CN108455997A - A kind of Al2O3-SiO2System high-performance nano cellular insulant and preparation method - Google Patents
A kind of Al2O3-SiO2System high-performance nano cellular insulant and preparation method Download PDFInfo
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- CN108455997A CN108455997A CN201810083570.XA CN201810083570A CN108455997A CN 108455997 A CN108455997 A CN 108455997A CN 201810083570 A CN201810083570 A CN 201810083570A CN 108455997 A CN108455997 A CN 108455997A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- 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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Abstract
The present invention relates to a kind of Al2O3‑SiO2The preparation method of system high-performance nano cellular insulant improves intergranular connection by composite inorganic fiber combination doped microcrystalline whisker reinforcement microstructure；Sample is made to have good hydrophobicity, flexibility, decorative surface by multiple surface treatment procedure.Has the honest and clean feature of simple process and low cost, material has high-strength, low-density, low thermal conductivity, high temperature resistant and excellent high temperature insulating performance, and another surface smoothness is high, and impulse- free robustness is without picking.This method reaches its high performance nature using a variety of innovative technologies.By Dispersing Technology activated particle surface growing point, the combination of binary system is improved.
Description
Technical field
The present invention relates to a kind of Al2O3-SiO2The preparation method of system high-performance nano cellular insulant, belongs to inorganic
Thermal insulation material application field.
Background technology
With the continuous development of scientific and technological industry, new diseases be it is with rapid changepl. never-ending changes and improvements, it is glittering one, heat-insulating material field
Nova obtained the enterprise of every field and consumer is favored, she is exactly aeroge.Aeroge is with its unique preparation side
Formula（Sol-gal process）Her unique structure feature, nanoporous are cast.Nanoporous aerogel, which has, is substantially better than biography
System porous insulation material, and silica aerogel, with its excellent anti-flammability, the stability of structure, lower production cost, which becomes, works as
The main force of preceding heat insulating material.However pure silicon aeroge system limits its development there is also some defects and grows,
Mainly its high temperature resistance is also limited, only under the conditions of less than 450 DEG C can relatively stable use without influencing its performance；Separately
Outside since autologous density is low, brittleness is big, so the silica aerogel felt pan surface prepared is easy phenomena such as burr plays ash picking.
The two big defects i.e. heat-resisting quantity and picking that the present invention considers current silica aerogel is made by process optimization
It obtains this two large problems to significantly improve, first using introducing compound phase aluminium phase, and grinding technics activation is combined to mix aluminium phase table
Face activity so that the smooth formation of-Si-O-Al- keys in gel process, and be uniformly distributed, form uniform, the guarantor of macroscopically structure
Hinder the high-temperature stability of structure.The another crystallite whisker that introduces is effectively improved the linking between the aerogel particle to be formed, and binding fiber increases
By force, the intensity of its structure is further strengthened, then modification liquid 2 is surface-treated to improve its surface texture by self-control, forms multilayer
Secondary enhancement measures solve dusting problems.
It is no lack of Al by looking into the current aeroge research of new discovery or disclosed patent2O3-SiO2Compound system improves resistance to height
Warm nature, be to use compound primary gas gel rubber system, that is to say, that is by introducing the sources Al colloidal sol, that is to say, that be with high
The alkoxide of expensive Al, inorganic salts Al (NO3)3Deng, corresponding chelating agent such as acetylacetone,2,4-pentanedione or propylene oxide etc. are also used, it is this
Technique is in addition to relative cost is high, and preparation control difficulty is larger, and collosol stability is poor, and industrial production realizes that difficulty is big, currently not yet
See that being useful for industrial related process appears in the newspapers.
Invention content
Fiber-reinforcement silicon dioxide aerogel is the relatively conventional preparation process of industrial circle, however is changed by crystallite whisker
Kind silica aerogel microstructure is there is not yet open report.
The present invention is the Al reached not less than product characteristic in the prior art2O3-SiO2System high-performance nano porous insulation
Material provides a kind of at low cost, simple for process, high preparation method of stability, and obtaining sample has thermal coefficient low, high temperature resistant
The strong feature of property.
The technical solution adopted by the present invention includes the following steps：
A kind of preparation method of Al2O3-SiO2 systems high-performance nano cellular insulant, includes the following steps：
1）It is in molar ratio by silicon source（0.01~1）It is added in organic solvent, is added a certain amount of water, water and organic solvent
Molar ratio is（0.2~0.6）：1.A certain amount of acid for adjusting pH value is added to 1~5, room temperature to 60 DEG C of reaction hydrolysis 1~
After for 24 hours, a certain amount of alkali is added and adjusts pH value to 7~9, is stood after stirring evenly, it is spare；
2）By step 1）In reserve liquid be transferred to ball grinder, and aluminium phase is added, the molar ratio of the aluminium phase and SiO2 is 0.1~
10：1；Crystallite whisker is added, it is 0.1%~10% that the crystallite whisker, which accounts for the SiO2 mass percents,；Ball-milling Time is 10
~60 minutes；
3）At high temperature by fiber felt pan（300~700 DEG C）Lower processing 2~10h, it is spare；
4）It learns from else's experience step 3）In treated that the glass fiber mat is transferred to step（2）Obtained pre- solidifying hydrolyzate fully soaks
It is taken out after profit, is placed in closing saturation alcohol vapour room and stands gel, be transferred in ethyl alcohol at 20~70 DEG C and be aged 1~7 day after gel,
Period washs displacement 2~10 times with ethyl alcohol repeatedly；
5）It will（4）Obtained wet gel block is transferred to mass percent containing N3390 0.05~0.5%, and ethanol solution is placed in 60 DEG C of bakings
Case is modified 12h；It is transferred to the petroleum ether solution of the mass percents of 1-10% containing trim,ethylchlorosilane, modified 5h again；
6）It is dry after then taking out, obtain Al2O3-SiO2System high-performance nano cellular insulant.
Further, the silicon source is the mixture of a kind of siloxanes containing alkyl or a variety of siloxanes containing alkyl.
Further, the organic solvent is the lower alcohols such as propyl alcohol, ethyl alcohol, methanol, organic solvent and silicon source molar ratio
For（1~20）：1.
Further, the aluminium includes mainly mutually α phases and γ phases Al2O3, Al (OH)3And the bauxite of high alumina, kaolin or
The powder of metakaolin, aluminium phase crosses 200 mesh sieve extracting screen underflow.
Further, Al is added2O3:SiO2=0.1~1：1, and accelerate dispersion using ball milling；Ball-milling Time is 10~30 points
Clock.
Further, the fiber felt pan is glass fibre, ceramic fibre, a kind of high-temperature fibre material in alumina silicate fibre
Material is made；The whisker is hydrated calcium sulfate, hydrated calcium silicate, calcium carbonate, zinc oxide, one or more groups in silicon carbide
It closes, whisker accounts for the SiO2Mass percent be 0.1%~1%.
Further, the time of the gel is half an hour.
Further, first modification liquid is trim,ethylchlorosilane and n-hexane mixed liquor or hexamethyldisilazane；Institute
It is inorganic nano lotion to state the second modification liquid, there is Al2O3, SiO2, MgO, CaO are modified for surface.
Further, after modified, processing is dried using constant pressure and dry technique in aging wet gel, and drying time is 2~
24 hours.
Further, the modified liquid of aging wet gel is modified, is dried through supercritical carbon dioxide.
The present invention improves silica aerogel microstructure by crystallite whisker；Have the honest and clean feature of simple process and low cost, material
Material has high-strength, low-density, low thermal conductivity, high temperature resistant and excellent high temperature insulating performance, and another surface smoothness is high, impulse- free robustness
Without picking.This method reaches its high performance nature using a variety of innovative technologies.Pass through Dispersing Technology activated particle surface
Growing point improves the combination of binary system；It is carried by composite inorganic fiber combination doped microcrystalline whisker reinforcement microstructure
High intergranular connection；Sample is made to have good hydrophobicity, flexibility, incrustation by multiple surface treatment procedure
Property.
Description of the drawings
Fig. 1 is 1 comprehensive silicon aeroge felt pan of example；
Fig. 2 is 2 comprehensive silicon aeroge felt pan of example.
Specific implementation mode
The present invention is made a more thorough explanation below with embodiment.The present invention can be presented as a variety of different forms,
It should not be construed as limited to the exemplary embodiments described herein.
Embodiment 1
High-performance nano cellular insulant preparation process in the present embodiment is as follows：
（1）Take a certain amount of ethyl orthosilicate（TEOS）For silicon source, sequentially add a certain amount of absolute ethyl alcohol (EtOH) and go from
Sub- water；Molar ratio is TEOS:EtOH:H2O=1:10:6, add acid for adjusting pH value to 3.0, at 60 DEG C after reaction hydrolysis 36h, is added
A certain amount of alkali adjusts pH value to 8.0, is stood after stirring evenly, spare.
（2）It is transferred to ball grinder, and alumina powder is added, alumina powder and SiO2Molar ratio be 0.2：1, when ball milling
Between be 20 minutes.
（3）Glass fiber mat is taken to be transferred to step（2）Obtained pre- solidifying hydrolyzate takes out after fully infiltrating, and it is full to be placed in closing
Gel is stood with alcohol vapour room, is transferred in ethyl alcohol after gel and is aged 12h at 70 DEG C, during which wash displacement 5 times with ethyl alcohol repeatedly.
（4）By step（3）Obtained wet gel block is transferred to the ethanol solution of mass percent containing N3390 0.2%, modified
12h；It is transferred to the petroleum ether solution that mass percent containing trimethylchloro-silicane is 10%, modified 5h again.
（5）It is dry after then taking out, obtain Al2O3-SiO2System high-performance nano cellular insulant.
It is 0.2% to measure picking rate；Measure thermal coefficient, 25 DEG C of thermal coefficient λ=0.01875W/m.K；Mean temperature is
The W/m.K of λ=0.03216 at 240 DEG C；By test block through 700 DEG C of high-temperature process 12h, dimensional contraction 3.5%.12h are handled through 900 DEG C,
Shrinking percentage 14.7%.
Embodiment 2
（1）Take a certain amount of ethyl orthosilicate（TEOS）For silicon source, a certain amount of absolute ethyl alcohol (EtOH), deionization are sequentially added
Water；（Molar ratio TEOS:EtOH:H2O=1:10:6）, add acid for adjusting pH value to 3.0, at 60 DEG C after reaction hydrolysis 36h, be added one
Quantitative alkali adjusts pH value to 8.0, is stood after stirring evenly, spare；
（2）It is transferred to ball grinder, and alumina powder is added, accounts for SiO2Molar ratio be 0.2；Crystallite whisker is added, SiO is accounted for2
Mass percent 20%；Ball-milling Time is 20 minutes.
（3）Glass fiber mat is taken to be transferred to step（2）Obtained pre- solidifying hydrolyzate takes out after fully infiltrating, and it is full to be placed in closing
Gel is stood with alcohol vapour room, is transferred in ethyl alcohol after gel and is aged 12h at 70 DEG C, during which wash displacement 5 times with ethyl alcohol repeatedly.
（4）It will（3）Obtained wet gel block is transferred to mass percent containing N3390 0.2%, and ethanol solution is placed in 60 DEG C of bakings
Case, modified 12h；It is transferred to the petroleum ether solution of 10% mass percent containing trimethylchloro-silicane, modified 5h again.
（5）It is dry after then taking out, obtain Al2O3-SiO2System high-performance nano cellular insulant.
It is 0.05% to measure picking rate, and picking rate is substantially better than conventional aerogel powder, is primarily due to crystallite whisker
The space structure for further enhancing matrix is added；Measure thermal coefficient, room temperature thermal coefficient λ（25℃）=0.01955 W/
m.K；The W/m.K of λ=0.03025 when mean temperature is 240 DEG C；By test block through 700 DEG C of high-temperature process 12h, dimensional contraction is less than
1.2%, through 900 DEG C of processing 12h, shrinking percentage 10.9%.Equally there is certain help to its thermal stability after introducing crystallite whisker.
Fig. 2 show the sample appearance prepared by example 2, and the sample surfaces character is smooth bright and clean, the nothing in dither process
Common silica aerogel felt pan significantly loses powder phenomenon.
Embodiment 3
（1）Take a certain amount of ethyl orthosilicate（TEOS）For silicon source, a certain amount of absolute ethyl alcohol (EtOH), deionization are sequentially added
Water（Molar ratio TEOS:EtOH:H2O=1:10:6）, add acid for adjusting pH value to 3.0, at 60 DEG C after reaction hydrolysis 36h, be added certain
The alkali of amount adjusts pH value to 8.0, is stood after stirring evenly, spare；
（2）It is transferred to ball grinder, and alumina powder is added, accounts for SiO2Molar ratio be 0.2, Ball-milling Time be 20 minutes；Again plus
Enter calcium sulfate crystallite whisker, accounts for SiO2Mass percent is 20%；Ball-milling Time is 20 minutes.
（3）Take pending glass fiber mat at high temperature（600℃）Lower processing 4h, it is spare；
（4）Take step (3) treated that fiber felt pan is transferred to step（2）Obtained pre- solidifying hydrolyzate takes out after fully infiltrating, and sets
Gel is stood in closing saturation alcohol vapour room, is transferred in ethyl alcohol at 70 DEG C and is aged 1 day after gel, during which washed repeatedly with ethyl alcohol
Displacement 5 times.
（5）By step（3）Obtained wet gel block is transferred to mass percent containing N3390 0.2%, ethanol solution, modified 12h；
It is transferred to the petroleum ether solution of 10% mass percent containing trimethylchloro-silicane, modified 5h again.
（6）It is dry after then taking out, obtain Al2O3-SiO2System high-performance nano cellular insulant.
It is 0.04% to measure picking rate；Measure thermal coefficient, room temperature thermal coefficient λ（25℃）=0.01856W/m.K；It is average
The W/m.K of λ=0.03116 when temperature is 240 DEG C；By test block through 700 DEG C of high-temperature process 12h, dimensional contraction 2.9%.At 900 DEG C
Manage 12h, shrinking percentage 13.8%.
Parameter in embodiment is optimized parameter；The present invention is not limited to the optimized parameters.Wherein, silicon source can suitably increase
Subtract, should control in molar ratio TEOS:EtOH is in (0.1~10):Between 1.The molar ratio of organic solvent and water should be controlled 1:
（0.2~0.6）Between；Aluminium phase and the molar ratio adjustable range of SiO2 are（0.1~10）：1；Other technological parameters can also be appropriate
Adjustment.
The present invention is by being added high-temperature stable mutually as alumina powder improves the high temperature resistance of aeroge；Pass through N3390
Surface modification is carried out, picking rate is reduced；High-temperature stability and structural stability are further enhanced by the way that crystallite whisker is added so that
Picking rate further decreases；On the one hand improve glass surface characteristic by the heat treatment to former glass felt pan base material, further changes
Kind picking phenomenon, while also having certain help to thermal stability.
The sample finally obtained has excellent heat-proof quality, keeps extremely low picking characteristic, and its thermal stability has
It is obviously improved, be the applications expanding of aeroge wider application market.The simple process and low cost is honest and clean, reproducibility
It is good, it is easy to control, there is great economic value and market application value.
Above-mentioned example is only intended to illustrate the present invention, and in addition to this, also there are many different embodiments, and these are implemented
Mode be all those skilled in the art after comprehension inventive concept it is also envisioned that therefore, will not enumerate herein.
Claims (9)
1. a kind of Al2O3-SiO2The preparation method of system high-performance nano cellular insulant, which is characterized in that including following step
Suddenly：
1）It is in molar ratio by silicon source（0.01~1）It is added in organic solvent, addition water, the molar ratio of water and organic solvent is
（0.2~0.6）：1；A certain amount of acid for adjusting pH value is added to 1~5, after room temperature to 60 DEG C of reaction hydrolysis 1~for 24 hours, is added
A certain amount of alkali adjusts pH value to 7~9, is stood after stirring evenly, spare；
2）By step 1）In reserve liquid be transferred to ball grinder, and aluminium phase is added, the aluminium phase and SiO2Molar ratio be 0.1~10：
1；Crystallite whisker is added, the crystallite whisker accounts for the SiO2Mass percent is 0.1%~10%；Ball-milling Time is 10~60
Minute；
3）At high temperature by fiber felt pan（300~700 DEG C）Lower processing 2~10h, it is spare；
4）It learns from else's experience step 3）In treated that the glass fiber mat is transferred to step（2）Obtained pre- solidifying hydrolyzate fully soaks
It is taken out after profit, is placed in closing saturation alcohol vapour room and stands gel, be transferred in ethyl alcohol at 20~70 DEG C and be aged 1~7 day after gel,
Period washs displacement 2~10 times with ethyl alcohol repeatedly；
5）It will（4）Obtained wet gel block is transferred to mass percent containing N3390 0.05~0.5%, and ethanol solution is placed in 60 DEG C of bakings
Case is modified 12h；It is transferred to the petroleum ether solution of the mass percents of 1-10% containing trim,ethylchlorosilane, modified 5h again；
6）It is dry after then taking out, obtain Al2O3-SiO2System high-performance nano cellular insulant.
2. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In the silicon source is the mixture of a kind of siloxanes containing alkyl or a variety of siloxanes containing alkyl.
3. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In the organic solvent is lower alcohols, and organic solvent is with silicon source molar ratio（1~20）：1.
4. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In the aluminium includes mainly mutually α phases and γ phases Al2O3, Al (OH)3And the bauxite of high alumina, kaolin or metakaolin, aluminium phase
Powder cross 200 mesh sieve extracting screen underflow.
5. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In addition Al2O3:SiO2=0.1~1：1, and accelerate dispersion using ball milling；Ball-milling Time is 10~30 minutes.
6. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
It is glass fibre in, the fiber felt pan, a kind of ceramic fibre, refractory fibrous material in alumina silicate fibre is made；It is described
Whisker is hydrated calcium sulfate, hydrated calcium silicate, calcium carbonate, zinc oxide, and one or more combinations in silicon carbide, whisker accounts for described
SiO2Mass percent be 0.1%~1%.
7. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In the time of the gel is half an hour.
8. Al as described in claim 12O3-SiO2The preparation method of system high-performance nano cellular insulant, feature exist
In the modified liquid of aging wet gel is modified, is dried through supercritical carbon dioxide.
9. a kind of Al2O3-SiO2System high-performance nano cellular insulant, which is characterized in that using such as claim 1 to 8 institute
It is prepared by the preparation method stated.
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| CN115404085A (en) * | 2022-08-23 | 2022-11-29 | 爱彼爱和新材料有限公司 | Method for preparing fireproof and heat-insulating aerogel composite material, fireproof and heat-insulating aerogel composite material and application thereof |
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| CN115404085A (en) * | 2022-08-23 | 2022-11-29 | 爱彼爱和新材料有限公司 | Method for preparing fireproof and heat-insulating aerogel composite material, fireproof and heat-insulating aerogel composite material and application thereof |
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Application publication date: 20180828 |