CN105597634A - Supercritical drying method for glass wool/silicon-aluminum aerogel composite heat preservation plate - Google Patents
Supercritical drying method for glass wool/silicon-aluminum aerogel composite heat preservation plate Download PDFInfo
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- CN105597634A CN105597634A CN201610065778.XA CN201610065778A CN105597634A CN 105597634 A CN105597634 A CN 105597634A CN 201610065778 A CN201610065778 A CN 201610065778A CN 105597634 A CN105597634 A CN 105597634A
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- mineral wool
- drying method
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- 239000004964 aerogel Substances 0.000 title claims abstract description 41
- 238000000352 supercritical drying Methods 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 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
- 239000011491 glass wool Substances 0.000 title abstract 3
- 238000004321 preservation Methods 0.000 title abstract 2
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000012986 modification Methods 0.000 claims abstract description 19
- 230000004048 modification Effects 0.000 claims abstract description 19
- 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 14
- 239000011240 wet gel Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000011490 mineral wool Substances 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 31
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- 239000004411 aluminium Substances 0.000 claims description 27
- 238000009413 insulation Methods 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 235000019353 potassium silicate Nutrition 0.000 claims description 12
- 239000002994 raw material Substances 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
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000499 gel Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000011521 glass 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
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 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
- 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 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
- 238000010521 absorption reaction Methods 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
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000006063 cullet Substances 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
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 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
- 229910000514 dolomite Inorganic materials 0.000 claims description 2
- 239000010459 dolomite Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral 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
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 claims description 2
- 238000005728 strengthening Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 230000003176 fibrotic effect Effects 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 210000002268 wool Anatomy 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 3
- 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
- 230000002209 hydrophobic effect Effects 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000007872 degassing Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 238000009776 industrial production 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
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 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
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003365 glass fiber Substances 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
- 150000004703 alkoxides Chemical class 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
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000009795 fibrotic process Effects 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
- -1 Acetonitrile Ethanol Carbon dioxide Ethanol Chemical compound 0.000 description 1
- 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
- 238000001816 cooling Methods 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
- 238000006073 displacement reaction 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
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 235000010755 mineral Nutrition 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
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000026676 system process Effects 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
-
- 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)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Microbiology (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Thermal Insulation (AREA)
Abstract
The invention provides a supercritical drying method for a glass wool/silicon-aluminum aerogel composite heat preservation plate. The supercritical drying method comprises the following steps: firstly, performing solvent replacement and hydrophobic modification on glass wool/silicon-aluminum aerogel, then putting wet gel subjected to hydrophobic modification into a high-pressure reaction kettle, pouring into a supercritical medium, setting heating temperature for heating, and performing degassing or backflow to bring out a solvent in the wet gel after the medium in the reaction kettle is supercritical until the solvent is completely recycled, wherein the supercritical medium is an acetonitrile, ethyl alcohol or carbon dioxide solvent. A product produced by the supercritical drying method provided by the invention is high in product yield and high in production efficiency, is slight in powder falling, and can realize industrial amplification; the supercritical drying method can be integrated to an assembly line; the whole preparation method is simple and easy to understand; no strong acid and strong alkali corrosion exists, and the requirement on equipment is low; and after being amplified, the method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of drying means of warming plate, be specifically related to a kind of super facing of mineral wool/silicon-aluminium aerogel composite insulation boardsBoundary's drying means.
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, compare 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 mineral wool/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 mineral wool/silicon-aluminium aerogel composite insulation boards, is first undertaken molten by mineral wool/sial wet gelAgent displacement and hydrophobically modified, then put into autoclave by the good wet gel of hydrophobically modified, pours supercritical medium into, setsHeating-up temperature, heats, the medium state of reactor reach overcritical after, exit or reflux, in wet gelSolvent take 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 mineral wool/silicon-aluminium aerogel composite insulation boards, supercritical drying drying methodSetting heating-up temperature 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 mineral wool/silicon-aluminium aerogel composite insulation boards, prepares mineral wool/sialAeroge 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) mineral wool is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the glass obtainingThe cotton compound wet gel of sial strengthening, at room temperature aging 12h;
(4) carry out solvent exchange, the compound wet gel of sial that the mineral wool that step (3) is obtained strengthens immerses ethanolic solution,Through insulation, solvent exchange, modification, obtains mineral wool after being dried and strengthens silicon-aluminium aerogel warming plate.
The 3rd preferred version of the supercritical drying drying method of mineral wool/silicon-aluminium aerogel composite insulation boards, the preparation side of waterglassMethod 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 mineral wool/silicon-aluminium aerogel composite insulation boards, the compound wet gel of sialLight transmittance more than 80%.
The 5th preferred version of the supercritical drying drying method of mineral wool/silicon-aluminium aerogel composite insulation boards, mineral wool is by white cloudsAfter stone, boron magnesium ore deposit, calcium oxide and cullet mix, after molten system and fibrotic processes, make; The fiber of described mineral woolDiameter is 3～4 μ m, and the mass content in the silicon-aluminium aerogel that described mineral wool strengthens at described mineral wool is 50～70%.
The 6th preferred version of the supercritical drying drying method of mineral wool/silicon-aluminium aerogel composite insulation boards, solvent exchange adopts secondAlcohol, 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 mineral wool/silicon-aluminium aerogel composite insulation boards, the raw material of modification adoptsSiloxy group modification liquid, modification temperature is 50～70 DEG C, modification time is 7～9h.
The 8th preferred version of the supercritical drying drying method of mineral wool/silicon-aluminium aerogel composite insulation boards, mineral wool strengthens sialThe thermal conductivity factor of aeroge warming plate is 0.015～0.022W/ (mK), and density is 220～450kg/m3, water absorption rate is less than3％。
The 9th preferred version of the supercritical drying drying method of mineral wool/silicon-aluminium aerogel composite insulation boards, mineral wool strengthens sialAeroge 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 a kind of supercritical drying that uses two kinds of alkaline, inorganic salts to prepare mineral wool enhancing sial composite aerogelThe simple process of method;
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 mineral wool, 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.
Mineral wool is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the mineral wool obtaining increasesThe compound wet gel of strong sial, at room temperature aging 12h; Then, carry out solvent exchange, the silicon that the mineral wool obtaining is strengthenedThe compound wet gel of aluminium immerses ethanolic solution. After solvent exchange completes, adopt siloxy group modification liquid to carry out modification, modification temperatureBe 50～70 DEG C, modification time is 7～9h. Finally, carry out normal pressure bake drying, must sting the sial composite aerogel that felt strengthensParticle.
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 mineral wool:
Prepare raw material: in quality %, by 3% dolomite, 20% boron magnesium ore deposit, 5% calcium oxide and 80% cullet carry outMix;
Founding of raw material: by above-mentioned raw materials melting, successively through persilicate formation stages, glass formation stages, glass metal clarificationStage, glass metal homogenizing stage and glass metal cooling stage, obtain pretreatment glass metal;
Fibrotic processes: make pretreatment glass metal flow into the centrifuge of High Rotation Speed, form glass fibre, then at high-speed and high-temperatureGas-flow effect under make described glass fibre through heating, stretch after obtain soft and thin glass fibre.
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 mineral wool/silicon-aluminium aerogel composite insulation boards, is characterized in that, by solvent exchange and thinMineral wool/sial wet gel of water modification is put into autoclave, pours supercritical medium into, sets heating-up temperature heating, reactionThe medium state of still reach overcritical after, exit or reflux; Described supercritical medium is acetonitrile, ethanol or titanium dioxideCarbon solvent.
2. the supercritical drying drying method of a kind of mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 1, its featureBe, 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, and pressure is high by 0.5～2MPa。
3. the supercritical drying drying method of a kind of mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 1, its featureBe, the preparation of described mineral wool/silicon-aluminium aerogel 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) mineral wool is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the glass obtainingThe cotton compound wet gel of sial strengthening, at room temperature aging 12h;
(4) carry out solvent exchange, the compound wet gel of sial that the mineral wool that step (3) is obtained strengthens immerses ethanolic solution,Through insulation, solvent exchange, modification, obtains mineral wool after being dried and strengthens silicon-aluminium aerogel warming plate.
4. the supercritical drying drying method of a kind of mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, 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 mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, 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 mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, described mineral wool is after being mixed by dolomite, boron magnesium ore deposit, calcium oxide and cullet, through molten system and fibrotic processesAfter make; The fibre diameter of described mineral wool is 3～4 μ m, in the silicon-aluminium aerogel that described mineral wool strengthens at described mineral woolMass content is 50～70%.
7. the supercritical drying drying method of a kind of mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, described solvent exchange adopts ethanol, hexane equal solvent, and described holding temperature is 50～70 DEG C, when described solvent exchangeBetween be more than 8h.
8. the supercritical drying drying method of a kind of mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, 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 mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its featureBe, the thermal conductivity factor that described mineral wool 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 mineral wool/silicon-aluminium aerogel composite insulation boards according to claim 3, its spyLevy and be, it is the fire prevention of A level that described mineral wool strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
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