JP7238064B2 - Multi-layer smoke particles, method of making, method of use and use thereof - Google Patents

Description

TECHNICAL FIELD The present invention belongs to the technical field of heat-not-burn cigarettes, and specifically relates to multi-layer smoke particles, methods of making, methods of use and uses thereof.

BACKGROUND ART With the improvement of living standards, people attach more and more importance to their own health, and in recent years, the health problems caused by smoking have attracted great attention. Domestic and foreign major enterprises are actively developing new tobacco products to replace traditional cigarettes in order to meet diverse consumption needs. E-cigarettes and heat-not-burn cigarettes dominate among these growing new tobacco products.

Electronic cigarettes have the advantage of being able to arbitrarily adjust the flavor and taste of the smoke by adjusting the components of the liquid. Because it is produced mainly by electronic atomizers, its mouthfeel, especially temperature, is still somewhat different from conventional cigarettes that generate smoke by heating, and is therefore less acceptable to cigarette smokers.

Heat-not-burn cigarettes generate smoke by heating the smoking core portion of the tobacco, and the smoke has a highly acceptable mouthfeel. In recent years, with the efforts of major Chinese companies, a new type of heated cigarette that uses particles as the base material for smoking has appeared. Since it has a certain degree of adsorption to , there are defects such as less smoke generation.

The present invention is presented to solve the above problems.

A first aspect of the present invention is a smoking particle 1 including at least a core layer 11, a smoking layer 12, and a coating layer 13 from the inside to the outside,
The core layer 11 contains micropores with a diameter of less than 2 nm, mesopores with a diameter of 2-50 nm, and macropores with a diameter of greater than 50 nm,
Smoke layer 12 provides a multi-layer structure of smoke particles comprising a solid substrate, a perfume, and a smoke agent.

Preferably, the core layer 11 has a specific surface area of 180 to 450 m ² /g. This is because if the specific surface area of the core layer 11 is too small or too large, the amount of smoke generated will be significantly reduced. It is believed that this range can better provide smoke condensation nuclei in the pores during initial atomization and reduce the energy required for initial atomization, and its role is to add zeolite to the heating solution This is the same as the case of preventing bumping by

Preferably, the specific surface area distribution of micropores, mesopores and macropores is micropore/mesopore=1/1 to 1/2 and mesopore/macropore=2/1 to 4/1. This is because if the specific surface area distribution of micropores and macropores is too large, the amount of smoke generated is reduced. If there are too many micropores, the thermal energy during heating will dissipate and smoke generation will be delayed. (adsorbed in the pores) is increased and the amount of smoke generated is reduced. The smoke generation process begins with the generation of condensation nuclei in the micropores and smoothly reaches the macropore regions through the mesopores. The role of the macropore region is mainly to (1) make the core layer 11 have a predetermined roughness to ensure that the smoke layer 12 covers the core layer 11 well, and (2) the condensation nuclei The area is in contact with the smoke agent and perfume in the smoke layer 12 to grow rapidly and break through the smoke layer 12 violently to generate smoke.
In this specification, the particle size of the core layer 11 is not specified, and the particle size of the final smoke particles 1 is also not specified. It is the specific surface area and pore size distribution of the core layer that have the main influence on smoke generation. Preferably, the particle size of the core layer 11 is 20-40 mesh. Of course, it can be in other particle size ranges, if it is a little larger or a little smaller, it will be modified when carrying the smoke layer, the final particle size difference will be small, and the smoke effect will be slightly affected, but especially Not a big scatter.

Preferably, the melting point of the coating layer 13 is 300° C. or less so that it melts first when heated, and if the melting point is too high, it will hinder the release of smoke. The material of the coating layer 13 is one or more kinds of non-toxic and odorless polymer films such as sodium alginate, polylactic acid (PLA), and polymeric saccharides. The main role of the coating layer 13 is to prevent the particles from absorbing water during storage and to prevent blocking between the particles.

Preferably, the core layer 11 is one or two materials selected from natural materials and synthetic materials. The core layer 11 may be activated carbon, zeolite, modified natural ore, or the like having a specific pore structure.

Preferably, the smoke layer 12 includes at least one sub-smoke layer, two adjacent sub-smoke layers have the same or different solid substrates, two adjacent sub-smoke layers have the same or different fragrances, The smoke-producing agents in two adjacent sub-smoke-producing layers are the same or different. It is preferable that the smoke-generating agent is one or two selected from glycerol and propylene glycol.

Preferably, the solid substrate is at least one selected from powdery plant roots, stems and leaves, such as kudzu root, tobacco leaves, mint leaves, backbone, agarwood, and the like.

Preferably, the smoke layer 12 has a moisture content of 8 to 22%. If the water content is too low, the production is difficult and difficult to achieve, and the smoke effect of the particles cannot be significantly improved. put away.

A second aspect of the present invention is
a core layer 11 production step (1) of obtaining the core layer 11 by subjecting the core material to high temperature degassing, vacuum degassing or high temperature vacuum degassing;
A step (2) of supporting the smoke generating layer 12, in which the core layer 11 obtained in step (1) is supported with the blended solid base material, perfume and smoke generating agent, and dried to obtain coarse particles;
If the smoke layer 12 includes two or more sub-layers, the above step (2) must be repeated until the set number of layers is reached.
a step (3) of coating the coating layer 13 by dissolving the coating material in a solvent and coating the coarse particles obtained in step (2) by fluidized spray or rolling deposition to obtain the smoke particles 1 2. A method for producing smoke particles according to 1. is provided.

The purpose of degassing the core material is to remove the volatiles it contains and to prevent the development of objectionable odors when heated.
The supporting method in step (2) depends on the state of the mixture after blending. If the viscosity is high, fluidized spray or rolling adhesion may be adopted, and if the viscosity is low, immersion may be used.
Step (3) typically does not employ dip coating to prevent re-dissolution release of components in smoke layer 12 .

Preferably, in step (1), the temperature of high-temperature degassing is 300° C. or higher, the pressure of vacuum degassing is 600 mbar or less, and the processing conditions for high-temperature vacuum degassing are temperature of 250° C. or higher, pressure is less than or equal to 800 mbar,
Degassing time is 30 minutes or more,
In step (3), the amount of the coating material used is preferably 0.5-2% of the total mass of the core layer 11 and the smoking layer 12. If the amount is too large, smoking will be inhibited.

A third aspect of the present invention provides a method of using the smoke particles 1 according to the first aspect, wherein the smoke particles 1 are put into a heated cigarette, tobacco cartridge or smoking device.

Preferably, the structure of the heated cigarette is the same as that of ordinary particulate smoking material cigarettes, and as shown in FIG. and a filter portion 24 in this order, and the smoke generating particles 1 are filled in the smoking core portion 22 .

Preferably, the structure of the smoke chamber and filter of the smoking article is such that the smoke particles 1 are housed in the smoke chamber, and the filter part 34 of the smoking article is connected to the upper end of the smoke chamber, as shown in FIG. If the smoking article is of the circumferential heating type (Fig. 3a), circumferential heating members 31 are provided on the sidewalls of the smoke chamber. When the smoking article is of the microwave heating type (Fig. 3c), a microwave generating member 33 is provided on the side wall of the smoking chamber. If the smoking article is centrally heated (Fig. 3b), a central heating member 32 is provided within the smoke chamber. After the smoking particles 1 are heated by the smoking tool, the generated smoke is sucked by the filter portion 34 of the smoking tool.

Of course, the smoke particles 1 can also be used in a tobacco cartridge.

The smoking process of the smoking particles 1 is that when the particles are sucked, the coating layer 13 of the particles melts or undergoes a phase change and bursts due to the heat from the outside. The gas inside is released to form condensation nuclei, which reach the surface macropores through the mesopores, and the condensation nuclei contact the smoke agent and fragrance in the smoke layer 12 in the macropores and grow rapidly; It violently breaks through the smoke layer 12 to generate smoke, and finally enters the oral cavity of the smoker through the filter part.

The beneficial effects of the present invention compared to the prior art are as follows.
1. The multi-layered smoke generating particles according to the present invention solves the problem that the fragrance and the smoke generating agent cannot be released from the inside by granulating only the conventional smoke generating material by using a porous material as the core, so that the problem is wasted. , The rational combination of micropores, mesopores and macropores provides condensation nuclei when smoke is generated, clears the vaporization passage of condensation nuclei, reduces the re-adsorption action, and increases the amount of smoke generated.
2. The multi-layered smoke particles according to the present invention have one or more smoke layers, providing more options for combining the flavor and taste of smoke.
3. By providing a coating layer on the outermost layer of the smoke particles having a multilayer structure according to the present invention, it is possible to prevent water absorption during storage of the particles, prevent blocking between particles, and melt or melt when heated. Or the smoke is released smoothly by phase change.

FIG. 3 is a structural schematic view of the multi-layered smoke particles of the present invention; 1 is a structural schematic view of a heated cigarette containing multi-layer smoke particles of the present invention; FIG. FIG. 3 is a structural schematic diagram of a smoke chamber and a filter in the special smoking article that directly heats the multi-layer smoke particles of the present invention;

EXAMPLES The present invention will be described in detail below with reference to Examples, but the present invention is not limited to these Examples. Experimental methods that do not specify specific conditions in the examples are performed according to the usual conditions and conditions described in the manual, or the conditions recommended by the manufacturer, and the general-purpose equipment, materials, reagents, etc. used are Commercially available unless otherwise stated. All raw materials required for the following examples and comparative examples are commercially available.

In the examples below, the micropore diameter is less than 2 nm, the mesopore diameter is between 2 and 50 nm, and the macropore diameter is greater than 50 nm. The method for measuring the specific surface area is the nitrogen adsorption method.

Example 1
The smoking particle of this embodiment has a three-layer structure including a core layer 11, a smoking layer 12, and a coating layer 13.
The core layer 11 is activated carbon with a particle size of 20 to 40 meshes, and when measured, has a specific surface area of 450 m ² /g. = 1/1 and mesopores/macropores = 4/1.
Smoke layer 12 is a single layer that includes a solid substrate, a perfume, and a smoke agent.
The solid substrate is powdered tobacco leaves, the flavoring agent is a mint-flavoured flavoring agent, and the smoke agent is glycerol.
The covering layer 13 is a sodium alginate film.
The method for producing smoke particles having a multi-layer structure according to this embodiment includes:
a step (1) of washing the core layer 11, in which the selected activated carbon core material is deaerated at high temperature in an oven at 300°C for 30 minutes, then washed with water and dried at 80°C;
A solid base material, a fragrance, and a smoking agent are mixed and stirred at a mass ratio of 3:2:2 to obtain a smoking slurry. % and obtaining coarse grains (2);
Sodium alginate is dissolved in water, and the coarse granules obtained in step (2) are coated by fluidized spray and dried at 80° C. for 0.5 h to obtain fuming particles. coating step (3) with a coating layer 13 of 0.5% of the total mass with the layers.
When the smoke particles of this example were used as sample 1 and screened and measured, the particle diameter was 10 to 24 mesh.

Example 2
The smoking particle of this embodiment has a three-layer structure including a core layer 11, a smoking layer 12, and a coating layer 13.
The core layer 11 is an aluminophosphate zeolite with a particle size of 20 to 40 mesh, and when measured, has a specific surface area of 250 m ² /g. /mesopores = 1/2, mesopores/macropores = 2/1.
Smoke layer 12 is a single layer that includes a solid substrate, a perfume, and a smoke agent.
The solid substrate is powdered kudzu root, the flavor is an ice blueberry flavored blend, and the smoke agent is propylene glycol.
The coating layer 13 is polylactic acid (PLA).
The method for producing smoke particles having a multi-layer structure according to this embodiment includes:
a washing step (1) of the core layer 11 in which the selected aluminophosphate zeolite core material is vacuum degassed at a pressure of 600 mbar for 50 minutes, then washed with water and dried;
A solid base material, a perfume, and a smoking agent are mixed and stirred at a mass ratio of 4:2:3 to obtain a smoking slurry, which is supported on the core layer 11 by rolling adhesion, and dried to reduce the water content to 22%. % and obtaining coarse particles (2);
PLA is dissolved in ethyl acetate, the coarse particles are coated by fluidized spray, and dried at 80° C. for 0.5 h to obtain smoke particles, the amount of PLA used is 2% of the total mass of the core layer and smoke layer. a coating step (3) of the coating layer 13;
Sample 2 of the smoke particles of this example was screened and measured, and the particle diameter was 10 to 24 mesh.

Example 3
The smoking particle of this embodiment has a three-layer structure including a core layer 11, a smoking layer 12, and a coating layer 13.
The core layer 11 is modified montmorillonite with a particle size of 20 to 40 mesh, and when measured, has a specific surface area of 180 m ² /g. Pores=2/3, mesopores/macropores=4/1.
Smoke layer 12 is a single layer that includes a solid substrate, a perfume, and a smoke agent.
The solid substrate is a mixture of powdered mint leaves and bones, the flavor is a coffee-flavored blend flavor, the smoke agent is a mixture of glycerol and propylene glycol, and the weight of glycerol and propylene glycol is The ratio is 1:1.
The coating layer 13 is a maltose film.
The method for producing smoke particles having a multi-layer structure according to this embodiment includes:
a step (1) of washing the core layer 11, in which the selected modified montmorillonite core material is degassed at a high temperature of 350° C. for 30 minutes, then washed with water and dried;
A solid base material, a perfume, and a smoking agent are mixed and stirred at a mass ratio of 5:3:2 to obtain a smoking slurry, and the smoking slurry is supported on the core layer 11 by a fluidized spray, and dried to reduce the water content to 12. a step (2) of supporting the fuming layer 12 to reduce the
Maltose is dissolved in a small amount of water, coated by rolling adhesion and dried to obtain smoke particles, the coating step of coating layer 13 with a coating amount of 1.5% of the total weight of the core layer and smoke layer (3 ) and including.
Sample 3 of the smoke particles of this example was screened and measured, and the particle diameter was 10 to 24 mesh.

Example 4
The smoking particle of this embodiment has a three-layer structure including a core layer 11, a smoking layer 12, and a coating layer 13.
The core layer 11 is activated carbon with a particle size of 20 to 40 mesh, a specific surface area of 350 m ² /g, and a specific surface area distribution of micropores, mesopores, and macropores of micropores/mesopores=3/4. , mesopores/macropores=3/1.
Smoke layer 12 is a single layer that includes a solid substrate, a perfume, and a smoke agent.
The solid substrate is powdered kudzu root and agarwood, the flavor is an orange flavored flavoring agent, and the smoke agent is a mixture of glycerol and propylene glycol.
The covering layer 13 is a sodium alginate film.
The method for producing smoke particles having a multi-layer structure according to this embodiment includes:
a washing step (1) of the core layer 11 in which the selected activated carbon core material is degassed at 300° C. and 600 mbar for 30 minutes, then washed with water and dried;
A carrying step (2) of the smoke generating layer 12 in which the mixed solid base material, perfume and smoke generating agent are carried on the core layer 11 by a fluidized spray, and dried to reduce the water content to 16%;
Sodium alginate is dissolved in water, coated by fluidized spray, dried at 80° C. for 0.5 h to obtain smoke particles, and the coating amount is 1% of the total mass of the core layer and the smoke layer. and step (3).
The smoke particles of this example were used as Sample 4, and the particle diameter was 10 to 24 mesh when screened and measured.

Example 5
The smoke particle of this embodiment has a four-layer structure including a core layer 11 , a smoke layer 12 divided into both a smoke layer 121 and a smoke layer 122 , and a coating layer 13 .
The core layer 11 is modified bentonite having a particle size of 20 to 40 mesh, a specific surface area of 220 m ² /g, and a specific surface area distribution of micropores, mesopores, and macropores of micropores/mesopores=2/ 3, mesopores/macropores = 3/1.
The smoke layer 12 comprises two layers of a mixture of solid substrate, perfume and smoke agent, a first sub-smoke layer 121 and a second sub-smoke layer 122 respectively.
The solid substrate of sub-smoke layer 121 is powdered mint leaves and agarwood. The solid substrate of sub-smoke layer 122 is powdered tobacco leaves. Fragrance uses a mint-flavored blended fragrance. Glycerol is used as smoke-generating agent.
The coating layer 13 is polylactic acid (PLA).
The method for producing smoke particles having a multi-layer structure according to this embodiment includes:
a washing step (1) of the core layer 11, in which the selected modified bentonite core material is vacuum degassed at a pressure of 400 mbar for 40 minutes, then washed with water and dried;
A mixture of two kinds of solid base materials, a perfume and a smoke-generating agent, which are blended, is carried on the core layer 11 in two portions by rolling adhesion, and dried to reduce the water content to 18% to form a smoke-generating layer 12. a carrying step (2);
Coating layer 13 in which PLA is dissolved in ethyl acetate, coated by fluidized spray, dried at 80° C. for 0.5 h to obtain smoke particles, and the coating amount of PLA is 1% of the total mass of the core layer and the smoke layer. and a coating step (3) of
The smoke particles of this example were used as sample 5, and the particle diameter was 10 to 24 mesh when screened and measured.

表１からわかるように、本発明で製造された発煙粒子は、同一のタバコにおいて、発煙量が大きく、香気品質が高く、発煙剤の利用率が高いという顕著な特徴を有する。
三、発煙剤の残留比較
上記の０－１、１、０－５及び５を代表とし、１０種の発煙粒子サンプルに入れ、特別喫煙具の発煙室（図３に示される）に入れ、その発煙剤の残留率を測定し、比較結果を表２に示した。

表２からわかるように、本発明で製造された発煙粒子は、３つの異なる加熱モードにおいて、通常の製造方法で得られた粒子よりも発煙剤の残留が少ないことから、本発明で製造された発煙粒子はより高い発煙剤の利用率を有することが分かった。 Application example 1
Particles produced by a normal production method (that is, particles produced only from the material of the smoke layer 12) were used as control samples, corresponding to the samples in the above five examples. Similarly, the control samples were labeled 0-1, 0-2, 0-3, 0-4 and 0-5, respectively, where 0-5 was the smoke layer 121 and smoke layer 122 at a 1:1 mass ratio. It is granulated by mixing at a ratio.
1. Comparison of blocking status after 10 kinds of particle samples were left in 80% humidity environment for 48 hours Blocking occurred to some extent in each case, but no blocking occurred in Samples 1, 2, 3, 4, and 5 in Examples. found to be preventable.
2. Sucking evaluation comparison According to Yunnan Zhongyi Industry Co., Ltd.'s corporate standard "QYNZY.J07.022-2015 Sensory evaluation method for new cigarettes", sensory evaluation of cigarettes was performed by multiple sensory evaluators, and smoking was completed. After measuring the residual rate of the smoke-producing agent in the particles, the functional superiority of the smoke-producing particles and the utilization rate of the smoke-producing agent were considered. Here, the sensory qualities are scored from 0 to 10 points for the amount of smoke generated and 0 to 10 points for the fragrance quality.
The ten smoke particle samples described above were placed in conventional particulate smoke material cigarettes (the structure is shown in FIG. 2) and inhaled using a centrally heated smoking device. Table 1 shows the results.

As can be seen from Table 1, the smoke granules produced in the present invention have outstanding characteristics of high smoke volume, high aroma quality and high smoke agent utilization in the same cigarette.
3. Comparison of smoke agent residue, taking the above 0-1, 1, 0-5 and 5 as representatives, put them in 10 kinds of smoke particle samples, put them in the smoke chamber of the special smoking article (shown in Figure 3), The residual rate of the smoke generating agent was measured, and the comparison results are shown in Table 2.

As can be seen from Table 2, the smoke particles produced according to the invention have less residual smoke agent than the particles obtained by conventional production methods in three different heating modes. Smoke particles were found to have higher smoke agent utilization.

表１からわかるように、本発明で製造された発煙粒子は、同一のタバコにおいて、発煙量が大きく、香気品質が高く、発煙剤の利用率が高いという顕著な特徴を有する。以上の利点は、コア層の比表面積及びミクロ孔・メソ孔・マクロ孔の割合に関わる。 Application example 2
The core layer 11 used is activated carbon with a particle size of 20 to 40 mesh, and when measured, has a specific surface area of 800 m ² /g. Smoke particles 1A were produced in the same manner as in Example 1, except that /mesopores = 1/5 and mesopores/macropores = 1/1.
The core layer 11 used is an aluminophosphate zeolite with a particle size of 20 to 40 mesh, and when measured, has a specific surface area of 95 m ² /g, and a specific surface area distribution of micropores, mesopores and macropores. , micropores/mesopores=1/8, and mesopores/macropores=6/1.
The above two smoke particle samples were placed in a conventional particulate smoke material cigarette (structure shown in FIG. 2) and inhaled using a centrally heated smoking device to form Samples 1 and 2 in Table 1. compared.

As can be seen from Table 1, the smoke granules produced in the present invention have outstanding characteristics of high smoke volume, high aroma quality and high smoke agent utilization in the same tobacco. The above advantages relate to the specific surface area of the core layer and the ratio of micropores, mesopores and macropores.

1: Smoke-emitting particles 11: Core layer 12: Smoke-emitting layer 13: Coating layer 21: Sealing film 22: Smoke-emitting core material part 23: Hollow support part 24: Cooling part and filter part 31: Circumferential heating member 32: Central heating member 33: Microwave generating member 34: Filter part of smoking article

Claims (8)

A smoking particle having a multilayer structure, wherein the smoking particle (1) includes at least a core layer (11), a smoking layer (12), and a coating layer (13) from the inside to the outside,
The core layer (11) comprises micropores with a diameter of less than 2 nm, mesopores with a diameter of 2-50 nm, and macropores with a diameter of more than 50 nm,
The smoke layer (12) comprises a solid substrate, a perfume, and a smoke agent,
The specific surface area distribution of the micropores, the mesopores and the macropores is characterized by micropores/mesopores=1/1 to 1/2 and mesopores/macropores=2/1 to 4/1. multi-layered smoke particles. The multi-layer smoke generating particle according to claim 1, characterized in that the core layer (11) has a specific surface area of 180-450 m ² /g. 2. The method according to claim 1, characterized in that the melting point of the covering layer (13) is below 300[deg.] C. and the core layer (11) is selected from one or both of natural and synthetic materials. multi-layered smoke particles. The smoke layer (12) includes at least one sub-smoke layer, two adjacent sub-smoke layers have the same or different solid substrates, and two adjacent sub-smoke layers have the same perfume. or different, and the smoke agents in two adjacent sub-layers are the same or different. 2. The multi-layer smoke generating particle according to claim 1, wherein said solid substrate is selected from at least one of powdered plant roots, stems and leaves. A method for producing smoke particles according to any one of claims 1 to 4 ,
Hot degassing, vacuum degassing or hot vacuum degassing the core material to form a core layer containing micropores with a diameter less than 2 nm, mesopores with a diameter between 2 and 50 nm, and macropores with a diameter greater than 50 nm ( 11) is obtained, and the specific surface area distribution of the micropores, the mesopores and the macropores is micropores/mesopores = 1/1 to 1/2 and mesopores/macropores = 2/1 to 4/1. a manufacturing step (1) of the core layer (11);
a step (2) of supporting a smoke layer (12) in which the blended solid substrate, perfume and smoke agent are supported on the core layer (11) obtained in step (1) and dried to obtain coarse particles; ,
Coating step (3) of coating layer (13), dissolving the coating material in a solvent and coating the coarse particles obtained in step (2) by fluidized spray method or rolling adhesion method to obtain smoke particles (1) A manufacturing method, comprising: In step (1), the temperature of the high-temperature degassing is 300° C. or higher, the pressure of the vacuum degassing is 600 mbar or less, and the processing conditions for the high-temperature vacuum degassing are temperature of 250° C. or higher and pressure of 800 mbar. and
Degassing time is 30 minutes or more,
The production according to claim 6 , characterized in that in step (3), the coating amount of the coating material is 0.5-2% of the total mass of the core layer (11) and smoke layer (12). Method. A method of using the smoke particles (1) according to any one of claims 1 to 4 , characterized in that the smoke particles (1) are put into a heated cigarette, tobacco cartridge or smoking device.

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