Cigarette paper additive, tipping paper and preparation method thereof

Abstract

The present application discloses a method for preparing a cigarette paper additive, comprising the following steps: 1) extracting ground wood lignin in a cigarette rod using a 1,4-dioxane-water solution; 2) mixing ground wood lignin with silk fibroin, treating with a composite enzyme, and obtaining a lignin-silk fibroin complex, which is an additive. The present application also provides a cigarette paper additive. The present application also provides a plugging paper using the above-mentioned cigarette paper additive and a method for preparing the same. The method provided in the present application is reasonable and easy to operate. The cigarette paper additive prepared in the present application can be added as a filler during the production of the plugging paper, and has the aroma of tobacco, antibacterial properties, and the like, and can greatly enhance the experience and antibacterial properties of cigarettes when smoking.

Description

Technical Field

[0001] The present application relates to the technical field of tobacco preparation, and in particular to a cigarette paper additive, tipping paper and a preparation method thereof. Background Art

[0002] Cigarette tipping paper is a special paper used to connect filter rods to cigarettes, and is one of the essential cigarette packaging materials. Traditional cigarette tipping paper has no flavor, and the taste is monotonous on the lips, which cannot adapt to and meet the requirements of various consumer groups. Domestic and foreign studies have shown that adding various flavors or mixed flavors of various styles to tipping paper, tipping paper with different tastes can directly contact the tongue and lips of the human body, while not changing the taste of cigarettes, to improve the feeling of the mouth and lips, reduce chapped lips, enrich the taste of cigarettes, and increase the pleasure of smoking. Therefore, tipping paper with different flavors has gradually become popular and has become a research hotspot in recent years.

[0003] As the part that comes into direct contact with the lips of consumers, the antibacterial properties of tipping paper have also attracted attention. Traditional tipping paper is made directly from plant fibers, which have poor antibacterial properties, and synthetic antibacterial agents have certain safety risks. Compared with synthetic antibacterial agents, natural antibacterial agents are safer and more environmentally friendly, and have received great attention. Summary of the invention

[0004] In order to solve the above technical problems, the first purpose of the present invention is to provide a method for preparing a cigarette paper additive; the second purpose of the present invention is to provide a cigarette paper additive prepared by the above method; the third purpose of the present invention is to provide a tipping paper; the fourth purpose of the present invention is to provide a method for preparing tipping paper. The method provided in this application is reasonable and easy to operate. The cigarette paper additive prepared in this application can be added as a filler during the production of tipping paper, has the aroma of tobacco, antibacterial properties, etc., and can greatly improve the experience of smoking cigarettes and antibacterial properties.

[0005] The technical solution provided by the present invention is as follows:

[0006] A method for preparing a cigarette paper additive comprises the following steps:

[0007] 1) Using 1,4-dioxane-water solution to extract ground wood lignin from tobacco stems;

[0008] 2) The ground wood lignin and silk fibroin are mixed and treated with a composite enzyme to obtain a lignin-silk fibroin complex, which is the additive.

[0009] Preferably, step 1) is specifically: extracting the tobacco stem powder in a 1,4-dioxane-water solution for 22-24 hours, repeating 2-3 times, and separating to obtain a crude extract;

[0010] The crude extract was treated with acetic acid-water mixture, dimethyl sulfoxide and anhydrous ether in sequence to obtain purified groundwood lignin.

[0011] Preferably, the method further comprises the step of secondary purification of the purified ground wood lignin using acetic acid-water mixture, acetone, acetic acid-acetone mixture, anhydrous ether and petroleum ether in sequence.

[0012] Preferably, before the 1,4-dioxane-water solution, a pretreatment step is also included: crushing the tobacco stems to 200-250 mesh, then using benzene-methanol solution for extraction for 48-52 hours, solid-liquid separation, drying the solid to obtain powder, and grinding to 40-60 mesh for use.

[0013] Preferably, step 1) is specifically:

[0014] The pretreated tobacco stem powder is extracted in a 1,4-dioxane-water solution for 22-24 hours, and the extraction is repeated 2-3 times. The resulting precipitate is centrifuged as a crude extract;

[0015] The crude extract is extracted with an acetic acid-water mixture for 22-24 hours, and the process is repeated 2-3 times. The solution obtained by centrifugation is concentrated and dried, and then extracted with dimethyl sulfoxide. The solution obtained by centrifugation is dripped into anhydrous ether, centrifuged, and the obtained precipitate is dried, and then dissolved with an acetic acid-water mixture. The dissolved solution is dripped into acetone, centrifuged, and the obtained precipitate is dried, washed with an acetic acid-acetone mixture containing 1-1.5% acetic acid by mass, and then washed with anhydrous ether for 2-3 times, and then washed with petroleum ether, and dried to obtain ground wood lignin;

[0016] Wherein, the volume ratio of acetic acid to water in the acetic acid-water mixture is (1-1.5):1.

[0017] Preferably, in the 1,4-dioxane-water solution, the volume ratio of 1,4-dioxane to water is (94-96):(4-6).

[0018] Preferably, the complex enzyme used in step 2) is β-glucosidase and laccase.

[0019] Preferably, the dosage of β-glucosidase is 500-600U, and the dosage of laccase is 1600-1700U.

[0020] Preferably, step 2) specifically comprises: centrifuging the silk fibroin, taking the supernatant, and diluting it for later use;

[0021] Dissolve the ground wood lignin in a buffer solution, heat it to 60-65°C, keep it warm for 10-15 minutes, then cool it to 25-27°C, then add the silk fibroin solution, β-glucosidase and laccase at 30-32°C, mix well, react for 4-6 hours, and terminate the reaction by heating; centrifuge, and dry the resulting precipitate to obtain the lignin-silk fibroin complex.

[0022] Preferably, the mass ratio of groundwood lignin to silk fibroin is (3-4):1.

[0023] Preferably, the centrifugal rotation speed is 9000-10000 r / min.

[0024] Preferably, the ground wood lignin is mixed with the silk fibroin solution, β-glucosidase and laccase, reacted for 4-6 hours under the condition of continuous blowing of sterile air, and then heated to 60-65°C to terminate the reaction; centrifuged, and the obtained precipitate is dried at 60-65°C to obtain the lignin-silk fibroin complex.

[0025] A cigarette paper additive prepared by any of the preparation methods described above.

[0026] A tipping paper, added with the above-mentioned cigarette paper additive.

[0027] The method for preparing the tipping paper comprises the following steps:

[0028] The coniferous wood and the hardwood are mixed in a mass ratio of 6:4, and pulped by a sulfite method. A cigarette paper additive is added during pulping, and papermaking is performed to obtain tipping paper.

[0029] Preferably, the coniferous wood is spruce and the hardwood wood is poplar.

[0030] Natural antibacterial agents can be mainly divided into rhubarb anthraquinones, organic acids, polyphenols, flavonoids, proteins (peptides), polysaccharides, and aldehydes and ketones in some spices. Most antibacterial drugs with plants as the main raw materials mainly include phenolic compounds, terpenes and alkaloids. Lignin is a natural high-molecular compound that contains a large number of phenolic compounds. These structures determine that lignin has an antibacterial effect. Lignin metabolism is related to plant disease resistance. When plants are infected by pathogens or need to produce induced resistance, the lignin content increases. In the interaction with pathogens, the lignification of the cell wall at the infected part of the plant is one of the characteristics of the disease resistance response. As an important physical antibacterial substance in plants, lignin strengthens the cell wall and protects cells from infection by pathogens.

[0031] The present invention first provides a preparation method of a cigarette paper additive, comprising the following steps: 1) extracting ground wood lignin in a cigarette rod using a 1,4-dioxane-water solution; 2) mixing the ground wood lignin and silk fibroin, and treating them with a composite enzyme to obtain a lignin-silk fibroin complex, which is the additive. The method provided by the present application is reasonable and simple to operate. The cigarette paper additive prepared by the present application can be added as a filler during the production of tipping paper. The ground wood lignin prepared from the cigarette rod in the filler can improve the taste of the cigarette when it is smoked; at the same time, because the ground wood lignin has an antibacterial effect, the tipping paper can be made to have an antibacterial effect, and the cigarette can have a longer shelf life. When cigarettes are prepared using the tipping paper added with the above-mentioned additive, bacteria in the oral cavity can be removed at the same time during smoking, thereby achieving the effect of protecting the oral cavity. The lignin-silk fibroin complex prepared by the present invention has the characteristics of tobacco flavor, antibacterial and the like, and can greatly improve the experience and antibacterial properties of cigarettes when they are smoked.

[0032] The lignin-silk fibroin complex is prepared by grafting ground wood lignin and silk fibroin under the action of enzymes and self-assembling silk fibroin. Since the lignin-silk fibroin complex has both hydrophilic polysaccharide segments and hydrophobic lignin segments that can provide strength, using it as a filler can make the plugging paper have good mechanical strength and adjust the water absorption performance, improve the problem of poor mechanical strength and easy water absorption of the plugging paper, reduce the water absorption rate of the plugging paper and improve water resistance, and will not have an adverse effect on the taste of the cigarette when smoking. At the same time, since the lignin-silk fibroin complex can cause active oxygen-induced oxidative stress response in bacterial cells, the pH value in the bacterial cells is reduced, and the ATP in the bacterial cells is consumed, it has a good antibacterial effect.

[0033] In addition, as people's environmental awareness gradually increases, the utilization of waste materials such as cigarette stems can not only reduce environmental pressure and reduce the cost of waste treatment, but also give the filling paper antibacterial properties.

[0034] Tobacco is a plant of the genus Nicotiana in the Solanaceae family, an annual or limited perennial herb. Tobacco stems refer to agricultural waste left after tobacco leaves are harvested, which belongs to the category of biomass. The main components are lignin, cellulose, sugar, oil, etc.

[0035] Preferably, the method further comprises a pretreatment step of crushing the tobacco stem to 200-250 meshes, then extracting with a benzene-methanol solution for 48-52 hours, separating the solid from the liquid, drying the solid to obtain a powder, and grinding the powder to 40-60 meshes for use. The extraction with a benzene-methanol solution can remove impurities such as pectin and tannin in the tobacco stem.

[0036] The present application also provides a method for preparing the above-mentioned plugging paper, comprising the following steps: mixing coniferous wood and hardwood in a mass ratio of 6:4, pulping by the sulfite method, adding a cigarette paper additive during pulping, and making paper to obtain plugging paper. When pulping by the sulfite method, the raw materials and the sulfite cooking liquid are added to the cooking pot, and the first stage of heating is carried out. At this time, indirect heating is used to avoid diluting the liquid. In order to avoid overpressure, continuous small air release should be performed, and a small insulation should be performed when the temperature is raised to the critical temperature; then the second stage of heating is performed, and the temperature is kept at the highest temperature; when approaching the end of the cooking, a large air release is performed, and finally the pulp is washed. The pulp prepared by the sulfite method is added with the prepared tobacco stem lignin-silk protein complex during pulping, and then papermaking is performed to obtain this plugging paper with antibacterial function.

[0037] Preferably, the coniferous wood used is spruce, and the broadleaf wood is poplar. Spruce wood is close to white, and has very good whiteness when used as the main fiber raw material, so that the obtained pulp is easier to bleach, and the amount of bleaching agent used in the subsequent bleaching can be reduced, the damage to the fiber can be reduced, and the pollution to the environment is small. Adding a certain amount of broadleaf wood raw material can increase the hemicellulose content in the raw material and adjust the water absorption performance of the finished paper. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0039] Figure 1 The results of the antibacterial experiment in the embodiment of the present invention are shown in the following figure; DETAILED DESCRIPTION

[0040] In order to enable those skilled in the art to better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0041] It should be noted that when an element is referred to as being "fixed on" or "set on" another element, it can be directly on the other element or indirectly set on the other element; when an element is referred to as being "connected to" another element, it can be directly connected to the other element or indirectly connected to the other element.

[0042] It should be understood that the terms "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0043] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, "multiple" and "several" mean two or more, unless otherwise clearly and specifically defined.

[0044] It should be noted that the structures, proportions, sizes, etc. illustrated in the drawings of this specification are only used to match the contents disclosed in the specification for people familiar with this technology to understand and read, and are not used to limit the conditions under which this application can be implemented. Therefore, they have no substantive technical significance. Any structural modification, change in proportional relationship or adjustment of size should still fall within the scope of the technical content disclosed in this application without affecting the effects and purposes that can be achieved by this application.

[0045] Example 1

[0046] (1) Pretreatment of tobacco stem raw materials

[0047] First, the tobacco stem raw material is chopped, and then ground into a powder of about 200 mesh in a pulverizer, and then extracted with a benzene-methanol solution for 48 hours, solid-liquid separation, and the solid is dried to obtain a powder, which is then ground with a vibration ball mill for 72 hours to 40 mesh before use.

[0048] (2) Extraction of lignin from ground tobacco stems

[0049] The tobacco stem powder was reacted in 400 mL of 1,4-dioxane-water solution (volume ratio 96:4) on a heat-collecting constant temperature heating magnetic stirrer (DF-101S) for 24 h, for a total of three times. Then centrifuge using a high-speed centrifuge (SIGMA, 4-16K); extract the precipitate after centrifugation with 400 mL of acetic acid-water mixture (volume ratio 1:1) for 24 hours, three times in total; the solution obtained after centrifugation is rotary evaporated by a rotary evaporator (IKA, RV-10), and the concentrated solution after rotary evaporation is vacuum dried in a vacuum drying oven, and then extracted with 75 mL of dimethyl sulfoxide (DMSO) and centrifuged at high speed; the solution obtained after centrifugation is added dropwise to 1000 mL of anhydrous ether, centrifuged again, and the precipitate obtained after centrifugation is vacuum dried, dissolved with acetic acid-water mixture (volume ratio 1:1), and the dissolved solution is added dropwise to 400 mL of acetone; the precipitate obtained by centrifugation is vacuum dried, washed once with acetone containing 1% acetic acid (mass fraction), then washed twice with anhydrous ether, and finally washed once with low boiling point (boiling range 30-50°C) petroleum ether, and finally vacuum dried to obtain the ground wood lignin of tobacco stems.

[0050] (3) Preparation of lignin-silk fibroin complex

[0051] The silk fibroin was centrifuged at 9000r / min, the supernatant was taken and diluted to 100mg / mL with deionized water. 3g of ground wood lignin was weighed and dissolved in 100mL of PBS solution, heated to 60℃ in a water bath, kept warm for 10min and cooled to 25℃, the reaction device was immersed in a 30℃ water bath, 10mL of 100mg / mL silk fibroin solution, 500U β-glucosidase and 1600U laccase were added, mixed evenly, sterile air was continuously blown in, and the reaction was continued for 4h. The solution gradually became turbid without precipitation. Distilled water was added and placed in a 60℃ water bath to terminate the reaction. The above solution was centrifuged at 9000r / min, and the precipitate after centrifugation was dried at 60℃ to obtain a lignin-silk fibroin complex.

[0052] (3) Preparation of antibacterial tipping paper

[0053] A mixed raw material of spruce and poplar (6:4) was selected to make pulp by the sulfite method. The prepared lignin-silk fibroin complex was added as a filler to the tipping paper for papermaking to obtain the tipping paper with antibacterial function.

[0054] Antibacterial test

[0055] (1) Prepare LB (beef extract peptone) solution

[0056] Tryptone 10 g / L; NaCl 10 g / L; Yeast 5 g / L; pH=7.0-7.4

[0057] (2) Sample preparation

[0058] The antibacterial tipping paper and ordinary tipping paper prepared in Example 1 were respectively made into circular samples with a diameter of 6 mm.

[0059] (3) Sterilization operation

[0060] Wrap the culture dish, cut filter paper, applicator, deionized water (put in a conical flask), LB solution, and LB solution with 2% agar (20 g / L) (100 ml in each conical flask) in newspaper, place in an autoclave, and sterilize at 121°C for 45 minutes.

[0061] (4) Activation of E. coli

[0062] Take 100 μL of the frozen Escherichia coli and put it in 5 mL of LB culture medium. Place the culture solution on a shaker at 37°C and 200 r / min. Take it out after 12 hours. Then take 100 μL of the above culture solution and put it in 5 ml of LB culture medium. Place the culture solution on a shaker at 37°C and 200 r / min. Take it out after 2-3 hours.

[0063] (5) Measure OD value

[0064] Take 1 mL of the cultured bacterial solution, centrifuge at 8000 r / min for 5 min, pour off the supernatant and add 3 mL of water, stir evenly and measure the absorbance of the bacterial solution at 600 nm in a UV spectrophotometer, then dilute the bacterial solution (with sterile water) to 5~5*106 cfu / mL (1 OD=1*109 cfu / mL)

[0065] (6) Experimental steps

[0066] Place the above disinfected instruments and samples on a sterile workbench and irradiate with ultraviolet light for 30 min. Then pour the LB solution into the culture dish, about 30 mL each, and then let it stand for 15 min until the agar solidifies. Take 200 μL of the diluted bacterial solution into the culture dish, rotate the culture dish to evenly distribute the bacterial solution on the surface, let it stand for about 15 min, and stick the sample on the surface of the culture medium, 4 pieces per dish (3 pieces of antibacterial tipping paper samples (labeled A, B, C respectively) and 1 piece of ordinary tipping paper control sample (labeled D)). Cover the culture dish with a lid, seal it with a sealing film, and place it in an incubator at 37.5℃. After 7 hours, observe and measure the diameter of the antibacterial zone around the filter paper and keep a record.

[0067] like Figure 1 As shown, the average inhibition zone diameter of the three antibacterial tipping papers is 14.36 mm.

[0068] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a cigarette paper additive, characterized in that: The following steps are involved: 1) Using 1,4-dioxane-water solution to extract ground wood lignin from tobacco stems; 2) Centrifuge the silk fibroin, take the supernatant, and dilute it for later use; The ground wood lignin is dissolved in a PBS buffer solution, heated to 60-65°C, kept warm for 10-15 minutes, and then cooled to 25-27°C, and then a silk fibroin solution, β-glucosidase and laccase are added at 30-32°C, mixed, reacted for 4-6 hours under the condition of continuous blowing of sterile air, and then heated to 60-65°C to terminate the reaction; centrifuged at a speed of 9000-10000 r / min, and the obtained precipitate was dried at 60-65°C to obtain a lignin-silk fibroin complex; wherein the mass ratio of ground wood lignin to silk fibroin is (3-4):1; The dosage of β-glucosidase is 500-600U, and the dosage of laccase is 1600-1700U.

2. The method for preparing the cigarette paper additive according to claim 1, characterized in that: Step 1) is specifically: extracting the tobacco stem powder in a 1,4-dioxane-water solution for 22-24 hours, repeating 2-3 times, and separating to obtain a crude extract; The crude extract was treated with acetic acid-water mixture, dimethyl sulfoxide and anhydrous ether in sequence to obtain purified groundwood lignin.

3. The method for preparing the cigarette paper additive according to claim 2, characterized in that: The method also includes the step of secondary purification of the purified ground wood lignin by sequentially using an acetic acid-water mixture, acetone, an acetic acid-acetone mixture, anhydrous ether and petroleum ether.

4. The method for preparing the cigarette paper additive according to claim 3, characterized in that: Before the 1,4-dioxane-water solution, a pretreatment step is also included: the tobacco stems are crushed to 200-250 meshes, then extracted with a benzene-methanol solution for 48-52 hours, solid-liquid separation, the solid is dried to obtain a powder, and ground to 40-60 meshes for use.

5. The method for preparing the cigarette paper additive according to claim 4, characterized in that: Step 1) is as follows: The pretreated tobacco stem powder is extracted in a 1,4-dioxane-water solution for 22-24 hours, and the extraction is repeated 2-3 times. The resulting precipitate is centrifuged as a crude extract; The crude extract is extracted with an acetic acid-water mixture for 22-24 hours, and the process is repeated 2-3 times. The solution obtained by centrifugation is concentrated and dried, and then extracted with dimethyl sulfoxide. The solution obtained by centrifugation is dripped into anhydrous ether, centrifuged, and the obtained precipitate is dried, and then dissolved with an acetic acid-water mixture. The dissolved solution is dripped into acetone, centrifuged, and the obtained precipitate is dried, washed with an acetic acid-acetone mixture containing 1-1.5% acetic acid by mass, and then washed with anhydrous ether for 2-3 times, and then washed with petroleum ether, and dried to obtain ground wood lignin; Wherein, the volume ratio of acetic acid to water in the acetic acid-water mixture is (1-1.5):

1.

6. The method for preparing the cigarette paper additive according to any one of claims 1 to 5, characterized in that: In the 1,4-dioxane-water solution, the volume ratio of 1,4-dioxane to water is (94-96):(4-6).

7. The cigarette paper additive obtained by the preparation method according to any one of claims 1 to 6.

8. A tipping paper, characterized in that: Add the cigarette paper additive according to claim 7.

9. The method for preparing the tipping paper according to claim 8, characterized in that: The following steps are involved: The coniferous wood and the hardwood are mixed in a mass ratio of 6:4, and pulped by a sulfite method. A cigarette paper additive is added during pulping, and papermaking is performed to obtain tipping paper.

10. The method for preparing tipping paper according to claim 9, characterized in that: The coniferous wood is spruce and the broad-leaved wood is poplar.

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