CN106431187A - Fiber and silicon dioxide aerogel composite heat insulation material and preparation method thereof - Google Patents
Fiber and silicon dioxide aerogel composite heat insulation material and preparation method thereof Download PDFInfo
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- CN106431187A CN106431187A CN201610826777.2A CN201610826777A CN106431187A CN 106431187 A CN106431187 A CN 106431187A CN 201610826777 A CN201610826777 A CN 201610826777A CN 106431187 A CN106431187 A CN 106431187A
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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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses a fiber and silicon dioxide aerogel composite heat insulation material and a preparation method thereof. The fiber and silicon dioxide aerogel composite heat insulation material has thermal conductivity of 0.020 to 0.040W/m.K, porosity of 80 to 90 percent, density of 0.10 to 0.18g/cm<3>, a specific surface area of 800 to 1,000m<2>/g, a hydrophobic angle of 120 to 170 degrees and an aperture distribution of 2 to 50nm. According to the prepared heat insulation material, the thermal property of aerogel is maximally reserved, the mechanical performance of the aerogel is improved, the material has certain strength and toughness, the compressive strength of the material is 0.3 to 5MPa, and the bending strength is 0.5 to 1.5Mpa. A preparation process is simple, short in period, low in equipment cost and safe in production, and the prepared material has high heat insulation performance, has the advantages of low thermal conductivity, low density, environment friendliness, safety, nontoxicity, flame retardancy, anticorrosion and the like compared with an ordinary inorganic heat-preservation material, and can be applied to a heat insulation material for pipeline transportation, a firefighting material and the like.
Description
Technical field
The present invention relates to a kind of fiber composite aerogel heat-insulating material and preparation method thereof, more particularly, to a kind of pre- to fiber
Process the independent hydrolysis process of colloidal sol, fiber composite silica is obtained by soda acid two step sol-gel process and in constant pressure and dry
Aerogel material, is applied to heat-barrier material field.
Background technology
Aerosil is a kind of light nanoporous amorphous solid material of excellent performance, by SiO2Network skeleton
Constituted with the gas being filled in nanoaperture.Its porosity may be up to 80-99.8%, and the typical sizes of hole are 1-
100nm, specific surface area is 200-1000m2/ g, density low can reach 0.003g/cm3, room temperature thermal conductivity factor low can reach 0.012w/
(m K), its distinctive dimensional network structure, extremely low density is hindered in insulation, photoconduction, dielectric, sound with thermal conductivity factor
Every, absorption, catalysis etc. field have broad application prospects.
Supercritical Drying Technology is combined by sol-gel process, changes formula composition to control the structure of aeroge, permissible
The aerosil that meet varying environment use requirement is obtained.But supercritical drying equipment has high demands, energy consumption is larger, makes gas
The cost of gel raises, and preparation is difficult, thus hindering SiO2The large-scale application of aerogel heat-insulating material produces.In this regard, mesh
Front research there has also been some improvement, is changed into cost from relatively costly, dangerous larger supercritical drying, freeze-drying
Low, the high atmosphere pressure desiccation of safety coefficient.
The low thermal conductivity of aerosil, the excellent thermal property such as high temperature resistant make it possible to be applied to thermal insulating material
Material field, serves as the raw material of heat-barrier material.But mechanical strength itself is low, limits range of application.Fiber composite aerogel heat-proof
Material refers to that fiber is added in colloidal sol profit, becomes an entirety using sol-gel process, wherein fiber is as skeleton
Support aeroge matrix, thus activeness and quietness aeroge, overcome the shortcomings of its low intensity, poor toughness, become truly
Superinsulation insulation material.
It is noted that a kind of constant pressure and dry prepares the tough SiO of fiber in patent CN101671030A2Aerogel composite
Method, reinforcing material used is short quartz fiber felt, high silica fiber felt or carbon fiber felt.This Fiber In Composite Material content
Larger, its thermal conductivity is less than 0.04W/m K, and material is in bulk, hydrophobic.
It is noted that a kind of aerogel heat-insulating composite material and preparation method thereof in patent CN1749214A, this material is also adopted
With aerosil and fibre reinforcement, by sol-gal process by colloidal sol fibrofelt or fiber preform, add red
Outer opacifier titanium dioxide, finally carries out supercritical fluid drying and is obtained.This thermal insulation of materials performance is good, has good hydrophobic
Performance, but need supercritical drying, cost is larger.
It is noted that a kind of system of the silicon dioxide aerogel composite thermal insulation material containing fiber in patent CN102010179B
Preparation Method, is characterized in first passing through by fiber and the prepared composite granule of infrared light screening agent addition aerogel precursor liquid, then utilizes
The technology path of semi-dry pressing, it is to avoid the supercritical drying of high cost.The aerosil that the method is obtained is combined
Material.
In patent CN1803602A, mention being split natural brucite fibre bundle with chemical dispersion method and be divided into after nanometer grade diameter
As reinforcing material, solid aerogel material is obtained under multi step strategy, constant pressure and dry.In Publication No. CN1636917A,
Inventor adopts the hollow secondary particle of the xonotlite fiber formation of ultrafine diameter as rigid support skeleton and silica
Aeroge forms composite, colloidal sol is poured in the hard calcium stone structure of porous by osmosis process, the dioxy that the method is obtained
SiClx aerogel composite heat-proof quality is good, but preparation technology is complex.
A kind of in patent CN101318659A it is noted that side of preparing silicon dioxide silica aerogel composite material by drying in atmosphere pressure
Method, wherein reinforcement are one of corpus fibrosum and soft polyurethane foam or two kinds, obtained material can be applicable to building heat preservation,
Sound insulation, the aspect such as industrial pipeline transport, but soft polyurethane foam therein is combustible material, leads to material fire safety performance poor.
Based on above-mentioned patent, this patent provide a kind of to fiber pretreatment, using sol-gel and in constant pressure and dry situation
The method of lower preparation fiber composite aerosil heat-barrier material.Wherein, fiber raw material glass fibers preferably cheap and easy to get
Dimension, handling process is simple, cost-effective, Environmental Safety, reduces fiber addition, improves in the case of ensureing material mechanical performance
The heat-proof quality of material, can be applicable to pipe insulation, the field such as transport heating.
Content of the invention
It is an object of the invention to provide a kind of fiber composite aerosil heat-barrier material and preparation method thereof, its
It is based on fiber pretreatment, using soda acid two step sol-gel process and at ambient pressure dry preparation method.This method can be
Big degree retain the excellent heat-proof quality of aeroge, strengthen the mechanical property of aeroge simultaneously, can be obtained with some strength
Aerosil heat-barrier material with toughness.
A kind of fiber composite aerosil heat-barrier material of the present invention, it is with aerosil as base
Body, adding wherein has glass fibre or other inorfils to be formed as reinforcement, described glass fibre or other are inorganic
Fiber is between 16-26% in the mass fraction in heat-barrier material；The thermal conductivity factor of this heat-barrier material is in 0.020-0.040W/
M K, porosity is 80-90%, and density is 0.10-0.18g/cm3, specific surface area 800-1000m2/ g, hydrophobic angle 120-
170 °, pore-size distribution is in 2-50nm, compression strength 0.3-5MPa, bending strength 0.5-1.5Mpa.
The preparation method of fiber composite aerosil heat-barrier material of the present invention, including step：
(1) preparation of aerosil precursor liquid：
Tetraethyl orthosilicate, ethanol, water, drying control chemical agent are mixed according to a certain percentage, hydrochloric acid adjust pH 3-6 it
Between, hydrolyze 4-8h after stirring at 45-60 DEG C；
(2) fiber composite silica wet gel is formed：
Measure the precursor liquid having hydrolyzed, be cooled to 10-20 DEG C, in the case of not higher than 25 DEG C of room temperature, add ammoniacal liquor to adjust
PH7-8, pours in mould after stirring 2-3 minute, more intermeshing fluffy fibre thin layer is tiled in mould by different level,
Ensure that fibrage is evenly distributed；Mould is sealed, puts in 42-48 DEG C of water-bath, 2-10min inner gel obtains wet gel；
(3) aging with exchange of solvent, modification：
Wet gel is taken out in mould and puts into container, seal after adding the ethanol of wet gel volume 2-3 times, 45-60 DEG C
The aging 4-6h of water-bath；Seal after ethanol in container being replaced by the n-hexane of wet gel volume 2-3 times, 45-50 DEG C of water-bath exchanges
Twice, each 4-6h；Pour out exchanging liquid n-hexane, add the TMCS hexane solution that volume fraction is 10-20%, seal,
45-50 DEG C of water-bath 18-24h；
(4) it is dried：
Wet gel n-hexane after the completion of modification is soaked surface modifier is removed in 8-12min backlash eccysis and other are anti-
Answer product, in 120 DEG C of drying boxes, 8-12h is dried.
In the preparation method of fiber composite aerosil heat-barrier material described above, the described each raw material of step (1)
Mol ratio be tetraethyl orthosilicate: ethanol: water: drying control chemical additive=1：(8-12)：(1.5-4.5)：
(0.25-2).
In the preparation method of fiber composite aerosil heat-barrier material described above, step (2) is described mutually to twine
The fluffy fibre thin layer of knot is by with fiber as raw material, is flowed back successively cleaning with ethanol, distilled water, 115-125 DEG C of drying,
Subsequently carry out combing with fiber carding machine fluffy, make mutually to tangle between fiber, and so that the fiber being originally bonded together is become
Fluffy and prepared.
In the preparation method of fiber composite aerosil heat-barrier material described above, described fiber is glass fibers
Dimension or other inorganic refractory fibers, including at least one in alumina fibre, ceramic fibre, fibre length in 4-8cm, directly
Footpath is 5-20 μm.Glass fibre is chosen as no alkali fiber (E-Glass), and mass fraction in composite heat-insulated material for the fiber exists
Between 16-26%, the fiber according to different cultivars can adjust fiber content in the material.Due to the rising with fiber content,
The heat-proof quality of aerogel material can significantly be affected, fiber content will be unable to play a supporting role very little, and aeroge is easily opened
Split, affect material mechanical performance, fiber quality fraction need to control within the specific limits.
Drying control chemical additive (DCCA) described above is formamide or DMF, its addition
For the amount of tetraethyl orthosilicate material 0.25-2 times.DCCA mainly makes aeroge aperture homogeneous, and it is in aeroge preparation
Typical additives.
In the preparation method of fiber composite aerosil heat-barrier material described above, also include doing step (4)
The step that fiber composite silica aerogel material after dry is heat-treated；The step of described heat treatment is will be dried
Fiber composite silica aerogel material is put in Muffle furnace, successively adjustment temperature be 270-280 DEG C, 295-305 DEG C and
345-355 DEG C is heat-treated 10-15 minute respectively.
In soda acid two step sol-gel process of the present invention, acid base catalysator used respectively hydrochloric acid and ammoniacal liquor, two kinds
Catalyst concn can not be too high, and, preferably in 0.1-0.3Mol/L, ammonia concn is preferably in 0.5-1Mol/L for concentration of hydrochloric acid.Hydrochloric acid is dense
When degree is higher, hydrolysis rate is accelerated, but subsequent gel step adds the amount of alkali to increase, and produced by-product ammonium chloride is difficult to remove
Go, crystallization in gel separates out.When ammonia concn is too high, gel time is accelerated, and is unfavorable for the interpolation of fiber, affects colloidal particle
Size and distribution.
In fiber composite aerosil heat-barrier material preparation method of the present invention, molten after step (2) hydrolysis
Glue temperature need to be cooled to 10-20 DEG C, and environment temperature need to control below 25 DEG C, environment temperature and collosol temperature too high quickening gel
Speed, is unfavorable for arrangement and the interpolation of fiber.
Fiber composite aerosil heat-barrier material of the present invention, thermal conductivity factor is in 0.020-0.040W/m
K, porosity is 80-90%, and density is 0.10-0.18g/cm3Specific surface area 800-1000m2/ g, hydrophobic angle 120-170 °, aperture
It is distributed in 2-50nm.Obtained heat-barrier material retains the thermal property of aeroge to greatest extent, improves the power of aeroge
Learn performance, material has some strength and toughness, compression strength 0.3-5MPa of material, bending strength 0.5-1.5Mpa.This
Bright preparation process is simple, cycle is short, equipment cost is low, production safety, and obtained material heat-proof quality is excellent, more inorganic
Insulation material has thermal conductivity factor low, and density is little, environmental protection, and safety non-toxic is fire-retardant, the advantages of anticorrosive, can be applicable to pipeline
Transport heat-barrier material, fire protective materials etc..
The beneficial effects of the present invention is：
1) provide a kind of simple fiber preprocess method.Because general inorfil anti acid alkali performance can be well it is difficult to change
Property, DeGrain after chemical treatment, fail to reach chemical bonds truly, this method considers from physical angle,
By in the fiber fluffy neatly colloidal sol after adding hydrolysis, control fiber addition, compared to fiber felt pan is directly entered or
Chopped strand is stirred and adds, in material, to add mass fraction lower for fiber, and dispersion evenly, obtains the silica of excellent performance
Aerogel composite.
2) normal pressure prepares glass fibre composite silicon dioxide wet gel, it is to avoid high cost and the supercritical drying that Keep Clear-High Voltage
Dry, easy to operate, cost-effective, improve production efficiency, good mechanical properties simultaneously, there is higher-strength, it is easy to accomplish industry
Metaplasia is produced.
3) the material heat-proof quality obtained by the present invention is excellent, low cost, and more general inorganic heat insulation material has thermal conductivity factor
Low, nontoxic pollution-free, can be applicable to pipeline transportation heat-barrier material, fire protective materials etc..
Brief description
Fig. 1 is fiber composite aerosil heat-barrier material preparation flow figure of the present invention；
Fig. 2 is the SiO of the embodiment of the present invention 1 preparation2The N of aeroge2Adsorption/desorption isothermal curve figure, wherein abscissa is
Relative pressure (p/p0), ordinate is volumetric adsorption (cm3/g STP)；It can be seen that curve belongs to IV type, it is typical mesoporous material
The adsorption curve of material.
Fig. 3 is the SiO of the embodiment of the present invention 1 preparation2The graph of pore diameter distribution of aeroge, wherein abscissa are aperture (nm),
Ordinate is pore volume (cm3/g)；SiO2Aeroge aperture is distributed in macropore range (2-50nm), and most apertures are all
Less than the mean free path (～70nm) of air molecule under normal temperature, therefore can effectively suppress its gaseous state heat conduction and convection heat transfer' heat-transfer by convection, can
So that material has relatively low thermal conductivity.
Fig. 4 a is SiO in heat-barrier material2The amplified SEM figure of aeroge, it may be seen that SiO2Aeroge is by nanoscale
Particle is crosslinked to constitute three-dimensional network skeleton, and internal is to show that fiber is interspersed in SiO as skeleton full of nanoaperture, Fig. 4 b2Gas
Wrapped up by aeroge in gel-in-matrix, Fig. 4 c distribution map in aeroge for composite fiber, in figure can be seen that
SiO2Aeroge matrix is supported by crisscross glass fibre, fiber distribution dispersion, the glass fiber mat with market sale
Toughening composition is compared laboratory sample fiber content and is reduced, and improves the heat-proof quality of material.
Fig. 5 is the embodiment of the present invention 1 gained fiber composite aerogel material pictorial diagram.
Specific embodiment
Following embodiments are to further illustrate using as the explaination to the technology of the present invention content for present invention,
But the flesh and blood of the present invention is not limited in described in following embodiments, those of ordinary skill in the art can and should know
Any simple change based on true spirit or replacement all should belong to protection domain of the presently claimed invention.
Embodiment 1：
Weigh certain mass glass fibre, washed successively with ethanol, distilled water, put in fiber carding machine after being dried and carry out
Fluffy process, the fluffy fiber thin layer after processing is stacked stand-by by level.Measure tetraethyl orthosilicate (TEOS)：4ml, ethanol
(EtOH)：35ml, H2O：12ml, formamide：2ml, adds in glass container and is uniformly mixed, and 0.1Mol/L hydrochloric acid adjusts pH to exist
Between 4-5, put into hydrolysis 6h in 45 DEG C of water-baths.After the completion of hydrolysis, cooling colloidal sol, to 15 DEG C, controls environment temperature to be 18 DEG C,
0.5Mol/L ammoniacal liquor adjusts pH7-8, pours long 8cm, wide 6cm into, in thick 2cm mould of plastics, weigh 0.5g fluffy after stirring 2-3min
Fibre thin layer is pressed level tiling and is added, sealing, 8-10min gel at 45 DEG C.After gel take out sample put into more slightly larger than sample
In container, add 45 DEG C of aging 8h of ethanol, 45 DEG C of n-hexane exchanges twice 6h every time, adds the TMCS that volume fraction is 10% to change
Property liquid (hexane solution of trim,ethylchlorosilane), modified 24h.After the completion of modification, soak sample 10min with n-hexane and rush
Wash, remove other product.Sample is dried 12h as 120 DEG C.By dried fiber composite aerosil material
Material put in Muffle furnace adjustment temperature be respectively 275 DEG C, 300 DEG C, 350 DEG C when each heat treatment take out after 10 minutes.
Obtained fiber composite aerogel material 2.2g, porosity 87.35%, density 0.149g/cm3, BET specific surface area
963.88m2/ g, in hydrophobicity, thermal conductivity factor 0.0228W/m K.Compression strength 3.68MPa, bending strength 1.16Mpa.
Embodiment 2：
Weigh certain mass glass fibre ethanol, distilled water washs successively, put in fiber carding machine after being dried and carry out
Fluffy process, the fibre thin layer after processing is stacked stand-by by level.Measure TEOS：6ml, EtOH：60ml, H2O：12ml, first
Acid amides：It is uniformly mixed in 3ml addition glass container, 0.1Mol/L hydrochloric acid adjusts pH between 4-5, puts into water in 50 DEG C of water-baths
Solution 6h.After the completion of hydrolysis, cooling colloidal sol, to 15 DEG C, controls environment temperature to be 18 DEG C, 0.5Mol/L ammoniacal liquor adjusts pH7-8, stirs 2-
Pour long 8cm, wide 6cm after 3min into, in thick 1.5cm mould of plastics, weigh 0.6g fluffy fiber and add by level tiling, sealing,
2-10min gel at 45 DEG C.Take out sample after gel to put in the container more slightly larger than sample, add 50 DEG C of aging 6h of ethanol, just
45 DEG C of hexane exchanges twice 6h every time, adds the TMCS modification liquid that volume fraction is 20%, modified 24h.After the completion of modification, with just
Hexane soaks sample 10min and rinses, and removes other product.Sample is dried 12h as 120 DEG C.By dried fibre
Dimension dioxide composite Silica Aerogels are put into adjustment temperature in Muffle furnace and are respectively 275 DEG C, 300 DEG C, 350 DEG C of each heat treatments
Take out after 10 minutes.
Obtained fiber composite aerogel material 3.1g, porosity 87.12%, density 0.152g/cm3, BET specific surface area
917.24m2/ g, in hydrophobicity, thermal conductivity factor 0.0231W/m K.Compression strength 4.15MPa, bending strength 1.2Mpa.
Embodiment 3：
Weigh certain mass glass fibre ethanol, distilled water washs successively, put in fiber carding machine after being dried and carry out
Fluffy process, the fibre thin layer after processing is stacked stand-by by level.Measure TEOS：6ml, EtOH：60ml, H2O：16ml, first
Acid amides：It is uniformly mixed in 3ml addition glass container, 0.1Mol/L hydrochloric acid adjusts pH between 3-4, puts into water in 60 DEG C of water-baths
Solution 4h.After the completion of hydrolysis, cooling colloidal sol, to 15 DEG C, controls environment temperature to be 18 DEG C, 0.5Mol/L ammoniacal liquor adjusts pH7-8, stirs 2-
Pour long 8cm, wide 6cm after 3min into, in thick 1.5cm mould of plastics, weigh 0.8g fluffy fiber and add by level tiling, sealing,
2-10min gel at 45 DEG C.Take out sample after gel to put in the container more slightly larger than sample, add 50 DEG C of aging 6h of ethanol, just
45 DEG C of hexane exchanges twice 6h every time, adds the TMCS modification liquid that volume fraction is 30%, modified 24h.After the completion of modification, with just
Hexane soaks sample 10min and rinses, and removes other product.Sample is dried 12h as 120 DEG C.By dried fibre
Dimension dioxide composite Silica Aerogels are put into adjustment temperature in Muffle furnace and are respectively 275 DEG C, 300 DEG C, 350 DEG C of each heat treatments 10
Take out after minute.
Obtained fiber composite aerogel material 3.5g, porosity 86.69%, density 0.156g/cm3, BET specific surface area
904.68m2/ g, in hydrophobicity, thermal conductivity factor 0.0232W/m K.Compression strength 4.2MPa, bending strength 1.3Mpa.
Embodiment 4：
Weigh certain mass glass fibre ethanol, distilled water washs successively, put in fiber carding machine after being dried and carry out
Fluffy process, the fibre thin layer after processing is stacked stand-by by level.Measure TEOS：8ml, EtOH：70ml, H2O：25ml, first
Acid amides：It is uniformly mixed in 4ml addition glass container, 0.1Mol/L hydrochloric acid adjusts pH between 3-4, puts into water in 50 DEG C of water-baths
Solution 6h.After the completion of hydrolysis, cooling colloidal sol, to 15 DEG C, controls environment temperature to be 18 DEG C, 0.5Mol/L ammoniacal liquor adjusts pH7-8, stirs 2-
Pour long 8cm, wide 6cm after 3min into, in thick 1.5cm mould of plastics, weigh 0.8g fluffy fiber and add by level tiling, sealing,
2-10min gel at 45 DEG C.Take out sample after gel to put in the container more slightly larger than sample, add 50 DEG C of aging 6h of ethanol, just
45 DEG C of hexane exchanges twice 6h every time, adds the TMCS modification liquid that volume fraction is 10%, modified 24h.After the completion of modification, with just
Hexane soaks sample 10min and rinses, and removes other product.Sample is dried 12h as 120 DEG C.Three are taken after drying
Sample is respectively put in Muffle furnace, and adjustment temperature is respectively 275 DEG C, 300 DEG C, 350 DEG C, and each 10min that processes takes out.
Obtained fiber composite aerogel material 4.5g, porosity 86.44%, density 0.160g/cm3, BET specific surface area
887.53m2/ g, in hydrophobicity, thermal conductivity factor 0.0243W/m K.Compression strength 4.0MPa, bending strength 1.2Mpa.
Claims (8)
1. a kind of fiber composite aerosil heat-barrier material, it is with aerosil as matrix, wherein plus
Enter to have glass fibre or other inorfils to be formed as reinforcement, described glass fibre or other inorfils are in heat-insulated material
Mass fraction in material is between 16-26%；The thermal conductivity factor of this heat-barrier material in 0.020-0.040W/m K, porosity is
80-90%, density is 0.10-0.18g/cm3, specific surface area 800-1000m2/ g, hydrophobic angle 120-170 °, pore-size distribution is in 2-
50nm, compression strength 0.3-5MPa, bending strength 0.5-1.5Mpa.
2. the preparation method of fiber composite aerosil heat-barrier material described in a kind of claim 1, including step：
（1）The preparation of aerosil precursor liquid：
Tetraethyl orthosilicate, ethanol, water, drying control chemical agent are mixed according to a certain percentage, hydrochloric acid adjusts pH between 3 and 6,
Hydrolyze 4-8h at 45-60 DEG C after stirring；
（2）Fiber composite silica wet gel is formed：
Measure the precursor liquid having hydrolyzed, be cooled to 10-20 DEG C, in the case of not higher than 25 DEG C of room temperature, add ammoniacal liquor to adjust pH7-
8, pour in mould after stirring 2-3 minute, more intermeshing fluffy fibre thin layer is tiled in mould by different level it is ensured that
Fibrage is evenly distributed；Mould is sealed, puts in 42-48 DEG C of water-bath, 2-10min inner gel obtains wet gel；
（3）Aging with exchange of solvent, modification：
Wet gel is taken out in mould and puts into container, seal after adding the ethanol of wet gel volume 2-3 times, 45-60 DEG C of water-bath
Aging 4-6h；Seal after ethanol in container being replaced by the n-hexane of wet gel volume 2-3 times, 45-50 DEG C of water-bath exchanges twice,
4-6h every time；Pour out exchanging liquid n-hexane, add the TMCS hexane solution that volume fraction is 10-20%, seal, 45-50 DEG C
Water-bath 18-24h；
（4）It is dried：
Wet gel n-hexane after the completion of modification is soaked 8-12min backlash eccysis goes surface modifier and other reactions to produce
Thing, is dried 8-12h in 120 DEG C of drying boxes.
3. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 2 is it is characterised in that step
（1）The mol ratio of described each raw material is tetraethyl orthosilicate: ethanol: water: drying control chemical additive 1：（8-12）：
（1.5-4.5）：（0.25-2）.
4. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 2 is it is characterised in that step
（2）Described intermeshing fluffy fibre thin layer is by with fiber as raw material, is flowed back successively cleaning with ethanol, distilled water,
115-125 DEG C of drying, subsequently carry out combing with fiber carding machine fluffy, makes mutually to tangle between fiber, and makes originally to be bonded in
Fiber together becomes fluffy and prepared.
5. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 4 is it is characterised in that described
Fiber be glass fibre or other inorganic refractory fibers, including at least one in alumina fibre, ceramic fibre, fiber
Length in 4-8cm, a diameter of 5-20 μm.
6. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 2 is it is characterised in that described
Drying control chemical additive be formamide or DMF, its addition be tetraethyl orthosilicate material amount
0.25-2 times.
7. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 2 is it is characterised in that also wrap
Include step（4）The step that dried fiber composite silica aerogel material is heat-treated.
8. the preparation method of fiber composite aerosil heat-barrier material as claimed in claim 7 is it is characterised in that described
The step of heat treatment is to put in Muffle furnace by dried fiber composite silica aerogel material, and successively adjustment temperature is
270-280 DEG C, 295-305 DEG C and 345-355 DEG C are heat-treated 10-15 minute respectively.
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