An atomized agent-diatomite composite material, preparation thereof and application thereof in a heated non-combustion cigarette

Abstract

The present application relates to the technical field of new herbs, in particular to a kind of atomization agent diatomite composite material, it includes diatomite with mesopore and macropore, and atomization agent filled in diatomite pore structure;Wherein, the weight ratio of diatomite and atomization agent is greater than or equal to 1.The present application also includes the preparation method and application of the material.The technical scheme of the present application can solve the problem of atomization agent moisture absorption, in addition, can also synergistically improve atomization amount, atomization transfer rate and utilization rate.

Description

Technical Field

[0001] This invention belongs to the field of novel tobacco technology, specifically relating to a novel tobacco sheet. Background Technology

[0002] Heated cigarettes have seen rapid growth in recent years due to the significantly lower levels of harmful components in their smoke compared to traditional cigarettes. However, heated cigarettes lack a combustion process during inhalation, failing to achieve the same smoke effect as traditional cigarettes. Therefore, a larger amount of atomizing agent is added to the heating medium (usually tobacco sheets) of heated cigarettes. Currently, the atomizing agents in mainstream heated cigarette sheets are primarily glycerol and propylene glycol, with glycerol being present in a higher concentration.

[0003] The presence of high-content glycerol and other atomizing agents, while providing smoke volume, also has significant drawbacks: (1) The atomizing agents have strong hygroscopicity, which leads to poor processing performance of heated cigarette sheets, reduced cigarette yield, and the need for strict control of temperature and humidity in the processing area, making the processing technology more complex; (2) The finished cigarettes still have the above problems, causing the cigarettes to absorb moisture and become moldy, and the cigarette paper to have yellow spots, significantly shortening the shelf life of the products. The main reason for this is the polyhydroxy structure of atomizing agents such as glycerol. On the one hand, it is highly hydrophilic, which makes it easy to absorb moisture; on the other hand, there are strong hydrogen bonding forces between glycerol molecules, making it difficult for glycerol to escape from the sheet and transfer into the smoke during the heating process. According to literature reports, the migration rate of glycerol in the current mainstream heated cigarette sheets is only 30-40% (Zhao Deqing, Deng Yong, Guo Linqing, et al. Rapid determination of glycerol content in heated cigarettes by enzyme electrode method [J]. Journal of Tobacco Science, 2020, 26(6).), and most of the glycerol is in a "useless" state. If the proportion of glycerol remaining in the film can be reduced, the utilization rate of glycerol can be effectively improved, the amount of atomizing agents such as glycerol used in the film preparation process can be reduced, and the product quality can be significantly improved.

[0004] In summary, existing heated non-combustible cigarette tobacco sheets generally suffer from problems such as poor stability of atomizing agents, difficulty in processing, and difficulty in effective utilization. Summary of the Invention

[0005] To address the problems of poor stability, difficulty in processing, and difficulty in effective release of tobacco sheets in existing heated non-combustible cigarettes, the primary objective of this invention is to provide an atomizing agent@diatomaceous earth composite material, which aims to improve the stability and utilization rate of the atomizing agent.

[0006] The second objective of this invention is to provide a method for preparing the aforementioned atomizing agent@diatomite composite material.

[0007] A third objective of this invention is to provide the application of the aforementioned atomizing agent@diatomite composite material in heated non-combustible cigarettes.

[0008] A fourth objective of this invention is to provide a tobacco sheet comprising the aforementioned atomizing agent@diatomite composite material.

[0009] The fifth objective of this invention is to provide a heated, non-combustible cigarette comprising the tobacco sheet.

[0010] The atomizing agent has significant hygroscopic properties, and inappropriate addition of the atomizing agent can affect the stability and processing performance of the film. To address this issue, this invention initially attempted to improve hygroscopicity by adding the atomizing agent to a mesoporous structure. However, in-depth research revealed that to successfully implement this approach, it is necessary to overcome problems such as the difficulty in guiding and filling the atomizing agent within the pore structure, and the difficulty in achieving confined stability. Furthermore, it is also necessary to overcome the challenge of balancing stability and the release rate of the atomizing agent during the suction phase. To address the technical problems faced by this approach, this invention provides the following improvement:

[0011] An atomizing agent@diatomite composite material, comprising diatomite having mesopores and macropores, and an atomizing agent filling the pore structure of the diatomite;

[0012] The weight ratio of diatomaceous earth to atomizing agent is greater than or equal to 1.

[0013] In this invention, diatomaceous earth with a special structure is innovatively used to confine and control the atomizing agent. In addition, the combined control of the ratio of the two can effectively stabilize the atomizing agent. Moreover, it can also unexpectedly and effectively promote the release of the atomizing agent and improve its utilization rate.

[0014] In this invention, the control of the diatomaceous earth, its microstructure, and its ratio with the atomizing agent is key to synergistically improving the stability of the atomizing agent and enhancing its effective release.

[0015] As a preferred option, further control over the pore structure of diatomaceous earth helps to further improve the balance between the confined stability and utilization rate of the atomizer.

[0016] Preferably, in diatomaceous earth, the pore size of the macropores is 1 to 50 micrometers;

[0017] Preferably, the particle size of diatomaceous earth is 20–400 mesh.

[0018] Preferably, the diatomaceous earth contains more than 60% macropores.

[0019] Preferably, the diatomaceous earth is diatomaceous earth that has undergone microwave modification with alkali solution. This invention has found that this modified diatomaceous earth can further reduce hygroscopicity and improve its smoke transfer rate.

[0020] Preferably, the atomizing agent is at least one of glycerol and propylene glycol.

[0021] Preferably, the weight ratio of diatomaceous earth to atomizing agent is 1 to 4:1, more preferably 1.2 to 2:1. In this invention, at this preferred ratio, the synergistic effect of the diatomaceous earth and atomizing agent in the structure can be further improved, contributing to a better balance between atomizing agent stability and release efficiency.

[0022] The present invention also provides a method for preparing the aforementioned atomizing agent@diatomite composite material, wherein the atomizing agent and diatomite are mixed, and the atomizing agent is filled into the pore structure of the diatomite to obtain the aforementioned atomizing agent@diatomite composite material.

[0023] In this invention, thanks to the chemical and pore structure characteristics of diatomaceous earth, it can effectively guide the filling of atomizing agents, which is conducive to the preparation of composite materials that take into account both atomizing agent stability and effective release.

[0024] In this invention, to further improve the induction filling and release efficiency of the atomizing agent, it is preferable to pretreat the diatomaceous earth in an alkaline solution with microwave assistance before mixing. This invention has found that this pretreatment improves the pore structure, optimizes the guiding active sites, helps to further improve the confined stability of the atomizing agent, and can also unexpectedly induce the effective release of the atomizing agent during the suction phase, improving its utilization rate.

[0025] Preferably, the alkaline solution is an aqueous solution of an alkali metal hydroxide, and the preferred solute concentration is 0.1–3 M, more preferably 0.5–1 M;

[0026] Preferably, the pretreatment time is 0.5 to 3 hours, and more preferably 1 to 2 hours.

[0027] The atomizing agent and diatomaceous earth are premixed and then compounded under an applied DC electric field to obtain the atomizing agent@diatomaceous earth composite material.

[0028] The present invention also found that, under the action of an electric field, it helps to further improve the confinement stability of the prepared material for the atomizer, and in addition, it can also take into account the release efficiency.

[0029] In this invention, the voltage of the DC electric field is 1-5 kV, preferably 1-2 kV; the recombination time under electric field assistance is 0.5-1 h.

[0030] The present invention also provides an application of the aforementioned atomizing agent@diatomite composite material, using it as an atomizing additive for the preparation of heated non-combustible cigarettes.

[0031] In this invention, existing methods can be used to prepare heated non-combustible cigarettes from the atomizing agent@diatomite composite material described in this invention.

[0032] For example, a preferred application of the present invention is its use as an atomizing additive in the preparation of tobacco sheets for heated non-combustible cigarettes. Preferably, the preparation of tobacco sheets for heated non-combustible cigarettes is carried out using a slurry method.

[0033] Preferably, the atomizing agent@diatomaceous earth composite material, tobacco powder, adhesive, and fiber are slurried with water, and then tobacco sheets are prepared by a thick slurry process.

[0034] Preferably, in the tobacco sheet of the heated non-combustible cigarette, the content of the atomizing agent in the diatomaceous earth composite material is 5-10 wt%.

[0035] This invention also provides a tobacco sheet for heating non-combustible cigarettes, incorporating the aforementioned atomizing agent@diatomaceous earth composite material. The tobacco sheet of this invention, apart from the addition of the composite material described herein, may have other known components and structures.

[0036] Preferably, in the heated non-combustible cigarette tobacco sheet, the content of the atomizing agent in the atomizing agent@diatomite composite material is 5-10 wt%.

[0037] In this invention, thanks to the excellent atomizer confinement stability and release effect of the composite material, considerable physicochemical effects can be obtained even with a reduced atomizer dosage.

[0038] This invention discloses a preferred method for preparing tobacco sheets, which involves using a slurry method to prepare heated cigarette sheets from atomizing agent@diatomaceous earth composite material, tobacco powder, water, adhesive, and fibers. Heated cigarettes rolled using these sheets can reduce the amount of atomizing agent to below 10 wt% while maintaining the existing smoke volume, significantly lower than existing commercially available heated cigarette products.

[0039] The present invention also provides a heated non-combustible cigarette comprising the tobacco sheet described herein.

[0040] The main advantages of this invention are:

[0041] 1. This invention provides an atomizer@diatomite composite material, which, based on the combined control of the physicochemical properties of its components, can achieve synergy, significantly improve the stability of the atomizer, and further significantly improve the release efficiency of the atomizer during the inhalation stage.

[0042] In this invention, the proportion of atomizing agent transferred into the smoke during the heating and smoking process of heated cigarettes prepared using this sheet can reach over 13%, significantly higher than the approximately 5% of existing commercially available products. That is, while maintaining the existing atomization volume, the amount of atomizing agent added during sheet preparation can be reduced by more than 50%, lowering production costs. Simultaneously, the hygroscopicity of the sheet and the cigarette is significantly improved, greatly simplifying the cigarette rolling process and significantly enhancing product quality.

[0043] 2. Thanks to the diatomaceous earth structure, pretreatment process and electric field composite process, the stability of the prepared composite material and the atomizer release efficiency during the suction stage can be further improved in a synergistic way.

[0044] Specific implementation examples

[0045] Using glycerol as the atomizing agent, the following examples are intended to illustrate the present invention, rather than to further limit the scope of protection of the present invention.

[0046] Example 1

[0047] Diatomaceous earth A (macropore content 20-25 vol%, mesopore content 60-65 vol%) was soaked in 0.5 M sodium hydroxide aqueous solution and treated under microwave at 200 W for 2 hours. Then, solid-liquid separation was performed to obtain diatomaceous earth B.

[0048] 60g of glycerol and 80g of diatomaceous earth B were mixed evenly and activated in an electrostatic field (voltage 2kV) for 0.5h to prepare a glycerol-diatomaceous earth composite material. 500g of tobacco powder (200 mesh), 50g of fiber, 20g of guar gum, and 1000g of water were added and stirred evenly. Air bubbles were removed under negative pressure, and the mixture was then evenly coated onto a heated steel belt, dried, and peeled off. The glycerol content in the sheet was measured to be 8%. The sheet was cut into 1.0mm wide tobacco shreds and rolled into heated cigarettes. The hygroscopicity, smoke volume, and glycerol utilization rate in the sheet and smoke of the cigarettes are shown in Appendix Table 1.

[0049] Example 2

[0050] Diatomaceous earth A (macropore content 20-25 vol%, mesopore content 60-65 vol%) was soaked in 1M sodium hydroxide aqueous solution and treated under microwave at 250W for 1 hour, followed by solid-liquid separation to obtain diatomaceous earth C.

[0051] 60g of glycerol and 120g of diatomaceous earth C were mixed evenly and activated in an electrostatic field (1kV) for 1 hour to prepare a glycerol-diatomaceous earth composite material. 500g of tobacco powder (200 mesh), 50g of fiber, 20g of guar gum, and 1000g of water were added and stirred evenly. Air bubbles were removed under negative pressure, and the mixture was then evenly coated onto a heated steel belt, dried, and peeled off. The glycerol content in the sheet was measured to be 7%. The sheet was cut into 1.0mm wide tobacco shreds and rolled into heated cigarettes. The hygroscopicity, smoke volume, and glycerol utilization rate in the sheet and smoke of the cigarettes are shown in Appendix Table 1.

[0052] Example 3

[0053] Compared with Example 1, the only difference is that the diatomaceous earth A was not subjected to microwave alkali pretreatment; all other operations and parameters are the same as in Example 1.

[0054] Example 4

[0055] Compared with Example 1, the only difference is that no electric field was used to assist in the recombination stage; the other operations and parameters are the same as in Example 1.

[0056] Comparative Example 1

[0057] Compared with Example 1, the only difference is that diatomaceous earth is not used; all other operations and parameters are the same as in Example 1.

[0058] Comparative Example 2

[0059] Compared to Example 1, the only difference is that the diatomaceous earth and glycerin were not pre-combined; instead, all components were mixed together. For example, 60g of glycerol, 500g of tobacco powder (200 mesh), 50g of fiber, 20g of guar gum, and 80g of diatomaceous earth B were dissolved in 1000g of water, stirred evenly, and the air bubbles were removed under negative pressure. The mixture was then evenly coated onto a heated steel belt, dried, and peeled off. The glycerol content in the sheet was measured to be 20%. The sheet was cut into 1.0mm wide tobacco shreds and rolled into heated cigarettes. The hygroscopicity, smoke volume, and glycerol utilization rate in the sheet and smoke of the cigarettes are shown in Appendix Table 1.

[0060] Comparative Example 3

[0061] Compared with Example 1, the only difference is that the amount of diatomaceous earth B remains the same, the weight of glycerol is twice the weight of diatomaceous earth B, and other operations and parameters are the same as in Example 1.

[0062] Performance tests were conducted on the materials for each case study, for example:

[0063] Moisture absorption rate: At 22℃ and 50% humidity, the sheet is placed for 24 hours and then weighed. The increase in weight is the moisture absorption rate of the sheet.

[0064] Atomizing agent transfer rate: Take thin film before and after heating and suction respectively, extract with solvent, and measure the atomizing agent content with GC-MS. The percentage of the difference between the two values ​​relative to the atomizing agent content of the thin film before heating is the atomizing agent transfer rate.

[0065] Smoke atomizer utilization rate: The smoke atomizer utilization rate is the percentage of the smoke released under the standard smoking method using Cambridge filters to capture the smoke release. The smoke release is measured by GC-MS and is the percentage of the smoke atomizer content before heating.

[0066] Appendix 1: Performance of Different Heated Cigarettes and Utilization Rate of Atomizing Agents

[0067]

[0068] As shown in Table 1, Examples 1, 1, and 2, pre-combining diatomaceous earth and glycerol can effectively reduce the moisture absorption rate. Furthermore, further microwave pretreatment of diatomaceous earth and compounding under voltage can further control and reduce the moisture absorption rate, and significantly improve the transfer rate and utilization rate of the atomizing agent.

Claims

1. A composite material of atomizing agent@diatomaceous earth, characterized in that, This includes diatomaceous earth with mesoporous and macroporous structures, and atomizing agents filling the pore structure of diatomaceous earth. The weight ratio of diatomaceous earth to atomizing agent is 1-4:1; the diatomaceous earth contains 20-25% macropores and 60-65% mesopores. The preparation method of the atomizing agent@diatomite composite material is as follows: the atomizing agent and diatomite are mixed, and the atomizing agent is filled into the pore structure of the diatomite to obtain the atomizing agent@diatomite composite material. Before mixing, the diatomaceous earth is pretreated in an alkaline solution with microwave assistance. The atomizing agent and diatomaceous earth were premixed and then compounded under an applied DC electric field to obtain the atomizing agent@diatomaceous earth composite material. The voltage of the DC electric field is 1~5kV; the recombination time under electric field assistance is 0.5~1h.

2. The atomizing agent@diatomaceous earth composite material as described in claim 1, characterized in that, In diatomaceous earth, the pore size of the macropores is 1~50μm; The particle size of diatomaceous earth is 20~400 mesh.

3. The atomizing agent@diatomaceous earth composite material as described in claim 1, characterized in that, The atomizing agent is at least one of glycerol and propylene glycol.

4. A method for preparing the atomizing agent@diatomite composite material according to any one of claims 1 to 3, characterized in that, The atomizing agent and diatomaceous earth are mixed, and the atomizing agent fills the pore structure of the diatomaceous earth to obtain the atomizing agent@diatomaceous earth composite material. Before mixing, the diatomaceous earth is pretreated in an alkaline solution with microwave assistance. The atomizing agent and diatomaceous earth are premixed and then compounded under an applied DC electric field to obtain the atomizing agent@diatomaceous earth composite material.

5. The preparation method of the atomizing agent@diatomite composite material as described in claim 4, characterized in that, The alkaline solution is an aqueous solution of an alkali metal hydroxide with a solute concentration of 0.1~3 mol / L; The pretreatment time is 0.5~3 hours.

6. The application of the atomizing agent@diatomite composite material according to any one of claims 1 to 3 or the atomizing agent@diatomite composite material prepared by the preparation method according to any one of claims 4 to 5, characterized in that, It is used as an atomizing additive in the preparation of heated non-combustible cigarettes.

7. The application as described in claim 6, characterized in that, It is used as an atomizing additive in the preparation of tobacco sheets for heated, non-combustible cigarettes.

8. The application as described in claim 7, characterized in that, Tobacco sheets for heating non-combustible cigarettes were prepared using the slurry method.

9. The application as described in claim 8, characterized in that, The atomizing agent@diatomite composite material, tobacco powder, adhesive, and fiber are slurried with water, and then tobacco sheets are prepared by a thick slurry process.

10. The application as described in any one of claims 6 to 9, characterized in that, In the tobacco sheet of heated non-combustible cigarettes, the content of the atomizing agent in the atomizing agent@diatomite composite material is 5~10 wt%.

11. A tobacco sheet for heating non-combustible cigarettes, characterized in that, The atomizing agent@diatomite composite material according to any one of claims 1 to 3 or the atomizing agent@diatomite composite material prepared by the preparation method according to any one of claims 4 to 5 is added.

12. The tobacco sheet for heating non-combustible cigarettes as described in claim 11, characterized in that, In the tobacco sheet of heated non-combustible cigarettes, the content of the atomizing agent in the atomizing agent@diatomite composite material is 5~10 wt%.

13. A heated non-combustible cigarette, characterized in that, It includes the tobacco sheet as described in any one of claims 11 to 12.

Images