An aerogel with the function of encapsulating a smoke-generating agent, its preparation method and application
By preparing an aerogel-loaded smoke-generating agent with a nano-protrusion structure, the problem of strong hygroscopicity of smoke-generating agents in heated cigarettes was solved, thereby improving the smoke output and storage stability, reducing the ammonia content in the smoke, and improving the consumer experience.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGSU XINYUAN TOBACCO SHEET CO LTD
- Filing Date
- 2023-08-08
- Publication Date
- 2026-05-26
AI Technical Summary
The smoking agents used in existing heated cigarettes, such as glycerol and propylene glycol, are highly hygroscopic, which leads to a decline in quality after storage, affects the compatibility of cigarettes and smoking devices, and affects the smoking effect and consumer experience when the dosage is high or low.
Aerogels were prepared using xanthan gum, sodium carboxymethyl cellulose, copper nitrate, and magnesium nitrate. A nano-protrusion structure was formed through complexation to load a smoke-generating agent. The ammonia content in the flue gas was reduced by adsorbing the ammonia using bimetallic oxides.
While reducing the amount of smoke-generating agent, it improves storage stability, reduces the ammonia content of harmful substances in the smoke, and enhances the consumer experience.
Smart Images
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of heated cigarette technology, specifically relating to an aerogel with the function of encapsulating a smoke-generating agent, its preparation method, and its application. Background Technology
[0002] Heated cigarettes, as a promising new type of tobacco product, can effectively reduce environmental pollution and lower the potential health risks associated with smoking, making them one of the important directions for future tobacco product development. Heated cigarettes attract attention because they produce smoke through heating rather than combustion, providing smokers with the aroma and satisfaction of tobacco. Therefore, to simulate the "smoke-generating" effect of traditional cigarettes, a certain proportion of smoke-generating agents needs to be added during the manufacturing process.
[0003] However, commonly used smoke-generating agents such as glycerol and propylene glycol are highly hygroscopic, which leads to a decline in processing quality and makes them difficult to store.
[0004] CN 113647666A discloses a method for preparing heated cigarettes. Addressing the problem that adding tobacco to heated cigarettes can easily cause adverse effects such as dryness and irritation in the throat, this method innovatively uses hydrated organic acid salts as humectants and 1,2-propanediol and glycerin as smoking agents to prepare tobacco specifically for heated cigarettes. Within the commonly used heating temperature range of below 400℃ for heated cigarettes, moisture is released at specific temperatures depending on the heating device, thus achieving the purpose of controlling the amount of moisture released.
[0005] CN111990681A discloses a smoke-generating particle for a heated non-combustible cigarette and its preparation method. The smoke-generating particle includes a bioactively treated carrier, food additives, and a smoke-generating agent. The carrier includes one or more of the following: gramineous plant particles, gelatin, sodium alginate, diatomaceous earth, methylcellulose, rush chitosan, and lignin. The smoke-generating agent includes one or more of the following: glycerol, pentylene glycol, butylene glycol, glycerol, propylene glycol, diacetate, and trimethylolpropane. The food additives include astragalus extract, licorice powder flavoring, fixative, chocolate flavoring, selenium yeast, and maltose. The smoke-generating particle of this invention is not only harmless to the human body but also has a sweet taste when inhaled, enhancing the user's smoking experience.
[0006] However, the smoke-generating agents added to the heated cigarettes, such as glycerol and propylene glycol, are highly hygroscopic, which leads to a decline in the quality of the heated cigarettes after storage and also affects the compatibility between the cigarettes and smoking devices. Summary of the Invention
[0007] In view of the shortcomings of the prior art, the purpose of this invention is to provide an aerogel with the function of encapsulating a smoke-generating agent, its preparation method and application.
[0008] To achieve this objective, the present invention adopts the following technical solution:
[0009] In a first aspect, the present invention provides an aerogel with the function of encapsulating a smoke-generating agent, wherein the raw materials for preparing the aerogel with the function of encapsulating a smoke-generating agent include xanthan gum, sodium carboxymethyl cellulose, copper nitrate and magnesium nitrate.
[0010] In this invention, both xanthan gum and sodium carboxymethyl cellulose have good biocompatibility. Xanthan gum and sodium carboxymethyl cellulose can form an aerogel through complexation. The aerogel is modified with copper nitrate and magnesium nitrate to have a large number of nano-protrusions, which can effectively support the smoke-generating agents and other materials in heated cigarettes. Moreover, the aerogel has a good adsorption effect on ammonia, a harmful substance in heated cigarette smoke. The aerogel obtained by this invention has a small pore diameter and numerous pores, resulting in poor internal gas flow. However, when the smoke passes through the gel, it is confined inside the material until adsorption saturation. The bimetallic oxide in the gel can form a complex with ammonia in heated cigarette smoke, thereby effectively reducing the ammonia content. In addition, the surface of the bimetallic oxide is rich in a large number of hydroxyl groups, which can also achieve ammonia adsorption through hydrogen bonding with NH3.
[0011] Preferably, the mass ratio of xanthan gum, sodium carboxymethyl cellulose, copper nitrate, and magnesium nitrate is (0.5-3):(1-10):(15-25):(20-30).
[0012] "0.5-3" can be 0.6, 0.8, 1, 1.2, 1.4, 16, 1.8, 2, 2.2, 2.4, 2.6, or 2.8, etc.
[0013] "1-10" can be 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, etc.
[0014] "15-25" can be 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25, etc.
[0015] "20-30" can be 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30, etc.
[0016] Preferably, the copper nitrate comprises copper nitrate pentahydrate.
[0017] Preferably, the magnesium nitrate comprises magnesium nitrate hexahydrate.
[0018] Other specific point values within the range of the above values can be selected, and will not be elaborated on here.
[0019] In a second aspect, the present invention provides a method for preparing an aerogel with the function of encapsulating a smoke-generating agent as described in the first aspect, the preparation method comprising:
[0020] (1) Xanthan gum and sodium carboxymethyl cellulose were mixed in deionized water, and after being uniformly mixed, the mixture was allowed to stand and then freeze-dried to obtain a mixed aerogel.
[0021] (2) Mix copper nitrate and magnesium nitrate in deionized water, then add the mixed aerogel obtained in step (1), sonicate and heat to react, cool and vacuum dry to obtain the product.
[0022] Preferably, the solid-liquid ratio of xanthan gum to deionized water in step (1) is 1:(250-350)g / mL, for example, it can be 1:260g / mL, 1:270g / mL, 1:280g / mL, 1:290g / mL, 1:300g / mL, 1:310g / mL, 1:320g / mL, 1:330g / mL or 1:340g / mL, etc.
[0023] Preferably, the mixing in step (1) is performed under ultrasonic conditions.
[0024] Preferably, the temperature during the standing period in step (1) is -5 to 0℃ (e.g., -4℃, -3℃, -2℃ or -1℃, etc.), and the time is 0.5 to 1.5h (e.g., 0.6h, 0.8h, 1h, 1.2h or 1.4h, etc.).
[0025] Preferably, after standing, the freezing is carried out at -85 to -75°C for 1-3 hours, for example, the temperature can be -84°C, -82°C, -80°C, -78°C or -76°C, and the time can be 1.2h, 1.5h, 1.8h, 2h, 2.2h, 2.5h or 2.8h.
[0026] Preferably, the freeze-drying method in step (1) is vacuum freeze-drying.
[0027] Preferably, the vacuum degree during vacuum freeze drying is 0-30 Pa, for example, it can be 5 Pa, 10 Pa, 15 Pa, 20 Pa or 25 Pa.
[0028] Preferably, the vacuum freeze-drying process is carried out at a temperature of -10 to 0°C for 20 to 30 hours. For example, the temperature can be -9°C, -7°C, -5°C, -3°C, or -1°C, and the time can be 21 hours, 23 hours, 25 hours, 27 hours, or 29 hours.
[0029] Preferably, the solid-liquid ratio of copper nitrate to deionized water in step (2) is 1:(40-60)g / mL, for example, it can be 1:42g / mL, 1:44g / mL, 1:46g / mL, 1:50g / mL, 1:52g / mL, 1:54g / mL, 1:56g / mL or 1:58g / mL, etc.
[0030] Preferably, the ultrasonic treatment time in step (2) is 50-70 min, for example, it can be 52 min, 54 min, 56 min, 58 min, 60 min, 62 min, 64 min, 66 min or 68 min, etc.
[0031] Preferably, after the ultrasonic treatment in step (2), the pH of the system is adjusted to 9.5-11, for example, it can be 9.8, 10, 10.2, 10.5 or 10.8.
[0032] Preferably, after adjusting the pH, the ultrasonic treatment continues for 20-40 minutes, for example, 22 minutes, 24 minutes, 26 minutes, 28 minutes, 30 minutes, 32 minutes, 34 minutes, 36 minutes, or 38 minutes.
[0033] Preferably, the heating reaction in step (2) is carried out at a temperature of 140-160℃ for 20-30 hours. For example, the temperature can be 142℃, 145℃, 148℃, 150℃, 152℃, 155℃ or 158℃, and the time can be 21 hours, 23 hours, 25 hours, 27 hours or 29 hours.
[0034] Preferably, the cooling to 25-35°C in step (2) can be, for example, 26°C, 28°C, 30°C, 32°C or 34°C.
[0035] Preferably, the product needs to be cleaned after cooling.
[0036] Preferably, the cleaning solution used in the cleaning process is DMF and / or anhydrous methanol.
[0037] Preferably, the vacuum degree during vacuum drying is 0-30 Pa, for example, it can be 5 Pa, 10 Pa, 15 Pa, 20 Pa or 25 Pa.
[0038] Preferably, the vacuum drying temperature is 20-30℃ and the time is 12-18h. For example, the temperature can be 21℃, 23℃, 25℃, 27℃ or 29℃, and the time can be 13h, 14h, 15h, 16h or 17h.
[0039] Other specific point values within the range of the above values can be selected, and will not be elaborated on here.
[0040] Thirdly, the present invention provides an application of an aerogel with the function of encapsulating a smoke-generating agent as described in the first aspect in the preparation of heated cigarettes.
[0041] Using a smoke-generating agent in heated cigarettes can simulate the "smoke-generating" effect of traditional cigarettes. However, if the amount used is too low, the "smoke-generating" effect of heated cigarettes is poor, which affects the consumer's experience. If the amount used is too high, it can easily increase the hygroscopicity of heated cigarettes, which will affect the appearance quality and make them difficult to store. The aerogel of the present invention, which has the function of encapsulating smoke-generating agents, can reduce the amount of smoke-generating agent used when used in heated cigarettes without reducing the amount of smoke generated by heated cigarettes. It also has a significant adsorption effect on ammonia, a harmful substance in the smoke.
[0042] Preferably, the method of application includes mixing a smoke-generating agent with an aerogel that has the function of encapsulating the smoke-generating agent, coating it on tobacco sheets, cutting it into shreds, and then loading it into heated cigarette segments.
[0043] Preferably, the mass ratio of the smoke-generating agent to the aerogel with the function of encapsulating the smoke-generating agent is 1:(1-3), for example, it can be 1:1.2, 1:1.5, 1:1.8, 1:2, 1:2.2, 1:2.5 or 1:2.8, etc.
[0044] Preferably, the smoke-generating agent comprises any one or a combination of at least two of glycerol, 1,2-propanediol, or 1,3-butanediol.
[0045] Preferably, the mixture is dissolved in an aqueous ethanol solution after mixing.
[0046] Preferably, the concentration of the ethanol aqueous solution is 50-60%, for example, it can be 51%, 53%, 55%, 57% or 59%, etc.
[0047] Preferably, the solid-liquid ratio of the mixture to the aqueous ethanol solution is 1:(10-20)g / mL, for example, it can be 1:11g / mL, 1:12g / mL, 1:13g / mL, 1:14g / mL, 1:15g / mL, 1:16g / mL, 1:17g / mL, 1:18g / mL or 1:19g / mL, etc.
[0048] Preferably, the mixture accounts for 15-20% of the total amount of tobacco sheets, for example, it can be 15%, 16%, 17%, 18%, 19% or 20%, etc.
[0049] Preferably, after coating, the tobacco sheet is left to stand until the ethanol evaporates before being shredded.
[0050] Other specific point values within the range of the above values can be selected, and will not be elaborated on here.
[0051] Compared with the prior art, the present invention has the following beneficial effects:
[0052] (1) In this invention, xanthan gum and sodium carboxymethyl cellulose both have good biocompatibility. Xanthan gum and sodium carboxymethyl cellulose can form an aerogel through complexation. The aerogel is modified with copper nitrate and magnesium nitrate, so that the aerogel has more nano-protrusion structures, which can well support the smoke-generating agents and other materials in heated cigarettes.
[0053] (2) The aerogel of the present invention has a good adsorption effect on ammonia, a harmful substance in heated cigarette smoke. The aerogel has small pore diameter and numerous pores, resulting in poor internal gas flow. However, when the smoke passes through the gel, it is confined inside the material until the adsorption is saturated. The bimetallic oxide in the gel can form a complex with ammonia in heated cigarette smoke, thereby effectively reducing the ammonia content. In addition, the surface of the bimetallic oxide is rich in a large number of hydroxyl groups, which can also achieve ammonia adsorption through hydrogen bonding with NH3.
[0054] (3) The preparation method of the aerogel with the function of encapsulating smoke-generating agent involved in this invention is simple and easy to operate, and is very suitable for industrial application. Detailed Implementation
[0055] To further illustrate the technical means and effects of the present invention, the following describes the technical solution of the present invention in conjunction with preferred embodiments of the present invention. However, the present invention is not limited to the scope of the embodiments.
[0056] All raw materials used in the embodiments of this invention can be purchased through commercial channels.
[0057] Example 1
[0058] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0059] (1) Weigh 0.1g xanthan gum and 0.5g sodium carboxymethyl cellulose and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0060] (2) Disperse 2.33g copper nitrate pentahydrate and 2.56g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0061] Example 2
[0062] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0063] (1) Weigh 0.3g xanthan gum and 0.8g sodium carboxymethyl cellulose into a beaker, slowly add 100mL deionized water and stir thoroughly at 25℃ to dissolve completely, then sonicate to remove air bubbles, and after forming a colorless and transparent gel, transfer it to a 24-well plate, age it at 0℃ for 1.5h, then transfer it to an ultra-low temperature freezer at -85℃ for 1.5h, take it out, and freeze-dry it under vacuum at 25Pa and -8℃ for 20h to obtain a mixed aerogel;
[0064] (2) Disperse 1.83g copper nitrate pentahydrate and 2.85g magnesium nitrate hexahydrate in 90mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 70 minutes. Then add sodium hydroxide to adjust the pH of the solution to 11 and continue sonication for 20 minutes. After sonication, heat the system to 140℃ and react for 30 hours. After cooling to 25℃, wash away the unreacted substances with DMF and vacuum dry at 25Pa and 20℃ for 15 hours to obtain the aerogel with the function of encapsulating smoke generator.
[0065] Example 3
[0066] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0067] (1) Weigh 0.2g xanthan gum and 0.6g sodium carboxymethyl cellulose into a beaker, slowly add 50mL deionized water and stir thoroughly at 30℃ to dissolve completely, then sonicate to remove air bubbles, and after forming a colorless and transparent gel, transfer it to a 24-well plate, age it at -3℃ for 0.8h, then transfer it to an ultra-low temperature freezer at -75℃ for 3h, take it out, and freeze-dry it under vacuum at 10Pa and -10℃ for 30h to obtain a mixed aerogel;
[0068] (2) Disperse 2.05g copper nitrate pentahydrate and 2.12g magnesium nitrate hexahydrate in 120mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 50 minutes. Then add sodium hydroxide to adjust the pH of the solution to 9.5 and continue sonication for 35 minutes. After sonication, heat the system to 155℃ and react for 20 hours. After cooling to 35℃, wash away the unreacted substances with anhydrous methanol and vacuum dry at 10Pa and 25℃ for 18 hours to obtain the aerogel with the function of encapsulating smoke generator.
[0069] Example 4
[0070] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0071] (1) Weigh 0.4g xanthan gum and 0.1g sodium carboxymethyl cellulose and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0072] (2) Disperse 2.85g copper nitrate pentahydrate and 1.83g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0073] Example 5
[0074] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0075] (1) Weigh 0.1g xanthan gum and 1.1g sodium carboxymethyl cellulose into a beaker, slowly add 30mL deionized water and stir thoroughly at 25℃ to dissolve completely, then sonicate to remove air bubbles, and after forming a colorless and transparent gel, transfer it to a 24-well plate, age it at -5℃ for 1h, then transfer it to an ultra-low temperature freezer at -80℃ for 2h, take it out, and freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel;
[0076] (2) Disperse 1.25g copper nitrate pentahydrate and 3.30g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0077] Example 6
[0078] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0079] 2.33 g of copper nitrate pentahydrate and 2.56 g of magnesium nitrate hexahydrate were dispersed in 100 mL of deionized water and stirred magnetically to obtain a homogeneous solution. 0.1 g of xanthan gum and 0.5 g of sodium carboxymethyl cellulose were added to the solution and sonicated for 60 minutes. Then, sodium hydroxide was added dropwise to adjust the pH of the solution to 10, and sonication was continued for 30 minutes. After sonication, the system was heated to 150 °C and reacted for 24 hours. After cooling to 30 °C, unreacted substances were washed away with DMF and anhydrous methanol. After vacuum drying at 15 Pa and 25 °C for 12 hours, the aerogel with the function of encapsulating smoke-generating agent was obtained.
[0080] Example 7
[0081] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0082] (1) Weigh 0.1g xanthan gum, 0.5g carboxymethyl cellulose, 2.33g copper nitrate pentahydrate and 2.56g sodium magnesium nitrate hexahydrate and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After forming a colorless and transparent gel, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain the aerogel with the function of encapsulating smoke-generating agent.
[0083] Example 8
[0084] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0085] (1) Weigh 0.1g xanthan gum and 0.5g sodium carboxymethyl cellulose into a beaker, slowly add 30mL deionized water and stir thoroughly at 25℃ to dissolve completely, then sonicate to remove air bubbles, and after forming a colorless and transparent gel, transfer it to a 24-well plate, age it at -5℃ for 1h, and then freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel;
[0086] (2) Disperse 2.33g copper nitrate pentahydrate and 2.56g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0087] Example 9
[0088] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0089] (1) Weigh 0.1g xanthan gum and 0.5g sodium carboxymethyl cellulose and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0090] (2) Disperse 2.33g copper nitrate pentahydrate and 2.56g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. After sonication, heat the system to 150℃ and react for 24h. After cooling to 30℃, wash away unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12h, obtain the aerogel with the function of encapsulating smoke generator.
[0091] Comparative Example 1
[0092] This comparative example provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0093] (1) Weigh 0.1g xanthan gum and 0.5g sodium carboxymethyl cellulose and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0094] (2) Disperse 2.89g of copper nitrate pentahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonication for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0095] Comparative Example 2
[0096] This comparative example provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0097] (1) Weigh 0.1g xanthan gum and 0.5g sodium carboxymethyl cellulose and place them in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0098] (2) Disperse 2.89g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0099] Comparative Example 3
[0100] This comparative example provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0101] (1) Weigh 0.6g xanthan gum into a beaker, slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve it completely. Then, sonicate to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ for 2h and take it out. Then, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0102] (2) Disperse 2.33g copper nitrate pentahydrate and 2.56g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0103] Comparative Example 4
[0104] This embodiment provides an aerogel with the function of encapsulating a smoke-generating agent. The preparation method of the aerogel with the function of encapsulating a smoke-generating agent is as follows:
[0105] (1) Weigh 0.6g sodium carboxymethyl cellulose and place it in a beaker. Slowly add 30mL of deionized water and stir thoroughly at 25℃ to dissolve it completely. Then, use sonication to remove air bubbles. After a colorless and transparent gel is formed, transfer it to a 24-well plate and age it at -5℃ for 1h. Then, transfer it to an ultra-low temperature freezer at -80℃ and freeze it for 2h. After taking it out, freeze-dry it under vacuum at 15Pa and -5℃ for 24h to obtain a mixed aerogel.
[0106] (2) Disperse 2.33g copper nitrate pentahydrate and 2.56g magnesium nitrate hexahydrate in 100mL of deionized water and stir magnetically to obtain a uniformly mixed solution. Add the mixed aerogel from step (1) to the solution and sonicate for 60 minutes. Then add sodium hydroxide to adjust the pH of the solution to 10 and continue sonicating for 30 minutes. After sonication, heat the system to 150℃ and react for 24 hours. After cooling to 30℃, wash away the unreacted substances with DMF and anhydrous methanol. After vacuum drying at 15Pa and 25℃ for 12 hours, the aerogel with the function of encapsulating smoke generator is obtained.
[0107] Application Example 1
[0108] This application example provides a heated cigarette, the method for preparing the heated cigarette is as follows:
[0109] (1) Mix 1,3-butanediol with the aerogel with the function of encapsulating smoke generator obtained in Example 1 at a mass ratio of 1:1.25 to obtain a mixture;
[0110] (2) The mixture from step (1) is mixed and dissolved with a 50% ethanol aqueous solution at a solid-liquid ratio of 1:15 g / mL, and then evenly coated onto tobacco sheets (the tobacco sheets are 5 times the mass of the mixture), cut into shreds and loaded into heated cigarette segments to obtain the final product.
[0111] Application Example 2-9
[0112] Application Examples 2-9 provide eight types of heated cigarettes. The only difference between these heated cigarettes and Application Example 1 is that the aerogel with the function of encapsulating smoke-generating agents obtained in Example 1 is replaced in equal amounts with the tobacco polymer aerogel obtained in Examples 2-9. The rest of the methods are consistent with Application Example 1.
[0113] Application Example 10-13
[0114] Application Examples 10-13 provide four types of heated cigarettes. The only difference between these heated cigarettes and Application Example 1 is that in step (1), the mass ratio of 1,3-butanediol to the aerogel with the function of encapsulating the smoke-generating agent obtained in Example 1 is 1:3, 1:1, 1:0.5, and 1:5, respectively. The rest of the method is consistent with Application Example 1.
[0115] Compare and contrast examples 1-4
[0116] Comparative Application Examples 1-4 provide a heated cigarette, which differs from Application Example 1 only in that the aerogel with smoke-generating agent function obtained in Example 1 is replaced in equal amounts with the aerogel with smoke-generating agent function obtained in Comparative Examples 1-4. The rest of the method is the same as Application Example 1.
[0117] Comparative Application Example 5
[0118] This comparative application example provides a heated cigarette, the preparation method of which is as follows:
[0119] 1,3-Butanediol is mixed and dissolved with a 50% aqueous ethanol solution at a solid-liquid ratio of 1:15 g / mL. The solution is then evenly coated onto tobacco sheets (the tobacco sheets are 5 times the mass of 1,3-butanediol). After being shredded, the solution is inserted into heated cigarette segments to obtain the final product.
[0120] Comparative Application Example 6
[0121] This comparative application example provides a heated cigarette, the preparation method of which is as follows:
[0122] 1,3-Butanediol is mixed and dissolved with a 50% aqueous ethanol solution at a solid-liquid ratio of 1:15 g / mL. The solution is then evenly coated onto tobacco sheets (the tobacco sheets are 7 times the mass of 1,3-butanediol). After being shredded, the solution is inserted into heated cigarette segments to obtain the final product.
[0123] Comparative Application Example 7
[0124] This comparative application example provides a heated cigarette, the preparation method of which is as follows:
[0125] 1,3-Butanediol is mixed and dissolved with a 50% aqueous ethanol solution at a solid-liquid ratio of 1:15 g / mL. The solution is then evenly coated onto tobacco sheets (the tobacco sheets are 10 times the mass of 1,3-butanediol). After being shredded, the solution is inserted into heated cigarette segments to obtain the final product.
[0126] Test Example 1
[0127] (1) The heated cigarettes according to Application Examples 1-13 and Comparative Application Examples 1-7 were stored in a constant temperature and humidity chamber at a designed temperature of 25°C and a humidity of 80%rH for 60 days. The appearance was then observed and the standards were as follows:
[0128] Grade A: No yellow spots; Grade B: Spots present; Grade C: Patchy yellow spots present; Grade D: Large yellow spots.
[0129] (2) The ammonia content in cigarettes was determined in accordance with the standard YC / T 377-2019 Determination of ammonia in mainstream cigarette smoke by Cambridge filter trapping-ion chromatography after impregnation treatment.
[0130] (3) The heated cigarettes used in Application Examples 1-13 and Comparative Application Examples 1-7 were smoked. In accordance with the national standard "Sensory Technical Requirements for Cigarettes" (GB5606.4-2005), seven sensory evaluators were organized to conduct sensory evaluations of the heated cigarettes, mainly examining the amount of smoke exhaled from the heated cigarettes under a fixed ambient wind. The above indicators were scored, with the amount of smoke exhaled under ambient wind ranging from 0 to 10 points. The higher the score, the better the feeling or the higher the acceptance of the evaluation indicator during the smoking process.
[0131] The test results are shown in Table 1 below.
[0132] Table 1
[0133]
[0134]
[0135] As can be seen from the data in Table 1, the aerogel of the present invention, which has the function of encapsulating smoke-generating agent, can reduce the amount of smoke-generating agent used without reducing the sensory experience of heated cigarettes. The reduction in the amount of smoke-generating agent can reduce the "moisture absorption" of heated cigarettes, thereby increasing their storage time. Furthermore, the ammonia content in heated cigarette smoke is also significantly reduced after adding the aerogel of the present invention.
[0136] The applicant declares that this invention illustrates an aerogel with encapsulated smoke-generating agent function, its preparation method, and its application through the above embodiments. However, this invention is not limited to the above embodiments, meaning that this invention does not necessarily rely on the above embodiments for implementation. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials, additions of auxiliary components, and selection of specific methods, etc., all fall within the protection and disclosure scope of this invention.
[0137] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details of the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.
[0138] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.
Claims
1. A method for preparing an aerogel with the function of encapsulating a smoke-generating agent, characterized in that, The preparation method includes: (1) Xanthan gum and sodium carboxymethyl cellulose were mixed in deionized water, allowed to stand evenly, and then freeze-dried to obtain a mixed aerogel. (2) Mix copper nitrate and magnesium nitrate in deionized water, then add the mixed aerogel obtained in step (1), sonicate and heat to react, cool and vacuum dry to obtain the product; The mass ratio of xanthan gum, sodium carboxymethyl cellulose, copper nitrate and magnesium nitrate is (0.5-3):(1-10):(15-25):(20-30).
2. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The copper nitrate includes copper nitrate pentahydrate.
3. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The magnesium nitrate includes magnesium nitrate hexahydrate.
4. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The solid-liquid ratio of xanthan gum to deionized water in step (1) is 1:(250-350)g / mL.
5. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The mixing in step (1) is performed under ultrasonic conditions.
6. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The temperature during the static setting in step (1) is -5 to 0℃ and the time is 0.5 to 1.5h.
7. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, After standing, freeze at -85 to -75°C for 1-3 hours.
8. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The freeze-drying method described in step (1) is vacuum freeze-drying.
9. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 8, characterized in that, The vacuum degree during the vacuum freeze-drying process is 0-30 Pa.
10. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 8, characterized in that, The vacuum freeze-drying process is carried out at a temperature of -10 to 0°C for 20 to 30 hours.
11. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, In step (2), the solid-liquid ratio of copper nitrate to deionized water is 1:(40-60)g / mL.
12. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The ultrasonic treatment time in step (2) is 50-70 minutes.
13. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, After ultrasonic treatment in step (2), the pH of the system is adjusted to 9.5-11.
14. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 13, characterized in that, After adjusting the pH of the system, continue ultrasonic treatment for 20-40 minutes.
15. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The heating reaction in step (2) is carried out at a temperature of 140-160℃ for 20-30 hours.
16. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, Step (2) involves cooling to 25-35°C.
17. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, After cooling, a cleaning process is required.
18. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 17, characterized in that, The cleaning solution used in the cleaning process is DMF and / or anhydrous methanol.
19. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The vacuum degree during the vacuum drying process is 0-30 Pa.
20. The method for preparing the aerogel with the function of encapsulating a smoke-generating agent as described in claim 1, characterized in that, The vacuum drying process is carried out at a temperature of 20-30℃ for 12-18 hours.
21. The application of the aerogel with the function of encapsulating smoke-generating agent prepared by the preparation method according to any one of claims 1-20 in the preparation of heated cigarettes.
22. The application as described in claim 21, characterized in that, The method of application includes mixing a smoke-generating agent with an aerogel that has the function of encapsulating the smoke-generating agent to obtain a mixture, then coating the mixture onto tobacco sheets, cutting it into shreds, and inserting it into heated cigarette segments to obtain the final product.
23. The application as described in claim 22, characterized in that, The mass ratio of the smoke-generating agent to the tobacco polymer aerogel is 1:(1-3).
24. The application as described in claim 22, characterized in that, The smoke-generating agent includes any one or a combination of at least two of glycerol, 1,2-propanediol, or 1,3-butanediol.
25. The application as described in claim 22, characterized in that, The mixture is then dissolved in an aqueous ethanol solution.
26. The application as described in claim 25, characterized in that, The concentration of the ethanol aqueous solution is 50-60%.
27. The application as described in claim 25, characterized in that, The solid-liquid ratio of the mixture to the ethanol aqueous solution is 1:(10-20)g / mL.
28. The application as described in claim 22, characterized in that, The mixture comprises 15-20% of the total amount of tobacco sheets.
29. The application as described in claim 22, characterized in that, After coating, the tobacco sheets are left to stand until the ethanol evaporates, and then they are shredded.