CN106866106A - A kind of preparation method of silicon dioxide silica aerogel composite material - Google Patents
A kind of preparation method of silicon dioxide silica aerogel composite material Download PDFInfo
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- CN106866106A CN106866106A CN201710162902.9A CN201710162902A CN106866106A CN 106866106 A CN106866106 A CN 106866106A CN 201710162902 A CN201710162902 A CN 201710162902A CN 106866106 A CN106866106 A CN 106866106A
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- 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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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/2038—Resistance against physical degradation
- C04B2111/2046—Shock-absorbing materials
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- 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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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The present invention relates to aeroge technical field, especially a kind of preparation method of silicon dioxide silica aerogel composite material；Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring dissolves silane coupler, then the glass fibre by aerosil and surface treatment is added, glass fibre and silica gel colloidal sol is fully combined and is uniformly dispersed, fibre-reinforced silicon dioxide silica aerogel composite material is obtained after aging, addition alcoholic solution and alkane difference substitution, drying after gel-forming；The introducing of reinforcement effectively reduces the surface tension between hole in the present invention, enhance the intensity of aeroge skeleton, overcome pure silicon dioxide aeroge low intensity and the big shortcoming of fragility, avoid the problems such as aging and drying stage volume excess shrinkage, structure collapses, face crack is reduced, blockiness preferable aerogel composite is obtained.
Description
Technical field
The present invention relates to aeroge technical field, especially a kind of preparation method of silicon dioxide silica aerogel composite material.
Background technology
Aerosil is a kind of poroid material of new structure-controllable, the property for having multiple uniqueness, such as low
Refractive index, low elastic modulus, lower thermal conductivity and strong adsorptivity, typical fractal structure etc., can be made into acoustic impedance coupling material,
Various high performance materials such as filtering material, high temperature insulating material, have wide application prospect in various fields.
In actual applications, aerosil is generally using pulverulence as a kind of packing material, be filled into it is heat-insulated,
In the carriers such as noise reduction, damping energy-absorbing, absorption, catalyst.But this aerogel powder shape can reduce the performance of aeroge itself,
The effect that aeroge low-heat is led, adsorbed by force can not well be played.And due to poor mechanical performance, silica airsetting
The cracking of glue is still a main obstacle；So silicon dioxide silica aerogel composite material need to carry out deeper into grind
Study carefully.
The content of the invention
The purpose of the present invention is：Overcome deficiency of the prior art, there is provided a kind of silicon dioxide silica aerogel composite material
Preparation method, silicon dioxide silica aerogel composite material mechanical strength that the method is prepared is good, performance is good.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and is made after aging, addition alcoholic solution and alkane difference substitution, drying after gel-forming
Obtain fibre-reinforced silicon dioxide silica aerogel composite material.
Preferably, the silane coupler and the mass ratio of methyl alcohol and acetum are 1:3-6.
Preferably, the silane coupler and the mass ratio of methyl alcohol and acetum are 1:4.5.
Preferably, the glass fibre is processed using following methods：Glass fibre is protected under 160-180 DEG C of temperature conditionss
Warm 6-8min, 6-8min is soaked after being subsequently cooled to room temperature by glass fibre in concentrated hydrochloric acid, with deionized water to glass fibre
Surface p H be sprayed to more than 7, the glass fibre after glass fibre drying is processed.
Preferably, after the alcoholic solution and alkane difference substitution, the carbon fiber of 1.8mm is added, magnetic agitation, plus
Enter dispersant MC, disperse fiber, form gel, further ageing and solvent displacement, are finally dried.
Preferably, the drying uses the condition of supercritical drying, supercritical drying to be：240 DEG C of temperature, pressure
7.5MPa, drying time 6-18h.
Preferably, the ageing time is 6-8h.
Beneficial effect using technical scheme is：
The introducing of reinforcement effectively reduces the surface tension between hole in the present invention, enhances the strong of aeroge skeleton
Degree, overcomes pure silicon dioxide aeroge low intensity and the big shortcoming of fragility, it is to avoid excessive in aging and drying stage volume
The problems such as contraction, structure collapses, face crack is reduced, obtain blockiness preferable aerogel composite；
Silicon dioxide silica aerogel composite material obtained in preparation method of the invention resists compared with existing aerogel plate product
Compressive Strength improves 100~200%, and thermal conductivity factor reduces 10~50%, and it is more to be that aeroge extensive utilization is opened
Passage, can widely apply to the fields such as insulation, damping energy-absorbing, modified aeroge, and not only original performance is more
It is prominent, and it is compound after obtain some new performances, compression strength is high, good flame resistance, with explosion-proof and damping energy-absorbing effect.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and through aging after gel-forming, ageing time is 6h, adds alcoholic solution and alkane to replace respectively
Fibre-reinforced silicon dioxide silica aerogel composite material is obtained after modified, dry；Drying uses supercritical drying, supercritical drying
Condition be：240 DEG C of temperature, pressure 7.5MPa, drying time 6h.
Wherein, silane coupler and the mass ratio of methyl alcohol and acetum are 1:3.
Wherein, glass fibre is processed using following methods：Glass fibre is incubated 6min under 160 DEG C of temperature conditionss, so
After be cooled to room temperature after glass fibre is soaked into 6min in concentrated hydrochloric acid, glass fibre is carried out with deionized water be sprayed to surface
PH is 7.1, the glass fibre after glass fibre drying is processed.
Wherein, after alcoholic solution and alkane distinguish substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersion
Agent MC, disperses fiber, forms gel, and further ageing and solvent displacement, are finally dried.
Obtained silicon dioxide composite aerogel porosity 90%, density 0.22g/cm3, BET specific surface area 912m2/ g,
140 ° of water contact angle, in hydrophobicity, pore-size distribution is concentrated mainly on 3~48nm.Thermal conductivity factor is 0.03Wm-1·K-1, resistance to compression
Intensity 0.8MPa (25% deformation), elastic modelling quantity 3.2MPa or so.
Embodiment 2
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and through aging after gel-forming, ageing time is 6.5h, adds alcoholic solution and alkane to put respectively
Fibre-reinforced silicon dioxide silica aerogel composite material is obtained after changing modified, drying；Wherein, drying uses supercritical drying, surpasses
Critical dry condition is：240 DEG C of temperature, pressure 7.5MPa, drying time 8h.
Wherein, silane coupler and the mass ratio of methyl alcohol and acetum are 1:4.
Wherein, glass fibre is processed using following methods：Glass fibre is incubated 7min under 165 DEG C of temperature conditionss, so
After be cooled to room temperature after glass fibre is soaked into 7min in concentrated hydrochloric acid, glass fibre is carried out with deionized water be sprayed to surface
PH is 7.5, the glass fibre after glass fibre drying is processed.
Wherein, after alcoholic solution and alkane distinguish substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersion
Agent MC, disperses fiber, forms gel, and further ageing and solvent displacement, are finally dried.
Obtained silicon dioxide composite aerogel porosity 92%, density 0.2g/cm3, BET specific surface area 920m2/ g,
142 ° of water contact angle, in hydrophobicity, pore-size distribution is concentrated mainly on 4~40nm.Thermal conductivity factor is 0.03Wm-1·K-1, resistance to compression
Intensity 0.8MPa (25% deformation), elastic modelling quantity 3.2MPa or so.
Embodiment 3
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and through aging after gel-forming, ageing time is 7h, adds alcoholic solution and alkane to replace respectively
Fibre-reinforced silicon dioxide silica aerogel composite material is obtained after modified, dry, drying uses supercritical drying, supercritical drying
Condition be：240 DEG C of temperature, pressure 7.5MPa, drying time 12h.
Wherein, silane coupler and the mass ratio of methyl alcohol and acetum are 1:4.5.
Wherein, glass fibre is processed using following methods：Glass fibre is incubated 7min under 170 DEG C of temperature conditionss, so
After be cooled to room temperature after glass fibre is soaked into 7min in concentrated hydrochloric acid, glass fibre is carried out with deionized water be sprayed to surface
PH is 7.8, the glass fibre after glass fibre drying is processed.
Wherein, after alcoholic solution and alkane distinguish substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersion
Agent MC, disperses fiber, forms gel, and further ageing and solvent displacement, are finally dried.
Obtained silicon dioxide composite aerogel porosity 93%, density 0.19g/cm3, BET specific surface area 930m2/ g,
145 ° of water contact angle, in hydrophobicity, pore-size distribution is concentrated mainly on 4~40nm.Thermal conductivity factor is 0.03Wm-1·K-1, resistance to compression
Intensity 0.8MPa (25% deformation), elastic modelling quantity 3.2MPa or so.
Embodiment 4
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and through aging after gel-forming, ageing time is 7h, adds alcoholic solution and alkane to replace respectively
Fibre-reinforced silicon dioxide silica aerogel composite material is obtained after modified, dry；Drying uses supercritical drying, supercritical drying
Condition be：240 DEG C of temperature, pressure 7.5MPa, drying time 15h.
Wherein, silane coupler and the mass ratio of methyl alcohol and acetum are 1:5.
Wherein, glass fibre is processed using following methods：Glass fibre is incubated 7min under 175 DEG C of temperature conditionss, so
After be cooled to room temperature after glass fibre is soaked into 7min in concentrated hydrochloric acid, glass fibre is carried out with deionized water be sprayed to surface
PH is 8, the glass fibre after glass fibre drying is processed.
Wherein, after alcoholic solution and alkane distinguish substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersion
Agent MC, disperses fiber, forms gel, and further ageing and solvent displacement, are finally dried.
Obtained silicon dioxide composite aerogel porosity 91.8%, density 0.2g/cm3, BET specific surface area 920m2/
G, 142 ° of water contact angle, in hydrophobicity, pore-size distribution is concentrated mainly on 4~40nm.Thermal conductivity factor is 0.03Wm-1·K-1, resist
Compressive Strength 0.8MPa (25% deformation), elastic modelling quantity 3.2MPa or so.
Embodiment 5
A kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with dioxy
SiClx is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate
(TEOS) it is silicon source material, the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane idol
Connection agent dissolving, then adds the glass fibre by aerosil and surface treatment, makes glass fibre and silica gel molten
Glue is fully combined and is uniformly dispersed, and through aging after gel-forming, ageing time is 8h；Alcoholic solution and alkane is added to replace respectively
Fibre-reinforced silicon dioxide silica aerogel composite material is obtained after modified, dry；Drying uses supercritical drying, supercritical drying
Condition be：240 DEG C of temperature, pressure 7.5MPa, drying time 18h.
Wherein, silane coupler and the mass ratio of methyl alcohol and acetum are 1:6.
Wherein, glass fibre is processed using following methods：Glass fibre is incubated 8min under 180 DEG C of temperature conditionss, so
After be cooled to room temperature after glass fibre is soaked into 8min in concentrated hydrochloric acid, glass fibre is carried out with deionized water be sprayed to surface
PH is 8.2, the glass fibre after glass fibre drying is processed.
Wherein, after alcoholic solution and alkane distinguish substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersion
Agent MC, disperses fiber, forms gel, and further ageing and solvent displacement, are finally dried.
Obtained silicon dioxide composite aerogel porosity 92.8%, density 0.2g/cm3, BET specific surface area 925m2/
G, 142 ° of water contact angle, in hydrophobicity, pore-size distribution is concentrated mainly on 4~40nm.Thermal conductivity factor is 0.03Wm-1·K-1, resist
Compressive Strength 0.8MPa (25% deformation), elastic modelling quantity 3.2MPa or so.
Embodiment 3 is preferred embodiment.
Although above-described embodiment is described in detail to technical scheme, technical side of the invention
Case is not limited to above example, in the case where thought of the invention and objective is not departed from, to technical scheme institute
Any change done falls within claims of the present invention limited range.
Claims (7)
1. a kind of preparation method of silicon dioxide silica aerogel composite material, the silicon dioxide silica aerogel composite material is with titanium dioxide
Silicon is matrix, and glass fibre is reinforcement, using silane coupler as Fiber strength reagent, tetraethyl orthosilicate (TEOS)
It is silicon source material, it is characterised in that the preparation method is comprised the following steps：
Weigh in silane coupler addition beaker, it is 1 to add volume ratio:4 methyl alcohol and acetum, stirring makes silane coupler
Dissolving, then adds the glass fibre by aerosil and surface treatment, fills glass fibre and silica gel colloidal sol
Divide and combine and be uniformly dispersed, fibre is obtained after aging, addition alcoholic solution and alkane difference substitution, drying after gel-forming
Tie up enhanced silicon dioxide silica aerogel composite material.
2. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that：It is described
Silane coupler is 1 with the mass ratio of methyl alcohol and acetum:3-6.
3. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 2, it is characterised in that：It is described
Silane coupler is 1 with the mass ratio of methyl alcohol and acetum:4.5.
4. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that described
Glass fibre is processed using following methods：Glass fibre is incubated 6-8min under 160-180 DEG C of temperature conditionss, is subsequently cooled to
Glass fibre is soaked into 6-8min in concentrated hydrochloric acid after room temperature, glass fibre is carried out being sprayed to surface p H with deionized water is more than
7, the glass fibre after glass fibre drying is processed.
5. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that：It is described
After alcoholic solution and alkane difference substitution, the carbon fiber of 1.8mm is added, magnetic agitation adds dispersant MC, makes fiber point
Dissipate, form gel, further ageing and solvent displacement, are finally dried.
6. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that：It is described
Drying uses the condition of supercritical drying, supercritical drying to be：240 DEG C of temperature, pressure 7.5MPa, drying time 6-18h.
7. the preparation method of a kind of silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that：It is described
Ageing time is 6-8h.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249943A (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 water-fast aerogel material |
| CN108640643A (en) * | 2018-07-20 | 2018-10-12 | 成都上泰科技有限公司 | A kind of aerosil manufacturing process containing reinforcing fiber |
| CN108892470A (en) * | 2018-07-05 | 2018-11-27 | 江苏泛亚微透科技股份有限公司 | The heat-insulated elastic silica aerogel sheet material of vibration damping and automobile lithium-ion-power cell heat management system thin slice |
| CN110845145A (en) * | 2019-07-01 | 2020-02-28 | 重庆文理学院 | Composite heat-resistant material for automobile engine heat shield and preparation method thereof |
| CN112119037A (en) * | 2018-11-27 | 2020-12-22 | 株式会社Lg化学 | Preparation method of silicon dioxide aerogel |
| CN112759353A (en) * | 2021-01-07 | 2021-05-07 | 深圳市中科华深科技有限公司 | Fireproof heat-insulating material and preparation method thereof |
| CN114014633A (en) * | 2021-11-22 | 2022-02-08 | 中凝科技(湖北)有限公司 | Preparation method of aerogel heat insulation felt |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
| CN115850786A (en) * | 2022-10-27 | 2023-03-28 | 重庆文理学院 | Preparation method of glass fiber aerogel |
| CN115925386A (en) * | 2022-12-28 | 2023-04-07 | 江苏汉信天诚新材料有限公司 | Low-density silicon dioxide aerogel coiled material and preparation method thereof |
| CN117601512A (en) * | 2023-11-30 | 2024-02-27 | 广东埃力生科技股份有限公司 | Aerogel composite board and preparation method thereof |
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| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN105731470A (en) * | 2016-01-21 | 2016-07-06 | 长春工业大学 | Method for preparing silicon dioxide aerogel composite material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN105731470A (en) * | 2016-01-21 | 2016-07-06 | 长春工业大学 | Method for preparing silicon dioxide aerogel composite material |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249943A (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 water-fast aerogel material |
| CN108892470A (en) * | 2018-07-05 | 2018-11-27 | 江苏泛亚微透科技股份有限公司 | The heat-insulated elastic silica aerogel sheet material of vibration damping and automobile lithium-ion-power cell heat management system thin slice |
| CN108640643A (en) * | 2018-07-20 | 2018-10-12 | 成都上泰科技有限公司 | A kind of aerosil manufacturing process containing reinforcing fiber |
| CN112119037A (en) * | 2018-11-27 | 2020-12-22 | 株式会社Lg化学 | Preparation method of silicon dioxide aerogel |
| CN112119037B (en) * | 2018-11-27 | 2023-06-30 | 株式会社Lg化学 | Preparation method of silica aerogel |
| CN110845145A (en) * | 2019-07-01 | 2020-02-28 | 重庆文理学院 | Composite heat-resistant material for automobile engine heat shield and preparation method thereof |
| CN112759353A (en) * | 2021-01-07 | 2021-05-07 | 深圳市中科华深科技有限公司 | Fireproof heat-insulating material and preparation method thereof |
| CN114014633A (en) * | 2021-11-22 | 2022-02-08 | 中凝科技(湖北)有限公司 | Preparation method of aerogel heat insulation felt |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
| CN115850786A (en) * | 2022-10-27 | 2023-03-28 | 重庆文理学院 | Preparation method of glass fiber aerogel |
| CN115925386A (en) * | 2022-12-28 | 2023-04-07 | 江苏汉信天诚新材料有限公司 | Low-density silicon dioxide aerogel coiled material and preparation method thereof |
| CN117601512A (en) * | 2023-11-30 | 2024-02-27 | 广东埃力生科技股份有限公司 | Aerogel composite board and preparation method thereof |
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