Low-nicotine tobacco extract and preparation method thereof

Abstract

The invention discloses a low-nicotine tobacco extract and a preparation method thereof. The preparation method comprises the following steps: mixing tobacco leaves and a solvent, and standing; heating and refluxing the mixed solution, and extracting to obtain a tobacco extracting solution; crushing bamboos to obtain bamboo powder particles; placing the bamboo powder particles in phosphoric acid ethylenediamine, and performing ultrasonic oscillation to obtain activated bamboo powder particles; heating and dehydrating, and then sealing and pressurizing; the treated bamboo powder particles are heated and pyrolyzed, obtained bamboo charcoal is sieved and then washed until a washing solution is clear and colorless and the pH value is kept unchanged, and a porous bamboo charcoal material is obtained through air drying; soaking the porous bamboo charcoal material in NaOH, filtering and cleaning until the pH value of filtrate is not changed, and drying to obtain a modified porous bamboo charcoal material; and mixing the modified porous bamboo charcoal adsorption material with a tobacco extracting solution, and concentrating to obtain the low-nicotine tobacco extract. The preparation method of the low-nicotine tobacco extract is easy to operate, raw materials are low in cost, and the low-nicotine tobacco extract is non-toxic and renewable; meanwhile, nicotine can be better adsorbed. The low-nicotine tobacco extract can obviously soften smoke and reduce dry feeling and irritation.

Description

Technical Field

[0001] The present invention relates to the technical field of tobacco flavorings, and particularly relates to a low-nicotine tobacco extract and a preparation method thereof. Background Art

[0002] With the improvement of living standards and the popularization of health knowledge, the public's awareness of the harm of smoking has been increasing. People have begun to pay attention to how to reduce the harm of smoking to health, and reducing tar and harm has become an important concern. At present, the tar content can be effectively reduced by screening tobacco varieties with low tar content, using new filter tips and other methods. However, with the reduction of tar content, the aroma concentration in cigarettes or new tobacco products decreases, affecting the sensory experience of consumers. Therefore, while promoting the reduction of tar and harm, it is necessary to add flavorings to tobacco products to make up for the lack of aroma. Tobacco extract is an important flavor in tobacco flavorings, which can increase the natural aroma of tobacco and improve the sensory experience when inhaled, and is widely used in cigarettes. However, when extracting the aroma from tobacco, nicotine in tobacco is also extracted. Nicotine in tobacco extract will affect the smoking sensory experience of new tobacco products such as cigarettes. Therefore, selectively reducing nicotine in tobacco extract, when using low-nicotine tobacco extract, can add tobacco-derived aroma without introducing nicotine, effectively solving the problem of the decline in cigarette quality caused by the reduction of tar and harm.

[0003] Currently, the main method for low-nicotine tobacco extract is to remove nicotine through molecular distillation. However, this method has a high cost and is not suitable for large-scale production. Molecular distillation removes nicotine substances through boiling points. However, substances such as methyl phenylacetate and megastigmatrienone with boiling points similar to nicotine will be removed together during the molecular distillation process. Therefore, the molecular distillation method will remove some aroma substances during the process of reducing nicotine, affecting the quality of tobacco extract. Nicotine in tobacco extract can also be adsorbed by the above-mentioned hygroscopic adsorbents (substances such as bentonite and cross-linked polyvinylpyrrolidone). This method uses the hygroscopic adsorbent to absorb moisture and expand, and utilizes the water solubility of nicotine to adsorb nicotine. However, the use conditions of this method are limited. A large amount of water is required to expand the hygroscopic adsorbent, and nicotine in tobacco extract extracted by ethanol or solvents such as ketones and esters cannot be effectively adsorbed. Nicotine in concentrated tobacco extract with less water cannot be effectively adsorbed either. Although the hygroscopic adsorbent can selectively adsorb water-soluble nicotine by utilizing the water solubility of nicotine, and has a weak adsorption capacity for aroma substances with low water solubility in tobacco extract. However, in addition to nicotine, there are also some water-soluble sugars, glycoside substances, etc. in the water-soluble substances in tobacco extract. These substances will be adsorbed by the hygroscopic adsorbent together, thus affecting the quality of tobacco extract.

[0004] Therefore, the above methods are difficult to effectively ensure reducing nicotine in tobacco extract while maintaining the quality of tobacco extract. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide a low-nicotine tobacco extract and a preparation method thereof, wherein porous bamboo charcoal is used to adsorb the tobacco extract to obtain a tobacco extract with low nicotine content and high quality.

[0006] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0007] A method for preparing a low-nicotine tobacco extract comprises the following steps:

[0008] (1) placing tobacco leaves in a reaction kettle, adding a solvent, and allowing the reaction to stand; heating the mixed solution to reflux, extracting the tobacco, and obtaining a tobacco extract;

[0009] (2) Select fresh and hard bamboo, wash and dry it, crush it with a plant crusher and sieve it to obtain bamboo powder particles, and dry it for later use;

[0010] (3) placing the bamboo powder particles obtained in step (2) in ethylenediamine phosphate, mixing and stirring, and then subjecting to ultrasonic vibration treatment to prepare activated bamboo powder particles;

[0011] (4) heating and dehydrating the activated bamboo powder particles obtained in step (3), placing the dehydrated particles in a closed tube furnace, passing nitrogen gas through the furnace to expel air, and pressurizing the furnace in an airtight state without air;

[0012] (5) heating the bamboo powder particles treated in step (4) to 800-900° C. for pyrolysis, stopping heating and naturally cooling to room temperature, sieving the obtained bamboo charcoal and washing it with deionized water for multiple times until the washing liquid is clear and colorless and the pH remains unchanged, and air-drying it in an oven to obtain a porous bamboo charcoal material;

[0013] (6) immersing the porous bamboo charcoal material obtained in step (5) in 10% NaOH, filtering and washing repeatedly until the pH value of the filtrate remains unchanged, and drying in an oven to a constant weight to obtain a modified porous bamboo charcoal material;

[0014] (7) Mixing the modified porous bamboo charcoal adsorption material obtained in step (6) and the tobacco extract obtained in step (2), placing the mixture in a single-effect concentration device, concentrating the mixture, and filtering the mixture to obtain a low-nicotine tobacco extract.

[0015] Preferably, in the above technical solution, in step (1), the solvent is ethanol and / or water, the amount of the solvent is 3 to 9 times the mass of the tobacco leaves, the standing time is 8 to 15 hours; the extraction temperature is 80 to 98°C, and the heating time is 4 to 12 hours.

[0016] Preferably, in the above technical solution, in step (2), the particle size of the bamboo powder is 40-50 mesh, the drying temperature is 50-80 °C, and the drying time is 5-8 h.

[0017] Preferably, in the above technical solution, in step (3), the mass ratio of the bamboo powder particles to the ethylenediamine phosphate is (1-2):(3-5), the ultrasonic power is 200-400 w, and the ultrasonic time is 2-4 h.

[0018] Preferably, in the above technical solution, in step (4), the dehydration degree of the bamboo powder particles is 15-25%, and the pressure is 0.2-0.3 MPa.

[0019] Preferably, in the above technical solution, in step (5), the pyrolysis time is 6-8 h, the size of the porous bamboo charcoal material is 90-110 mesh, and the drying temperature is 100-110 °C.

[0020] Preferably, in the above technical solution, in step (6), the soaking temperature of the porous bamboo charcoal in NaOH is 60 °C, the soaking time is 5-7 h, and the oven temperature is 100-110 °C.

[0021] Preferably, in the above technical solution, in step (7), the concentration vacuum degree is 0.1 MPa, the concentration temperature is 45-55 °C, the dosage of the bamboo charcoal adsorption particles is 0.5-2 g / L, and the concentration is up to a density of 1.05 g / cm 3 .

[0022] A low-nicotine tobacco extract, which is prepared according to the above preparation method.

[0023] An application of a low-nicotine tobacco extract in improving the quality of cigarettes.

[0024] The above technical solution of the present invention has the following beneficial effects:

[0025] (1) The present invention uses pyrolysis to carbonize bamboo into porous charcoal, prepares porous bamboo charcoal, adsorbs nicotine in the tobacco extract, and obtains a low-nicotine tobacco extract;

[0026] (2) The present invention prepares an adsorption material from bamboo, which has simple operation, low cost of raw materials required, no toxicity, and is renewable.

[0027] (3) The present invention modifies the porous bamboo charcoal, which has better adsorption of nicotine. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The drawings incorporated in and constituting a part of this specification illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

[0029] Figure 1 Spectrum comparison diagram of low-nicotine extract and nicotine extract. Detailed implementation manners

[0030] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that: Unless otherwise specifically stated, the relative arrangements, numerical expressions, and numerical values of the components and steps set forth in these embodiments do not limit the scope of the present invention.

[0031] Unless otherwise specified, the experimental methods used in the following examples are all conventional methods. The materials and reagents used, unless otherwise specified, can all be obtained from commercial sources. The equipment used in the experiments, unless otherwise specified, are all well-known to those skilled in the art.

[0032] Bamboo charcoal is a renewable porous carbonaceous green material, which has a lower specific surface area, more oxygen-containing functional groups, and a porous structure compared to adsorption materials such as activated carbon. By calcining bamboo charcoal, its micropores are carbonized, and the porous bamboo charcoal is modified. Porous bamboo charcoal is added during the concentration stage of tobacco extract to adsorb the nicotine component in the tobacco extract, and finally a low-nicotine tobacco extract is prepared. The pores of bamboo charcoal are similar to those of fullerene carbon and carbon nanotubes with five-membered and six-membered rings, and have better adsorption properties for nicotine, a nitrogen heterocycle, lower cost, and are more environmentally friendly. Bamboo charcoal modified with NaOH increases the specific surface area and micropore volume of bamboo charcoal, reduces the surface hydrophobicity of bamboo charcoal, and has a better nicotine removal effect.

[0033] Example 1

[0034] A preparation method of a low-nicotine tobacco extract, comprising the following steps:

[0035] (1) Add 100 kg of tobacco leaves and 600 L of water to a reaction kettle, and let it stand for 12 h to impregnate the tobacco leaves. After impregnation, heat and reflux the tobacco leaf aqueous solution at 98 °C for 6 h, cool it, and filter to obtain a tobacco extract;

[0036] (2) Select fresh and hard bamboo, wash and dry it, crush it with a plant crusher and pass through a 40-mesh sieve, and obtain bamboo powder particles after drying; mix the bamboo powder particles with twice the mass of ethylene diamine phosphate, and ultrasonically treat it at a power of 200 w for 3 h to obtain activated bamboo powder particles; dehydrate the activated bamboo powder particles to 20%, place them in a closed tubular furnace, close and pressurize it to 0.2 MPa under nitrogen, then pyrolyze it at 800 °C for 8 h, stop heating and naturally cool to room temperature, wash the obtained bamboo charcoal with deionized water through a 100-mesh sieve for multiple times until the washing liquid is clear, colorless, and the pH remains unchanged, and dry it in an oven to obtain a porous bamboo charcoal material;

[0037] (3) Mix the porous bamboo charcoal material into 10% NaOH solution, heat it to 60 °C and soak for 5 h, filter and wash repeatedly until the pH value of the filtrate remains unchanged, and dry it to constant weight at 100 °C in an oven to obtain the modified porous bamboo charcoal material;

[0038] (4) Take 300 g of the modified porous bamboo charcoal adsorbent and mix it with the tobacco extract, and concentrate it to a low nicotine tobacco extract with a density of about 1.05 g / cm 3 at 50 °C and a vacuum of 0.1 MPa.

[0039] Detection of low nicotine tobacco extract:

[0040] Adopt the direct injection method, and analyze the aroma components of the low nicotine tobacco extract by GC-MS. The specific steps are as follows:

[0041] Take 0.1 g of the sample, dissolve it in 10 g of anhydrous ethanol, shake well, and filter the solution with a 0.45 μm microporous filter membrane;

[0042] Analyze and detect the aroma of the low nicotine extract by using an Agilent 7890-5975C gas chromatography-mass spectrometry instrument. The chromatographic column is DB-5 (60 m × 0.25 mm × 0.25 μm), the inlet temperature is 250 °C, the split ratio is 15:1, the injection volume is 1 μL, and the temperature programming is: hold at 50 °C for 10 minutes, and then increase the temperature to 260 °C at a rate of 8 °C / min, and hold for 10 min.

[0043] Referring to Example 1, replace the solvent in step (1) with ethanol or a 1:1 mixture (by volume) of the two, and the detection results are found to be basically the same as those in Example 1.

[0044] Preparation and detection of the control (CK) tobacco extract:

[0045] Preparation: Add 100 kg of tobacco leaves and 600 L of water to the reaction kettle, and let it stand for 12 h to impregnate the tobacco leaves. After impregnation, heat and reflux the tobacco leaf aqueous solution at 98 °C for 6 h, cool and filter to obtain the tobacco extract, and concentrate it to a tobacco extract with a density of about 1.05 g / cm3 at 50 °C and a vacuum of 0.1 MPa.

[0046] Detection: Dilute the obtained nicotine tobacco extract with chromatographic grade anhydrous ethanol, filter it through a 0.45 μm microporous filter membrane, and take 1 μL of the solution for GC-MS analysis. The analysis conditions are the same as those in the detection of Example 1.

[0047] The detection results are as Figure 1 shown, in Figure 1Among them, the low-nicotine tobacco extract in Example 1 shows a blue chromatogram, and the tobacco extract shows a black chromatogram. After adsorption by porous bamboo charcoal, the nicotine content in the nicotine extract of the low-nicotine tobacco extract is significantly reduced.

[0048] Application Example 1

[0049] The extracted low-nicotine tobacco extract was injected into blank cigarettes at a content of 100 ppm and evaluated by suction after being stabilized for 48 h in an environment of 25°C and 80% humidity.

[0050] The smoking evaluation results show (Table 1) that the low-nicotine tobacco extract can significantly soften the smoke in cigarettes, increase the aroma concentration of cigarettes, and reduce the dryness and irritation, etc.

[0051] Table 1 Smoking Evaluation Results

[0052]

[0053] Note: "+" indicates a positive impact, and "-" indicates a negative impact.

[0054] Although the present invention has been disclosed above by way of examples, it is not intended to limit the present invention. Any person skilled in the art can make various different selections and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention is defined by the claims and their equivalent forms.

Claims

1. A preparation method of a low-nicotine tobacco extract, characterized in that, It includes the following steps: (1) Place the tobacco leaves in a reaction kettle, add a solvent, and let it stand; heat and reflux the mixed solution to extract the tobacco to obtain a tobacco extract; (2) Select fresh and hard bamboo, wash and dry it, crush it with a plant crusher and sieve it to obtain bamboo powder particles, and dry them for standby; (3) Place the bamboo powder particles obtained in step (2) in ethylenediamine phosphate, mix and stir, and then perform ultrasonic oscillation treatment to prepare activated bamboo powder particles; (4) Heat the activated bamboo powder particles obtained in step (3) for dehydration, and after dehydration, place them in a closed tubular furnace, pass nitrogen into it to discharge air, and apply pressure in a closed state under air isolation; (5) Heat up the bamboo powder particles treated in step (4), pyrolyze at 800 - 900 °C, stop heating and let it cool naturally to room temperature. Sieve the obtained bamboo charcoal and wash it with deionized water for multiple times until the washing liquid is clear, colorless and the pH remains unchanged, and dry it in an oven to obtain a porous bamboo charcoal material; (6) Immerse the porous bamboo charcoal material obtained in step (5) in 10% NaOH, filter and wash repeatedly until the pH value of the filtrate remains unchanged, and dry it in an oven to constant weight to obtain a modified porous bamboo charcoal material; (7) Mix the modified porous bamboo charcoal adsorbent material obtained in step (6) and the tobacco extract obtained in step (2), put it into a single-effect concentration device, concentrate and then filter to obtain a low-nicotine tobacco extract.

2. The preparation method of the low-nicotine tobacco extract according to claim 1, characterized in that In step (1), the solvent is ethanol and / or water, the dosage of the solvent is 3 - 9 times the mass of the tobacco leaves, the standing time is 8 - 15 hours; the extraction temperature is 80 - 98 °C, and the heating time is 4 - 12 h.

3. The preparation method of the low-nicotine tobacco extract according to claim 1, characterized in that, In step (2), the size of the bamboo powder particles is 40 - 50 mesh, the drying temperature is 50 - 80 °C, and the drying time is 5 - 8 h.

4. The preparation method of the low-nicotine tobacco extract according to claim 1, wherein, In step (3), the mass ratio of the bamboo powder particles to the ethylenediamine phosphate is (1 - 2):(3 - 5), the ultrasonic power is 200 - 400 w, and the ultrasonic time is 2 - 4 h.

5. The preparation method of the low-nicotine tobacco extract according to claim 1, characterized in that, In step (4), the dehydration degree of the bamboo powder particles is 15 - 25%, and the pressure is 0.2 - 0.3 MPa.

6. The preparation method of the low-nicotine tobacco extract according to claim 1, wherein, In step (5), the pyrolysis time is 6 - 8 h, the size of the porous bamboo charcoal material is 90 - 110 mesh, and the drying temperature is 100 - 110 °C.

7. The preparation method of the low-nicotine tobacco extract according to claim 1, characterized in that, In step (6), the soaking temperature of the porous bamboo charcoal in NaOH is 60 °C, the soaking time is 5 - 7 h, and the oven temperature is 100 - 110 °C.

8. The preparation method of the low-nicotine tobacco extract according to claim 1, wherein, In step (7), the concentration vacuum is 0.1 MPa, the concentration temperature is 45 - 55 °C, the dosage of bamboo charcoal adsorption particles is 0.5 - 2 g / L, and it is concentrated to a density of 1.05 g / cm 3 .

9. A low-nicotine tobacco extract, characterized in that, The low-nicotine tobacco extract is prepared by the preparation method according to any one of claims 1 - 8.

10. Use of the low-nicotine tobacco extract according to claim 9 in improving the quality of cigarettes.

Images