CN110255567A - Lightweight heat-proof noise reduction SiO2Aerogel material and preparation method thereof - Google Patents
Lightweight heat-proof noise reduction SiO2Aerogel material and preparation method thereof Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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Abstract
The invention discloses a kind of lightweight heat-proof noise reduction SiO2Aerogel material and preparation method thereof belongs to high-performance porous material technical field.The preparation method includes replacing that aerogel material is made through soda acid two-step method and standing in aqueous solvent using trifunctional silicon source and cationic surfactant, wherein, trifunctional silicon source molecule includes the alkoxy grp of a non-polar group for not participating in hydrolytic condensation and three participation hydrolysis-condensation reactions.The preparation method that the present invention designs reduces solvent surface tension by addition surfactant using water as solvent, and forms organized assembles in aqueous solution to provide a micro- reaction vessel, SiO obtained with hydrophobic trifunctional silicon source2Aerogel material has the advantages that low-density, low thermal conductivity, high grade of transparency.
Description
Technical field
The present invention relates to aerogel materials, belong to high-performance porous material technical field, more particularly to a kind of lightweight every
Heat drop is made an uproar SiO2Aerogel material and preparation method thereof.
Background technique
Aeroge is the novel super heat-insulating material being made of three-dimensional manometer network, has low-density, low thermal conductivity, height
The features such as specific surface and high porosity, and in partiting thermal insulation, environmental protection, medicine, catalysis, building energy conservation, petrochemical industry, aerospace
Equal fields have broad application prospects.
Aeroge is usually using four-functional group silicon source and alcohols solvent as raw material, using sol-gel technique and overcritical
Dry technology preparation.The aeroge bad mechanical property being prepared, and there is hydrophily, it is difficult to apply to engineering reality
In border.With the development of gel process, the flexible aeroge prepared by using trifunctional silicon source, mechanical performance obtain compared with
Big improvement, and the skeleton formed with methyl blocking is but also this aerogel-like has good hydrophobic performance.
Surfactant can substantially reduce interfacial tension in adsorbed on interfaces, change the surface chemistry property of system.Together
When, surfactant also can inside solution autohemagglutination formed diversified forms Molecular Organized Assemblies, such as micella, reverse micelle, capsule
Bubble and liquid crystal etc..These Molecular Organized Assemblies show diversified application function.Wherein it is based on micella and other molecules
The solubilization of organized assembles derives micellar catalysis, forms microemulsion and as being spaced chemical reaction medium and micro- anti-
Answer device.I.e. suitable surfactant enables to that there is hydrophobic trifunctional silicon source can be hydrolyzed in aqueous systems
Condensation reaction, and obtained aeroge has visibly homogeneous pore-size distribution.
At the same time, the replacement process of wet gel is often a very long cumbersome process, especially on surface
The addition of activating agent, common replacement process are often difficult to replace impurity thorough.It is primarily due to the table in the hole of wet gel
Face activating agent is still to exist in the form of micella, can be remained in inside gel always in replacement process, and low-density
Wet gel easily ruptures in the case where larger concentration difference.It is usually the case that surfactant and trifunctional is difficult to be utilized
Silicon source prepares complete low-density flexibility aeroge in water.The study found that SiO2Wet gel is in strong alkali environment gel skeleton
Negatively charged, cationic surfactant would generally be adsorbed on gel skeleton at this time, so that surfactant is in gel
With the presence of unimolecule state in hole, it is easy to replace.And biggish concentration difference is also because part of the surface is living in replacement process
Property agent by skeleton attraction avoid the rupture so that wet gel.
Chinese invention patent (application publication number: CN101691227A, data of publication of application: 2010-04-07) discloses one kind
The preparation method of silica aerogel material specifically uses tetraethyl orthosilicate for silicon source, methyltrimethoxysilane or
Methyltriethoxysilane is co-precursor modifying agent, and dehydrated alcohol is solvent, and hydrochloric acid and ammonium hydroxide are catalyst.Using colloidal sol-
Gel soda acid two-step method, which is catalyzed, is made SiO2Wet gel, after carrying out aging process under certain condition, again to wet gel sample
Modification, and finally atmospheric low-temperature is dried to obtain SiO in air atmosphere2Aeroge.Preparation process equipment cost is lower, produces
Product function admirable, reaction process are controllable.But the aeroge sound insulation property of invention preparation is poor, frangible, does not have flexibility, and past
The process complicated toward needs could obtain hydrophobic performance.
Chinese invention patent (application publication number: CN106467388A, data of publication of application: 2017-03-01) discloses one kind
Large volume flexibility aeroge and preparation method thereof, being specifically includes following component: 12~18 parts of methyltriethoxysilane, 2
~6 parts of vinyltrimethoxysilanes, 110~160 parts of methanol, 3~8 parts of ammonium hydroxide.The present invention utilizes trifunctional silicon source, although
Its preparation process is relatively easy, but there are poor transparency, high thermal conductivity coefficient and highdensity disadvantages for aeroge obtained.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of lightweight heat-proof noise reduction SiO2Aerogel material and its preparation
Method, the preparation method reduce solvent surface tension by addition surfactant using water as solvent, and in aqueous solution
Organized assembles are formed to provide a micro- reaction vessel, SiO obtained with hydrophobic trifunctional silicon source2Airsetting glue material
Material has the advantages that low-density, low thermal conductivity, high grade of transparency.
To achieve the above object, the invention discloses a kind of lightweight heat-proof noise reduction SiO2The preparation method of aerogel material,
It includes being made in aqueous solvent through soda acid two-step method and standing displacement using trifunctional silicon source and cationic surfactant
Aerogel material, the trifunctional silicon source molecule include a non-polar group for not participating in hydrolytic condensation and three participation water
Solve the alkoxy grp of condensation reaction.
Further, the trifunctional silicon source includes methyltriethoxysilane, methyltrimethoxysilane, ethyl three
At least one of Ethoxysilane or ethyl trimethoxy silane.
Preferably, the trifunctional silicon source is methyltriethoxysilane.
Further, the cationic surfactant includes quaternary ammonium salt cationic surfactant.
Preferably, the cationic surfactant is cetyl trimethylammonium bromide.
Further, it includes the following steps:
1) micella or microemulsion are prepared: taking acidic catalyst and deionized water to mix to obtain acid solution, adds cation
Surfactant stirs to get micella or microemulsion；
2) it prepares colloidal sol: trifunctional silicon source being added into the micella or microemulsion of step 1), adds alkalinity and urges
Agent obtains mixed solution, and colloidal sol is made in sealing and standing；
3) aging and displacement: deionized water being added into colloidal sol described in step 2), takes out, is placed in ammonium hydroxide after to be aging,
Sealing and standing waits first time replacement completion；It continuously adds ethyl alcohol and completes second of displacement；
4) dry: the wet gel that step 3) has been replaced is placed in closed container, through the dried medium for being in critical state
Processing, obtains aerogel material.
Further, the pH value of acid solution described in step 1) is 3~4, and the acidic catalyst includes hydrofluoric acid, salt
At least one of acid, nitric acid, acetic acid or oxalic acid.
Further, the additional amount of cationic surfactant described in step 1) is to be added in every 30mL acid solution
0.01g~5g.
Preferably, step 1) is to obtain micella or microemulsion, using mechanical stirring or ultrasonic vibration.
Further, the pH value of mixed solution described in step 2) is 7~8；The basic catalyst includes ammonium hydroxide or hydrogen
Sodium oxide molybdena.
Preferably, ammonia concn described in step 2) is 1~6.5mol/L.
Preferably, the volume ratio of the trifunctional silicon source and deionized water in step 1) is 1:(1.5~6).
Further, the sealing and standing in step 2) and step 3) is to carry out in the water-bath for be placed in 40 DEG C~80 DEG C.
Preferably, ammonia concn described in step 3) is 1~6.5mol/L.
Preferably, displacement carries out 8~12h in the environment of pH=9~10 for the first time in step 3).
Further, dried medium described in step 4) includes ethyl alcohol or carbon dioxide.
In order to preferably realize the technology of the present invention purpose, the invention also discloses a kind of lightweight heat-proof noise reduction SiO2Aeroge
Material, it is to be prepared using above-mentioned preparation method, and the density of the aerogel material is 30mg/cm3~100mg/cm3, lead
Heating rate is 0.015~0.025W/ (mK).
Further, the hydrophobic angle of the aerogel material reaches 168.8 °.
Further, all band visible transparency of the aerogel material of 1cm thickness is 5%~90%.
Further, 1cm thickness, density 60mg/cm3Sound of the aerogel material between 500~1600HZ
Transmitting loss is 13~21dB.
Further, the temperature of initial decomposition of the aerogel material is 480 DEG C.
The beneficial effects are mainly reflected as follows following aspects:
1, the preparation method that the present invention designs forms low-density flexible air using trifunctional silicon source in aqueous solvent
Gel effectively reduces cost of material, and makes production process more safely controllable；
2, the preparation method that the present invention designs uses cationic surfactant to form self-assembly in aqueous solution as silicon
Source reaction provides micro- reacting environment, avoids the premature generation of trifunctional silicon source and mutually separates, has obtained the soft of low thermal conductivity
Property aeroge；
3, the preparation method that the present invention designs in strong alkali solution by replacing, so that displacement efficiency mentions significantly
Height, impurity displacement thoroughly, effectively reduce displacement number and time swap, reduce the use cost of displacement liquid, and guarantee
The integrality of low-density sample；
4, the aerogel material that the present invention is prepared has the skeleton structure of threadiness, is a kind of with super-hydrophobic, low
Density, it is transparent, heat-insulated and sound insulation etc. it is multi-functional in one light material, the fields such as environmental protection, medicine, aerospace have compared with
Good application prospect.
Detailed description of the invention
Fig. 1 is aerogel material sample object photo prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope microscopic appearance figure of aerogel material sample prepared by the embodiment of the present invention 1；
Fig. 3 is the hydrophobic performance test chart of aerogel material sample prepared by the embodiment of the present invention 1；
Fig. 4 is the thermogravimetric curve of aerogel material sample prepared by the embodiment of the present invention 1；
Fig. 5 is the test of all band visible light transmittance rate of aerogel material 1cm thickness sample prepared by the embodiment of the present invention 1
Figure；
Fig. 6 is the density and thermal coefficient distribution map of aerogel material sample prepared by the embodiment of the present invention 1,2,3 and 4；
Fig. 7 is the sound insulation property test chart of aerogel material sample prepared by the embodiment of the present invention 1.
Specific embodiment
The invention discloses a kind of lightweight heat-proof noise reduction SiO2The preparation method of aerogel material, it includes the following steps:
1) micella or microemulsion are prepared: 30mL deionized water being added in beaker, acidic catalyst is added and makes pH value of solution
=3~4,0.1~5g cationic surfactant is added after stirring 5min, stirs 20~60min；
2) prepare colloidal sol: being 1:(0.5~6 by the volume ratio of silicon source and deionized water) trifunctional silicon source is added, normal
Continue 3~5h of stirring under temperature, add ammonium hydroxide that a certain amount of molar concentration is 1~6.5mol/L until pH value of solution=7~8,
Continue 0.5~1h of stirring；
3) aging and displacement: wet gel aging two days at 40~80 DEG C, next spent under 40~80 DEG C of water-baths from
Sub- water replaces 8~12h, and ammonium hydroxide that molar concentration is 1~6.5mol/L is added to pH value of solution=9~10 in when displacement, removes surface
Activating agent and other unreacted substances.After replacing, replaced 3 times with ethyl alcohol at normal temperature, 8~12h every time；
4) dry: the wet gel replaced is put into can be in high-temperature and high-presure resistent container, and seals, and is added in a reservoir
CO2, and increasing temperature and pressure continues to replace in high temperature and high pressure kettle, makes gel pore afterwards for several times to the critical state of dried medium
Interior is liquid CO2, then decrease temperature and pressure, CO2Complete aeroge is obtained after being converted into gaseous state.
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
30mL deionized water is added in beaker, adds acetic acid and makes pH value of solution=3~4, stirring is added after five minutes
0.4g cetyl trimethylammonium bromide CTAB stirs 20min, 7.5mL methyltriethoxysilane MTES is then added, normal
Continue to stir 3h under temperature.Adding a certain amount of molar concentration is the ammonium hydroxide of 1mol/L up to pH value of solution=7, continues to stir 1h,
The gel under 60 DEG C of water-baths.Next wet gel aging two days at 60 DEG C are replaced 8h with deionized water under 60 DEG C of water-baths, are set
It is the ammonium hydroxide of 1mol/L to pH value of solution=9~10 that molar concentration is added when changing, and removes surfactant and other unreacted objects
Matter.After replacing, replaced 3 times with ethyl alcohol at normal temperature, each 12h.Finally use CO2Supercritical drying obtains SiO2Aeroge.
Embodiment 2
30mL deionized water is added in beaker, adds acetic acid and makes pH value of solution=3~4, stirring is added after five minutes
0.2g cetyl trimethylammonium bromide CTAB stirs 20min, 7.5mL methyltriethoxysilane MTES is then added, normal
Continue to stir 3h under temperature.Adding a certain amount of molar concentration is the ammonium hydroxide of 1mol/L up to pH value of solution=7, continues to stir 1h,
The gel under 60 DEG C of water-baths.Next wet gel aging two days at 60 DEG C are replaced 8h with deionized water under 60 DEG C of water-baths, are set
It is the ammonium hydroxide of 1mol/L to pH value of solution=9~10 that molar concentration is added when changing, and removes surfactant and other unreacted objects
Matter.After replacing, replaced 3 times with ethyl alcohol at normal temperature, each 12h.Finally use CO2Supercritical drying obtains SiO2Aeroge.
Embodiment 3
30mL deionized water is added in beaker, adds acetic acid and makes pH value of solution=3~4, stirring is added after five minutes
0.1g cetyl trimethylammonium bromide CTAB stirs 20min, 7.5mL methyltriethoxysilane MTES is then added, normal
Continue to stir 3h under temperature.Adding a certain amount of molar concentration is the ammonium hydroxide of 1mol/L up to pH value of solution=7, continues to stir 1h,
The gel under 60 DEG C of water-baths.Next wet gel aging two days at 60 DEG C are replaced 8h with deionized water under 60 DEG C of water-baths, are set
It is the ammonium hydroxide of 1mol/L to pH value of solution=9~10 that molar concentration is added when changing, and removes surfactant and other unreacted objects
Matter.After replacing, replaced 3 times with ethyl alcohol at normal temperature, each 12h.Finally use CO2Supercritical drying obtains SiO2Aeroge.
Embodiment 4
30mL deionized water is added in beaker, adds acetic acid and makes pH value of solution=3~4, stirring is added after five minutes
0.8g cetyl trimethylammonium bromide CTAB stirs 20min, 7.5mL methyltriethoxysilane MTES is then added, normal
Continue to stir 3h under temperature.Adding a certain amount of molar concentration is the ammonium hydroxide of 1mol/L up to pH value of solution=7, continues to stir 1h,
The gel under 60 DEG C of water-baths.Next wet gel aging two days at 60 DEG C are replaced 8h with deionized water under 60 DEG C of water-baths, are set
It is the ammonium hydroxide of 1mol/L to pH value of solution=9~10 that molar concentration is added when changing, and removes surfactant and other unreacted objects
Matter.After replacing, replaced 3 times with ethyl alcohol at normal temperature, each 12h.Finally use CO2Supercritical drying obtains SiO2Aeroge.
Embodiment 5
30mL deionized water is added in beaker, adds acetic acid and makes pH value of solution=3~4, stirring is added after five minutes
0.2g cetyl trimethylammonium bromide CTAB stirs 20min, 10mL methyltrimethoxysilane MTMS is then added, normal
Continue to stir 3h under temperature.Adding a certain amount of molar concentration is the ammonium hydroxide of 1mol/L up to pH value of solution=7, continues to stir 1h,
The gel under 60 DEG C of water-baths.Next wet gel aging two days at 60 DEG C are replaced 8h with deionized water under 60 DEG C of water-baths, are set
It is the ammonium hydroxide of 1mol/L to pH value of solution=9~10 that molar concentration is added when changing, and removes surfactant and other unreacted objects
Matter.After replacing, replaced 3 times with ethyl alcohol at normal temperature, each 12h.Finally use CO2Supercritical drying obtains SiO2Aeroge.
As shown in Figures 1 and 2, SiO is prepared in the present invention2Aerogel material, inside have porous structure, specific surface
Product is larger, has preferable application prospect in fields such as absorption, heat-insulated, noise reductions.
As shown in figure 3, SiO prepared by the present invention2Aerogel material has super-hydrophobicity, and hydrophobic angle reaches 168.8 °.
As shown in figure 4, SiO prepared by the present invention2Aerogel material has good heat-insulation and heat-preservation, and thermal conductivity exists
It is controllable between 0.015~0.025W/ (mK).
As shown in figure 5, SiO prepared by the present invention2Aerogel material, 1cm thickness material all band visible transparency is 5%
~90% is controllable.
As shown in fig. 6, SiO prepared by the present invention2Aerogel material has low-density, and density is in 30mg/cm3~100mg/
cm3Between it is controllable.
As shown in fig. 7, SiO prepared by the present invention2Aerogel material has good sound insulation property, for 1cm thickness density
For 60mg/cm3Material, between 500~1600HZ sound transmission loss be 13~21dB.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment
Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention
It is required that protection scope.
Claims (10)
1. a kind of lightweight heat-proof noise reduction SiO2The preparation method of aerogel material, it includes using trifunctional silicon source and cation
Surfactant through soda acid two-step method and stands the obtained aerogel material of displacement, the trifunctional silicon source molecule in aqueous solvent
The alkoxy grp of the non-polar group for not participating in hydrolytic condensation comprising one and three participation hydrolysis-condensation reactions.
2. lightweight heat-proof noise reduction SiO according to claim 12The preparation method of aerogel material, it is characterised in that: described three
Functional group's silicon source includes methyltriethoxysilane, methyltrimethoxysilane, ethyl triethoxysilane or ethyl trimethoxy
At least one of base silane.
3. lightweight heat-proof noise reduction SiO according to claim 1 or claim 22The preparation method of aerogel material, it is characterised in that: described
Cationic surfactant includes quaternary ammonium salt cationic surfactant.
4. lightweight heat-proof noise reduction SiO according to claim 1 or claim 22The preparation method of aerogel material, it is characterised in that: it is wrapped
Include following steps:
1) micella or microemulsion are prepared: taking acidic catalyst and deionized water to mix to obtain acid solution, adds cationic surface
Activating agent stirs to get micella or microemulsion；
2) it prepares colloidal sol: trifunctional silicon source being added into the micella or microemulsion of step 1), adds basic catalyst
Mixed solution is obtained, colloidal sol is made in sealing and standing；
3) aging and displacement: deionized water is added into colloidal sol described in step 2), takes out, is placed in ammonium hydroxide after to be aging, sealed
It stands, waits first time replacement completion；It continuously adds ethyl alcohol and completes second of displacement；
4) dry: the wet gel that step 3) has been replaced is placed in closed container, is handled through the dried medium in critical state,
Obtain aerogel material.
5. lightweight heat-proof noise reduction SiO according to claim 42The preparation method of aerogel material, it is characterised in that: step 1)
Described in acid solution pH value be 3~4, the acidic catalyst includes in hydrofluoric acid, hydrochloric acid, nitric acid, acetic acid or oxalic acid
It is at least one.
6. lightweight heat-proof noise reduction SiO according to claim 52The preparation method of aerogel material, it is characterised in that: step 1)
Described in cationic surfactant additional amount be every 30mL acid solution in be added 0.01g~5g.
7. lightweight heat-proof noise reduction SiO according to claim 42The preparation method of aerogel material, it is characterised in that: step 2)
Described in mixed solution pH value be 7~8；The basic catalyst includes ammonium hydroxide or sodium hydroxide.
8. according to claim 4 or 5 or the 6 or 7 lightweight heat-proof noise reduction SiO2The preparation method of aerogel material, feature exist
In: the sealing and standing in step 2) and step 3) is to carry out in the water-bath for being placed in 40 DEG C~80 DEG C.
9. lightweight heat-proof noise reduction SiO according to claim 42The preparation method of aerogel material, it is characterised in that: step 4)
Described in dried medium include ethyl alcohol or carbon dioxide.
10. a kind of lightweight heat-proof noise reduction SiO2Aerogel material, it is prepared into for any one of claim 1~9 preparation method
It arrives, it is characterised in that: the density of the aerogel material is 30mg/cm3~100mg/cm3, thermal conductivity is 0.015~0.025W/
(m·K)。
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Inventor after: Yang Zichun Inventor after: Li Xiaohua Inventor after: Li Kunfeng Inventor after: Chen Guobing Inventor after: Zhao Shuang Inventor after: Fei Zhifang Inventor after: Zhang Zhen Inventor before: Yang Zichun Inventor before: Li Xiaohua Inventor before: Li Kunfeng Inventor before: Chen Guobing Inventor before: Zhao Shuang Inventor before: Fei Zhifang Inventor before: Zhang Zhen |
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Application publication date: 20190920 |