Method for reducing use amount of atomizing agent in heat-not-burn cigarette

Abstract

The invention discloses a method for reducing the use amount of an atomizing agent in a heat-not-burn cigarette. A mixture of a propylene glycol ester compound and a propylene glycol acetal derivative is adopted to replace part of propylene glycol to serve as the atomizing agent of the heat-not-burn cigarette. According to the method, the propylene glycol derivative is adopted to replace propylene glycol, the problem that the reconstituted tobacco is high in hygroscopicity can be well solved, the propylene glycol derivative can be subjected to thermal cracking at the use temperature of the heated cigarette to generate propylene glycol and small-molecule flavor substances, and it is guaranteed that the smoke amount of the heated cigarette is not reduced in the smoking process. In addition, gradual release of fragrance of different components is achieved, the uncomfortable taste caused by mass use of propylene glycol is weakened, the puff-by-puff release consistency of the fragrance components of the heat-not-burn cigarette is improved, and technical support is provided for development of heat-not-burn tobacco products.

Description

Technical Field

[0001] The present invention relates to the field of cigarette processing, and more particularly to a method for reducing the amount of atomizer used in heat-not-burn cigarettes. Background Art

[0002] Heat-not-burn cigarettes (HNB) are a new type of tobacco product that uses a heat source to heat cigarette heating rods made of recycled tobacco materials, generating smoke for consumers to inhale at temperatures below 350°C. The aerosol produced contains fewer toxic substances than traditional tobacco products.

[0003] Reconstituted tobacco (also known as reconstituted tobacco leaves) is a porous carbohydrate material. Storage conditions and relative humidity can easily affect its moisture content, significantly impacting the quality of heat-not-burn (HNB) tobacco products. Propylene glycol and glycerol are used as aerosols in HNB cigarettes, accounting for up to 20%-30% or even over 40% of the tobacco mass. However, due to their strong hygroscopicity, reconstituted tobacco leaves are often exposed to relatively high humidity (RH) for extended periods. Excessive moisture content can accelerate product quality deterioration and even mold.

[0004] Therefore, how to reduce the use of propylene glycol and glycerol in heat-not-burn cigarettes has become an urgent problem to be solved in the tobacco industry. Summary of the Invention

[0005] An object of the present invention is to provide a new technical solution for reducing the amount of propylene glycol and glycerol used in heat-not-burn cigarettes.

[0006] According to a first aspect of the present invention, a method for reducing the amount of atomizer used in heat-not-burn cigarettes is provided.

[0007] The method for reducing the amount of atomizer used in heat-not-burn cigarettes adopts a mixture of a propylene glycol ester compound and a propylene glycol acetal derivative to replace part of propylene glycol as the atomizer of the heat-not-burn cigarettes.

[0008] Optionally, the propylene glycol ester compound is at least one of propylene glycol benzoate and propylene glycol cinnamate, and the propylene glycol acetal derivative is at least one of benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotrope aldehyde propylene glycol acetal.

[0009] Optionally, the mixture comprises propylene glycol monobenzoate, propylene glycol monocinnamate, benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotrope propylene glycol acetal.

[0010] Optionally, the mass ratio of the propylene glycol monobenzoate to the propylene glycol monocinnamate is 1:1, and the mass ratio of the benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotropein propylene glycol acetal is 1:1:1.

[0011] Optionally, the mass ratio of the propylene glycol monobenzoate, propylene glycol monocinnamate, benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotrope aldehyde propylene glycol acetal is (0.085-0.17):(0.085-0.17):(0.114-0.17):(0.114-0.17):(0.114-0.17).

[0012] Optionally, the mass ratio of the propylene glycol monobenzoate, the propylene glycol monocinnamate, the benzaldehyde propylene glycol acetal, the vanillin propylene glycol acetal and the heliotropin propylene glycol acetal is 0.085:0.085:0.17:0.17:0.17.

[0013] Optionally, the replacement ratio of propylene glycol is 30wt%-40wt%.

[0014] This application utilizes propylene glycol derivatives as a replacement for propylene glycol, effectively addressing the high hygroscopicity of reconstituted tobacco leaves. Furthermore, the propylene glycol derivatives undergo thermal decomposition at the operating temperature of heated cigarettes to produce propylene glycol and small-molecule flavoring substances, ensuring that the smoke volume of heated cigarettes does not decrease during smoking. Furthermore, this approach achieves a gradual release of different aroma components, mitigating the unpleasant taste associated with high-volume propylene glycol use and improving the consistency of aroma release from puff to puff in heat-not-burn (HNB) cigarettes, providing technical support for the development of HNB tobacco products.

[0015] Further features and advantages of the present invention will become apparent from the following detailed description of exemplary embodiments of the present invention with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

[0017] Figure 1 and Figure 2 These are the test results of moisture content on dry basis of reconstituted tobacco leaves at different times.

[0018] Figure 3 These are the smoke volume test results when propylene glycol is used as a single replacement compound at different proportions.

[0019] Figure 4 The results show the smoke volume test results of different proportions of composite atomizers in thick pulp method reconstituted tobacco leaves. DETAILED DESCRIPTION

[0020] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that unless otherwise specifically stated, the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention.

[0021] The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.

[0022] Technologies, methods, and equipment known to ordinary technicians in the relevant art may not be discussed in detail, but where appropriate, the technologies, methods, and equipment should be considered part of the specification.

[0023] In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not limiting. Therefore, other examples of the exemplary embodiments may have different values.

[0024] Synthetic propylene glycol ester compounds

[0025] Propylene glycol, benzoyl chloride, DMAP, and triethylamine were stirred in a round-bottom flask containing 2.5 mL of anhydrous dichloromethane at a ratio of 1 mmol:0.5 mmol:2.0 mmol:0.5 mmol for 4 hours. The reaction was monitored by thin-layer chromatography. After all starting materials disappeared, 20 mL of water was added to the round-bottom flask to terminate the reaction. The reaction solution was then poured into a separatory funnel. The aqueous layer was extracted twice with ethyl acetate. The ester layer was extracted once with 20 mL of 1 mol / L HCl and once with 20 mL of saturated NaCl solution. The mixture was dried over anhydrous Na₂SO₄ for 24 hours, filtered, and dried by spin-drying. The mixture was then purified by recrystallization and column chromatography to obtain various high-purity propylene glycol esters. The crude product was purified by silica gel column chromatography (V (petroleum ether):V (ethyl acetate) = 1:1) to obtain light yellow liquid compounds 1a (propylene glycol benzoate monoester) (yield 63%) and 2a (propylene glycol benzoate diester) (yield 15%).

[0026] By replacing benzoyl chloride with cinnamoyl chloride and following the same procedures as above, compounds 1b propylene glycol monocinnamate (yield 61%) and 2b propylene glycol diester cinnamate (yield 20%) were obtained.

[0027] Effects of propylene glycol ester compounds and propylene glycol acetal derivatives on the hygroscopicity of reconstituted tobacco leaves

[0028] First, reconstituted tobacco leaves were shredded and passed through a 20-mesh sieve to remove fines. The shredded reconstituted tobacco leaves were then placed in a constant temperature and humidity chamber at 22 ± 1°C and 40 ± 2% relative humidity for 48 hours to reach equilibrium. 20 mg of each propylene glycol compound (propylene glycol ester compound and / or propylene glycol acetal derivative) was weighed and added to distilled water to make a 1.2% solution. The propylene glycol solution was evenly sprayed onto the surface of the reconstituted tobacco until the propylene glycol content reached 0.4% of the total weight of the tobacco (5 g). A control group was also sprayed with the same mass of propylene glycol and distilled water. The moisture content (also known as dry basis moisture content) of the reconstituted tobacco leaves was determined according to "YC / T31-1996 Preparation and Moisture Determination of Tobacco and Tobacco Products Samples."

[0029] The hygroscopicity and moisture retention of reconstituted tobacco sprayed with propylene glycol ester compounds were tested. Figure 1 As shown. From ( Figure 1 a and Figure 1 c) (relative humidity is 84%). It can be seen that under high humidity conditions, the humectant has good hydrophilicity, so that the initial moisture content of the reconstituted tobacco shreds with the addition of the humectant is higher than that of the blank tobacco shreds. During the moisture absorption process, the moisture content of the tobacco shreds slowly increased in the first 20 hours, and then showed a linear upward trend with the passage of time. It gradually slowed down after 80 hours and tended to equilibrium at 100 hours. When equilibrium was reached, the dry basis moisture content of the tobacco shreds with different humectants added was in the following order from high to low: propylene glycol>1a>2a>blank, propylene glycol>1b>2b>blank (1a is propylene glycol monoester of benzoic acid, 2a is propylene glycol diester of benzoic acid, 1b is propylene glycol monoester of cinnamic acid, and 2b is propylene glycol diester of cinnamic acid). As ( Figure 1 b and Figure 1 As shown in Figure d (relative humidity 32%), the moisture content of the cut tobacco samples at 32% relative humidity decreases with increasing desorption time. All samples show a nearly identical downward trend within the first 6 hours, before reaching equilibrium at 100 hours. The order of moisture content from high to low at this point is consistent with the results from the high-humidity environment.

[0030] from Figure 1 Overall, the moisturizing and hygroscopic capacities of 1a (propylene glycol monobenzoate) and 1b (propylene glycol monocinnamate) are higher than those of the control group, but lower than those of propylene glycol. This is because the highly hygroscopic propylene glycol binds water molecules through hydrogen bonds, enhancing the tobacco's affinity for water and its adsorption capacity. Compared to glycerol, 1a and 1b have fewer hydroxyl groups, resulting in fewer hydrogen bonds. Furthermore, the hydrophobic effect of the ester bonds significantly weakens the tobacco's water absorption capacity, reducing the strong hygroscopicity of propylene glycol while maintaining a certain degree of moisture-proofing and moisture-retaining properties.

[0031] The hygroscopicity and moisture retention of reconstituted tobacco sprayed with propylene glycol acetal derivatives (7a is benzaldehyde propylene glycol acetal, 7b is vanillin propylene glycol acetal, and 7c is heliotropin propylene glycol acetal, all of which are commercially available analytically pure samples) were tested. The results are as follows: Figure 2 As shown ( Figure 2 The relative humidity of a is 84%, Figure 2 The relative humidity of b is 32%). During the moisture absorption process, the moisture content of tobacco cut slowly increased in the first 20 h, and then showed a linear upward trend with the passage of time. It gradually slowed down after 80 h and reached equilibrium at 100 h. Figure 2 The moisture content in sample b) decreases with increasing desorption time, with all samples showing a nearly identical downward trend within the first 6 hours before reaching equilibrium after 100 hours. Propylene glycol, a traditional humectant, binds water molecules through hydrogen bonding, enhancing the tobacco's water adsorption capacity and increasing its moisture content. Compared to propylene glycol, propylene glycol acetal compounds 7a, 7b, and 7c (7a is benzaldehyde propylene glycol acetal, 7b is vanillin propylene glycol acetal, and 7c is heliotrope aldehyde propylene glycol acetal) have fewer hydroxyl groups and hydrogen bonds, significantly reducing propylene glycol's strong hygroscopicity while also exhibiting a certain degree of moisture-proofing and moisturizing properties.

[0032] Effects of Propylene Glycol Compounds on Smoke Yield of Reconstituted Tobacco

[0033] The reconstituted tobacco leaves are produced according to the thick pulp method, and the preparation method can be, for example:

[0034] First, place 10.4 g of outer fiber, 6 g of concentrate, 210 g of water, 10.29 g of glycerol, and 1.71 g of propylene glycol in a blender and stir for 20 minutes. Then, add 1.5 g of sodium carboxymethyl cellulose (CMC) and stir again for 5 minutes. Finally, add 50 g of tobacco powder and stir for 30 minutes. Set the micrometer gauge of the MS-ZN320A laboratory coating machine to 0.7 mm, the coating stroke to 350 mm, and the coating speed to 200 cm / min. Pour the beaten slurry onto the coating machine and apply it. The heating switch automatically heats to 70°C. Wait 5-7 minutes to dry the coated reconstituted tobacco leaves to remove excess moisture. Then, gently remove the leaves from the coating machine with a plastic spatula to obtain the reconstituted tobacco leaves.

[0035] The propylene glycol in the above-mentioned reconstituted tobacco preparation method was partially replaced by the above-mentioned single propylene glycol compound at a ratio of 20%, 30%, 40% and 50% respectively. The rest of the operations were the same to prepare reconstituted tobacco, and the smoke volume was measured. The results are shown in FIG. Figure 3 .

[0036] from Figure 3As can be seen, the smoke volume of all samples increases first and then decreases with the number of puffs. With the exception of the propylene glycol group (b3), smoke volume for all samples reaches its maximum at the second puff and is zero at the fifth puff. Furthermore, when the propylene glycol acetal derivatives 7a, 7b, and 7c are replaced at 20%, 30%, 40%, and 50%, smoke volume drops to zero at the fourth puff. This may be due to the instability of the acetal structure, which causes premature changes during heating and reduces the uniformity of the smoke from puff to puff. As the replacement ratio increases, smoke volume for all samples increases, reaching its maximum at a 40% replacement ratio. However, when the replacement ratio reaches 50%, smoke volume for all samples decreases. This may be due to the low amount of propylene glycol used, resulting in poor smoke generation. When the substitution ratio is 40%, the maximum smoke volume of propylene glycol (b2), glycerol (b3), 1a, 2a, 1b, 2b, 7a, 7b and 7c are 51.3, 77.85, 42.3, 24.88, 43.31, 27.94, 38.71, 43.83 and 39.71.

[0037] According to the test results of the smoke volume of single propylene glycol compounds, propylene glycol ester compounds 1a and 1b with a replacement ratio of 30% to 40% and good smoke volume effect are suitable for compounding with propylene glycol carbonyl condensate compounds 7a, 7b, and 7c.

[0038] Effects of compounded propylene glycol on smoke yield of reconstituted tobacco leaves

[0039] The reconstituted tobacco leaves are produced according to the thick pulp method, and the preparation method can be, for example:

[0040] First, place 10.4 g of outer fiber, 6 g of concentrate, 210 g of water, 10.29 g of glycerol, and 1.71 g of propylene glycol in a blender and stir for 20 minutes. Then, add 1.5 g of sodium carboxymethyl cellulose (CMC) and stir again for 5 minutes. Finally, add 50 g of tobacco powder and stir for 30 minutes. Set the micrometer gauge of the MS-ZN320A laboratory coating machine to 0.7 mm, the coating stroke to 350 mm, and the coating speed to 200 cm / min. Pour the beaten slurry onto the coating machine and apply it. The heating switch automatically heats to 70°C. Wait 5-7 minutes to dry the coated reconstituted tobacco leaves to remove excess moisture. Then, gently remove the leaves from the coating machine with a plastic spatula to obtain the reconstituted tobacco leaves.

[0041] According to the propylene glycol ratio in Table 1, partial replacement was performed and the smoke volume was measured. The results are shown in Figure 4 .

[0042] Table 1. Ratio of fog-forming components (g)

[0043]

[0044] from Figure 4 As can be seen, the smoke production of all samples shows a trend of initially increasing and then decreasing with increasing puff count. Samples 1-1, 1-2, and 1-3 reached peaks of 22.87%, 28.35%, and 33.16% at the 7th puff, respectively. Samples 1-4, 1-5, and 1-6 reached peaks of 77.90%, 64.92%, and 56.45% at the 8th puff. Sample 1-7 reached a peak of 60.75% at the 7th puff. Taking into account the smoke production from puffs 1-9, samples 1-1, 1-2, and 1-3 exhibited the most stable smoke production. Sample 1-4 produced higher smoke production than the control sample DZ from the 5th puff, and sample 1-5 produced higher smoke production than the control sample DZ from the 6th puff. However, their smoke production from puffs 1-2 was lower than that of samples 1-1, 1-2, and 1-3. Analysis of the thermal decomposition of the compounds suggests that this may be due to the higher content of 1,2-propylene glycol in the pyrolysis of the propylene glycol acetal compound compared to the propylene glycol ester compound. Samples 1-4 and 1-5, which have a high proportion of propylene glycol acetal compounds, will pyrolyze more 1,2-propylene glycol to carry in the smoke during the subsequent smoking process.

[0045] Sensory evaluation

[0046] Recipes 1-4 and 1-5, which exhibit relatively high smoke yields, were used to create reconstituted samples A and B, which were then rolled into heated cigarettes. A pure propylene glycol control group, designated CK, was also selected. The smoking test results in Table 2 (according to GB 5606.4-2005, "Cigarettes - Part 4: Sensory Technical Requirements") show that, compared with the control group CK, sample A (recipes 1-4) exhibited a richer aroma profile, higher smoke density, and higher overall smoke volume. The smoke agent exhibited no off-flavor, a refreshing aroma, moderate strength, and good uniformity, resulting in a pleasant and clean aftertaste. Sample B (recipes 1-5) exhibited higher smoke density, a slightly stronger aroma, and a sweet aftertaste. The strength was comparable to the control group, with reduced irritation and better uniformity before and after puffs. Both samples significantly improved the sensory comfort of heated cigarettes compared to the control group.

[0047] Table 2 Sensory quality evaluation score sheet for heated cigarettes

[0048]

[0049] Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the present invention. It should be understood by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the present invention. The scope of the present invention is defined by the appended claims.

Claims

1. A method for reducing the amount of atomizer used in heat-not-burn cigarettes, characterized in that: A mixture of propylene glycol ester compounds and propylene glycol acetal derivatives is used to replace part of propylene glycol as an atomizer for heat-not-burn cigarettes.

2. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to claim 1, characterized in that: The propylene glycol ester compound is at least one of propylene glycol benzoate and propylene glycol cinnamate, and the propylene glycol acetal derivative is at least one of benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotrope aldehyde propylene glycol acetal.

3. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to claim 2, characterized in that: The mixture includes propylene glycol monobenzoate, propylene glycol monocinnamate, benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotrope propylene glycol acetal.

4. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to claim 3, characterized in that: The mass ratio of the propylene glycol monobenzoate to the propylene glycol monocinnamate is 1:1, and the mass ratio of the benzaldehyde propylene glycol acetal, vanillin propylene glycol acetal and heliotropein propylene glycol acetal is 1:1:

1.

5. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to claim 4, characterized in that: The mass ratio of the propylene glycol monoester of benzoic acid, the propylene glycol monoester of cinnamic acid, the benzaldehyde propylene glycol acetal, the vanillin propylene glycol acetal and the heliotropin propylene glycol acetal is (0.085-0.17):(0.085-0.17):(0.114-0.17):(0.114-0.17):(0.114-0.17).

6. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to claim 5, characterized in that: The mass ratio of the propylene glycol monoester of benzoic acid, the propylene glycol monoester of cinnamic acid, the benzaldehyde propylene glycol acetal, the vanillin propylene glycol acetal and the heliotropin propylene glycol acetal is 0.085:0.085:0.17:0.17:0.

17.

7. The method for reducing the amount of atomizer used in heat-not-burn cigarettes according to any one of claims 1 to 6, characterized in that: The replacement ratio of propylene glycol is 30wt%-40wt%.

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