A filter rod forming paper based on tobacco concentrate supplemented with bioelectric fermentation and a preparation method thereof

Abstract

This invention belongs to the field of tobacco processing technology, and provides a filter rod forming paper with flavoring based on bio-electrofermentation of tobacco concentrate and its preparation method. The filter rod forming paper consists of a low-tar cigarette high-filtration filter rod forming paper base paper and a flavoring layer. The flavoring layer is a flavoring composition obtained by microbial electrofermentation using tobacco waste extract as a substrate. The filter rod forming paper has a basis weight of 30 g / m³. 2 ~45g / m 2 The moisture content is 5%~8%, and the physicochemical properties are adapted to the requirements of cigarette production. The preparation method is as follows: First, tobacco waste extract is prepared; then, a mixed bacterial flora, including Bacillus subtilis, is domesticated and inoculated to obtain a fermentation substrate. After fermentation under segmented dynamic control of parameters such as electric field and temperature, the extract is concentrated and filtered to obtain a purified aroma liquid. This purified aroma liquid is then loaded onto the substrate through a dip-coating process, and dried to obtain the finished product. This invention can precisely compensate for the aroma loss during the high-filtration process of low-tar cigarettes, significantly improving the richness and harmony of cigarette aroma, and reducing off-flavors and irritation.

Description

Technical Field

[0001] This application relates to the field of tobacco processing technology, and in particular to a filter rod forming paper based on bio-electro-fermented tobacco concentrate for flavor enhancement and its preparation method. Background Technology

[0002] Filter rod forming paper is an important material in tobacco processing. In low-tar cigarettes, while high-filtration filters can reduce the content of harmful substances, they can easily lead to the loss of aroma and a bland taste. Therefore, flavor-enhancing forming paper has become key to improving the quality of low-tar cigarettes. As the tobacco industry moves towards "high aroma, low harm, and low tar," the development of flavor-enhancing forming paper adapted to high-filtration filters is crucial.

[0003] Currently, the flavoring methods for forming paper used in low-tar cigarettes mainly involve adding chemically synthesized flavorings and coating with natural plant-extracted flavorings. The former suffers from poor flavor coordination and is prone to introducing off-flavors, while the latter is constrained by natural conditions, has high costs, and is difficult to mass-produce. At the same time, existing flavoring technologies have defects such as unstable flavor combination and uneven aroma release, which cannot accurately compensate for the aroma loss of high-filtration filters, affecting the smoking experience.

[0004] With the rapid development of microbial fermentation technology, it has shown significant application potential in the field of tobacco flavor improvement. Through microbial metabolic transformation, it can generate a rich variety of small-molecule aroma substances such as alcohols, aldehydes, ketones, and esters, providing a green and sustainable path for enriching and improving the aroma quality of tobacco. However, at the industrial application level, traditional microbial fermentation methods have many problems: due to the complexity of microbial metabolic pathways and unclear regulatory mechanisms, the synthesis efficiency of target aroma components is low, and the yield is difficult to increase; at the same time, the fermentation process is often accompanied by the generation of various byproducts, which not only interfere with the target aroma, but also pose challenges to the consistent control of product flavor due to the instability of their components. In addition, the long cycle and insufficient precision of condition control in traditional fermentation processes make it difficult to accurately match the modern tobacco industry, especially the demand for efficient, stable, and targeted aroma supply for flavoring materials in high-filtration filter rods.

[0005] To overcome the regulatory challenges of traditional microbial fermentation, microbial electrofermentation (MEF) technology has emerged as a novel bioelectrochemical strategy. The core of this technology lies in using an external electric field or electrode interface to directly or indirectly influence the intracellular redox state and energy metabolism of microorganisms, thereby achieving precise guidance and enhancement of specific metabolic pathways. Compared to traditional methods, MEF can more effectively promote the synthesis of target products, inhibit unnecessary side reaction pathways, and improve the directionality and efficiency of the entire fermentation process, providing a new approach for the precise construction of complex flavor systems. However, a review of existing technical literature reveals that there are currently no publicly available reports or mature processes for specifically applying microbial electrofermentation technology to the preparation of flavor-enhanced formed paper. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides a filter rod forming paper based on bio-electrofermentation of tobacco concentrate and its preparation method. It uses microbial electrofermentation technology to directionally synthesize aroma components that match the natural aroma of tobacco, and combines this with an impregnation coating process to prepare the filter rod forming paper. This enables precise and continuous compensation for aroma loss in high-filtration filters, ultimately achieving the goal of improving the smoking quality of low-tar cigarettes.

[0007] To achieve the above and related objectives, the present invention employs the following technical means:

[0008] The first aspect of this invention provides a filter rod forming paper based on bio-electrofermentation of tobacco concentrate for flavor enhancement, comprising a low-tar cigarette high-filtration filter rod forming paper base paper substrate and a flavoring layer loaded on the substrate; the flavoring layer comprises a flavoring composition obtained by microbial electrofermentation using tobacco waste extract as a fermentation substrate; and the basis weight of the filter rod forming paper is 30 g / m³. 2 ~45 g / m 2 The moisture content is 5% to 8%.

[0009] Furthermore, the longitudinal tensile strength of the filter rod forming paper is ≥2.5kN / m, and the transverse tensile strength is ≥1.0kN / m.

[0010] Furthermore, the content of the aroma-inducing composition on the filter rod forming paper is 58.4 μg / g to 81.2 μg / g.

[0011] A second aspect of this invention provides a method for preparing filter rod forming paper based on bio-electro-fermented tobacco concentrate for flavor enhancement, comprising the following steps:

[0012] (1) Preparation of tobacco waste extract;

[0013] (2) The activated abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium were respectively composed of an aerobic mixed bacterial group, and inoculated into LB-glucose composite acclimatization medium containing tobacco waste extract for acclimatization culture to obtain acclimatized bacterial solution;

[0014] (3) The acclimatized bacterial solution was inoculated into the tobacco waste extract and aerobic culture was carried out; after 24 hours of culture, the associated lactobacillus was inoculated and the environment was switched to low oxygen or anaerobic to obtain the fermentation substrate;

[0015] (4) The fermentation substrate is subjected to segmented electro-fermentation. During the fermentation process, the electric field, temperature, dissolved oxygen and stirring parameters are dynamically controlled. The pH is maintained at 6.0~7.0 using sterile acid solution or sterile alkali solution. The fermentation process is monitored to obtain the fermentation broth.

[0016] (5) The fermentation broth is concentrated and filtered to obtain a purified aroma-enhancing liquid;

[0017] (6) Using the base paper of low tar cigarette high filter rod forming paper as the base, the dip coating liquid is loaded onto the base through the dip coating process, and the filter rod forming paper is obtained by low temperature drying and shaping. The dip coating liquid is prepared by using purified aroma liquid and aroma fixing agent as raw materials.

[0018] Furthermore, the reaction conditions in step (2) satisfy at least one of the following conditions (a) to (b):

[0019] (a) The mass ratio of activated *Wickhamia lanceolata*, *Bacillus subtilis*, and *Acetobacter pasteurellium* in the mixed microbial community was 1:(0.9–1.2):(1.2–1.6);

[0020] (b) The content of tobacco waste extract in LB-glucose composite acclimatization medium is 5%.

[0021] Furthermore, the reaction conditions in step (4) satisfy at least one of the following conditions (d) to (j):

[0022] (d) Dynamic control of the electric field includes: applying a voltage of 0.3V to 0.5V during the fermentation period of 0h to 24h; applying a voltage of 0.5V to 0.8V during the fermentation period of 24h to 48h; and applying a voltage of 0.3V to 0.5V during the fermentation period of 48h to 72h.

[0023] (e) Dynamic temperature control includes: maintaining an ambient temperature of 25°C to 30°C during the fermentation period from 0h to 24h; maintaining an ambient temperature of 30°C to 35°C during the fermentation period from 24h to 48h; and maintaining an ambient temperature of 25°C to 30°C during the fermentation period from 48h to 72h.

[0024] (f) Dynamic pH control includes: automatically adding sterile acid or sterile alkali solution to maintain pH at 6.0~7.0.

[0025] (j) Dynamic control of dissolved oxygen and stirring parameters includes: dissolved oxygen of 1.5 mg / L to 2 mg / L during 0 h to 24 h of fermentation; dissolved oxygen of 0.5 mg / L to 1 mg / L during 24 h to 48 h of fermentation; dissolved oxygen of 1 mg / L to 1.5 mg / L during 48 h to 72 h of fermentation; and stirring speed of 50 r / min to 150 r / min.

[0026] Furthermore, the reaction conditions in step (3) satisfy at least one of the following conditions (h) to (i):

[0027] (h) Inoculate the acclimatization bacterial solution into the tobacco waste extract at an inoculation rate of 5% to 10% of the volume of the acclimatization bacterial solution, and then carry out aerobic culture.

[0028] (i) When the culture reaches 24h, add the bacterial solution of the associated lactobacillus at an inoculation rate of 1%~3% of the total volume of the system, stop aeration or reduce the aeration rate, switch to a low-oxygen or anaerobic environment, and obtain the fermentation substrate.

[0029] Furthermore, step (5) also includes: concentrating the fermentation broth to 1 / 5 to 1 / 3 of its original volume under vacuum of 0.04 MPa to 0.08 MPa and 50°C to 65°C, and filtering it through a 0.45 μm filter membrane to obtain a purified aroma-enhancing liquid.

[0030] Further, the dip coating process in step (6) includes: mixing and stirring the purified fragrance liquid with ethanol at a volume ratio of 1:(3~5), and adding 0.5%~2% of fragrance fixative to obtain the dip coating solution; taking the single dip coating load as 0.2%~1.0% of the base mass as a benchmark, performing quantitatively controllable dip coating, and after dip coating, the total load of the dip coating solution is 0.2%~0.8% of the base mass; and after dip coating, performing roller extrusion, wherein the fragrance fixative is selected from one or more of β-cyclodextrin, chitosan, propylene glycol, and triacetin.

[0031] Further, the drying in step (6) includes: using a low-temperature drying process, with a drying temperature of 40℃~60℃, and stopping when the moisture content is 5%~8%.

[0032] The beneficial technical effects of this invention are as follows:

[0033] This invention innovatively employs microbial electrofermentation technology to prepare flavor-enhancing formed paper. Compared to traditional chemically synthesized flavorings, the aroma components synthesized through microbial electrofermentation technology have a stronger harmony with the natural aroma of tobacco. This allows for precise matching of the flavor enhancement needs of high-filtration filters in low-tar cigarettes, effectively compensating for aroma loss during the high-filtration process and significantly improving the aroma concentration and richness of low-tar cigarettes. Simultaneously, the microbial electrofermentation technology used in this invention completely avoids the off-flavors caused by chemical synthesis byproducts, greatly improving smoking comfort.

[0034] This invention, by dynamically controlling the electric field, temperature, pH, dissolved oxygen, and stirring parameters during microbial electrofermentation and monitoring the fermentation process, can precisely regulate the microbial metabolic process. This promotes the efficient synthesis of aroma-producing compounds such as alcohols, esters, and heterocyclic compounds (i.e., aroma components) while significantly inhibiting the formation of irrelevant byproducts. Test data shows that, compared to traditional microbial fermentation without an applied electric field, the purified aroma-producing liquid prepared by this invention has a 20%–30% higher content of aroma-producing compounds, demonstrating both quality advantages and economic value.

[0035] This invention employs a dip-coating process to load purified aroma-producing liquid, followed by a low-temperature drying process. This allows the aroma-producing components to be evenly dispersed and firmly bound to the fibers of the base paper used in the high-filtration filter rod forming paper for low-tar cigarettes. The dip-coating process of this invention not only achieves continuous and stable compensation for aroma loss from the high-filtration filter rod, but also effectively solves the problems of uneven aroma distribution and volatility in traditional coating processes, ensuring aroma balance throughout the entire smoking process of low-tar cigarettes.

[0036] The fermentation substrate of this invention uses tobacco waste extract, which can realize the resource reuse of tobacco waste and meet the needs of the circular economy development of the tobacco industry.

[0037] Meanwhile, performance test data further verified that the aroma composition content of the filter rod forming paper prepared by the present invention can reach 58.4μg / g to 81.2μg / g, and the total sensory score of the matching cigarette can reach up to 44.7 points. Compared with the forming paper prepared by traditional fermentation process, the aroma richness is increased by more than 11.5% and the impurities are reduced.

[0038] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and do not limit this application. Detailed Implementation

[0039] Unless otherwise defined, all technical and / or scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. It should be understood that certain features of the invention (described in the context of separate embodiments for clarity) may also be provided in a single embodiment. Conversely, multiple features of the invention (described in the context of a single embodiment for brevity) may also be provided separately or in any suitable combination or, where appropriate, in any other described embodiment of the invention. Certain features described in the context of various embodiments will not be considered essential features of those embodiments unless the embodiment is inoperable without those elements. The invention is further illustrated below by specific examples; however, it should be noted that the specific process conditions and results described in the embodiments of the invention are merely illustrative and should not be construed as limiting the scope of protection of the invention. All equivalent changes or modifications made in accordance with the spirit and essence of the invention should be covered within the scope of protection of the invention.

[0040] This invention provides a filter rod forming paper with added flavor based on bio-electrofermentation of tobacco concentrate. It comprises a low-tar cigarette high-filtration filter rod forming paper base paper substrate and a flavoring layer loaded on the substrate. The flavoring layer includes a flavoring composition obtained by microbial electrofermentation using tobacco waste extract as a fermentation substrate. Furthermore, the filter rod forming paper has an air permeability of 6000 CU to 12000 CU and a basis weight of 30 g / m³. 2 ~45 g / m 2 The moisture content is 5% to 8%.

[0041] Furthermore, the longitudinal tensile strength of the filter rod forming paper is ≥2.5kN / m, and the transverse tensile strength is ≥1.0kN / m.

[0042] Furthermore, the content of the aroma-enhancing composition on the filter rod forming paper is 58.4 μg / g to 81.2 μg / g. The aroma-enhancing composition of this application comprises a variety of aroma-enhancing flavor substances.

[0043] This invention also provides a method for preparing filter rod forming paper based on bioelectrofermentation of tobacco concentrate for flavor enhancement. The preparation method of this application requires the prior construction of a targeted microbial electrofermentation system, in which microbial electrofermentation is carried out.

[0044] Furthermore, this application employs an integrated intelligent control fermentation system to achieve real-time monitoring and closed-loop control of parameters during the fermentation process. The core components and parameter requirements of the system are as follows:

[0045] 1) Reactor assembly: Cylindrical high-pressure reactor with an effective volume of 5L~10L. The reactor body is made of 316L stainless steel with an acid and alkali corrosion resistance level ≥10. The reactor lid is equipped with a fluororubber sealing gasket with a high temperature resistance ≥150℃ and a pressure resistance ≥0.5MPa. An external jacketed constant temperature heating device is installed with a temperature control accuracy of ±0.5℃. A propeller-type stirring paddle is installed at the bottom of the reactor, and its speed is adjustable from 0r / min to 300r / min.

[0046] 2) Electrode System: A dual-chamber electrofermentation system is adopted. The anode chamber contains deionized water / electrolyte solution for oxygen generation through water electrolysis and for adjusting the redox potential of the system. The cathode chamber contains tobacco concentrate fermentation substrate for aroma production by microorganisms. The anode and cathode are placed in their respective chambers, parallel and vertically, with an immersion depth of ≥80% and a distance of ≥2cm from the reactor wall. The anode is a water-electrolysis type titanium-based coated anode (titanium plate substrate thickness 1mm~2mm, pore size 0.5mm~1mm, surface IrO2-Ta2O5 coating thickness 5μm~10μm). The cathode is a modified carbon cloth electrode, which is prepared by soaking carbon cloth in 65% concentrated nitric acid for 2h for activation, rinsing with deionized water until neutral, and drying at 80℃. The specific surface area of ​​the modified carbon cloth electrode is ≥100m². 2 / g, conductivity ≥10S / m; electrode leads are made of polytetrafluoroethylene-coated wires (temperature resistance ≥200℃).

[0047] 3) Power supply and control system: Equipped with a high-precision constant voltage DC power supply (output voltage 0V~2V, current 0A~1A, voltage regulation accuracy ±0.01V, with overcurrent / overvoltage protection); connected to a pH / ORP composite probe (measurement range pH 0~14, ORP -1000~1000mV, accuracy ±0.02pH, ±1mV); adopts a PLC intelligent control system to collect pH, ORP, and temperature in real time (collection frequency 1 time / minute), and automatically adjust the power supply output voltage (adjustment step size 0.05V), heating power, and stirring speed.

[0048] 4) Aeration and exhaust gas treatment system: The bottom of the vessel is equipped with an annular microporous aeration device (pore size 0.2μm~0.5μm, aeration uniformity error ≤5%), which is connected in sequence to a gas flow meter (range 0L / min~5L / min, accuracy ±0.01L / min), a sterile filter (filtration accuracy 0.45μm) and an air compressor; the exhaust gas outlet at the top of the vessel is connected to an activated carbon adsorption device to adsorb volatile impurities.

[0049] Furthermore, the preparation method of this application includes the following steps:

[0050] (1) Preparation of tobacco waste extract.

[0051] Specifically, the steps are as follows: Mix waste tobacco dust and stems at a mass ratio of 1:(1~3), pulverize to 60-120 mesh, add 8-12 times the mass of deionized water, and extract at a constant temperature of 50-60℃ for 2-4 hours. After filtration, obtain tobacco waste extract.

[0052] (2) The activated abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium were respectively composed into an aerobic mixed bacterial group, and inoculated into LB-glucose composite acclimatization medium containing tobacco waste extract for acclimatization culture to obtain acclimatized bacterial solution.

[0053] Specifically, the steps are detailed as follows: Incubate *G. dermatologica* (GDMCC 2.247) aerobically at 30°C for 24 hours until OD (dose-to-displacement) reaches zero. 600 =1.2~1.5; Bacillus subtilis (CICC 10275) was cultured aerobically at 37℃ for 18h until the bacterial concentration reached 10. 8 ~10 9 CFU / mL; Acetobacter pasteurellosis (CGMCC1.41) was cultured aerobically at 30℃ for 20 h until OD. 600 =0.8~1.0. Activated *Wickham's abnormal* yeast, *Bacillus subtilis*, and *Acetobacter pastoris* were mixed in an aerobic bacterial culture at a mass ratio of 1:(0.9~1.2):(1.2~1.6). This mixed culture was inoculated into an LB-glucose composite acclimatization medium containing 5% tobacco waste extract and cultured at 30℃ and 100 rpm for 8 hours to obtain the acclimatized bacterial solution. The LB-glucose composite acclimatization medium consisted of 20 g / L glucose, 10 g / L peptone, 5 g / L yeast extract, and 5 g / L NaCl, with a pH of 6.5~7.0.

[0054] (3) The acclimatized bacterial solution obtained in step (2) is inoculated into the tobacco waste extract for aerobic culture; after 24 hours of culture, it is inoculated with associated lactobacillus, aeration is stopped or the aeration rate is reduced, and the environment is switched to low oxygen / anaerobic to obtain the fermentation substrate.

[0055] Specifically, the steps are detailed as follows: The *Lactobacillus symbioticus* (JCM14932) is anaerobically cultured at 37°C for 16-20 hours until the OD (Organic Depth) is reached. 600 =1.0~1.2; Inoculate the acclimatized bacterial solution into the tobacco waste extract at an inoculation rate of 5%~10% of the volume of the acclimatized bacterial solution, and carry out aerobic culture; After 24 hours of culture, add the bacterial solution of associated lactobacillus at an inoculation rate of 1%~3% of the total volume of the system, switch to a low-oxygen / anaerobic environment, and obtain the fermentation substrate.

[0056] (4) The fermentation substrate is subjected to segmented electro-fermentation. During the fermentation process, the electric field, temperature, dissolved oxygen and stirring parameters are dynamically controlled. Sterile acid solution or sterile alkali solution is automatically added to maintain the pH at 6.0~7.0, and the fermentation process is monitored to obtain the fermentation broth.

[0057] Specifically, this step is carried out in the aforementioned integrated intelligent control fermentation system, as detailed below: The fermentation parameters of the fermentation substrate are adjusted in stages:

[0058] The dynamic regulation of the electric field includes: applying a voltage of 0.3V to 0.5V during the fermentation period of 0h to 24h to promote microbial colonization; applying a voltage of 0.5V to 0.8V during the fermentation period of 24h to 48h to promote the synthesis of aroma components (aroma flavor substances); and applying a voltage of 0.3V to 0.5V during the fermentation period of 48h to 72h to reduce by-products.

[0059] Dynamic temperature control includes: maintaining an ambient temperature of 25℃~30℃ during the fermentation period of 0h~24h to promote growth; maintaining an ambient temperature of 30℃~35℃ during the fermentation period of 24h~48h to improve enzyme activity; and maintaining an ambient temperature of 25℃~30℃ during the fermentation period of 48h~72h to stabilize the product. The temperature control accuracy is ±0.5℃ throughout the entire process.

[0060] Dynamic pH control includes: automatically adding sterile acid or alkali solutions to maintain the pH at 6.0-7.0; the electric field is only used to regulate microbial metabolism and does not participate in pH regulation.

[0061] Dynamic control of dissolved oxygen and stirring parameters includes: dissolved oxygen of 1.5 mg / L to 2 mg / L during fermentation from 0 h to 24 h; dissolved oxygen of 0.5 mg / L to 1 mg / L during fermentation from 24 h to 48 h; and dissolved oxygen of 1 mg / L to 1.5 mg / L during fermentation from 48 h to 72 h; and stirring speed of 50 r / min to 150 r / min to adapt to dissolved oxygen requirements.

[0062] The total fermentation time for this application is 48-72 hours. Samples are taken every 12 hours to detect the aroma component content in the intermediate fermentation broth. Fermentation is stopped when the content reaches its peak value. Every 12 hours, aroma components (GC-MS method), pH, dissolved oxygen, and cell density (OD) are measured. 600 ), plot the fermentation curve, and stop the machine to troubleshoot any abnormalities.

[0063] (5) The fermentation broth is concentrated and filtered to obtain purified aroma liquid.

[0064] Specifically, the steps are as follows: After fermentation, remove the electrode and concentrate the fermentation broth to 1 / 5 to 1 / 3 of its original volume under a vacuum of 0.04MPa to 0.08MPa and a temperature of 50℃ to 65℃. Filter the broth through a 0.45μm filter membrane to obtain a purified aroma-enhancing liquid, and store it at 4℃ for later use.

[0065] (6) Using the base paper of low tar cigarette high filter rod forming paper as the base, the dip coating liquid is loaded onto the base through the dip coating process, and the filter rod forming paper is obtained by low temperature drying and shaping. The dip coating liquid is prepared by using purified aroma liquid and aroma fixing agent as raw materials.

[0066] Specifically, this step is detailed as follows: A commercially available low-tar cigarette high-filter rod forming paper base is selected as the substrate. This substrate has a longitudinal tensile strength ≥2.8kN / m, a transverse tensile strength ≥1.2kN / m, an air permeability of 6000CU~12000CU, and a basis weight of 28g / m³. 2 ~42g / m 2 .

[0067] The purified aroma-generating liquid was mixed with ethanol at a volume ratio of 1:(3~5), and 0.5%~2% food-grade flavor fixative was added to prepare the impregnation solution. The impregnation loading was based on 0.2%~1.0% of the base mass, and quantitatively controllable impregnation was performed at a temperature of 25℃~35℃ and a time of 30s~60s. After impregnation, the total loading of the impregnation solution was 0.2%~0.8% of the base mass. After impregnation, the solution was extruded using rollers at a pressure of 0.1MPa~0.2MPa to ensure uniform loading of the purified aroma-generating liquid. A low-temperature drying process was used to avoid the volatilization of aroma components. The drying temperature was 40℃~60℃, and the moisture content was monitored in real time. Drying was stopped when the moisture content reached 5%~8%. After shaping treatment, filter rod forming paper based on microbial electrofermentation flavoring was obtained.

[0068] The food-grade flavoring agent used in this application is selected from one or more of β-cyclodextrin, chitosan, propylene glycol, and triacetin.

[0069] The present invention will be described in detail below through specific examples and embodiments. It should also be understood that the following embodiments are only for specific illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0070] Example 1

[0071] An integrated intelligent control fermentation system will be constructed, with the following core components and parameter requirements:

[0072] Reactor assembly: Cylindrical high-pressure reactor with an effective volume of 5L~10L, the reactor body is made of 316L stainless steel with an acid and alkali corrosion resistance level ≥10; the reactor lid is equipped with a fluororubber sealing gasket with a high temperature resistance ≥150℃ and a pressure resistance ≥0.5MPa; a jacketed constant temperature heating device is installed on the outside with a temperature control accuracy of ±0.5℃; a propeller-type stirring paddle is installed at the bottom of the reactor, and its speed is adjustable from 0r / min to 300r / min.

[0073] Electrode system: A dual-chamber electrofermentation structure is adopted. The anode is placed in the aqueous solution in the anode chamber, and the cathode is placed in the tobacco fermentation broth in the cathode chamber. They are placed parallel and vertically, with an immersion depth of ≥80% and a distance of 3cm from the reactor wall. The anode is an electrolytic water-type titanium-based coated anode (titanium plate substrate thickness 1.5mm, pore size 0.8mm, surface IrO2-Ta2O5 coating thickness 8μm); the cathode is a modified carbon cloth electrode, which is prepared by soaking carbon cloth in 65% concentrated nitric acid for 2h for activation, rinsing with deionized water until neutral, and drying at 80℃. The specific surface area of ​​the modified carbon cloth electrode is ≥100m². 2 / g, conductivity ≥10S / m; electrode leads are made of polytetrafluoroethylene-coated wires (temperature resistance ≥200℃).

[0074] Power supply and control system: Equipped with a high-precision constant voltage DC power supply (output voltage 0V~2V, current 0A~1A, voltage regulation accuracy ±0.01V, with overcurrent / overvoltage protection); connected to a pH / ORP composite probe (measurement range pH 0~14, ORP -1000~1000mV, accuracy ±0.02pH, ±1mV); adopts a PLC intelligent control system to collect pH, ORP, and temperature in real time (collection frequency 1 time / minute), and automatically adjust the power supply output voltage (adjustment step size 0.05V), heating power, and stirring speed.

[0075] Aeration and exhaust gas treatment system: The bottom of the vessel is equipped with an annular microporous aeration device (pore size 0.5μm, aeration uniformity error ≤5%), which is connected in sequence to a gas flow meter (range 0L / min~5L / min, accuracy ±0.01L / min), a sterile filter (filtration accuracy 0.45μm) and an air compressor; the exhaust gas outlet at the top of the vessel is connected to an activated carbon adsorption device.

[0076] (1) Mix waste tobacco dust and tobacco stems at a mass ratio of 1:2, crush them to 80 mesh, add deionized water at a solid-liquid ratio of 1:10, extract at a constant temperature of 55℃ for 3 hours, and filter to obtain tobacco waste extract.

[0077] (2) Incubate abnormal Wickham yeast (GDMCC 2.247) at 30°C with aerobic culture for 24 h until OD. 600=1.3; Bacillus subtilis (CICC 10275) was cultured aerobically at 37℃ for 18 h until the bacterial concentration reached 5×10⁻⁶. 8 CFU / mL; Acetobacter pasteurellosis (CGMCC1.41) was cultured aerobically at 30℃ for 20 h until OD. 600 =0.9. Activated abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium were combined into an aerobic mixed bacterial group at a mass ratio of 1:1:1.5 and inoculated into LB-glucose composite acclimatization medium containing 5% tobacco waste extract. The culture was carried out at 30℃ and 100r / min for 8h to obtain the acclimatized bacterial solution.

[0078] (3) Inoculate the domesticated bacterial solution into the tobacco waste extract at an inoculation rate of 8%, and culture aerobically for 24 hours; then inoculate with the associated lactobacillus solution (inoculation rate of 1%), stop aeration or reduce the aeration rate, switch to a low-oxygen environment, and obtain the fermentation substrate.

[0079] (4) In the above-mentioned integrated intelligent control fermentation system, the fermentation parameters of the fermentation substrate are controlled in stages:

[0080] During the fermentation period from 0h to 24h, a voltage of 0.3V was applied, maintaining an ambient temperature of 28℃, dissolved oxygen of 1.8mg / L, and stirring at 100r / min; during the fermentation period from 24h to 48h, a voltage of 0.6V was applied, maintaining an ambient temperature of 32℃, dissolved oxygen of 0.8mg / L, and stirring at 80r / min; during the fermentation period from 48h to 72h, a voltage of 0.5V was applied, maintaining an ambient temperature of 28℃, dissolved oxygen of 1.2mg / L, and stirring at 100r / min.

[0081] The pH was maintained at 6.5–7.0 by dropwise addition of sterile acid or alkali solutions, and the electric field did not participate in pH adjustment. The total fermentation time was 72 hours, with samples taken every 12 hours to detect the aroma component content in the intermediate fermentation broth. Fermentation was stopped when the content reached its peak. Furthermore, the aroma components (GC-MS method), pH, dissolved oxygen, and cell concentration (OD) were measured every 12 hours. 600 ), plot the fermentation curve, and stop the machine to troubleshoot any abnormalities.

[0082] (5) After fermentation, remove the electrode and centrifuge the fermentation liquid at 4℃ and 6000r / min for 12min. The supernatant is concentrated to 1 / 4 of the original volume of the fermentation liquid under vacuum of 0.06MPa and 60℃. The purified aroma liquid is obtained by filtration through a 0.45μm filter membrane and stored at 4℃ for later use.

[0083] (6) Commercially available low-tar cigarette high-filter rod forming paper is used as the base. The longitudinal tensile strength of the base is 3.0 kN / m, the transverse tensile strength is 1.3 kN / m, the air permeability is 8000 CU, and the basis weight is 30 g / m. 2 .

[0084] The purified fragrance extract was mixed with ethanol at a volume ratio of 1:4 and stirred. 0.5% propylene glycol fixative was added to prepare the impregnation solution. The substrate was impregnated at 30°C for 45 seconds, and excess liquid was removed by extrusion with a 0.15MPa roller. The substrate was dried at 50°C to a moisture content of 6%. After shaping treatment, filter rod forming paper based on microbial electrofermentation fragrance was obtained. The total loading of the impregnation solution was 0.3% of the substrate mass.

[0085] Example 2

[0086] The difference between this embodiment and Embodiment 1 is that:

[0087] (1) Mix waste tobacco dust and tobacco stems at a mass ratio of 1:1, crush them to 60 mesh, add deionized water at a solid-liquid ratio of 1:8, extract at a constant temperature of 50℃ for 2 hours, and filter to obtain tobacco waste extract.

[0088] (2) Aerobic mixed bacterial group was prepared by mixing abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium in a mass ratio of 1:0.9:1.2, and then domesticated to obtain domesticated bacterial solution.

[0089] (3) Aseptic inoculation was carried out at an inoculation amount of 5% of the volume of the tobacco waste extract liquid. The culture was first aerobic for 24 hours, and then the associated lactobacillus liquid was inoculated. Aeration was stopped or the aeration rate was reduced to switch to a low-oxygen environment to obtain the fermentation substrate.

[0090] (4) The parameters for segmented control during fermentation are as follows: During the fermentation period from 0h to 24h, apply a voltage of 0.3V, maintain an ambient temperature of 25℃, dissolved oxygen of 1.5mg / L, and stir at 80r / min; During the fermentation period from 24h to 48h, apply a voltage of 0.5V, maintain an ambient temperature of 30℃, dissolved oxygen of 0.5mg / L, and stir at 50r / min; Sterile acid / alkali solution is added dropwise to maintain the pH at 6.5~7.0, the electric field does not participate in pH adjustment, and the total fermentation time is 48h.

[0091] (5) During separation and purification, the centrifugation speed is 5000 r / min and the time is 10 min. The vacuum degree is 0.04 MPa and the temperature is 50℃. The volume is concentrated to 1 / 5 of the original volume and filtered through a 0.45 μm filter membrane to obtain the purified aroma solution. It is then stored at 4℃ for later use.

[0092] (6) The purified fragrance liquid and ethanol were mixed and stirred at a volume ratio of 1:3, and 1% food-grade β-cyclodextrin was added to prepare the impregnation solution. The substrate was impregnated at 25°C for 30s, and the excess liquid was removed by 0.1MPa roller extrusion. The substrate was dried at 40°C to a moisture content of 5%. The filter rod forming paper based on microbial electrofermentation fragrance was obtained after shaping treatment. The total loading of the impregnation solution was 0.2% of the substrate mass.

[0093] Example 3

[0094] The difference between this embodiment and Embodiment 1 is that:

[0095] (1) Mix waste tobacco dust and tobacco stems at a mass ratio of 1:3, crush them to 120 mesh, add deionized water at a solid-liquid ratio of 1:12, extract at a constant temperature of 60℃ for 4 hours, and filter to obtain tobacco waste extract.

[0096] (2) The activated abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium were combined into a mixed bacterial group in a mass ratio of 1:1.2:1.6 and domesticated to obtain a domesticated bacterial solution.

[0097] (3) Aseptic inoculation was carried out at an inoculation amount of 10% of the volume of the tobacco waste extract liquid. The culture was first aerobic for 24 hours, and then the associated lactobacillus liquid was inoculated. Aeration was stopped or the aeration rate was reduced to switch to a low-oxygen environment to obtain the fermentation substrate.

[0098] (4) The segmented control parameters during fermentation are as follows: During the fermentation period from 0h to 24h, a voltage of 0.5V is applied to maintain an ambient temperature of 30℃, dissolved oxygen of 2.0mg / L, and stirring at 150r / min; During the fermentation period from 24h to 48h, a voltage of 0.7V is applied to maintain an ambient temperature of 35℃, dissolved oxygen of 1.0mg / L, and stirring at 100r / min; During the fermentation period from 48h to 72h, a voltage of 0.5V is applied to maintain an ambient temperature of 30℃, dissolved oxygen of 1.5mg / L, and stirring at 120r / min; Sterile acid / alkali solution is added dropwise to maintain pH at 7.0, the electric field does not participate in pH adjustment, and the total fermentation time is 72h.

[0099] (5) During separation and purification, the centrifugation speed is 8000 r / min and the time is 15 min. The vacuum degree is 0.08 MPa and the temperature is 65℃. The volume is concentrated to 1 / 3 of the original volume and filtered through a 0.45 μm filter membrane to obtain the purified aroma solution. It is then stored at 4℃ for later use.

[0100] (6) The purified fragrance liquid and ethanol were mixed and stirred at a volume ratio of 1:5, and 1% propylene glycol fragrance fixative was added to prepare the impregnation solution; the substrate was impregnated at 35°C for 60s, and the excess liquid was removed by 0.2MPa roller extrusion. The substrate was dried at 50°C to a moisture content of 6%, and the filter rod forming paper based on microbial electrofermentation fragrance was obtained after shaping treatment. The total loading of the impregnation solution was 0.8% of the substrate mass.

[0101] Comparative Example 1

[0102] The difference between this comparative example and Example 1 is as follows:

[0103] The aroma-generating liquid was prepared using traditional microbial fermentation methods, without constructing a microbial electrofermentation system or applying an electric field.

[0104] Comparative Example 2

[0105] The difference between this comparative example and Example 1 is as follows:

[0106] This comparative example directly uses the forming paper base paper used in Example 1, without microbial electrofermentation, dip coating, drying and other fragrance-related processes.

[0107] Comparative Example 3

[0108] The difference between this comparative example and Example 1 is as follows:

[0109] Instead of preparing the fragrance liquid through microbial electrofermentation, commercially available chemically synthesized fragrances were mixed according to the proportion of fragrance components in Example 1, and then mixed with ethanol at a ratio of 1:4 (volume ratio) to prepare the dipping solution. All other fragrance-adding and shaping processes were completely consistent with those in Example 1.

[0110] Comparative Example 4

[0111] The difference between this comparative example and Example 1 is as follows:

[0112] The fragrance addition process uses a traditional coating method instead of the dip coating process, that is, it is coated on the surface of the base paper of the forming paper by a doctor blade coating method (the coating amount is the same as the loading amount in Example 1). After coating, it is dried at 60°C to a moisture content of 6%. All other process parameters are completely consistent with those in Example 1.

[0113] Comparative Example 5

[0114] The difference between this comparative example and Example 1 is as follows:

[0115] During the microbial electrofermentation process, constant parameters were used throughout the entire process without segmented adjustments. Specifically, a voltage of 0.6V was applied throughout the fermentation process, the temperature was maintained at 30℃, the dissolved oxygen was 1.2mg / L, the stirring speed was 100r / min, the pH was maintained at 6.5~7.0, and the total fermentation time was 60h.

[0116] Performance testing

[0117] Physicochemical properties of the formed paper: The key physicochemical properties of the filter rod formed paper prepared in each embodiment and each comparative example were tested, and the test results are shown in Table 1.

[0118] Table 1. Test results of key physicochemical properties of filter rod forming paper

[0119]

[0120] As shown in Table 1, the longitudinal tensile strength of Examples 1-3 and Comparative Examples 1-3 of this application is 2.6-3.1 kN / m, all meeting the ≥2.5 kN / m standard, while Comparative Example 4 is only 2.3 kN / m. The transverse tensile strength of Examples 1-3 and Comparative Examples 1-3 is 1.2-1.4 kN / m, all meeting the ≥1.0 kN / m standard, while Comparative Example 4 is only 0.8 kN / m. This is because the conventional blade coating method used in Comparative Example 4 may damage the fiber structure of the substrate. The air permeability of Examples 1-3 and Comparative Examples 1-3 is 9450 CU-10500 CU, while that of Comparative Example 4 is 8950 CU. This is because the conventional blade coating method used in Comparative Example 4 may have caused pore blockage. The quantitative values ​​of each example and each comparative example are 30.2 g / m³. 2 ~32.1g / m 2 Both the moisture content and the water content (5.1%~7.8%) meet the standards. The moisture content meeting the standard is due to the low-temperature drying control. The aroma content of Examples 1~3 is 58.4μg / g~81.2μg / g. This is because the microbial electrofermentation technology can directionally synthesize aroma components. Example 3 has the highest aroma composition content due to the high aroma liquid loading. Example 2 has a lower aroma content due to the low coating amount. The comparative examples 1 (traditional fermentation) is 38.3μg / g, 2 (no added flavoring) is 0μg / g, 3 (chemical flavoring) is 28.2μg / g, and 4 (scraper coating process) is 40.3μg / g. The content is low due to technical defects. The physical properties of Comparative Example 5, such as longitudinal and transverse tensile strength and air permeability, are similar to those of Example 1. However, the aroma content is 52.6 μg / g, which is significantly lower than the 69.2 μg / g of Example 1. This is because Comparative Example 5 uses constant parameters throughout the microbial electrofermentation process, which cannot precisely control key parameters such as electric field and temperature according to the metabolic characteristics of different growth stages of microorganisms. It can only maintain basic aroma-producing metabolism and cannot directionally enhance the synthesis of aroma components. At the same time, the inhibition effect on by-products is weaker than that of segmented precise control, which ultimately leads to a significant decrease in the synthesis efficiency of aroma substances.

[0121] Sensory evaluation: Filter rods were prepared using the filter rod forming paper prepared in the above embodiments and comparative examples as raw materials. Based on slim cigarettes (cigarette length 97mm, circumference 17mm, filter length 30mm), the same series of filter rod samples were prepared on the same machine. Based on the slim cigarettes in production, the same series of slim cigarette samples were rolled on the same machine using the above-mentioned filter rods and the same type of tobacco, and sensory evaluation was conducted. The evaluation results are shown in Table 2.

[0122] Table 2 Sensory evaluation results

[0123]

[0124] As shown in Table 2, Example 1 of this application performed best with a total score of 44.7. The core reason is that the aroma components synthesized by microbial electrofermentation technology are rich and highly compatible with the natural aroma of tobacco. Combined with the dip-coating process, it achieves stable aroma release, with no off-flavors and low irritation during smoking, resulting in the best overall experience. Example 2 scored 39.5 points, which was slightly lacking in aroma richness and layering due to the low coating amount. Example 3 scored 42.8 points, slightly lower than Example 1. This is mainly because the aroma liquid loading reached 5% of the original paper mass (achieved through two dip-coatings). The excessive amount of flavoring led to some flavor overlap, and the influence of by-products became more prominent, reducing the sensory experience. In the comparative examples, Comparative Example 1 (traditional fermentation) scored 40.1 points, indicating insufficient flavor substance content and inferior aroma performance compared to the Example group due to limitations of traditional fermentation technology; Comparative Example 2 (no flavoring process) scored only 34.4 points, failing to compensate for aroma loss caused by the high-efficiency filter rod due to the lack of any flavoring treatment, resulting in a noticeably weak aroma during inhalation; Comparative Example 3 (chemical flavoring) scored 32.6 points, showing poor harmony between the synthetic flavoring and the natural tobacco aroma, with prominent issues of off-flavors and irritation; Comparative Example 4 (traditional coating process) scored the worst, with an uneven distribution and volatility of the flavoring, and localized overheating caused by the coating process, leading to additional off-flavors and irritation; The total sensory score of Example 5 was 38.9 points, lower than the 44.7 points of Example 1, and there were significant differences in all aroma indicators. Among them, the richness and harmony of aroma were poor. The core reason is that the flavor substance content in the aroma-generating liquid prepared by fermentation is insufficient, and a small amount of by-products are generated due to the lack of segmented control. Although it has certain advantages compared with the comparative example 1 of traditional fermentation and the comparative example 3 of chemical flavoring, it cannot reflect the core technical value of segmented and precise control of microbial electrofermentation. It directly verifies that the segmented control strategy of this invention can more accurately guide microbial metabolism, directionally synthesize aroma components that match the natural aroma of tobacco, and effectively inhibit by-products, thereby greatly improving the aroma-enhancing effect of filter rod forming paper.

[0125] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. A filter rod forming paper based on bio-electro-fermented tobacco concentrate for flavor enhancement, characterized in that, The filter rod forming paper comprises a base paper substrate for low-tar cigarette high-filtration filter rod forming paper, and an aroma layer loaded on the substrate; the aroma layer comprises an aroma composition obtained by microbial electrofermentation using tobacco waste extract as a fermentation substrate; and the basis weight of the filter rod forming paper is 30 g / m³. 2 ~45 g / m 2 The moisture content is 5% to 8%.

2. The filter rod forming paper according to claim 1, characterized in that, The longitudinal tensile strength of the filter rod forming paper is ≥2.5kN / m, and the transverse tensile strength is ≥1.0kN / m.

3. The filter rod forming paper according to claim 1, characterized in that, The content of the aroma-inducing composition on the filter rod forming paper is 58.4 μg / g to 81.2 μg / g.

4. A method for preparing filter rod forming paper based on aroma-enhancing tobacco concentrate from bio-electro-fermentation, characterized in that, Includes the following steps: (1) Preparation of tobacco waste extract; (2) The activated abnormal Wickham yeast, Bacillus subtilis and Acetobacter pasteurellium were respectively arranged into an aerobic mixed bacterial group, and inoculated into LB-glucose composite acclimatization medium containing the tobacco waste extract for acclimatization culture to obtain acclimatization bacterial solution; (3) The acclimatized bacterial solution is inoculated into the tobacco waste extract and aerobic culture is carried out; after 24 hours of culture, the associated lactobacillus is inoculated and the environment is switched to low oxygen or anaerobic to obtain the fermentation substrate; (4) The fermentation substrate is subjected to segmented electro-fermentation. During the fermentation process, the electric field, temperature, dissolved oxygen and stirring parameters are dynamically controlled. The pH is maintained at 6.0~7.0 using sterile acid solution or sterile alkali solution. The fermentation process is monitored to obtain fermentation broth. (5) The fermentation broth is concentrated and filtered to obtain a purified aroma-enhancing liquid; (6) Using the base paper of low tar cigarette high filter rod forming paper as a base, the base paper is loaded with the dip coating liquid through the dip coating process, and the filter rod forming paper is obtained by low temperature drying and shaping. The dip coating liquid is prepared by using the purified aroma liquid and the aroma fixing agent as raw materials.

5. The preparation method according to claim 4, characterized in that, The reaction conditions in step (2) satisfy at least one of the following conditions (a) to (b): (a) The mass ratio of the activated *Wickham's abnormal yeast*, *Bacillus subtilis*, and *Acetobacter pasteurellium* in the mixed microbial community is 1:(0.9~1.2):(1.2~1.6); (b) The content of the tobacco waste extract in the LB-glucose composite acclimatization medium is 5%.

6. The preparation method according to claim 4, characterized in that, The reaction conditions in step (4) satisfy at least one of the following conditions (d) to (j): (d) The dynamically controlled electric field includes: applying a voltage of 0.3V to 0.5V during the fermentation period of 0h to 24h; applying a voltage of 0.5V to 0.8V during the fermentation period of 24h to 48h; and applying a voltage of 0.3V to 0.5V during the fermentation period of 48h to 72h. (e) The dynamic temperature control includes: maintaining an ambient temperature of 25°C to 30°C during the fermentation period of 0h to 24h; maintaining an ambient temperature of 30°C to 35°C during the fermentation period of 24h to 48h; and maintaining an ambient temperature of 25°C to 30°C during the fermentation period of 48h to 72h. (f) The dynamic pH control includes: automatically adding sterile acid solution or sterile alkali solution to maintain the pH at 6.0~7.

0. (j) The dynamic control of dissolved oxygen and stirring parameters includes: dissolved oxygen of 1.5 mg / L to 2 mg / L during the fermentation period of 0 h to 24 h; dissolved oxygen of 0.5 mg / L to 1 mg / L during the fermentation period of 24 h to 48 h; dissolved oxygen of 1 mg / L to 1.5 mg / L during the fermentation period of 48 h to 72 h; and stirring speed of 50 r / min to 150 r / min.

7. The preparation method according to claim 4, characterized in that, The reaction conditions in step (3) satisfy at least one of the following conditions (h) to (i): (h) Inoculate the acclimatized bacterial solution into the tobacco waste extract at an inoculation rate of 5% to 10% of the volume of the acclimatized bacterial solution, and then perform aerobic culture. (i) When the culture reaches 24h, add the bacterial solution of the associated lactobacillus at an inoculation rate of 1% to 3% of the total system volume, stop aeration or reduce the aeration rate, switch to a low-oxygen or anaerobic environment, and obtain the fermentation substrate.

8. The preparation method according to claim 4, characterized in that, Step (5) further includes: concentrating the fermentation broth to 1 / 5 to 1 / 3 of its original volume under vacuum of 0.04 MPa to 0.08 MPa and temperature of 50°C to 65°C, and filtering it through a 0.45 μm filter membrane to obtain the purified aroma-enhancing liquid.

9. The preparation method according to claim 4, characterized in that, The dip coating process in step (6) includes: mixing the purified fragrance liquid with ethanol at a volume ratio of 1:(3~5) and stirring, and adding 0.5%~2% of fragrance fixative to prepare a dip coating solution; taking the single dip coating load as 0.2%~1.0% of the substrate mass as a benchmark, performing quantitatively controllable dip coating, and after dip coating, the total load of the dip coating solution is 0.2%~0.8% of the substrate mass; and after dip coating, performing roller extrusion, wherein the fragrance fixative is selected from one or more of β-cyclodextrin, chitosan, propylene glycol, and triacetin.

10. The preparation method according to claim 4, characterized in that, The drying process in step (6) includes: using a low-temperature drying process, with a drying temperature of 40℃~60℃, and stopping when the moisture content is 5%~8%.