CN109851380A - A kind of preparation method of aerosil functional material - Google Patents
A kind of preparation method of aerosil functional material Download PDFInfo
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- CN109851380A CN109851380A CN201910154010.3A CN201910154010A CN109851380A CN 109851380 A CN109851380 A CN 109851380A CN 201910154010 A CN201910154010 A CN 201910154010A CN 109851380 A CN109851380 A CN 109851380A
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Abstract
The present invention relates to a kind of preparation methods of aerosil functional material, belong to aeroge technical field.The present invention prepares aerosil functional material by carbonization treatment, can not only keep original nanoporous network structure, but also have many excellent characteristics, and if specific surface area is high, mass density is low, the continuous hole of nanoscale, mechanical property is good；Montmorillonite is a kind of two-dimensional molecular sieve analog porous mass, since it is with the performances such as big specific surface area and big adsorption capacity, make its absorption, hydrogen storage, catalysis, bio-separation, electronic device and in terms of be widely used, pass through carbonization treatment, utilize the expansiveness of the layer structure of montmorillonite, the interchangeability energy of cation, some inorganic cations are inserted into its interlayer, the layer of montmorillonite is strutted with layer, the two-dimensional channel with opening is formed, so that the adsorptivity and mechanical property of aerosil functional material are improved.
Description
Technical field
The present invention relates to a kind of preparation methods of aerosil functional material, belong to aeroge technical field.
Background technique
Aeroge is a kind of tridimensional nano net structure solid material being piled by nano particle or the high-polymer molecule.
Gas decentralized medium is filled in its nanoaperture.Due to its with porosity height, large specific surface area, thermal conductivity is low, density is low,
The excellent characteristics such as refractive index is low, transmitance is high, and dielectric constant is low, can be applicable to construction material, sensor, catalyst carrier, light
Learn the fields such as material.
Sol-gel technique is to make predecessor with metal alkoxide or metalloid alkoxide, in comparatively gentle certain reaction
Under the conditions of, by hydrolysis condensation reaction, so that sol particle or monomer connect to form three-dimensional network junction structure, form gel.Benefit
SiO is prepared with sol-gel technique2Airsetting adhesive process is broadly divided into two steps: (1) sol-gel prepares SiO2Wet gel；(2) right
Wet gel is dried to form aeroge.When the liquid in gel network hole is water or alcohol, corresponding wet gel is respectively
Hydrogel or alcogel；It is referred to as xerogel with the material that conventional drying process obtains.Only when the liquid quilt in gel network
Air substitution, when network structure or gel volume remain unchanged, referred to as aeroge.
Aeroge has very small thermal conductivity, is the 1~10% of general solid thermal conductance, in addition, it includes very small
The measurements of the chest, waist and hips network structure that particle is cross-linked to form, and there are many closed ends, the heat transfer of internal solids is needed by very bent
The path of folding, therefore effectively weakened.
SiO2Aeroge can use lower-cost presoma and prepare in normal pressure, therefore have very high commercial potential.
In civil field, aeroge be can be applied in the insulation system of insulation, solar collector coating, pipeline of building etc..
If aeroge glass can substitute general cladding glass, the thermal insulation property for not only improving glass wall also acts as fireproofing function.
The heat-barrier material very low as a kind of density, aeroge can be used for substituting refrigerator cold-storage heat-barrier material --- polyurethane foam modeling
Material.Current this polyurethane foam is advanced in refrigerator outer wall by fluorochlorohydrocarbon class propellant, can be inevitably generated non-
The fluorochlorohydrocarbon substance of environmental protection, this material, which is replaced with aeroge, can solve these problems.
As a kind of novel porous functional material, SiO2The hole and solid phase particulates of aeroge internal structure are nanometers
Magnitude, therefore there are high porosity, lower thermal conductivity, high-specific surface area, low-k and the excellent properties such as material is translucent,
There is huge application prospect in the fields such as super insulating material, catalyst and carrier, adsorbent material.
Preparation method and Study on functional properties comparative maturity at present, but SiO2Aeroge is applied with industrialization still
So there are problems, such as: supercritical drying risk is big, and air drying long preparation period, technique is cumbersome and solvent usage
Greatly, aeroge serious cracking, intensity are lower.More air drying preparation process, obtained SiO are especially applied at present2Gas
Gel Tear is than more serious, globality is poor, the low-density of these defects and aeroge, irregular pore structure, unordered three-dimensional
Non- accuracy connection and intensive agglomerate into density gradient etc. and have direct relation between network morphology, particle, these are all limitations
The bottleneck of pure silicon dioxide aeroge application.Pure SiO is solved at present2The method of the various defects of aeroge concentrates on enhancing initial life
At network of silica toughness and stability in terms of, it is main to enhance skeletons and further by adding various functional materials
Silica three-dimensional network is agglomerated with molecular precursor, obtains various SiO2Aerogel composite, to make up or be promoted gas
The property of gel.
Summary of the invention
The technical problems to be solved by the invention: it for the problem that existing aerosil mechanical property is poor, mentions
A kind of preparation method of aerosil functional material is supplied.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) montmorillonite, carbon fiber, galactooligosaccharide, deionized water are taken, montmorillonite and deionized water are mixed, carries out ultrasound point
Processing is dissipated to get dispersion liquid, carbon fiber, ultrasonic disperse and magnetic agitation processing is added in dispersion liquid to get mixed liquor, is being mixed
Close liquid in galactooligosaccharide is added, continue 1~2h of stirring to get matrix liquid, filter to obtain filter residue, by filter residue be placed in temperature be 60~
It dries in 80 DEG C of baking oven to constant weight, is cooled to room temperature to get filler；
(2) take ethyl orthosilicate, dehydrated alcohol, deionized water, filler, n,N-Dimethylformamide, mass fraction be 1% hydrochloric acid,
Mass fraction be 1% ammonium hydroxide, by ethyl orthosilicate, dehydrated alcohol, deionized water and filler mix, at room temperature magnetic agitation 10~
For 15min to get mixture A, it is 1% hydrochloric acid that mass fraction, which is added, in mixture A, continues 30~40min of stirring to get mixing
Object B, is added n,N-Dimethylformamide in mixture B and mass fraction is 1% ammonium hydroxide, stirs evenly up to semi-finished product；
(3) by semi-finished product be aged and aging process to get age gelation, by age gelation immersion treatment to get immersion after
Desiccant gel is placed in calcination processing in Muffle furnace, with furnace temperature to get desiccant gel by gel drying processing after immersion by gel
Cooling is to get aerosil functional material.
Montmorillonite described in step (1), carbon fiber, galactooligosaccharide, the ratio between deionized water are respectively as follows: by weight
Number meter weighs 20~30 parts of montmorillonites, 1~10 part of carbon fiber, 1~5 part of galactooligosaccharide, 50~60 parts of deionizations respectively
Water.
Montmorillonite and deionized water are mixed described in step (1), carry out ultrasonic disperse processing step are as follows: by montmorillonite and
Deionized water mixing, 20~30min of ultrasonic disperse in the case where power is 200~300W.
Carbon fiber, ultrasonic disperse and magnetic agitation processing step is added described in step (1) in dispersion liquid are as follows: dispersing
Be added carbon fiber in liquid, continue 5~10min of ultrasonic disperse, and in the case where revolving speed is 100~160r/min magnetic agitation 30~
40min。
Ethyl orthosilicate, dehydrated alcohol, deionized water, filler, n,N-Dimethylformamide, quality described in step (2)
Score is 1% hydrochloric acid, mass fraction is that ratio between 1% ammonium hydroxide is respectively as follows: according to parts by weight, is weighing 20~30 parts respectively just
Silester, 40~50 parts of dehydrated alcohols, 20~30 parts of deionized waters, 10~15 parts of fillers, 1~5 part of N, N- dimethyl formyl
Amine, 1~3 part of mass fraction are 1% hydrochloric acid, 1~3 part of mass fraction is 1% ammonium hydroxide.
Semi-finished product be aged simultaneously aging process step described in step (3) are as follows: semi-finished product are aged 1~2 at room temperature
After it, be placed in Ageing solution temperature be 40~60 DEG C at each aging process 1~2 day.
By age gelation immersion treatment step described in step (3) are as follows: use acetone soak age gelation 3~5 times, soak every time
Steep 5~10min.
Described in step (3) will impregnate after gel drying processing step are as follows: by gel after immersion temperature be 100~150
Dry 1~2h at DEG C.
Desiccant gel is placed in calcination processing step in Muffle furnace described in step (3) are as follows: desiccant gel is placed in Muffle
In furnace, nitrogen is passed through with the air velocity of 50mL/min, 1~2h of holding at 250~300 DEG C is warming up to, is continuously heating to 1000
3~4h is kept at~1100 DEG C.
It is 20% ethanol water and mass fraction is 20% ethyl orthosilicate-second that the Ageing solution, which is respectively mass fraction,
Alcoholic solution.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention mixes montmorillonite and carbon fiber in water phase, prepares a kind of filler, and two components form " plastering hedge
The structure of wall " plays synergistic effect to the compressive strength for improving aeroge, and the addition of galactooligosaccharide improves carbon fiber
Between bonding, play the role of improve physical crosslinking intensity, thus significantly improve aeroge compression modulus and compression bend
Take intensity；
(2) silicon source reacts to form monomer in preparation process of the present invention, aggregates into primary particle between each monomer, to obtain sol body
System；Primary particle is gradually grown up, and particle connection under mutual collision forms cluster；Cluster further polymerize, and ultimately forms mutually
The chain three-dimensional network-like structure of crosslinking, then forms gel；Wet gel is usually silicon source under the action of acidand basecatalysts
It is obtained by hydrolysis and polycondensation, wet gel has just formed that back skeleton intensity is lower, and aging is the equal of the continuation of gelation, leads to
Crossing aging can be improved the network skeleton intensity of wet gel, and alcogel is obtained after aging, finally by dry removal gel pore
Interior liquid is to obtain aeroge；
(3) present invention prepares aerosil functional material by carbonization treatment, can not only keep original nanometer
Porous network structure, but also there are many excellent characteristics, if specific surface area is high, mass density is low, the continuous hole of nanoscale,
Mechanical property is good；Montmorillonite is a kind of two-dimensional molecular sieve analog porous mass, since it is with big specific surface area and big absorption
The performances such as capacity, make its absorption, hydrogen storage, catalysis, bio-separation, electronic device and in terms of obtained it is extensive
Using by carbonization treatment, using the expansiveness of the layer structure of montmorillonite, the interchangeability energy of cation, by some nothings
Machine cation is inserted into its interlayer, and layer and the layer of montmorillonite are strutted, and the two-dimensional channel with opening is formed, so that silica gas
The adsorptivity and mechanical property of gel functional material are improved；
(4) present invention uses soda acid two-step catalysis method, hydrolyzes in acid condition, gel under alkaline condition, the water under acid catalysis
Solution reaction is a kind of electrophilic reaction, H+- OR in first attack silicon source molecule simultaneously makes its protonation, cause electron cloud to-
OR offset, makes the other side surface void of silicon atomic core increase and present electrophilicity, the stronger anion attack silicon of elecrtonegativity
Ion hydrolyzes silicon source, reduces hydrolysis rate since-OR increases steric hindrance, in the case, H in solution+Concentration control reaction
Rate, pH is lower, and reaction rate is faster, and the hydrolysis of this type primarily forms short chain, and the polymer network because obtained from is weaker；
And when base catalyst is added, silicon atomic core will obtain a negative electrical charge in pilot process, due to the circumnuclear easy attraction of silicon atom
The inducing action of the-OH and-OSi of electronics can stablize the negative electrical charge, be conducive to hydrolyze, and thus solve merely with base catalysis
When hydrolysis initial stage due to-OR steric effect and the problem that keeps first-OH hydrolysis difficult, to greatly accelerate hydrolysis speed
For hydrolysis under base catalysis OH occurs for degree-OH in the necleophilic reaction of replacement-OR group, reaction rate and solution-Concentration has
It closes, hydrolysis is slow, and polymerization reaction is fast, can form highly cross-linked polymer or colloidal solid.
Specific embodiment
According to parts by weight, 20~30 parts of montmorillonites, 1~10 part of carbon fiber, 1~5 part of galactooligosaccharide, 50 are weighed respectively
~60 parts of deionized waters mix montmorillonite and deionized water, 20~30min of ultrasonic disperse in the case where power is 200~300W, i.e.,
Dispersion liquid is obtained, carbon fiber is added in dispersion liquid, continues 5~10min of ultrasonic disperse, and in the case where revolving speed is 100~160r/min
Galactooligosaccharide is added to get mixed liquor in 30~40min of magnetic agitation in mixed liquor, continues 1~2h of stirring to get matrix
Liquid filters to obtain filter residue, and filter residue is placed in the baking oven that temperature is 60~80 DEG C and is dried to constant weight, is cooled to room temperature to get filler；
According to parts by weight, 20~30 parts of ethyl orthosilicates, 40~50 parts of dehydrated alcohols, 20~30 parts of deionized waters, 10 are weighed respectively
~15 parts of fillers, 1~5 part of n,N-Dimethylformamide, 1~3 part of mass fraction are 1% hydrochloric acid, 1~3 part of mass fraction is 1% ammonia
Water mixes ethyl orthosilicate, dehydrated alcohol, deionized water and filler, and 10~15min of magnetic agitation is at room temperature to get mixing
Object A, it is 1% hydrochloric acid that mass fraction, which is added, in mixture A, continues 30~40min of stirring to get mixture B, in mixture B
N,N-Dimethylformamide is added and mass fraction is 1% ammonium hydroxide, stirs evenly up to semi-finished product, semi-finished product is aged 1 at room temperature
After~2 days, be placed in Ageing solution temperature be 40~60 DEG C at each aging process 1~2 day, Ageing solution is respectively that mass fraction is
20% ethanol water and mass fraction are 20% ethyl orthosilicate-ethanol solution to get age gelation, solidifying with acetone soak aging
Glue 3~5 times, 5~10min of immersion is dry at being 100~150 DEG C in temperature by gel after immersion to get gel after immersion every time
Desiccant gel is placed in Muffle furnace by 1~2h to get desiccant gel, is passed through nitrogen with the air velocity of 50mL/min, is warming up to
1~2h is kept at 250~300 DEG C, is continuously heating to keep 3~4h at 1000~1100 DEG C, it is cooling to get titanium dioxide with furnace temperature
Silica aerogel functional material.
Montmorillonite, carbon fiber, galactooligosaccharide, deionized water are taken, montmorillonite and deionized water are mixed, is carried out at ultrasound
To get dispersion liquid carbon fiber is added, simultaneously magnetic agitation processing is to get mixed liquor for ultrasonic disperse, in mixed liquor in reason in dispersion liquid
Middle addition galactooligosaccharide continues to stir 1h to get matrix liquid, filters to obtain filter residue, filter residue is placed in the baking oven that temperature is 60 DEG C
Middle drying is cooled to room temperature to constant weight to get filler；Take ethyl orthosilicate, dehydrated alcohol, deionized water, filler, N, N- diformazan
Base formamide, mass fraction are 1% hydrochloric acid, mass fraction is 1% ammonium hydroxide, by ethyl orthosilicate, dehydrated alcohol, deionized water and are filled out
Material mixing, for magnetic agitation 10min to get mixture A, it is 1% hydrochloric acid that mass fraction, which is added, in mixture A at room temperature, continues to stir
30min is mixed to get mixture B, n,N-Dimethylformamide is added in mixture B and mass fraction is 1% ammonium hydroxide, stirring is equal
Even semi-finished product to obtain the final product；Semi-finished product be aged and aging process is to get age gelation, by age gelation immersion treatment to get
Desiccant gel is placed in calcination processing in Muffle furnace to get desiccant gel by gel drying processing after immersion by gel after immersion,
It is cooling to get aerosil functional material with furnace temperature.Montmorillonite, carbon fiber, galactooligosaccharide, between deionized water
Ratio is respectively as follows: according to parts by weight, weighs 20 parts of montmorillonites, 1 part of carbon fiber, 1 part of galactooligosaccharide, 50 parts of deionizations respectively
Water.Montmorillonite and deionized water are mixed, ultrasonic disperse processing step is carried out are as follows: is mixed montmorillonite and deionized water, in function
Rate is ultrasonic disperse 20min under 200W.Carbon fiber, ultrasonic disperse and magnetic agitation processing step are added in dispersion liquid are as follows:
Carbon fiber is added in dispersion liquid, continues ultrasonic disperse 5min, and the magnetic agitation 30min in the case where revolving speed is 100r/min.Positive silicic acid
Ethyl ester, dehydrated alcohol, deionized water, filler, n,N-Dimethylformamide, mass fraction are 1% hydrochloric acid, mass fraction is 1% ammonia
Ratio between water is respectively as follows: according to parts by weight, weigh respectively 20 parts of ethyl orthosilicates, 40 parts of dehydrated alcohols, 20 parts go from
Sub- water, 10 parts of fillers, 1 part of n,N-Dimethylformamide, 1 part of mass fraction are 1% hydrochloric acid, 1 part of mass fraction is 1% ammonium hydroxide.It will
Semi-finished product be aged and aging process step are as follows: after semi-finished product are aged 1 day at room temperature, being placed in Ageing solution in temperature is 40
Each aging process 1 day at DEG C.By age gelation immersion treatment step are as follows: use acetone soak age gelation 3 times, impregnate every time
5min.Gel drying processing step after impregnating are as follows: dry 1h at being 100 DEG C in temperature by gel after immersion.By desiccant gel
It is placed in calcination processing step in Muffle furnace are as follows: desiccant gel is placed in Muffle furnace, nitrogen is passed through with the air velocity of 50mL/min
Gas is warming up at 250 DEG C and keeps 1h, is continuously heating to keep 3h at 1000 DEG C.Ageing solution is respectively that mass fraction is 20% ethyl alcohol
Aqueous solution and mass fraction are 20% ethyl orthosilicate-ethanol solution.
Montmorillonite, carbon fiber, galactooligosaccharide, deionized water are taken, montmorillonite and deionized water are mixed, carries out ultrasound point
Processing is dissipated to get dispersion liquid, carbon fiber, ultrasonic disperse and magnetic agitation processing is added in dispersion liquid to get mixed liquor, is being mixed
It closes in liquid and galactooligosaccharide is added, continue to stir 1h to get matrix liquid, filter to obtain filter residue, it is 70 DEG C that filter residue, which is placed in temperature,
It dries in baking oven to constant weight, is cooled to room temperature to get filler；Take ethyl orthosilicate, dehydrated alcohol, deionized water, filler, N, N-
Dimethylformamide, mass fraction are 1% hydrochloric acid, mass fraction is 1% ammonium hydroxide, by ethyl orthosilicate, dehydrated alcohol, deionized water
It is mixed with filler, for magnetic agitation 12min to get mixture A, it is 1% hydrochloric acid that mass fraction is added in mixture A at room temperature, after
For continuous stirring 35min to get mixture B, it is 1% ammonium hydroxide that n,N-Dimethylformamide and mass fraction, which is added, in mixture B, is stirred
It mixes uniformly up to semi-finished product；Semi-finished product be aged and aging process is to get age gelation, by age gelation immersion treatment,
Up to gel after immersion, desiccant gel is placed in Muffle furnace at calcining by gel drying processing after immersion to get desiccant gel
Reason, it is cooling to get aerosil functional material with furnace temperature.Montmorillonite, carbon fiber, galactooligosaccharide, deionized water it
Between ratio be respectively as follows: according to parts by weight, weigh respectively 25 parts of montmorillonites, 5 parts of carbon fibers, 3 parts of galactooligosaccharides, 55 parts go
Ionized water.Montmorillonite and deionized water are mixed, ultrasonic disperse processing step is carried out are as follows: montmorillonite and deionized water are mixed,
The ultrasonic disperse 25min in the case where power is 250W.Carbon fiber, ultrasonic disperse and magnetic agitation processing step are added in dispersion liquid
Are as follows: carbon fiber is added in dispersion liquid, continues ultrasonic disperse 8min, and the magnetic agitation 35min in the case where revolving speed is 130r/min.Just
Silester, dehydrated alcohol, deionized water, filler, n,N-Dimethylformamide, mass fraction are 1% hydrochloric acid, mass fraction is
Ratio between 1% ammonium hydroxide is respectively as follows: according to parts by weight, weighs 25 parts of ethyl orthosilicates, 45 parts of dehydrated alcohols, 25 parts respectively
Deionized water, 12 parts of fillers, 3 parts of n,N-Dimethylformamide, 2 parts of mass fractions are 1% hydrochloric acid, 2 parts of mass fractions are 1% ammonia
Water.Semi-finished product be aged simultaneously aging process step are as follows: after semi-finished product are aged 1 day at room temperature, be placed in Ageing solution in temperature
Degree is each aging process 1 day at 50 DEG C.By age gelation immersion treatment step are as follows: use acetone soak age gelation 4 times, soak every time
Steep 8min.Gel drying processing step after impregnating are as follows: dry 1h at being 125 DEG C in temperature by gel after immersion.It will be dry solidifying
Glue is placed in calcination processing step in Muffle furnace are as follows: desiccant gel is placed in Muffle furnace, is passed through with the air velocity of 50mL/min
Nitrogen is warming up at 275 DEG C and keeps 1h, is continuously heating to keep 3h at 1050 DEG C.Ageing solution is respectively that mass fraction is 20% second
Alcohol solution and mass fraction are 20% ethyl orthosilicate-ethanol solution.
Montmorillonite, carbon fiber, galactooligosaccharide, deionized water are taken, montmorillonite and deionized water are mixed, carries out ultrasound point
Processing is dissipated to get dispersion liquid, carbon fiber, ultrasonic disperse and magnetic agitation processing is added in dispersion liquid to get mixed liquor, is being mixed
It closes in liquid and galactooligosaccharide is added, continue to stir 2h to get matrix liquid, filter to obtain filter residue, it is 80 DEG C that filter residue, which is placed in temperature,
It dries in baking oven to constant weight, is cooled to room temperature to get filler；Take ethyl orthosilicate, dehydrated alcohol, deionized water, filler, N, N-
Dimethylformamide, mass fraction are 1% hydrochloric acid, mass fraction is 1% ammonium hydroxide, by ethyl orthosilicate, dehydrated alcohol, deionized water
It is mixed with filler, for magnetic agitation 15min to get mixture A, it is 1% hydrochloric acid that mass fraction is added in mixture A at room temperature, after
For continuous stirring 40min to get mixture B, it is 1% ammonium hydroxide that n,N-Dimethylformamide and mass fraction, which is added, in mixture B, is stirred
It mixes uniformly up to semi-finished product；Semi-finished product be aged and aging process is to get age gelation, by age gelation immersion treatment,
Up to gel after immersion, desiccant gel is placed in Muffle furnace at calcining by gel drying processing after immersion to get desiccant gel
Reason, it is cooling to get aerosil functional material with furnace temperature.Montmorillonite, carbon fiber, galactooligosaccharide, deionized water it
Between ratio be respectively as follows: according to parts by weight, weigh 30 parts of montmorillonites, 10 parts of carbon fibers, 5 parts of galactooligosaccharides, 60 parts respectively
Deionized water.Montmorillonite and deionized water are mixed, carry out ultrasonic disperse processing step are as follows: mix montmorillonite and deionized water
It closes, the ultrasonic disperse 30min in the case where power is 300W.Carbon fiber, ultrasonic disperse and magnetic agitation processing step are added in dispersion liquid
Suddenly are as follows: carbon fiber is added in dispersion liquid, continues ultrasonic disperse 10min, and the magnetic agitation in the case where revolving speed is 160r/min
40min.Ethyl orthosilicate, dehydrated alcohol, deionized water, filler, n,N-Dimethylformamide, mass fraction are 1% hydrochloric acid, matter
It measures ratio of the score between 1% ammonium hydroxide to be respectively as follows: according to parts by weight, weighs 30 parts of ethyl orthosilicates, 50 parts of anhydrous second respectively
Alcohol, 30 parts of deionized waters, 15 parts of fillers, 5 parts of n,N-Dimethylformamide, 3 parts of mass fractions are 1% hydrochloric acid, 3 parts of mass fractions
For 1% ammonium hydroxide.Semi-finished product be aged simultaneously aging process step are as follows: after semi-finished product are aged 2 days at room temperature, be placed in Ageing solution
In temperature be 60 DEG C at each aging process 2 days.By age gelation immersion treatment step are as follows: it uses acetone soak age gelation 5 times,
10min is impregnated every time.Gel drying processing step after impregnating are as follows: dry 2h at being 150 DEG C in temperature by gel after immersion.It will
Desiccant gel is placed in calcination processing step in Muffle furnace are as follows: desiccant gel is placed in Muffle furnace, with the gas velocity of 50mL/min
Degree is passed through nitrogen, is warming up at 300 DEG C and keeps 2h, is continuously heating to keep 4h at 1100 DEG C.Ageing solution is respectively mass fraction
It is 20% ethyl orthosilicate-ethanol solution for 20% ethanol water and mass fraction.
Experiment shows: SiO prepared by the present invention2The mechanical strength of aeroge is by 1.6 × 104Pa increases to 1.2 × 105Pa,
Thermal conductivity under room temperature is 0.029W/mK, and for porosity up to 80%~99.8%, aperture size compares table between 1~100nm
Area may be up to 1000m2/g。
Claims (10)
1. a kind of preparation method of aerosil functional material, it is characterised in that specific preparation step are as follows:
(1) montmorillonite, carbon fiber, galactooligosaccharide, deionized water are taken, montmorillonite and deionized water are mixed, carries out ultrasound point
Processing is dissipated to get dispersion liquid, carbon fiber, ultrasonic disperse and magnetic agitation processing is added in dispersion liquid to get mixed liquor, is being mixed
Close liquid in galactooligosaccharide is added, continue 1~2h of stirring to get matrix liquid, filter to obtain filter residue, by filter residue be placed in temperature be 60~
It dries in 80 DEG C of baking oven to constant weight, is cooled to room temperature to get filler；
(2) take ethyl orthosilicate, dehydrated alcohol, deionized water, filler, N,N-dimethylformamide, mass fraction be 1% hydrochloric acid,
Mass fraction be 1% ammonium hydroxide, by ethyl orthosilicate, dehydrated alcohol, deionized water and filler mix, at room temperature magnetic agitation 10~
For 15min to get mixture A, it is 1% hydrochloric acid that mass fraction, which is added, in mixture A, continues 30~40min of stirring to get mixing
Object B, is added n,N-Dimethylformamide in mixture B and mass fraction is 1% ammonium hydroxide, stirs evenly up to semi-finished product；
(3) by semi-finished product be aged and aging process to get age gelation, by age gelation immersion treatment to get immersion after
Desiccant gel is placed in calcination processing in Muffle furnace, with furnace temperature to get desiccant gel by gel drying processing after immersion by gel
Cooling is to get aerosil functional material.
2. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(1) ratio between montmorillonite, carbon fiber, galactooligosaccharide, deionized water described in is respectively as follows: according to parts by weight, respectively
Weigh 20~30 parts of montmorillonites, 1~10 part of carbon fiber, 1~5 part of galactooligosaccharide, 50~60 parts of deionized waters.
3. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(1) mixing montmorillonite and deionized water described in, carries out ultrasonic disperse processing step are as follows: mix montmorillonite and deionized water
It closes, 20~30min of ultrasonic disperse in the case where power is 200~300W.
4. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(1) carbon fiber, ultrasonic disperse and magnetic agitation processing step are added in dispersion liquid described in are as follows: carbon fiber is added in dispersion liquid
Dimension continues 5~10min of ultrasonic disperse, and 30~40min of magnetic agitation in the case where revolving speed is 100~160r/min.
5. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(2) ethyl orthosilicate, dehydrated alcohol, deionized water, filler, N,N-dimethylformamide, mass fraction described in be 1% hydrochloric acid,
Ratio of the mass fraction between 1% ammonium hydroxide is respectively as follows: according to parts by weight, weigh respectively 20~30 parts of ethyl orthosilicates, 40~
50 parts of dehydrated alcohols, 20~30 parts of deionized waters, 10~15 parts of fillers, 1~5 part of N,N-dimethylformamide, 1~3 part of quality
Score is 1% hydrochloric acid, 1~3 part of mass fraction is 1% ammonium hydroxide.
6. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(3) semi-finished product be aged simultaneously aging process step described in are as follows: after semi-finished product are aged 1~2 day at room temperature, be placed in aging
Each aging process 1~2 day at being 40~60 DEG C in temperature in liquid.
7. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(3) described in by age gelation immersion treatment step are as follows: use acetone soak age gelation 3~5 times, impregnate 5~10min every time.
8. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(3) gel drying processing step after will impregnate described in are as follows: dry 1 at being 100~150 DEG C in temperature by gel after immersion~
2h。
9. a kind of preparation method of aerosil functional material according to claim 1, it is characterised in that: step
(3) desiccant gel is placed in calcination processing step in Muffle furnace described in are as follows: desiccant gel is placed in Muffle furnace, with 50mL/
The air velocity of min is passed through nitrogen, is warming up to 1~2h of holding at 250~300 DEG C, is continuously heating to protect at 1000~1100 DEG C
Hold 3~4h.
10. a kind of preparation method of aerosil functional material according to claim 6, it is characterised in that: institute
It is 20% ethanol water and mass fraction is 20% ethyl orthosilicate-ethanol solution that the Ageing solution stated, which is respectively mass fraction,.
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| CN115433020A (en) * | 2022-08-20 | 2022-12-06 | 浙江大学 | Preparation method of silicon dioxide aerogel heat insulation material |
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| CN116200937A (en) * | 2023-04-28 | 2023-06-02 | 江苏米格新材料有限公司 | Composite heat insulation felt and preparation method thereof |
| CN116200937B (en) * | 2023-04-28 | 2023-09-01 | 江苏米格新材料股份有限公司 | Composite heat insulation felt and preparation method thereof |
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