WO2023116767A1 - Matière solide biodégradable pour cigarettes chauffante de type à tabac granulaire, et son procédé de préparation - Google Patents

Matière solide biodégradable pour cigarettes chauffante de type à tabac granulaire, et son procédé de préparation Download PDF

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Publication number
WO2023116767A1
WO2023116767A1 PCT/CN2022/140710 CN2022140710W WO2023116767A1 WO 2023116767 A1 WO2023116767 A1 WO 2023116767A1 CN 2022140710 W CN2022140710 W CN 2022140710W WO 2023116767 A1 WO2023116767 A1 WO 2023116767A1
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WIPO (PCT)
Prior art keywords
pva
solid material
glycerin
modified
hours
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PCT/CN2022/140710
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English (en)
Chinese (zh)
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张劲
周顺
张晓宇
王孝峰
曹芸
丁乃红
王鹏
管明婧
李延岩
邢伟义
田慧娟
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安徽中烟工业有限责任公司
中国科学技术大学先进技术研究院
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Publication of WO2023116767A1 publication Critical patent/WO2023116767A1/fr

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A24D1/20—Cigarettes specially adapted for simulated smoking devices
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A24D1/02—Cigars; Cigarettes with special covers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

Definitions

  • the invention belongs to the technical field of novel tobacco products, and in particular relates to a biodegradable solid material used for granular heating cigarettes and a preparation method thereof.
  • Particulate heated cigarettes are one of the important forms of new tobacco products. Different from the current heat-not-burn cigarette products on the market, particle-type heated cigarettes use tobacco particles as the smoke-releasing substance, with sufficient smoke volume, good continuity of smoke release, excellent sensory quality, and large room for formula optimization and adjustment. However, how to encapsulate the tobacco particles in the cigarette so as not to drop and inhale during the heating and smoking process is a key technical issue in the production of cigarettes.
  • the solid material used to block tobacco particles is one of the important components of particle-type heating cigarettes.
  • high-temperature-resistant plastic fasteners are used as the middle section barrier material, but the mainstream plastic products on the market are non-degradable materials and the heat resistance is not good enough. They will soften and melt during the heating and suction process, which not only cannot play an effective barrier role. , It will also release peculiar smell, which seriously reduces the quality of smoke and the smoking experience. After use, it is not easy to degrade when discarded in the environment, which will pollute the environment.
  • the purpose of the present invention is to overcome the deficiencies of the prior art, to provide a biodegradable solid material for granular heating cigarettes and its preparation method, aiming to make it have good support and heat resistance in the cigarette Does not affect the sensory quality of cigarettes.
  • the present invention adopts following technical scheme for realizing the purpose:
  • the present invention is used for the biodegradable solid material of granular heating cigarettes, and the composition of each raw material according to the mass percentage is:
  • the base material is 25-50%, and the heat-resistant filling material is 50%-75%.
  • the base material is PBAT (polybutylene adipate/terephthalate), PBS (polybutylene succinate), PVA (polyvinyl alcohol) and PLA (polylactic acid). at least one of .
  • the heat-resistant filling material is at least one of glycerin-modified jute fiber, silane coupling agent-modified bamboo powder or straw powder, carbon fiber and calcium carbonate whiskers.
  • the preparation method of the glycerol-modified jute fiber is as follows: the jute fiber is cut to a length of not more than 3cm, then put into a NaOH solution with a concentration of 10g/L and soaked for 24h at room temperature, take it out and rinse until neutral, Dry at 60°C for 24 hours to obtain the jute fiber after alkali treatment; stir and mix hydrochloric acid, glycerin and deionized water according to the mass fraction of 1.2%: 78.8%: 20% to obtain water-acidified glycerin; jute fiber after alkali treatment according to 10% The mass concentration was added to the water-acidified glycerin, stirred and refluxed at 130°C for 30 minutes, then diluted, dried by suction filtration, and dried in an oven at 80°C for 12 hours to obtain glycerin-modified jute fiber.
  • the preparation method of the bamboo powder or straw powder modified by the silane coupling agent is as follows: the bamboo powder or straw powder is placed in a H2SO4 solution with a mass concentration of 0.1%, soaked at 55°C for 1.5h , washed and dried to obtain the acid-treated material; the acid-treated material was added to a NaOH solution with a mass concentration of 0.5%, soaked at room temperature for 2 hours, removed and rinsed until neutral, and dried at 80°C for 4 hours to obtain the alkali Treated material; mix silane coupling agent (KH550) and absolute ethanol according to the mass percentage of 1.5%:98.5%, then add the alkali-treated material, soak at room temperature for 4 hours, take it out and dry at 60°C for 24 hours to obtain silane Coupling agent modified bamboo powder or straw powder.
  • the PVA is glycerol-modified PVA
  • the modification method is to add glycerol accounting for 10% to 50% of the PVA mass into the PVA, and obtain the glycerin-modified PVA after sufficient infiltration.
  • the preparation method of the biodegradable fastener material of the present invention is as follows: weighing each raw material according to the proportion, adding it to an internal mixer for melting and blending, and then hot pressing to obtain a finished product.
  • the invention also discloses the application of the above-mentioned firmware material, which is used in particle-type heating cigarettes to support cigarettes and resist heat.
  • PLA, PVA, PBAT, and PBS are emerging bio-based polymer materials, which have attracted widespread attention due to their excellent biocompatibility and degradability.
  • bamboo powder and straw powder are added to the above polymer materials as additive bio-based materials, which can effectively improve the heat resistance of the polymer and prepare degradable high-temperature resistant firmware materials. Due to its large specific surface area and other reasons, fiber materials can promote the crystallization of PLA, PBS and other materials, thereby improving their heat resistance.
  • the firmware material of the present invention is made of fully biodegradable materials, and it will not cause pollution when discarded in the environment.
  • the firmware material of the present invention can play a supporting role in the use of granular heating cigarettes, and has high thermal stability. After being heated, there is no obvious shrinkage and thermal collapse, and it does not appear in the mainstream smoke of heating cigarettes. Increase the release of harmful substances and have no negative impact on the sensory quality of cigarettes.
  • the firmware material of the present invention has a simple preparation process, readily available raw materials, easy industrial production, and is environmentally friendly.
  • Fig. 1 is the DSC curve of sample 11 ⁇ 15 prepared in embodiment 1;
  • Fig. 2 is the DSC curve of sample 16 ⁇ 20 prepared in embodiment 1;
  • Fig. 3 is the TG and DTG curve of samples 11-15 prepared in embodiment 1;
  • Fig. 4 is the TG and DTG curves of samples 16-20 prepared in Example 1.
  • the preparation method of the jute fiber modified with glycerol is: the jute fiber is cut to a length of no more than 3cm, then put into a NaOH solution with a concentration of 10g/L and soaked for 24h at room temperature, take out and rinse until neutral , dry at 60°C for 24h to obtain the jute fiber after alkali treatment; stir and mix hydrochloric acid, glycerin and deionized water according to the mass percentage of 1.2%:78.8%:20% to obtain water-acidified glycerin; jute fiber after alkali treatment according to 10% The mass concentration was added to water-acidified glycerin, stirred and refluxed at 130°C for 30 minutes, then diluted, dried by suction filtration, and dried in an oven at 80°C for 12 hours to obtain glycerin-modified jute fiber.
  • the preparation method of the bamboo powder modified by the silane coupling agent used is as follows: the bamboo powder is placed in a H2SO4 solution with a mass concentration of 0.1%, soaked at 55°C for 1.5h, washed, dried Dry to obtain the acid-treated material; add the acid-treated material to a NaOH solution with a mass concentration of 0.5%, soak it at room temperature for 2 hours, take it out and rinse until neutral, and dry it at 80°C for 4 hours to obtain the alkali-treated material; The coupling agent (KH550) and absolute ethanol are mixed uniformly according to the mass percentage of 1.5%:98.5%, then the alkali-treated material is added, soaked at room temperature for 4 hours, taken out and dried at 60°C for 24 hours to obtain the bamboo powder modified by the silane coupling agent.
  • glycerol-modified PVA is used by adding glycerol, which accounts for 10% to 50% of the PVA mass, into the PVA, and after sufficient infiltration, the glycerin-modified PVA is obtained.
  • the firmware material prepared in this embodiment is used in Vicat thermal deformation testing machine (Meters Industrial Systems (China) Co., Ltd.), DSC8500 (Perkin Elmer, USA), TA Q5000IR thermo-analyzer (TA Instruments Inc., U.S.) , to test its Vicat softening temperature, DSC, TG and DTG, the specific methods and results are as follows:
  • Vicat softening temperature test method place the sample in a high-temperature silicone oil heat transfer medium, use a heating rate of 50°C/h to raise the temperature, place a 50N weight, and test the temperature when the sample is pressed into 1mm by a 1mm 2 needle.
  • the card softens.
  • the sample size is 10mm ⁇ 10mm ⁇ 3mm, and the number of stacked layers is 1.
  • DSC test method the sample is ground into powder and tested under a nitrogen atmosphere with a heating rate of 20°C/min.
  • TG and DTG test methods Grind the sample into powder and test it in an air atmosphere. The heating rate is 20°C/min, and the temperature is raised to 800°C.
  • Vicat softening temperature test results Table 2 shows the Vicat softening temperature of the firmware material with PVA as the main matrix. It can be seen from Table 2 that the greater the amount of glycerin added, the lower the Vicat softening temperature of PVA. Therefore, screening out the effective ratio of glycerin addition is a key step to balance the processing performance and heat resistance of PVA heat-resistant composite materials. Through the Vicat softening point test, it can be seen that when the amount of glycerin added is 10%, the Vicat softening temperatures of the composites prepared with different amounts of jute fiber and bamboo powder are almost above 100°C. The highest Vicat softening temperature is the composite material mixed with 20% glycerin swollen PVA and 60% jute fiber.
  • DSC test results for the barrier firmware material with PVA as the main substrate, the DSC curves of samples No. 11-15 are shown in Figure 1, and the DSC curves of samples No. 16-20 are shown in Figure 2. It can be seen that all samples have no obvious melting peaks and phase transitions, and no obvious chemical reactions have occurred. It shows that the existence of glycerol obviously destroys the crystallization property of PVA, makes its processing temperature drop, thus makes it feasible to fill it with heat-resistant filler.
  • the PVA composite material with a glycerol content of 20% appears crystallization and melting at 105°C, which shows that there are still some PVAs that are not swollen by glycerin, so there are still crystallized PVAs, which will have a negative impact on the melt processability of PVA. impact, thus resulting in insufficient dispersion of fillers in PVA composites.
  • the PVA composite material with a glycerol content of 20% has a certain degree of side group elimination and main chain decomposition at about 160 °C. Therefore, the PVA composite material with a glycerol content of 30% has the best practicability.
  • thermogravimetric analysis results of samples No. 11-15 are shown in Figure 3
  • thermogravimetric analysis results of samples No. 16-20 are shown in Figure 4. Since samples No. 11-15 are all PVA with 30% glycerin content, the average Vicat softening temperature (94.9°C) is higher in PVA composites with different glycerin content, and the average hardness is lower, and the average thermal conductivity is the lowest. The softening temperature is higher than 80 °C, and it is the largest proportion of PVA swellable glycerin. Therefore, samples No. 11-15 were selected for thermogravimetric analysis.
  • the thermal decomposition of PVA with a glycerol content of 30% is mainly divided into four stages: dehydration (room temperature-100°C), glycerin overflow (100-261°C), elimination of PVA side groups (261-400°C °C), the main chain of PVA decomposes (400-600 °C).
  • the 30% glycerin PVA without filler has a weight loss of 33% in the second stage, and the peak weight loss rate is 0.44%/min.
  • the weight loss in the third stage is 37%, and the peak weight loss rate is 42%/min.
  • the weight loss in the fourth stage is 19%.
  • the weight loss rate was 0.28%/min.
  • the peak weight loss rate temperature of each stage decreases.
  • the second stage weight loss of the filled PVA composite was lower than that of the 30% glycerol content PVA without filler.
  • the peak weight loss rates of the third and fourth stages of PVA composites with fillers were higher than those of PVA with 30% glycerol content without fillers.
  • No. 16-20 samples are all PVA with 20% glycerol content, and the average Vicat softening temperature is 94.1°C (removing the No. 16 sample without filler), which is lower than the composite material average Vicat softening temperature (94.9 °C).
  • the decomposition of the composite material with a glycerol content of 20% PVA is mainly divided into two parts: the side group elimination of PVA and the decomposition of most of the main chain (280-400 ° C), and the decomposition of the remaining part of the main chain (450 ° C). -600°C). It can be seen that the thermal stability of the PVA composite material with 20% glycerin addition is poorer than that of the PVA composite material with 30% addition. The PVA material with an amount of 30% still has 19% undecomposed at 400°C.
  • the PVA modified by glycerol has a relatively lower temperature processing performance, and then the heat resistance performance is significantly improved by adding heat-resistant fillers.
  • the increase in Vicat softening point means that The prepared material can play a supporting role after being heated without collapsing.
  • the analysis of TG and DTG can prove that the thermal stability of the material is good. For PVA swollen with 20% glycerin, only glycerol volatilization overflows below 280°C, while for PVA swollen with 30% glycerin, only glycerol volatilization overflows below 261°C. .

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Abstract

L'invention concerne une matière solide biodégradable pour cigarettes chauffantes de type à tabac granulaire, et son procédé de préparation. Elle concerne des matières polymères d'origine biologique tels que PLA, PVA, PBAT et PBS, qui sont utilisées en tant que matières de base, ainsi que des fibres de jute modifiées par du glycérol, de la poudre de bambou modifiée par un agent de couplage au silane ou de la poudre de paille, des fibres de carbone ou des trichites de carbonate de calcium et analogues, qui sont utilisées en tant que matières de remplissage résistant à la chaleur, sont ajoutées à un mélangeur interne, fondues, mélangées et pressées à chaud pour obtenir la matière solide. La matière solide peut jouer un rôle de support lorsqu'une cigarette chauffante de type à tabac granulaire est consommée. Elle présente une stabilité thermique relativement élevée et n'est pas sujette au retrait et à l'affaissement provoqué par la chaleur après avoir été chauffée. La matière solide n'ajoute pas de substances dangereuses libérées dans la fumée principale de la cigarette chauffante, et n'a pas d'influence négative sur la qualité sensorielle de la cigarette.
PCT/CN2022/140710 2021-12-22 2022-12-21 Matière solide biodégradable pour cigarettes chauffante de type à tabac granulaire, et son procédé de préparation WO2023116767A1 (fr)

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CN202111578714.7 2021-12-22

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CN114158766B (zh) * 2021-12-22 2024-02-23 安徽中烟工业有限责任公司 一种用于颗粒型加热卷烟的生物可降解固件材料及其制备方法

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