CN108996985A - A kind of preparation method of aerogel blanket heat-insulating heat-preserving material - Google Patents
A kind of preparation method of aerogel blanket heat-insulating heat-preserving material Download PDFInfo
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- CN108996985A CN108996985A CN201810889041.9A CN201810889041A CN108996985A CN 108996985 A CN108996985 A CN 108996985A CN 201810889041 A CN201810889041 A CN 201810889041A CN 108996985 A CN108996985 A CN 108996985A
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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
- 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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- 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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Abstract
The invention belongs to heat-insulating heat-preserving material fields, disclose a kind of preparation method of aerogel blanket heat-insulating heat-preserving material.It takes positive esters of silicon acis, second alcohol and water to be uniformly mixed, sequentially adds NH4F solution and ammonium hydroxide stir evenly, and obtain silicon dioxide gel A；Resin, initiator, coupling agent, hollow glass micropearl are uniformly mixed to obtain slurries B in resealable container；Fibrofelt is first impregnated in silicon dioxide gel A, it is impregnated in the slurries B of Fresh again after taking-up, it repeats operation 3 ~ 4 times and silicon dioxide gel A is in stirring always when fibrofelt impregnates in slurries B, take out fibrofelt later and be placed on sealing and standing under vacuum condition；Gained fibrofelt is subjected to aging and modification, then carries out solvent displacement with dehydrated alcohol, re-dry processing and heat treatment are to get aerogel blanket heat-insulating heat-preserving material.The present invention overcomes the case where traditional aerosil felt picking falls off under the premise of not influencing felt body heat insulation and preservation effect.
Description
Technical field
The invention belongs to heat-insulating heat-preserving material fields, and in particular to a kind of preparation side of aerogel blanket heat-insulating heat-preserving material
Method.
Background technique
Aeroge is the nano-porous materials that a kind of hole ratio may be up to 80 ~ 99.8%, specific surface area can reach 200 ~
1000m2The density of/g, aeroge are extremely low, are most light solids in the world at present, in addition, aeroge also has lower thermal conductivity (most
Down to 0.01W/mK), high porosity (up to 99%), high photopermeability (up to 99%), low-k are (down to 1.0
~ 2.0), low-refraction (most down to 1.05) etc..
SiO2Aerogel blanket has impayable superiority compared with other traditional heat-insulating heat-preserving materials, be at present every
The best solid material of hot performance of heat protective material is energy-saving preferred material.But also due to the design feature of aeroge,
So that aeroge the disadvantages of that there are brittleness is big, flexible difference, simultaneously as the reason of preparation method, SiO2Aerogel blanket is being transported
It is defeated, construction and use process in generally existing felt body fall off airsetting rubber powder the case where, picking situation not only brought not to construction
Just, threat is brought to construction personnel's health, while can also reduces the performance of aerogel blanket itself, greatly limit aeroge
The application range of felt.Therefore under the premise of guarantee aerogel blanket good heat preservation and insulation, a kind of gas not lost powder is developed
Gel complex material guarantees the health of production, user of service, and it is dirty to reduce dust of the aerogel blanket in storage and transportation, installation, use
Dye problem, and the demand for being able to satisfy every field in the market is very important.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of aerogel blanket heat-insulating heat-preserving material, are not influencing aeroge
Under the premise of felt heat-insulating heat-preserving material heat preservation and insulation, guarantee that the aerogel blanket heat-insulating heat-preserving material being prepared does not lose powder,
Reduce dust pollution question of the aeroge in storage and transportation, installation, use.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of aerogel blanket heat-insulating heat-preserving material, steps are as follows:
(1), it takes positive esters of silicon acis, second alcohol and water to be uniformly mixed, sequentially adds NH later4F solution and ammonium hydroxide stir evenly, and obtain two
Silica sol A；
(2), by weight, by 2 ~ 20 parts of resin, 0.02 ~ 0.05 part of initiator, 0.5 ~ 5 part of coupling agent, hollow glass micropearl 100
Part is uniformly mixed to obtain slurries B in resealable container；
(3), it will be impregnated in fibrofelt first the silicon dioxide gel A obtained by step (1), again in the slurries B of Fresh after taking-up
Middle dipping；
(4), repetitive operation step (3) process 3 ~ 4 times, and silicon dioxide gel A is in always when fibrofelt impregnates in slurries B
Stirring takes out fibrofelt later and is placed on 1 ~ 3 h of sealing and standing under vacuum condition；
(5), fibrofelt obtained by step (4) is subjected to aging process, the fibrofelt after aging is then impregnated in 12- in modification liquid
24 h, then carry out solvent displacement with dehydrated alcohol, and re-dry processing obtains aerogel heat-proof felt；
(6), aerogel heat-proof felt obtained by step (5) is heat-treated to get aerogel blanket heat-insulating heat-preserving material；
Wherein, in step (1): with molar ratio computing, positive esters of silicon acis: ethyl alcohol: water=1: (4 ~ 12): (2 ~ 4)；NH4The addition of F solution
Amount guarantees with molar ratio computing, NH4F: positive esters of silicon acis=(0.002 ~ 0.01): 1；The additional amount of ammonium hydroxide guarantees with molar ratio computing, NH3∶
Positive esters of silicon acis=(0.005 ~ 0.015): 1；In step (4), modification liquid is that hexamethyldisiloxane is in molar ratio with dehydrated alcohol
1: the mixed liquor that (2 ~ 5) mix.
Preferably, in step (1), the positive esters of silicon acis is ethyl orthosilicate or methyl orthosilicate.
Preferably, in step (2), the resin is epoxy resin or unsaturated-resin, and the unsaturated-resin is insatiable hunger
With one of polyester resin 191#, unsaturated polyester resin 197#, vinylite MFE-2, vinylite VER-2 or two
Kind or more mixture.
Preferably, in step (2), the initiator be one of methyl ethyl ketone peroxide, cobalt naphthenate, BPO, AIBN or
Two or more mixtures.
Preferably, in step (2), the coupling agent is silane coupling agent, the density of the hollow ceramic microspheres is 0.15 ~
0.60 g/cm3。
Preferably, in step (3), the dip time in silicon dioxide gel A is 4 ~ 6 h to the fibrofelt every time, often
The secondary dip time in slurries B is 2 ~ 3 h.
Preferably, in step (5), aging in a heated condition, the heating temperature of aging is 30 ~ 60 DEG C, ageing time is
8~24 h。
Preferably, in step (5), the fibrofelt after aging is impregnated in 12 ~ 24 h in modification liquid.
Preferably, in step (5), solvent displacement number is 2 ~ 3 times, and the time replaced every time is 12 ~ 36 h.
Preferably, in step (6), the temperature of heat treatment is 600 ~ 650 DEG C, the time is 0.5 ~ 2 h.
In the present invention, the pure rank of ethyl alcohol Optimization Analysis or chemical pure rank.
The present invention is using fibrofelt alternating impregnating silicon dioxide gel A and slurries B, fibrofelt table after the completion of finally being impregnated
Face is covered with slurries B, can play layer-by-layer fixed function to silica aerogel particles after cured, reduce later period airsetting
The picking situation of glue particle, while step impregnation can guarantee the uniformity of aerogel particle distribution, so that its pore structure be allowed to divide
Cloth is more orderly complete.Secondly, slurries B will be close between hollow glass micropearl and silica aerogel particles after curing molding
Combination is cut, thermal processes act is eventually passed through and removes unsaturated-resin, remaining hollow glass micropearl and silica aerogel particles
It is in three-dimensional space skeletal distribution in fibrofelt, can guarantees that fibrofelt has good heat preservation and insulation while also one
Determine to avoid traditional silicon dioxide aerogel blanket picking phenomenon in degree, has to the various demands for meeting market and greatly facilitate
Meaning.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The range of invention and is not intended to limit the present invention.
Dehydrated alcohol in following embodiments is to analyze pure rank.
Embodiment 1
A kind of preparation method of aerogel blanket heat-insulating heat-preserving material, steps are as follows:
(1), it takes ethyl orthosilicate, dehydrated alcohol and water to be uniformly mixed, sequentially adds the NH of 2 mol/L later4F solution and 0.2
The ammonium hydroxide of moL/L stirs evenly, and obtains silicon dioxide gel A；
(2), by weight, by 20 parts of resin, 0.04 part of initiator, 3 parts of coupling agent, 100 parts of hollow glass micropearl salable
It is uniformly mixed to obtain slurries B in container；
(3), 6 h will be impregnated in glass mat first the silicon dioxide gel A obtained by step (1), again in Fresh after taking-up
Slurries B in impregnate 3 h；
(4), repetitive operation step (3) process 4 times and silicon dioxide gel A locates always when glass mat impregnates in slurries B
In stirring, glass mat is taken out later and is placed on 2 h of sealing and standing under vacuum condition；
(5), by glass mat aging in a heated condition obtained by step (4), when the heating temperature of aging is 60 DEG C, aging
Between be 20 h, be then immersed in the mixed liquor of hexamethyldisiloxane and dehydrated alcohol modification (with molar ratio computing, pregnancy
Base disiloxane: dehydrated alcohol=1: 5) 12 h, and carry out solvent with dehydrated alcohol and replace 2 times, the time replaced every time is 24
H, then constant pressure and dry processing, obtain aerogel heat-proof felt；
(6), aerogel heat-proof felt obtained by step (5) is heat-treated 1.5 h at 600 DEG C to get aerogel blanket heat-insulation and heat-preservation material
Material；
Wherein, in step (1): with molar ratio computing, ethyl orthosilicate: dehydrated alcohol: water=1: 10: 4；NH4The additional amount of F solution
Guarantee with molar ratio computing, NH4F: ethyl orthosilicate=0.006: 1；The additional amount of ammonium hydroxide guarantees with molar ratio computing, NH3: positive silicic acid second
Ester=0.014: 1；In step (2), the resin is epoxy resin, and the initiator is methyl ethyl ketone peroxide, and the coupling agent is
KH-560, the hollow glass micropearl are 3M company K20 product, and density is 0.20 g/cm3。
Embodiment 2
A kind of preparation method of aerogel blanket heat-insulating heat-preserving material, steps are as follows:
(1), it takes ethyl orthosilicate, dehydrated alcohol and water to be uniformly mixed, sequentially adds the NH of 2 mol/L later4F solution and 0.2
The ammonium hydroxide of moL/L stirs evenly, and obtains silicon dioxide gel A；
(2), by weight, by 18 parts of resin, 0.05 part of initiator, 4 parts of coupling agent, 100 parts of hollow glass micropearl salable
It is uniformly mixed to obtain slurries B in container；
(3), 5 h will be impregnated in glass mat first the silicon dioxide gel A obtained by step (1), again in Fresh after taking-up
Slurries B in impregnate 3 h；
(4), repetitive operation step (3) process 3 times and silicon dioxide gel A locates always when glass mat impregnates in slurries B
In stirring, glass mat is taken out later and is placed on 2 h of sealing and standing under vacuum condition；
(5), by glass mat aging in a heated condition obtained by step (4), when the heating temperature of aging is 50 DEG C, aging
Between be 18 h, be then immersed in the mixed liquor of hexamethyldisiloxane and dehydrated alcohol modification (with molar ratio computing, pregnancy
Base disiloxane: dehydrated alcohol=1: 4) 20 h, and carry out solvent with dehydrated alcohol and replace 3 times, the time replaced every time is 20
H, then constant pressure and dry processing, obtain aerogel heat-proof felt；
(6), aerogel heat-proof felt obtained by step (5) is heat-treated 0.5 h at 650 DEG C to get aerogel blanket heat-insulation and heat-preservation material
Material；
Wherein, in step (1): with molar ratio computing, ethyl orthosilicate: dehydrated alcohol: water=1: 12: 3；NH4The additional amount of F solution
Guarantee with molar ratio computing, NH4F: ethyl orthosilicate=0.008: 1；The additional amount of ammonium hydroxide guarantees with molar ratio computing, NH3: positive silicic acid second
Ester=0.008: 1；In step (2), the resin is unsaturated polyester resin 191#, and the initiator is BPO, the coupling agent
For KH-560, the hollow glass micropearl is 3M company XLD3000 product, and density is 0.23 g/cm3。
Embodiment 3
A kind of preparation method of aerogel blanket heat-insulating heat-preserving material, steps are as follows:
(1), it takes ethyl orthosilicate, dehydrated alcohol and water to be uniformly mixed, sequentially adds the NH of 2 mol/L later4F solution and 0.2
The ammonium hydroxide of moL/L stirs evenly, and obtains silicon dioxide gel A；
(2), by weight, by 15 parts of resin, 0.02 part of initiator, 2 parts of coupling agent, 100 parts of hollow glass micropearl salable
It is uniformly mixed to obtain slurries B in container；
(3), 6 h will be impregnated in glass mat first the silicon dioxide gel A obtained by step (1), again in Fresh after taking-up
Slurries B in impregnate 2 h；
(4), repetitive operation step (3) process 3 times and silicon dioxide gel A locates always when glass mat impregnates in slurries B
In stirring, glass mat is taken out later and is placed on 3 h of sealing and standing under vacuum condition；
(5), by glass mat aging in a heated condition obtained by step (4), when the heating temperature of aging is 40 DEG C, aging
Between be 24 h, be then immersed in the mixed liquor of hexamethyldisiloxane and dehydrated alcohol modification (with molar ratio computing, pregnancy
Base disiloxane: dehydrated alcohol=1: 3) 24 h, and carry out solvent with dehydrated alcohol and replace 3 times, the time replaced every time is 15
H, then constant pressure and dry processing, obtain aerogel heat-proof felt；
(6), aerogel heat-proof felt obtained by step (5) is heat-treated 1 h at 650 DEG C to get aerogel blanket heat-insulation and heat-preservation material
Material；
Wherein, in step (1): with molar ratio computing, ethyl orthosilicate: dehydrated alcohol: water=1: 8: 2；NH4The additional amount of F solution is protected
Card is with molar ratio computing, NH4F: ethyl orthosilicate=0.01: 1；The additional amount of ammonium hydroxide guarantees with molar ratio computing, NH3: ethyl orthosilicate=
0.013:1；In step (2), the resin is vinylite MFE-2, and the initiator is cobalt naphthenate, and the coupling agent is
KH-560, the hollow glass micropearl are 3M company VS5500 product, and density is 0.38 g/cm3。
The heat property test result of aerogel blanket heat-insulating heat-preserving material obtained by embodiment 1-3 see the table below:
As seen from the above table: the aerogel blanket heat-insulating heat-preserving material that the present invention is prepared has splendid thermal and insulating performance.
Claims (10)
1. a kind of preparation method of aerogel blanket heat-insulating heat-preserving material, which is characterized in that steps are as follows:
(1), it takes positive esters of silicon acis, second alcohol and water to be uniformly mixed, sequentially adds NH later4F solution and ammonium hydroxide stir evenly, and obtain two
Silica sol A；
(2), by weight, by 2 ~ 20 parts of resin, 0.02 ~ 0.05 part of initiator, 0.5 ~ 5 part of coupling agent, hollow glass micropearl 100
Part is uniformly mixed to obtain slurries B in resealable container；
(3), it will be impregnated in fibrofelt first the silicon dioxide gel A obtained by step (1), again in the slurries B of Fresh after taking-up
Middle dipping；
(4), repetitive operation step (3) process 3 ~ 4 times, and silicon dioxide gel A is in always when fibrofelt impregnates in slurries B
Stirring takes out fibrofelt later and is placed on 1 ~ 3 h of sealing and standing under vacuum condition；
(5), fibrofelt obtained by step (4) is subjected to aging process, then the fibrofelt after aging is impregnated in modification liquid, so
Solvent displacement is carried out with dehydrated alcohol afterwards, re-dry processing obtains aerogel heat-proof felt；
(6), aerogel heat-proof felt obtained by step (5) is heat-treated to get aerogel blanket heat-insulating heat-preserving material；
Wherein, in step (1): with molar ratio computing, positive esters of silicon acis: ethyl alcohol: water=1: (4 ~ 12): (2 ~ 4)；NH4The additional amount of F solution
Guarantee with molar ratio computing, NH4F: positive esters of silicon acis=(0.002 ~ 0.01): 1；The additional amount of ammonium hydroxide guarantees with molar ratio computing, NH3: just
Esters of silicon acis=(0.005 ~ 0.015): 1；
In step (4), modification liquid is hexamethyldisiloxane and dehydrated alcohol is 1 in molar ratio: the mixing that (2 ~ 5) mix
Liquid.
2. preparation method as described in claim 1, it is characterised in that: in step (1), the positive esters of silicon acis is ethyl orthosilicate
Or methyl orthosilicate.
3. preparation method as described in claim 1, it is characterised in that: in step (2), the resin is epoxy resin or insatiable hunger
And resin, the unsaturated-resin be unsaturated polyester resin 191#, unsaturated polyester resin 197#, vinylite MFE-2,
The mixture of one or more of vinylite VER-2.
4. preparation method as described in claim 1, it is characterised in that: in step (2), the initiator is peroxidating first and second
The mixture of one or more of ketone, cobalt naphthenate, BPO, AIBN.
5. preparation method as described in claim 1, it is characterised in that: in step (2), the coupling agent is silane coupling agent,
The density of the hollow ceramic microspheres is 0.15 ~ 0.60 g/cm3。
6. preparation method as described in claim 1, it is characterised in that: in step (3), the fibrofelt is every time in silica
Dip time in Sol A is 4 ~ 6 h, and the dip time in slurries B is 2 ~ 3 h every time.
7. preparation method as described in claim 1, it is characterised in that: in step (5), aging in a heated condition, aging
Heating temperature is 30 ~ 60 DEG C, ageing time is 8 ~ 24 h.
8. preparation method as described in claim 1, it is characterised in that: in step (5), the fibrofelt after aging is impregnated in and is changed
12 ~ 24 h in property liquid.
9. preparation method as described in claim 1, it is characterised in that: in step (5), solvent displacement number is 2 ~ 3 times, every time
The displaced time is 12 ~ 36 h.
10. preparation method as described in claim 1, it is characterised in that: in step (6), the temperature of heat treatment is 600 ~ 650
DEG C, the time be 0.5 ~ 2 h.
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Cited By (8)
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| CN109503116A (en) * | 2018-12-17 | 2019-03-22 | 山东鲁阳节能材料股份有限公司 | A kind of preparation method of aeroge compound insulating material |
| CN110922095A (en) * | 2019-11-07 | 2020-03-27 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of composite silica aerogel felt |
| CN111825423A (en) * | 2020-07-28 | 2020-10-27 | 巩义市泛锐熠辉复合材料有限公司 | Efficient heat insulation sheet and preparation method thereof |
| CN113603423A (en) * | 2021-08-24 | 2021-11-05 | 杭州金鼎实业有限公司 | Foam concrete and preparation method thereof |
| CN113651592A (en) * | 2021-08-20 | 2021-11-16 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of anti-buffering silicon dioxide aerogel heat insulation sheet |
| CN114033922A (en) * | 2021-11-18 | 2022-02-11 | 青海省水文地质工程地质环境地质调查院 | Preparation method of heat-insulating combined material suitable for hot dry rock single-hole heat-taking steam-discharging device |
| CN115110311A (en) * | 2022-07-08 | 2022-09-27 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant alumina aerogel felt and alumina aerogel felt |
| CN116199522A (en) * | 2023-01-17 | 2023-06-02 | 武汉中科先进材料科技有限公司 | PU sponge-based silicon aerogel felt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109503116A (en) * | 2018-12-17 | 2019-03-22 | 山东鲁阳节能材料股份有限公司 | A kind of preparation method of aeroge compound insulating material |
| CN110922095A (en) * | 2019-11-07 | 2020-03-27 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of composite silica aerogel felt |
| CN110922095B (en) * | 2019-11-07 | 2021-07-09 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of composite silica aerogel felt |
| CN111825423A (en) * | 2020-07-28 | 2020-10-27 | 巩义市泛锐熠辉复合材料有限公司 | Efficient heat insulation sheet and preparation method thereof |
| CN113651592A (en) * | 2021-08-20 | 2021-11-16 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of anti-buffering silicon dioxide aerogel heat insulation sheet |
| CN113603423A (en) * | 2021-08-24 | 2021-11-05 | 杭州金鼎实业有限公司 | Foam concrete and preparation method thereof |
| CN114033922A (en) * | 2021-11-18 | 2022-02-11 | 青海省水文地质工程地质环境地质调查院 | Preparation method of heat-insulating combined material suitable for hot dry rock single-hole heat-taking steam-discharging device |
| CN115110311A (en) * | 2022-07-08 | 2022-09-27 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant alumina aerogel felt and alumina aerogel felt |
| CN115110311B (en) * | 2022-07-08 | 2024-01-12 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant alumina aerogel felt and alumina aerogel felt |
| CN116199522A (en) * | 2023-01-17 | 2023-06-02 | 武汉中科先进材料科技有限公司 | PU sponge-based silicon aerogel felt and preparation method thereof |
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