CN105753439A - Fiber punched felt/sliicon-alumininm aerogel composite insulation board - Google Patents

Fiber punched felt/sliicon-alumininm aerogel composite insulation board Download PDF

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Publication number
CN105753439A
CN105753439A CN201610067212.0A CN201610067212A CN105753439A CN 105753439 A CN105753439 A CN 105753439A CN 201610067212 A CN201610067212 A CN 201610067212A CN 105753439 A CN105753439 A CN 105753439A
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China
Prior art keywords
needled felt
silicon
fiber needled
composite insulation
aerogel composite
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CN201610067212.0A
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Chinese (zh)
Inventor
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 CN201610067212.0A priority Critical patent/CN105753439A/en
Publication of CN105753439A publication Critical patent/CN105753439A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00Compositions for artificial stone, not containing binders
    • C04B30/02Compositions for artificial stone, not containing binders containing fibrous materials
    • 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

Abstract

The invention provides a fiber punched felt/sliicon-alumininm aerogel composite insulation board, which is prepared from the following raw materials: sodium metaaluminate, sodium silicate and fiber punched felt, wherein the mass ratio of the sodium metaaluminate to the sodium silicate is 1:4 to 1:40; the mass percent of water solution of the sodium metaaluminate is more than 5 percent; the solid content after the sodium silicate is diluted is more than 5 percent. According to the fiber punched felt/sliicon-alumininm aerogel composite insulation board provided by the invention, the production raw materials are cheap; the gel processing is characterized by carrying out gel reaction after blending two materials, so that the complex processes of other aerogel sol-gel are avoided; the obtained product integrality and the mechanical property can be remarkably improved; a whole preparation method is simple and easy to implement, has no strong acid and strong base corrosion, is low in equipment requirement, and suitable for industrial production after process scale-up.

Description

A kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards
Technical field
The present invention relates to a kind of warming plate, concrete one relates to fiber needled felt/silicon-aluminium aerogel composite insulation boards.
Background technology
Aeroge is the material that in solid matter, heat conductivity is minimum, is only slightly higher than vacuum, is approximately 0.013W/m K.Aeroge also has extremely low density, is the minimum solid of the density generally acknowledged in the world, and least density can accomplish 3kg/m3, more slightly higher than the density of air.Therefore aeroge is the insulation material that heat insulation effect is best in the world, density is minimum.
The kind of current aeroge is more, has carbon aerogels, silicon system aeroge, alumina aerogels etc..The preparing raw material and can adopt tetraethyl orthosilicate or waterglass of silica aerogel, preparation technology can be respectively adopted non-pressure process and supercritical, and its preparation technology is highly developed.The preparation of alumina aerogels, mainly alkoxide process, drying process adopts supercritical process substantially.And the preparation of silica/alumina composite aerogel, rarely having report, even if being prepared into pluralgel, being also adopt alkoxide process to carry out gel.
Inorganic salt method prepares the method for sial composite aerogel, rarely has report, and at present major part aeroge composition is one pack system, for instance silica aerogel is mainly silicon dioxide, aluminum aeroge be mainly composed of aluminium oxide.The raw material of silica aerogel has two kinds, and one is tetraethyl orthosilicate, and one is waterglass, and two kinds of raw materials have different sol gel processings.The raw material major part that alumina aerogels adopts is aluminium-alcohol salt, adopts supercritical process.Therefore, the raw material production cost that tradition prepares alumina aerogels is expensive, and gel process is complicated;If what traditional alumina aerogels preparation adopted is tetraethyl orthosilicate, sol-gel process is also intended to the hydrolysis through raw material and polycondensation, and preparation technology is more complicated.
Inorganic salt method, is adopt two kinds of inorganic salts, according to certain processing compound, as long as according to certain dispensing order, it is possible to easily preparation quality and the good gel of condition.Production process is simple, and former material is cheap, has the prospect that Large scale processes is applied.
Summary of the invention
Simple in order to obtain preparation technology, the composite aerogel that cost is low, it is good and have the fiber needled felt/silicon-aluminium aerogel composite insulation boards of some strength that the present invention proposes globality.
In order to achieve the above object, the invention provides employing following technical proposals:
A kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, raw material includes sodium metaaluminate, waterglass and fiber needled felt, the mass ratio of described sodium metaaluminate and waterglass is 1:4~1:40, the mass percent of the aqueous solution of described sodium metaaluminate is more than 5%, and the solid content after the dilution of described waterglass is more than 5%
A kind of first preferred version of fiber needled felt/silicon-aluminium aerogel composite insulation boards, a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards of preparation comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1~2min obtains forerunner's mixed solution;
(3) fiber needled felt is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the fiber needled felt obtained strengthens, at room temperature aging 12h;
(4) carrying out solvent displacement, the sial compound wet gel that fiber needled felt step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains fiber needled felt after drying and strengthens silicon-aluminium aerogel warming plate.
A kind of second preferred version of fiber needled felt/silicon-aluminium aerogel composite insulation boards, the preparation method of waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) mechanical grinding;
3) acidleach: at 150 DEG C~220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%~98% with the ratio that solid-to-liquid ratio is 2:1~1:1 of sulphuric acid in flyash, reacts 4~6h;
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2~1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75~95 DEG C, after stirring 1~3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1~1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%~12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1~1:2, heat after 6~10h in reactor at 160~200 DEG C, be cooled to room temperature, filter and wash solid slag with water.
3rd preferred version of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, the light transmittance of sial compound wet gel is more than 80%.
A kind of 4th preferred version of fiber needled felt/silicon-aluminium aerogel composite insulation boards, the composite fibre Nomex that fiber needled felt is made up of glass fibre and polypropylene fibre, heated cure under pressure and get final product;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.
5th preferred version of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, solvent displacement adopts ethanol, and hexane equal solvent, described holding temperature is 50~70 DEG C, and described solvent time swap is more than 8 hours.
6th preferred version of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, modified raw material adopts siloxanyl modified liquid, and modification temperature is 50~70 DEG C, and modification time is 7~9h.
A kind of 7th preferred version of fiber needled felt/silicon-aluminium aerogel composite insulation boards, dry employing constant pressure and dry technique.
8th preferred version of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, it is 0.015~0.022W/ (m K) that fiber needled felt strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220~450kg/m3, water absorption rate is less than 3%.
9th preferred version of a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards, it is the fire prevention of A level that fiber needled felt strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C.
Compared with immediate prior art, technical scheme provided by the invention has following excellent effect:
1. the invention provides a kind of simple process using two kinds of alkaline, inorganic salts to prepare fiber needled felt enhancing sial composite aerogel;
2. the raw material of the present invention is sodium metaaluminate, waterglass and fiber needled felt, and raw materials for production are cheap;
3. the gel process of the present invention be carry out mixture by two kinds of materials after, carry out gel reaction, it is to avoid the complicated technology of other aeroge collosol and gel;
4. integrity and the mechanical property of the fiber needled felt enhancing sial composite aerogel that the present invention obtains all are significantly increased;
5. whole preparation method is simple and easy to control, corrodes without strong acid and strong base, low for equipment requirements, after technique is amplified, is suitable for industrialized production.
Detailed description of the invention
It is described in further detail below in conjunction with specific embodiment, technical scheme is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Inorganic salt method prepares the process of sial composite aerogel:
First configuring the sodium aluminate solution of certain mass concentration, stirring, until sodium metaaluminate complete hydrolysis;Then, by the requirement of waterglass dilution technique proportioning;When stirring, in the water glass solution after diluted, add the sodium aluminate solution of required amount, after continuing stirring 1~2min, it is ensured that when solution mix homogeneously, stop stirring, stand 5~30min, obtain forerunner's mixed solution.
Fiber needled felt is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the fiber needled felt obtained strengthens, at room temperature aging 12h;Then, carry out solvent displacement, the sial compound wet gel that the fiber needled felt obtained strengthens is immersed alcoholic solution.After solvent has been replaced, adopting siloxanyl modified liquid to be modified, modification temperature is 50~70 DEG C, and modification time is 7~9h.Finally, carry out normal pressure and dry dry, the sial composite aerogel granule that felt strengthens must be stung.
The sodium aluminate solution of configuration, it is necessary to all dissolve, it is not possible to have impurity, solution requires transparent limpid, and sodium aluminate solution requires matching while using, can not long storage time;Waterglass is in the process of dilution, after adding a certain amount of deionized water, and more than magnetic agitation 5min, it is ensured that dilute solution mix homogeneously.
The preparation of waterglass: flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 4min, then with 82% sulphuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C react 4h;Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 90 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 1:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 10.5%, and put into autoclave heat 10h, reaction temperature 180 DEG C;After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass.
The preparation of fiber needled felt: composite fibre glass fibre and polypropylene fibre formed introduces two rollers of filament throwing roller through guide eyelit, by the extruding mutually of two filament throwing rollers and rotation, multiple yarns is carried out top-down acupuncture with certain speed by the needle plate first passing through a rectangle subsequently, then with certain speed, multiple yarns is carried out acupuncture from bottom to top then through another rectangle needle plate, namely obtain fiber needled felt then through pressure roller.
Properties of product test different technical parameters prepared, is shown in following table.
Technological parameter in each embodiment of table 1 and performance
Above example is only limited in order to technical scheme to be described; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention.

Claims (10)

1. fiber needled felt/silicon-aluminium aerogel composite insulation boards, it is characterized in that, raw material contains sodium metaaluminate, waterglass and fiber needled felt, the mass ratio of described sodium metaaluminate and waterglass is 1:4~1:40, the mass percent of the aqueous solution of described sodium metaaluminate is more than 5%, and the solid content after the dilution of described waterglass is more than 5%.
2. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 1, it is characterised in that the preparation of described fiber needled felt/silicon-aluminium aerogel comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1~2min obtains forerunner's mixed solution;
(3) fiber needled felt is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the fiber needled felt obtained strengthens, at room temperature aging 12h;
(4) carrying out solvent displacement, the sial compound wet gel that fiber needled felt step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains fiber needled felt after drying and strengthens silicon-aluminium aerogel warming plate.
3. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the preparation method of described waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) mechanical grinding;
3) acidleach: at 150 DEG C~220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%~98% with the ratio that solid-to-liquid ratio is 2:1~1:1 of sulphuric acid in flyash, reacts 4~6h;
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2~1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75~95 DEG C, after stirring 1~3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1~1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%~12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1~1:2, heat after 6~10h in reactor at 160~200 DEG C, be cooled to room temperature, filter and wash solid slag with water.
4. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the light transmittance of described sial compound wet gel is more than 80%.
5. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the composite fibre Nomex that described fiber needled felt is made up of glass fibre and polypropylene fibre, heated cure under pressure and get final product;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.
6. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the displacement of described solvent adopts ethanol, and hexane equal solvent, described holding temperature is 50~70 DEG C, and described solvent time swap is more than 8h.
7. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that described modified raw material adopts siloxanyl modified liquid, and modification temperature is 50~70 DEG C, and modification time is 7~9h.
8. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that described dry employing constant pressure and dry technique.
9. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterized in that, it is 0.015~0.022W/ (m K) that described fiber needled felt strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220~450kg/m3, water absorption rate is less than 3%.
10. a kind of fiber needled felt/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised 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.
CN201610067212.0A 2016-01-29 2016-01-29 Fiber punched felt/sliicon-alumininm aerogel composite insulation board Pending CN105753439A (en)

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Application Number Priority Date Filing Date Title
CN201610067212.0A CN105753439A (en) 2016-01-29 2016-01-29 Fiber punched felt/sliicon-alumininm aerogel composite insulation board

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562753A (en) * 2004-03-25 2005-01-12 浙江大学 Method for preparing alumina in fire resistant and high specific surface
CN1629381A (en) * 2004-08-10 2005-06-22 泰山玻璃纤维股份有限公司 Process for making composite fabric needle felt
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
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
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
US20120025127A1 (en) * 2009-06-11 2012-02-02 Korea Institute Of Energy Research Aerogel Mat and Manufacturing Method Thereof
CN103396086A (en) * 2013-08-08 2013-11-20 厦门大学 Preparation method for glass fiber-reinforced water glass-based silica composite aerogel

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562753A (en) * 2004-03-25 2005-01-12 浙江大学 Method for preparing alumina in fire resistant and high specific surface
CN1629381A (en) * 2004-08-10 2005-06-22 泰山玻璃纤维股份有限公司 Process for making composite fabric needle felt
US20120025127A1 (en) * 2009-06-11 2012-02-02 Korea Institute Of Energy Research Aerogel Mat and Manufacturing Method Thereof
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
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
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
CN103396086A (en) * 2013-08-08 2013-11-20 厦门大学 Preparation method for glass fiber-reinforced water glass-based silica composite aerogel

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Application publication date: 20160713