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CN105601983A - Natural polysaccharide aerogel, preparation method thereof and application thereof in cigarettes - Google Patents

Natural polysaccharide aerogel, preparation method thereof and application thereof in cigarettes Download PDF

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CN105601983A
CN105601983A CN201610133214.5A CN201610133214A CN105601983A CN 105601983 A CN105601983 A CN 105601983A CN 201610133214 A CN201610133214 A CN 201610133214A CN 105601983 A CN105601983 A CN 105601983A
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natural polysaccharide
natural
polysaccharide
agent
ethanol
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CN105601983B (en
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王猛
朱保昆
张天栋
凌军
颜克亮
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China Tobacco Yunnan Industrial Co Ltd
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    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
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  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention discloses natural polysaccharide aerogel. A preparation method of the natural polysaccharide aerogel includes the following steps that natural polysaccharides and filler are dispersed in a solvent, a cross-linking agent and a reinforcing agent are added, mixed and evenly stirred, and then natural polysaccharide hydrogel is obtained through processing; the natural polysaccharide hydrogel is soaked in ethanol or acetone, and the natural polysaccharide aerogel is obtained through drying. The invention further discloses application of the natural polysaccharide aerogel in combined filter sticks of filters of cigarettes.

Description

一种天然多糖气凝胶、其制备方法及在卷烟中的应用A kind of natural polysaccharide airgel, its preparation method and its application in cigarette

技术领域 technical field

本发明具体涉及一种天然多糖气凝胶、其制备方法及在卷烟中的应用,属于烟用材料技术领域。 The invention specifically relates to a natural polysaccharide airgel, its preparation method and its application in cigarettes, belonging to the technical field of tobacco materials.

背景技术 Background technique

我国烟草行业正向高香、低害、低焦油的中式卷烟高端品牌方向发展,这势必要求科技工作者不断提供新技术新材料方向的产品开发和成果转化。其中,在传统加香加料基础上发掘新的应用添加方式来修正和补偿中式低焦卷烟的香气、吃味和劲头显得尤为重要。滤棒作为卷烟烟气的过滤体系,除了能对烟气进行吸附、截留外,还可通过进一步的功能化对主流烟气进行修饰校正。近年来,轻质、高弹性气凝胶材料因具备超低的密度(ρ=0.15~10mg/cm3)、高的比表面积和孔隙率以及优异的弹性和机械加工性吸引了科技工作者的广泛关注。通过在气凝胶载体上添加功能物质,如生津清润的植物提取物、烟用香精香料以及改变烟气pH的特定烟用添加剂等,可以对卷烟产品进行感官质量修正。 my country's tobacco industry is developing towards high-end brands of Chinese-style cigarettes with high aroma, low harm and low tar. This will inevitably require scientific and technological workers to continuously provide product development and achievement transformation in the direction of new technologies and materials. Among them, it is particularly important to discover new application addition methods on the basis of traditional flavoring and addition to correct and compensate the aroma, taste and strength of Chinese-style low-focus cigarettes. As a filter system for cigarette smoke, filter rods can not only absorb and retain smoke, but also modify and correct mainstream smoke through further functionalization. In recent years, lightweight and highly elastic airgel materials have attracted the attention of scientific and technological workers due to their ultra-low density (ρ=0.15-10mg/cm 3 ), high specific surface area and porosity, and excellent elasticity and machinability. extensive attention. By adding functional substances on the airgel carrier, such as plant extracts that promote body fluids and clearness, tobacco flavors and fragrances, and specific tobacco additives that change the pH of smoke, etc., the sensory quality of cigarette products can be corrected.

目前天然多糖凝胶在药物控制释放领域研究的比较多,并且大多为多糖基水凝胶,针对气凝胶的研究还比较少。专利CN102793271B公开了一种具有较高比表面积的交联壳聚糖多孔微球在卷烟滤嘴中的应用,用于吸附烟气中的有害成分;专利CN104525126A公开了一种海藻纤维素气凝胶吸油材料的制备方法,通过浸渍吡咯液体调节其疏水性用于水中溢油吸附。菲利普·莫里斯生产公司公开了一项包含香味递送材料的吸烟制品,所述的香味递送材料包含具有3D网络结构的聚合物基质,该聚合物基质由一种或多种多糖组合交联而成,可以很好地保护所包含的香味组分,但是只有当基质受热至高于220℃时才能释放出吸烟制品中的香味添加剂,限制了它在常规卷烟中的应用。 At present, there are many studies on natural polysaccharide gels in the field of controlled drug release, and most of them are polysaccharide-based hydrogels, while there are relatively few studies on aerogels. Patent CN102793271B discloses the application of cross-linked chitosan porous microspheres with a higher specific surface area in cigarette filters to absorb harmful components in smoke; patent CN104525126A discloses a seaweed cellulose airgel The preparation method of the oil-absorbing material adjusts its hydrophobicity by impregnating pyrrole liquid and is used for absorbing oil spill in water. Philip Morris Manufacturing Co. discloses a smoking article comprising a flavor delivery material comprising a polymer matrix having a 3D network structure cross-linked by a combination of one or more polysaccharides , can well protect the contained flavor components, but the flavor additives in smoking articles can only be released when the matrix is heated above 220°C, which limits its application in conventional cigarettes.

发明内容 Contents of the invention

本发明第一方面公开了一种新型的天然多糖气凝胶,其通过包括以下步骤的方法制备: The first aspect of the present invention discloses a novel natural polysaccharide airgel, which is prepared by a method comprising the following steps:

(1)将10重量份的天然多糖、0~0.1重量份填料分散到溶剂中超声分散处理20-40min,得到均匀的天然多糖悬浮液; (1) Disperse 10 parts by weight of natural polysaccharides and 0-0.1 parts by weight of fillers in a solvent for ultrasonic dispersion treatment for 20-40 minutes to obtain a uniform suspension of natural polysaccharides;

(2)将0.1~0.5重量份的交联剂、0.05~0.1重量份的增强剂加入到上述的天然多糖悬浮液中,混合搅拌均匀,得到天然多糖混合体系分散液; (2) adding 0.1 to 0.5 parts by weight of a crosslinking agent and 0.05 to 0.1 parts by weight of a reinforcing agent into the above natural polysaccharide suspension, mixing and stirring evenly to obtain a natural polysaccharide mixed system dispersion;

(3)将上述天然多糖混合体系分散液在100~120℃下通N2条件下反应2~10h;或者在功率200~400W条件下超声处理20~40min,获得3D结构的天然多糖水凝胶; (3) React the dispersion of the above natural polysaccharide mixed system at 100-120°C under N2 for 2-10 hours; or ultrasonically treat it for 20-40 minutes at a power of 200-400W to obtain a natural polysaccharide hydrogel with a 3D structure ;

(4)用乙醇或丙酮分步浸泡上述天然多糖水凝胶1~2次,每次持续1~3h,所述的天然多糖水凝胶与乙醇或丙酮的质量比为1:10~15,然后在真空度为0.5~2.5KPa,温度为-40~-60℃条件下冷冻干燥20~60h,得到所述天然多糖气凝胶。 (4) Soak the above-mentioned natural polysaccharide hydrogel step by step with ethanol or acetone for 1-2 times, each time for 1-3 hours, the mass ratio of the natural polysaccharide hydrogel to ethanol or acetone is 1:10-15, Then freeze-dry for 20-60 hours under the condition of vacuum degree of 0.5-2.5KPa and temperature of-40--60°C to obtain the natural polysaccharide airgel.

优选地,所述天然多糖选自海藻酸钠、葛根纤维、甘蔗纤维、烟梗纤维、辣木纤维、多聚半乳糖醛酸、微晶纤维素、羧甲基纤维素、淀粉、壳聚糖或透明质酸中的一种或几种; Preferably, the natural polysaccharide is selected from sodium alginate, kudzu root fiber, sugarcane fiber, tobacco stem fiber, Moringa fiber, polygalacturonic acid, microcrystalline cellulose, carboxymethyl cellulose, starch, chitosan Or one or more of hyaluronic acid;

所述填料选自亚微米级二氧化硅、碳酸钡、硫酸钡、碳酸钙或蒙脱土中的一种或几种; The filler is selected from one or more of submicron silica, barium carbonate, barium sulfate, calcium carbonate or montmorillonite;

所述溶剂选自水、离子液体、质量浓度为2~10%氢氧化钠水溶液、质量浓度为10~20%的乙酸水溶液、质量浓度为20~50%的氯化钙水溶液、质量浓度为20~50%的氯化钡水溶液或质量浓度为20~50%的氯化锌水溶液中的一种; The solvent is selected from water, ionic liquid, 2-10% sodium hydroxide aqueous solution, 10-20% acetic acid aqueous solution, 20-50% calcium chloride aqueous solution, and 20% mass concentration. One of ~50% barium chloride aqueous solution or zinc chloride aqueous solution with a mass concentration of 20-50%;

所述交联剂选自乙二醇二缩水甘油醚、戊二醛、烯丙基蔗糖醚、乙酸酐、京尼平或羧甲基纤维素钠中的一种; The crosslinking agent is selected from one of ethylene glycol diglycidyl ether, glutaraldehyde, allyl sucrose ether, acetic anhydride, genipin or sodium carboxymethyl cellulose;

所述增强剂为碳酸钙与葡萄糖酸内酯质量比为2:1的混合物。 The enhancer is a mixture of calcium carbonate and gluconolactone with a mass ratio of 2:1.

优选地,所述天然多糖气凝胶的孔隙中吸附有烟气修饰剂成分;优选地,所述烟气修饰剂成分为天然有机酸、植物多酚类、氨基酸类、皂苷类、凉味剂薄荷醇、烟草提取物、花果提取物中的一种或几种。 Preferably, smoke modifier components are adsorbed in the pores of the natural polysaccharide airgel; preferably, the smoke modifier components are natural organic acids, plant polyphenols, amino acids, saponins, cooling agents One or more of menthol, tobacco extract, flower fruit extract.

本发明第二方面公开了所述天然多糖气凝胶用于卷烟滤嘴复合滤棒中以增加流经其的烟气浓度、吸附烟气中有害物质和释放烟气修饰剂的用途。 The second aspect of the present invention discloses that the natural polysaccharide airgel is used in a cigarette filter composite filter rod to increase the concentration of smoke flowing through it, absorb harmful substances in the smoke and release smoke modifiers.

所述烟气修饰剂的释放能够保持卷烟香气的稳定性、持久性和/或香气释放随时间的均匀一致性。 The release of the smoke modifying agent can maintain the stability and persistence of the cigarette aroma and/or the uniform consistency of the aroma release over time.

本发明的有益效果: Beneficial effects of the present invention:

1、本发明的天然多糖气凝胶材料,表面极性与孔径可调,对不同直径大小和极性强弱的分子、甚至低浓度或微量的吸附质都具有较好的吸附能力,能大量吸附烟气中有害物质; 1. The natural polysaccharide airgel material of the present invention has adjustable surface polarity and pore size, and has good adsorption capacity for molecules with different diameters and polarities, and even low-concentration or trace amounts of adsorbates. Adsorb harmful substances in flue gas;

2、本发明的天然多糖气凝胶材料通过键合交联,其组装单元不易脱落,制备加工过程也不易引起粉尘。 2. The natural polysaccharide airgel material of the present invention is bonded and cross-linked, and its assembly units are not easy to fall off, and the preparation process is not easy to cause dust.

3、本发明的天然多糖气凝胶材料内部具有3D网状结构和较大孔体积,比表面积较高,其超低的密度和高孔隙率能大量吸附有烟气修饰剂成分;且主流烟气倾向于流经气凝胶材料所在区域,增加流经的烟气浓度使流向改变集中到气凝胶所在区域、吸附有烟气修饰剂成分更容易被主流烟气洗脱携带进入吸食者口腔。 3. The natural polysaccharide airgel material of the present invention has a 3D network structure and a large pore volume inside, and has a high specific surface area. Its ultra-low density and high porosity can absorb a large amount of smoke modifier components; and mainstream smoke The air tends to flow through the area where the airgel material is located, increasing the concentration of the flowing smoke makes the change of flow direction concentrated to the area where the airgel is located, and the adsorbed smoke modifier components are more likely to be eluted by the mainstream smoke and carried into the mouth of the smoker .

4、本发明的天然多糖气凝胶材料能够长期保持并稳定释放,延缓烟气修饰剂在储存过程中的损失同时保证抽吸时相对均匀的释放,能够保持卷烟香气的稳定性、持久性和/或香气释放随时间的均匀一致性。 4. The natural polysaccharide airgel material of the present invention can maintain and release stably for a long time, delay the loss of the smoke modifier during storage and ensure relatively uniform release during smoking, and can maintain the stability, persistence and and/or uniform consistency of aroma release over time.

具体实施方式 detailed description

为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例对本发明的技术方案作进一步的说明。应当理解,此处所描述的具体实施例仅用于解释本发明,并不是对本发明技术方案的限定。 In order to make the object, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be further described in conjunction with the following examples. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the technical solution of the present invention.

实施例1 Example 1

将10重量份的天然多聚半乳糖醛酸、0.1重量份SiO2填料分散到10%的乙酸水溶液中超声分散处理1h,得到均匀的多糖悬浮液;再将0.1重量份的交联剂乙二醇二缩水甘油醚,0.05重量份的碳酸钙-葡萄糖酸内酯混合物加入到上述的天然多糖悬浮液中,混合搅拌均匀,最终形成15mg/ml的混合体系分散液。在100℃通N2条件下反应5h,得到3D结构的天然多糖水凝胶,用乙醇、丙酮、乙醇先后分步浸泡上述多糖凝胶各1、1、2次,每次持续3h,所述的多糖水凝胶与乙醇或丙酮的质量体积比为1:10,然后在真空度为1.0KPa,温度为-45℃条件下冷冻干燥25h得到所述的天然多糖气凝胶。 10 parts by weight of natural polygalacturonic acid, 0.1 parts by weight of SiO Fillers are dispersed into 10 % aqueous acetic acid for ultrasonic dispersion treatment for 1h to obtain a uniform polysaccharide suspension; Add alcohol diglycidyl ether and 0.05 parts by weight of calcium carbonate-gluconolactone mixture into the above natural polysaccharide suspension, mix and stir evenly, and finally form a 15 mg/ml mixed system dispersion. React for 5 hours at 100°C under N2 conditions to obtain natural polysaccharide hydrogels with a 3D structure. Soak the polysaccharide gels with ethanol, acetone, and ethanol step by step, respectively, for 1, 1, and 2 times, each time for 3 hours. The mass volume ratio of the polysaccharide hydrogel to ethanol or acetone is 1:10, and then freeze-dried at a vacuum degree of 1.0 KPa and a temperature of -45° C. for 25 hours to obtain the natural polysaccharide aerogel.

将所得到天然多糖气凝胶浸渍0.1%的清甜香烟草提取物水溶液,以料棒的形式加入到卷烟滤嘴中制备成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel is impregnated with 0.1% aqueous solution of Qingtian tobacco extract, and added into cigarette filter in the form of a rod to prepare a composite cigarette filter rod.

实施例2 Example 2

将8重量份的葛根纤维和2重量份的微晶纤维素分散到20%的CaCl2水溶液中,同时添加0.05%的碳酸钠超声分散处理1h,得到均匀的悬浮液,将0.05重量份碳酸钙-葡萄糖酸内酯混合物加入到上述的悬浮液,再加入0.1重量份的乙酸酐,混合搅拌均匀,最终形成10mg/ml的混合体系分散液;将上述的混合体系分散液,超声功率为200W条件下处理30min,获得3D结构的天然多糖水凝胶,用乙醇先后浸泡上述多糖凝胶2次,每次持续3h,所述的多糖水凝胶与乙醇的质量体积比为1:10,然后在真空度为0.5KPa,温度为-40℃条件下冷冻干燥35h得到所述的天然多糖气凝胶材料。 The kudzu root fiber of 8 weight parts and the microcrystalline cellulose of 2 weight parts are dispersed in 20% CaCl In the aqueous solution, add the sodium carbonate ultrasonic dispersion treatment of 1h simultaneously, obtain uniform suspension, 0.05 weight part calcium carbonate - Add the gluconolactone mixture to the above-mentioned suspension, then add 0.1 parts by weight of acetic anhydride, mix and stir evenly, and finally form a 10 mg/ml mixed system dispersion liquid; the above-mentioned mixed system dispersion liquid, the ultrasonic power is 200W The natural polysaccharide hydrogel with a 3D structure was obtained after treatment for 30 minutes. The above polysaccharide gel was soaked in ethanol twice for 3 hours each time. The mass-volume ratio of the polysaccharide hydrogel to ethanol was 1:10, and then The natural polysaccharide airgel material was obtained by freeze-drying for 35 hours at a vacuum degree of 0.5KPa and a temperature of -40°C.

将所得的天然多糖气凝胶材料加工成微球,浸渍0.05%的香料植物提取物的水溶液中,干燥后以颗粒的形式加入到卷烟滤嘴中制备成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel material is processed into microspheres, immersed in 0.05% aqueous solution of spice plant extracts, dried and added to cigarette filters in the form of particles to prepare composite cigarette filter rods.

实施例3 Example 3

将5重量份的壳聚糖、5重量份的羧甲基纤维素分散到水/乙醇混合溶剂中(v/v=2:1)超声分散处理1h,得到均匀的悬浮液,将0.1份戊二醛、0.05重量份的碳酸钙-葡萄糖酸内酯混合物加入到上述的悬浮液中,混合搅拌均匀,最终形成5mg/ml的混合体系分散液。然后在120℃条件下通N2反应8h,获得3D结构的天然多糖水凝胶。用乙醇浸泡上述多糖凝胶2次,每次持续3h,所述的多糖凝胶与乙醇的质量体积比为1:15,然后在真空度为2.5KPa,温度为-40℃条件下冷冻干燥20h得到所述的天然多糖气凝胶材料。 Disperse 5 parts by weight of chitosan and 5 parts by weight of carboxymethyl cellulose in a water/ethanol mixed solvent (v/v=2:1) for ultrasonic dispersion for 1 h to obtain a uniform suspension. Dialdehyde and 0.05 parts by weight of calcium carbonate-gluconolactone mixture were added to the above suspension, mixed and stirred evenly, and finally a 5 mg/ml mixed system dispersion was formed. Then, it was reacted under N 2 at 120℃ for 8h to obtain a natural polysaccharide hydrogel with 3D structure. Soak the polysaccharide gel with ethanol twice, each time for 3 hours, the mass volume ratio of the polysaccharide gel to ethanol is 1:15, and then freeze-dry at a vacuum degree of 2.5KPa and a temperature of -40°C for 20 hours The natural polysaccharide airgel material is obtained.

将所得的天然多糖气凝胶材料加工成圆柱体,浸渍到0.1%的薄荷提取物水溶液中,以料棒的形式加入到卷烟滤嘴中制备成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel material is processed into a cylinder, immersed in 0.1% mint extract aqueous solution, and added to a cigarette filter in the form of a rod to prepare a composite cigarette filter rod.

实施例4 Example 4

将10份的微晶纤维素、0.1份BaSO4分散到离子液体中超声分散处理1h,得到均匀的悬浮液。将1重量份的烯丙基蔗糖醚、0.05重量份的碳酸钙-葡萄糖酸内酯混合物加入到上述的悬浮液中,混合搅拌均匀,最终形成10mg/mL的分散体系。将上述的分散体系在300W条件下超声处理40min,得到3D结构的天然多糖水凝胶。用丙酮和乙醇先后浸泡上述多糖凝胶各2次,每次持续3h,所述的多糖凝胶与乙醇或丙酮的质量体积比为1:15,然后在真空度为2.0KPa,温度为-50℃条件下冷冻干燥30h得到所述的天然多糖气凝胶材料。 Disperse 10 parts of microcrystalline cellulose and 0.1 part of BaSO 4 into the ionic liquid for ultrasonic dispersion treatment for 1 h to obtain a uniform suspension. Add 1 part by weight of allyl sucrose ether and 0.05 part by weight of calcium carbonate-gluconolactone mixture into the above suspension, mix and stir evenly, and finally form a dispersion system of 10 mg/mL. The above dispersion system was ultrasonically treated at 300W for 40min to obtain a natural polysaccharide hydrogel with a 3D structure. Soak the above-mentioned polysaccharide gel twice in succession with acetone and ethanol for 3 hours each time. The mass-volume ratio of the polysaccharide gel to ethanol or acetone is 1:15, and then the vacuum degree is 2.0KPa, the temperature is -50 The natural polysaccharide airgel material was obtained by freeze-drying at ℃ for 30 h.

将所得的天然多糖气凝胶材料加工成柱状体,浸渍到0.01%的津巴布韦烟草提取物的水溶液中,以料棒的形式加入到卷烟滤嘴中制备成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel material is processed into a columnar body, impregnated into an aqueous solution of 0.01% Zimbabwean tobacco extract, and added to a cigarette filter in the form of a rod to prepare a composite cigarette filter rod.

实施例5 Example 5

将4份的甘蔗纤维、3份的微晶纤维素、3份海藻酸钠以及0.05份蒙脱土填料分散到10%的NaOH溶液中,搅拌1h得到均匀的悬浮液。将0.1份戊二醛/京尼平(w/w=1:1)、碳酸钙-葡萄糖酸内酯混合物加入到上述的悬浮液中,混合搅拌均匀,最终形成15mg/mL的分散液,将上述的分散液在100℃条件下通N2反应5h,得到3D结构的天然多糖水凝胶。用乙醇-丙酮-乙醇先后浸泡上述天然多糖凝胶各1、1、2次,每次持续3h,所述的多糖水凝胶与乙醇、丙酮的质量体积比为1:15,然后在真空度为1.5KPa,温度为-50℃条件下冷冻干燥30h得到所述的天然多糖气凝胶材料。 Disperse 4 parts of sugarcane fiber, 3 parts of microcrystalline cellulose, 3 parts of sodium alginate and 0.05 part of montmorillonite filler into a 10% NaOH solution, and stir for 1 h to obtain a uniform suspension. Add 0.1 part of glutaraldehyde/genipin (w/w=1:1) and calcium carbonate-gluconolactone mixture to the above suspension, mix and stir evenly, and finally form a 15 mg/mL dispersion. The above dispersion was reacted under N 2 at 100° C. for 5 hours to obtain a natural polysaccharide hydrogel with a 3D structure. Use ethanol-acetone-ethanol to soak the above-mentioned natural polysaccharide gel successively 1, 1, 2 times, each time for 3 hours, the mass-volume ratio of the polysaccharide hydrogel to ethanol and acetone is 1:15, and then The natural polysaccharide airgel material is obtained by freeze-drying for 30 hours under the condition of 1.5KPa and a temperature of -50°C.

将所得的天然多糖气凝胶材料加工成微球,喷涂0.1%的天然有机酸水溶液,干燥后以颗粒的形式加入到卷烟滤嘴中制备成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel material is processed into microspheres, sprayed with 0.1% natural organic acid aqueous solution, dried and added to cigarette filters in the form of particles to prepare composite cigarette filter rods.

实施例6 Example 6

将8份的辣木纤维和2份的透明质酸分散到5%的NaOH水溶液中超声处理1h,得到均匀的悬浮液。将0.1份的戊二醛、0.05份的碳酸钙-葡萄糖酸内酯混合物加入到上述的悬浮液中,混合搅拌均匀,形成20mg/mL的分散液,在400W条件下超声处理30min,得到3D结构的天然多糖水凝胶。用丙酮、乙醇浸泡上述天然多糖水凝胶各2次,每次持续3h,所述的天然多糖水凝胶与丙酮、乙醇的质量体积比为1:10,然后在真空度为1.0KPa,温度为-50℃条件下冷冻干燥40h得到所述的天然多糖气凝胶材料 Disperse 8 parts of Moringa fiber and 2 parts of hyaluronic acid into 5% NaOH aqueous solution and sonicate for 1 h to obtain a homogeneous suspension. Add 0.1 part of glutaraldehyde and 0.05 part of calcium carbonate-gluconolactone mixture to the above suspension, mix and stir evenly to form a 20mg/mL dispersion, and ultrasonically treat it at 400W for 30min to obtain a 3D structure natural polysaccharide hydrogels. Soak the above-mentioned natural polysaccharide hydrogel with acetone and ethanol for 2 times each time for 3 hours. The mass-to-volume ratio of the natural polysaccharide hydrogel to acetone and ethanol is 1:10, and then in a vacuum of 1.0KPa, the temperature Freeze-drying at -50°C for 40 hours to obtain the natural polysaccharide airgel material

将所得的天然多糖气凝胶材料加工成直径较小的柱状体,浸渍0.01%的生津剂溶液,干燥后以滤棒中线的形式在滤嘴中添加制成复合卷烟滤嘴滤棒。 The obtained natural polysaccharide airgel material is processed into a columnar body with a smaller diameter, impregnated with 0.01% body fluid-stimulating agent solution, dried and added to the filter tip in the form of the center line of the filter rod to make a composite cigarette filter tip filter rod.

将上述实施例所制得的含天然多糖气凝胶材料的复合卷烟滤嘴滤棒加工成卷烟,制成的卷烟样品分别在储存1个月、3个月和6个月后进行抽吸感官评吸,并与普通卷烟(对照例)对比,结果如表1所示: The composite cigarette filter tip filter rod containing natural polysaccharide airgel material prepared in the above examples is processed into cigarettes, and the cigarette samples made are respectively smoked and sensory after being stored for 1 month, 3 months and 6 months. Appraise smoking, and compare with common cigarette (control example), the result is as shown in table 1:

可见,含本发明的天然多糖气凝胶材料的滤棒能够长期保持烟气修饰剂,延缓其在储存过程中的损失;同时,实验中发现,在滤棒工作温度(略高于室温)下即可保证抽吸时相对均匀的释放烟气修饰剂,能够保持卷烟香气的稳定性、持久性和/或香气释放随时间的均匀一致性。 It can be seen that the filter stick containing the natural polysaccharide airgel material of the present invention can keep the smoke modifier for a long time and delay its loss during storage; at the same time, it is found in the experiment that at the filter stick working temperature (slightly higher than room temperature) It can ensure the relatively uniform release of the smoke modifier during smoking, and can maintain the stability and persistence of the cigarette aroma and/or the uniform consistency of the aroma release over time.

以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。 The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.

Claims (5)

1. a natural polysaccharide aeroge, is characterized in that, it is prepared by the method comprising the following steps:
(1) by the natural polysaccharide of 10 weight portions, 0~0.1 weight portion fillers dispersed to ultrasonic dispersion treatment 20-40 in solventMin, obtains uniform natural polysaccharide suspension;
(2) reinforcing agent of the crosslinking agent of 0.1~0.5 weight portion, 0.05~0.1 weight portion is joined above-mentioned natural manyIn sugar suspension, mixing and stirring, obtains natural polysaccharide mixed system dispersion liquid;
(3) by above-mentioned natural polysaccharide mixed system dispersion liquid logical N at 100~120 DEG C2Under condition, react 2~10h; OrUltrasonic processing 20~40min under power 200~400W condition, obtains the natural polysaccharide hydrogel of 3D structure;
(4) soak above-mentioned natural polysaccharide hydrogel 1~2 time with ethanol or acetone substep, continue 1~3h at every turn, describedThe mass ratio of natural polysaccharide hydrogel and ethanol or acetone is 1:10~15, is then 0.5~2.5KPa in vacuum, temperatureFor freeze drying 20~60h under-40~-60 DEG C of conditions, obtain described natural polysaccharide aeroge.
2. natural polysaccharide aeroge according to claim 1, is characterized in that, wherein:
Described natural polysaccharide is selected from sodium alginate, root of kudzu vine fiber, sugarcane fibre, tobacco stalk fibre, Moringa fiber, poly galactolipinOne or more in aldehydic acid, microcrystalline cellulose, carboxymethyl cellulose, starch, shitosan or hyaluronic acid;
Described filler is selected from one or more in submicron order silica, brium carbonate, barium sulfate, calcium carbonate or imvite;
It is that 2~10% sodium hydrate aqueous solutions, mass concentration are 10~20% that described solvent is selected from water, ionic liquid, mass concentrationAcetic acid aqueous solution, the calcium chloride water that mass concentration is 20~50%, the barium chloride solution that mass concentration is 20~50%Or one in the mass concentration solder(ing)acid that is 20~50%;
Described crosslinking agent is selected from ethylene glycol diglycidylether, glutaraldehyde, allylsucrose ether, acetic anhydride, Geniposide or carboxylic firstOne in base sodium cellulosate;
Described reinforcing agent is the mixture that calcium carbonate and glucolactone mass ratio are 2:1.
3. natural polysaccharide aeroge according to claim 1, is characterized in that, in its hole, absorption has flue gas dressing agentComposition, described flue gas dressing agent composition be natural organic acids, plant polyphenol kind, amino acids, saponins, coolant agent menthol,One or more in tobacco extract, flowers and fruits extract.
Natural polysaccharide aeroge according to claim 3 for cigarette filter composite filter to increase its cigarette of flowing throughThe purposes of gas concentration, absorption harmful substances from flue gases and release flue gas dressing agent.
5. purposes according to claim 4, is characterized in that, the release of described flue gas dressing agent can keep cigarette perfume (or spice)Stability, persistence and/or the fragrance of gas discharge uniformity consistency in time.
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