Preparation method of composite paper filter tip and application of composite paper filter tip in reducing nitrosamine in smoke

Abstract

The invention discloses a preparation method of a composite paper filter tip, which comprises the following steps: (1) ultrasonically extracting stem barks of air-cured tobaccos with hot water, and then carrying out solid-liquid separation; (2) performing solid-liquid separation and pulping to obtain bark pulp, and preparing a substrate by adopting a method for preparing reconstituted tobacco by a papermaking method; (3) preparing a coating liquid by using the stem bark paste; (4) spraying the coating liquid on a substrate, then spraying by using a polyvinyl alcohol solution, then coating by using the zeolite composite material, and finally spraying by using the polyvinyl alcohol solution; (5) obtaining a paper filter tip; and (6) compounding to obtain the composite paper filter tip. According to the composite paper filter tip, the sensory quality of cigarettes can be obviously improved, and particularly, the content of nitrosamine in the smoke of the cigarettes can be obviously reduced.

Description

Technical Field

[0001] The present invention relates to a cigarette material, in particular to a preparation method of a composite paper mouthpiece and an application thereof in reducing nitrosamines in smoke. Background Art

[0002] In the modern tobacco industry, mouthpieces, as a crucial component of cigarettes, not only filter out harmful substances but also play a key role in improving the taste and aroma of cigarettes. As consumers' demands for a more comfortable smoking experience and increased health and safety continue to rise, optimizing mouthpiece design to achieve the dual goals of enhancing flavor and reducing harm has become a key research topic in tobacco research.

[0003] During the tobacco processing process, a large amount of scraps and discarded tobacco leaves are generated, especially the residues generated in the initial processing stage of sun-cured tobacco (such as burley tobacco, oriental tobacco, etc.), which are often regarded as low-value-added products or directly discarded, resulting in waste of resources and environmental pollution. However, these wastes still contain rich plant fibers, aromatic compounds and some aroma active ingredients, and have high reuse value. Using the sun-cured tobacco waste after proper treatment for the preparation of composite paper mouthpieces can not only achieve efficient utilization of agricultural waste, but also help reduce production costs and promote the green and sustainable development of the tobacco industry.

[0004] Tobacco smoke contains a variety of chemicals harmful to the human body, among which nitrosamines (TSNAs) are a class of potent carcinogens. Research shows that TSNAs are primarily generated by the conversion of nitrogen compounds in tobacco raw materials during combustion. Therefore, effectively reducing the formation and release of nitrosamines in tobacco smoke is a key issue in improving cigarette safety.

[0005] Compared to acetate and polypropylene filter rods, paper filter rods are highly biodegradable and cost-effective. At the same filtration pressure drop, they are more efficient at intercepting tar and harmful components in smoke. Suitable particulate aroma carriers can also be added to the recycled tobacco filter rod substrate, or flavors and fragrances can be coated on the substrate surface to improve draw quality and smoke characteristics.

[0006] However, the sheet base of conventional reconstituted tobacco leaf mouthpieces is made of tobacco pulp and stem pulp as the main materials. Since the fibers in the pulp are short, low in strength, and have a high content of fine components, the sheet base obtained by papermaking has poor strength and suffers from serious powder and hair loss.

[0007] The present invention is proposed for this purpose. Summary of the Invention

[0008] In order to solve the above problems, the application discloses a method for preparing a reconstituted tobacco leaf composite filter stick by taking tobacco stem bark as the main material. Since the strength and toughness of the tobacco stem bark are much higher than those of tobacco leaves and tobacco stems, the problem of poor base strength of conventional reconstituted tobacco leaves can be effectively solved. Meanwhile, by loading the adsorbent material with high specific surface area, the waste of air-cured tobacco can be effectively utilized, and the effects of increasing tobacco aroma and reducing nitrosamines can be achieved.

[0009] Unless otherwise specified, the percentages used in the present application are all weight percentages.

[0010] The object of the present application is achieved by the following technical solutions.

[0011] The first aspect of the present application discloses a preparation method of a composite paper nozzle stick, comprising the following steps:

[0012] (1) hot water ultrasonic extraction is performed on the stem bark of air-cured tobacco, and then solid-liquid separation is performed; the raw material is a local characteristic Yunnan sun-cured tobacco stem bark; the collection method is as follows: after the tobacco leaves are picked, the stem bark is torn off from the root incision and naturally dried in a ventilated place;

[0013] (2) the solid part of the solid-liquid separation is pulped to obtain stem bark pulp, and a base sheet is prepared by using the method of preparing reconstituted tobacco leaves by papermaking;

[0014] (3) the liquid part of the solid-liquid separation is concentrated to obtain stem bark paste, and a coating liquid is prepared by using the stem bark paste;

[0015] (4) the coating liquid obtained in step (3) is sprayed on the base sheet obtained in step (2), then polyvinyl alcohol solution is sprayed, then zeolite composite material is coated, and finally polyvinyl alcohol solution is sprayed again;

[0016] (5) after the base sheet after spraying and coating is dried, it is directly wound, wrapped with filter stick forming paper, and cut to the required length; that is, a paper nozzle stick is obtained;

[0017] (6) the obtained paper nozzle stick is compounded with an acetate fiber filter stick; and the paper nozzle stick is obtained.

[0018] Preferably, the hot water ultrasonic extraction step of step (1) is as follows: the naturally dried and cut into 0.5-3.0 cm long stem bark of air-cured tobacco is rehydrated to 13-18% moisture content, naturally fermented at 35-45℃ for 20-30 days, and then ultrasonically extracted in hot water at 50-90℃ for 40-90min; the mass ratio of the stem bark to the hot water is 1:(3-5).

[0019] Preferably, the solid part of the solid-liquid separation in step (2) is 50-200 mesh, and the preparation of the bast pulp is as follows: mixing the fire grass fiber, waste cotton, polyglycerol, polyglycerol fatty acid ester, modified polylactic acid fiber, sodium carboxymethyl cellulose, cationic starch, solid part and water, and then performing defibration and beating, the beating degree being 15-50°SR, to obtain the bast pulp; the obtained bast pulp is used to make the base sheet by the method of reconstituting tobacco leaf by papermaking, so that the thickness of the base sheet is 100-200 g / m 2 ; the mass percentage ratio of each component in the bast pulp is as follows: fire grass fiber 1-2wt%, waste cotton 5-10wt%, polyglycerol 0.5-2wt%, polyglycerol fatty acid ester 0.2-1wt%, modified polylactic acid fiber 2-5wt%, sodium carboxymethyl cellulose 0.5-2wt%, and cationic starch 0.5-1wt%; water is added in a solid-liquid mass ratio of 1:(5-10).

[0020] Preferably, the preparation method of the coating solution in step (3) is as follows: uniformly mixing the alcohol precipitated bast paste, sun-cured tobacco high nicotine extract, biological calcium carbonate, xanthan gum, polyglycerol stearate, glycerol and ethanol solution to obtain the coating solution; the mass percentage of each component in the coating solution is as follows: alcohol precipitated bast paste 10-20wt%, sun-cured tobacco high nicotine extract 5-8wt%, biological calcium carbonate 5-8wt%, xanthan gum 0.5-2.0wt%, polyglycerol stearate 0.1-5wt%, glycerol 3-5wt%, and the rest is an ethanol solution, which is an aqueous solution containing 30-50wt% ethanol.

[0021] Preferably, the content of the polyvinyl alcohol solution used in step (4) is 10-30wt%, and the molecular weight of the polyvinyl alcohol is 5000-50000.

[0022] Preferably, the preparation method of the zeolite composite material used in step (4) is as follows: selecting a zeolite with a specific surface area of not less than 400m 2 / g and a particle size of more than 40 mesh, soaking it in a polylysine compound solution with a content of 0.5-3.0wt% for 1-2 days; after soaking, drying to obtain the zeolite composite material; the polylysine compound is a mixture of one or more of poly-L-lysine, poly-S-lysine or poly-meso-lysine, and the molecular weight is 5000-30000.

[0023] Preferably, the spraying amount of the coating solution in step (4) is 15-20% of the dry weight of the sheet base; the first spraying amount of the polyvinyl alcohol solution is 10-20% of the dry weight of the sheet base; the coating amount of the zeolite composite material is 30-100% of the dry weight of the sheet base; the second spraying amount of the polyvinyl alcohol solution is 10-20% of the dry weight of the sheet base.

[0024] Preferably, the step (6) paper nozzle stick and acetate fiber filter rod are compounded on a compound nozzle stick forming machine to be compounded and rolled; the length of the paper nozzle stick is 5-15 mm, the length of the acetate fiber filter rod is 15-25 mm, and then cut into 25 mm or 30 mm filter rods; that is, the compound paper nozzle stick.

[0025] The second aspect of the present application discloses the use of the compound paper nozzle stick prepared by the preparation method for reducing nitrosamine in smoke.

[0026] The beneficial effects of the present application are:

[0027] 1. The raw material used in the preparation method of the paper nozzle stick is full plant fiber, which is a waste of local characteristic tobacco, and can effectively solve the problem of recycling of tobacco stems after air-dried tobacco is harvested, the raw material cost is low, and there is a wide supply source.

[0028] 2. The pulp compound formula involved in the preparation method of the paper nozzle stick can fully consider the aspects of enhancing the strength of the base sheet and solving the conventional base sheet problems, improve the water resistance of the paper through the synergistic effect of the air-dried tobacco stem skin fiber and other auxiliary materials, solve the problems of poor strength, powder and hair loss, improve the utilization rate of raw materials and reduce the production cost, and improve the paper machine speed and output.

[0029] 3. The preparation method of the paper nozzle stick is simple, can be prepared by using existing equipment, the production process is simple, the pulp and the extraction liquid can be fully used, and the applicability of green production is obvious.

[0030] 4. The coating liquid formula involved in the preparation method of the paper nozzle stick not only fully considers the preservation and production strength demand of the base sheet, but also greatly meets the demand of the base sheet for quality improvement and fragrance enhancement, and can be effectively applied to the production and processing of subsequent cigarette products.

[0031] 5. The compound paper nozzle stick obtained by the present application can significantly improve the sensory quality of cigarettes, and has obvious effects in increasing the richness of cigarette aroma, reducing irritation, and masking woodiness. In particular, it can significantly reduce the content of nitrosamine in cigarette smoke. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 Schematic diagram of the reconstituted tobacco leaf obtained in Example 1.

[0033] Figure 2 Schematic diagram of the zeolite used in Example 1.

[0034] Figure 3 Schematic diagram of the reconstituted tobacco leaf coated with zeolite in Example 1.

[0035] Figure 4 Schematic diagram of the paper nozzle stick of the reconstituted tobacco leaf in Example 1.

[0036] Figure 5 A schematic diagram of the composite paper tip stick structure is obtained in Example 1.

[0037] Figure 6 Polylysine and 4-N-nitrosomethylamino-1-(3-pyridyl)butanone (NNK) molecular docking simulation results. DETAILED DESCRIPTION

[0038] The present application will be described with respect to the following examples, but the embodiments of the present application are not limited thereto. Unless otherwise indicated, the experimental methods in the examples were carried out according to conventional conditions and conditions described in manuals, or using general equipment, materials, reagents, etc. recommended by manufacturers, and are commercially available.

[0039] Example 1: Preparation of a composite paper tip stick, the steps are as follows:

[0040] Step 1: Raw material collection and processing

[0041] Shaihong tobacco stem bark collection: After the tobacco leaves are harvested, use a knife to cut the tobacco stem from the root, carefully tear off the stem bark, and place it in a well-ventilated place for natural drying. This is the starting material for the entire preparation process.

[0042] Reconstituted tobacco leaf paper base sheet production: Dry the stem bark after drying and re-moisturize it to a moisture content of 15%. Then, use plastic film to seal the stem bark and place it in an environment with a temperature of 40°C for natural fermentation. The fermentation time is controlled to be 20 days.

[0043] Step 2: Stem bark pulp production

[0044] Cut the fermented stem bark into 2 cm long pieces and put them into an ultrasonic extraction tank. Add hot water at a temperature of 60°C according to 3 times the weight of the raw material, and perform 2 times of ultrasonic extraction, each time for 50 min. After extraction, perform solid-liquid separation, and the solid part is used for pulp production and screening. Collect the tobacco stem bark pulp between 80 meshes during screening for subsequent sheet making; the extract (liquid phase) is concentrated for use in the preparation of tobacco paste for coating process.

[0045] Step 3: Pulp compounding

[0046] Fire grass fiber, waste cotton, polyglycerol, polyglycerol fatty acid ester, modified polylactic acid fiber, sodium carboxymethyl cellulose, cationic starch, solid part and water are mixed, and the mixed pulp is defibrated and beaten by a refiner to control the final beating degree at 45-50°SR; the compounding ratio of the pulp (calculated by dry weight) is: fire grass fiber 1%, waste cotton 5%, polyglycerol fatty acid ester 0.5%, modified polylactic acid fiber 3%, sodium carboxymethyl cellulose 1%, cationic starch 0.6%; the balance is the solid part; water is added at a material-to-liquid mass ratio of 1:7.

[0047] Step four, sheet making

[0048] The prepared mixed pulp is made into a base sheet by using the method of papermaking to reconstruct tobacco leaves, and the thickness of the base sheet is set to 120 g / m 2 . The obtained reconstructed tobacco leaves are as shown in Figure 1 .

[0049] Step five, coating liquid preparation:

[0050] The coating material is prepared according to the following formula: alcohol precipitation (sugar, pectin and protein are removed by ethanol precipitation) cortex paste 15%, sun-cured tobacco high nicotine extract 6%, biological calcium carbonate 6%, xanthan gum 1%, polyglyceryl stearate 3%, glycerol 3%, and the balance is 40% (v / v) ethanol.

[0051] Step six, zeolite composite material preparation

[0052] A zeolite with a specific surface area of 450 m 2 / g and a particle size of 50 mesh is selected, and is soaked in a poly-L-lysine solution with a content of 1%. The molecular weight of poly-L-lysine is 10000. After soaking is completed, the zeolite is taken out and dried. The obtained zeolite is as shown in Figure 2 .

[0053] Step seven, coating and coating

[0054] The prepared coating liquid is sprayed on the base sheet, and the spraying amount of the coating liquid is controlled to be 16% of the dry weight of the base sheet; after coating is completed, the first spraying amount of polyvinyl alcohol solution is 15% of the dry weight of the base sheet; the coating amount of the zeolite composite material is 50% of the dry weight of the base sheet; and the second spraying amount of polyvinyl alcohol solution is 15% of the dry weight of the base sheet. The content of the polyvinyl alcohol solution is 20wt%, and the molecular weight of the polyvinyl alcohol is 20000. Figure 3 The schematic diagram of the reconstructed tobacco leaves coated with zeolite.

[0055] Step eight, paper filter rod forming

[0056] After the spraying and coating are completed, drying is performed, and then a winding operation is directly performed, and finally a filter rod forming paper is wrapped, and is cut to a required length, and thus a paper tip rod is obtained. A schematic diagram of the obtained reconstituted tobacco paper tip rod is shown in Figure 4 .

[0057] Step nine, paper tip rod compounding and tipping

[0058] The paper tip rod is compounded on a compound tip rod forming machine, wherein the length of the paper tip rod is set to 15 mm, and the length of the acetate filter rod is set to 15 mm. Then, according to actual requirements of a cigarette product, the compound paper tip rod is cut into a filter rod with a length of 30 mm, and is tipped to a cigarette, and finally a cigarette product with a compound paper filter rod is obtained. The obtained compound paper tip rod and a structural diagram thereof are shown in Figure 5 .

[0059] Comparative Example 1

[0060] The reconstituted tobacco obtained in steps one to four is the reconstituted tobacco of Example 1; the cured tobacco waste in Example 1 is replaced by common tobacco stems and tobacco leaves (with a mass ratio of 3:1), and the reconstituted tobacco of Comparative Example 1 is prepared according to steps one to four of Example 1; the reconstituted tobacco of Comparative Example 2 with a conventional gram weight of 120 g / m 2 The tensile strength of the reconstituted tobacco of Comparative Example 2 is detected according to the standard of YC / T 16-2014 Reconstituted Tobacco, and the results are shown in Table 1.

[0061] Table 1: Tensile strength data of reconstituted tobacco

[0062] ID Tensile strength kN / m Tensile strength kN / m Control 1 Reconstituted Tobacco Leaf 0.17±0.04 0.46±0.08 Control 2 Reconstituted Tobacco Leaf 0.21±0.03 0.49±0.05 Example 1 Reconstituted Tobacco Leaf 0.25±0.04 0.56±0.06

[0063] As shown in Table 1, the tensile strength of the reconstituted tobacco obtained by the method of the present application is obviously improved.

[0064] Comparative Example 2

[0065] The reconstituted tobacco of Comparative Example 1 and the reconstituted tobacco of Comparative Example 2 are compounded into compound paper tip rods according to step nine of Example 1, and the reconstituted tobacco of Comparative Example 3 is prepared into a compound paper tip rod by using only zeolite instead of a zeolite composite material, and other steps are completely consistent, and then is added to a cigarette to prepare a cigarette, and is subjected to sensory evaluation according to YC / T 138-1998 Sensory Evaluation Method for Tobacco and Tobacco Products, and the results are shown in Table 2.

[0066] Table 2: Sensory evaluation data

[0067] ID Gloss Aroma Harmony Strangeness Irritation Aftertaste Total Example 1 Composite Tipped Rod 5 35 5 15 15 16 91 Control 3 Composite Tipped Rod 5 33 4 15 15 15 87 Control 1 Composite Tipped Rod 5 32 4.5 13.5 13 14 82 Control 2 Composite Tipped Rod 5 31.5 4 14 14 14 82.5

[0068] As shown in the sensory results in Table 2, the compound paper tip rod obtained by the preparation method of the present application can significantly improve the scores of aroma and aftertaste, and other scores are also improved, and the overall score is obviously increased. The tip rod coated only with zeolite does not have obvious improvement in aroma and aftertaste.

[0069] The detection of smoke nitrosamines was carried out according to the standard "ISO 19290:2021 Determination of tobacco-specific nitrosamines in mainstream smoke of cigarettes - LC-MS / MS method", and the results are shown in Table 3.

[0070] Table 3 Nitrosamine data ng / cig

[0071] ID NNN NNK NAT NAB Total Example 1 Composite Tipped Rod 2.07 3.80 0.31 0.15 6.33 Control 3 Composite Tipped Rod 3.18 6.77 1.08 0.22 11.25 Control 1 Composite Tipped Rod 4.32 9.63 1.39 0.43 15.77 Control 2 Composite Tipped Rod 4.45 9.36 1.57 0.53 15.91

[0072] As shown by the nitrosamine results in Table 3, the composite paper tip rod prepared by the preparation method of the present application can significantly reduce the content of smoke nitrosamines. In order to verify the nitrosamine adsorption capacity of poly-L lysine, molecular docking was used to simulate the interaction between tobacco nitrosamine and lysine, and the results are shown in Table 4. Figure 6 The binding energy is -16.35 kJ / mol, indicating good adsorption effect.

[0073] The above is only one of the embodiments of the present application, which is described in more detail and in detail, but it cannot be interpreted as a limitation on the scope of the present application. It should be noted that for ordinary skilled persons in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, which are all within the scope of the present application. Therefore, the protection scope of the present application should be subject to the appended claims.

Claims

1. A method of making a composite paper tip stick, characterized by, The method comprises the following steps: (1) hot water ultrasonic extraction is performed on the stems of air-cured tobacco, and then solid-liquid separation is performed; (2) the solid part obtained through the solid-liquid separation is pulped to obtain stem pulp, and a base sheet is prepared by using a papermaking method; (3) the liquid part obtained through the solid-liquid separation is concentrated to obtain stem paste, and a coating solution is prepared by using the stem paste; (4) the coating solution obtained in step (3) is sprayed on the base sheet obtained in step (2), then polyvinyl alcohol solution is sprayed, then zeolite composite material is coated, and finally polyvinyl alcohol solution is sprayed again; (5) after drying, the base sheet after spraying and coating is directly wound, wrapped with filter rod forming paper, and cut to a desired length; namely, a paper tip rod is obtained; (6) the paper tip rod is combined with an acetate fiber filter rod; and a combined paper tip rod is obtained.

2. The production method according to claim 1, characterized by, In step (1), the hot water ultrasonic extraction is performed as follows: the stems of air-cured tobacco, which are naturally dried and cut into 0.5-3.0 cm long, are rehydrated to have a moisture content of 13-18%, naturally fermented at 35-45°C for 20-30 days, and then ultrasonically extracted in hot water at 50-90°C for 40-90 min; the mass ratio of the stems to the hot water is 1:(3-5).

3. The production method according to claim 1, characterized by, In step (2), the solid part obtained through the solid-liquid separation is 50-200 mesh, and the preparation of the stem pulp is performed as follows: fire grass fibers, waste cotton, polyglycerol, polyglycerol fatty acid ester, modified polylactic acid fibers, sodium carboxymethyl cellulose, cationic starch, the solid part and water are mixed, and then defibrated and pulped to obtain the stem pulp, wherein the beating degree is 15-50°SR; The obtained bast pulp is used to prepare base sheet by papermaking method to prepare reconstituted tobacco leaf, so that the thickness of the base sheet is 100-200 g / m 2 ; the mass percentage ratio of each component in the bast pulp is as follows: 1-2 wt% of fire grass fiber, 5-10 wt% of waste cotton, 0.5-2 wt% of polyglycerol, 0.2-1 wt% of polyglycerol fatty acid ester, 2-5 wt% of modified polylactic acid fiber, 0.5-2 wt% of sodium carboxymethyl cellulose, 0.5-1 wt% of cationic starch, and the balance is a solid part; water is added at a material-to-liquid mass ratio of 1:(5-10).

4. The method of claim 1, wherein, In step (3), the preparation method of the coating solution is as follows: the stem paste after alcohol precipitation, air-cured tobacco high nicotine extract, biological calcium carbonate, xanthan gum, polyglycerol stearate, glycerol and ethanol solution are uniformly mixed to obtain the coating solution; the mass percentage of each component in the coating solution is as follows: the stem paste after alcohol precipitation is 10-20 wt%; the air-cured tobacco high nicotine extract is 5-8 wt%; the biological calcium carbonate is 5-8 wt%; the xanthan gum is 0.5-2.0 wt%; the polyglycerol stearate is 0.1-5 wt%; the glycerol is 3-5 wt%; and the rest is an ethanol solution, which is an aqueous solution containing 30-50% (v / v) ethanol.

5. The preparation method according to claim 1, characterized in that In step (4), the content of the polyvinyl alcohol solution used is 10-30 wt%, and the molecular weight of the polyvinyl alcohol is 5000-50000.

6. The method of claim 1, wherein, The zeolite composite used in step (4) is prepared by the following steps: selecting a zeolite with a specific surface area of not less than 400 m 2 / g and a particle size of greater than 40 mesh, immersing it in a solution of a polylysine compound at a content of 0.5-3.0 wt% for 1-2 days; after the immersion is complete, removing and drying, to obtain the zeolite composite; the polylysine compound is a mixture of one or more of poly-L-lysine, poly-S-lysine, or poly-meso-lysine, with a molecular weight of 5000-30000.

7. The preparation method according to claim 1, characterized in that In step (4), the spraying amount of the coating solution is 15-20% of the dry weight of the base sheet; the spraying amount of the polyvinyl alcohol solution for the first time is 10-20% of the dry weight of the base sheet; the coating amount of the zeolite composite material is 30-100% of the dry weight of the base sheet; and the spraying amount of the polyvinyl alcohol solution for the second time is 10-20% of the dry weight of the base sheet.

8. The preparation method according to claim 1, characterized in that In step (6), the combination of the paper tip rod and the acetate fiber filter rod is performed on a combined tip rod forming machine; the length of the paper tip rod is 5-15 mm, the length of the acetate fiber filter rod is 15-25 mm, and then the filter rods with a length of 25 mm or 30 mm are cut; namely, the combined paper tip rod is obtained.

9. The use of the combined paper tip rod prepared by the preparation method of claim 8 for reducing nitrosamines in smoke.

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