CN114158766A - Biodegradable firmware material for granular heating cigarette and preparation method thereof - Google Patents
Biodegradable firmware material for granular heating cigarette and preparation method thereof Download PDFInfo
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Images
Classifications
-
- 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
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a biodegradable firmware material for granular heating cigarettes and a preparation method thereof, wherein a PLA, PVA, PBAT, PBS and other bio-based polymer materials are used as a base material, glycerol-modified jute fiber, silane coupling agent-modified bamboo powder or straw powder, carbon fiber or calcium carbonate whisker and the like are used as heat-resistant filling materials, and the heat-resistant filling materials are added into an internal mixer for melt blending and then are subjected to hot press molding, so that the biodegradable firmware material is obtained. The firmware material can play a supporting role in the use process of the granular heating cigarette, has higher thermal stability, does not have obvious shrinkage and thermal collapse after being heated, does not add harmful substance release in the mainstream smoke of the heating cigarette, and has no negative influence on the sensory quality of the cigarette.
Description
Technical Field
The invention belongs to the technical field of novel tobacco products, and particularly relates to a biodegradable firmware material for granular heating cigarettes and a preparation method thereof.
Background
Along with the improvement of economic culture level of people, more and more people pay more attention to physical health, and the development of novel tobacco products is imperative. Particulate type heated cigarettes are one of the important forms of novel tobacco products. The granular heating cigarette is different from the currently marketed cigarette products which are not burnt by heating, the tobacco granules are used as the smoke release substances, the smoke quantity is sufficient, the continuity of the smoke release is good, the sensory quality is excellent, and the optimization and adjustment space of the formula is large. However, how to pack the tobacco particles in the cigarette is a key technical problem in cigarette production, and the tobacco particles do not fall and are not sucked in the heating and suction processes.
The fixing material for blocking tobacco particles is one of the important components of the particle type heating cigarette. At present, high-temperature-resistant plastic firmware is used as a middle section barrier material, but mainstream plastic products in the market are non-degradable materials and have poor heat resistance, can be softened and melted in the heating and sucking process, cannot play an effective barrier role, can release peculiar smell, seriously reduce the smoke quality and the sucking experience, and are discarded after the use, so that the smoke quality and the sucking experience are not easily degraded in the environment, and the environment is polluted.
Therefore, it is important to research new firmware materials.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a biodegradable firmware material for granular heating cigarettes and a preparation method thereof, and aims to ensure that the biodegradable firmware material has good supporting and heat-resisting effects in cigarettes and does not influence the sensory quality of the cigarettes.
The invention adopts the following technical scheme for realizing the purpose:
the invention relates to a biodegradable firmware material for granular heating cigarettes, which comprises the following raw materials in percentage by mass:
25-50% of a base material and 50-75% of a heat-resistant filling material.
Further, the substrate material is at least one of PBAT (poly (butylene adipate/terephthalate)), PBS (poly (butylene succinate)), PVA (polyvinyl alcohol) and PLA (polylactic acid).
Further, the heat-resistant filling material is at least one of jute fiber modified by glycerol, bamboo powder or straw powder modified by silane coupling agent, carbon fiber and calcium carbonate whisker.
Further, the preparation method of the glycerol-modified jute fiber comprises the following steps: cutting jute fiber to length of no more than 3cm, soaking in 10g/L NaOH solution at normal temperature for 24 hr, washing to neutral, and drying at 60 deg.C for 24 hr to obtain alkali treated jute fiber; 1.2% of hydrochloric acid, glycerol and deionized water by mass: 78.8%: stirring and mixing 20% of the mixture evenly to obtain water-acidified glycerol; and adding the jute fiber after alkali treatment into the water-acidified glycerol according to the mass concentration of 10%, stirring and refluxing at 130 ℃ for reaction for 30min, then diluting, filtering and drying, and drying in an oven at 80 ℃ for 12h to obtain the glycerol-modified jute fiber.
Furthermore, the preparation method of the silane coupling agent modified bamboo powder or straw powder comprises the following steps: placing bamboo powder or straw powder in H with mass concentration of 0.1%2SO4In solutionSoaking at 55 deg.C for 1.5h, cleaning, and oven drying to obtain acid-treated material; adding the material subjected to acid treatment into a NaOH solution with the mass concentration of 0.5%, soaking at normal temperature for 2h, taking out and washing to be neutral, and drying at 80 ℃ for 4h to obtain a material subjected to alkali treatment; 1.5 percent of silane coupling agent (KH550) and absolute ethyl alcohol by mass: and (3) mixing 98.5% of the mixture uniformly, adding the alkali-treated material, soaking at normal temperature for 4 hours, taking out, and drying at 60 ℃ for 24 hours to obtain the silane coupling agent modified bamboo powder or straw powder.
Further, the PVA is glycerol modified PVA, and the modification method is to add 10-50% of glycerol in the PVA by mass into the PVA and obtain the glycerol modified PVA after the glycerol is fully infiltrated.
The preparation method of the biodegradable firmware material comprises the following steps: weighing the raw materials according to the proportion, adding the raw materials into an internal mixer for melt blending, and then carrying out hot press molding to obtain the finished product.
The invention also discloses application of the firmware material, which is used for granular heating cigarettes and has the effects of supporting the cigarettes and resisting heat.
The biodegradable firmware material of the invention comprises: PLA, PVA, PBAT, PBS, and the like are all new bio-based polymer materials, and have attracted much attention due to excellent biocompatibility and degradability. The bamboo powder, the straw powder and the like are used as additive type bio-based materials and added into the polymer material, so that the heat resistance of the polymer can be effectively improved, and the degradable high-temperature-resistant firmware material is prepared. The fiber material can promote the crystallization of materials such as PLA, PBS and the like due to the reasons of larger specific surface area and the like, thereby improving the heat resistance of the fiber material.
Compared with the prior art, the invention has the beneficial effects that:
1. the firmware material is prepared by using a full biodegradable material, and cannot cause pollution when being discarded in the environment.
2. The firmware material can play a supporting role in the use process of the granular heating cigarette, has higher thermal stability, does not have obvious shrinkage and thermal collapse after being heated, does not add harmful substance release in the mainstream smoke of the heating cigarette, and has no negative influence on the sensory quality of the cigarette.
3. The firmware material disclosed by the invention is simple in preparation process, easy in acquisition of raw materials, easy in industrial production and environment-friendly.
Drawings
FIG. 1 is a DSC curve of samples 11-15 prepared in example 1;
FIG. 2 is a DSC curve of samples 16-20 prepared in example 1;
FIG. 3 is a TG-DTG curve for samples 11-15 prepared in example 1;
FIG. 4 is a plot of TG versus DTG for samples prepared in example 1 ranging from 16 to 20.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
In the following examples, the preparation method of the glycerin-modified jute fiber was as follows: cutting jute fiber to length of no more than 3cm, soaking in 10g/L NaOH solution at normal temperature for 24 hr, washing to neutral, and drying at 60 deg.C for 24 hr to obtain alkali treated jute fiber; 1.2 percent of hydrochloric acid, glycerol and deionized water by mass: 78.8%: stirring and mixing 20% of the mixture evenly to obtain water-acidified glycerol; and adding the jute fiber after alkali treatment into water-acidified glycerol according to the mass concentration of 10%, stirring and refluxing at 130 ℃ for reaction for 30min, then diluting, filtering and drying, and drying in an oven at 80 ℃ for 12h to obtain the glycerol-modified jute fiber.
In the following examples, the preparation method of the bamboo powder modified by the silane coupling agent comprises the following steps: placing bamboo powder in H with mass concentration of 0.1%2SO4Soaking in the solution at 55 deg.C for 1.5h, cleaning, and oven drying to obtain acid-treated material; adding the material after acid treatment into a NaOH solution with the mass concentration of 0.5%, soaking at normal temperature for 2h, taking out and washing to be neutral, and drying at 80 ℃ for 4h to obtain a material after alkali treatment; 1.5 percent of silane coupling agent (KH550) and absolute ethyl alcohol by mass: 98.5 percent of the mixture is mixed evenlyThen adding the alkali-treated material, soaking for 4h at normal temperature, taking out and drying for 24h at 60 ℃ to obtain the bamboo powder modified by the silane coupling agent.
In the following examples, the glycerin-modified PVA used was obtained by adding glycerin, which accounts for 10 to 50% of the PVA by mass, to PVA and sufficiently infiltrating the PVA.
Example 1
The firmware material of the embodiment comprises the following raw materials in percentage by mass as shown in table 1:
TABLE 1 formulation of PVA-based firmware material
The firmware material prepared in this example was used in a vicat thermomechanical tester (merts industrial system (china) limited), DSC8500(Perkin Elmer, USA), TA Q5000IR thermo-analyzer (TA Instruments inc., u.s.) to test vicat softening temperature, DSC, TG, and DTG, with the following specific methods and results:
vicat softening temperature test method: placing the sample wafer in a high-temperature silicone oil heat transfer medium, heating at a heating rate of 50 ℃/h, placing a 50N weight, and testing the sample by 1mm2The Vicat softening point is the temperature at which the needle is pressed in for 1 mm. The size of the sample piece was 10mm × 10mm × 3mm, and the number of layers was 1.
DSC test method: the samples were ground to a powder and tested in nitrogen atmosphere with a temperature rise rate of 20 ℃/min.
TG and DTG test methods: grinding the sample into powder, and testing under air atmosphere, wherein the heating rate is 20 ℃/min, and the temperature is increased to 800 ℃.
Vicat softening temperature test results: the vicat softening temperature of the PVA-based firmware material is shown in table 2. As can be seen from Table 2, the more the amount of glycerin is added, the lower the Vicat softening temperature of PVA is, and therefore, the screening of an effective glycerin addition ratio is a key step for balancing the processability and heat resistance of the heat-resistant composite PVA material. The Vicat softening point test shows that when the addition amount of the glycerol is 10 percent, the Vicat softening temperature of the composite materials prepared by the jute fiber and the bamboo powder with different addition amounts is almost above 100 ℃. The 20% glycerin-swollen PVA with the highest vicat softening temperature was mixed with 60% jute fiber.
TABLE 2 Vicat softening temperature of firmware material with PVA as main matrix
DSC test results: the DSC curves of samples No. 11-15 and 16-20 are shown in figure 1 and figure 2 respectively for the barrier firmware material with PVA as the main substrate. It can be seen that no significant melting peaks and phase transitions occurred for all samples, nor was there any significant chemical reaction. The existence of the glycerol obviously destroys the crystallization property of the PVA, so that the processing temperature of the PVA is reduced, and the filling of the temperature-resistant filler is feasible. As can be seen from FIG. 2, the phenomenon of crystalline melting at 105 ℃ occurs in the PVA composite having a glycerin content of 20%, which means that a part of the PVA is still not swollen by glycerin and therefore crystalline PVA is still present, which affects the melt processability of PVA, thus resulting in insufficient dispersion of the filler in the PVA composite. From the DSC curve, it can be seen that the PVA composite material with 20% of glycerin content has a certain degree of side group elimination and main chain decomposition at about 160 ℃. Thus, the PVA composite having a glycerol content of 30% is most practical.
TG and DTG test results: the thermal gravimetric analysis results of samples No. 11-15 and 16-20 are shown in FIG. 3 and FIG. 4 respectively for the barrier firmware material with PVA as the main substrate. As the samples No. 11-15 are all PVA with 30% of glycerin content, in PVA composite materials with different glycerin contents, the average Vicat softening temperature is higher (94.9 ℃), the average hardness is lower, the average thermal conductivity is lowest, the Vicat softening temperature is higher than 80 ℃, and the Vicat softening temperature is the maximum proportion of swelling glycerin of PVA. Samples nos. 11-15 were therefore selected for thermogravimetric analysis. As can be seen from fig. 3, the thermal decomposition of PVA with a glycerol content of 30% is mainly divided into four stages: dehydration (room temperature-100 ℃), glycerol overflow (100-. The weight loss of the 30% glycerol PVA without the filler in the second stage is 33%, the peak weight loss rate is 0.44%/min, the weight loss in the third stage is 37%, the peak weight loss rate is 42%/min, the weight loss in the fourth stage is 19%, and the peak weight loss rate is 0.28%/min. It can be seen that the peak weight loss rate temperature decreases for each stage with filler addition. The weight loss in the second stage of the filled PVA composite was lower than that of the unfilled PVA with 30% glycerol content. The peak weight loss rates for the third and fourth stages of the filled PVA composite were higher than the unfilled PVA with 30% glycerol content.
Samples 16-20 were all PVA with a 20% glycerol content and an average Vicat softening temperature of 94.1 deg.C (sample 16 without filler removed), which was lower than the average Vicat softening temperature (94.9 deg.C) of the composite of PVA with a 30% glycerol content. As can be seen from fig. 4, the decomposition of the composite material with a PVA with a glycerol content of 20% is mainly divided into two parts: the side groups of PVA are eliminated, most of the main chain is decomposed (280 ℃ C. and 400 ℃ C.), and the rest of the main chain is decomposed (450 ℃ C. and 600 ℃ C.). It can be seen that the PVA composite with 20% glycerol addition has a slightly poorer thermal stability compared with the PVA composite with 30% glycerol addition, the main chain is decomposed completely before 400 ℃, and the PVA material with 30% glycerol addition without filler still has 19% non-decomposition at 400 ℃.
By analyzing DSC, the PVA modified by the glycerol has the processing performance at a relatively lower temperature, and then the heat resistance is obviously improved by adding the heat-resistant filler, and the improvement of the Vicat softening point means that the prepared material can play a supporting role after being heated and does not collapse. Analysis of TG and DTG can prove that the thermal stability of the material is good, and only glycerin volatilizes and overflows below 280 ℃ in 20% glycerin-swollen PVA, and only glycerin volatilizes and overflows below 261 ℃ in 30% glycerin-swollen PVA.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A biodegradable firmware material for granular type heating cigarette is characterized in that: the biodegradable firmware material comprises the following raw materials in percentage by mass:
25-50% of a base material and 50-75% of a heat-resistant filling material.
2. The biodegradable firmware material of claim 1, wherein: the substrate material is at least one of PBAT, PBS, PVA and PLA.
3. The biodegradable firmware material of claim 1, wherein: the heat-resistant filling material is at least one of glycerol-modified jute fiber, silane coupling agent-modified bamboo powder or straw powder, carbon fiber and calcium carbonate whisker.
4. The biodegradable firmware material of claim 3, wherein the glycerol-modified jute fiber is prepared by the following steps:
cutting jute fiber to length of no more than 3cm, soaking in 10g/L NaOH solution at normal temperature for 24 hr, washing to neutral, and drying at 60 deg.C for 24 hr to obtain alkali treated jute fiber;
hydrochloric acid, glycerol and deionized water are mixed according to the mass percentage of 1.2%: 78.8%: stirring and mixing 20% of the mixture evenly to obtain water-acidified glycerol;
and adding the jute fiber after alkali treatment into the water-acidified glycerol according to the mass concentration of 10%, stirring and refluxing at 130 ℃ for reaction for 30min, then diluting, filtering and drying, and drying in an oven at 80 ℃ for 12h to obtain the glycerol-modified jute fiber.
5. The biodegradable firmware material of claim 3, wherein: the preparation method of the silane coupling agent modified bamboo powder or straw powder comprises the following steps:
placing bamboo powder or straw powder in H with mass concentration of 0.1%2SO4Soaking in the solution at 55 deg.C for 1.5h, cleaning, and oven drying to obtain acid-treated material;
adding the material subjected to acid treatment into a NaOH solution with the mass concentration of 0.5%, soaking at normal temperature for 2h, taking out and washing to be neutral, and drying at 80 ℃ for 4h to obtain a material subjected to alkali treatment;
1.5% of silane coupling agent and absolute ethyl alcohol by mass percent: and (3) mixing 98.5% of the mixture uniformly, adding the alkali-treated material, soaking at normal temperature for 4 hours, taking out, and drying at 60 ℃ for 24 hours to obtain the silane coupling agent modified bamboo powder or straw powder.
6. The biodegradable firmware material of claim 2, wherein: the PVA is glycerol modified PVA, and the modification method is to add 10-50% of glycerol in the PVA mass into the PVA and obtain the glycerol modified PVA after full infiltration.
7. A method for preparing a biodegradable firmware material as claimed in any one of claims 1 to 6, wherein: weighing the raw materials according to the proportion, adding the raw materials into an internal mixer for melt blending, and then carrying out hot press molding to obtain the finished product.
8. Use of a biodegradable fastener material according to any one of claims 1 to 6, wherein: the heat-resistant composite material is used for granular heating cigarettes, and has the effects of supporting the cigarettes and resisting heat.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111578714.7A CN114158766B (en) | 2021-12-22 | 2021-12-22 | Biodegradable firmware material for granular heating cigarettes and preparation method thereof |
| PCT/CN2022/140710 WO2023116767A1 (en) | 2021-12-22 | 2022-12-21 | Biodegradable solid material for granular tobacco-type heating cigarettes, and preparation method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111578714.7A CN114158766B (en) | 2021-12-22 | 2021-12-22 | Biodegradable firmware material for granular heating cigarettes and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023116767A1 (en) * | 2021-12-22 | 2023-06-29 | 安徽中烟工业有限责任公司 | Biodegradable solid material for granular tobacco-type heating cigarettes, and preparation method therefor |
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| CN110477446A (en) * | 2019-08-26 | 2019-11-22 | 安徽中烟工业有限责任公司 | It is a kind of not burn the cooling particle and preparation method thereof of cigarette smoke temperature for reducing heating |
| US20200229487A1 (en) * | 2018-08-16 | 2020-07-23 | Yunnan Xike Science & Technology Co., Ltd. | Integrally-formed Heat-not-burn Smoking Article and Manufacturing Method therefor |
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| CN101538401A (en) * | 2009-03-13 | 2009-09-23 | 上海大学 | High temperature resistance binary fiber/polylactic acid based composite material and preparation method thereof |
| US8434498B2 (en) * | 2009-08-11 | 2013-05-07 | R. J. Reynolds Tobacco Company | Degradable filter element |
| CN107501884A (en) * | 2017-09-25 | 2017-12-22 | 江苏长龙国际贸易有限公司 | A kind of fire-retardant and smoke-inhibiting type bamboo fibre/lactic acid composite material and preparation method thereof |
| CN111150108B (en) * | 2020-01-17 | 2023-02-28 | 深圳新火瑞升技术有限公司 | Functional barrier sheet for heating non-combustible cigarettes and preparation method and application thereof |
| CN112521730B (en) * | 2020-11-23 | 2022-07-08 | 陈京灿 | Biodegradable composite material and preparation method thereof |
| CN113080509A (en) * | 2021-04-12 | 2021-07-09 | 上海华宝生物科技有限公司 | Temperature-reducing member master batch for heating non-combustible cigarettes and preparation method thereof |
| CN113679096A (en) * | 2021-08-31 | 2021-11-23 | 安徽中烟工业有限责任公司 | Granular heating cigarette and preparation method thereof |
| CN114158766B (en) * | 2021-12-22 | 2024-02-23 | 安徽中烟工业有限责任公司 | Biodegradable firmware material for granular heating cigarettes and preparation method thereof |
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- 2021-12-22 CN CN202111578714.7A patent/CN114158766B/en active Active
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| US4506684A (en) * | 1978-08-02 | 1985-03-26 | Philip Morris Incorporated | Modified cellulosic smoking material and method for its preparation |
| US20200229487A1 (en) * | 2018-08-16 | 2020-07-23 | Yunnan Xike Science & Technology Co., Ltd. | Integrally-formed Heat-not-burn Smoking Article and Manufacturing Method therefor |
| CN110477446A (en) * | 2019-08-26 | 2019-11-22 | 安徽中烟工业有限责任公司 | It is a kind of not burn the cooling particle and preparation method thereof of cigarette smoke temperature for reducing heating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023116767A1 (en) * | 2021-12-22 | 2023-06-29 | 安徽中烟工业有限责任公司 | Biodegradable solid material for granular tobacco-type heating cigarettes, and preparation method therefor |
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| CN114158766B (en) | 2024-02-23 |
| WO2023116767A1 (en) | 2023-06-29 |
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