CN118285558A - Biodegradable filter stick capable of reducing smoke temperature of cigarettes and preparation method thereof - Google Patents
Biodegradable filter stick capable of reducing smoke temperature of cigarettes and preparation method thereof Download PDFInfo
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- CN118285558A CN118285558A CN202410476276.0A CN202410476276A CN118285558A CN 118285558 A CN118285558 A CN 118285558A CN 202410476276 A CN202410476276 A CN 202410476276A CN 118285558 A CN118285558 A CN 118285558A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 51
- 239000000779 smoke Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 10
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
A biodegradable filter stick capable of reducing the smoke temperature of cigarettes is formed by bonding and solidifying biodegradable particles through a biodegradable adhesive, and a netlike three-dimensional porous structure is formed inside the filter stick. The invention also discloses a preparation method of the filter stick, and aims to solve the problems that the effect of reducing the temperature of smoke of the cooling filter stick in the prior art is not obvious and the biodegradability is poor. The filter rod is provided with a firm three-dimensional, through and nonlinear gap porous network structure, a complex and continuous through hole channel is formed in the filter rod, high-temperature flue gas can be rapidly dispersed in a gap of the filter rod after entering the filter rod from one end of the cooling filter rod, and compared with the through cooling filter rod, the relative stroke of the high-temperature flue gas in the cooling filter rod is greatly prolonged, so that the obtained cooling effect is better. The filter stick can be completely degraded in natural environment for a period of time, does not cause burden to the environment, and has good economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of tobacco products, and relates to a cigarette filter, in particular to a biodegradable filter rod for reducing the temperature of cigarette smoke and a preparation method thereof.
Background
Along with the decrease of the proportion of traditional cigarette consumers and the increasingly serious smoke control regulations in the international market, a plurality of international tobacco enterprises develop and market popularization of novel cigarettes which are not burnt by heating, such as the development of tobacco heating products of IQOS of the Feimo international, GLO of Yinmei tobacco, PLOOM TECH of Japanese tobacco, lil of Korean ginseng, KT & G and the like, the market scale, the consumption population and the production and marketing capacity of the cigarette are rapidly expanding year by year, and important influence is generated on the world tobacco market situation.
The heating non-burning tobacco technology is to heat tobacco at 200-400 deg.c with smoldering carbon rod or heating electronic element to make tobacco not burn, but the tobacco components still can be distilled and cracked to release fume. Compared with the traditional combustion tobacco products, the cigarette which is not burnt after being heated has obviously reduced released harmful ingredients compared with the traditional cigarette, and the product safety is obviously improved under the condition of close smoking quality. On the other hand, the use mode of the heated non-combustible cigarettes also faces a problem, namely: the temperature of the high-temperature atomized smoke entering the oral cavity through the filter tip section is higher than the combustion temperature of the traditional cigarettes, so that the inlet smoke is burnt, and a great difference exists between the high-temperature atomized smoke and the traditional cigarettes in the aspects of smoking physical examination, smoking feeling and the like. Lowering the smoke temperature is therefore a critical technique for heating non-burning cigarettes.
For example, iQOS matched cigarettes pushed by the Feimo company adopt a folded polylactic acid film as a cooling material of smoke, but the material is easy to collapse and shrink when heated, influences the cooling effect, and has poor sensory evaluation of odor absorption. The patent CN105686078A adopts ammonium salt as a cigarette cooling agent, so that the temperature of smoke at the end of a filter stick can be obviously reduced, but a small amount of ammonia gas can be generated when the ammonium salt is heated, and the irritation and the health risk are brought. Patent CN109430943a adds water absorbing agent or absorbent cotton water absorbing material in the filter stick, patent CN104449586a adds C 19～C21 alkane loaded expanded graphite or porous silica gel particles in the filter stick, the above materials can reduce the temperature of smoke at the filter tip end, but there is the disadvantage of intercepting smoke, reducing smoke amount and increasing the absorption resistance of the filter stick. Chinese patent CN201510045745 provides a filter tip and a cigarette, the temperature of smoke is reduced by adding a phase change material at the tip of the filter tip, the phase change material is a mixture of hydrated inorganic salt and urea, the application mode is that the phase change material is sprayed on a acetate fiber tip rod or a crystal is placed between two filters, the industry knows that the thermal stability of the hydrated salt is poor in the use process, and the hydrated salt is extremely volatile, so that the enthalpy value is reduced.
Disclosure of Invention
The invention aims to provide a biodegradable filter stick capable of reducing the smoke temperature of cigarettes and a preparation method thereof, and overcomes the defects and shortcomings in the prior art.
In order to achieve the above object, the solution of the present invention is:
On one hand, the invention provides a filter stick with low suction resistance, low filtration and biodegradability, which can reduce the smoke temperature of cigarettes, wherein the filter stick is formed by bonding and solidifying biodegradable particles through a biodegradable adhesive, and the filter stick is bonded to form a netty three-dimensional porous structure, has a void ratio of 40-85%, is used for heating non-combustible cigarettes, and does not bring any peculiar smell to the smoke.
The low-absorption-resistance and high-biodegradation cooling filter stick comprises biodegradable particles and biodegradable adhesive particles.
Optionally, the mass ratio of the components of the filter stick is 5-60% of the weight of the adhesive, 40-95% of the weight of the biodegradable particles and 100% of the sum of the two.
The biodegradable particles may be biodegradable, optionally selected from the group consisting of cellulose acetate having a degree of substitution of 2.2 or less, plant particles, and any combination thereof.
Generally, the substitution degree of industrial cellulose diacetate is about 2.5, and the biodegradation time is long. Reducing the substitution degree of cellulose acetate is a very effective method for improving the biodegradability thereof. When the substitution degree of the cellulose acetate is less than 2.2, the biodegradation speed is greatly improved. Thus, the industrial diacetyl cellulose can be prepared into degradable cellulose acetate with low substitution degree by adopting an acid hydrolysis method, and then the degradable cellulose acetate particles are prepared by adopting a granulation technology such as extrusion spheronization. After the cellulose diacetate is hydrolyzed, the substitution degree is reduced, the polarity is enhanced, and when the cellulose diacetate is used for heating cigarettes, the moisture in the smoke can be adsorbed better due to the high surface polarity. When the high-temperature flue gas contacts with the moisture on the surfaces of the particles, the moisture is heated, so that the moisture on the surfaces of the particles is evaporated, and a large amount of heat is required in the moisture evaporation process, thereby being more beneficial to reducing the temperature of the flue gas. In addition, the cellulose acetate with low substitution degree after hydrolysis has chemical homology with the traditional cellulose diacetate tows, so that the cellulose acetate is used for heating cigarettes, and peculiar smell and miscellaneous gas can not be brought to cigarette smoke.
The plant particles must meet the requirements of safety, degradability, filter rod processing and the like. The edible plant granule comprises millet or puffed millet, corn, scented rice, millet and sorghum. The edible plant particles not only can be degraded in natural environment, but also can emit unique characteristic fragrance of food materials after being bonded with the adhesive at high temperature, and have the functions of enhancing and supplementing fragrance of smoke, thereby improving the comfort of smoking of cigarettes.
The biodegradable particle shape includes spherical, spheroid, pie, flake, ribbon, needle, polygonal, faceted, or random shape.
Optionally, the biodegradable particles have an average diameter in at least one dimension from a lower limit of 50 microns, 100 microns, 150 microns, 200 microns, or 250 microns to an upper limit of 5000 microns, 2000 microns, 1000 microns, 900 microns, or 700 microns.
Optionally, the adhesive particle having biodegradability includes at least one selected from the group consisting of: polylactic acid (PLA), polybutylene succinate (PBS), polybutylene adipate and terephthalate copolymer (PBAT), polyhydroxyalkanoate (PHA), polycaprolactone (PCL), thermoplastic starch polymers, polyvinyl acetate (PVAc), and the like, and further, any combinations of binder particles including these different items may be used.
Alternatively, the adhesive particles may take any shape, including spherical, star-shaped, granular, potato, irregular; the adhesive particles may be any combination of these shaped adhesive particles.
Optionally, the adhesive particle has in at least one dimension: a lower limit of 5 microns, 10 microns, 50 microns, 100 microns, or 150 microns to an average diameter of an upper limit of 500 microns, 400 microns, 300 microns, 250 microns, or 200 microns.
Optionally, the adhesive particle melt flow index is less than or equal to 3.5g/10min.
In another aspect, the present invention provides a method for preparing the filter stick, including:
(1) Continuously introducing a mixed material of biodegradable particles and a biodegradable adhesive into a mold cavity, wherein the weight ratio of the biodegradable adhesive particles to the biodegradable particles is mixed according to the requirements of the porosity and the suction resistance of the final filter rod, and optionally, the mass ratio of the biodegradable particles is 40-95%, and the other components are the biodegradable adhesive particles;
(2) Filling a mold containing a liner paper with a mixture of biodegradable particles and biodegradable adhesive particles, optionally the liner paper may have a grammage of 70-90g and a thickness of 0.08-0.12mm, optionally heating the mixed material to 100-180 ℃ to bond the matrix material at a plurality of contact points, thereby forming a wrapped cylindrical porous mass;
(3) The porous filter rod is then removed from the mould and cooled, and the filter rod is cut into small pieces of the desired length.
Alternatively, the biodegradable particles are 40% to 95%, preferably 67% to 75% by weight;
in yet another aspect, the invention also provides the use of the filter rod described above in heating non-combustible cigarettes.
By adopting the technical scheme, the beneficial effects of the invention include:
1) The cooling filter stick has a stable three-dimensional, through and nonlinear gap porous network structure, is formed by heating, solidifying and forming biodegradable particles and biodegradable adhesive particles, and is internally provided with complex and continuous through holes, and high-temperature smoke can be rapidly dispersed in the gaps of the filter stick after entering the filter stick from one end of the cooling filter stick;
2) The low substitution degree cellulose diacetate has enhanced polarity, and can better adsorb the moisture in the smoke due to the high surface polarity when being used for heating cigarettes. When the high-temperature flue gas contacts with the moisture on the surfaces of the particles, the moisture is heated, so that the moisture on the surfaces of the particles is evaporated, and a large amount of heat is required in the moisture evaporation process, thereby being more beneficial to reducing the temperature of the flue gas.
3) The adhesive particles have extremely low hot melt index, and after the high-temperature flue gas contacts with the particles, the morphology change of the particles is very small, and the inside of the filter stick still maintains an original structure;
4) Because the filter stick presents a through gap structure, the filter stick suction resistance can be controlled by adjusting the sizes of the biodegradable particles and the adhesive particles, the mixing proportion of the biodegradable particles and the adhesive particles and the heating temperature. The filter rod draw resistance can be as low as 0.15mmH2O/mm in length.
5) The material used for the filter stick has good biodegradability, and after the filter stick is used, the filter stick can be completely degraded after a period of time in a natural environment, so that the burden on the environment is avoided, and the filter stick has good economic benefit and environmental benefit.
Drawings
FIG. 1 is a schematic view of an embodiment of a rapid cooling porous filter rod of the present invention containing biodegradable particles.
FIG. 2 is a schematic representation of an embodiment of a ternary composite filter rod comprising a rapid cooling porous filter rod of the present invention.
Fig. 3 is a schematic structural view of an embodiment of a heated cigarette incorporating the rapid cooling porous filter rod of the present invention.
Fig. 4 is a schematic diagram of a smoke temperature test against a heated smoking article structure.
Fig. 5 is a schematic diagram of a heated smoking article construction and smoke temperature test using a rapid cooling filter rod of the present invention.
In the figure: 11-thermocouple detection position; 12-ternary composite filter rod with cellulose diacetate tow; 13-heating the tobacco raw material; 14-electrically heating the body cavity; 15-an electric heating rod; 16-ventilation guide holes; 17-a battery element; 18-a smoking set element; 21-thermocouple detection position; 22-a rapid cooling porous ternary composite filter rod containing biodegradable particles; 23-heating the tobacco material; 24-electrically heating the body cavity; 25-an electric heating rod; 26-ventilation guide holes; 27-a battery element; 28-smoking set element.
Detailed Description
The invention relates to a biodegradable filter stick capable of reducing the temperature of cigarette smoke and a preparation method thereof, and aims to solve the problems that the effect of reducing the temperature of the smoke of the filter stick is not obvious and the biodegradability is poor in the prior art. The filter stick is formed by heating degradable cellulose acetate particles or plant particles and degradable adhesive particles in a die cavity to form contact point bonding, so that the porous cooling filter stick is manufactured. The filter rod is provided with a firm three-dimensional, through and nonlinear gap porous network structure, a complex and continuous through hole channel is formed in the filter rod, high-temperature flue gas can be rapidly dispersed in a gap of the filter rod after entering the filter rod from one end of the cooling filter rod, and compared with the through cooling filter rod, the relative stroke of the high-temperature flue gas in the cooling filter rod is greatly prolonged, so that the obtained cooling effect is better. After the filter stick is used, the filter stick can be completely degraded in natural environment after a period of time, does not cause burden to the environment, and has good economic benefit and environmental benefit.
The invention is further described below with reference to the drawings and examples.
The following percentages (%) are mass percentages unless otherwise indicated. The melt flow index of the biodegradable adhesive particles is 3.5g/10min or less.
The void volume of the porous filter rod is the free space remaining after the space occupied by the degradable cellulose acetate microspheres. Tests have shown that the final density of the porous mass mixture is almost entirely comprised of degradable acetate microspheres, and therefore the binder particles in the porous mass occupy a negligible volume. The void volume is thus calculated hereinafter on the basis of the space remaining after calculation of the degradable cellulose acetate microspheres. To determine void volume, the average of the upper and lower diameters based on particle size was first determined for degradable cellulose acetate microspheres, and then the volume was calculated using the density of the degradable cellulose acetate (assuming spheres based on the average diameter). The void fraction was calculated as follows.
The term "closed pressure drop" as used herein refers to the difference in static pressure between the two ends of a sample when the sample is air flowed through under steady conditions at a volumetric flow rate of 17.5mL/s at the outlet end, and when the sample is completely closed in the measuring device so that air cannot pass through the package. The closed pressure drop has been measured herein according to CORESTA ("the center of tobacco science research collaboration") recommendation 41, published 6 th 2007. A higher closed pressure drop indicates that the smoker must draw on the smoking device with a greater force.
Example 1
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 1, the porous filter rod of the invention is of a porous cylindrical structure, the closed suction resistance of the filter rod with the circumference 21.96mm is 65mmH 2 O (120 mm in length), and the void ratio is 77%.
(2) Structural part of the filter stick of the invention
Further, the porous filter stick is a cylindrical structure formed by physically binding polymer biodegradable adhesive particles and cellulose acetate particles with substitution degree of 2.08 wrapped by molding paper.
The porous filter stick is prepared from 85% of cellulose acetate particles with the particle size of 16-24 meshes and substitution degree of 2.08 and 15% of polylactic acid adhesive with the average particle size of 125 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Preparation method of particles used in filter stick structure of the invention
The biodegradable cellulose acetate particle is prepared from cellulose acetate with substitution degree of 2.08 by an extrusion spheronization method.
(4) Preparation method of particles used in filter stick structure of the invention
15 Kg of industrial cellulose diacetate with a substitution degree of 2.5 was dissolved in 92 kg of aqueous acetic acid solution (acetic acid to water mass ratio of 70:30) to prepare a homogeneous slurry, and heated to 60 ℃. Then, 2.3 liters of acetic acid solution containing 630 g of sulfuric acid was added, hydrolysis was carried out at 60℃for 2.5 to 8 hours, and 10.8 liters of aqueous solution containing 1500 g of magnesium acetate was further added to the above mixture to neutralize sulfuric acid to terminate the reaction. Then 173 liters of deionized water is added into the mixture after the reaction to precipitate cellulose acetate, 43 liters of deionized water is added, and stirring is continued for 45 minutes to harden the cellulose acetate. And then separating cellulose acetate by adopting a filtering mode, removing acetic acid by washing, finally performing heat stabilization treatment by using an aqueous solution containing calcium acetate, and drying the filtered cellulose acetate at 80 ℃. The degree of substitution of the cellulose acetate hydrolyzed by the above process was tested using NMR analysis techniques.
Table 1: degree of substitution of cellulose acetate under acidic hydrolysis conditions at different hydrolysis times
| Sequence number | Hydrolysis time (h) | Degree of substitution of cellulose acetate | Cellulose acetate intrinsic viscosity, dL/g |
| 1 | 2.5 | 2.20 | 1.61 |
| 2 | 5 | 2.08 | 1.59 |
| 3 | 8 | 1.84 | 1.60 |
The cellulose acetate with the substitution degree of 2.08 prepared by the process is ground by a wet method to prepare powder with the average particle size of 45 microns. Weighing 0.7 kg of the ground cellulose acetate powder sample and 0.3 kg of pregelatinized starch respectively, adding 1.0 kg of deionized water solution, and fully stirring and uniformly mixing on a laboratory wet mixer to obtain a wet material. The soft wet material prepared above was subjected to wet extrusion granulation on an E-50 wet extruder (distribution plate aperture 1.0 mm) to obtain a cylindrical bar. The extruder feed speed was 23rpm and the extrusion speed was 26rpm. The cylindrical bar is formed by rounding on an S-250 rounding machine to obtain wet spherical particles. The rounding conditions are as follows: the spheronizer was operated at 600rpm for 1.5 minutes and then at 500rpm for 3 minutes. The wet spherical particles were fluidized and dried at 65℃for 1 to 2 hours, and the water was removed to obtain dried particles. Sieving with 16 mesh and 24 mesh sieve to obtain biodegradable cellulose acetate granule with required particle size.
(5) Method for preparing porous filter rod of the invention by using the particles
The porous filter rod was made from polylactic acid from Nature works Inc. of U.S. and degradable cellulose acetate particles prepared by the foregoing method.
1) Mixing 15% by weight of PLA resin powder (prepared by freeze-milling PLA resin particles having an average particle diameter of 125 μm) and 85% by weight of degradable cellulose acetate spherical particles prepared by the foregoing method;
2) Filling the mold with the mixture without applying pressure to the mixture;
3) The mold was then heated to 140 ℃ and held for 10 minutes;
4) Then taking out the porous filter rod from the mould, cooling, and wrapping the filter rod by using forming paper with gram weight of 32g/m, thickness of 0.09mm and air permeability of 10000 CU;
5) The filter rod is cut into small segments of equal length, such as 120mm.
The porous filter rod had a percent porosity of 77%, a 21.96mm circumference, a 65mmH2O (120 mm length) closed draw resistance.
(6) Application of porous filter stick
The porous filter rod prepared as described above was cut into 18mm small sections, which had the same circumference as the porous filter rod, and the length was 8mm cellulose acetate tow hollow tube and 7mm cellulose acetate filter rod, respectively, were manufactured by a filter rod compounding process to obtain a ternary composite filter rod, wherein the middle section of the ternary composite filter rod was based on the rapid cooling porous filter rod 22 (see fig. 2) containing biodegradable particles according to the present invention. And then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 21.96 mm) (see figure 3).
Simulated smoking was performed according to the cigarette smoking model specified in national standard GB/T19609-2004, using the canadian deep drawing pattern (HCI) with smoking parameters of: the aspiration capacity was 55mL/L, the aspiration frequency was 30s, and the aspiration duration was 2s. The temperature of the center of the cigarette filter rod at a distance of 5mm from the mouth end at the time of cigarette smoking was detected using a thermocouple temperature detector (see thermocouple detection position 21 in fig. 5). Smoke evaluation is carried out according to the sensory technical requirements of GB5606.4-2005 cigarettes.
The comparative filter rod adopts 22.0Y/31500 diacetate fiber bundles, and is processed by a filter rod forming machine to prepare the acetate fiber base rod with the length of 108mm, the circumference of 22.08mm and the suction resistance of 61.3mmH 2 O. The base rod is cut into filter rods with the length of 18mm, 18mm gathering PLA films in IQOS cigarette filter rods are replaced, a heating non-burning control cigarette containing cellulose acetate filter rods is manufactured, and the same smoking and smoke temperature testing method (see figure 4) as the cigarette containing the porous filter rods is adopted. The test results are shown in Table 2.
Example 2
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 21.80mm, the closed suction resistance of the filter rod is 56mmH 2 O (120 mm in length), and the void ratio is 79.3%.
(2) Structural part of the filter stick of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles and cellulose acetate particles with substitution degree of 2.2 wrapped by forming paper.
The porous filter stick is prepared from 75% of biodegradable cellulose acetate particles with the particle size of 16-24 meshes and substitution degree of 2.2 and 25% of PBAT/PCL (polybutylene adipate and polybutylene terephthalate copolymer and polycaprolactone) blending adhesive with the average particle size of 118 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Preparation method of particles used in filter stick structure of the invention
Biodegradable cellulose acetate particles were prepared as in example 1 (except that the degree of substitution of cellulose acetate was 2.2)
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contained 25% PBAT/PCL (PCL content 1% based on PBAT mass) and 75% biodegradable cellulose acetate particles prepared as described above. The porous filter rod had a percent porosity of 79.3% and a closed draw resistance of 56mmH 2 O (120 mm length). After the PBAT/PCL cryo-milled powder (average particle diameter 118 μm) and the biodegradable cellulose acetate particles prepared above were mixed, the mold was filled with the mixture without applying pressure to the mixture. The mold was then heated to 145 ℃ and held for 10 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on biodegradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. Then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 21.80 mm) (see figure 3). The smoke cooling performance evaluation and smoke sensory evaluation method of the porous cooling filter stick are the same as those of example 1. The results are shown in Table 2.
Example 3
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 21.92mm, the closed suction resistance of the filter rod is 49mmH 2 O (the length of 120 mm), and the void ratio is 80.1%.
(2) Structural part of the filter stick structure of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles and cellulose acetate particles with substitution degree of 1.84 wrapped by molding paper.
The porous filter stick is prepared from 70% of spherical cellulose acetate particles with the particle size of 16-24 meshes and the biodegradable substitution degree of 1.84 and 30% of PLA/PBS/PVAC blending adhesive with the average particle size of 100 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Method for preparing particles used in the filter rod structure of the invention
Biodegradable cellulose acetate particles were prepared as in example 1 (except that the degree of substitution of cellulose acetate was 1.84)
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contained 30% pla/PBS/PVAC blended binder particles and 70% biodegradable cellulose acetate particles prepared as described above. The porous filter rod had a percent porosity of 80.1% and a closed draw resistance of 49mmH 2 O (120 mm length). PLA/PBS/PVAC blended freeze-milled powder (PLA, PBS and polyvinyl acetate PVAC were melt-blended at a mass ratio of 45:35:20, and extruded particles were freeze-milled to obtain binder powder having an average particle diameter of 100 μm) and the above-prepared degradable cellulose acetate particles were mixed, and then the mold was filled with the mixture without applying pressure to the mixture. The mold was then heated to 135 ℃ and held for 30 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on the degradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. Then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 21.92 mm) (see figure 3). A smoke cooling performance evaluation method of a porous cooling filter stick and smoke sensory evaluation are the same as in example 1. The results are shown in Table 2.
Example 4
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 22.08mm, the filter rod is closed, the suction resistance is 42mmH 2 O (120 mm in length), and the void ratio is 76.8%.
(2) Structural part of the filter stick of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles and edible plant millet particles which are wrapped by forming paper.
The porous filter stick is prepared from 75% of biodegradable edible millet particles with the particle size of 12-30 meshes and 25% of PHA/PLA/PVAC blending adhesive with the average particle size of 132 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Method for preparing particles used in the filter rod structure of the invention
The Liaoning Chaoyang dehulled millet with the trademark "Hongshan green beads" is adopted, and the millet with the required grain size of 12-30 meshes is obtained through sieving.
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contained 25% pha/PLA/PVAC blended binder particles and 75% biodegradable millet particles prepared as described above. The porous filter rod had a percent porosity of 76.8% and a closed draw resistance of 42mmH 2 O (120 mm length). PHA/PLA/PVAC blended freeze-milled powder (polyhydroxyalkanoate PHA, PLA and polyvinyl acetate PVAC are melt-blended according to a mass ratio of 40:30:30, extruded particles are freeze-milled to obtain binder powder with an average particle diameter of 132 μm), and the prepared degradable cellulose acetate particles are mixed, and then the mixture is filled into a mold without applying pressure to the mixture. The mold was then heated to 120 ℃ and held for 15 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on the degradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. And then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 22.08 mm) (see figure 3). A smoke cooling performance evaluation method of a porous cooling filter stick and smoke sensory evaluation are the same as in example 1. The results are shown in Table 2.
Example 5
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 22.01mm, the filter rod is closed, the suction resistance is 47mmH 2 O (the length of 120 mm), and the void ratio is 78.2%.
(2) Structural part of the filter stick of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles and corn particles which are wrapped by forming paper.
The porous filter stick is prepared from 70% of biodegradable corn particles with the particle size of 16-24 meshes and 30% of PLA/starch blending adhesive with the average particle size of 124 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Method for preparing particles used in the filter rod structure of the invention
The corn is crushed by a machine and is sieved to obtain the corn particles with the particle size of 16-24 meshes.
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contained 30% pla/starch blended binder particles and 75% biodegradable corn particles prepared as described above. The porous filter rod had a percent porosity of 78.2% and a closed draw resistance of 47mmH 2 O (120 mm length). PLA/starch blending cryo-milled powder (PLA and starch were melt-blended at a mass ratio of 80:20, and extruded particles were cryo-milled to give a binder powder having an average particle diameter of 124 μm) was mixed with the above-prepared degradable corn particles, and then the mold was filled with the mixture without applying pressure thereto. The mold was then heated to 140 ℃ and held for 15 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on the degradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. Then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 22.01 mm) (see figure 3). A smoke cooling performance evaluation method of a porous cooling filter stick and smoke sensory evaluation are the same as in example 1. The results are shown in Table 2.
Example 6
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 21.75mm, the filter rod is sealed and sucked with 85mmH 2 O (120 mm in length), and the void ratio is 43%.
(2) Structural part of the filter stick of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles and cellulose acetate particles with substitution degree of 2.2 wrapped by forming paper.
The porous filter stick is prepared from 95% of biodegradable cellulose acetate particles with the particle size of 20-40 meshes, substitution degree of 2.2 and 5% of PBAT/PCL (polybutylene adipate and polybutylene terephthalate copolymer and polycaprolactone) blending adhesive with the average particle size of 85 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Preparation method of particles used in filter stick structure of the invention
Biodegradable cellulose acetate pellets were prepared in the same manner as in example 1 (except that the degree of substitution of cellulose acetate was 2.2 and the particle size of the pellets was 20 to 40 mesh).
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contained 5% PBAT/PCL (PCL content 1% based on PBAT mass) and 95% biodegradable cellulose acetate particles prepared as described above. The porous filter rod had a percent porosity of 43% and a closed draw resistance of 85mmH 2 O (120 mm length). After the PBAT/PCL cryo-milled powder (average particle diameter 85 μm) and the biodegradable cellulose acetate particles prepared above were mixed, the mold was filled with the mixture without applying pressure to the mixture. The mold was then heated to 145 ℃ and held for 10 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on biodegradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. Then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 21.80 mm) (see figure 3). The smoke cooling performance evaluation and smoke sensory evaluation method of the porous cooling filter stick are the same as those of example 1. The results are shown in Table 2.
Example 7
(1) Integral aspects of the filter rod structure of the invention
As shown in FIG. 2, the porous filter rod of the invention is of a porous cylindrical structure, the circumference of the filter rod is 21.89mm, the filter rod is closed, the suction resistance is 18mmH 2 O (the length of 120 mm), and the void ratio is 83.1%.
(2) Structural part of the filter stick of the invention
Furthermore, the porous filter stick is a cylindrical structure formed by physically binding polymer degradable adhesive particles, cellulose acetate with low substitution degree and edible plant millet particles by wrapping molding paper.
The porous filter stick is prepared from 70% of mixed particles of cellulose acetate with the particle size of 10-20 meshes and substitution degree of 2.08 and edible plant millet, and 30% of PHA/PLA/PVAC blend adhesive with the average particle size of 104 microns. The wrapping material is formed paper with gram weight of 32g/m 2, thickness of 0.09mm and air permeability of 10000 CU.
(3) Method for preparing particles used in the filter rod structure of the invention
The Liaoning Chaoyang dehulled millet with the trademark "Hongshan green beads" is adopted, and the millet with the required grain size of 10-20 meshes is obtained through sieving. Biodegradable cellulose acetate particles were prepared in the same manner as in example 1 (except that the cellulose acetate particles had a particle size of 10-20 mesh)
(4) Method for preparing porous filter rod with certain size and porosity by using particles
The porous filter rod contains 30% PHA/PLA/PVAC blended binder particles and 70% biodegradable millet prepared as described above and low substitution cellulose acetate particles. The porous filter rod had a percent porosity of 83.1% and a closed draw resistance of 18mmH 2 O (120 mm length). PHA/PLA/PVAC blended freeze-milled powder (polyhydroxyalkanoate PHA, PLA and polyvinyl acetate PVAC were melt-blended at a mass ratio of 40:30:30, and extruded particles were freeze-milled to obtain binder powder having an average particle diameter of 104 μm), and the prepared degradable particles were mixed, and then the mold was filled with the mixture without applying pressure to the mixture. The mold was then heated to 120 ℃ and held for 15 minutes. The porous filter rod was then removed from the mould and cooled and wrapped with a plug wrap having a grammage of 32g/m 2, a thickness of 0.09mm and an air permeability of 10000 CU. The filter rod is cut into small segments of equal length, such as 120mm.
(5) Application of porous filter stick with size and porosity
The prepared rapid cooling porous filter rod based on the degradable particles is cut into 18mm small sections, the sections have the same circumference as the porous filter rod, and the cellulose acetate tow hollow tube with the length of 8mm and the cellulose acetate filter rod with the length of 7mm are respectively manufactured into a ternary composite filter rod through a filter rod composite process, wherein the middle section of the ternary composite filter rod is the rapid cooling porous filter rod 22 (see figure 2) based on the biodegradable particles. And then preparing the novel heating non-combustible cigarette by a cigarette rubbing process and a 12mm length tobacco material aerosol atomization unit (circumference 22.08 mm) (see figure 3). A smoke cooling performance evaluation method of a porous cooling filter stick and smoke sensory evaluation are the same as in example 1. The results are shown in Table 2.
TABLE 2 mainstream smoke temperature test results
The filter sticks prepared in examples 1-7 above were compared for degradation performance testing using conventional tobacco cellulose diacetate tow filter sticks as control samples. The test results are shown in Table 3. The filter stick degradation performance test adopts a weight method. The weighed filter rods (approximately 3.9-4.1 g) were placed in a defined amount of water (150 g) and magnetically stirred at room temperature (stirring speed 120 rpm), after 60 days, filtered and dried, and the residual filter rods were tested for quality. The higher the weight loss rate, the better the degradation performance of the filter rod.
Table 3 results of different filter rod degradation tests
The foregoing description of the embodiments is provided to facilitate the understanding and appreciation of the invention by those skilled in the art. It will be apparent to those skilled in the art that various modifications can be readily made to these teachings and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the invention is not limited to the above description and the description of the embodiments, and those skilled in the art, based on the disclosure of the invention, should make improvements and modifications without departing from the scope of the invention.
Claims (16)
1. The biodegradable filter stick capable of reducing the smoke temperature of cigarettes is characterized in that the filter stick is formed by bonding and solidifying biodegradable particles through a biodegradable adhesive, and a netty three-dimensional porous structure is formed inside the filter stick.
2. A filter rod according to claim 1, wherein the filter rod has a void fraction of 40-85%.
3. The filter rod of claim 1, wherein the filter rod comprises biodegradable particles, biodegradable binder particles, and a wrapper; the biodegradable adhesive particles and the biodegradable adhesive particles, the biodegradable adhesive particles and the biodegradable particles, and the contact points formed between the biodegradable particles and the biodegradable particles are physically bonded at a plurality of places, the wrapping material wraps the outside to form the filter rod with a porous structure, and the mass of the contained biodegradable particles is 40-95% of that of the filter rod according to the mass percentage.
4. The filter rod of claim 1, wherein the biodegradable particles are selected from the group consisting of cellulose acetate having a degree of substitution of 2.2 or less, plant particles, and any combination thereof; optionally, the cellulose acetate with the substitution degree less than or equal to 2.2 is prepared by acid hydrolysis of industrial diacetyl cellulose; optionally, the plant particles include millet or puffed millet, corn, scented rice, millet, and sorghum.
5. The filter rod of claim 1, wherein the biodegradable particle shape comprises a sphere, spheroid, cake, flake, ribbon, needle, polygonal, faceted, or random shape.
6. The filter rod of claim 1, wherein the biodegradable particles have an average diameter in at least one dimension from a lower limit of 50 microns, 100 microns, 150 microns, 200 microns, or 250 microns to an upper limit of 5000 microns, 2000 microns, 1000 microns, 900 microns, or 700 microns.
7. The filter rod of claim 1, wherein the biodegradable binder comprises: polylactic acid, polybutylene succinate, polybutylene adipate and polybutylene terephthalate copolymer, polyhydroxyalkanoate, polycaprolactone, thermoplastic starch polymer and polyvinyl acetate, and any combination of one or more of the above.
8. A filter rod according to claim 3, wherein the shape of the biodegradable adhesive particles comprises spheres, stars, granules, potatoes, irregular shapes and any combination thereof.
9. The filter rod of claim 1, wherein the biodegradable binder particles have in at least one dimension: a lower limit of 5 microns, 10 microns, 50 microns, 100 microns, or 150 microns to an average diameter of an upper limit of 500 microns, 400 microns, 300 microns, 250 microns, or 200 microns.
10. The filter rod of claim 1, wherein the biodegradable binder particles have a melt flow index of 3.5g/10min or less.
11. A method of making a filter rod as claimed in claims 1 to 10, comprising the steps of:
Continuously introducing a mixed material of biodegradable particles and a biodegradable adhesive into a die cavity, wherein the weight ratio of the biodegradable adhesive particles to the biodegradable particles is mixed according to the requirements of the porosity and the suction resistance of the final filter rod;
A step (2) of filling a mold containing a lining paper with a biodegradable particle and a biodegradable adhesive mixture, and heating the mixed material so as to bond the matrix material at a plurality of contact points, thereby forming a wrapped cylindrical porous substance;
Step (3) the porous filter rod is then removed from the mould and cooled, and the filter rod is cut into small pieces of the required length.
12. The method of producing a filter rod according to claim 11, wherein in the step (1), the mass ratio of the biodegradable particles is 40% to 95%, and the balance is the biodegradable binder.
13. The method of producing a filter rod according to claim 11, wherein in the step (2), the liner paper has a grammage of 70 to 90g and a thickness of 0.08 to 0.12mm.
14. The method of producing a filter rod according to claim 11, wherein in step (2), the mixed material is heated to 100 ℃ to 180 ℃.
15. A method of preparing a filter rod according to claim 12, wherein the biodegradable particles are present in a mass ratio of 55% to 85%, preferably 67% to 75%.
16. Use of a filter rod according to any one of claims 1 to 10 for heating non-combustible cigarettes.
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