CN105605885A - Super-critical drying method for fiber needled felt/silicon-aluminum aerogel composite insulation board - Google Patents
Super-critical drying method for fiber needled felt/silicon-aluminum aerogel composite insulation board Download PDFInfo
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- CN105605885A CN105605885A CN201610065744.0A CN201610065744A CN105605885A CN 105605885 A CN105605885 A CN 105605885A CN 201610065744 A CN201610065744 A CN 201610065744A CN 105605885 A CN105605885 A CN 105605885A
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- needled felt
- silicon
- fiber needled
- drying method
- composite insulation
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- 239000000835 fiber Substances 0.000 title claims abstract description 59
- 239000004964 aerogel Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000000352 supercritical drying Methods 0.000 title claims abstract description 30
- 238000009413 insulation Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 20
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title abstract 3
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000012986 modification Methods 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011240 wet gel Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 32
- 229910052782 aluminium Inorganic materials 0.000 claims description 25
- 239000004411 aluminium Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 14
- 235000019353 potassium silicate Nutrition 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000010881 fly ash Substances 0.000 claims description 11
- 239000000499 gel Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 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 8
- 238000002386 leaching Methods 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 7
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 claims description 6
- 239000003365 glass fiber Substances 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
- -1 polypropylene Polymers 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 229920000784 Nomex Polymers 0.000 claims description 3
- 230000032683 aging 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
- 238000000227 grinding Methods 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 238000007885 magnetic separation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004763 nomex Substances 0.000 claims description 3
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 239000010883 coal ash Substances 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 230000002265 prevention Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 3
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000002209 hydrophobic effect Effects 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000006467 substitution reaction 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 8
- 239000000047 product Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000004965 Silica aerogel Substances 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 238000001467 acupuncture Methods 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 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
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- MJEMIOXXNCZZFK-UHFFFAOYSA-N ethylone Chemical compound CCNC(C)C(=O)C1=CC=C2OCOC2=C1 MJEMIOXXNCZZFK-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B2210/00—Drying processes and machines for solid objects characterised by the specific requirements of the drying good
- F26B2210/14—Veneer, i.e. wood in thin sheets
Landscapes
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a super-critical drying method for a fiber needled felt/silicon-aluminum aerogel composite insulation board. The super-critical drying method comprises the following steps: performing solvent substitution and hydrophobic modification on fiber needled felt/silicon-aluminum wet gel; placing the wet gel subjected to the hydrophobic modification in a high pressure reactor; pouring a super-critical medium into the reactor; setting a heating temperature for heating; deflating or reflowing after the medium state of the reactor reaches a super-critical state to carry a solvent out of the wet gel till the solvent is recovered fully, wherein the super-critical medium is an acetonitrile, ethanol or carbon dioxide solvent. A product produced with the super-critical drying method provided by the invention has high product yield, high production efficiency and low powder falling rate, and can be amplified industrially; the super-critical drying method can be integrated into a production line; a whole preparation method is easy to operate, is free from strong acid and strong alkali corrosion, has low equipment requirement, and is suitable for industrial production after amplification.
Description
Technical field
The present invention relates to a kind of drying means of warming plate, be specifically related to a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boardsSupercritical drying drying method.
Background technology
Aeroge is the minimum material of thermal conductivity factor in solid matter, only a little more than vacuum, is approximately 0.013W/mK. AirsettingGlue also has extremely low density, is the solid of the density minimum of generally acknowledging in the world, and least density can be accomplished 3kg/m3, compares airDensity slightly high. Therefore aeroge is the insulation material that heat insulation effect is best in the world, density is minimum.
The kind of aeroge is more at present, and having carbon aerogels, silicon is aeroge, alumina aerogels etc. Silica aerogelRaw materials can adopt ethyl orthosilicate or waterglass, and preparation technology can adopt respectively non-pressure process and overcritical, its preparationTechnique is very ripe. The preparation of alumina aerogels, is mainly alkoxide process, and drying process adopts supercritical process substantially.And the preparation of silica/alumina composite aerogel rarely has report, even if be prepared into plural gel, be also to adopt alkoxide processCarry out gel.
Inorganic salts legal system, for the method for sial composite aerogel, rarely has report, and current most of aeroge composition is one pack system, exampleIf silica aerogel is mainly silica, the main component of aluminium aeroge is aluminium oxide. The raw material of silica aerogel have two kinds,One is ethyl orthosilicate, and one is waterglass, and two kinds of raw material have different sol gel processings. Alumina aerogelsThe raw material major part adopting is aluminium-alcohol salt, adopts supercritical process. Therefore, tradition is prepared the raw material life of alumina aerogelsProduct cost costliness, gel process complexity; If what the preparation of traditional alumina aerogels adopted is ethyl orthosilicate, sol-gelProcess is also will be through hydrolysis and the polycondensation of raw material, and preparation technology is more complicated.
Inorganic salts method, is to adopt two kinds of inorganic salts, according to certain processing compound, as long as according to certain batching order, just canWith light preparation quality and product lover's gel. Production process is simple, former material is cheap, has extensive process applicationProspect.
Summary of the invention
The composite aerogel simple in order to obtain preparation technology, cost is low, the present invention proposes globality well and has some strengthThe supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards.
In order to achieve the above object, the invention provides employing following technical proposals:
A supercritical drying drying method for fiber needled felt/silicon-aluminium aerogel composite insulation boards, first by wet fiber needled felt/sial solidifyingGlue carries out solvent exchange and hydrophobically modified, then the good wet gel of hydrophobically modified is put into autoclave, pours overcritical Jie intoMatter, set heating-up temperature, heat, the medium state of reactor reach overcritical after, exit or reflux, willSolvent in wet gel is taken out of, until solvent recovery is complete; Described supercritical medium is that acetonitrile, ethanol or carbon dioxide are moltenAgent.
First preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, supercritical dryingThe setting heating-up temperature of method is higher 5～10 DEG C than the temperature of the super critical point of medium, the high 0.5～2MPa of pressure.
Second preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, prepares sial multipleClosing aeroge comprises the following steps:
(1) the preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, to add in water glass solution preparation in step (1) sodium metaaluminateSolution, is uniformly mixed 1～2min and obtains forerunner's mixed solution;
(3) fiber needled felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, obtainsThe compound wet gel of sial that fiber needled felt strengthens, at room temperature aging 12h;
(4) carry out solvent exchange, it is molten that the compound wet gel of sial that the fiber needled felt that step (3) is obtained strengthens immerses ethanolLiquid, through insulation, solvent exchange, modification, obtains fiber needled felt after being dried and strengthens silicon-aluminium aerogel warming plate.
The 3rd preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, the system of waterglassPreparation Method 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, the ratio that is 2:1～1:1 in the solid-to-liquid ratio of flyash and sulfuric acid by flyash withConcentration is 80%～98% sulfuric acid mixing, reaction 4～6h;
4) Separation of Solid and Liquid: reactant is cooled to after room temperature, is that 1:2～1:6 preparation adds water by the solid-to-liquid ratio of flyash and water,At 75～95 DEG C, stir after 1～3h, suction filtration, the water washing that it is 2:1～1:2 that filter cake is used by the solid-to-liquid ratio of flyash and water,Obtain solution and the high silicon acid leaching residue of ferric sulfate and aluminum sulfate;
5) acid leaching residue is prepared waterglass: the ratio that is 1:1～1:2 by solid-to-liquid ratio by acid leaching residue and 9%～12% soda lyeExample preparation mixed liquor heats after 6～10h at 160～200 DEG C in reactor, is cooled to room temperature, filters and wash with water solidSlag.
The 4th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, sial is compound wetThe light transmittance of gel is more than 80%.
The 5th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, fiber needled feltThe composite fibre Nomex being formed by glass fibre and polypropylene fibre, the mass content of described glass fibre is 50～70%;The diameter of described glass fibre is 5～10um, and the diameter of described polypropylene fibre is 10～15um.
The 6th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, solvent exchange is adoptedWith ethanol, hexane equal solvent, described holding temperature is 50～70 DEG C, the described solvent exchange time is more than 8 hours.
The 7th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, the raw material of modificationAdopt siloxy group modification liquid, modification temperature is 50～70 DEG C, and modification time is 7～9h.
The 8th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, fiber needled feltThe thermal conductivity factor that strengthens silicon-aluminium aerogel warming plate is 0.015～0.022W/ (mK), and density is 220～450kg/m3, inhaleWater rate is less than 3%.
The 9th preferred version of the supercritical drying drying method of fiber needled felt/silicon-aluminium aerogel composite insulation boards, fiber needled feltStrengthening silicon-aluminium aerogel warming plate is the fire prevention of A level, 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 two kinds of alkaline, inorganic salts of a kind of use and prepare the overcritical of fiber needled felt enhancing sial composite aerogelThe simple process of drying means;
2. the invention provides the product that supercritical drying drying method is produced, product yield is high, and production efficiency is high, and product dry linting is slight,Can carry out industrialization amplification;
3. supercritical drying drying method can be integrated to streamline, is convenient to suitability for industrialized production;
4. raw material of the present invention are sodium metaaluminate, waterglass and fiber needled felt, and raw materials for production are cheap;
Gel method of the present invention be carry out mixture by two kinds of materials after, carry out gel reaction, avoided other aerogeThe complicated approach of collosol and gel;
6. whole preparation method is simple and easy to control, without strong acid and strong base corrosion, low for equipment requirements, after method is amplified, is applicable to industryChange and produce.
Detailed description of the invention
Be described in further detail below in conjunction with specific embodiment, technical scheme of the present invention be clearly and completely described,Obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment. Based on the reality in the present inventionExecute example, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong toThe scope of protection of the invention.
Inorganic salts legal system is for the process of sial composite aerogel:
First configure the sodium aluminate solution of certain mass concentration, stir, until sodium metaaluminate complete hydrolysis; Then, by water glassThe requirement of glass dilution technique proportioning; Under the condition stirring, in dilution water glass solution later, add the inclined to one side aluminium of required amountAcid sodium solution, continues to stir after 1～2min, guarantees, in situation that solution mixes, to stop stirring, and leaves standstill 5～30min,Obtain forerunner's mixed solution.
Fiber needled felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the fiber obtainingThe compound wet gel of sial that Nomex strengthens, at room temperature aging 12h; Then, carry out solvent exchange, by the fiber needle obtainingThe compound wet gel of sial that thorn felt strengthens immerses ethanolic solution. After solvent exchange completes, adopt siloxy group modification liquid to changeProperty, modification temperature is 50～70 DEG C, modification time is 7～9h. Finally, carry out normal pressure bake drying, must sting the silicon that felt strengthensAluminium composite aerogel particle.
The sodium aluminate solution of configuration, must all dissolve, and cannot have impurity, and solution requires transparent limpid, and sodium metaaluminate is moltenLiquid requires matching while using, can not long storage time; Waterglass dilution process in, after adding a certain amount of deionized water,More than magnetic agitation 5min, guarantee that dilute solution mixes.
Postcritical medium can adopt acetonitrile, ethanol or carbon dioxide solvent, and the supercritical temperature of acetonitrile is 274.7 DEG C, super facingThe pressure 4.83MPa of boundary; The supercritical temperature of ethanol is 243 DEG C, supercritical pressure 6.7MPa; The supercritical temperature of carbon dioxideBe 31.1 DEG C, supercritical pressure is 7.29MPa; The temperature requirement of critical drying process than the temperature of the super critical point of medium high by 5～10 DEG C, the high 0.5～2MPa of pressure, to guarantee the dry protection effect to sample of superfluid.
The preparation of waterglass: flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 4minAfter the fine powder powder that obtains, then mix by solid-to-liquid ratio 5:4 with 82% sulfuric acid, and react 4h at 200 DEG C; Reaction finishesBeing cooled to after room temperature, is that 1:3 adds water by the solid-to-liquid ratio of flyash and water, is heated to 90 DEG C, stirs 2h, and suction filtration obtains filter cakeAfter, and be that 1:1 washs by the solid-to-liquid ratio of flyash and water, obtain solution and the high silicon acid leaching residue of ferric sulfate and aluminum sulfate;By the solid-to-liquid ratio of acid leaching residue and solution be 1:1 to add concentration be 10.5% soda lye, and put into autoclave heating10h, 180 DEG C of reaction temperatures; Be cooled to after room temperature, filter and use a small amount of water washing solid slag, obtain waterglass.
The preparation of fiber needled felt: the composite fibre of glass fibre and polypropylene fibre composition is introduced to filament throwing roller two through guide eyelitBetween individual roller, by mutual extruding and the rotation of two filament throwing rollers, subsequently first through the needle plate of a rectangle with certain speed pairMultiple yarns is carried out top-down acupuncture, and then multiple yarns is entered with certain speed through another rectangle needle plateRow acupuncture from bottom to top, more obtain fiber needled felt through pressure roller.
Properties of product test prepared by different technical parameters, sees the following form.
Technological parameter and performance in the each embodiment of table 1
| 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 exchange time/h | 8 | 24 | 12 | 12 |
| Modification temperature/DEG C | 50 | 70 | 55 | 60 |
| Modification time/h | 7 | 9 | 8 | 8 |
| Thermal conductivity factor W/ (mK) | 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 embodiment is only in order to technical scheme of the present invention to be described but not be limited those of ordinary skill in the fieldShould be appreciated that with reference to above-described embodiment and can modify or be equal to replacement the specific embodiment of the present invention, these be not de-From any amendment of spirit and scope of the invention or within being equal to and replacing the claim protection domain all awaiting the reply in application.
Claims (10)
1. a supercritical drying drying method for fiber needled felt/silicon-aluminium aerogel composite insulation boards, is characterized in that, by solvent exchangePut into autoclave with fiber needled felt/sial wet gel of hydrophobically modified, pour supercritical medium into, set heating-up temperature and addHeat, the medium state of reactor reach overcritical after, exit or reflux; Described supercritical medium is acetonitrile, ethanolOr carbon dioxide solvent.
2. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 1, itsBe characterised in that, the setting heating-up temperature of described supercritical drying drying method is higher 5～10 DEG C than the temperature of the super critical point of medium, pressureHigh 0.5～2MPa.
3. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 1, itsBe characterised in that, the preparation of described fiber needled felt/sial wet gel comprises the following steps:
(1) the preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, to add in water glass solution preparation in step (1) sodium metaaluminateSolution, is uniformly mixed 1～2min and obtains forerunner's mixed solution;
(3) fiber needled felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, obtainsThe compound wet gel of sial that fiber needled felt strengthens, at room temperature aging 12h;
(4) carry out solvent exchange, it is molten that the compound wet gel of sial that the fiber needled felt that step (3) is obtained strengthens immerses ethanolLiquid, through insulation, solvent exchange, modification, obtains fiber needled felt after being dried and strengthens silicon-aluminium aerogel warming plate.
4. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe 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, the ratio that is 2:1～1:1 in the solid-to-liquid ratio of flyash and sulfuric acid by flyash withConcentration is 80%～98% sulfuric acid mixing, reaction 4～6h;
4) Separation of Solid and Liquid: reactant is cooled to after room temperature, is that 1:2～1:6 preparation adds water by the solid-to-liquid ratio of flyash and water,At 75～95 DEG C, stir after 1～3h, suction filtration, the water washing that it is 2:1～1:2 that filter cake is used by the solid-to-liquid ratio of flyash and water,Obtain solution and the high silicon acid leaching residue of ferric sulfate and aluminum sulfate;
5) acid leaching residue is prepared waterglass: the ratio that is 1:1～1:2 by solid-to-liquid ratio by acid leaching residue and 9%～12% soda lyeExample preparation mixed liquor heats after 6～10h at 160～200 DEG C in reactor, is cooled to room temperature, filters and wash with water solidSlag.
5. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe characterised in that, the light transmittance of the compound wet gel of described sial is more than 80%.
6. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe characterised in that the composite fibre Nomex that described fiber needled felt is made up of glass fibre and polypropylene fibre, described glassThe mass content of fiber is 50～70%; The diameter of described glass fibre is 5～10um, and the diameter of described polypropylene fibre is10～15um。
7. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe characterised in that, described solvent exchange adopts ethanol, hexane equal solvent, and described holding temperature is 50～70 DEG C, described solvent is putThe time of changing is more than 8h.
8. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe characterised in that, the raw material of described modification adopts siloxy group modification 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 fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3, itsBe characterised in that, the thermal conductivity factor that described fiber needled felt strengthens silicon-aluminium aerogel warming plate is 0.015～0.022W/ (mK),Density is 220～450kg/m3, water absorption rate is less than 3%.
10. the supercritical drying drying method of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 3,It is characterized in that, it is the fire prevention of A level that described fiber needled felt strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
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| CN111148721A (en) * | 2017-11-13 | 2020-05-12 | 株式会社Lg化学 | Method for recovering supercritical waste liquid generated in process of producing silica aerogel felt |
| CN111517747A (en) * | 2020-04-21 | 2020-08-11 | 浙江岩谷科技有限公司 | Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material |
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