CN104130444B - A kind of preparation method of Triafol T aeroge - Google Patents
A kind of preparation method of Triafol T aeroge Download PDFInfo
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- CN104130444B CN104130444B CN201410354796.0A CN201410354796A CN104130444B CN 104130444 B CN104130444 B CN 104130444B CN 201410354796 A CN201410354796 A CN 201410354796A CN 104130444 B CN104130444 B CN 104130444B
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- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 46
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 6
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims abstract 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 50
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- 238000005352 clarification Methods 0.000 claims description 26
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 14
- 150000001298 alcohols Chemical class 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 230000008929 regeneration Effects 0.000 abstract description 4
- 238000011069 regeneration method Methods 0.000 abstract description 4
- 230000001112 coagulating effect Effects 0.000 abstract description 3
- 238000000352 supercritical drying Methods 0.000 abstract description 3
- 229920006304 triacetate fiber Polymers 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000499 gel Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 238000001746 injection moulding Methods 0.000 abstract 1
- 239000011240 wet gel Substances 0.000 abstract 1
- 238000010992 reflux Methods 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 229920002678 cellulose Polymers 0.000 description 19
- 235000010980 cellulose Nutrition 0.000 description 19
- 239000001913 cellulose Substances 0.000 description 18
- 238000013019 agitation Methods 0.000 description 13
- 238000007789 sealing Methods 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000004964 aerogel Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000010408 film Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
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- 230000015572 biosynthetic process Effects 0.000 description 4
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- 241000196324 Embryophyta Species 0.000 description 2
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- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
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- 231100000053 low toxicity Toxicity 0.000 description 1
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- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The invention provides a kind of preparation method of Triafol T aeroge.The method comprises the steps：By in triacetate fiber crude granule addition Isosorbide-5-Nitrae dioxane, heating and stirring makes Triafol T fully dissolve to form colourless transparent solution；Add anhydrous alcohols solvent and be sufficiently stirred for dispersion to the solution under heating stirring state and re-form colourless transparent solution；Near room temperature in the solution injection moulding mould, will be stood and be naturally cooling to, wet gel and aging a period of time is formed；Dried with CO 2 supercritical and remove solvent therein, obtain Triafol T aeroge.Technology of preparing proposed by the present invention, needs not move through coagulating bath regeneration, supercritical drying can be directly carried out after forming gel, without cumbersome and time-consuming solvent time swap.The Triafol T density prepared using the method for the present invention is low, and specific surface area is high, good toughness, good moldability.
Description
Technical field
The invention belongs to cellulose aerogels field of material preparation, and in particular to a kind of system of Triafol T aeroge
Preparation Method.
Background technology
Aeroge is one of minimum solid material of current known density, loose structure with three-dimensional manometer network and
High porosity, high-specific surface area, low heat conduction coefficient, low-k, in a low voice low optical index, unique property such as speed, no
Only so that the material is intriguing in basic research, and contain the prospect of being widely applied in many fields, be expected to
It is applied to heat-insulated, sound absorption, absorption, catalysis and the aspect such as optically and electrically.Cellulose is most abundant natural organic in the world
Thing, accounts for more than the 50% of plant kingdom's carbon content.Plant（Particularly cotton, fiber crops, timber, bamboo etc.）Every year by photosynthesis,
Hundreds of millions tons of celluloses can be produced, is the topmost source of cellulose.With the airsetting that cellulose and its derivates are prepared as raw material
Glue is referred to as cellulose aerogels (aerocellulose), with the distinctive nanometer porous structure of aerogel material and high
The characteristics such as porosity, are a kind of new aerogel materials developed in recent years.Someone is referred to as the third generation gas of new life
Gel rubber material, has incorporated the excellent properties of itself while possessing traditional aerogel property, such as good biocompatibility and
Degradability, has great application prospect at aspects such as pharmacy industry, cosmetics, forestry, the energy, environment, catalysis, be one not
The biological species polymeric material of disconnected development.With the intensification recognized cellulose aerogels, and global energy crisis aggravation,
People are stepped up for the research enthusiasm of cellulose aerogels, and various researchs also gradually increase, such as to cellulose origin, molten
The research of agent, drying mode etc..
Source and preparation process according to cellulose are divided into native cellulose aeroge, regenerated cellulose aeroge and fibre
The plain class of derivative aeroge three of dimension.The preparation method that current cellulose aerogels are used is usually in molten first by cellulose dissolution
In agent（Ion liquid solvent or common solvent）In, then form regenerated cellulose gel, Ran Houjing through coagulating bath solidification regeneration
Solvent is repeatedly replaced（Generally alcohols solvent）, most afterwards through drying（Supercritical drying or freeze-drying）Removal solvent, obtains
Cellulose aerogels.The cellulose aerogels prepared using the method have the essential characteristic of aeroge, but have the disadvantage to prepare
Cheng Jing dissolvings, regeneration, solvent displacement, dry etc., manufacturing cycle is more long, and the quantity of solvent for using is big, high cost, and its gas for obtaining
The density of gel is generally larger.
Triafol T is a kind of important cellulose derivative, industrially has very important application, for example, three
Bexoid has good, transparent good, excellent mechanical performance of thermoplasticity etc., be widely used in security film film,
Photographic sheet substance（Or film）The extraordinary film such as raw material, X- light and chip base and insulation film barrier film；It is used in aerospace field
Film and solid propellant clad in space power system material etc.；The excellent raw material of Triafol T or reverse osmosis membrane；
Cellulose triacetate film is because of its excellent optical characteristics, it has also become indispensable in the liquid crystal display of positive place's Chaoyang phase
Critical function optical film materials.
Low-density fibre element aerogel material is prepared as raw material using Triafol T, is expected to hydrophobic because of its uniqueness
The characteristic such as property, toughness, insulating properties, thermal insulation, high porosity, low-density and being widely used in is adsorbed, is catalyzed, heat-insulated, optics, electricity
Each field such as, space flight.There was only Lie Bie Jeff physics Institute of Russian national academy of sciences in the world at present（Lebedev
Physical Institute）Carried out the development work of the Triafol T aeroge of low-density, and for laser etc. from
Daughter generation and the research of energy transmission.The method that they use is that Triafol T is first dissolved in into three in a heated state
Gel is formed after methyl alcohol cooling is subsequently adding in chloromethanes, supercritical carbon dioxide is dry after repeatedly being replaced with alcohols solvent
Arrive.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of Triafol T aeroge.
Triafol T aeroge density prepared by the preparation method of Triafol T aeroge of the invention for 3 ~
100mg/cm3, the three-dimensional netted nanoporous structure with the interlaced formation of nanofibers, by mould excipient.
The preparation method of Triafol T aeroge of the invention, comprises the steps successively：
1）Triafol T is incorporated in Isosorbide-5-Nitrae-dioxane, magnetic agitation is heated and condensing reflux, to three acetic acid
Cellulose is completely dissolved, and obtains achromaticity and clarification clear solution.
2）To step 1 under heating stirring and condensing reflux state）Middle that anhydrous alcohols solvent is added dropwise, solution remained colorless is clear
It is clear bright.
3）By step 2）In obtain hot solution injection mould in, after sealing stand and natural cooling, place certain hour,
Obtain the gel of Triafol T.
4）Using supercritical carbon dioxide drying means to step 3）In the gel that obtains be dried treatment, from mould
Take out, obtain the low-density Triafol T aeroge of mould institute figuration shape.
Wherein, step 1）Described in heating-up temperature be 50 DEG C to 80 DEG C.
Step 2）Described in heating-up temperature be 50 DEG C to 80 DEG C.Anhydrous alcohols solvent is methyl alcohol, ethanol, isopropanol etc., its
In preferably isopropanol.
Step 3）Described in natural cooling, to be cooled near room temperature and following, be specially cooled to 0 DEG C ~ 30 DEG C.
Step 1）、2）、3）The Triafol T solution of middle preparation, the mass percent of wherein Triafol T is
0.1% to 10%, Isosorbide-5-Nitrae-dioxane is 80 with the volume ratio of anhydrous alcohols:20 to 30:70, preferably 50:50.
Triafol T aeroge is prepared using the method for the present invention, Triafol T is dissolved in double solvents
Afterwards, gel can be formed through natural cooling, needs not move through coagulating bath regeneration, supercritical drying can be directly carried out after forming gel
It is dry, without cumbersome and time-consuming solvent time swap.The raw material that uses of preparation and solvent is simple and easy to get, low toxicity, preparation method letter
It is single controllable, there is no waste and pollution that a large amount of solvent displacements are produced, short preparation period, mild condition is economic and environment-friendly.Using this hair
The Triafol T of bright preparation, density is low, minimum to 3mg/cm3, the three-dimensional with the interlaced formation of nanofibers
Mesh nano microcellular structure, specific surface area is high, good toughness, with certain transparency, good moldability.This aeroge is in energy
The fields such as source, environment, catalysis, optics and inertial confinement fusion（ICF）Target material application field has important application prospect.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of Triafol T aeroge sample pore structure prepared by embodiment 2；
Fig. 2 is the stereoscan photograph of Triafol T aeroge sample pore structure prepared by embodiment 3；
Fig. 3 is that the photo of Triafol T aeroge sample prepared by embodiment 6 and its ESEM of pore structure shine
Piece；
Fig. 4 is that the photo of Triafol T aeroge sample prepared by embodiment 9 and its ESEM of pore structure shine
Piece.
Specific embodiment
The present invention is further elaborated by the following examples.But the invention is not limited in this, the skill of association area
Art personnel can realize the present invention by the method different from specific examples below.
Experimental technique used in following embodiments is conventional method unless otherwise specified
Material used in following embodiments, reagent etc., unless otherwise specified, commercially obtain.
Embodiment 1
Weigh in 10g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, 70 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 50ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 20 DEG C are stood and naturally cooled to after sealing, about 20 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, is had
Mould assigns the translucent Triafol T aeroge sample of shape, and density is 103.8mg/cm3。
Embodiment 2
Weigh in 5g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, 70 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 50ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 10 DEG C are stood and naturally cooled to after sealing, about 20 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, is had
Mould assigns the translucent Triafol T aeroge sample of shape, and Fig. 1 is triacetate fiber manufactured in the present embodiment
The stereoscan photograph of plain aeroge, it can be seen that the aeroge has nano level microcellular structure, aperture is several nanometers to number
Hundred nanometers.The aeroge sample rate is 54.1mg/cm3, specific surface area is 229m2/g。
Embodiment 3
Weigh in 2.5g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, be heated in oil bath
70 DEG C apply condensing reflux simultaneously, and magnetic agitation about 2 hours obtains the solution of water white transparency clarification, are then keeping heating to stir
Mix and condensing reflux state under, thereto be added dropwise 50ml isopropanol, obtain water white transparency clarification solution.Solution is poured into mould
20 DEG C are stood and naturally cooled in tool, after sealing, about 30 hours are stood, and obtain transparent Triafol T gel.Through super
Isosorbide-5-Nitrae-dioxane and isopropanol solvent in critical carbon dioxide dry technology removal gel, then remove mould, are had
There is mould to assign the translucent Triafol T aeroge sample of shape, Fig. 2 is fine three acetic acid manufactured in the present embodiment
The stereoscan photograph of the plain aeroge of dimension, it can be seen that the aeroge has by interlaced three wieners for being formed of nanofibers
Rice micro-structural, aperture is less than 100 nanometers.The aeroge sample rate is 28.6mg/cm3, specific surface area is 296m2/g。
Embodiment 4
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 80ml, 50 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 20ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 0 DEG C is stood and naturally cooled to after sealing, about 50 hours are stood, obtain transparent Triafol T gel.Through overcritical
Carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, obtains with mould
Tool assigns the translucent Triafol T aeroge sample of shape, and density is 13.2mg/cm3。
Embodiment 5
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 60ml, 60 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 40ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 10 DEG C are stood and naturally cooled to after sealing, about 50 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, is had
Mould assigns the translucent Triafol T aeroge sample of shape, and density is 12.7mg/cm3。
Embodiment 6
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, 80 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 50ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 30 DEG C are stood and naturally cooled to after sealing, about 40 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, is had
Mould assigns the translucent Triafol T aeroge sample of shape, and Fig. 3 left sides are three acetic acid manufactured in the present embodiment
The optical photograph of cellulose aerogels bead, the right is stereoscan photograph, it can be seen that the aeroge has by nanofiber
The three-dimensional manometer micro-structural of the interlaced formation of silk, aperture is less than 100 nanometers.The aeroge density is 11.5mg/cm3, compare table
Area is 451m2/g。
Embodiment 7
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 30ml, 70 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the isopropanol of 70ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 20 DEG C are stood and naturally cooled to after sealing, about 50 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and isopropanol solvent in technology removal gel, then removes mould, is had
Mould assigns the translucent Triafol T aeroge sample of shape, and density is 12.1mg/cm3。
Embodiment 8
Weigh in 0.5g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, be heated in oil bath
70 DEG C apply condensing reflux simultaneously, and magnetic agitation about 2 hours obtains the solution of water white transparency clarification, are then keeping heating to stir
Mix and condensing reflux state under, thereto be added dropwise 50ml isopropanol, obtain water white transparency clarification solution.Solution is poured into mould
20 DEG C are stood and naturally cooled in tool, after sealing, about 50 hours are stood, and obtain transparent Triafol T gel.Through super
Isosorbide-5-Nitrae-dioxane and isopropanol solvent in critical carbon dioxide dry technology removal gel, then remove mould, are had
There is mould to assign the translucent Triafol T aeroge sample of shape, density is 7.2mg/cm3。
Embodiment 9
Weigh in 0.2g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, be heated in oil bath
70 DEG C apply condensing reflux simultaneously, and magnetic agitation about 2 hours obtains the solution of water white transparency clarification, are then keeping heating to stir
Mix and condensing reflux state under, thereto be added dropwise 50ml isopropanol, obtain water white transparency clarification solution.Solution is poured into mould
20 DEG C are stood and naturally cooled in tool, after sealing, about 60 hours are stood, and obtain transparent Triafol T gel.Through super
Isosorbide-5-Nitrae-dioxane and isopropanol solvent in critical carbon dioxide dry technology removal gel, then remove mould, are had
There is mould to assign the translucent Triafol T aeroge sample of shape, Fig. 4 left sides are three vinegar manufactured in the present embodiment
The optical photograph of acid cellulose aeroge cylinder, the right is stereoscan photograph, it can be seen that the aeroge has by nanometer
The three-dimensional manometer micro-structural of the interlaced formation of filament, aperture is less than 100 nanometers.The aeroge density is 4.6mg/cm3。
Embodiment 10
Weigh in 0.1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, be heated in oil bath
70 DEG C apply condensing reflux simultaneously, and magnetic agitation about 2 hours obtains the solution of water white transparency clarification, are then keeping heating to stir
Mix and condensing reflux state under, thereto be added dropwise 50ml isopropanol, obtain water white transparency clarification solution.Solution is poured into mould
20 DEG C are stood and naturally cooled in tool, after sealing, about 72 hours are stood, and obtain transparent Triafol T gel.Through super
Isosorbide-5-Nitrae-dioxane and isopropanol solvent in critical carbon dioxide dry technology removal gel, then remove mould, are had
There is mould to assign the translucent Triafol T aeroge sample of shape, density is 3.0mg/cm3。
Embodiment 11
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, 70 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the ethanol of 50ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 20 DEG C are stood and naturally cooled to after sealing, about 60 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and alcohol solvent in technology removal gel, then removes mould, obtains with mould
Tool assigns the translucent Triafol T aeroge sample of shape, and the aeroge density is 12.7mg/cm3。
Embodiment 12
Weigh in 1g Triafol Ts addition flask, add the Isosorbide-5-Nitrae-dioxane of 50ml, 70 are heated in oil bath
DEG C simultaneously apply condensing reflux, magnetic agitation about 2 hours, obtain water white transparency clarification solution, then keep heating stirring
And under condensing reflux state, the methyl alcohol of 50ml is added dropwise thereto, obtain the solution of water white transparency clarification.Solution is poured into mould
In, 20 DEG C are stood and naturally cooled to after sealing, about 60 hours are stood, obtain transparent Triafol T gel.Face through super
Boundary's carbon dioxide dries the Isosorbide-5-Nitrae-dioxane and methanol solvate in technology removal gel, then removes mould, obtains with mould
Tool assigns the translucent Triafol T aeroge sample of shape, and the aeroge density is 13.1mg/cm3。
Claims (6)
1. a kind of preparation method of Triafol T aeroge, it is characterised in that comprise the steps successively：
1）Triafol T is dissolved in Isosorbide-5-Nitrae-dioxane under heating stirring state, isopropanol is then added dropwise thereto
Solvent, obtains the solution of the Triafol T of the achromaticity and clarification clear homogeneous of heat；
2）By in described Triafol T solution injection mould, rear Temperature fall cooling is then sealed against, and stand one
The section time, obtain the Triafol T gel of clear homogeneous；
3）Treatment is dried to the Triafol T gel using supercritical carbon dioxide seasoning, three acetic acid is obtained fine
The plain aeroge of dimension.
2. preparation method according to claim 1, it is characterised in that：Step 1）In heating-up temperature be 50 DEG C to 80 DEG C.
3. preparation method according to claim 1, it is characterised in that：Step 1）In 1,4- dioxane and isopropanol
Volume ratio is 80:20 to 30:70.
4. preparation method according to claim 1, it is characterised in that：Step 1）In 1,4- dioxane and isopropanol body
Product is than being 50:50.
5. preparation method according to claim 1, it is characterised in that：Step 1）In the mass ratio of Triafol T be
0.1~10%。
6. preparation method according to claim 1, it is characterised in that：Step 2）In time of repose be 20 ~ 72 hours.
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