CN109463796A - A kind of glass fibre toughening composite aerogel and preparation method thereof - Google Patents

A kind of glass fibre toughening composite aerogel and preparation method thereof Download PDF

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Publication number
CN109463796A
CN109463796A CN201811179578.2A CN201811179578A CN109463796A CN 109463796 A CN109463796 A CN 109463796A CN 201811179578 A CN201811179578 A CN 201811179578A CN 109463796 A CN109463796 A CN 109463796A
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CN
China
Prior art keywords
glass fibre
composite aerogel
preparation
glass
aeroge
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811179578.2A
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Chinese (zh)
Inventor
杨光远
彭三文
刘强
邓少鹏
程占刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hubei China Tobacco Cigarette Materials Factory
China Tobacco Hunan Industrial Co Ltd
Original Assignee
Hubei China Tobacco Cigarette Materials Factory
China Tobacco Hunan Industrial Co Ltd
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Publication date
Application filed by Hubei China Tobacco Cigarette Materials Factory, China Tobacco Hunan Industrial Co Ltd filed Critical Hubei China Tobacco Cigarette Materials Factory
Priority to CN201811179578.2A priority Critical patent/CN109463796A/en
Publication of CN109463796A publication Critical patent/CN109463796A/en
Pending legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/308Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances vitamins

Abstract

The present invention provides a kind of preparation method of glass fibre toughening composite aerogel, use silicon source, dehydrated alcohol, deionized water and hydrochloric acid as preparation SiO2 aeroge raw material, using glass fibre as filter rod segments bracket, it is prepared and does not burn the glass fibre toughening composite aerogel composite material that cigarette filter rod temperature descending section uses as heating.The SiO that the present invention is had excellent performance by synthesizing materialization2Aeroge, as base material and in conjunction with glass fibre, it makes mechanical property and the efficiency that cools down meets the raw material for heating cigarette filter rod temperature descending section requirement of not burning, the silicon source of use is relatively broad, higher cost and control condition are not needed, it can prepare at normal temperatures and pressures, be conducive to be mass produced.

Description

A kind of glass fibre toughening composite aerogel and preparation method thereof
Technical field
The present invention relates to novel tobacco manufacturing field, specifically a kind of glass fibre toughening composite aerogel and its preparation side Method.
Background technique
Aeroge generally can be divided into oxide silica aerogel, such as SiO2、A12O3、TiO2、ZrO2、B2O3、CuO、MoO2、MgO、 SnO2、Nb2O5、Cr2O3Deng;Organic charcoal-aero gel, such as the after heat treatment gained airsetting of RF, PF, MF, PUR precursor aeroge Glue and carbide aeroge, such as SiC, TiC, MoC aeroge, in addition there are some multicomponent aeroges, such as multiphase aeroge A12O3/SiO2、TiO2/SiO2、Fe2O3/A12O3、CuO/ZnO/A12O3、MgO/A12O3/SiO2Deng.Due to the unique object of aeroge Reason feature and performance have relatively broad application in various industries at present.
High porosity and nanometer network the skeleton interconnection that aerogel material has are formed by meso-hole structure, determine It has fabulous temperature reduction performance, be expected to high temperature catalyst support, high temperature kiln and hypersonic aircraft etc. it is military, Civil field is as temperature with high efficiency materials'use.Wherein SiO2Aeroge is as a kind of light nanoporous that temperature reduction performance is excellent Amorphous solid material, thermal coefficient are highly suitable to be applied for heating not burning cigarette down to 0.011-0.017W/ (mK) Filter stick temperature descending section.Because it is not only nontoxic, but also can realize that filter rod segments resistance to suction is big by adjusting the porosity of aeroge Small adjusting is controllable.But due to SiO2The network skeleton of aeroge is very fragile, and mechanical property is unable to reach filter stick production and answers The requirement of conjunction, and toughness is poor, therefore how to improve the mechanical performance of aeroge, increasing its toughness is by SiO2Aeroge application It does not burn the key of cigarette filter rod temperature descending section in low temperature.
Summary of the invention
The present invention provides a kind of glass fibre toughening composite aerogel and preparation method thereof, is had excellent performance by synthesizing materialization SiO2Aeroge, as base material and in conjunction with glass fibre, make mechanical property and cooling efficiency meet plus The raw material of hot cigarette filter rod temperature descending section requirement of not burning.
A kind of preparation method of glass fibre toughening composite aerogel, includes the following steps:
Step 1: silicon source, dehydrated alcohol, deionized water and the hydrochloric acid of aeroge 1:(8-15 in molar ratio will be prepared): (3- 9): 0.032 mixing adjusts pH to 3-4, the stirring hydrolysis 12h or more under conditions of 30-45 DEG C;
Step 2: 0.8mol/L ammonium hydroxide is added in above-mentioned mixed solution, additive amount is the mixed solution 200-450mL Addition ammonia vol is 20ml-35ml, stirs 3-5min rapidly and carries out gelation reaction, obtains silica dioxide gel;
Step 3: successively using ethyl alcohol, deionized water to wash repeatedly in glass fibre, and the dry 2h under 120 DEG C of environment;
Step 4: the glass that silica dioxide gel obtained in step 2 is poured into mold, while step 3 being handled Fiber is cut according to the size of mold, and layering is successively spread in mold, and mold is sealed;
Step 5: mold is put into 30-50 DEG C of water-bath, after 7-15min inner gel, gel, wet gel is continued It is placed in water-bath, is washed repeatedly using the mixed liquor of silicon alkoxide and dehydrated alcohol, and ethyl alcohol is used alone and impregnates 20min, SiO2 aeroge is made after aging 8-10h, the mechanical property and mechanical strength of gel can be increased;
Step 6: SiO made from step 52Aeroge is put into deionized water and washs, then in 60-120 DEG C of environment Glass fibre toughening composite aerogel can be obtained in middle dry 12h.
Further, the silicon source includes but is not limited to the base silanol and organic of ethyl orthosilicate, methyl orthosilicate, three Polyalcohol, the waterglass (sodium metasilicate) of Si modification.
Further, in step 3 the type of glass fibre include but is not limited to alkali-free glass fibre, have alkali containing glass fibre, Medium-alkali glass fibre;The form of glass fibre includes long glass fibres and glass mat.
Further, if the glass fibre used in step 3 be long glass fibres, using glass fibre carding machine into Row reprocessing, to increase the surface area of fiber.
Glass fibre toughening composite aerogel prepared by a kind of method as described above does not burn cigarette filter rod as heating Temperature descending section uses.
The invention has the following beneficial effects:
1, the silicon source that this method uses is relatively broad, and including cheap waterglass, reduces the production cost, and increases A possibility that having added large-scale production;
2, it is applied in actual product using the temperature descending section that this method makes, resistance to suction is adjustable to be extremely with circumference 24.0mm, the pole resistance to suction that length is 100mm or 120mm is close, i.e. 300mmH2O;
3, compared to the aerosil for not adding fiber, when fiber content is (21-35) %, material bending resistance is strong It spends up to 1.533MPa, compression strength is 1.904MPa (25% deformation), and elasticity modulus 1.120MPa is prepared using this method The mechanical property of composite aerogel significantly improve, as shown in table 1:
Influence (part) of 1 fiber content of table to material compression strength, bending strength
Sample number into spectrum Fiber content % Elasticity modulus (Mpa) Bending strength (Mpa)
1 12 0.298 0.382
2 14 0.352 0.504
3 16 0.411 0.626
4 18 0.592 0.821
5 20 0.689 0.99
6 22 0.875 1.105
7 24 0.98 1.276
8 26 1.103 1.387
4, the cooling effect of glass fiber reinforced composite aeroge prepared by the present invention can reach low temperature and not burn cigarette Requirement, when fiber additive amount is in (12-34) %, thermal coefficient (0.0195-0.0249) W/ (mK) of resulting materials, with The increase of glass fiber quality score, SiO2The bulk density of aerogel composite is gradually increased, and porosity is gradually reduced, Thermal coefficient gradually rises, and realizes according to cooling demand, realizes regulatory function;
5, not only has certain mechanical strength according to aerogel composite prepared by this method, there are also adjustable hot Energy (variation of aeroge porosity can bring the variation of thermal coefficient, to realize the adjustable of hot property), therefore not only Suitable for preparing novel tobacco product, can also be applied to other includes the fields such as aerospace, medicine and machinery.
Specific embodiment
Below in conjunction with specific embodiment, the technical solution in the present invention is clearly and completely described.
The present invention provides a kind of preparation method of glass fibre toughening composite aerogel, the compound airsetting of glass fibre toughening Glue can be used for making low temperature and not burn the filter stick temperature descending section of cigarette.Due to SiO2The temperature reduction performance of aeroge is excellent, and light weight is close It spends low, is a kind of ideal solid amorphous material, but due to its network structure fragility, bad mechanical strength, toughness is not high, limit It has been made not burn the application of cigarette filter rod section in low temperature.The present invention is by glass fibre and SiO2Aeroge combines, and realizes this The promotion of composite materials property and temperature reduction performance.
Embodiment one
A kind of preparation method of glass fibre toughening composite aerogel, by ethyl orthosilicate, dehydrated alcohol, deionized water and 1:10:9:0.032 is mixed hydrochloric acid in molar ratio, adjusts pH to 4, the stirring hydrolysis 12h or more under conditions of 40 DEG C;Then upper Addition 0.8mol/L ammonium hydroxide in solution is stated, 5min is stirred rapidly and carries out gelation reaction, obtain silica dioxide gel;By glass fibers Dimension is successively washed using ethyl alcohol, deionized water repeatedly, and the dry 2h under 120 DEG C of environment, if using long glass fibres, it is also necessary to It is reprocessed using glass fibre carding machine, increases the surface area of fiber;Aforementioned obtained silica dioxide gel is poured into again In specific mold, at the same glass fibre is proper according to the size cutting of mold, and according to 16% mass fraction, layering is successively It spreads in mold, is put into after mold is sealed in 45 DEG C of water-bath, in 10min inner gel.After gel, wet gel is continued to place It in water-bath, is washed repeatedly using the mixed liquor of silicon alkoxide and dehydrated alcohol, and ethyl alcohol is used alone and impregnates 20min, aging After 8h, the mechanical property and mechanical strength of gel can be increased, SiO2 aeroge is made;By the SiO of glass fibre toughening obtained2 Aeroge is put into deionized water and washs, then the dry 12h in 90 DEG C of environment, can be obtained and prepares low temperature and do not burn cigarette The composite material of filter stick temperature descending section, the resistance to suction of the material are about 292mmH2O, elasticity modulus 0.429MPa, bending modulus are 0.603MPa, thermal coefficient are 0.0211W/ (mK).
Embodiment two
A kind of preparation method of glass fibre toughening composite aerogel, by waterglass, dehydrated alcohol, deionized water and hydrochloric acid 1:8:6:0.032 is mixed in molar ratio, adjusts pH to 3, the stirring hydrolysis 12h or more under conditions of 35 DEG C;Then above-mentioned molten 0.8mol/L ammonium hydroxide is added in liquid, stirs 3min rapidly and carries out gelation reaction, silica dioxide gel is obtained, by above-mentioned preparation Silica dioxide gel is washed with deionized, and removes the impurity in silica dioxide gel;By glass fibre successively using ethyl alcohol, go Ionized water washs repeatedly, and the dry 2h under 120 DEG C of environment;Aforementioned obtained silica dioxide gel is poured into specific mold again In, while glass fibre is proper according to the size cutting of mold, it is 24% according to mass fraction, layering is successively spread into mold In, 8min in 50 DEG C of water-bath is put into after mold is sealed.After gel, wet gel is continued to be placed in water-bath, uses silicon The mixed liquor of alkoxide and dehydrated alcohol washs repeatedly, and ethyl alcohol is used alone and impregnates 20min, by glass fibers obtained after aging 8h Tie up the SiO of toughening2Aeroge is put into deionized water and washs, then in 80 DEG C of environment dry 12h can be obtained prepare it is low The composite material of the warm cigarette filter rod temperature descending section that do not burn.The resistance to suction of the material is about 314mmH2O, elasticity modulus are 1.033MPa, bending modulus 1.253MPa, thermal coefficient are 0.0229W/ (mK).
In above-described embodiment, it can also add functional particulate and realize that low temperature does not burn a variety of special function of cigarette filter rod temperature descending section Can, the functional particulate of addition has the high-temperature resistant particles such as SiC, BN or all kinds of fluorescent grains, to realize the illumination effect of filter stick.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Belong to those skilled in the art in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, all answers It is included within the scope of the present invention.

Claims (5)

1. a kind of preparation method of glass fibre toughening composite aerogel, it is characterised in that include the following steps:
Step 1: silicon source, dehydrated alcohol, deionized water and the hydrochloric acid of aeroge 1:(8-15 in molar ratio will be prepared): (3-9): 0.032 mixing, adjusts pH to 3-4, the stirring hydrolysis 12h or more under conditions of 30-45 DEG C;
Step 2: 0.8mol/L ammonium hydroxide is added in above-mentioned mixed solution, additive amount is mixed solution 200-450mL addition Ammonia vol is 20ml-35ml, stirs 3-5min rapidly and carries out gelation reaction, obtains silica dioxide gel;
Step 3: successively using ethyl alcohol, deionized water to wash repeatedly in glass fibre, and the dry 2h under 120 DEG C of environment;
Step 4: the glass fibre that silica dioxide gel obtained in step 2 is poured into mold, while step 3 being handled It is cut according to the size of mold, layering is successively spread in mold, and mold is sealed;
Step 5: mold is put into 30-50 DEG C of water-bath, after 7-15min inner gel, gel, wet gel is continued to place It in water-bath, is washed repeatedly using the mixed liquor of silicon alkoxide and dehydrated alcohol, and ethyl alcohol is used alone and impregnates 20min, aging SiO2 aeroge is made after 8-10h, the mechanical property and mechanical strength of gel can be increased;
Step 6: SiO2 aeroge made from step 5 is put into deionized water and washs, then done in 60-120 DEG C of environment Glass fibre toughening composite aerogel can be obtained in dry 12h.
2. the preparation method of glass fibre toughening composite aerogel as described in claim 1, it is characterised in that: the silicon source packet Include but be not limited to ethyl orthosilicate, methyl orthosilicate, three base silanol and organic-silicon-modified polyalcohol, waterglass.
3. the preparation method of glass fibre toughening composite aerogel as described in claim 1, it is characterised in that: glass in step 3 The type of glass fiber includes but is not limited to alkali-free glass fibre, has alkali containing glass fibre, medium-alkali glass fibre;The form of glass fibre Including long glass fibres and glass mat.
4. the preparation method of glass fibre toughening composite aerogel as described in claim 1, it is characterised in that: if in step 3 The glass fibre used is long glass fibres, then is reprocessed using glass fibre carding machine, to increase the surface area of fiber.
5. a kind of glass fibre toughening composite aerogel as prepared by any one of claim 1-4 method, not as heating The cigarette filter rod temperature descending section that burns uses.
CN201811179578.2A 2018-10-10 2018-10-10 A kind of glass fibre toughening composite aerogel and preparation method thereof Pending CN109463796A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113071186A (en) * 2021-03-26 2021-07-06 深圳市雷军科技有限公司 Impact-resistant heat-insulating nano material and preparation method thereof
CN115852739A (en) * 2022-11-29 2023-03-28 南京聚力纤维材料有限公司 Ultrathin glass fiber paper composite aerogel and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113071186A (en) * 2021-03-26 2021-07-06 深圳市雷军科技有限公司 Impact-resistant heat-insulating nano material and preparation method thereof
CN115852739A (en) * 2022-11-29 2023-03-28 南京聚力纤维材料有限公司 Ultrathin glass fiber paper composite aerogel and preparation method thereof

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Application publication date: 20190315