CN110282632A - A kind of preparation method of multifunction flexible oxidation silica-based aerogel - Google Patents
A kind of preparation method of multifunction flexible oxidation silica-based aerogel Download PDFInfo
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- CN110282632A CN110282632A CN201910683710.1A CN201910683710A CN110282632A CN 110282632 A CN110282632 A CN 110282632A CN 201910683710 A CN201910683710 A CN 201910683710A CN 110282632 A CN110282632 A CN 110282632A
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- preparation
- based aerogel
- wet gel
- coupling agent
- silane coupling
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
Abstract
The present invention relates to a kind of preparation methods of multifunction flexible oxidation silica-based aerogel.Using silsesquioxane and silane coupling agent as silicon source, aldehyde be bonding agent, alcohol is solvent, deionized water is hydrolytic reagent, a step sol-gel technology of hydrolysis is promoted to prepare wet gel by the way that organic acid is added, wet gel is by hydro-thermal process and is dried to obtain multifunction flexible oxidation silica-based aerogel.Preparation process of the present invention is simple, at low cost, be conducive to large-scale industrial production, prepared multifunction flexible oxidation silica-based aerogel has good mechanical property and absorption property, and with 60~90% reversible compression deformation, density is 0.047~0.163cm3/ g, 120.6~233.7m of specific surface area2/ g, 0.017~0.027W/ of thermal conductivity (mK), Ethanol Adsorption 8.9~16.2g/g of amount, formaldehyde (10ppm) 3.8~7.2mmol/g of adsorbance, can be used for the fields such as low temperature environment, the heat-insulation and heat-preservation of Cryo Equipment, gas absorption and water process.
Description
Technical field
The invention belongs to the preparation fields of new material, are related to a kind of preparation side of multifunction flexible oxidation silica-based aerogel
Method.
Background technique
The three-dimensional porous network structure that there is aerogel material nano particle to constitute, this structure assign its low-density, height
The characteristics such as specific surface area, big nanometer pore volume and porosity, heat-insulation and heat-preservation, absorption, catalysis and in terms of show
Excellent properties are widely used in the numerous areas such as aerospace, defense military, petrochemical industry, energy saving building and front line science.It passes
The SiO of system2Aeroge passes through a step acid-catalyzed sol-gel method and supercritical drying mostly with siloxanes etc. for single silicon source
Technique preparation.One side supercritical drying process equipment investment is big, production capacity is low；On the other hand, traditional SiO2Aeroge intensity
Disadvantage low, brittleness is big and not resistant to water, significantly limits SiO2The use of aeroge.Application No. is
The Chinese patent of CN201210245085.0, CN201611228188.0 and CN201811344883.2 disclose several flexible airs
The preparation method of gel, but technique is cumbersome, production is time-consuming, and obtained flexible aeroge has a single function, and pore structure can not root
It is adjusted according to practical application, it is not high to the concern of mechanics compression performance.And multifunction flexible oxidation silica-based aerogel can solve
State traditional Si O2Disadvantage of the aeroge in production and application.
Summary of the invention
In order to improve existing SiO2Deficiency of the aerogel material in terms of mechanical property and production technology, the present invention provides
A kind of preparation method of multifunction flexible oxidation silica-based aerogel.The flexibility aoxidizes silica-based aerogel using quickly green low cost
Method preparation, and have good mechanical property and hydrophobicity, compensate for traditional Si O2Aerogel material in synthesis technology and
Deficiency in performance.
The object of the invention technical solution are as follows: a kind of preparation method of multifunction flexible oxidation silica-based aerogel is specific to walk
It is rapid as follows:
At (1) 20~50 DEG C, in molar ratio by silicon source, aldehyde, silane coupling agent, pore structure adjustment, pure and mild deionized water
0.1:(0.05~0.35): (0.05~0.35): (0.00005~0.005): (3~15): (1~3) stirs 5 after mixing
~30 minutes, the organic acid of addition continued stirring 5~30 minutes；Wherein silicon source and the molar ratio of organic acid be 0.1:(0.001~
0.005)；
(2) mixed liquor that step (1) obtains carries out sol gel reaction at 20~60 DEG C and obtains wet gel；
(3) the wet gel submergence that step (2) obtains is sealed in the hydrothermal reaction kettle full of solvent, at 50~250 DEG C
Solvent heat treatment 1~5 day, the wet gel to be strengthened；
(4) the reinforcing wet gel that step (3) obtains, which is placed in container at 20~60 DEG C, is dried to obtain flexible oxidation silicon substrate
Aeroge.
The appearance of the above-mentioned flexible oxidation silica-based aerogel being prepared is complete flawless bulk product, have 60~
90% reversible compression deformation, density are 0.047~0.163cm3/ g, 120.6~233.7m of specific surface area2/ g, hydrophobic angle 131
~151 °, 25 DEG C of 0.017~0.027W/ of room temperature thermal conductivity (mK), Ethanol Adsorption amount 8.9~16.2g/g, 10ppm concentration first
3.8~7.2mmol/g of aldehyde adsorbance.
Silicon source described in preferred steps (1) is methyltrimethoxysilane, methyltriethoxysilane, trimethyl methoxy
One of base silane or dimethyldimethoxysil,ne are a variety of.
Aldehyde described in preferred steps (1) is formaldehyde, o-phthalaldehyde, m-terephthal aldehyde, terephthalaldehyde or glutaraldehyde
One of.
Silane coupling agent described in preferred steps (1) is Silane coupling agent KH550, silane coupling agent KH560, silane idol
Join one of agent KH570 or silane coupling agent KH791.
Pore structure regulator described in preferred steps (1) is cetyl trimethylammonium bromide, cetyl trimethyl
One of ammonium chloride or triblock copolymer F127.
Alcohol described in preferred steps (1) is one of methanol or ethyl alcohol；The organic acid is acetic acid, oxalic acid or anti-
One of bad hematic acid.
The surface aperture degree 50~90% of container in preferred steps (3), aperture size are 1~5mm.
Solvent described in preferred steps (3) is one of water, methanol, ethyl alcohol or tert-butyl alcohol.
Drying mode described in preferred steps (4) is constant pressure and dry, vacuum drying or CO2One in supercritical drying
Kind.
The utility model has the advantages that
Multifunction flexible oxidation silica-based aerogel according to the present invention and its preparation process have the following characteristics that
(1) drying process used by has diversity, realizes the quick cost effective preparation of green of aerogel products.
(2) the flexible oxidation silica-based aerogel prepared by compensates for traditional Si O2The deficiency that aeroge intensity is low, brittleness is big,
It can bear up to 90% linear invertible compression.
(3) the flexible oxidation silica-based aerogel prepared by, can be applied to solid heat-insulation and heat-preservation, liquid adsorption purification and gas
Adsorbing and trapping realizes the multifunction of flexible aeroge.
Detailed description of the invention
Fig. 1 is the infrared spectroscopy that flexibility made from example 1 aoxidizes silica-based aerogel.
Fig. 2 is the hydrophobic schematic diagram that flexibility made from example 1 aoxidizes silica-based aerogel.
Fig. 3 is the compression experiment photo that flexibility made from example 1 aoxidizes silica-based aerogel；Wherein a figure is b figure before compression
For in compression, c figure is after restoring.
Specific embodiment
Example 1
At 20 DEG C, by 0.1mol methyltrimethoxysilane, 0.05mol o-phthalaldehyde, 0.35mol silane coupling agent
KH550,0.05mmol triblock copolymer F127,5mol methanol, 1mol deionized water stir 30 minutes after mixing, then
1mmol acetic acid is added and continues stirring 20 minutes；Above-mentioned mixed liquor carries out sol gel reaction at 20 DEG C and obtains wet gel, will
Wet gel submergence is sealed in water-filled hydrothermal reaction kettle, is heat-treated at 50 DEG C 5 days, replacement in during which every 12 hours is primary
Water.The wet gel of reinforcing is placed in after the completion of heat treatment true at 20 DEG C in the container of surface aperture degree 90%, aperture size 1mm
Sky is dried to obtain flexible oxidation silica-based aerogel.Flexibility oxidation silica-based aerogel density 0.163g/cm3, specific surface area 125.6m2/
G, 151 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.027W/ (mK), Ethanol Adsorption amount 15.6g/g, 10ppm concentration formaldehyde is inhaled
Attached amount 6.7mmol/g, reversible compression deformation and 100% ground of energy with 80% restore rapidly to original shape.
Referring to attached drawing, Fig. 1 is the infrared spectroscopy that flexibility made from example 1 aoxidizes silica-based aerogel.1193 and 1023cm-1Place
Strong absworption peak be respectively Si-O-Si antisymmetric stretching vibration and symmetrical stretching vibration, illustrate prepared aeroge sample
In contain a large amount of Si-O-Si key, that is to say, that the bulk composition of prepared aeroge sample be silica；1270 Hes
771cm-1The peak at place is Si-CH3Characteristic absorption peak, show the hydrophobic functional groups methyl in methyltrimethoxysilane anti-
Still it is connected with silicon atom after should completing, so that aeroge has excellent hydrophobicity.
Referring to attached drawing, Fig. 2 is the hydrophobic schematic diagram that flexibility made from example 1 aoxidizes silica-based aerogel.Hydrophobic test shows
The droplet on the oxidation of flexibility prepared by present invention silica-based aerogel surface is able to maintain the mellow and full orbicule of almost Perfect, hydrophobic angle
Up to 151 °, there is super-hydrophobicity.
Referring to attached drawing, Fig. 3 is the compression experiment photo of flexibility Hydrophobic silica aeroge made from example 1.Compression experiment
Use steel ruler for object of reference, using the cylindric sample of ratio of height to diameter 1:1.As can be seen that institute of the present invention from compression experiment photo
The flexible oxidation silica-based aerogel of preparation can withstand up to 80% linear invertible compression, and 100% ground of energy restores rapidly
To original shape, there is excellent mechanical property.
Example 2
At 30 DEG C, by 0.1mol methyltriethoxysilane, 0.35mol formaldehyde, 0.05mol silane coupling agent KH560,
2mmol hexadecyltrimethylammonium chloride, 6mol ethyl alcohol, 1mol deionized water stir 25 minutes after mixing, are then added
2.5mmol oxalic acid continues stirring 20 minutes；Above-mentioned mixed liquor carries out sol gel reaction at 30 DEG C and obtains wet gel, will be wet
Gel submergence is sealed in the hydrothermal reaction kettle full of methanol, is heat-treated at 100 DEG C 4 days, replacement in during which every 12 hours is primary
Methanol.The wet gel of reinforcing is placed in the container of surface aperture degree 80%, aperture size 2mm at 30 DEG C after the completion of heat treatment
Constant pressure and dry obtains flexible oxidation silica-based aerogel.Flexibility oxidation silica-based aerogel density 0.074cm3/ g, specific surface area
165.3m2/ g, 135 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.018W/ (mK), Ethanol Adsorption amount 10.6g/g, 10ppm be dense
Formaldehyde absorbing amount 4.1mmol/g is spent, reversible compression deformation and 100% ground of energy with 68% restore rapidly to original shape.
Example 3
At 40 DEG C, by 0.1mol trimethylmethoxysilane, 0.05mol terephthalaldehyde, 0.15mol silane coupling agent
KH570,1mmol cetyl trimethylammonium bromide, 9mol methanol, 3mol deionized water stir 15 minutes after mixing, so
5mmol ascorbic acid is added afterwards and continues stirring 15 minutes；Above-mentioned mixed liquor carries out sol gel reaction at 40 DEG C and obtains wet coagulate
Wet gel submergence is sealed in the hydrothermal reaction kettle full of the tert-butyl alcohol, is heat-treated at 150 DEG C 3 days, during which every 12 hours by glue
Replace a tert-butyl alcohol.The wet gel of reinforcing is placed in the container of surface aperture degree 70%, aperture size 3mm after the completion of heat treatment
In at 40 DEG C vacuum drying obtain flexible oxidation silica-based aerogel.Flexibility oxidation silica-based aerogel density 0.084cm3/ g, than
Surface area 148.1m2/ g, 134 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.024W/ (mK), Ethanol Adsorption amount 13.8g/g,
10ppm concentration formaldehyde absorbing amount 4.2mmol/g, reversible compression deformation and 100% ground of energy with 75% restore rapidly to original
There is shape.
Example 4
At 50 DEG C, by 0.1mol dimethyldimethoxysil,ne, 0.05mol m-terephthal aldehyde, 0.1mol silane coupling agent
KH791,0.1mmol triblock copolymer F127,3mol ethyl alcohol, 1mol deionized water stir 5 minutes after mixing, then plus
Enter 5mmol acetic acid and continues stirring 5 minutes；Above-mentioned mixed liquor carries out sol gel reaction at 30 DEG C and obtains wet gel, will be wet solidifying
Glue submergence is sealed in water-filled hydrothermal reaction kettle, is heat-treated at 200 DEG C 2 days, the water of replacement in during which every 12 hours.Heat
The wet gel of reinforcing is placed in in the container of surface aperture degree 85%, aperture size 1.5mm the CO at 50 DEG C after the completion of processing2It is super
It is critical to be dried to obtain flexible oxidation silica-based aerogel.Flexibility oxidation silica-based aerogel density 0.174cm3/ g, specific surface area
120.6m2/ g, 131 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.021W/ (mK), Ethanol Adsorption amount 16.2g/g, 10ppm be dense
Formaldehyde absorbing amount 7.2mmol/g is spent, reversible compression deformation and 100% ground of energy with 90% restore rapidly to original shape.
Example 5
At 35 DEG C, by 0.05mol methyltrimethoxysilane, 0.05mol dimethyldimethoxysil,ne, 0.2mol penta 2
Aldehyde, 0.1mol Silane coupling agent KH550,3mmol hexadecyltrimethylammonium chloride, 15mol methanol, the mixing of 3mol deionized water
Then stirring 20 minutes after uniformly are added 5mmol oxalic acid and continue stirring 15 minutes；Above-mentioned mixed liquor carries out colloidal sol-at 35 DEG C
Gel reaction obtains wet gel, and wet gel submergence is sealed in the hydrothermal reaction kettle full of methanol, is heat-treated 1 at 250 DEG C
It, the methanol of replacement in during which every 12 hours.The wet gel of reinforcing is placed in surface aperture degree 60%, aperture after the completion of heat treatment
Constant pressure and dry obtains flexible oxidation silica-based aerogel at 60 DEG C in the container of size 4mm.Flexibility oxidation silica-based aerogel density
0.047cm3/ g, specific surface area 233.7m2/ g, 144 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.017W/ (mK), Ethanol Adsorption
8.9g/g, 10ppm concentration formaldehyde absorbing amount 4.4mmol/g are measured, reversible compression deformation and 100% ground of energy with 60% are rapid
Restore to original shape.
Example 6
At 25 DEG C, by 0.1mol methyltriethoxysilane, 0.1mol trimethylmethoxysilane, 0.1mol dimethyl two
Methoxy silane, 0.45mol o-phthalaldehyde, 0.9mol silane coupling agent KH791,15mmol cetyl trimethyl bromination
Ammonium, 36mol ethyl alcohol, 6mol deionized water stir 30 minutes after mixing, and 9mmol ascorbic acid is then added and continues stirring 30
Minute；Above-mentioned mixed liquor carries out sol gel reaction at 50 DEG C and obtains wet gel, and wet gel submergence is sealed in full of ethyl alcohol
Hydrothermal reaction kettle in, be heat-treated at 150 DEG C 3 days, the ethyl alcohol of replacement in during which every 12 hours.It will strengthen after the completion of heat treatment
Wet gel be placed in the container of surface aperture degree 50%, aperture size 5mm at 40 DEG C be dried in vacuo 2 hours, then 60 DEG C at
Vacuum drying obtains flexible oxidation silica-based aerogel for 2 hours.Flexibility oxidation silica-based aerogel density 0.064cm3/ g, specific surface area
146.9m2/ g, 139 ° of water contact angle, 25 DEG C of room temperature thermal conductivity 0.026W/ (mK), Ethanol Adsorption amount 11.4g/g, 10ppm be dense
Formaldehyde absorbing amount 3.8mmol/g is spent, reversible compression deformation and 100% ground of energy with 73% restore rapidly to original shape.
Claims (10)
1. a kind of preparation method of multifunction flexible oxidation silica-based aerogel, the specific steps of which are as follows:
At (1) 20~50 DEG C, silicon source, aldehyde, silane coupling agent, pore structure are adjusted, pure and mild deionized water in molar ratio 0.1:
(0.05~0.35): (0.05~0.35): (0.00005~0.005): (3~15): (1~3) stirs 5~30 after mixing
Minute, the organic acid of addition continues stirring 5~30 minutes；Wherein silicon source and the molar ratio of organic acid be 0.1:(0.001~
0.005)；
(2) mixed liquor that step (1) obtains carries out sol gel reaction at 20~60 DEG C and obtains wet gel；
(3) the wet gel submergence that step (2) obtains is sealed in the hydrothermal reaction kettle full of solvent, the solvent at 50~250 DEG C
Heat treatment 1~5 day, the wet gel to be strengthened；
(4) the reinforcing wet gel that step (3) obtains, which is placed in container at 20~60 DEG C, is dried to obtain flexible oxidation silicon substrate airsetting
Glue.
2. preparation method according to claim 1, it is characterised in that outside the flexible oxidation silica-based aerogel being prepared
Seeing is complete flawless bulk product, and with 60~90% reversible compression deformation, density is 0.047~0.163cm3/ g, than
120.6~233.7m of surface area2/ g, 131~151 ° of hydrophobic angle, 25 DEG C of 0.017~0.027W/ of room temperature thermal conductivity (mK), second
3.8~7.2mmol/g of alcohol adsorbance 8.9~16.2g/g, 10ppm concentration formaldehyde absorbing amount.
3. preparation method according to claim 1, it is characterised in that silicon source described in step (1) is methyl trimethoxy oxygroup
One of silane, methyltriethoxysilane, trimethylmethoxysilane or dimethyldimethoxysil,ne are a variety of.
4. preparation method according to claim 1, it is characterised in that aldehyde described in step (1) is formaldehyde, O-phthalic
One of aldehyde, m-terephthal aldehyde, terephthalaldehyde or glutaraldehyde.
5. preparation method according to claim 1, it is characterised in that silane coupling agent described in step (1) is that silane is even
Join one of agent KH550, silane coupling agent KH560, silane coupling agent KH570 or silane coupling agent KH791.
6. preparation method according to claim 1, it is characterised in that pore structure regulator described in step (1) is 16
One of alkyl trimethyl ammonium bromide, hexadecyltrimethylammonium chloride or triblock copolymer F127.
7. preparation method according to claim 1, it is characterised in that alcohol described in step (1) is in methanol or ethyl alcohol
It is a kind of；The organic acid is one of acetic acid, oxalic acid or ascorbic acid.
8. preparation method according to claim 1, it is characterised in that the surface aperture degree 50 of container in step (3)~
90%, aperture size is 1~5mm.
9. preparation method according to claim 1, it is characterised in that solvent described in step (3) is water, methanol, ethyl alcohol
Or one of tert-butyl alcohol.
10. preparation method according to claim 1, it is characterised in that drying mode described in step (4) is dry for normal pressure
Dry, vacuum drying or CO2One of supercritical drying.
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Cited By (3)
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| CN114408932A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
| CN114405457A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Preparation method of impregnation-modified flexible hydrophobic spherical silicon-based aerogel adsorbent |
| CN114805913A (en) * | 2022-04-29 | 2022-07-29 | 重庆大学 | Novel insulating material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114408932A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
| CN114405457A (en) * | 2022-02-18 | 2022-04-29 | 南京工业大学 | Preparation method of impregnation-modified flexible hydrophobic spherical silicon-based aerogel adsorbent |
| CN114408932B (en) * | 2022-02-18 | 2023-09-26 | 南京工业大学 | Method for preparing silica-based aerogel balls with controllable particle size by continuous liquid phase polymerization |
| CN114405457B (en) * | 2022-02-18 | 2023-12-22 | 南京工业大学 | Preparation method of impregnation modified flexible hydrophobic spherical silicon-based aerogel adsorbent |
| CN114805913A (en) * | 2022-04-29 | 2022-07-29 | 重庆大学 | Novel insulating material and preparation method and application thereof |
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