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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Publication number
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
aeroge
cigarette
flue gas
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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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China Tobacco Yunnan Industrial Co Ltd
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • 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
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
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    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/15—Heterocyclic compounds having oxygen in the ring
    • C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
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    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
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    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • C08L1/26—Cellulose ethers
    • C08L1/28—Alkyl ethers
    • C08L1/286—Alkyl ethers substituted with acid radicals, e.g. carboxymethyl cellulose [CMC]
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    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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    • C08J2205/00—Foams characterised by their properties
    • C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026—Aerogel, i.e. a supercritically dried gel
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    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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    • C08K2003/265—Calcium, strontium or barium carbonate
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  • Dispersion Chemistry (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • 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

A kind of natural polysaccharide aeroge, its preparation method and the application in cigarette
Technical field
The present invention is specifically related to a kind of natural polysaccharide aeroge, its preparation method and the application in cigarette, belongs to smoking material technical field.
Background technology
The Chinese-style cigarette High Tier Brand future development of high-quality slender joss stick, the low evil of China's tobacco business forward, low tar, this certainly will require scientific worker that product development and the achievements conversion of new technologies and materials direction are constantly provided. Wherein, on traditional flavoring and casing basis, excavate that the fragrance of the low burnt cigarette of Chinese style is revised and compensated to new application addition manner, jealous and strength seems particularly important. Filter stick, as the filtration system of cigarette smoke, except adsorbing flue gas, holding back, also can be modified correction to main flume by further functionalization. In recent years, lightweight, high resiliency aerogel material are because possessing ultralow density (ρ=0.15～10mg/cm3), high specific area and porosity and excellent elasticity and machining property attracted scientific worker's extensive concern. By add functional mass on aeroge carrier, as the specific cigarette additive of the clear and rich plant extracts that promotes the production of body fluid, essence spice for cigarette and change flue gas pH etc., can carry out aesthetic quality's correction to cigarette product.
Natural polysaccharide gel discharges the many of area research in medicine control at present, and is mostly polysaccharide-based hydrogel, also fewer for the research of aeroge. Patent CN102793271B discloses the application of a kind of cross-linked chitosan porous microsphere with high specific surface area in cigarette filter, for adsorbing the harmful components of flue gas; Patent CN104525126A discloses a kind of preparation method of alginate fibre element aeroge oil absorption material, regulates its hydrophobicity to adsorb for water oil spilling by dipping pyrroles liquid. Philip Mirris Products Inc discloses a smoking product that comprises flavor delivery material; described flavor delivery material comprises the polymer substrate with 3D network structure; this polymer substrate is cross-linked and is formed by one or more polysaccharide combinations; can protect well comprised aroma constituent; be heated and just can discharge the odor additive in smoking product when higher than 220 DEG C but only have when matrix, limited its application in conventional cigarette.
Summary of the invention
First aspect present invention discloses a kind of novel natural polysaccharide aeroge, and 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 20-40min in solvent, obtain 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 in above-mentioned natural polysaccharide 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; Or ultrasonic processing 20～40min under power 200～400W condition, the natural polysaccharide hydrogel of acquisition 3D structure;
(4) soak above-mentioned natural polysaccharide hydrogel 1～2 time with ethanol or acetone substep, each 1～3h that continues, described natural polysaccharide hydrogel and the mass ratio of ethanol or acetone are 1:10～15, then be 0.5～2.5KPa in vacuum, temperature is freeze drying 20～60h under-40～-60 DEG C of conditions, obtains described natural polysaccharide aeroge.
Preferably, described natural polysaccharide is selected from one or more in sodium alginate, root of kudzu vine fiber, sugarcane fibre, tobacco stalk fibre, Moringa fiber, polygalacturonase, 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;
Described solvent is selected from the one in the solder(ing)acid that water, ionic liquid, mass concentration are 2～10% sodium hydrate aqueous solutions, the mass concentration acetic acid aqueous solution that is 10～20%, mass concentration is 20～50% calcium chloride water, barium chloride solution that mass concentration is 20～50% or mass concentration are 20～50%;
Described crosslinking agent is selected from the one in ethylene glycol diglycidylether, glutaraldehyde, allylsucrose ether, acetic anhydride, Geniposide or sodium carboxymethylcellulose;
Described reinforcing agent is the mixture that calcium carbonate and glucolactone mass ratio are 2:1.
Preferably, in the hole of described natural polysaccharide aeroge, absorption has flue gas dressing agent composition; Preferably, described flue gas dressing agent composition is one or more in natural organic acids, plant polyphenol kind, amino acids, saponins, coolant agent menthol, tobacco extract, flowers and fruits extract.
Second aspect present invention disclose described natural polysaccharide aeroge for cigarette filter composite filter with increase flow through its flue gas concentration, absorption harmful substances from flue gases and discharge the purposes of flue gas dressing agent.
The release of described flue gas dressing agent can keep stability, persistence and/or the fragrance of cigarette flavor to discharge uniformity consistency in time.
Beneficial effect of the present invention:
1, natural polysaccharide aerogel material of the present invention, surface polarity and aperture are adjustable, and the adsorbate of molecule, even low concentration or trace to different-diameter size and polarity power all has good adsorption capacity, can adsorb in a large number harmful substances from flue gases;
2, natural polysaccharide aerogel material of the present invention is by bonding cross-linking, and its module units difficult drop-off, prepares process and be also difficult for causing dust.
3, natural polysaccharide aerogel material of the present invention inside has 3D network structure and compared with macropore volume, specific area is higher, and the density that it is ultralow and high porosity can adsorb in a large number flue gas dressing agent composition; And the main flume aerogel material region of tending to flow through, increase the flue gas concentration of flowing through make to flow to change focus on aeroge region, absorption has flue gas dressing agent composition more easily to be carried and enter smoker oral cavity by main flume wash-out.
4, natural polysaccharide aerogel material of the present invention can keep and Stable Release for a long time, when delaying the loss of flue gas dressing agent in storage process and ensureing to aspirate simultaneously, discharge relatively uniformly, can keep stability, persistence and/or the fragrance of cigarette flavor to discharge uniformity consistency in time.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, technical scheme of the present invention is further described. Should be appreciated that specific embodiment described herein, only for explaining the present invention, is not limited to the technical solution.
Embodiment 1
By the natural polygalacturonase of 10 weight portions, 0.1 weight portion SiO2Ultrasonic dispersion treatment 1h in the acetic acid aqueous solution of fillers dispersed to 10%, obtains uniform polysaccharide suspension; By the crosslinking agent ethylene glycol diglycidylether of 0.1 weight portion, calcium carbonate-glucolactone mixture of 0.05 weight portion joins in above-mentioned natural polysaccharide suspension again, and mixing and stirring finally forms the mixed system dispersion liquid of 15mg/ml. At 100 DEG C of logical N2Under condition, react 5h, obtain the natural polysaccharide hydrogel of 3D structure, soak above-mentioned polysaccharide gel each 1,1,2 time with ethanol, acetone, ethanol successively substep, each 3h that continues, described polysaccharide hydrogel and the mass volume ratio of ethanol or acetone are 1:10, then be 1.0KPa in vacuum, temperature is that under-45 DEG C of conditions, freeze drying 25h obtains described natural polysaccharide aeroge.
By the fresh and sweet cigarette grass solution of extract of obtained natural polysaccharide aeroge dipping 0.1%, join and in cigarette filter, be prepared into composite cigarette filter tip capable filter stick with the form of charge bar.
Embodiment 2
The microcrystalline cellulose of the root of kudzu vine fiber of 8 weight portions and 2 weight portions is distributed to 20% CaCl2In the aqueous solution, add 0.05% the ultrasonic dispersion treatment 1h of sodium carbonate simultaneously, obtain uniform suspension, 0.05 weight portion calcium carbonate-glucolactone mixture is joined to above-mentioned suspension, add again the acetic anhydride of 0.1 weight portion, mixing and stirring, finally forms the mixed system dispersion liquid of 10mg/ml; By above-mentioned mixed system dispersion liquid, ultrasonic power is to process 30min under 200W condition, obtain the natural polysaccharide hydrogel of 3D structure, successively soak above-mentioned polysaccharide gel 2 times with ethanol, each 3h that continues, described polysaccharide hydrogel and the mass volume ratio of ethanol are 1:10, are then 0.5KPa in vacuum, and temperature is that under-40 DEG C of conditions, freeze drying 35h obtains described natural polysaccharide aerogel material.
The natural polysaccharide aerogel material of gained is processed into microballoon, in the aqueous solution of dipping 0.05% spice berry extract, joins and in cigarette filter, be prepared into composite cigarette filter tip capable filter stick with the form of particle after dry.
Embodiment 3
The carboxymethyl cellulose of the shitosan of 5 weight portions, 5 weight portions is distributed to (v/v=2:1) ultrasonic dispersion treatment 1h in water/alcohol mixed solvent, obtain uniform suspension, calcium carbonate-glucolactone mixture of 0.1 part of glutaraldehyde, 0.05 weight portion is joined in above-mentioned suspension, mixing and stirring, finally forms the mixed system dispersion liquid of 5mg/ml. Then logical N under 120 DEG C of conditions2Reaction 8h, the natural polysaccharide hydrogel of acquisition 3D structure. With the above-mentioned polysaccharide gel of alcohol immersion 2 times, continue 3h at every turn, described polysaccharide gel and the mass volume ratio of ethanol are 1:15, are then 2.5KPa in vacuum, temperature is the natural polysaccharide aerogel material of freeze drying 20h described in obtaining under-40 DEG C of conditions.
The natural polysaccharide aerogel material of gained is processed into cylinder, is impregnated in 0.1% the mint extract aqueous solution, join and in cigarette filter, be prepared into composite cigarette filter tip capable filter stick with the form of charge bar.
Embodiment 4
By the microcrystalline cellulose of 10 parts, 0.1 part of BaSO4Be distributed to ultrasonic dispersion treatment 1h in ionic liquid, obtain uniform suspension. Calcium carbonate-glucolactone mixture of the allylsucrose ether of 1 weight portion, 0.05 weight portion is joined in above-mentioned suspension, and mixing and stirring, finally forms the dispersion of 10mg/mL. By above-mentioned dispersion ultrasonic processing 40min under 300W condition, obtain the natural polysaccharide hydrogel of 3D structure. Successively soak above-mentioned polysaccharide gel each 2 times with acetone and ethanol, each 3h that continues, the mass volume ratio of described polysaccharide gel and ethanol or acetone is 1:15, is then 2.0KPa in vacuum, and temperature is that under-50 DEG C of conditions, freeze drying 30h obtains described natural polysaccharide aerogel material.
The natural polysaccharide aerogel material of gained is processed into column, is impregnated in 0.01% the aqueous solution of Zimbabwe's tobacco extract, join and in cigarette filter, be prepared into composite cigarette filter tip capable filter stick with the form of charge bar.
Embodiment 5
The sugarcane fibre of 4 parts, the microcrystalline cellulose of 3 parts, 3 parts of sodium alginates and 0.05 part of montmorillonite filler are distributed in 10% NaOH solution, stir 1h and obtain uniform suspension. 0.1 part of glutaraldehyde/Geniposide (w/w=1:1), calcium carbonate-glucolactone mixture are joined in above-mentioned suspension, and mixing and stirring, finally forms the dispersion liquid of 15mg/mL, by above-mentioned dispersion liquid logical N under 100 DEG C of conditions2React 5h, obtain the natural polysaccharide hydrogel of 3D structure. Successively soak above-mentioned natural polysaccharide gel each 1,1,2 time with ethanol-acetone-ethanol, each 3h that continues, the mass volume ratio of described polysaccharide hydrogel and ethanol, acetone is 1:15, then be 1.5KPa in vacuum, temperature is that under-50 DEG C of conditions, freeze drying 30h obtains described natural polysaccharide aerogel material.
The natural polysaccharide aerogel material of gained is processed into microballoon, and spraying 0.1% the natural organic acids aqueous solution, joins and in cigarette filter, is prepared into composite cigarette filter tip capable filter stick with the form of particle after dry.
Embodiment 6
The hyaluronic acid of the Moringa fiber of 8 parts and 2 parts is distributed to ultrasonic processing 1h in 5% the NaOH aqueous solution, obtains uniform suspension. The glutaraldehyde of 0.1 part, calcium carbonate-glucolactone mixture of 0.05 part are joined in above-mentioned suspension, and mixing and stirring, forms the dispersion liquid of 20mg/mL, and ultrasonic processing 30min under 400W condition obtains the natural polysaccharide hydrogel of 3D structure. With each 2 times of acetone, the above-mentioned natural polysaccharide hydrogel of alcohol immersion, each 3h that continues, the mass volume ratio of described natural polysaccharide hydrogel and acetone, ethanol is 1:10, is then 1.0KPa in vacuum, and temperature is that under-50 DEG C of conditions, freeze drying 40h obtains described natural polysaccharide aerogel material
The natural polysaccharide aerogel material of gained is processed into the column that diameter is less, and the fluid generating agent solution of dipping 0.01% adds and makes composite cigarette filter tip capable filter stick with the form of filter stick center line after being dried in filter tip.
The prepared above-described embodiment composite cigarette filter tip capable filter stick containing natural polysaccharide aerogel material is processed into cigarette, the cigarette sample of making aspirates sensory evaluating smoking respectively after storing 1 month, 3 months and 6 months, and contrast with regular-size cigarette (reference examples), result is as shown in table 1:
Visible, can keep for a long time flue gas dressing agent containing the filter stick of natural polysaccharide aerogel material of the present invention, delay its loss in storage process; , in experiment, find meanwhile, can ensure to aspirate time, discharge relatively uniformly flue gas dressing agent under filter stick operating temperature (a little more than room temperature), can keep stability, persistence and/or the fragrance of cigarette flavor to discharge uniformity consistency in time.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

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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