CN106809842A - A kind of preparation method of high temperature oxidation resisting Silica Aerogels - Google Patents
A kind of preparation method of high temperature oxidation resisting Silica Aerogels Download PDFInfo
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- CN106809842A CN106809842A CN201510857626.9A CN201510857626A CN106809842A CN 106809842 A CN106809842 A CN 106809842A CN 201510857626 A CN201510857626 A CN 201510857626A CN 106809842 A CN106809842 A CN 106809842A
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Abstract
The present invention proposes a kind of preparation method of high temperature oxidation resisting Silica Aerogels, is prepared by colloidal sol, is gelled and aging, hydro-thermal process, solvent displacement and supercritical drying, obtains high temperature oxidation resisting Silica Aerogels.The present invention carries out hydro-thermal process to wet gel, and in water-heat process, gel network is further perfect, gel particle particle diameter increases to more than 20nm by 10~15nm, it is tightly combined between particle, therefore reduces the surface energy of aeroge nano particle, aeroge temperature tolerance is significantly improved.
Description
Technical field
The present invention relates to a kind of preparation method of high temperature oxidation resisting Silica Aerogels, belong to aeroge technology of preparing
Field.
Background technology
Aeroge is that a kind of nano-porous materials for being formed mutually are built up by nano particle, with lower thermal conductivity, height
Specific surface area, the typical feature of low-density, especially its nanometer of skeleton and nano-porous structure significantly limit solid
Phase heat transfer, gaseous exchange heat transfer and gas phase heat transfer, make it have splendid heat-proof quality, therefore in boat
Its aviation field receives extensive concern.As space flight and aviation technology develops, vehicle flight speeds are stepped up,
Demand is proposed to high temperature resistant heat insulation material.
At present in terms of aerogel material, what is studied and be most widely used is silica aerogel and aluminum oxide gas
Gel.Pure silica aeroge temperature tolerance is generally acknowledged no more than 650 DEG C, is sintered more than 650 DEG C, Kong Jie
Structure is collapsed, and appearance and size is substantially shunk heat-proof quality simultaneously and declined.Pure alumina aeroge turns due to high temperature crystal formation
Complicate, heat resistance is also limited, United States Patent (USP) US 6620458B2 are using low metering than water and overcritical first
Alcohol is dried and is prepared for Low-density high temperature resistant alumina aerogels material, and 1050 DEG C/4h linear shrinkage ratios are less than 2%.
Patent CN 1724354A《A kind of method for improving thermal stability of silicon dioxide deroyel》By in oxidation
Adulterate Fe in silica aerogel2O3Nano particle improves its stability, aeroge specific surface after 1000 DEG C of heat treatments
Product is by 1.3712m2/ g is improved to 148.0979m2/ g, heat treatment time and linear shrinkage ratio are not referred to.Patent
CN201010300112.0《The preparation method of heat-resisting alumina-silox aerogel thermal-protective composite material》It is logical
Mixing silica sol and alumina sol, and the compound fibrofelt containing SiC coatings are crossed, high temperature resistant is prepared
Aluminium oxide-silicon oxide aerogel composite, still has porosity and specific surface area higher under the conditions of 1200 DEG C.
Patent CN201310276044.2《A kind of preparation method of high temperature-resistanalumina alumina aerogel material》Using original position
Generation water law prepares alumina sol, silicon source is introduced in supercritical drying process, and used after high-temperature process
The treatment of HMDS atmosphere, makes silica coated aluminum oxide particle, suppresses the growth of alpha-alumina crystals,
Linear shrinkage ratio is 5% after 1200 DEG C for the treatment of 2h.
In terms of silica/alumina aerogel material heat resistance is improved, current main method is for doping or draws
Enter other colloidal sols and prepare binary aerogel, the macroshrinkage of aeroge is mainly resisted in doping by the particle that adulterates, because
This does not improve the temperature tolerance of aeroge substantially；Binary aerogel preparation technology is complicated, and its properity is difficult
With precise control, and due to there is complicated crystal transfer process under alumina high temperature, though macro manifestations go out compared with
Also there are significant changes in small high-temperature shrinkage rate, its specific surface area, pore volume, aperture etc., and then show heat-insulated
The decline of performance.There is no crystal transfer and pure silica aeroge preparation technology is relatively easy, and under high temperature,
The microstructure of stabilization can be kept, therefore, prepare the pure silica of high temperature tolerance (heatproof is more than 1000 DEG C)
Aeroge is the new approaches for improving aeroge heat resistance.
The content of the invention
It is an object of the invention to overcome prior art not enough, there is provided a kind of preparation process is simple, temperature tolerance show
Write and improve (after 1200 DEG C for the treatment of 0.5h, the preparation method of the silica aerogel materials of linear shrinkage ratio≤10%).
Technical solution of the invention：A kind of preparation method of high temperature oxidation resisting Silica Aerogels, including with
Lower step：
It is prepared by the first step, colloidal sol,
With silica hydrosol as silicon source, acid and base catalyst is separately added into order, be sufficiently stirred for
It is even, obtain colloidal sol；This step prepares conventional process means to prepare aeroge.
Silica hydrosol uses the silica hydrosol of commercially available high-purity, wherein sodium ions content to be less than
50ppm, solid content 10%~25%.Acidic catalyst is hydrochloric acid, hydrofluoric acid, nitric acid etc.；Base catalyst
It is ammoniacal liquor, ammonium fluoride etc..Silica hydrosol, acidic catalyst and base catalyst mass ratio are 1：
0.005~0.04：0.01~0.05, matched also dependent on adjustment is actually needed.
The present invention is in order to be able to the further temperature tolerance for improving silica aerogel, the two of 10~15nm of preferable particle size
Silica hydrogel is silicon source, can reduce the specific surface energy of sol particles, is favorably improved aeroge temperature tolerance.
Second step, gelling with it is aging,
The colloidal sol that the first step is obtained closed container under the conditions of 20~50 DEG C places 4~96h, and colloidal sol occurs
Gelling, be then placed in again in 20~50 DEG C of environment carry out it is aging, standing time be 8~96h, make gel reaction
Further carry out.This step prepares conventional process means to prepare aeroge, can use above-mentioned technique, also can root
Selected according to actual conditions.
3rd step, hydro-thermal process,
By through second step gelling with it is aging after wet gel be totally submerged in deionized water, at room temperature soak >=3
After it, deionized water is warming up to 150 DEG C~250 DEG C, hydro-thermal process >=24h is naturally cooling to normal temperature；
Wet gel will ensure to be totally submerged in deionized water in whole hydrothermal treatment process, it is to avoid gel structure is destroyed.
This step can be carried out in hydrothermal reaction kettle, can also be carried out in the container that other can heat water, as long as energy
Meet above-mentioned immersion and temperature requirement.In order to ensure that wet gel is complete in soaking at room temperature and hydrothermal treatment process
In deionized water, wet gel height will typically be less than the 1/3 of hydrothermal reaction kettle height for full submergence, add certain
The deionized water of amount, in order to ensure that wet gel is totally submerged in deionized water in a heated condition, in reactor
The compactedness of deionized water is 60%~90%, it is to avoid gel structure is destroyed.
Wet gel first immersion a period of time at room temperature, is in order that in the new deionized water for adding and wet gel
Liquid reaches diffusion balance, ensures that inside and outside liquid properties are homogeneous during hydro-thermal process.If soak time is too short, go from
Liquid in sub- water and wet gel does not reach the requirement of diffusion balance, if soak time is oversize, deionized water with it is wet
Liquid in gel has reached diffusion balance, loses time, and extends the production cycle；Therefore, soak time one
As be 3~5 days.
The present invention carries out hydro-thermal process to wet gel, and in water-heat process, gel network is further perfect, gel
Grain diameter increases to more than 20nm by 10-15nm, is tightly combined between particle, therefore reduces aeroge
The surface energy of nano particle, aeroge temperature tolerance is significantly improved.
Found in practical study work, under the same conditions, improving hydro-thermal process temperature can improve aeroge
Grain particle diameter, and then improve the temperature tolerance of aeroge, hydro-thermal process is improved to changing more bright after 150 DEG C by room temperature
It is aobvious, but after hydro-thermal process temperature is higher than 250 DEG C, the vapour pressure of water is changed significantly with the raising of temperature, to equipment
Resistance to pressure requirement is higher, while the DeGrain to improving heat resistance, therefore hydro-thermal process optimum temperature
Scope is 150~250 DEG C.At a temperature of a certain hydro-thermal process of the same terms, aerogel particle particle diameter is with treatment
The extension of time and increase, balance is can reach in general 24h, i.e., extend the specific surface of process time aeroge again
Also there is no significant change, therefore, the time of hydro-thermal process cannot be below 24h.
4th step, solvent displacement,
The wet gel of the 3rd step hydro-thermal process is carried out into solvent displacement, this step is that aeroge prepares conventional process hand
Section, can use following steps, be selected also dependent on actual conditions.
During the wet gel of hydro-thermal process is placed in into alcoholic solvent or ketone solvent, replace 2 times, water content is less than 1%
(mass ratio).Alcoholic solvent is the combination of one or two and the above in methyl alcohol, ethanol, propyl alcohol, isopropanol,
Ketone solvent is butanone and/or acetone.
5th step, supercritical drying,
Wet gel after 4th step solvent is replaced carries out supercritical drying treatment, and this step is that aeroge is prepared often
With process meanses, following steps can be used, be selected also dependent on actual conditions.
Wet gel after solvent is replaced carries out supercritical drying treatment, and supercritical fluid drying condition is：Dry
Medium is carbon dioxide, and wet gel is put into supercritical fluid drying equipment, the dioxy of 2~4MPa of preliminary filling
Change carbon, while supercritical fluid drying equipment is warming up to 50 DEG C, continue to be pressurized to 10~15MPa, pressurize bar
The alcoholic solvent or ketone solvent in wet gel are brought into separating still under part with 10~100 ls/h of flow to be divided
From；After alcoholic solvent or ketone solvent are separated completely, then pressure was slowly discharged with the speed of 1~6MPa/ hours, directly
Balanced to external atmosphere pressure, finally taken out, obtain high temperature oxidation resisting Silica Aerogels.
Present invention beneficial effect compared with prior art：
(1) present invention carries out hydro-thermal process to wet gel, and in water-heat process, gel network is further perfect,
Gel particle particle diameter increases to more than 20nm by 10~15nm, is tightly combined between particle, therefore reduces
The surface energy of aeroge nano particle, aeroge temperature tolerance is significantly improved；
(2) present invention carries out soaking at room temperature before hydro-thermal process to wet gel, make the deionized water of new addition with
Liquid in wet gel reaches diffusion balance, it is ensured that in hydro-thermal process, inside and outside liquid properties are homogeneous；
(3) it is silicon source that the present invention uses the silica hydrosol of 10~15nm of particle diameter, significantly reduces airsetting
The surface of glue nano particle can, be favorably improved its temperature tolerance, and methyl silicate commonly used in the prior art,
The aerosol particle size of the silicon sources such as tetraethyl orthosilicate generation is general in 5~10nm；
(4) preparation process is simple of the present invention, technological parameter is easily-controllable, and whole preparation process can be set using conventional
It is standby；
(5) 0.1~0.25g/cm of high temperature oxidation resisting Silica Aerogels density prepared by the present invention3, specific surface area
It is different according to hydrothermal conditions, it is 140~230m2/ g, after 1200 DEG C for the treatment of 0.5h, specific surface area change
In the range of measurement error, linear shrinkage ratio is 2%~10%.
Figure of description
Fig. 1 is preparation flow figure of the present invention；
Fig. 2 is comparative example 1 to be provided without hydro-thermal process of the present invention (remaining process conditions is consistent with embodiment 1)
Transmission electron microscope photo before and after the silica aerogel heat treatment of preparation, (a) is not thermally treated aeroge,
B () is 1200 DEG C of aeroges of high-temperature process 0.5h；
Fig. 3 is the transmission electron microscope photo before and after the embodiment of the present invention 1 prepares silica aerogel heat treatment, (a)
It is not thermally treated aeroge, (b) is 1200 DEG C of aeroges of high-temperature process 0.5h.
Specific embodiment
Below in conjunction with accompanying drawing and instantiation, the present invention is described in detail.
The present invention as shown in figure 1, it be silicon source to use silica hydrosol, after addition catalyst gel, will be wet
Gel carries out hydro-thermal process, and high temperature oxidation resisting Silica Aerogels are obtained after supercritical drying.Due in hydro-thermal
During, gel network is further perfect, and gel particle particle diameter becomes big, therefore reduces aeroge nano particle
Surface can, aeroge temperature tolerance is significantly improved.
Embodiment 1
(1) by the silica hydrosol of 25% solid content, hydrochloric acid, ammonium fluoride in mass ratio 1: 0.01:
0.02 mixing, is made into colloidal sol.(2) colloidal sol is placed into 4h under the conditions of 20 DEG C, colloidal sol is gelled, then
Being placed in again in 20 DEG C of environment carries out aging, and standing time is 24h.(3) the wet gel transfer for obtaining second step
Into hydrothermal reaction kettle, wet gel is highly the 1/4 of hydrothermal reaction kettle, adds a certain amount of deionized water, is filled out
Degree of filling is 80%, is warming up to 180 DEG C, hydro-thermal process 24h.Hydrothermal reaction kettle is naturally cooling to normal temperature, takes out
Sample.(4) wet gel is placed in ethanol, is replaced 2 times, water content is less than 1% (mass ratio).(5)
Wet gel is put into supercritical fluid drying equipment, the carbon dioxide of preliminary filling 3MPa, while supercritical fluid
Drying equipment is warming up to 50 DEG C, continues to be pressurized to 15MPa, will with 10 ls/h of flow under dwell condition
Solvent in wet gel is brought separating still into and is separated；After alcoholic solvent or ketone solvent are separated completely, then with 2MPa/
The speed of hour slowly discharges pressure, until being balanced with external atmosphere pressure, finally takes out, and obtains high temperature oxidation resisting
Silica Aerogels.
High temperature oxidation resisting Silica Aerogels density 0.25g/cm prepared by the present invention3, specific surface area is 196m2/ g,
After 1200 DEG C for the treatment of 0.5h, specific surface area is 189m2/ g, linear shrinkage ratio is 5%.
Table 1 is the embodiment 2~4 for changing hydro-thermal process temperature, remaining condition such as embodiment 1.
Comparative example
Silica aerogel is prepared using prior art, in addition to hydrothermal treatment step of the invention is provided without, remaining
Consistent with embodiment 1, specific performance is prepared and is shown in Table 1.
Table 1
According to table 1 it can be seen that under the same terms, improving hydro-thermal process temperature, specific surface area reduction, linear shrinkage
Rate reduction, heat resistance increases.
From Fig. 2 (a, b) and Fig. 3 (a, b) as can be seen that the silica aerogel of comparative example preparation is 1200
Aerogel particle particle diameter is significantly increased after DEG C high-temperature process 0.5h, illustrates that aerogel particle is sintered, airsetting
Glue microstructure changes, and silica aerogel prepared by embodiment 1 gas after 1200 DEG C of high-temperature process
There is no significant change in gel particle particle diameter, illustrate there is good temperature tolerance, and microstructure keeps not under high temperature
Become.
Embodiment 5
(1) by the silica hydrosol of 10% solid content, nitric acid, ammoniacal liquor in mass ratio 1: 0.03: 0.03
Mixing, is made into colloidal sol.(2) colloidal sol is placed into 8h under the conditions of 40 DEG C, colloidal sol is gelled, and then puts again
Carried out in 20 DEG C of environment aging, standing time is 48h.(3) wet gel that second step is obtained is transferred to water
In thermal response kettle, wet gel is highly the 1/3 of hydrothermal reaction kettle, adds a certain amount of deionized water, compactedness
It is 60%, is warming up to 150 DEG C, hydro-thermal process 24h.Hydrothermal reaction kettle is naturally cooling to normal temperature, takes out sample.
(4) wet gel is placed in acetone, is replaced 2 times, water content is less than 1% (mass ratio).(5) will be wet
Gel is put into supercritical fluid drying equipment, the carbon dioxide of preliminary filling 2MPa, while supercritical fluid drying
Equipment is warming up to 50 DEG C, continues to be pressurized to 10MPa, will be wet solidifying with 50 ls/h of flow under dwell condition
Solvent in glue is brought separating still into and is separated；After alcoholic solvent or ketone solvent are separated completely, then with 4MPa/ hours
Speed slowly discharge pressure, until with external atmosphere pressure balance, finally take out, obtain high temperature oxidation resisting silicon gas
Gel rubber material.
High temperature oxidation resisting Silica Aerogels density 0.10g/cm prepared by the present invention3, specific surface area is 228m2/ g,
After 1200 DEG C for the treatment of 0.5h, specific surface area is 201m2/ g, linear shrinkage ratio is 10%.
Embodiment 6
(1) by the silica hydrosol of 20% solid content, nitric acid, ammonium fluoride in mass ratio 1: 0.005:
0.04 mixing, is made into colloidal sol.(2) colloidal sol is placed into 4h under the conditions of 50 DEG C, colloidal sol is gelled, then
Being placed in again in 50 DEG C of environment carries out aging, and standing time is 8h.(3) the wet gel transfer for obtaining second step
Into hydrothermal reaction kettle, wet gel is highly the 1/5 of hydrothermal reaction kettle, adds a certain amount of deionized water, is filled out
Degree of filling is 70%, is warming up to 250 DEG C, hydro-thermal process 24h.Hydrothermal reaction kettle is naturally cooling to normal temperature, takes out
Sample.(4) wet gel is placed in methyl alcohol, is replaced 2 times, water content is less than 1% (mass ratio).(5)
Wet gel is put into supercritical fluid drying equipment, the carbon dioxide of preliminary filling 4MPa, while supercritical fluid
Drying equipment is warming up to 50 DEG C, continues to be pressurized to 12MPa, will with 80 ls/h of flow under dwell condition
Solvent in wet gel is brought separating still into and is separated；After alcoholic solvent or ketone solvent are separated completely, then with 6MPa/
The speed of hour slowly discharges pressure, until being balanced with external atmosphere pressure, finally takes out, and obtains high temperature oxidation resisting
Silica Aerogels.
High temperature oxidation resisting Silica Aerogels density 0.20g/cm prepared by the present invention3, specific surface area is 153m2/ g,
After 1200 DEG C for the treatment of 0.5h, specific surface area is 148m2/ g, linear shrinkage ratio is 2%.
Embodiment 7
(1) by the silica hydrosol of 15% solid content, hydrofluoric acid, ammoniacal liquor in mass ratio 1: 0.01:
0.03 mixing, is made into colloidal sol.(2) colloidal sol is placed into 12h under the conditions of 20 DEG C, colloidal sol is gelled, then
Being placed in again in 20 DEG C of environment carries out aging, and standing time is 96h.(3) the wet gel transfer for obtaining second step
Into hydrothermal reaction kettle, wet gel is highly the 1/3 of hydrothermal reaction kettle, adds a certain amount of deionized water, is filled out
Degree of filling is 90%, is warming up to 220 DEG C, hydro-thermal process 24h.Hydrothermal reaction kettle is naturally cooling to normal temperature, takes out
Sample.(4) wet gel is placed in butanone, is replaced 2 times, water content is less than 1% (mass ratio).(5)
Wet gel is put into supercritical fluid drying equipment, the carbon dioxide of preliminary filling 3MPa, while supercritical fluid
Drying equipment is warming up to 50 DEG C, continues to be pressurized to 15MPa, will with 20 ls/h of flow under dwell condition
Solvent in wet gel is brought separating still into and is separated；After alcoholic solvent or ketone solvent are separated completely, then with 1MPa/
The speed of hour slowly discharges pressure, until being balanced with external atmosphere pressure, finally takes out, and obtains high temperature oxidation resisting
Silica Aerogels.
High temperature oxidation resisting Silica Aerogels density 0.15g/cm prepared by the present invention3, specific surface area is 176m2/ g,
After 1200 DEG C for the treatment of 0.5h, specific surface area is 165m2/ g, linear shrinkage ratio is 6%.
Unspecified part of the present invention is known to the skilled person technology.
Claims (4)
1. a kind of preparation method of high temperature oxidation resisting Silica Aerogels, it is characterised in that comprise the following steps：
It is prepared by colloidal sol；
Gelling with it is aging；
Hydro-thermal process,
By the wet gel through gel after aging in 150 DEG C~250 DEG C deionized waters, hydro-thermal process >=24h, from
Room temperature so is cooled to, wet gel will ensure to be totally submerged in deionized water in whole hydrothermal treatment process；
Solvent is replaced；With
Supercritical drying, obtains high temperature oxidation resisting Silica Aerogels.
2. the preparation method of a kind of high temperature oxidation resisting Silica Aerogels according to claim 1, it is special
Levy and be：Before the hydro-thermal process, by through be gelled with it is aging after wet gel be totally submerged in deionized water,
Soak >=3 days at room temperature.
3. the preparation method of a kind of high temperature oxidation resisting Silica Aerogels according to claim 2, it is special
Levy and be：The described soaking at room temperature time is 3~5 days.
4. the preparation method of a kind of high temperature oxidation resisting Silica Aerogels according to claim 1, it is special
Levy and be：Silicon source uses silica hydrosol, 10~15nm of aerosol particle size in prepared by the colloidal sol.
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| CN108249901A (en) * | 2018-01-24 | 2018-07-06 | 航天特种材料及工艺技术研究所 | A kind of preparation method of high temperature resistant aeroge material |
| CN108955096A (en) * | 2018-05-22 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of method that supercritical carbon dioxide is dry |
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| CN112624130A (en) * | 2020-12-30 | 2021-04-09 | 中国科学技术大学 | Method for preparing silicon dioxide aerogel based on hydrothermal method, product and application thereof |
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| CN113956044A (en) * | 2021-11-28 | 2022-01-21 | 天津大学 | Preparation method of SiOC aerogel with high compressive strength |
| CN117819580A (en) * | 2024-03-05 | 2024-04-05 | 湖南荣岚智能科技有限公司 | High-temperature-resistant alumina aerogel and preparation method thereof |
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