CN106187069A - A kind of preparation method of super-hydrophobic high-strength light heat-barrier material - Google Patents
A kind of preparation method of super-hydrophobic high-strength light heat-barrier material Download PDFInfo
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- CN106187069A CN106187069A CN201610526462.6A CN201610526462A CN106187069A CN 106187069 A CN106187069 A CN 106187069A CN 201610526462 A CN201610526462 A CN 201610526462A CN 106187069 A CN106187069 A CN 106187069A
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Abstract
The present invention relates to the preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, with zirconium alkoxide and siloxanes as presoma, use the colloidal sol glue that pre-hydrolysis technique preparation is the most compound, after vacuum impregnation is in fiber felt, the ethanol solution using tetraethyl orthosilicate carries out aging, then using supercritical drying process to prepare fiber felt/aeroge complex, recycle silicon azane steam processes, and is prepared for the heat-barrier material of super-hydrophobic, low heat conductivity and high intensity.Its contact angle is 156 °, and room temperature thermal conductivity is 0.032W/m K, and comprcssive strength is (10% deformation) 0.42MPa.Solve that heat-barrier material is moistureproof in practice, the technical barrier such as mechanical strength and heat-proof quality.
Description
Technical field
The invention belongs to inorganic material preparation and sol-gal process technical field, be specifically related to one and change with silazane gas
The method that property aeroge/fiber composite prepares the super-hydrophobic heat-barrier material of high-strength light.
Background technology
At present, with ceramic fibres such as quartz fibre, mullite fiber, Zirconium oxide fibres with inorganic binder by sintering system
Standby rigid fiber thermal insulation tile, with the advantages such as its high-melting-point, antioxidation, low-density, excellent heat-proof quality and thermal shock resistance, quilt
It is widely used in the fields such as Aero-Space, steel and iron industry, petrochemical industry, Industrial Stoves and building materials fire-proof and thermal-insulation.In recent years,
Along with Aero-Space, industry etc. develop rapidly, intensity and heat-proof quality to heat-barrier material require more and more higher, traditional rigidity
Ceramic insulation watt, including full quartz fibre rigid ceramic thermal insulation tile, refractory fibre composite thermal insulation tile (FRCI) and aluminium oxide
Strengthening heatshield material (AETB), hot properties material (HTP), the performance such as it is high temperature resistant, mechanical strength can not expire completely
Foot needs.Dong Xue et al. have studied a kind in 2014 in periodical " Composites science and technology "
The textile porous materials of Bird's Nest structure, compares tradition thermal insulation tile and has compared with high mechanical strength that (during 10% deformation, comprcssive strength is big
In 2MPa), but this material but shows higher heat conductivity (0.231-0.248W/ (m K)) simultaneously, improves mechanics
Performance but sacrifices heat-proof quality.Aeroge is to be made up of the gel particles of Nano grade to have three-dimensional continuous print nanoporous net
The low density solid material of network structure, has high-specific surface area, high adsorption, low-density, lower thermal conductivity, low-refraction etc. excellent
Point, is with a wide range of applications at numerous areas such as catalysis, environmental protection, heat insulation, optics.The patent of publication number CN102765755A
In be successfully prepared the ZrO of low heat conduction (0.018W/ (m K))2Aeroge, but the extremely low mechanical strength of pure aeroge is big
Limit greatly the aeroge utilization in heat insulation field.In order to solve the fragility of aeroge and blockiness, many researcheres are by pottery
Rigidity thermal insulation tile is compound with aeroge prepares heat-barrier material.National University of Defense technology Wang Yan flies et al. 2008 at Master's thesis " gas
The preparation of gel composite ceramic fiber rigidity thermal insulation tile and performance study " just use SiO2Aeroge composite ceramic fiber rigidity is heat insulation
Watt prepared composite, compares former rigidity thermal insulation tile, while this heat conductivity (0.045W/ (m K)) reduces, by force
Degree (during 10% deformation, bending strength is 0.315MPa) have also been obtained raising.Li Jianfang et al. 2007 is " novel at Master's thesis
High temperature resistance multilayer heat insulating structural research " in have studied with high temperature resistant aluminum silicate fiber paper and quartz fiber felt as matrix, hydrophobicity
SiO2Aerogel particle is the novel fire resistant multistory steel structure of thermal insulating filling, improves the multilayer insulation material of tradition application
Heatproof and the performance such as effect of heat insulation.Exist, such as U.S. about the fiber felt insulation material that aeroge is compound in the market
Fiber aeroge is met the heat insulation aerogel products of flexibility of preparation by ASPEN company of state, and its tensile strength is about 0.088MPa.
From the foregoing, it will be observed that the heat-barrier material that pottery rigidity thermal insulation tile and aeroge are combined preparation is improving the strong of heat-barrier material
Degree and heat conduction aspect have obvious action.But heat-barrier material is in actual use, higher strong except needing to have
Degree and excellent heat-proof quality, owing to it uses in wet environment, the easy moisture absorption in thermal insulation tile surface and lost efficacy.Therefore, it is being improved
While intensity and heat-proof quality, it is carried out hydrophobic treatment also extremely important.The patent of Publication No. 104556063 uses fluorine
The surface tension of water is reduced to 15-20mN/m by carbon surface active agent, dramatically reduces hydrogel surface tension force thus possesses
Certain hydrophobicity, but the aeroge hydrophobic effect that this technique obtains is the most general.Publication No. CN103691370A special
Profit is then by changing silicon source, and such as RSiX3, (R represents alkyl, vinyl, phenyl etc.；X representation methoxy, ethyoxyl etc.) type
Silane, as silicon source, is prepared hydrophobic aerogel, but these silicon sources chosen is relatively costly, cut the blockiness not good enough and big day of one's doom
Make it to use.Hydrophobic treatment about aeroge fibrous thermal watt mainly uses trim,ethylchlorosilane etc. surpassing the most both at home and abroad
Processing before closing on, the composite obtained has certain hydrophobic effect, but introduces or aging at gel situ
During introduce silane or during siloxane compound, inside and outside in gel skeleton, there is concentration difference, the gas that this method prepares
Gel surface is modified not exclusively, and modified benefit is low；Meanwhile, in supercritical fluid, the-Si-OR in aeroge surface modification also may be used
Can decompose thus reduce the hydrophobic performance of aeroge.
The present invention, with zirconium alkoxide and siloxanes as raw material, uses pre-hydrolysis method to prepare zirconia-silica complex sol,
It is combined with Zirconium oxide fibre felt by vacuum impregnation technique, then prepares aeroge/fiber felt compound heat-insulation through supercritical drying
Material.Finally, complex is placed in hermetic container, processes with silazane steam at a certain temperature, be prepared for contact angle big
In 150 ° of super-hydrophobic thermal insulation tiles, there is higher mechanical strength and excellent heat-proof quality simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is to process aeroge/fiber felt complex with silazane steam to prepare low close
Degree, low heat conduction, high-temperature stability well, have the composite of super-hydrophobicity.
In order to solve above-mentioned technical problem, the present invention is with inorganic fibrous mats as precast body, with zirconium silica aerogel as obturator
Hydrophobically modified is carried out, it is provided that the preparation method of a kind of super-hydrophobic thermal insulation tile with silazane steam:
Concrete technical scheme is as follows:
The preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, concretely comprises the following steps:
(1) preparation of silica-zirconia complex sol
In the temperature of 4～40 DEG C, siloxanes is dissolved in alcohol by stirring the alcohol of the siloxanes that dose volume mark is 20%
Solution；Stating then up and dripping mass concentration in alcoholic solution is 65～68% concentrated nitric acid, drips deionization after stirring 10～20min
Water, continues stirring 5～60min, obtains the siloxane solution of prehydrolysis in advance；Quality is dripped to the siloxane solution of prehydrolysis
Concentration is the concentrated nitric acid of 65～68%, drips zirconium alkoxide, be stirring evenly and then adding into deionized water after mix homogeneously；Continue stirring 5-
60min, obtains clear colloidal sol；
(2) mullite fiber felt and zirconia-silica colloidal sol is compound
By fiber felt under vacuum, impregnated in the zirconia-silica colloidal sol of 0.5～1.5mol/L, and keep
Vacuum 30min～60min；
(3) mullite fiber felt is combined the preparation of wet gel
Then the fiber felt of described impregnant sol is transferred in mould, still aging 4～24h, obtains fiber felt/oxidation
Zirconium-silicon oxide is combined wet gel；
(4) mullite fiber felt is combined the aging of wet gel
Fiber felt in step (3) is combined wet gel aged solution carry out respectively soaking 12～72h at 30～100 DEG C；
Finally carry out soaking 2～5 times with the solvent identical with dry medium dehydrated alcohol or isopropanol, each soak time be 3～
12h；
(5) supercritical drying
Gains in step (3) are carried out supercritical drying and obtains fiber felt/zirconia-silica compound heat-insulation material
Material；
(6) hydrophobically modified；
The composite heat-insulated material and the silazane solution that step (5) are obtained are placed in hermetic container, be heated to 120 DEG C～
180 DEG C of insulations 2～8h, complex is modified by now silazane formation steam, obtains superhydrophobic aerogel/fiber felt heat insulation
Material.
Described siloxanes is tetraethyl orthosilicate, tetramethoxy-silicane or MTES；Zirconium alkoxide is positive fourth
Alcohol zirconium, zirconium-n-propylate or zirconium iso-propoxide.
Described fiber felt is mullite fiber felt, Zirconium oxide fibre felt or alumina silicate fiber felt.
Described silazane is hexamethyldisiloxane and 1,3-divinyl-1,1,3,3-tetramethyl-disilazane.
Described alcohol is ethanol, normal propyl alcohol, isopropanol or n-butyl alcohol.
Described step 1) tetraethyl orthosilicate in zirconia-silica complex sol: the mol ratio=1:0.11 of zirconium alkoxide～
9, in zirconia-silica complex sol, zirconium alkoxide is 0.25～2.0mol/L with the concentration sum of siloxanes.
Siloxanes in the preparation process of described step (1) prehydrolysis siloxane solution: water: the mol ratio=1:2 of nitric acid～
3:0.06～0.12；Zirconium alkoxide in the preparation process of zirconia-silica complex sol: water: the mol ratio=1:2～4 of nitric acid:
0.06～0.21.
Described aged solution in step (4) is dehydrated alcohol: tetraethyl orthosilicate volume ratio is the mixing of 1:0.25～4
Liquid.Described dry medium is ethanol or isopropanol.
Supercritical drying process in step (4) is: the wet gel after aging is loaded autoclave, adds and be dried medium
Submergence, nitrogen purging 5～40min, pre-inflated with nitrogen 0.5～5MPa；0.5～3 DEG C/min be warming up to higher than supercritical temperature 10～
30 DEG C and be incubated 0.5～3 hour, with 0.01～0.1MPa/min pressure release, pressure release complete after nitrogen purging 5～40min.The coldest
But to room temperature；Described dry medium is: dehydrated alcohol or isopropanol.
In middle the added silazane of step (6) quality is composite heat-insulated material quality 1/5～1/10.
In the preparation process in accordance with the present invention, it is first to make itself and zirconium alkoxide reactivity mutually by siloxanes prehydrolysis
Join, it is achieved uniformly mixing of the higher degree of Zr with Si, improve high-temperature stability.It is to enable that silazane pretreatment becomes steam
Uniform modified fibre felt/aeroge complex, improves its hydrophobic performance.
In the preparation process in accordance with the present invention, silazane steam is used to process fiber felt/aeroge complex, on the one hand can be all
The modified complex in even ground, improves its hydrophobic performance；The most modified complex surfaces-OH is by-Si-CH3Replace, silicon first
Base at high temperature can decomposite Si disperse on aeroge skeleton, is conducive to improving its high-temperature stability, simultaneously-Si-CH3Draw
Enter the intensity that can improve complex.
In sum, the present invention, with zirconium alkoxide and siloxanes as presoma, uses pre-hydrolysis technique preparation the most compound
Colloidal sol glue, after vacuum impregnation is in fiber felt, uses the ethanol solution of tetraethyl orthosilicate to carry out aging, then uses supercritical drying
Drying process has prepared fiber felt/aeroge complex, and recycle silicon azane steam processes, be prepared for super-hydrophobic, low heat conductivity and
The heat-barrier material of high intensity.Its contact angle is 156 °, and room temperature thermal conductivity is 0.032W/m K, and comprcssive strength is (10% deformation)
0.42MPa.Solve that heat-barrier material is moistureproof in practice, the technical barrier such as mechanical strength and heat-proof quality.
Accompanying drawing explanation
Fig. 1 HMDS steam processes aeroge schematic diagram.
Fig. 2 is the outside drawing of the fiber felt/aeroge complex of silazane modification prepared by the present invention.
Fig. 3 is the fiber felt/aeroge complex scanning electron microscope microscopic appearance figure of silazane modification prepared by the present invention.
Fig. 4 is the contact angle figure of the fiber felt/aeroge complex of silazane modification prepared by the present invention.
Fig. 5 is the mechanical stress strain figure of the fiber felt/aeroge complex of silazane modification prepared by the present invention.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, fiber felt selects mullite fiber felt, silazane choosing
With hexamethyldisiloxane, zirconium alkoxide selection zirconium-n-propylate, siloxanes selection tetraethyl orthosilicate, alcoholic solvent selects ethanol, aging
Solution is volume ratio dehydrated alcohol: the mixed liquor of tetraethyl orthosilicate=1:0.25, and dry medium is dehydrated alcohol, siloxanes: zirconium
Mol ratio=the 1:0.11 of alkoxide, in zirconia-silica complex sol, zirconium alkoxide with the concentration sum of siloxanes is
0.25mol/L.Follow the steps below successively:
(1) preparation of silica-zirconia complex sol
At 4 DEG C, tetraethyl orthosilicate being dissolved in ethanol, stirring mixes to obtain 0.225mol/L mixed solution；According to mol Si:
mol HNO3=1:0.06 dropping mass concentration is 65～68% concentrated nitric acid.According to mol Si:mol H2O=1:3 drips deionization
Water, continues stirring 60min and obtains prehydrolysis siloxane solution；According to mol Zr:mol HNO3=1:0.06 is to prehydrolysis siloxanes
Solution dropping concentrated nitric acid, drips zirconium-n-propylate according to mol Si:mol Zr=1:0.11 after mix homogeneously, according to mol Zr:mol
H2O=1:4 drips deionized water, continues stirring 60min, obtains clear colloidal sol；
(2) mullite fiber felt and zirconia-silica colloidal sol is compound
By mullite fiber felt under vacuum, impregnated in the zirconia-silica colloidal sol of 0.25mol/L, and protect
Hold vacuum 30min；
(3) mullite fiber felt is combined the preparation of wet gel
The mullite fiber felt of described impregnant sol is transferred in mould, still aging 24h, obtains mullite fiber
Felt/zirconia-silica is combined wet gel；
(4) mullite fiber felt is combined the aging of wet gel
Mullite fiber felt in step (3) is combined wet gel dehydrated alcohol: tetraethyl orthosilicate volume ratio is 1:2's
Aged solution carries out soaking 12h at 50 DEG C respectively；Finally carry out soaking 3 times, when soaking with dry medium dehydrated alcohol every time
Between be 3h；
(5) supercritical drying: the gained mullite fiber felt in step (4) is combined wet gel and carries out supercritical drying
Wet gel after aging is loaded autoclave, adds and be dried medium submergence, nitrogen purging 5min, pre-inflated with nitrogen
0.5MPa；0.5 DEG C/min is warming up to higher than supercritical temperature 10 DEG C and is incubated 0.5 hour, with 0.01MPa/min pressure release, pressure release
Nitrogen purging 5min after completing.Naturally cool to room temperature, drive still and obtain aeroge/mullite fiber felt heat-barrier material.
(6) hydrophobically modified；
The volume (5) obtained is 13.05cm-1, quality is that the complex of 3.94g is placed in hermetic container, such as Fig. 1 institute
Show, with the hexamethyldisiloxane steam modification 2h of 0.4g under 150 °, obtain superhydrophobic aerogel/mullite fiber felt heat insulation
Material；
The outward appearance of gained aeroge/fiber felt heat-barrier material is as shown in Figure 2；This sample microcosmic shape under surface sweeping Electronic Speculum
Looks figure is as shown in Figure 3；The contact angle test result figure of this sample is as shown in Figure 4；The stress-strain curve diagram of this sample such as Fig. 5
Shown in.
The macro surface of obtained complex is smooth, density 0.302g/m3, thermal conductivity 0.0341W/m K, contact angle
Size is 156 °, and during 10% deformation, comprcssive strength is 0.42MPa.It can be seen that aeroge and fiber from its micro-structure diagram
Having preferably connection, aeroge keeps its three-dimensional porous structure simultaneously.
Embodiment 2
The preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, fiber felt selects Zirconium oxide fibre felt, silazane choosing
With 1,3-divinyl-1,1,3,3-tetramethyl-disilazane, zirconium alkoxide selects zirconium-n-propylate, siloxanes selection tetramethoxy-silicane
Alkane, alcoholic solvent selection normal propyl alcohol, aged solution is volume ratio dehydrated alcohol: the mixed liquor of tetraethyl orthosilicate=1:1, is dried medium
For dehydrated alcohol, siloxanes: the mol ratio=1:1 of zirconium alkoxide, zirconium alkoxide and siloxanes in zirconia-silica complex sol
Concentration sum is 0.5mol/L.Follow the steps below successively:
(1) preparation of silica-zirconia complex sol
At 20 DEG C, tetramethoxy-silicane being dissolved in normal propyl alcohol, stirring mixes to obtain 0.25mol/L mixed solution；According to mol
Si:mol HNO3=1:0.09 dropping mass concentration is 65～68% concentrated nitric acid.According to mol Si:mol H2O=1:2.5 drips
Distilled water, continues stirring 30min and obtains prehydrolysis siloxane solution；According to mol Zr:mol HNO3=1:0.15 is to prehydrolysis silicon
Oxygen alkane solution dropping concentrated nitric acid, drips zirconium-n-propylate according to mol Si:mol Zr=1:1 after mix homogeneously, according to mol Zr:
mol H2O=1:3 drips deionized water, continues stirring 30min, obtains clear colloidal sol；
(2) Zirconium oxide fibre felt and zirconia-silica colloidal sol is compound
By Zirconium oxide fibre felt under vacuum, impregnated in the zirconia-silica colloidal sol of 0.5mol/L, and keep
Vacuum 45min；
(3) Zirconium oxide fibre felt is combined the preparation of wet gel
The fiber felt of described impregnant sol is transferred in mould, still aging 10h, obtains Zirconium oxide fibre felt/oxidation
Zirconium-silicon oxide is combined wet gel；
(4) Zirconium oxide fibre felt is combined the aging of wet gel
Zirconium oxide fibre felt in step (3) is combined wet gel dehydrated alcohol: tetraethyl orthosilicate volume ratio is the old of 1:1
Change solution to carry out respectively soaking 72h at 35 DEG C；Finally carry out soaking 5 times with dry medium dehydrated alcohol, each soak time
For 3h；
(5) supercritical drying: the gained Zirconium oxide fibre felt in step (4) is combined wet gel and carries out supercritical drying
Wet gel after aging is loaded autoclave, adds and be dried medium submergence, nitrogen purging 5min, pre-inflated with nitrogen
0.5MPa；0.5 DEG C/min is warming up to higher than supercritical temperature 10 DEG C and is incubated 0.5 hour, with 0.01MPa/min pressure release, pressure release
Nitrogen purging 5min after completing.Naturally cool to room temperature, drive still and obtain aeroge/Zirconium oxide fibre felt heat-barrier material.
(6) hydrophobically modified；
The volume (5) obtained is 14.02cm-1, quality is that 4.18g complex is placed in hermetic container, as it is shown in figure 1,
With the 1 of 0.8g under 160 °, 3-divinyl-1,1,3,3-tetramethyl-disilazane steam modification 4h, obtain super-hydrophobic airsetting
Glue/mullite fiber felt heat-barrier material；
The macro surface of obtained complex is smooth, density 0.298g/m3, thermal conductivity 0.0325W/m K, contact angle
Size is 153 °, and during 10% deformation, comprcssive strength is 0.45MPa.
Embodiment 3
The preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, fiber felt selects mullite fiber felt, silazane choosing
With 1,3-divinyl-1,1,3,3-tetramethyl-disilazane, zirconium alkoxide selects zirconium iso-propoxide, siloxanes selection methyl three ethoxy
Base silane, alcoholic solvent selection isopropanol, aged solution is volume ratio dehydrated alcohol: the mixed liquor of tetraethyl orthosilicate=1:2, is dried
Medium is isopropanol, siloxanes: the mol ratio=1:1 of zirconium alkoxide, zirconium alkoxide and siloxanes in zirconia-silica complex sol
Concentration sum be 1.0mol/L.Follow the steps below successively:
(1) preparation of silica-zirconia complex sol
At 20 DEG C, methyltriethoxy silane being dissolved in isopropanol, stirring mixes to obtain 0.5mol/L mixed solution；According to
Mol Si:mol HNO3=1:0.09 dropping mass concentration is 65～68% concentrated nitric acid.According to mol Si:mol H2O=1:2.5
Dropping distilled water, continues stirring 30min and obtains prehydrolysis siloxane solution；According to mol Zr:mol HNO3=1:0.15 is to pre-water
Solve siloxane solution dropping concentrated nitric acid, drip zirconium iso-propoxide according to mol Si:mol Zr=1:1 after mix homogeneously, according to mol
Zr:mol H2O=1:3 drips deionized water, continues stirring 30min, obtains clear colloidal sol；
(2) mullite fiber felt and zirconia-silica colloidal sol is compound
By mullite fiber felt under vacuum, impregnated in the zirconia-silica colloidal sol of 1.0mol/L, and keep
Vacuum 40min；
(3) mullite fiber felt is combined the preparation of wet gel
The mullite fiber felt of described impregnant sol is transferred in mould, still aging 12h, obtains mullite fiber
Felt/zirconia-silica is combined wet gel；
(4) mullite fiber felt is combined the aging of wet gel
Mullite fiber felt in step (3) is combined wet gel dehydrated alcohol: tetraethyl orthosilicate volume ratio is the old of 1:2
Change solution to carry out respectively soaking 72h at 35 DEG C；Finally carry out soaking 5 times with dry medium dehydrated alcohol, each soak time
For 12h；
(5) supercritical drying: the gained mullite fiber felt in step (4) is combined wet gel and carries out supercritical drying
Wet gel after aging is loaded autoclave, adds and be dried medium submergence, nitrogen purging 20min, pre-inflated with nitrogen
2MPa；2 DEG C/min is warming up to higher than supercritical temperature 20 DEG C and is incubated 1 hour, with 0.05MPa/min pressure release, after pressure release completes
Nitrogen purging 20min.Naturally cool to room temperature, drive still and obtain aeroge/mullite fiber felt heat-barrier material.
(6) hydrophobically modified；
The volume (5) obtained is 13.85cm-1, quality is that 4.26g complex is placed in hermetic container, as it is shown in figure 1,
With the 1 of 0.6g under 140 °, 3-divinyl-1,1,3,3-tetramethyl-disilazane steam modification 6h, obtain super-hydrophobic airsetting
Glue/mullite fiber felt heat-barrier material；
The macro surface of obtained complex is smooth, density 0.308g/m3, thermal conductivity 0.0301W/m K, contact angle
Size is 155 °, and during 10% deformation, comprcssive strength is 0.39MPa.
Embodiment 4
The preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, fiber felt selects alumina silicate fiber felt, silazane choosing
With hexamethyldisiloxane, zirconium alkoxide selection zirconium-n-butylate, siloxanes selection tetraethyl orthosilicate, alcoholic solvent selects n-butyl alcohol, always
Changing solution is volume ratio dehydrated alcohol: the mixed liquor of tetraethyl orthosilicate=1:4, dry medium is dehydrated alcohol, siloxanes: zirconium alcohol
Mol ratio=the 1:9 of salt, in zirconia-silica complex sol, zirconium alkoxide is 2.0mol/L with the concentration sum of siloxanes.Depend on
Secondary follow the steps below:
(1) preparation of silica-zirconia complex sol
At 20 DEG C, tetraethyl orthosilicate being dissolved in n-butyl alcohol, stirring mixes to obtain 0.2mol/L mixed solution；According to mol
Si:mol HNO3=1:0.12 dropping mass concentration is 65～68% concentrated nitric acid.According to mol Si:mol H2O=1:2 drips steaming
Distilled water, continues stirring 5min and obtains prehydrolysis siloxane solution；According to mol Zr:mol HNO3=1:0.21 is to prehydrolysis siloxanes
Solution dropping concentrated nitric acid, drips zirconium iso-propoxide according to mol Si:mol Zr=1:9 after mix homogeneously, according to mol Zr:mol
H2O=1:2 drips deionized water, continues stirring 5min, obtains clear colloidal sol；
(2) alumina silicate fiber felt and zirconia-silica colloidal sol is compound
By alumina silicate fiber felt under vacuum, impregnated in the zirconia-silica colloidal sol of 2.0mol/L, and keep
Vacuum 60min；
(3) alumina silicate fiber felt is combined the preparation of wet gel
The alumina silicate fiber felt of described impregnant sol is transferred in mould, still aging 20h, obtains alumina silicate fibre
Felt/zirconia-silica is combined wet gel；
(4) alumina silicate fiber felt is combined the aging of wet gel
Alumina silicate fiber felt in step (3) is combined wet gel dehydrated alcohol: tetraethyl orthosilicate volume ratio is the old of 1:4
Change solution to carry out respectively soaking 72h at 70 DEG C；Finally carry out soaking 3 times with dry medium dehydrated alcohol, each soak time
For 12h；
(5) supercritical drying: the gains in step (4) are carried out supercritical drying
Wet gel after aging is loaded autoclave, adds and be dried medium submergence, nitrogen purging 40min, pre-inflated with nitrogen
5MPa；3 DEG C/min is warming up to higher than supercritical temperature 30 DEG C and is incubated 3 hours, with 0.1MPa/min pressure release, pressure release complete after nitrogen
40min is swept in air-blowing.Naturally cool to room temperature, drive still and obtain aeroge/alumina silicate fiber felt heat-barrier material.
(6) hydrophobically modified；
The volume (5) obtained is 14.01cm-1, quality is that 4.44g complex is placed in hermetic container, as it is shown in figure 1,
With the hexamethyldisiloxane steam modification 8h of 0.7g under 150 °, obtain the heat insulation material of superhydrophobic aerogel/alumina silicate fiber felt
Material；
The macro surface of obtained complex is smooth, density 0.317g/m3, thermal conductivity 0.0351W/m K, contact angle
Size is 155 °, and during 10% deformation, comprcssive strength is 0.45MPa.
The present invention proposes the preparation method of a kind of super-hydrophobic high-strength light heat-barrier material, is entered by preferred embodiment
Having gone description, person skilled substantially can be to the techniques described herein side in without departing from present invention, spirit and scope
Method is modified or suitably changes and combine, and realizes the technology of the present invention.Special needs to be pointed out is, all similar replacements
Apparent to those skilled in the art with changing, they are considered as being included in present invention spirit, scope and interior
Rong Zhong.
Claims (10)
1. a preparation method for super-hydrophobic high-strength light heat-barrier material, is characterized in that concretely comprising the following steps:
(1) preparation of silica-zirconia complex sol
In the temperature of 4～40 DEG C, siloxanes is dissolved in alcohol by stirring the alcoholic solution of the siloxanes that dose volume mark is 20%；
Stating then up and dripping mass concentration in alcoholic solution is 65～68% concentrated nitric acid, drips deionized water, continue after stirring 10～20min
Continuous stirring 5～60min, obtains the siloxane solution of prehydrolysis in advance；Mass concentration is dripped to the siloxane solution of prehydrolysis
It is the concentrated nitric acid of 65～68%, drips zirconium alkoxide after mix homogeneously, be stirring evenly and then adding into deionized water；Continue stirring 5-
60min, obtains clear colloidal sol；
(2) mullite fiber felt and zirconia-silica colloidal sol is compound
By fiber felt under vacuum, impregnated in the zirconia-silica colloidal sol of 0.5～1.5mol/L, and keep vacuum
Degree 30min～60min；
(3) mullite fiber felt is combined the preparation of wet gel
Then the fiber felt of described impregnant sol is transferred in mould, still aging 4～24h, obtain fiber felt/zirconium oxide-
Silicon oxide is combined wet gel；
(4) mullite fiber felt is combined the aging of wet gel
Fiber felt in step (3) is combined wet gel aged solution carry out respectively soaking 12～72h at 30～100 DEG C；Finally
Carrying out soaking 2～5 times with the solvent identical with dry medium dehydrated alcohol or isopropanol, each soak time is 3～12h；
(5) supercritical drying
Gains in step (3) are carried out supercritical drying and obtains fiber felt/zirconia-silica composite heat-insulated material；
(6) hydrophobically modified；
The composite heat-insulated material and the silazane solution that step (5) are obtained are placed in hermetic container, are heated to 120 DEG C～180 DEG C
Insulation 2～8h, complex is modified by now silazane formation steam, obtains superhydrophobic aerogel/fiber felt heat-barrier material.
Preparation method the most according to claim 1, is characterized in that: described siloxanes is tetraethyl orthosilicate, tetramethoxy
Silane or MTES；Zirconium alkoxide is zirconium-n-butylate, zirconium-n-propylate or zirconium iso-propoxide.
Preparation method the most according to claim 1, is characterized in that: described fiber felt is mullite fiber felt, zirconium oxide
Fiber felt or alumina silicate fiber felt.
Preparation method the most according to claim 1, is characterized in that: described silazane is hexamethyldisiloxane and 1,3-
Divinyl-1,1,3,3-tetramethyl-disilazane.
Preparation method the most according to claim 1, is characterized in that: described alcohol is ethanol, normal propyl alcohol, isopropanol or positive fourth
Alcohol.
6. according to the preparation method described in right 1, it is characterized in that: described step 1) positive silicon in zirconia-silica complex sol
Acetoacetic ester: the mol ratio=1:0.11～9 of zirconium alkoxide, zirconium alkoxide and the concentration of siloxanes in zirconia-silica complex sol
Sum is 0.25～2.0mol/L.
Preparation method the most according to claim 1, is characterized in that: the preparation of described step (1) prehydrolysis siloxane solution
During siloxanes: water: mol ratio=1:2～3:0.06～0.12 of nitric acid；The preparation of zirconia-silica complex sol
During zirconium alkoxide: water: mol ratio=1:2～4:0.06～0.21 of nitric acid.
Preparation method the most according to claim 1, is characterized in that: the aged solution in step (4) is dehydrated alcohol: just
Silester volume ratio is the mixed liquor of 1:0.25～4.
Preparation method the most according to claim 1, is characterized in that: described dry medium is ethanol or isopropanol.
Preparation method the most according to claim 1, is characterized in that: silazane in step (6): composite heat-insulated material
Mass ratio is 1:5～10.
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Application publication date: 20161207 |
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