting nicotine-free tar from cigarette butts, which is applied to the field of cigarette butt recovery and comprises the following steps of: adding the cigarette butts into a 30L extraction kettle with a compression device, adding 6.32 kg of cigarette butts in total, adding ethanol, heating and extracting at 78 DEG C for three times, extracting for two hours at each time and 50.0 kg of ethanol in total, and concentrating an ethanol extracting solution to obtain 700.0 g of nicotine-containing tar with the extraction rate of 11% (in terms of cigarette butts). The method comprises the following steps: taking 429.9 g of nicotine-containing tar, adding 750ml of dichloromethane and 330ml of 1 equivalent diluted hydrochloric acid into the tar, stirring overnight at room temperature, adding dichloromethane into the solution, washing with water, and drying with anhydrous sodium sulfate to obtain 190.8 g of a nicotine-free tar product with the yield of 44.4% (metered by tar). According to the method, a feasible way is provided for recycling the effective components in the cigarette butts, after process parameters are further optimized, higher recycling efficiency and better economic benefits are achieved, meanwhile, pollution of the cigarette butts to the environment is reduced, and environmental protection is facilitated.

Description

Technical Field

[0001] The invention relates to the field of cigarette butt recycling, and in particular to a method for extracting nicotine-free tar from cigarette butts. Background Art

[0002] my country has a large number of smokers, which can generate a large number of discarded cigarette butts. Discarded cigarette butts are not only easy to cause fires, but also cause waste of resources and pollution to the environment.

[0003] Therefore, it is of great significance to reasonably recycle cigarette butts. At present, there is relatively little research and industrial development in this field. The purpose of the present invention is to provide a method for extracting nicotine-free tar from cigarette butts for secondary utilization. Summary of the invention

[0004] In order to overcome the above problems, the present invention aims to provide a method for extracting nicotine-free tar from cigarette butts, with the aim of solving the problem that there are relatively few research and industrial development in this field.

[0005] To this end, the specific technical solution adopted by the present invention is as follows:

[0006] According to one aspect of the present invention, there is provided a method for extracting nicotine-free tar from cigarette butts, the method comprising the following steps:

[0007] S1. Take cigarette butts and add them into a 30L extraction kettle with a compression device, add a total of 6.32kg of cigarette butts, add ethanol and heat at 78°C for extraction three times, each extraction takes two hours, a total of 50.0kg of ethanol is required, and the ethanol extract is concentrated to obtain 700.0g of nicotine tar, with an extraction rate of 11% (based on cigarette butts);

[0008] S2. Take 429.9 g of nicotine-containing tar, add 750 ml of dichloromethane and 330 ml of 1 equivalent dilute hydrochloric acid to the tar, stir at room temperature overnight, add dichloromethane to the solution, wash with water, and dry over anhydrous sodium sulfate to obtain 190.8 g of nicotine-free tar product with a yield of 44.4% (based on tar).

[0009] Optionally, S1 includes the following sub-steps:

[0010] S11. Before adding cigarette butts to the extraction kettle, pre-treat the cigarette butts. First, use a screening device to remove impurities in the cigarette butts, including dust, pebbles and other non-tobacco-related foreign matter. These impurities may affect the dissolution efficiency of ethanol on nicotine tar in the subsequent extraction process, and may remain in the extraction kettle, affecting the service life of the equipment. Therefore, removing them is more conducive to the extraction effect.

[0011] S12, crushing the screened cigarette butts using a crushing device to crush the cigarette butts into particles of uniform size, with a particle size controlled at 2-5 mm. Compared with intact cigarette butts, the crushed cigarette butts can significantly increase the contact area with ethanol, thereby improving the dissolution rate and extraction efficiency of nicotine tar;

[0012] S13. Before adding the ethanol to the extraction kettle, the ethanol is subjected to ultrasonic treatment. The ultrasonic frequency is set to 30-50kHz and the treatment time is 15-30 minutes. The ultrasonic treatment can make the ethanol molecules more active, destroy the tiny agglomeration structures that may exist inside them, and enhance the solubility of ethanol. At the same time, this pretreatment can also remove the trace amount of air that may be contained in the ethanol and reduce the impact of oxidation on nicotine tar;

[0013] S14. During the extraction process at 78°C, the pressure in the extraction kettle is precisely controlled. In the first 30 minutes of each extraction, the pressure is maintained at 1.2-1.5 standard atmospheres, and then the pressure is gradually reduced to normal pressure in the remaining 1.5 hours, so that ethanol can better penetrate into the cigarette butt particles to obtain ethanol extract. The coordinated control of temperature and pressure can further improve the extraction efficiency of nicotine tar. Moreover, during the extraction process, the concentration change of nicotine tar is monitored in real time by a new sensor installed in the extraction kettle. The sensor is based on advanced spectral analysis technology and can accurately and quickly feedback the extraction process, so as to fine-tune the extraction time and conditions according to actual conditions;

[0014] S15. After the extraction is completed, the ethanol extract is transferred to a special separation device. Using the principles of centrifugal force and density difference, under the condition of high-speed rotation, the macromolecular impurities and possible residual solid particles in the extract are quickly settled to the bottom to achieve preliminary purification, and the purified ethanol extract is obtained. The purified ethanol extract is then heated and concentrated.

[0015] Optionally, in S15, the ethanol vapor generated during the concentration process is recovered by a condensation recovery system, and the ethanol vapor is recovered and reused in the next extraction process, which greatly reduces the consumption of ethanol and improves the economy and environmental protection of the entire process.

[0016] Optionally, S2 includes the following sub-steps:

[0017] S21, adding 429.9 g of nicotine-containing tar to a clean and dry reaction container, then slowly adding 750 ml of dichloromethane, then adding 330 ml of 1 equivalent dilute hydrochloric acid to the reaction container, turning on a stirring device, setting the stirring speed to 300-500 rpm, stirring overnight to react, ensuring that the tar, dichloromethane and dilute hydrochloric acid are fully and evenly mixed to avoid uneven local reaction;

[0018] S22. After the reaction is completed, an appropriate amount of dichloromethane is added to the solution again, and then a water washing operation is performed. The water washing is performed in multiple times, and the amount of water used each time is 1.2 times the volume of the solution. The first water washing is intended to remove most of the water-soluble impurities and excess dilute hydrochloric acid. The subsequent water washing further improves the impurity removal efficiency. During the water washing process, the stirring speed is controlled at 100-200rpm to prevent emulsification.

[0019] S23. After washing, anhydrous sodium sulfate was slowly added to the solution according to the volume of the solution, and the mixture was stirred for 30-45 minutes to allow the solution to fully absorb water. The anhydrous sodium sulfate was then filtered out through a filter to obtain a dried solution, and finally 190.8 g of a nicotine-free tar product was obtained.

[0020] Optionally, in S21, the reaction container is equipped with a temperature control system to maintain the temperature at room temperature, and the temperature fluctuation is controlled within ±1°C, and a shading device is arranged around the container.

[0021] Optionally, in S23, anhydrous sodium sulfate is slowly added to the solution at a ratio of 10-15 g of anhydrous sodium sulfate per 100 ml of solution, depending on the volume of the solution.

[0022] Optionally, the ethanol is anhydrous ethanol or any one of 70-95% ethanol. In S2, in addition to dichloromethane, dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate may be added to the solution. The acid includes any one or more of an organic acid and an inorganic acid, wherein the organic acid includes dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate. The acid includes any one of an organic acid and an inorganic acid, wherein the inorganic acid includes any one of hydrochloric acid, sulfuric acid, and phosphoric acid.

[0023] Compared with the prior art, this application has the following beneficial effects:

[0024] 1. This method provides a feasible way to recycle the active ingredients in cigarette butts. After further optimizing the process parameters, it can achieve higher recycling efficiency and better economic benefits, while reducing the pollution of cigarette butts to the environment, which is beneficial to environmental protection;

[0025] 2. The pretreatment of cigarette butts was optimized by adding a screening device to remove impurities and using a crushing device to crush the cigarette butts to increase the contact area. Then, the ethanol in the extraction process was pretreated by using ultrasonic treatment to enhance solubility and remove air;

[0026] 3. Use the condensation recovery system to recycle ethanol vapor, reduce consumption and improve economy and environmental protection. These optimization measures are aimed at increasing the nicotine tar extraction rate and enhancing the innovation, environmental protection and economy of the process. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The above characteristics, features and advantages of the present invention and their implementation methods and methods will become more clearly understood in conjunction with the following description of the embodiments, which are described in detail in conjunction with the accompanying drawings. Herein, a schematic diagram is shown:

[0028] Figure 1 The present invention is a flowchart of a method for extracting nicotine-free tar from cigarette butts according to an embodiment of the present invention. DETAILED DESCRIPTION

[0029] In order to enable those skilled in the art to better understand the solution of the present application, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0030] According to an embodiment of the present invention, a method for extracting nicotine-free tar from cigarette butts is provided.

[0031] Embodiment 1

[0032] The present invention is further described with reference to the accompanying drawings and specific embodiments. Figure 1 As shown, according to one embodiment of the present invention, a method for extracting nicotine-free tar from cigarette butts is provided, the method comprising the following steps:

[0033] S1. Take cigarette butts and add them into a 30L extraction kettle with a compression device, add a total of 6.32kg of cigarette butts, add ethanol and heat to 78°C for extraction three times, each extraction takes two hours, a total of 50.0kg of ethanol is required, and the ethanol extract is concentrated to obtain 700.0g of nicotine tar, with an extraction rate of 11% (based on cigarette butts). The specific process is as follows:

[0034] S11. Before adding cigarette butts to the extraction kettle, pre-treat the cigarette butts. First, use a screening device to remove impurities in the cigarette butts, including dust, pebbles and other non-tobacco-related foreign matter. These impurities may affect the dissolution efficiency of ethanol on nicotine tar in the subsequent extraction process, and may remain in the extraction kettle, affecting the service life of the equipment. Therefore, removing them is more conducive to the extraction effect.

[0035] S12, crushing the screened cigarette butts using a crushing device to crush the cigarette butts into particles of uniform size, with a particle size controlled at 2-5 mm. Compared with intact cigarette butts, the crushed cigarette butts can significantly increase the contact area with ethanol, thereby improving the dissolution rate and extraction efficiency of nicotine tar;

[0036] S13. Before adding the ethanol to the extraction kettle, the ethanol is subjected to ultrasonic treatment. The ultrasonic frequency is set to 30-50kHz and the treatment time is 15-30 minutes. The ultrasonic treatment can make the ethanol molecules more active, destroy the tiny agglomeration structures that may exist inside them, and enhance the solubility of ethanol. At the same time, this pretreatment can also remove the trace amount of air that may be contained in the ethanol and reduce the impact of oxidation on nicotine tar;

[0037] S14. During the extraction process at 78°C, the pressure in the extraction kettle is precisely controlled. In the first 30 minutes of each extraction, the pressure is maintained at 1.2-1.5 standard atmospheres, and then the pressure is gradually reduced to normal pressure in the remaining 1.5 hours, so that ethanol can better penetrate into the cigarette butt particles to obtain ethanol extract. The coordinated control of temperature and pressure can further improve the extraction efficiency of nicotine tar. Moreover, during the extraction process, the concentration change of nicotine tar is monitored in real time by a new sensor installed in the extraction kettle. The sensor is based on advanced spectral analysis technology and can accurately and quickly feedback the extraction process, so as to fine-tune the extraction time and conditions according to actual conditions;

[0038] S15. After the extraction is completed, the ethanol extract is transferred to a special separation device. The principles of centrifugal force and density difference are used to make the macromolecular impurities and possible residual solid particles in the extract quickly settle to the bottom under high-speed rotation to achieve preliminary purification and obtain the purified ethanol extract. The purified ethanol extract is then heated and concentrated. The ethanol vapor generated during the concentration process is recovered by a condensation recovery system and the recovered ethanol vapor is reused in the next extraction process, which greatly reduces the consumption of ethanol and improves the economy and environmental protection of the entire process.

[0039] S2, take 429.9g of nicotine-containing tar, add 750ml of dichloromethane and 330ml of 1 equivalent dilute hydrochloric acid to the tar, stir at room temperature overnight, add dichloromethane to the solution, wash with water, dry over anhydrous sodium sulfate, and obtain 190.8g of nicotine-free tar product, with a yield of 44.4% (based on tar), the specific process is as follows:

[0040] S21, adding 429.9 g of nicotine-containing tar to a clean and dry reaction container, then slowly adding 750 ml of dichloromethane, and then adding 330 ml of 1 equivalent dilute hydrochloric acid to the reaction container, the reaction container is equipped with a temperature control system, the temperature is maintained at room temperature, and the temperature fluctuation is controlled within ±1°C, and a shading device is set around the container, and a stirring device is turned on, the stirring speed is set to 300-500 rpm, and the reaction is stirred overnight to ensure that the tar, dichloromethane and dilute hydrochloric acid are fully and evenly mixed to avoid local uneven reaction;

[0041] S22. After the reaction is completed, an appropriate amount of dichloromethane is added to the solution again, and then a water washing operation is performed. The water washing is performed in multiple times, and the amount of water used each time is 1.2 times the volume of the solution. The first water washing is intended to remove most of the water-soluble impurities and excess dilute hydrochloric acid. The subsequent water washing further improves the impurity removal efficiency. During the water washing process, the stirring speed is controlled at 100-200rpm to prevent emulsification.

[0042] S23. After washing, anhydrous sodium sulfate is slowly added to the solution at a ratio of 10-15 g of anhydrous sodium sulfate per 100 ml of solution according to the volume of the solution, and stirring is continued for 30-45 minutes to allow the solution to fully absorb water. The anhydrous sodium sulfate is then filtered out through a filtering device to obtain a dried solution, and finally 190.8 g of a nicotine-free tar product is obtained.

[0043] The ethanol is any one of anhydrous ethanol or 70-95% ethanol. In S2, in addition to dichloromethane, dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate can also be added to the solution. The acid includes any one or more of organic acids and inorganic acids, wherein the organic acid includes dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate. The acid includes any one of organic acids and inorganic acids, and the inorganic acid includes any one of hydrochloric acid, sulfuric acid, and phosphoric acid.

[0044] Comparative Example

[0045] 3.16 kg of cigarette butts were added into a 30 L extraction kettle, and ethanol was added to heat and extract at 78 ° C for three times, each time for two hours, a total of 46.9 kg of ethanol was required, and the ethanol extract was concentrated to obtain 333.5 g of nicotine tar, with an extraction rate of 10.5% (based on cigarette butts).

[0046] Embodiment 2

[0047] To remove nicotine from tar, 40.4 g of tar was added with 150 ml of ethyl acetate, and the mixture was heated and stirred at 40°C. A dihydrated oxalic acid solution (15.7 g, dissolved in 50 ml of ethyl acetate) was added to the tar solution. The reaction solution was filtered, and the filtrate was washed with water and dried over anhydrous sodium sulfate. After concentration, 12.65 g of tar without nicotine was obtained, with a yield of 31.3% (based on tar).

[0048] It can be seen from the experimental results of the embodiments and comparative examples that in the process of recovering nicotine-free tar from cigarette butts, the amount of cigarette butts used, the amount of extraction solvent used, and the method of removing nicotine will all have an impact on the final recovery effect. The present method provides a feasible way for the recovery and utilization of effective ingredients in cigarette butts. After further optimizing the process parameters, higher recovery efficiency and better economic benefits can be achieved, while reducing the pollution of cigarette butts to the environment.

[0049] Although the present invention has been disclosed as above with preferred embodiments, the embodiments are merely examples for the convenience of description and are not intended to limit the present invention. Those skilled in the art may make several changes and modifications without departing from the spirit and scope of the present invention. The scope of protection claimed by the present invention shall be based on the claims.

Claims

1. A method for extracting nicotine-free tar from cigarette butts, characterized in that: The method comprises the following steps: S1: adding cigarette butts into an extraction kettle, compressing, adding ethanol, heating and extracting to obtain an extract, and concentrating the extract to obtain nicotine tar; S2. Adding an organic solvent to the nicotine-containing tar to dissolve it, washing with dilute acid to remove the nicotine, and concentrating to obtain nicotine-free tar.

2. The method for extracting nicotine-free tar from cigarette butts according to claim 1, characterized in that: The S1 comprises the following sub-steps: S11. Take cigarette butts and add them into a 30L extraction kettle with a compression device, add a total of 6.32kg of cigarette butts, add ethanol and heat at 78°C for extraction three times, each extraction takes two hours, a total of 50.0kg of ethanol is required, and the ethanol extract is concentrated to obtain 700.0g of nicotine tar, with an extraction rate of 11% (based on cigarette butts). S12, before adding the cigarette butts to the extraction kettle, pre-treat the cigarette butts. First, use a screening device to remove impurities in the cigarette butts, including dust, pebbles and other non-tobacco related foreign matter; S13, crushing the screened cigarette butts using a crushing device to crush the cigarette butts into particles of uniform size, with a particle size controlled at 2-5 mm; S14, before adding to the extraction kettle, subjecting the ethanol to ultrasonic treatment. The ultrasonic frequency is set to 30-50kHz, and the treatment time is 15-30 minutes; S15. During the extraction process at 78° C., the pressure in the extraction kettle is precisely controlled. During the first 30 minutes of each extraction, the pressure is maintained at 1.2-1.5 standard atmospheres, and then the pressure is gradually reduced to normal pressure during the remaining 1.5 hours, so that ethanol can better penetrate into the cigarette butt particles to obtain an ethanol extract. S16. After the extraction is completed, the ethanol extract is transferred to a special separation device. Using the principles of centrifugal force and density difference, under the condition of high-speed rotation, the macromolecular impurities and possible residual solid particles in the extract are quickly settled to the bottom to achieve preliminary purification, and the purified ethanol extract is obtained. The purified ethanol extract is then heated and concentrated.

3. The method for extracting nicotine-free tar from cigarette butts according to claim 2, characterized in that: In S16, the ethanol vapor generated during the concentration process is recovered by a condensation recovery system, and the recovered ethanol vapor is reused in the next extraction process.

4. The method for extracting nicotine-free tar from cigarette butts according to claim 1, characterized in that: The S2 comprises the following sub-steps: S21, take 429.9g of nicotine-containing tar, add 750ml of dichloromethane and 330ml of 1 equivalent dilute hydrochloric acid to the tar, stir at room temperature overnight, add dichloromethane to the solution, wash with water, dry with anhydrous sodium sulfate, and obtain 190.8g of nicotine-free tar product, with a yield of 44.4% (based on tar) S22, adding 429.9 g of nicotine tar to a clean and dry reaction container, then slowly adding 750 ml of dichloromethane, then adding 330 ml of 1 equivalent dilute hydrochloric acid to the reaction container, turning on a stirring device, setting the stirring speed to 300-500 rpm, stirring overnight to react; S23, after the reaction is completed, an appropriate amount of dichloromethane is added to the solution again, and then a water washing operation is performed, the water washing is performed in multiple times, and the amount of water used each time is 1.2 times the volume of the solution. The first water washing is intended to remove most of the water-soluble impurities and excess dilute hydrochloric acid, and the subsequent water washing further improves the impurity removal efficiency; S24. After washing, anhydrous sodium sulfate is slowly added to the solution according to the volume of the solution, and stirring is continued for 30-45 minutes to allow it to fully absorb water. The anhydrous sodium sulfate is then filtered out through a filtering device to obtain a dried solution, and finally 190.8 g of a nicotine-free tar product is obtained.

5. The method for extracting nicotine-free tar from cigarette butts according to claim 4, characterized in that: In S22, the reaction container is equipped with a temperature control system to maintain the temperature at room temperature, and the temperature fluctuation is controlled within ±1°C, and a shading device is set around the container.

6. The method for extracting nicotine-free tar from cigarette butts according to claim 4, characterized in that: In S24, anhydrous sodium sulfate is slowly added to the solution at a ratio of 10-15 g of anhydrous sodium sulfate per 100 ml of solution, depending on the volume of the solution.

7. The method for extracting nicotine-free tar from cigarette butts according to claim 1, characterized in that: The ethanol is any one of anhydrous ethanol or 70-95% ethanol. In S2, in addition to dichloromethane, dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate can also be added to the solution. The acid includes any one or more of organic acids and inorganic acids, wherein the organic acid includes dichloroethane, ethyl acetate, isopropyl acetate, and butyl acetate. The acid includes any one of organic acids and inorganic acids, and the inorganic acid includes any one of hydrochloric acid, sulfuric acid, and phosphoric acid.

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