CN105727852A - Supercritical drying method of preoxidized fiber/silicon-aluminium aerogel composite insulation board - Google Patents
Supercritical drying method of preoxidized fiber/silicon-aluminium aerogel composite insulation board Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 66
- 239000004964 aerogel Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000352 supercritical drying Methods 0.000 title claims abstract description 32
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 29
- 239000004411 aluminium Substances 0.000 title claims abstract description 28
- 238000009413 insulation Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011240 wet gel Substances 0.000 claims abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 9
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 235000019353 potassium silicate Nutrition 0.000 claims description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 14
- 239000010881 fly ash Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000000499 gel Substances 0.000 claims description 9
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 8
- 238000006073 displacement reaction Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 6
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 238000007885 magnetic separation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 125000005401 siloxanyl group Chemical group 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000010883 coal ash Substances 0.000 claims description 2
- 230000002265 prevention Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010943 off-gassing Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000004965 Silica aerogel Substances 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- -1 Acetonitrile Ethanol Carbon dioxide Ethanol Chemical compound 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 238000001467 acupuncture Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a supercritical drying method of a preoxidized fiber/silicon-aluminium aerogel composite insulation board. The method is characterized by firstly carrying out solvent exchange and hydrophobic modification on preoxidized fiber/silicon-aluminium wet gel, then putting hydrophobically modified wet gel in a high pressure reactor, pouring a supercritical medium, setting the heating temperature, carrying out heating and carrying out outgassing or reflux after the medium in the reactor is in a supercritical state to bring out a solvent in wet gel until the solvent is completely recovered, wherein the supercritical medium is an acetonitrile, ethanol or carbon dioxide solvent. The supercritical drying method provided by the invention has the excellent effects that the product produced by the method has high yield and high production efficiency, dusts slightly and can undergo industrial scaling up; the supercritical drying method can be integrated onto assembly lines; the whole preparation method is simple and easy to control, avoids strong acid and alkali corrosion, has low requirements for equipment and is suitable for industrial production after scaling up.
Description
Technical field
The present invention relates to the drying means of a kind of warming plate, be specifically related to the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards.
Background technology
Aeroge is the material that in solid matter, heat conductivity is minimum, is only slightly higher than vacuum, is approximately 0.013W/m K.Aeroge also has extremely low density, is the minimum solid of the density generally acknowledged in the world, and least density can accomplish 3kg/m3, more slightly higher than the density of air.Therefore aeroge is the insulation material that heat insulation effect is best in the world, density is minimum.
The kind of current aeroge is more, has carbon aerogels, silicon system aeroge, alumina aerogels etc..The preparing raw material and can adopt tetraethyl orthosilicate or waterglass of silica aerogel, preparation technology can be respectively adopted non-pressure process and supercritical, and its preparation technology is highly developed.The preparation of alumina aerogels, mainly alkoxide process, drying process adopts supercritical process substantially.And the preparation of silica/alumina composite aerogel, rarely having report, even if being prepared into pluralgel, being also adopt alkoxide process to carry out gel.
Inorganic salt method prepares the method for sial composite aerogel, rarely has report, and at present major part aeroge composition is one pack system, for instance silica aerogel is mainly silicon dioxide, aluminum aeroge be mainly composed of aluminium oxide.The raw material of silica aerogel has two kinds, and one is tetraethyl orthosilicate, and one is waterglass, and two kinds of raw materials have different sol gel processings.The raw material major part that alumina aerogels adopts is aluminium-alcohol salt, adopts supercritical process.Therefore, the raw material production cost that tradition prepares alumina aerogels is expensive, and gel process is complicated；If what traditional alumina aerogels preparation adopted is tetraethyl orthosilicate, sol-gel process is also intended to the hydrolysis through raw material and polycondensation, and preparation technology is more complicated.
Inorganic salt method, is adopt two kinds of inorganic salts, according to certain processing compound, as long as according to certain dispensing order, it is possible to easily preparation quality and the good gel of condition.Production process is simple, and former material is cheap, has the prospect that Large scale processes is applied.
Summary of the invention
Simple in order to obtain preparation technology, the composite aerogel that cost is low, it is good and have the supercritical drying drying method of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards of some strength that the present invention proposes globality.
In order to achieve the above object, the invention provides employing following technical proposals:
A kind of supercritical drying drying method of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, first pre-oxidized fibers/sial wet gel is carried out solvent displacement and hydrophobically modified, then the wet gel that hydrophobically modified is good is put into autoclave, pour supercritical medium into, set heating-up temperature, be heated, after the medium state of reactor reaches supercritical, carry out exitting or refluxing, the solvent in wet gel is taken out of, until solvent recovery is complete；Described supercritical medium is acetonitrile, ethanol or carbon dioxide solvent.
First preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, the setting heating-up temperature of supercritical drying drying method is higher than the temperature of the super critical point of medium 5～10 DEG C, the high 0.5～2MPa of pressure.
Second preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, prepares pre-oxidized fibers/silicon-aluminium aerogel and comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution；
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1～2min obtains forerunner's mixed solution；
(3) pre-oxidized fibers is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the pre-oxidized fibers obtained strengthens, at room temperature aging 12h；
(4) carrying out solvent displacement, the sial compound wet gel that pre-oxidized fibers step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains pre-oxidized fibers after drying and strengthens silicon-aluminium aerogel warming plate.
A kind of 3rd preferred version of the supercritical drying drying method of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, the preparation method of waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) mechanical grinding；
3) acidleach: at 150 DEG C～220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%～98% with the ratio that solid-to-liquid ratio is 2:1～1:1 of sulphuric acid in flyash, reacts 4～6h；
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2～1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75～95 DEG C, after stirring 1～3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1～1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%～12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1～1:2, heat after 6～10h in reactor at 160～200 DEG C, be cooled to room temperature, filter and wash solid slag with water.
4th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, the light transmittance of sial compound wet gel is more than 80%.
5th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, pre-oxidized fibers is that low melting point polyester fiber and pre-oxidized polyacrylonitrile fiber prepare, and the fusing point of described low melting point polyester fiber is 160～180 DEG C；Described pre-oxidized fibers mass content in the silicon-aluminium aerogel that described pre-oxidized fibers strengthens is 50～70%.
6th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, solvent displacement adopts ethanol, and hexane equal solvent, described holding temperature is 50～70 DEG C, and described solvent time swap is more than 8 hours.
7th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, modified raw material adopts siloxanyl modified liquid, and modification temperature is 50～70 DEG C, and modification time is 7～9h.
8th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, it is 0.015～0.022W/ (m K) that pre-oxidized fibers strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220～450kg/m3, water absorption rate is less than 3%.
9th preferred version of the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, it is the fire prevention of A level that pre-oxidized fibers strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
Compared with immediate prior art, technical scheme provided by the invention has following excellent effect:
1. the invention provides the simple process of a kind of supercritical drying drying method using two kinds of alkaline, inorganic salts to prepare pre-oxidized fibers enhancing sial composite aerogel；
2. the invention provides the product that supercritical drying drying method produces, product yield is high, and production efficiency is high, and product dry linting is slight, it is possible to carry out industrialization amplification；
3. supercritical drying drying method can be integrated to streamline, it is simple to industrialized production；
4. the raw material of the present invention is sodium metaaluminate, waterglass and pre-oxidized fibers, and raw materials for production are cheap；
5. the gel method of the present invention be carry out mixture by two kinds of materials after, carry out gel reaction, it is to avoid the complicated approach of other aeroge collosol and gel；
6. whole preparation method is simple and easy to control, corrodes without strong acid and strong base, low for equipment requirements, after method is amplified, is suitable for industrialized production.
Detailed description of the invention
It is described in further detail below in conjunction with specific embodiment, technical scheme is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Inorganic salt method prepares the process of sial composite aerogel:
First configuring the sodium aluminate solution of certain mass concentration, stirring, until sodium metaaluminate complete hydrolysis；Then, by the requirement of waterglass dilution technique proportioning；When stirring, in the water glass solution after diluted, add the sodium aluminate solution of required amount, after continuing stirring 1～2min, it is ensured that when solution mix homogeneously, stop stirring, stand 5～30min, obtain forerunner's mixed solution.
Pre-oxidized fibers is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the pre-oxidized fibers obtained strengthens, at room temperature aging 12h；Then, carry out solvent displacement, the sial compound wet gel that the pre-oxidized fibers obtained strengthens is immersed alcoholic solution.After solvent has been replaced, adopting siloxanyl modified liquid to be modified, modification temperature is 50～70 DEG C, and modification time is 7～9h.Finally, carry out normal pressure and dry dry, the sial composite aerogel granule that felt strengthens must be stung.
The sodium aluminate solution of configuration, it is necessary to all dissolve, it is not possible to have impurity, solution requires transparent limpid, and sodium aluminate solution requires matching while using, can not long storage time；Waterglass is in the process of dilution, after adding a certain amount of deionized water, and more than magnetic agitation 5min, it is ensured that dilute solution mix homogeneously.
Postcritical medium can adopt acetonitrile, ethanol or carbon dioxide solvent, and the supercritical temperature of acetonitrile is 274.7 DEG C, supercritical pressure 4.83MPa；The supercritical temperature of ethanol is 243 DEG C, supercritical pressure 6.7MPa；The supercritical temperature of carbon dioxide is 31.1 DEG C, and supercritical pressure is 7.29MPa；The temperature requirement of critical drying process is higher than the temperature of the super critical point of medium 5～10 DEG C, the high 0.5～2MPa of pressure, to guarantee that superfluid dries the protected effect to sample.
The preparation of waterglass: flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 4min, then with 82% sulphuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C react 4h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 90 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 1:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 10.5%, and put into autoclave heat 10h, reaction temperature 180 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass.
The preparation of pre-oxidized fibers: by raw material mix homogeneously, feed components mass fraction is as follows: low melting point polyester fiber 10 parts, pre-oxidized polyacrylonitrile fiber 90 parts, the fusing point of low melting point polyester fiber is 160～180 DEG C；Spraying liquid antistatic in composite fibre, spray the composite fibre after liquid antistatic and bank up at normal temperatures 20～24 hours, liquid antistatic each constituent mass number is as follows: non-ionic antistatic agent 4 parts, 4 parts of weak cation antistatic additive, 92 parts of water；Being then passed through combing, become net, acupuncture prepares pre-oxidized fibers finished product.
Properties of product test different technical parameters prepared, is shown in following table.
Technological parameter in each embodiment of table 1 and performance
| Embodiment | 1 | 2 | 3 | 4 |
| Supercritical medium | Acetonitrile | Ethanol | Carbon dioxide | Ethanol |
| Supercritical temperature/DEG C | 280 | 250 | 40 | 250 |
| Supercritical pressure/MPa | 6 | 8 | 9 | 8 |
| Mixing time/min | 1 | 1 | 2 | 2 |
| Time of repose/min | 5 | 30 | 20 | 10 |
| Holding temperature/DEG C | 50 | 70 | 65 | 60 |
| Solvent time swap/h | 8 | 24 | 12 | 12 |
| Modification temperature/DEG C | 50 | 70 | 55 | 60 |
| Modification time/h | 7 | 9 | 8 | 8 |
| Heat conductivity W/ (m K) | 0.022 | 0.021 | 0.015 | 0.018 |
| Density/kg/m3 | 450 | 350 | 280 | 220 |
| Water absorption rate/% | 3 | 2.5 | 2 | 2.1 |
Above example is only limited in order to technical scheme to be described; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention.
Claims (10)
1. the supercritical drying drying method of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards, it is characterized in that, pre-oxidized fibers/sial the wet gel of solvent displacement and hydrophobically modified is put into autoclave, pour supercritical medium into, setting heating-up temperature heats, after the medium state of reactor reaches supercritical, carry out exitting or refluxing；Described supercritical medium is acetonitrile, ethanol or carbon dioxide solvent.
2. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 1, it is characterized in that, the setting heating-up temperature of described supercritical drying drying method is higher than the temperature of the super critical point of medium 5～10 DEG C, the high 0.5～2MPa of pressure.
3. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 1, it is characterised in that the preparation of described pre-oxidized fibers/silicon-aluminium aerogel comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution；
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1～2min obtains forerunner's mixed solution；
(3) pre-oxidized fibers is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the pre-oxidized fibers obtained strengthens, at room temperature aging 12h；
(4) carrying out solvent displacement, the sial compound wet gel that pre-oxidized fibers step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains pre-oxidized fibers after drying and strengthens silicon-aluminium aerogel warming plate.
4. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterised in that the preparation method of described waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) mechanical grinding；
3) acidleach: at 150 DEG C～220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%～98% with the ratio that solid-to-liquid ratio is 2:1～1:1 of sulphuric acid in flyash, reacts 4～6h；
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2～1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75～95 DEG C, after stirring 1～3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1～1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%～12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1～1:2, heat after 6～10h in reactor at 160～200 DEG C, be cooled to room temperature, filter and wash solid slag with water.
5. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterised in that the light transmittance of described sial compound wet gel is more than 80%.
6. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterized in that, described pre-oxidized fibers is that low melting point polyester fiber and pre-oxidized polyacrylonitrile fiber prepare, and the fusing point of described low melting point polyester fiber is 160～180 DEG C；Described pre-oxidized fibers mass content in the silicon-aluminium aerogel that described pre-oxidized fibers strengthens is 50～70%.
7. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterized in that, the displacement of described solvent adopts ethanol, hexane equal solvent, described holding temperature is 50～70 DEG C, and described solvent time swap is more than 8h.
8. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterised in that described modified raw material adopts siloxanyl modified liquid, and modification temperature is 50～70 DEG C, and modification time is 7～9h.
9. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterized in that, it is 0.015～0.022W/ (m K) that described pre-oxidized fibers strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220～450kg/m3, water absorption rate is less than 3%.
10. the supercritical drying drying method of a kind of pre-oxidized fibers/silicon-aluminium aerogel composite insulation boards according to claim 3, it is characterised in that it is the fire prevention of A level that described pre-oxidized fibers strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
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