CN105597635A - Normal-pressure drying method of felt/silicon-aluminum aerogel composite heat-preservation board - Google Patents

Normal-pressure drying method of felt/silicon-aluminum aerogel composite heat-preservation board Download PDF

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Publication number
CN105597635A
CN105597635A CN201610067650.7A CN201610067650A CN105597635A CN 105597635 A CN105597635 A CN 105597635A CN 201610067650 A CN201610067650 A CN 201610067650A CN 105597635 A CN105597635 A CN 105597635A
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felt
silicon
constant pressure
aerogel composite
aluminium aerogel
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杨卓舒
纪勇
孟宪娴
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Zhuoda New Material Technology Group Co Ltd
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Zhuoda New Material Technology Group Co Ltd
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Priority to CN201610067650.7A priority Critical patent/CN105597635A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091Preparation of aerogels, e.g. xerogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/32Alkali metal silicates
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00Drying solid materials or objects by processes involving the application of heat

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention provides a normal-pressure drying method of a felt/silicon-aluminum aerogel composite heat-preservation board. The normal-pressure drying method comprises the following steps: carrying out solvent displacement and hydrophobic modification on felt/silicon-aluminum wet gel; then, carrying out normal-pressure drying on the wet gel which is subjected to hydrophobic modification at a low temperature of 80-120 DEG C; and drying at a high temperature of 300-400 DEG C for 40 minutes. The felt/silicon-aluminum aerogel composite heat-preservation board produced by the normal-pressure drying method provided by the invention has the advantages of high quality rate, high production efficiency and slight powdering and can be industrially amplified; the normal-pressure drying method can be integrated to a production line, is simple and easy to control in the whole, has no strong acid corrosion or strong alkali corrosion, and has low requirements on equipment; and after being amplified, the method is suitable for industrial production.

Description

A kind of constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards
Technical field
The present invention relates to a kind of drying means of warming plate, the normal pressure that is specifically related to a kind of felt/silicon-aluminium aerogel composite insulation boards is dryDrying 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, 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 constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards.
In order to achieve the above object, the invention provides employing following technical proposals:
A constant pressure and dry method for felt/silicon-aluminium aerogel composite insulation boards, first carries out solvent exchange by felt/sial wet gelAnd hydrophobically modified, then wet gel good hydrophobically modified is carried out to constant pressure and dry at 80~120 DEG C of low temperature, then at high temperatureAt 300~400 DEG C, be dried 40 minutes.
First preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, prepares felt/silicon-aluminium aerogelComprise 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) felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the felt obtaining increasesThe compound wet gel of strong sial, at room temperature aging 12h;
(4) carry out solvent exchange, the compound wet gel of sial that the felt that step (3) is obtained strengthens immerses ethanolic solution, warpCross insulation, solvent exchange, modification, obtains felt after being dried and strengthens silicon-aluminium aerogel warming plate.
Second preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, the preparation method of waterglass asUnder:
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 3rd preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, the compound wet gel of sial thoroughlyLight rate is more than 80%.
The 4th preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, the preparation method of felt asUnder: wool fiber mixes; By sending into blending box through the wool fiber weighing and fully mixing, remove unnecessary composition residualStay, then wool fiber is passed through to opener combing and sends into cotton storage tank by wind-force; By the wool fiber process roller in cotton storage tankFormula carding machine is processed as the thin net of ultimate fibre composition; Plane formula lapping machine laying is crossed to by thin Netcom and become fleece; Fleece passes through pinThorn machined is fixed; Fleece, through the surface calendering of three-roller type calender, makes even thickness consistent.
The 5th preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, solvent exchange adopts ethanol,Hexane equal solvent, described holding temperature is 50~70 DEG C, the described solvent exchange time is more than 8 hours.
The 6th preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, the raw material of modification adopts silicaAlkyl-modified liquid, modification temperature is 50~70 DEG C, modification time is 7~9h.
The 7th preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, felt strengthens silicon-aluminium aerogelThe thermal conductivity factor of warming plate is 0.015~0.022W/ (mK), and density is 220~450kg/m3, water absorption rate is less than 3%.
The 8th preferred version of the constant pressure and dry method of felt/silicon-aluminium aerogel composite insulation boards, felt strengthens silicon-aluminium aerogelWarming 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 side that uses two kinds of alkaline, inorganic salts to prepare felt 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 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.
Felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the felt obtaining strengthensThe compound wet gel of sial, at room temperature aging 12h; Then, carry out solvent exchange, the sial that the felt obtaining is strengthened is compoundWet gel immerses ethanolic solution. After solvent exchange completes, adopt siloxy group modification liquid to carry out modification, modification temperature is50~70 DEG C, modification time is 7~9h. Finally, wet gel good hydrophobically modified is carried out to constant pressure and dry at 80~120 DEG C of low temperature,At 300~400 DEG C of high temperature dry 40 minutes again, must sting the sial composite aerogel particle of felt enhancing.
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.
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 felt:
A. select suitable wool fiber to mix;
B. by sending into blending box through the wool fiber weighing and fully mixing, remove unnecessary composition residual, then by wool fiberProcess opener combing is also sent into cotton storage tank by wind-force;
C. the wool fiber in cotton storage tank is processed as to the thin net of ultimate fibre composition through roller and clearer card;
D. thin Netcom is crossed to plane formula lapping machine laying and become fleece;
E. fleece is processed fixing by needing machine;
F. fleece, through the surface calendering of three-roller type calender, makes even thickness consistent.
The procedure of processing of step c middle roller formula carding machine is:
1) divide the compound of combing wool fiber, make it to become ultimate fibre;
2) make in the compound of wool fiber various fibers under ultimate fibre state fully, evenly mix;
3) removal of contamination, makes that ultimate fibre is parallel to be stretched;
4) ultimate fibre is processed into thin net.
Technological parameter and performance in the each embodiment of table 1
Embodiment 1 2 3 4
Low temperature drying temperature/DEG C 80 120 90 100
High temperature drying temperature/DEG C 400 300 330 360
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 (9)

1. a constant pressure and dry method for felt/silicon-aluminium aerogel composite insulation boards, is characterized in that, by solvent exchange and hydrophobic changingProperty good felt/sial wet gel at 80~120 DEG C of low temperature, carry out constant pressure and dry, then at 300~400 DEG C of high temperature dry 40 pointsClock.
2. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 1, is characterized in that,The preparation of described felt/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) felt is immersed to forerunner's mixed solution completely, adsorb fullly, leave standstill 30min, automatically gel, the felt obtaining increasesThe compound wet gel of strong sial, at room temperature aging 12h;
(4) carry out solvent exchange, the compound wet gel of sial that the felt that step (3) is obtained strengthens immerses ethanolic solution, warpCross insulation, solvent exchange, modification, obtains felt after being dried and strengthens silicon-aluminium aerogel warming plate.
3. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized 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.
4. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized in that,The light transmittance of the compound wet gel of described sial is more than 80%.
5. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized in that,The preparation method of described felt is as follows: wool fiber mixes; Blending box fully mixed will be sent into through the wool fiber weighingClose, remove unnecessary composition residual, then wool fiber is passed through to opener combing and sends into cotton storage tank by wind-force; By cotton storage tankIn wool fiber be processed as the thin net of ultimate fibre composition through roller and clearer card; Plane formula lapping machine laying is crossed to by thin NetcomFleece; Fleece is processed fixing by needing machine; Fleece, through the surface calendering of three-roller type calender, makes even thickness consistent.
6. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized in that,Described solvent exchange adopts ethanol, hexane equal solvent, and described holding temperature is 50~70 DEG C, the described solvent exchange time is 8hAbove.
7. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized 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.
8. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized in that,The thermal conductivity factor that described 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%.
9. the constant pressure and dry method of a kind of felt/silicon-aluminium aerogel composite insulation boards according to claim 2, is characterized in that,It is the fire prevention of A level that described felt strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
CN201610067650.7A 2016-01-29 2016-01-29 Normal-pressure drying method of felt/silicon-aluminum aerogel composite heat-preservation board Pending CN105597635A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113165978A (en) * 2019-09-03 2021-07-23 株式会社Lg化学 Aerogel felt
US12053753B2 (en) 2019-09-03 2024-08-06 Lg Chem, Ltd. Apparatus and method for preparing aerogel blanket
US12090460B2 (en) 2019-09-03 2024-09-17 Lg Chem, Ltd. Method for producing aerogel blanket
US12139410B2 (en) 2019-09-03 2024-11-12 Lg Chem, Ltd. Aerogel blanket

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CN101717214A (en) * 2009-11-26 2010-06-02 西南科技大学 Method for preparing silicon-aluminum aerogel by using fly ash as raw material through normal pressure drying
CN101962876A (en) * 2010-09-25 2011-02-02 李国华 Process for manufacturing needled wool felt
CN101993087A (en) * 2010-11-29 2011-03-30 中煤平朔煤业有限责任公司 Method for preparing water glass by using fly ash
WO2015016730A2 (en) * 2013-08-02 2015-02-05 Active Aerogels, Unipessoal, Lda. Method for production of flexible panels of hydrophobic aerogel reinforced with fibre felts

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Publication number Priority date Publication date Assignee Title
CN101318659A (en) * 2008-07-04 2008-12-10 绍兴纳诺气凝胶新材料研发中心有限公司 Method for preparing silicon dioxide silica aerogel composite material by drying in atmosphere pressure
CN101698592A (en) * 2009-11-13 2010-04-28 航天特种材料及工艺技术研究所 Silicon-aluminium aerogel composite material and manufacturing method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113165978A (en) * 2019-09-03 2021-07-23 株式会社Lg化学 Aerogel felt
US12053753B2 (en) 2019-09-03 2024-08-06 Lg Chem, Ltd. Apparatus and method for preparing aerogel blanket
US12090460B2 (en) 2019-09-03 2024-09-17 Lg Chem, Ltd. Method for producing aerogel blanket
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US12186721B2 (en) 2019-09-03 2025-01-07 Lg Chem, Ltd. Aerogel blanket and method for manufacturing same

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Application publication date: 20160525