Tobacco enzyme-deactivated cigarette manufacturing method capable of accurately regulating and controlling nicotine and tar content

Abstract

The invention discloses a tobacco enzyme-deactivated cigarette manufacturing method capable of accurately regulating and controlling nicotine and tar content, and belongs to the technical field of cigarette preparation. When the filter tip fiber is prepared, cellulose diacetate, polylactic acid and alkaline white carbon black are blended to prepare a spinning solution, and the cellulose diacetate / polylactic acid fiber is obtained through dry spinning. The binding force of the alkaline white carbon black and the fibers is destroyed through acetic acid, rich pores are formed in the fibers through ultrasonic treatment, the specific surface area is remarkably increased, nicotine, tar and other harmful substances are more effectively adsorbed, and harm of smoking to human health is reduced. 2, 9, 16, 23-tetraamino phthalocyanine and p-cyanobenzaldehyde are self-assembled on the pore surfaces of the fibers, so that the fibers contain active groups such as amino groups and cyano groups, and can generate specific interaction with nicotine and tar, which is different from the traditional physical adsorption, and the adsorption efficiency and selectivity of nicotine and tar are greatly improved. The raw materials such as the cellulose diacetate and the polylactic acid have biodegradability and have no pollution to the environment.

Description

Technical Field

[0001] The invention belongs to the technical field of cigarette preparation, and in particular relates to a method for preparing tobacco-killed cigarettes by accurately regulating the amounts of nicotine and tar. Background Art

[0002] Tobacco smoke is an extremely complex mixture, with more than 3,800 compounds. These compounds together form a special aerosol system, which is composed of volatile, semi-volatile and non-volatile compounds in the gas phase. The main reason why smokers become addicted to smoking is that they become dependent on nicotine. Nicotine is a natural alkaloid present in tobacco. It can quickly enter the blood circulation through the lungs and act on specific receptors in the brain, thereby stimulating the brain to release neurotransmitters such as dopamine, which makes people feel happy and satisfied. Tar is one of the main substances in cigarettes that harm human health and cause human cancer, and its harm should not be underestimated. Tar contains a large number of carcinogens, such as polycyclic aromatic hydrocarbons and nitrosamines. When smokers inhale cigarettes, tar will gradually deposit in the respiratory tract and lungs to form a layer of sticky substances. This layer of substance will not only irritate the respiratory mucosa, causing symptoms such as coughing and sputum, but long-term accumulation will also cause lesions in the respiratory mucosa and increase the risk of chronic obstructive pulmonary disease (COPD).

[0003] At present, cigarette filters are usually made of acetate fibers, and the common acetate fiber filters are not ideal for removing toxic compounds in smoke. In order to improve the removal efficiency, researchers often use other materials to replace acetate fibers, or add fillers to acetate fibers. The Chinese invention patent with publication number CN109156894A discloses a cigarette filter rod and a preparation method thereof. The application adopts an appropriate proportion of loofah and silk, and adopts a special preparation process to make full use of the adsorption characteristics of the two to prepare the filter rod, which has a significant filtering effect on harmful substances such as tar and nicotine in cigarettes. However, the adsorption in the application is only physical adsorption, which is not much improved compared to the adsorption effect of traditional filters. It can filter out sticky tar, but it cannot effectively remove nicotine. The Chinese invention patent with publication number CN104815630A discloses a method for preparing filter fibers that selectively adsorb benzopyrene and phenol. The application uses a graphene oxide aqueous solution or a mixed solution of graphene oxide and chitosan aqueous solution as a specific modification liquid, sprays the fiber, and other treatments are performed to prepare filter fibers treated with the modification liquid. The application makes the obtained filter fibers into cigarette filters, which can reduce the benzopyrene content in the smoke. However, the application involves other additives such as chitosan and the preparation process is cumbersome, and it cannot effectively reduce the amount of nicotine and tar. Therefore, in order to accurately control the amount of nicotine and tar in cigarettes, it is necessary to propose a new method for making cigarettes. Summary of the invention

[0004] In view of the above situation, in order to overcome the defects of the prior art, the present invention realizes precise control of the amount of nicotine and tar in cigarettes through an innovative tobacco fixing process and a unique filter fiber preparation method.

[0005] In order to achieve the above object, the following technical scheme is adopted: The present invention provides a method for making tobacco-killed cigarettes with precise control of nicotine and tar content, comprising the following steps:

[0006] S1, select freshly picked tobacco leaves, place the tobacco leaves in a tobacco fixing device, and use a steam fixing method to fix the tobacco leaves. After the fixing is completed, the tobacco leaves are quickly taken out, ventilated and air-dried, and then the dried tobacco leaves are shredded to obtain shredded tobacco;

[0007] S2, stirring and mixing the liquid and solid raw materials to form a spinning solution, wherein the liquid phase includes dichloromethane and acetone, and the solid phase includes diacetate cellulose, polylactic acid and alkaline white carbon black, filtering the spinning solution, and then heating it to 60° C. to perform dry spinning, soaking the collected fibers in a 20% by volume acetic acid solution for 4-8 hours, and then soaking them in deionized water for ultrasonic treatment for 2-4 hours, and then drying the obtained fibers in an oven at 60° C. for 12-18 hours to obtain diacetate cellulose / polylactic acid fibers;

[0008] S3, immersing the cellulose diacetate / polylactic acid fiber in methanol, adding 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to the methanol, adding glacial acetic acid after dissolution, and then heating to reflux reaction for 8-12 hours. After the reaction is completed, soaking the obtained fiber in deionized water for 2-4 hours, and drying it in an oven at 60° C. for 12-18 hours to obtain the filter fiber;

[0009] S4, filling the tobacco shreds into cigarette paper, rolling the cigarette into a cigarette, installing the prepared filter fiber on one end of the cigarette, and obtaining the cigarette.

[0010] Furthermore, the liquid phase comprises the following components in parts by weight: 50-60 parts of dichloromethane and 5-8 parts of acetone.

[0011] Furthermore, the solid phase comprises the following components in parts by weight: 40-60 parts of cellulose diacetate, 20-40 parts of polylactic acid and 5-12 parts of basic white carbon black.

[0012] Furthermore, the mass ratio of the liquid phase to the solid phase is 2:1.

[0013] Furthermore, during the spinning process of step S1, the distance between the spinneret and the collecting device is 1.5-2.0 m.

[0014] Furthermore, the draft ratio in the spinning process of step S1 is 1.5-2.0.

[0015] Furthermore, in step S2, the mass ratio of cellulose diacetate / polylactic acid fiber, methanol, 2,9,16,23-tetraaminophthalocyanine, p-cyanobenzaldehyde and glacial acetic acid is 10-20:50-80:1-4:2-5:5-10.

[0016] Furthermore, the steam temperature of the killing process is 100-120°C, and the killing time is 3-5 minutes.

[0017] Furthermore, the width of the shredded wire is 0.8-1.2 mm.

[0018] The beneficial effects of the present invention are:

[0019] (1) The present invention prepares a spinning solution by blending cellulose diacetate, polylactic acid and alkaline white carbon black, and obtains cellulose diacetate / polylactic acid fiber by dry spinning. When preparing the fiber, acetic acid destroys the binding force between alkaline white carbon black and the fiber, so that the alkaline white carbon black is more easily separated from the fiber by ultrasonic treatment during the subsequent soaking in deionized water, thereby leaving a rich pore structure inside the fiber, thereby significantly increasing the specific surface area of ​​the fiber. The filter fiber has more contact sites and can more effectively absorb harmful substances such as nicotine and tar, thereby reducing the content of harmful components inhaled by smokers and reducing the harm of smoking to human health;

[0020] (2) The present invention uses 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to self-assemble on the surface of the internal pores of cellulose diacetate / polylactic acid fibers, and the prepared filter fibers contain nitrogen-containing active groups such as amino and cyano groups. From the perspective of chemical structure, nicotine molecules contain nitrogen heterocyclic structures, and some polycyclic aromatic hydrocarbons in tar have certain electron cloud distribution characteristics. The amino groups on the filter fibers have lone pairs of electrons and can form hydrogen bonds with the nitrogen heterocyclic rings in the nicotine molecules, so that the nicotine molecules can be stably adsorbed on the fibers. The carbon atom in the cyanide group carries a partial positive charge, and the nitrogen atom carries a partial negative charge, which interacts with the electron cloud of polycyclic aromatic hydrocarbons in tar. Through specific interaction modes such as dipole-dipole force and π-π stacking, tar molecules can also be effectively adsorbed on the active sites of the fiber. Different from the traditional physical adsorption method, it can more accurately regulate the release of these two harmful substances in cigarettes, greatly improving the adsorption efficiency and selectivity of nicotine and tar, thereby significantly reducing the harmful components inhaled by smokers.

[0021] (3) The raw materials used in the present invention, such as cellulose diacetate and polylactic acid, have good biodegradability. Under the action of microorganisms, cellulose diacetate can be gradually decomposed into low molecular weight compounds and eventually absorbed by the environment. Polylactic acid is a typical biodegradable polymer material, and its degradation products are carbon dioxide and water, which are pollution-free to the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 A flow chart of a method for making tobacco-cured cigarettes with precise control of nicotine and tar content according to the present invention;

[0023] Figure 2 This is a diagram showing the effects of different filters on the nicotine content of cigarettes in a method for making tobacco-killed cigarettes that accurately controls the amount of nicotine and tar according to the present invention;

[0024] Figure 3 This is a diagram showing the effect of different filters on the tar content of cigarettes in a method for making tobacco-killed cigarettes for accurately controlling the amount of nicotine and tar according to the present invention;

[0025] Figure 4 Observation diagram of the cross-sectional microstructure of different filter tip fibers in a method for making a tobacco-killed cigarette for accurately controlling the amount of nicotine and tar of the present invention.

[0026] The accompanying drawings are used to provide further understanding of the present invention and constitute a part of the specification. They are used to explain the present invention together with the embodiments of the present invention and do not constitute a limitation of the present invention. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0028] Unless otherwise defined, all professional and scientific terms used herein have the same meanings as those familiar to those skilled in the art. In addition, any methods and materials similar or equivalent to those described herein may be applied to the present invention. The preferred implementation methods and materials described herein are for demonstration purposes only and are not intended to limit the content of this application.

[0029] The experimental methods in the following examples are conventional methods unless otherwise specified, and the experimental materials used in the following examples are purchased from commercial channels unless otherwise specified.

[0030] Example 1

[0031] A method for making a tobacco-killed cigarette with precise control of nicotine and tar content, comprising the following steps:

[0032] S1. Select freshly picked tobacco leaves, place the tobacco leaves in a tobacco-fixing device, and use a steam-fixing method to fix the leaves. The steam temperature is 120° C. and the fixing time is 5 min. After the fixing is completed, the tobacco leaves are quickly taken out and ventilated to dry. The dried tobacco leaves are then shredded. The shredded width is 1.2 mm to obtain shredded tobacco;

[0033] S2, stirring and mixing the liquid and solid raw materials to prepare a spinning solution, wherein the liquid phase includes 60 parts of dichloromethane and 8 parts of acetone; the solid phase includes 60 parts of diacetyl cellulose, 40 parts of polylactic acid and 12 parts of alkaline white carbon black, and the mass ratio of the liquid phase to the solid phase is 2:1. The spinning solution is filtered and then heated to 60°C for dry spinning. During the spinning process, the distance between the spinneret and the collecting device is 2.0m, and the draft ratio is 2.0. The collected fibers are immersed in an acetic acid solution with a volume fraction of 20% for 8 hours, and then immersed in deionized water for ultrasonic treatment for 4 hours, and then the obtained fibers are dried in an oven at 60°C for 18 hours to obtain diacetyl cellulose / polylactic acid fibers;

[0034] S3, immersing cellulose diacetate / polylactic acid fiber in methanol, adding 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to methanol in a mass ratio of cellulose diacetate / polylactic acid fiber: methanol: 2,9,16,23-tetraaminophthalocyanine: p-cyanobenzaldehyde: glacial acetic acid of 20:80:4:5:10, adding glacial acetic acid after dissolving, and then heating to reflux reaction for 12 hours. After the reaction is completed, soaking the obtained fiber in deionized water for 4 hours, and drying it in an oven at 60°C for 18 hours to obtain a filter fiber;

[0035] S4, filling tobacco shreds into cigarette paper, rolling into cigarette sticks, installing the prepared filter tip fiber at one end of the cigarette sticks, and obtaining cigarettes,

[0036] Example 2

[0037] A method for making a tobacco-killed cigarette with precise control of nicotine and tar content, comprising the following steps:

[0038] S1. Select freshly picked tobacco leaves, place the tobacco leaves in a tobacco-fixing device, and use a steam-fixing method to fix the leaves. The steam temperature is 100° C. and the fixing time is 3 min. After the fixing is completed, the tobacco leaves are quickly taken out and ventilated to dry. The dried tobacco leaves are then cut into shreds with a shred width of 0.8 mm to obtain shredded tobacco;

[0039] S2, stirring and mixing the liquid and solid raw materials to form a spinning solution, the liquid phase includes 50 parts of dichloromethane and 5 parts of acetone; the solid phase includes 40 parts of diacetyl cellulose, 20 parts of polylactic acid and 5 parts of alkaline white carbon black, the mass ratio of the liquid phase to the solid phase is 2:1, the spinning solution is filtered, and then heated to 60°C for dry spinning. During the spinning process, the distance between the spinneret and the collecting device is 1.5m, and the draft ratio is 1.5. The collected fibers are immersed in a 20% volume fraction acetic acid solution for 4 hours, and then immersed in deionized water for ultrasonic treatment for 2 hours, and then the obtained fibers are dried in an oven at 60°C for 12 hours to obtain diacetyl cellulose / polylactic acid fibers;

[0040] S3, immersing cellulose diacetate / polylactic acid fiber in methanol, adding 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to methanol in a mass ratio of cellulose diacetate / polylactic acid fiber: methanol: 2,9,16,23-tetraaminophthalocyanine: p-cyanobenzaldehyde: glacial acetic acid of 10:50:1:2:5, adding glacial acetic acid after dissolving, and then heating to reflux reaction for 8 hours. After the reaction is completed, soaking the obtained fiber in deionized water for 2 hours, and drying it in an oven at 60°C for 12 hours to obtain a filter fiber;

[0041] S4, filling tobacco shreds into cigarette paper, rolling into cigarette sticks, installing the prepared filter tip fiber at one end of the cigarette sticks, and obtaining cigarettes,

[0042] Example 3

[0043] A method for making a tobacco-killed cigarette with accurate control of nicotine and tar content, comprising the following steps:

[0044] S1. Select freshly picked tobacco leaves, place the tobacco leaves in a tobacco-fixing device, and use a steam-fixing method to fix the leaves. The steam temperature is 110° C. and the fixing time is 4 min. After the fixing is completed, the tobacco leaves are quickly taken out and ventilated to dry. The dried tobacco leaves are then shredded. The shredded width is 1.0 mm to obtain shredded tobacco;

[0045] S2, stirring and mixing the liquid and solid raw materials to prepare a spinning solution, wherein the liquid phase includes 55 parts of dichloromethane and 6.5 parts of acetone; the solid phase includes 50 parts of diacetyl cellulose, 30 parts of polylactic acid and 8.5 parts of alkaline white carbon black, and the mass ratio of the liquid phase to the solid phase is 2:1, the spinning solution is filtered, and then heated to 60°C for dry spinning. During the spinning process, the distance between the spinneret and the collecting device is 1.75m, and the draft ratio is 1.75. The collected fibers are immersed in a 20% by volume acetic acid solution for 6 hours, and then immersed in deionized water for ultrasonic treatment for 3 hours, and then the obtained fibers are dried in an oven at 60°C for 15 hours to obtain diacetyl cellulose / polylactic acid fibers;

[0046] S3, immersing cellulose diacetate / polylactic acid fiber in methanol, adding 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to methanol according to the mass ratio of cellulose diacetate / polylactic acid fiber: methanol: 2,9,16,23-tetraaminophthalocyanine: p-cyanobenzaldehyde: glacial acetic acid of 15:65:2.5:3.5:7.5, adding glacial acetic acid after dissolving, and then heating to reflux reaction for 10 hours. After the reaction is completed, soaking the obtained fiber in deionized water for 3 hours, and drying it in an oven at 60°C for 15 hours to obtain filter fiber;

[0047] S4, filling tobacco shreds into cigarette paper, rolling into cigarette sticks, installing the prepared filter tip fiber at one end of the cigarette sticks, and obtaining cigarettes,

[0048] Comparative Example 1

[0049] The difference between this comparative example and Example 3 is that no basic white carbon black is added during the preparation process, and the rest is the same as Example 3.

[0050] Comparative Example 2

[0051] The difference between this comparative example and Example 3 is that cellulose diacetate / polylactic acid fiber is used instead of filter fiber, and the rest is the same as Example 3.

[0052] Comparative Example 3

[0053] The difference between this comparative example and Example 3 is that diacetyl cellulose is used instead of the filter fiber, and the rest is the same as Example 3.

[0054] Results Analysis

[0055] Test Example 1

[0056] Effects of different filters on the nicotine and tar content of cigarettes

[0057] The cigarettes prepared in different embodiments and comparative examples were put into a Bowat-Kathy RM200A smoking machine and burned. The nicotine content and tar content in the filter of each cigarette were tested. The results are shown in Table 1. Figure 2 and Figure 3 .

[0058] from Figure 2 and Figure 3It can be seen that Examples 1-3 have a good adsorption effect on tar and nicotine in cigarettes, and can effectively regulate the amount of nicotine and tar in cigarettes. The cigarette filter fibers prepared in Examples 1-3 form a rich pore structure through a series of unique processes during their preparation. This structure greatly increases the specific surface area of ​​the fiber, so that the filter fiber has more sites for contact with nicotine molecules. More importantly, the filter fiber contains nitrogen-containing active groups such as amino and cyano groups. From the perspective of chemical structure, the nicotine molecule contains a nitrogen heterocyclic structure, and the amino group on the filter fiber has a lone pair of electrons. The two can form hydrogen bonds to stably adsorb nicotine molecules on the fiber surface. This adsorption mechanism is not a simple physical adsorption, but a specific interaction based on the chemical structure, which effectively reduces the nicotine content in cigarettes, significantly reduces the amount of nicotine inhaled by smokers, and plays a certain protective role in the health of smokers. Similarly, Examples 1-3 also show good adsorption capacity for tar in cigarettes. The cyanide group on the filter fiber has a special electronic structure, in which the carbon atom carries a partial positive charge and the nitrogen atom carries a partial negative charge. Some polycyclic aromatic hydrocarbons in tar have certain electron cloud distribution characteristics. Based on this, the cyanide group and the polycyclic aromatic hydrocarbons in the tar can interact with each other through specific interactions such as dipole-dipole forces and π-π stacking, so that the tar molecules are effectively adsorbed on the active sites of the fiber. Compared with the physical adsorption method of traditional filters, this adsorption has higher selectivity and adsorption efficiency, and can accurately capture tar molecules, thereby reducing the tar content in cigarettes, reducing the deposition of tar in the smoker's respiratory tract and lungs, and reducing health risks such as chronic obstructive pulmonary disease (COPD) caused by tar accumulation.

[0059] Test Example 2

[0060] Observation of cross-sectional microstructure of different filter fibers

[0061] The cross sections of the filter fibers of Example 3 and Comparative Examples 1-3 were observed using a VHX-5000 ultra-depth 3D digital fiber microscope. Figure 4 .

[0062] Example 3 presents a better porous structure. When preparing the fiber in Example 3, acetic acid is used to destroy the binding force between the alkaline white carbon black and the fiber during the fiber preparation process of Example 3, so that in the subsequent deionized water soaking process, the alkaline white carbon black is more easily separated from the inside of the fiber through ultrasonic treatment. As the alkaline white carbon black is separated, a large number of rich and regular pore structures are left inside the fiber. The existence of these pore structures not only provides more adsorption space for nicotine and tar molecules, but also further increases the specific surface area of ​​the fiber, and enhances the interaction between the fiber and the nicotine and tar molecules.

[0063] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

[0064] The present invention and its implementation methods are described above, which is not restrictive. The drawings are only one of the implementation methods of the present invention, and the actual application is not limited thereto. In short, if ordinary technicians in the field are inspired by it and design methods and embodiments similar to the technical solution without creativity without departing from the purpose of the invention, they should all fall within the protection scope of the present invention.

Claims

1. A method for making tobacco-cured cigarettes with accurate control of nicotine and tar content, characterized in that: The following steps are involved: S1, select freshly picked tobacco leaves, place the tobacco leaves in a tobacco fixing device, and use a steam fixing method to fix the tobacco leaves. After the fixing is completed, the tobacco leaves are quickly taken out, ventilated and air-dried, and then the dried tobacco leaves are shredded to obtain shredded tobacco; S2, stirring and mixing the liquid and solid raw materials to form a spinning solution, wherein the liquid phase includes dichloromethane and acetone, and the solid phase includes diacetate cellulose, polylactic acid and alkaline white carbon black, filtering the spinning solution, and then heating it to 60° C. to perform dry spinning, soaking the collected fibers in a 20% by volume acetic acid solution for 4-8 hours, and then soaking them in deionized water for 2-4 hours, and then drying the obtained fibers in an oven at 60° C. for 12-18 hours to obtain diacetate cellulose / polylactic acid fibers; S3, immersing the cellulose diacetate / polylactic acid fiber in methanol, adding 2,9,16,23-tetraaminophthalocyanine and p-cyanobenzaldehyde to the methanol, adding glacial acetic acid after dissolution, and then heating to reflux reaction for 8-12 hours. After the reaction is completed, soaking the obtained fiber in deionized water for 2-4 hours, and drying it in an oven at 60° C. for 12-18 hours to obtain the filter fiber; S4, filling tobacco shreds into cigarette paper, rolling the cigarette into a cigarette, installing the prepared filter fiber on one end of the cigarette, and obtaining the cigarette.

2. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 1, characterized in that: The liquid phase comprises the following components in parts by weight: 50-60 parts of dichloromethane and 5-8 parts of acetone.

3. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 2, characterized in that: The solid phase comprises the following components in parts by weight: 40-60 parts of cellulose diacetate, 20-40 parts of polylactic acid and 5-12 parts of basic white carbon black.

4. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 3, characterized in that: The mass ratio of the liquid phase to the solid phase is 2:

1.

5. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 4, characterized in that: During the spinning process of step S1, the distance between the spinneret and the collecting device is 1.5-2.0 m.

6. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 5, characterized in that: The draft ratio during the spinning process of step S1 is 1.5-2.

0.

7. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 6, characterized in that: In the step S2, the mass ratio of cellulose diacetate / polylactic acid fiber, methanol, 2,9,16,23-tetraaminophthalocyanine, p-cyanobenzaldehyde and glacial acetic acid is 10-20:50-80:1-4:2-5:5-10.

8. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 7, characterized in that: The steam temperature of the killing process is 100-120° C., and the killing time is 3-5 minutes.

9. The method for making tobacco-cured cigarettes with accurate control of nicotine and tar content according to claim 8, characterized in that: The width of the shredded wire is 0.8-1.2 mm.

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