CN109700070B - Particle capable of reducing cigarette smoke temperature and preparation method and application thereof - Google Patents
Particle capable of reducing cigarette smoke temperature and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of cigarette auxiliary materials, and relates to particles capable of reducing the temperature of main stream smoke of cigarettes, and a preparation method and application thereof. The particles are inactive particles or active particles or inactive particles of the outer coating layer. The thickness of the outer film layer of the inactive particles is 0-0.2mm, and the outer film layer accounts for 0-50% of the mass of the whole particles; the thickness of the outer coating layer of the active particles is 0.001-0.2mm, and the outer coating layer accounts for 0.001-50% of the mass of the whole particles. The inactive particles are less than 3.0mg/cm for absorbing nicotine in the smoke aerosol 3 The particles of (a); the inactive particles include inorganic particles or organic particles. The preparation method is simple, industrialization and industrialization are easy to realize, the particles are easy to add into the cigarette filter stick, the surfaces of the particles are compact, leakage does not exist, and the temperature of cigarette smoke can be greatly reduced by adding the particles into the cigarette filter stick.
Description
Technical Field
The invention belongs to the technical field of cigarette auxiliary materials, and relates to particles capable of reducing the temperature of main stream smoke of cigarettes as well as a preparation method and application thereof.
Background
Cigarettes are a special consumer product which is consumed in the form of smoke enjoyed by smoking. The cigarette smoke refers to a highly concentrated and constantly changing aerosol system generated by the complicated combustion process of the cut tobacco in the ignited cigarette. Cigarette combustion has two forms: one is combustion at suction, called smoking; the other is combustion in the suction gap, called smoldering (also called smoldering).
Smoke drawn from the filter end of a cigarette during smoking is called Mainstream Smoke (MS), and Smoke released from the combustion end in the smoking gap and diffused through the cigarette paper directly into the environment is called Sidestream Smoke (SS). During cigarette smoking, heat generated by the cigarette combustion cone is carried by the mainstream smoke to the filter, and as the cigarette smoking progresses, the temperature of the smoke passing through the filter increases gradually. The previous research results show that the highest smoke temperature at the filter tip can reach 70-80 ℃ when the suction is close to the first 2-3 mouths of suction, and the highest smoke temperature at the filter tip can even reach about 100 ℃ in the deep suction mode. Generally, higher smoke temperature can cause smoke irritation and burning sensation, and reduce the smoking comfort of the cigarette. In order to control the smoke temperature of the cigarette, cigarette design developers usually reduce the smoke temperature by means of lengthening the filter stick, improving the suction resistance of the filter stick, increasing the ventilation degree of the filter stick and the like. However, these techniques have problems such as reduction of smoke concentration of cigarettes and insufficient smoothness of smoking, and thus have great limitations in use.
In recent years, novel tobacco products are rapidly developed, novel products such as buccal cigarettes, chewing cigarettes, electronic atomization cigarettes and heating non-combustion tobacco products are widely available on the market, and compared with traditional cigarettes, the harmfulness of the products is remarkably reduced, so that the products are accepted by consumers and occupy certain market share in the international tobacco market. The heating non-combustible tobacco product is the product which is closest to the traditional cigarette in smoking quality and smoking habit, and has good development prospect.
The technology for heating the non-combustible tobacco is to heat the tobacco at 200-400 ℃ through a smoldering carbon rod or a heating electronic element, so that the tobacco is not combusted, but the tobacco components can still be distilled and cracked, and the smoke is released. Compared with the traditional tobacco products which burn, the cigarette which is not burnt when being heated has no combustion, so that the released harmful ingredients are obviously reduced compared with the traditional cigarette, and the product safety is obviously improved under the condition of approximate smoking quality. Therefore, the technology has good development prospect and market potential. However, the cigarette which is not heated and combusted releases less smoke than the traditional cigarette because the tobacco raw material is not combusted, and if the smoke temperature is reduced by adopting the technical means of increasing filtration and ventilation dilution, the smoke volume of the product can be further reduced, thereby influencing the smoking feeling of the product. Therefore, the reduction of the smoke temperature is a key technology for heating the non-combustible cigarettes.
Chinese patent CN104203015A describes that philips morris corporation in the united states uses a polylactic acid film as a cooling material for heating non-combustible cigarettes. The above-mentioned material for reducing the smoke temperature mainly absorbs heat through the glass transition of polylactic acid, i.e. the transition from the glassy state to the high elastic state, thereby reducing the smoke temperature of the smoking article. However, the problem is that when the polylactic acid undergoes glass transition, the polylactic acid undergoes melting or fusion bonding, so that the most polymer material at the end of the rod which is first contacted with the flue gas and is cooled can immediately undergo serious adhesion and collapse to block the pore channels, so that the flue gas cannot smoothly flow through the interior of the folded polymer, the cooling surface area is reduced, and the temperature of the flue gas is too high.
In view of the above technical requirements and the defects of the prior art, the present inventors have developed a technique for reducing the smoke temperature of cigarettes and novel tobacco products based on the summary of the prior art.
Disclosure of Invention
The invention aims to provide particles capable of reducing the smoke temperature of cigarettes and a preparation method and application thereof. In order to achieve the purpose, the invention adopts the technical scheme that:
a granule for reducing smoke temperature of cigarette.
Further, the particles are inactive particles or active particles or inactive particles of the outer coating layer.
Optionally, the inactive particles can also be coated with a film layer, the thickness of the coating layer is 0-0.2mm, and the coating layer accounts for 0-50% of the total mass of the particles; obviously, when the thickness of the outer coating layer or the mass of the whole particle is 0, the inactive particle is not coated with the outer coating layer; the active particles need non-activation treatment, and the thickness of the outer coating layer is 0.001-0.2mm and accounts for 0.001-50% of the mass of the whole particles.
Optionally, the inactive particles are less than 3.0mg/cm for nicotine adsorption in the smoke aerosol 3 The particles of (4).
Optionally, the inactive particles comprise inorganic particles or organic particles.
Optionally, the inorganic particles comprise one or more of alumina, zirconia, calcium carbonate spheres, glass beads, silica, iron, copper, aluminum, gold, platinum, magnesium silicate spheres, or calcium sulfate.
Optionally, the organic particle comprises one or more of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, microcrystalline cellulose, sucrose powder, dextrin, lactose, powdered sugar, glucose, mannitol, starch, methyl cellulose, ethyl cellulose, polylactic acid, polyethylene, polypropylene, polyhydroxybutyrate, poly-epsilon-caprolactone, polyglycolic acid, polyhydroxyalkanoate, or a starch-based thermoplastic resin.
Optionally, the active particles are nicotine in aerosol to smokeAdsorption is more than or equal to 3.0mg/cm 3 The particles of (1).
Optionally, the active particles comprise one or more of molecular sieves, activated carbon, diatomaceous earth, zeolites, perlite, ceramics, sepiolite, fuller's earth, ion exchange resins.
Optionally, the overcoat layer is a film-forming material.
Optionally, the film-forming material includes one or more of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, ethylcellulose, polyvinylpyrrolidone, polyvinyl acetal diethylamine acetate, styrene maleic acid copolymer, styrene-vinylpyridine copolymer, cellulose acetate phthalate, hydroxypropylmethylcellulose phthalate, cellulose acetate/polyethylene glycol, methylcellulose/polyethylene glycol, carboxymethylcellulose/polyethylene glycol, hydroxypropylmethylcellulose/polyethylene glycol, ethylcellulose/polyethylene glycol, acrylic resin/polyethylene glycol, or polylactic acid.
Optionally, the particle shape comprises one or more of a sphere, a spheroid, a pie, a flake, a ribbon, an acicular, a polygonal shape, a faceted shape, or a random shape.
Optionally, the particles have an average diameter in at least one dimension of 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.
The preparation method of the particle capable of reducing the smoke temperature of the cigarette comprises the following steps:
(1) mixing the active/inactive powder with the binder solution to prepare a wet material;
(2) extruding and cutting the wet material obtained in the step (1) into smooth and compact cylindrical strips with the same diameter by adopting a wet extrusion granulation process, and carrying out rounding molding on the prepared cylindrical strips in a rounding machine to obtain initial wet granules;
(3) the initial wet granulation is dried to remove water and obtain active/inactive granulation.
Optionally, the binder in step (1) includes one or more of hydroxypropyl methylcellulose aqueous solution, pregelatinized starch aqueous solution, or sodium carboxymethyl cellulose aqueous solution.
Optionally, the concentration of the hydroxypropyl methylcellulose aqueous solution or the pregelatinized starch aqueous solution is 8-12%.
Optionally, the mass ratio of the binder to the powder in step (1) is 1.0-1.2: 1.
Optionally, the rotary extrusion granulator in step (2) is fed at a speed of 23-25rpm and extruded at a speed of 25-30 rpm.
Optionally, the spheronizer in step (2) is operated at 600-700rpm for 1-2 minutes, and then decelerated at 450-500rpm for another 3-4 minutes.
The preparation method of the particles of the outer coating layer capable of reducing the smoke temperature of the cigarettes comprises the following steps:
(1) coating the surface of the particles with coating liquid by a fluidized bed coating method at a certain air temperature and atomization pressure to form a solid-solid composite phase change coating film layer to obtain initial wet particles;
(2) heating and drying to remove the solvent on the surfaces of the initial wet particles to obtain initial particles;
(3) and screening to obtain the coated particles.
Optionally, the coating solution in step (1) is one or more of a water-soluble coating solution, an ethanol coating solution or an acetone coating solution.
Optionally, the water-soluble coating solution comprises more than one of hydroxypropyl methylcellulose/polyethylene glycol aqueous solution, carboxymethyl cellulose/polyethylene glycol aqueous solution or acrylic resin/polyethylene glycol aqueous solution; the solvent is water; the molecular weight of the polyethylene glycol is 1000-20000.
Optionally, the mass concentration of the water-soluble coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
Optionally, the ethanol coating solution comprises an ethyl cellulose/polyethylene glycol ethanol solution; the solvent is 95% ethanol; the polyethylene glycol has a molecular weight of 1000-.
Optionally, the mass concentration of the ethanol coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
Optionally, the acetone coating solution comprises more than one of a cellulose diacetate/polyethylene glycol acetone solution or a cellulose acetate butyrate/polyethylene glycol acetone solution; the solvent is acetone; the molecular weight of the polyethylene glycol is 1000-20000.
Optionally, the mass concentration of the acetone coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
Optionally, the coating film layer in the step (1) accounts for 0-50% of the mass of the whole granule.
Optionally, the inlet air temperature of the fluidized bed in the step (1) is 40-60 ℃; the material temperature is 30-45 ℃; the diameter of the spray nozzle of the spray gun is 1.0 mm; the atomization pressure is 0.15-0.20 MPa; the flow rate of the pump liquid of the peristaltic pump is 5-15 r/min.
The application of the particles capable of reducing the temperature of the main stream smoke of the cigarette in the cigarette filter stick.
The technical scheme of the invention is further explained from another angle as follows:
the invention relates to a particle capable of reducing the smoke temperature of cigarettes, which is an inactive particle or an active particle coated film layer.
Particle shapes include spherical, spheroidal, pie, flake, ribbon, needle, polygonal (e.g., cubic), random (e.g., crushed stone), faceted (e.g., crystal) or any mixture.
The particles may have an average diameter in at least one dimension of from a lower limit of 50 microns, 100 microns, 150 microns, 200 microns, 250 microns to an upper limit of 5000 microns, 2000 microns, 1000 microns, 900 microns, 700 microns. Wherein the average diameter may range from any lower limit to any upper limit and encompass any subset thereof.
The active particles may be any material suitable for enhancing the flow of smoke therethrough. The term "adapted to enhance the flow of smoke" meansAny material capable of removing, reducing or adding components to the flue gas stream. Generally, the active particles have a nicotine absorption of 3.0mg/cm or more in the smoke aerosol 3 . Otherwise, the particles are inactive particles. Active particles have been widely used in the field of tobacco filter sticks, and the main function of the active particles is to remove harmful substances, such as tar, phenol and the like, generated in the combustion process of tobacco. The heating non-combustible smoke contains less harmful ingredients, and the active particles have stronger adsorption capacity to nicotine, so the heating non-combustible smoke is not suitable for being directly used for heating filter sticks of the non-combustible smoke. If the active particles are used in the field of heating non-combustible smoke, the surfaces of the active particles need to be subjected to non-activation treatment. Non-activating treatments include a wide variety of methods such as surface corona discharge treatment, plasma modification, flame treatment, chemical modification, radiation modification, photochemical modification, mechanochemical modification, coupling agent modification, and the like, one of which is coating of the particle surface. Such as film coating, spraying, dipping, and the like.
The active particles comprise more than one of molecular sieve, active carbon, diatomite, zeolite, perlite, ceramic, sepiolite, bleaching earth and ion exchange resin.
Inactive particles include organic or inorganic particles. The inorganic particles include alumina, zirconia, calcium carbonate spheres, glass beads, silica, iron, copper, aluminum, gold, platinum, magnesium silicate spheres, or calcium sulfate. The organic particles include at least one of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, microcrystalline cellulose, sucrose powder, dextrin, lactose, powdered sugar, glucose, mannitol, starch, methyl cellulose, ethyl cellulose, polylactic acid, polyethylene, polypropylene, polyhydroxybutyrate, poly-epsilon-caprolactone, polyglycolic acid, polyhydroxyalkanoate, and starch-based thermoplastic resin.
The outer layer film of the particles has the effects of cooling the smoke, covering the smell of the inner layer particles and preventing the inner layer particles from adsorbing smoke aerosol to cause insufficient smoke. The outer film layer is prepared by fluidized bed coating. The coating solution contains high molecular materials with good film-forming property, such as more than one of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, hydroxypropyl cellulose, hydroxypropyl methylcellulose, ethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol diethylamine acetate, styrene maleic acid copolymer, styrene-vinylpyridine copolymer, phthalic acid cellulose acetate, phthalic acid cavity propyl methylcellulose, cellulose acetate/polyethylene glycol, methylcellulose/polyethylene glycol, carboxymethyl cellulose/polyethylene glycol, hydroxypropyl methylcellulose/polyethylene glycol, ethyl cellulose/polyethylene glycol, acrylic resin/polyethylene glycol or polylactic acid. In the coating process, the film coating is formed by film forming for multiple times, and then the layer films are overlapped and combined. The film layer has the thickness of 0.001-0.2 micron and has very good compactness and moisture resistance, so that the smoke aerosol with the particle size of 0.3-0.5 micron can be prevented from permeating into the inner layer of the particles, and the absorption effect of the inner layer material on the smoke aerosol is prevented. And the coating film layer is compact, and the smell emitted by the inner layer material can be covered, so that the influence on the smoking feeling of consumers caused by offensive odor brought to the smoke is avoided. After the flue gas aerosol passes through the cooling particles, if the film layer material is a phase-change material, the temperature of the flue gas is cooled due to the fact that phase change or specific heat fusion is increased to absorb heat, water in the aerosol is condensed on the surfaces of the particles, and due to compactness of the film layer, condensed water cannot penetrate into the particles, so that the condensed water deposited on the surfaces of the particles can adsorb phenol in the aerosol, and the rejection rate of the phenol is improved.
A method for preparing active or inactive particles capable of reducing the smoke temperature of cigarettes comprises the following steps:
(1) mixing the active/inactive powder with the binder solution to prepare a wet material;
(2) extruding and cutting the wet material obtained in the step (1) into smooth and compact cylindrical strips with the same diameter by adopting a wet extrusion granulation process, and carrying out rounding molding on the prepared cylindrical strips in a rounding machine to obtain initial wet granules;
(3) the initial wet granulation is dried to remove water and obtain active/inactive granulation.
The adhesive in the step (1) comprises more than one of hydroxypropyl methylcellulose aqueous solution, pregelatinized starch aqueous solution or sodium carboxymethyl cellulose aqueous solution.
The concentration of the hydroxypropyl methylcellulose aqueous solution or the pregelatinized starch aqueous solution is 8-12%.
The mass ratio of the adhesive to the powder in the step (1) is 1.0-1.2: 1.
the rotary extrusion granulator in step (2) is fed at a speed of 23-25rpm and extruded at a speed of 25-30 rpm.
The rounder in the step (2) works at 600-700rpm for 1-2 minutes, and then works at 450-500rpm for 3-4 minutes after deceleration.
A preparation method of active particle outer coating layer particles capable of reducing cigarette smoke temperature comprises the following steps:
(1) coating liquid on the surfaces of the active particles by a fluidized bed coating method at a certain air temperature and under an atomization pressure to form a solid-solid composite phase change coating film layer so as to obtain initial wet particles;
(2) heating and drying to remove the solvent on the surfaces of the initial wet particles to obtain initial particles;
(3) and screening to obtain the coated particles.
The coating liquid in the step (1) is more than one of water-soluble coating liquid, ethanol coating liquid or acetone coating liquid.
The water-soluble coating solution comprises more than one of hydroxypropyl methylcellulose/polyethylene glycol aqueous solution, carboxymethyl cellulose/polyethylene glycol aqueous solution or acrylic resin/polyethylene glycol aqueous solution; the solvent is water; the molecular weight of the polyethylene glycol is 1000-20000.
The mass concentration of the water-soluble coating liquid is 3.5-6.5%; the polyethylene glycol accounts for 20-40% of the coating liquid by mass.
The ethanol coating solution comprises ethyl cellulose/polyethylene glycol ethanol solution; the solvent is 95% ethanol; the molecular weight of the polyethylene glycol is 1000-20000.
The mass concentration of the ethanol coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-45% of the coating liquid by mass.
The acetone coating solution comprises more than one of a cellulose diacetate/polyethylene glycol acetone solution or a cellulose acetate butyrate/polyethylene glycol acetone solution; the solvent is acetone; the molecular weight of the polyethylene glycol is 1000-20000.
The mass concentration of the acetone coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
The coating film layer in the step (1) accounts for 0-50% of the mass of the whole granule.
The air inlet temperature of the fluidized bed in the step (1) is 40-60 ℃; the material temperature is 30-45 ℃; the diameter of the spray nozzle of the spray gun is 1.0 mm; the atomization pressure is 0.15-0.20 MPa; the flow rate of the pump liquid of the peristaltic pump is 5-15 r/min.
The application of the particles capable of reducing the temperature of the main stream smoke of the cigarette in the cigarette filter stick.
The invention has the following beneficial effects:
(1) simple, easy industrialization and industrialization;
(2) the prepared particles are easy to be added into the cigarette filter stick;
(3) the particles have compact surfaces and no leakage, and the temperature of the smoke of the cigarettes can be greatly reduced by adding the particles into the cigarette filter stick.
Drawings
Figure 1 is a schematic illustration of an IQOS control heated non-burning smoking article construction and smoke temperature test.
FIG. 11-thermocouple detection position; 12-a filter stick with a PLA film; 13-heating the non-combustible tobacco material; 14-electric heater cavity; 15-an electric heating rod; 16-a vent guide hole; 17-a battery element; 18-smoking article elements.
Figure 2 is a schematic view of the heated non-burning smoking article structure and smoke temperature test using the cooling particles of the present invention.
FIG. 21-thermocouple detection position; 22-a filter stick with the cooling particles of the invention; 23-heating the non-combustible tobacco material; 24-electric heater cavity; 25-an electrical heating rod; 26-a vent guide hole; 27-a battery element; 28-smoking set element.
Detailed Description
The present invention is further illustrated by the following examples. The percentages (%) in the following examples are by weight unless otherwise indicated.
Example 1
Industrial cellulose diacetate was wet ground to a powder with an average particle size of 48 microns. 1 kg of the above ground powder sample was weighed, 1.18 kg of 7.8% Hydroxypropylmethylcellulose (HPMC) aqueous solution was added, and the mixture was sufficiently stirred and mixed in a laboratory wet mixer to prepare a wet material. And (3) performing wet extrusion granulation on the prepared soft wet material on an E-50 wet extruder (the aperture of a distribution plate is 1.0mm) to obtain a cylindrical strip-shaped object. The extruder was fed at 23rpm and the extrusion speed was 26 rpm. And (3) rolling and molding the cylindrical strip-shaped object on an S-250 rolling machine to obtain spherical wet particles. The rounding conditions were: the spheronizer was first run at 600rpm for 1.5 minutes and then at 500rpm for 3 minutes. The above wet spherical pellets were dried at 105-120 ℃ for 5-6 hours to remove moisture, resulting in dried active pellets (and used as comparative spherical pellets for the smoke temperature test in Table 1 below). And (3) coating the dried active particles with a film layer by fluidized bed bottom spraying, and controlling the using amount of the coating liquid to ensure that the coating film layer accounts for 13 percent of the mass of the final spherical particles. After coating, drying the spherical particles for 15 minutes at the air inlet temperature of 60 ℃, drying the surface moisture of the spherical particles, taking out, and sieving with 14-mesh and 20-mesh sieves (0.83-1.18mm) to obtain the cooling spherical particles with the required particle size. The bulk density of the spherical particles was tested to be 0.50 g/mL. The concentration of the coating liquid is 5.25%. The main components are hydroxypropyl methylcellulose and polyethylene glycol 6000, and the solvent is water. Wherein the proportion of polyethylene glycol in the main component is 23.3%. The fluidized bed coating operating conditions were: air inlet temperature: 60 ℃, material temperature: 37.5-38.5 ℃, the diameter of a spray gun nozzle is 1.0mm, the atomization pressure is 0.17MPa, and the flow rate of the peristaltic pump liquid is 10 r/min.
By adopting a composite technology of cavity filter stick preparation, 250mg of the prepared cooling spherical particles or contrast spherical particles are added into an original PLA film section in an IQOS heating non-combustible cigarette filter stick, simulated smoking is carried out according to a cigarette smoking model specified by the national standard GB/T19609-2004, a Canada deep smoking mode (HCI) is adopted, and smoking parameters are as follows: aspiration volume 55mL/L, aspiration frequency 30s, duration of aspiration 2 s. The heater used in the measurement process is an IQOS heater. In the test process, the thermocouple temperature detector detects the temperature of the center of the cigarette filter stick at a position 5mm away from the mouth end when the cigarette is smoked (see the attached figure 2), and the test of smoking of the heated non-combustible cigarette (IQOS) and the temperature of smoke is consistent with the test (see the attached figure 1). The test results are shown in Table 1.
Table 1 mainstream smoke temperature test results
The test data in table 1 show that the mainstream smoke temperature of the cigarette using the cooling spherical particle filter stick of the invention is lower than the control cigarette sample temperature, the reduction amplitude is reduced along with the increasing of the number of the suction openings, wherein the reduction amplitude of the suction temperature of the first opening and the second opening is large and reaches more than 15 ℃. The lowest temperature drop of the rest of the mouth number reaches 4.7 ℃. Compared with the contrast spherical particles, the cooling effect of the flue gas is also obviously improved, which shows that the particles have the cooling effect on the flue gas.
Example 2
1 kg of industrial microcrystalline cellulose (produced by Anhui mountain river, Inc., with an average powder particle size of 45 μm) was weighed, 1.22 kg of 9.1% pregelatinized starch aqueous solution was added, and the mixture was sufficiently stirred and mixed in a laboratory wet mixer to prepare a wet material. And (3) performing wet extrusion granulation on the prepared soft wet material on an E-50 wet extruder (the aperture of a distribution plate is 1.0mm) to obtain a cylindrical strip-shaped object. The extruder was fed at 24rpm and the extrusion speed was 27 rpm. And (3) rolling and molding the cylindrical strip-shaped object on an S-250 rolling machine to obtain spherical wet particles. The rolling circle condition is as follows: the spheronizer was first operated at 650rpm for 2 minutes and then at 450rpm for 3 minutes. Drying the prepared spherical wet particles at the temperature of 105-120 ℃ for 5-6 hours, and removing moisture to obtain dried active particles. And (3) coating the dried rigid solid spheres at the inner layer by adopting fluidized bed bottom spraying, and controlling the using amount of the coating liquid to ensure that the coating film layer accounts for 13 percent of the mass of the final spherical particles. After coating, drying the spherical particles for 15 minutes at the air inlet temperature of 60 ℃, and drying the surface moisture of the spherical particles. Taking out, and sieving with 18 mesh and 24 mesh sieves (0.7-0.88mm) to obtain temperature-reducing spherical granules with required particle size. The bulk density of the spherical particles tested was 0.86 g/mL. The concentration of the coating liquid is 5.25%. The main components are hydroxypropyl methylcellulose and polyethylene glycol 6000, and the solvent is water. Wherein the proportion of polyethylene glycol in the main component is 23.3%. The fluidized bed coating operating conditions are as follows: air inlet temperature: 60 ℃, material temperature: 37.5-38.5 ℃, the diameter of a spray gun nozzle is 1.0mm, the atomization pressure is 0.17MPa, and the flow rate of the peristaltic pump liquid is 10 r/min.
By adopting a composite technology of cavity filter stick preparation, 400mg of the prepared cooling spherical particles are added into an original PLA film section in an IQOS heating non-combustible cigarette filter stick, simulated smoking is carried out according to a cigarette smoking model specified by the national standard GB/T19609-2004, and a Canadian deep smoking mode (HCI) is adopted, wherein the smoking parameters are as follows: aspiration volume 55mL/L, aspiration frequency 30s, duration of aspiration 2 s. The heater used in the measurement process is the IQOS heater. The thermocouple temperature detector during the test detects the temperature at the position 5mm away from the mouth end of the center of the cigarette filter stick when the cigarette is smoked (see figure 2), and the test of smoking of the non-combustible cigarette (IQOS) and the temperature of the smoke is consistent with the test (see figure 1). The test results are shown in Table 2.
TABLE 2 mainstream Smoke temperature test results
The test data in table 2 show that the mainstream smoke temperature of the cigarette using the cooling spherical particle filter stick of the invention is lower than the temperature of a control cigarette sample, and the reduction amplitude is reduced along with the increment of the number of the suction openings, wherein the suction temperature of the first opening and the second opening is greatly reduced and reaches more than 18.6 ℃. The lowest temperature drop amplitude of the rest of the mouth number is 6.3 ℃.
Example 3
1 kg of industrial microcrystalline cellulose powder sample (produced by Anhui mountain river, average particle size of powder is 45 μm) was weighed, 1.22 kg of 9.1% pregelatinized starch aqueous solution was added, and the mixture was thoroughly stirred and mixed in a laboratory wet mixer to obtain a wet material. And (3) performing wet extrusion granulation on the prepared soft wet material on an E-50 wet extruder (the aperture of a distribution plate is 1.0mm) to obtain a cylindrical strip-shaped object. The extruder was fed at 24rpm and the extrusion speed was 27 rpm. And (3) rolling and molding the cylindrical strip-shaped object on an S-250 rolling machine to obtain spherical wet particles. The rounding conditions were: the spheronizer was first operated at 650rpm for 2 minutes and then at 450rpm for 3 minutes. Drying the prepared spherical wet particles at the temperature of 105-120 ℃ for 5-6 hours, and removing moisture to obtain dried active particles. And (3) coating the dried active particles with a film layer by adopting a bottom jet fluidized bed, and controlling the using amount of the coating liquid to ensure that the coating film layer accounts for 9 percent of the mass of the final spherical particles. After coating, drying the spherical particles for 15 minutes at the air inlet temperature of 50 ℃, and drying the surface moisture of the spherical particles. Taking out, and sieving with 18 mesh and 24 mesh sieves (0.7-0.88mm) to obtain temperature-reduced spherical particles with desired particle size, wherein the bulk density of the spherical particles is 0.88 g/mL. The concentration of the coating solution is 5.25%. The main components are hydroxypropyl methylcellulose and polyethylene glycol 1500, and the solvent is water. Wherein the proportion of polyethylene glycol in the main component is 23.3%. The fluidized bed coating operating conditions are as follows: air inlet temperature: 50 ℃ and material temperature: 37.5-38.5 ℃, the diameter of a spray gun nozzle is 1.0mm, the atomization pressure is 0.15MPa, and the flow rate of the peristaltic pump liquid is 10 r/min.
By adopting a composite technology of cavity filter stick preparation, adding 400mg of the prepared cooling spherical particles into an original PLA film section in a heated non-burning cigarette filter stick (IQOS), simulating smoking according to a cigarette smoking model specified in the national standard GB/T19609-2004, and adopting a Canadian deep smoking mode (HCI) with smoking parameters as follows: aspiration volume 55mL/L, aspiration frequency 30s, aspiration duration 2 s. The heater used in the measurement process is the IQOS heater. The thermocouple temperature detector during the test detects the temperature at the position 5mm away from the mouth end of the center of the cigarette filter stick when the cigarette is smoked (see figure 2), and the test of smoking of the non-combustible cigarette (IQOS) and the temperature of the smoke is consistent with the test (see figure 1). The test results are shown in Table 3.
TABLE 3 mainstream Smoke temperature test results
The test data in table 3 show that the mainstream smoke temperature of the cigarette using the cooling spherical particle filter stick of the invention is lower than the control cigarette sample temperature, the reduction amplitude is reduced along with the increasing of the number of the suction openings, wherein the reduction amplitude of the suction temperature of the first opening and the second opening is large and reaches more than 29.1 ℃. The lowest temperature drop of the rest of the opening number reaches 5.9 ℃.
Example 4
Industrial cellulose diacetate was wet ground to a powder with an average particle size of 48 microns. Weighing 1 kg of the above ground powder sample, adding 1.18 kg of 7.8% hydroxypropyl methylcellulose (HPMC) aqueous solution, and fully stirring and uniformly mixing on a laboratory wet mixer to obtain a wet material. And (3) performing wet extrusion granulation on the prepared soft wet material on an E-50 wet extruder (the aperture of a distribution plate is 1.0mm) to obtain a cylindrical strip-shaped object. The extruder was fed at 23rpm and the extrusion speed was 26 rpm. And (3) rolling and molding the cylindrical strip-shaped object on an S-250 rolling machine to obtain spherical wet particles. The rolling circle condition is as follows: the spheronizer was first run at 600rpm for 1.5 minutes and then at 500rpm for 3 minutes. Drying the prepared spherical wet particles at the temperature of 105-120 ℃ for 5-6 hours, and removing moisture to obtain dried active particles. And (3) coating the dried active particles with a film layer by adopting a bottom jet fluidized bed, and controlling the using amount of the coating liquid to ensure that the coating film layer accounts for 13 percent of the mass of the final spherical particles. After coating, drying the spherical particles for 15 minutes at the air inlet temperature of 40 ℃, and drying the surface moisture of the spherical particles. Taking out, and sieving with 14 mesh and 20 mesh sieves (0.83-1.18mm) to obtain temperature-reduced spherical particles with desired particle size and bulk density of 0.52 g/mL. The concentration of the coating solution is 5.0%. The main components are cellulose diacetate and polyethylene glycol 6000, and the solvent is acetone. Wherein the polyethylene glycol accounts for 30% of the main component. The fluidized bed operating conditions were: air inlet temperature: 40 ℃, material temperature: the diameter of a spray gun nozzle is 1.0mm at 32.5 ℃, the atomization pressure is 0.17MPa, and the flow rate of the peristaltic pump liquid is 10 r/min.
By adopting a composite technology of cavity filter stick preparation, 250mg of the prepared cooling spherical particles are added into an original PLA film section in a heating non-combustible cigarette (IQOS) filter stick, simulated smoking is carried out according to a cigarette smoking model specified by the national standard GB/T19609-2004, a Canada deep smoking mode (HCI) is adopted, and smoking parameters are as follows: aspiration volume 55mL/L, aspiration frequency 30s, aspiration duration 2 s. The heater used in the measurement process is an IQOS heater. The thermocouple temperature detector detects the temperature of 5mm away from the mouth end at the center of the cigarette filter stick during smoking of the cigarette (see figure 2), and the smoking of the heated non-combustible cigarette (IQOS) and the test of the smoke temperature are consistent with the above (see figure 1). The test results are shown in Table 4.
TABLE 4 mainstream smoke temperature test results
The test data in table 4 show that the mainstream smoke temperature of the cigarette using the cooling spherical particle filter stick of the invention is lower than the temperature of the control cigarette sample, and the reduction amplitude is reduced along with the increment of the number of the suction openings, wherein the suction temperature of the first opening and the second opening is greatly reduced and reaches more than 14.2 ℃. The lowest temperature drop of the rest of the mouth number reaches 4.9 ℃.
Example 5
By adopting a composite technology of cavity filter stick preparation, spherical particles with different preparation methods are added into an original PLA film section in an IQOS heating non-combustion cigarette filter stick, simulated smoking is carried out according to a cigarette smoking model specified by national standard GB/T19609-2004, and a Canadian deep smoking mode (HCI) is adopted. Phenol was quantitatively tested by HPLC-fluorescence using cambridge filter to intercept the classified material. The effect of the spherical particle coating film layer on the total mainstream aerosol phenol content was investigated and compared with a reference aerosol-generating article containing a gathered PLA cooling unit. The results are shown in Table 5. As is apparent from the experimental results of table 5, the spherical particles having a coating film layer have higher filtration efficiency for phenol.
TABLE 5 Effect of coating film layer on phenol content in mainstream Smoke
The embodiments described above are intended to facilitate a person skilled in the art to understand and use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (26)
1. A particle capable of reducing the smoke temperature of a cigarette is characterized in that: the particles are active or inactive particles of the outer coating layer;
the outer coating layer is a material capable of forming a film;
the film-forming material comprises hydroxypropyl methylcellulose;
the particles capable of reducing the smoke temperature of the cigarettes are prepared by the following method:
(1) mixing active/inactive powder and adhesive solution to prepare wet material;
(2) extruding and cutting the wet material obtained in the step (1) into smooth and compact cylindrical strips with the same diameter by adopting a wet extrusion granulation process through a rotary extrusion granulator, and carrying out rounding forming on the prepared cylindrical strips in a rounding machine to obtain initial wet granules;
(3) drying the initial wet granules, and removing moisture to obtain active/inactive granules;
the method for preparing the active particles or the inactive particles of the outer coating layer further comprises:
coating liquid on the surfaces of active particles or inactive particles by a fluidized bed coating method to form a solid-solid composite phase change coating film layer to obtain initial wet particles;
in the coating process, the film coating is formed by film forming for multiple times, and then the layer films are overlapped and combined.
2. The particle capable of lowering the smoke temperature of a cigarette according to claim 1, wherein: the thickness of the outer coating layer of the inactive particles is 0-0.2mm, and the outer coating layer accounts for 0-50% of the mass of the whole particles; the thickness of the outer coating layer of the active particles is 0.001-0.2mm, and the mass of the outer coating layer accounts for 0.001-50% of the total mass of the particles.
3. The particle capable of lowering the smoke temperature of a cigarette according to claim 1, wherein: the inactive particles can absorb nicotine in the smoke aerosol by less than 3.0mg/cm 3 The particles of (4).
4. The particle capable of reducing the smoke temperature of a cigarette according to claim 2, wherein: the inactive particles include inorganic particles or organic particles.
5. The particle capable of lowering the smoke temperature of a cigarette according to claim 4, wherein: the inorganic particles comprise more than one of aluminum oxide, zirconium oxide, calcium carbonate balls, glass beads, silicon dioxide, iron, copper, aluminum, gold, platinum, magnesium silicate balls or calcium sulfate.
6. The particle capable of lowering the smoke temperature of a cigarette according to claim 4, wherein: the organic particles comprise more than one of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, microcrystalline cellulose, dextrin, lactose, powdered sugar, glucose, mannitol, starch, methyl cellulose, ethyl cellulose, polylactic acid, polyethylene, polypropylene, poly epsilon-caprolactone, polyglycolic acid, polyhydroxyalkanoate or starch-based thermoplastic resin.
7. The particle capable of lowering the smoke temperature of a cigarette according to claim 1, wherein: the active particles are used for adsorbing nicotine in the smoke aerosol by more than or equal to 3.0mg/cm 3 The particles of (1).
8. The particle capable of lowering the smoke temperature of a cigarette according to claim 1, wherein: the active particles comprise more than one of molecular sieve, active carbon, diatomite, zeolite, perlite, ceramic, sepiolite, bleaching earth and ion exchange resin.
9. The particle capable of lowering the smoke temperature of a cigarette according to claim 1, wherein: the shape of the particles capable of reducing the smoke temperature of the cigarettes comprises more than one of spherical shape, spheroidal shape, cake shape, flake shape, belt shape, needle shape, polygonal shape, faceted shape or random shape.
10. A method of preparing a particle for lowering the smoke temperature of a cigarette according to any one of claims 1 to 9, wherein: comprises the following steps:
(1) mixing the active/inactive powder with the binder solution to prepare a wet material;
(2) extruding and cutting the wet material obtained in the step (1) into smooth and compact cylindrical strips with the same diameter by adopting a wet extrusion granulation process, and carrying out rounding molding on the prepared cylindrical strips in a rounding machine to obtain initial wet granules;
(3) drying the initial wet granules, and removing water to obtain active/inactive granules;
the method for preparing the active particles or the inactive particles of the outer coating layer further comprises:
coating the surface of the particles with a coating solution by a fluidized bed coating method to form a solid-solid composite phase change coating film layer, thereby obtaining the incipient wetness particles.
11. The method for producing as claimed in claim 10, characterized in that: the adhesive in the step (1) comprises more than one of hydroxypropyl methylcellulose aqueous solution, pregelatinized starch aqueous solution or sodium carboxymethyl cellulose.
12. The method for producing according to claim 11, characterized in that: the concentration of the hydroxypropyl methylcellulose aqueous solution or the pregelatinized starch aqueous solution is 8-12%.
13. The method of manufacturing according to claim 10, wherein: the mass ratio of the adhesive to the powder in the step (1) is 1.0-1.2: 1.
14. The method of manufacturing according to claim 10, wherein: the rotary extrusion granulator in step (2) is fed at a speed of 23-25rpm and extruded at a speed of 25-30 rpm.
15. The method for producing as claimed in claim 10, characterized in that: the spheronizer in step (2) works at 600-700rpm for 1-2 minutes, and then works at 450-500rpm for 3-4 minutes after being decelerated.
16. The method for producing as claimed in claim 10, characterized in that: also comprises the following steps:
heating and drying to remove the solvent on the surfaces of the initial wet particles to obtain initial particles;
and screening to obtain the coated particles.
17. The method of manufacturing according to claim 10, wherein: the coating liquid is more than one of water-soluble coating liquid, ethanol coating liquid or acetone coating liquid.
18. The method of claim 17, wherein: the water-soluble coating solution comprises more than one of hydroxypropyl methylcellulose/polyethylene glycol aqueous solution, carboxymethyl cellulose/polyethylene glycol aqueous solution or acrylic resin/polyethylene glycol aqueous solution; the solvent is water; the polyethylene glycol has a molecular weight of 1000-.
19. The method of claim 18, wherein: the mass concentration of the water-soluble coating liquid is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
20. The method of manufacturing according to claim 17, wherein: the ethanol coating solution comprises ethyl cellulose/polyethylene glycol ethanol solution; the solvent is 95% ethanol; the polyethylene glycol has a molecular weight of 1000-.
21. The method of manufacturing according to claim 20, wherein: the mass concentration of the ethanol coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
22. The method of manufacturing according to claim 17, wherein: the acetone coating solution comprises more than one of a cellulose diacetate/polyethylene glycol acetone solution or a cellulose acetate butyrate/polyethylene glycol acetone solution; the solvent is acetone; the molecular weight of the polyethylene glycol is 1000-20000.
23. The method of manufacturing according to claim 22, wherein: the mass concentration of the acetone coating solution is 3.5-6.5%; the polyethylene glycol accounts for 20-50% of the coating liquid by mass.
24. The method for producing as claimed in claim 10, characterized in that: the coating film layer accounts for 0-50% of the total weight of the granule.
25. The method for producing as claimed in claim 10, characterized in that: the air inlet temperature of the fluidized bed is 40-60 ℃; the material temperature is 30-45 ℃; the diameter of the spray nozzle of the spray gun is 1.0 mm; the atomization pressure is 0.15-0.20 MPa; the flow rate of the pump liquid of the peristaltic pump is 5-15 r/min.
26. Use of the particle according to any one of claims 1 to 9 for reducing the mainstream smoke temperature of a cigarette in a cigarette filter.
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| CN110477446B (en) * | 2019-08-26 | 2022-02-18 | 安徽中烟工业有限责任公司 | Cooling particles for reducing smoke temperature of heated non-combustible cigarette and preparation method thereof |
| CN110903619B (en) * | 2019-11-12 | 2022-03-08 | 湖北中烟工业有限责任公司 | Preparation method of modified PLA cooling material |
| CN111053294A (en) * | 2020-01-14 | 2020-04-24 | 深圳新火瑞升技术有限公司 | A lead tobacco pipe for electron cigarette |
| CN111218099A (en) * | 2020-03-05 | 2020-06-02 | 南通大学 | Cellulose diacetate composite shaping phase-change material and preparation method and application thereof |
| CN111944493B (en) * | 2020-08-25 | 2021-11-05 | 甘肃烟草工业有限责任公司 | Composite phase-change material for reducing cigarette smoke temperature and preparation method and application thereof |
| CN112273717A (en) * | 2020-10-30 | 2021-01-29 | 南通醋酸纤维有限公司 | Aroma-enhancing and cooling particles for cigarettes, and preparation method and application thereof |
| CN114431524A (en) * | 2022-03-01 | 2022-05-06 | 湖北中烟工业有限责任公司 | Cooling type composite filter rod and application thereof |
| CN116102060A (en) * | 2023-02-10 | 2023-05-12 | 广州市汉宵科研技术有限公司 | Nanoscale zirconia particle material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101128130A (en) * | 2005-02-24 | 2008-02-20 | 菲利普莫里斯生产公司 | Smoking article with tobacco beads |
| CN102551203A (en) * | 2011-12-26 | 2012-07-11 | 云南正邦生物技术有限公司 | Preparation method of adsorption-type base materials |
| CN104411189A (en) * | 2012-07-13 | 2015-03-11 | 菲利普莫里斯生产公司 | Degradable filter for smoking articles |
| CN104449586A (en) * | 2014-11-06 | 2015-03-25 | 湖南中烟工业有限责任公司 | Organic/inorganic composite phase-changing material capable of controlling smoke temperature of cigarette filter as well as preparation method and application of organic/inorganic composite phase-changing material |
| CN108065456A (en) * | 2017-12-22 | 2018-05-25 | 安徽中烟工业有限责任公司 | A kind of heating comprising tobacco particle is not burnt tobacco product and preparation method |
| CN108201169A (en) * | 2017-12-22 | 2018-06-26 | 云南养瑞科技集团有限公司 | With reducing gas flow temperature and supplement the filter element of beneficiating ingredient |
| CN108542001A (en) * | 2018-05-12 | 2018-09-18 | 浙江大学 | A kind of hollow fiber membrane filter and its application based on composite phase-change material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103704882B (en) * | 2013-12-03 | 2015-05-27 | 红云红河烟草(集团)有限责任公司 | Cocoa shell porous particles and application thereof in cigarettes |
| CN103689785B (en) * | 2013-12-03 | 2016-04-20 | 红云红河烟草(集团)有限责任公司 | A kind of offal porous particle and the application in cigarette thereof |
| CN107536095B (en) * | 2016-06-24 | 2020-08-14 | 湖南中烟工业有限责任公司 | Preparation method of homogenized special-shaped cigarette |
| CN107951070A (en) * | 2017-11-22 | 2018-04-24 | 曹宏 | A kind of composite cigarette filter and preparation method thereof and a kind of cigarette |
-
2019
- 2019-03-01 CN CN201910157268.9A patent/CN109700070B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101128130A (en) * | 2005-02-24 | 2008-02-20 | 菲利普莫里斯生产公司 | Smoking article with tobacco beads |
| CN102551203A (en) * | 2011-12-26 | 2012-07-11 | 云南正邦生物技术有限公司 | Preparation method of adsorption-type base materials |
| CN104411189A (en) * | 2012-07-13 | 2015-03-11 | 菲利普莫里斯生产公司 | Degradable filter for smoking articles |
| CN104449586A (en) * | 2014-11-06 | 2015-03-25 | 湖南中烟工业有限责任公司 | Organic/inorganic composite phase-changing material capable of controlling smoke temperature of cigarette filter as well as preparation method and application of organic/inorganic composite phase-changing material |
| CN108065456A (en) * | 2017-12-22 | 2018-05-25 | 安徽中烟工业有限责任公司 | A kind of heating comprising tobacco particle is not burnt tobacco product and preparation method |
| CN108201169A (en) * | 2017-12-22 | 2018-06-26 | 云南养瑞科技集团有限公司 | With reducing gas flow temperature and supplement the filter element of beneficiating ingredient |
| CN108542001A (en) * | 2018-05-12 | 2018-09-18 | 浙江大学 | A kind of hollow fiber membrane filter and its application based on composite phase-change material |
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