CN104494225B - Silica aerogel combined rigidity thermal insulation tile and preparation method thereof can be processed - Google Patents
Silica aerogel combined rigidity thermal insulation tile and preparation method thereof can be processed Download PDFInfo
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- CN104494225B CN104494225B CN201410783684.7A CN201410783684A CN104494225B CN 104494225 B CN104494225 B CN 104494225B CN 201410783684 A CN201410783684 A CN 201410783684A CN 104494225 B CN104494225 B CN 104494225B
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- thermal insulation
- insulation tile
- silica aerogel
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- gel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B13/00—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material
- B32B13/02—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material with fibres or particles being present as additives in the layer
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- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/42—Glass
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- 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
Abstract
The present invention relates to a kind of preparation method for processing silica aerogel combined rigidity thermal insulation tile, carries out hydrophobic dried process after silica sol is compound with rigid thermal insulation tile；Its composition is：Rigid thermal insulation tile is quartz fibre rigidity thermal insulation tile, and density is 0.12 0.35g/cm3；Silica sol dispensing mole ratio is：Tetraethyl orthosilicate：Ethanol：Deionized water：Catalyst=1：2‑10：2‑12：0‑0.01.The present invention prepares silica aerogel composite heat-insulating tile material, and porosity is high, and aperture is little, has good iris action to solid heat transfer and air heat transfer and convection current；The preparation method of the present invention is scientific and reasonable, simple, convenient to carry out, and that made can be processed into flat board, cover body and other complicated abnormal shape parts from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile.
Description
Technical field
The present invention relates to one kind can process silica aerogel combined rigidity thermal insulation tile and preparation method thereof, belong to heat-insulated material
Material technical field.
Background technology
With the development of Aero-Space cause, requirement of the aircraft to heat-barrier material is more and more harsher, such as repeatable
Using the heat-insulated field of the middle temperature of the thermal protection system of vehicle, traditional thermal insulation tile thermal conductivity factor is higher, insulation system thicker and
Increase the demand that weight etc. can not meet practical application.Therefore exploitation aerogel heat-proof composite material has become at present and has developed efficiently
The dominant direction of heat-barrier material.Aeroge is due to three-dimensional nanoparticles skeleton, high-specific surface area, nanoscale hole hole, low close
The special microstructures such as degree, can effectively suppress the gentle body convection heat transfer' heat-transfer by convection of solid-state heat transfer, with excellent insulative properties, be mesh
The minimum solid-state material of front generally acknowledged thermal conductivity.It is supercritical drying to prepare the maximally effective drying means of aeroge at present, but by
In supercritical drying equipment more expensive, there is potential safety hazard and be not easy to, therefore, normal pressure prepares aeroge
Combined rigidity thermal insulation tile becomes a up-and-coming method；Rigid thermal insulation tile is due to high porosity, therefore existing
Easily absorb water in the middle of the process of storage, the heat-insulated and dielectric properties of meeting large effect thermal insulation tile after water suction, but also can increase
The unfavorable factors such as the weight of thermal insulation tile, therefore, it is to solve heat-barrier material field to stablize nonhygroscopic thermal insulation tile under preparation room temperature
Key problem in technology.
Content of the invention
It is an object of the invention to provide one kind can process silica aerogel combined rigidity thermal insulation tile, with shaping fast,
Density is low, effectively insulating, machinable feature；Invention also provides its preparation method, preparation method is simple, it is easy to grasp
Make.
One kind of the present invention can be processed from Hydrophobic silica aeroge combined rigidity thermal insulation tile, silica sol with firm
Property thermal insulation tile compound after carry out hydrophobic dried process；Its composition is：Rigid thermal insulation tile is quartz fibre rigidity thermal insulation tile, close
Spend for 0.12-0.35g/cm3；Silica sol dispensing mole ratio is：Tetraethyl orthosilicate：Ethanol：Deionized water：Catalyst=
1：2-10：2-12：0-0.01.
Silica sol dispensing mole ratio is preferably：Tetraethyl orthosilicate：Ethanol：Deionized water：Catalyst=1：2-6：
4-10：0.005-0.01.
The preparation method of silica aerogel combined rigidity thermal insulation tile can be processed, is comprised the steps：
(1) silica sol：Measure ethanol first, add tetraethyl orthosilicate and deionized water while stirring, mix
Afterwards, add catalyst to continue stirring, obtain silica sol；
(2) it is combined：Rigid thermal insulation tile is de-gassed process, and the silica for then step (1) being prepared by negative pressure is molten
Partly or entirely being filled into inside rigid thermal insulation tile for glue, is allowed to be combined with rigid thermal insulation tile；
(3) gel-aging：The thermal insulation tile silica sol composite of step (2) is added catalyst quiet at 50 DEG C
Gel is formed after putting 1-8 hour, alcohol solvent is subsequently adding, so that the material after gel is completely immersed in alcohol solvent, carry out old
Change is processed, and ageing time is 18-72 hour；
(4) hydrophobic treatment：To in gel of the step (3) after aging, add the hexane solution of trim,ethylchlorosilane to carry out instead
Should, the time be 1-3 days, then gel is carried out with hexane solution, until cleaning fluid control pH=6.5-7.5 it
Between；
(5) constant pressure and dry：Rigid thermal insulation tile is taken out from gel and is dried；
(6) process：Aeroge combined rigidity thermal insulation tile after step (5) constant pressure and dry is can be prepared by certainly after processing
Hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile.
Gel of the hydrophobic treatment for step (3) after aging is reacted with the hexane solution of trim,ethylchlorosilane, is occurred
Hydrophobic effect, reaches the effect of hydrophobic treatment.
Catalyst described in step (1) is acidity.
Catalyst described in step (1) is hydrochloric acid or nitric acid.
Catalyst described in step (3) is alkalescence.
Catalyst described in step (3) is ammoniacal liquor.
Water-repelling agent described in step (4) is trim,ethylchlorosilane.
Dry run is to dry 18-24 hour under room temperature, dries 24 hours at 50 DEG C, 70 DEG C of dryings 24 hours.
Machining center described in step (6) is four-shaft numerically controlled machining center.
Detailed process is as follows：
The ethanol of measured amounts first, adds tetraethyl orthosilicate and water while stirring, after mixing, adds catalyst
Continue stirring, obtain silica sol；Again rigid thermal insulation tile is de-gassed process, the colloidal sol portion that then will be prepared by negative pressure
Divide or be stuffed entirely with inside rigid thermal insulation tile, add catalyst to form gel after 1-8 hour being stood at 50 DEG C, be subsequently adding
Alcohol solvent carries out burin-in process, and ageing time is 18-72 hour；The hexane solution of addition trim,ethylchlorosilane carries out hydrophobic
Process, process 1-3 days, then gel is carried out with hexane solution, until cleaning fluid is close to neutrality；By rigid thermal insulation tile
Take out from gel and be dried, 18-24 hour under room temperature, is dry, dry 24 hours at 50 DEG C, 70 DEG C of dryings 24 hours；Finally
The variously-shaped rigid thermal insulation tile compound from hydrophobic atmospheric pressure oxidation silica aerogel be can be prepared by through processing.
The present invention can process thermal insulation tile in silica aerogel combined rigidity thermal insulation tile and carry out selection sizing as needed.
Silica aerogel composite heat-insulating tile material, porosity are high, and aperture is little, to solid heat transfer and air heat transfer and convection current
There is good iris action；After introducing aeroge phase, composite heat-insulating tile is compared purer thermal insulation tile and is almost carried in terms of compressive strength
Double, material mechanical performance strengthens；Aeroge combined rigidity thermal insulation tile is prepared by the method for constant pressure and dry can be with mass
Production, low cost, can apply to civil area；By hydrophobic treatment, the storage capability of aeroge combined rigidity thermal insulation tile has
Obvious improvement.
Compared with prior art, the present invention has the advantages that：
The present invention prepares silica aerogel composite heat-insulating tile material, and porosity is high, and aperture is little, to solid heat transfer and air
Heat transfer and convection current have good iris action；The preparation method of the present invention is scientific and reasonable, simple, convenient to carry out, makes
Flat board, cover body and other complicated abnormal shape parts can be processed into from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile.
Specific embodiment
With reference to embodiment, the invention will be further described.
Raw material in embodiment and the Instrument specification for using as follows：
Rigid thermal insulation tile (quartz fibre rigidity thermal insulation tile, density 0.12-0.35g/cm3, Shandong industrial ceramics research and design
Co., Ltd of institute)；
Tetraethyl orthosilicate (analyzes pure, SiO2Content >=28%, Tianjin Bo Di chemical inc)；
Ethanol (analyzes pure, content >=99.7%, Laiyang City Kant Chemical Co., Ltd.)；
Electric mixer (model JJ-1, Jintan City of Jiangsu Province Xin Xin laboratory apparatus factory)
Vavuum pump (Zibo the Kunlun is had made to order)
Embodiment 1
Measure 20 moles of ethanol first, add 5 moles of tetraethyl orthosilicate and 30 moles of deionized water while stirring,
After mixing, add 0.002 mole of hydrochloric acid to continue stirring, obtain silica sol；Again rigid thermal insulation tile is dried and weigh
After carry out degassing process, then the colloidal sol of preparation is stuffed entirely with inside rigid thermal insulation tile by negative pressure, pressurize 10 minutes, plus
Enter 0.004 mole of ammoniacal liquor, form gel, be subsequently adding 3 liters of alcohol solvent, after making gel after 6 hours being stood at 50 DEG C
Material be completely immersed in alcohol solvent, carry out burin-in process, ageing time be 24 hours；Add 3 liter 10% of trimethyl chlorine
The hexane solution of silane carries out hydrophobic treatment, processes 2 days, then gel is carried out with 3 liters of hexane solutions every time, directly
To cleaning fluid pH=6.5；Rigid thermal insulation tile is taken out from gel and is dried, dry 24 hours under room temperature, dry at 50 DEG C
24 hours, 70 DEG C of dryings 24 hours；Eventually pass processing and can be prepared by the multiple from hydrophobic atmospheric pressure oxidation silica aerogel of different-thickness
The rigid thermal insulation tile of conjunction.
Performance test is carried out prepared by the invention described above from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile, close
Spend for 0.26g/cm3, at 300 DEG C, thermal conductivity is 0.03W/m K, and room temperature thickness direction compressive strength (5% decrement) is
1.9MPa.
Embodiment 2
Measure 50 moles of ethanol first, add 5 moles of tetraethyl orthosilicate and 15 moles of deionized water while stirring,
After mixing, add 0.001 mole of hydrochloric acid to continue stirring, obtain silica sol；Again rigid thermal insulation tile is dried and weigh
After carry out degassing process, then the colloidal sol of preparation is stuffed entirely with inside rigid thermal insulation tile by negative pressure, pressurize 10 minutes, plus
Enter 0.005 mole of ammoniacal liquor, form gel, be subsequently adding 4.5 liters of alcohol solvents, after making gel after 6 hours being stood at 50 DEG C
Material be completely immersed in alcohol solvent, carry out burin-in process, ageing time be 24 hours；Add 4.5 liter 10% of trimethyl
The hexane solution of chlorosilane carries out hydrophobic treatment, processes 2 days, then gel is carried out clearly with 4.5 liters of hexane solutions every time
Wash, until cleaning fluid pH=6.5；Rigid thermal insulation tile is taken out from gel and is dried, dry 24 hours under room temperature, at 50 DEG C
Dry 24 hours, 70 DEG C of dryings 24 hours；Eventually pass processing can be prepared by different-thickness from hydrophobic normobaric oxygen SiClx airsetting
The compound rigid thermal insulation tile of glue.
Performance test is carried out prepared by the invention described above from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile, close
Spend for 0.35g/cm3, at 300 DEG C, thermal conductivity is 0.04W/m K, and room temperature thickness direction compressive strength (5% decrement) is
2.5MPa.
Embodiment 3
Measure 400 moles of ethanol first, add 50 moles of tetraethyl orthosilicate and 200 moles of deionization while stirring
Water, after mixing, adds 0.01 mole of hydrochloric acid to continue stirring, obtains silica sol；Again rigid thermal insulation tile is dried and claim
Degassing process is carried out after weight, then the colloidal sol of preparation is stuffed entirely with inside rigid thermal insulation tile by negative pressure, pressurize 10 minutes,
0.05 mole of ammoniacal liquor is added, and forms gel, be subsequently adding 40 liters of alcohol solvents, after making gel after 6 hours being stood at 50 DEG C
Material be completely immersed in alcohol solvent, carry out burin-in process, ageing time be 24 hours；Add 40 liter 10% of trimethyl chlorine
The hexane solution of silane carries out hydrophobic treatment, processes 2 days, then gel is carried out with 40 liters of hexane solutions every time,
Until cleaning fluid pH=6.5；Rigid thermal insulation tile is taken out from gel and is dried, dry 24 hours under room temperature, do at 50 DEG C
Dry 24 hours, 70 DEG C of dryings 24 hours；Eventually pass processing can be prepared by mask body shape from hydrophobic atmospheric pressure oxidation silica aerogel
Compound rigid thermal insulation tile.
Mask body shape prepared by the invention described above carries out stone from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile
English lamp simulation test and wave transparent test, when cover body surface temperature is 500 DEG C, back temperature only has 90 DEG C, wave transmission rate ＞ 90%.
Claims (5)
1. one kind can process silica aerogel combined rigidity thermal insulation tile, it is characterised in that silica sol and rigid thermal insulation tile
Dry to be obtained after compound and can process silica aerogel combined rigidity thermal insulation tile；Its composition is：Rigid thermal insulation tile is quartz
Fiber rigidity thermal insulation tile, density are 0.12-0.35g/cm3；Silica sol dispensing mole ratio is：Tetraethyl orthosilicate：Ethanol：
Deionized water：Catalyst=1：2-10：2-12：0-0.01；
The preparation method of the described silica aerogel processed combined rigidity thermal insulation tile, comprises the steps：
（1）Silica sol：Measure ethanol first, add tetraethyl orthosilicate and deionized water while stirring, after mixing, plus
Enter catalyst and continue stirring, obtain silica sol；
（2）Compound：Rigid thermal insulation tile is de-gassed process, then passes through negative pressure by step（1）The silica sol of preparation
Partly or entirely it is filled into inside rigid thermal insulation tile, is allowed to be combined with rigid thermal insulation tile；
（3）Gel-aging：By step（2）Thermal insulation tile silica sol composite add catalyst stand 1-8 at 50 DEG C
Gel is formed after hour, alcohol solvent is subsequently adding, so that the material after gel is completely immersed in alcohol solvent, carries out aging place
Reason, ageing time are 18-72 hour；
（4）Hydrophobic treatment：To step（3）The hexane solution of trim,ethylchlorosilane is added to be reacted in gel after aging,
Time is 1-3 days, then gel is carried out with hexane solution, until cleaning fluid controls between pH=6.5-7.5；
（5）Constant pressure and dry：Rigid thermal insulation tile is taken out from gel be dried and obtain silica aerogel rigidity thermal insulation tile；
（6）Processing：By step（5）Silica aerogel combined rigidity thermal insulation tile after constant pressure and dry is can be prepared by after processing
Can process from hydrophobic atmospheric pressure oxidation silica aerogel combined rigidity thermal insulation tile；
Dry run is to dry 18-24 hour under room temperature, dries 24 hours at 50 DEG C, 70 DEG C of dryings 24 hours.
2. according to claim 1 silica aerogel combined rigidity thermal insulation tile is processed, it is characterised in that step（1）
Described catalyst is acidity.
3. according to claim 2 silica aerogel combined rigidity thermal insulation tile is processed, it is characterised in that step（1）
Described catalyst is hydrochloric acid or nitric acid.
4. according to claim 1 silica aerogel combined rigidity thermal insulation tile is processed, it is characterised in that step（3）
Described catalyst is alkalescence.
5. according to claim 4 silica aerogel combined rigidity thermal insulation tile is processed, it is characterised in that step（3）
Described catalyst is ammoniacal liquor.
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| CN104842217B (en) * | 2015-05-05 | 2017-03-01 | 山东工业陶瓷研究设计院有限公司 | Sky and space plane ceramic fibre rigidity thermal insulation tile precision machining method |
| CN104892014B (en) * | 2015-05-25 | 2017-05-24 | 哈尔滨工业大学 | Preparation method of 1200 DEG C resistant lightweight rigid ceramic fiber insulation tile |
| CN106747267B (en) * | 2016-12-02 | 2019-01-08 | 航天特种材料及工艺技术研究所 | A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof |
| CN108774072B (en) * | 2018-07-06 | 2020-04-17 | 航天特种材料及工艺技术研究所 | Rigid heat insulation tile and preparation method thereof |
| CN114213156B (en) * | 2021-12-28 | 2023-06-16 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat-insulating tile surface coating |
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| US6718776B2 (en) * | 2001-07-10 | 2004-04-13 | University Of Alabama In Huntsville | Passive thermal control enclosure for payloads |
| CN101450852A (en) * | 2008-11-27 | 2009-06-10 | 长沙星纳气凝胶有限公司 | Nano-pore SiO2 aerogel thermal insulation composite material and preparation method thereof |
| CN103241391B (en) * | 2013-04-25 | 2016-03-16 | 上海卫星工程研究所 | For the insulating assembly and preparation method thereof of Mars landing device heat control |
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