CN102674374B - Preparation method of silica aerogel - Google Patents
Preparation method of silica aerogel Download PDFInfo
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- CN102674374B CN102674374B CN 201210123526 CN201210123526A CN102674374B CN 102674374 B CN102674374 B CN 102674374B CN 201210123526 CN201210123526 CN 201210123526 CN 201210123526 A CN201210123526 A CN 201210123526A CN 102674374 B CN102674374 B CN 102674374B
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Abstract
The invention discloses a preparation method of silica aerogel, and belongs to the field of preparation of inorganic porous materials. The preparation method includes: allowing alkaline silica sol to form aerogel directly under the action of acid catalyst and base catalyst; performing solvent displacement and surface silylanizing; and supercritical or atmospheric drying to obtain SiO2 aerogel. Organic solvents are not used in sol formation, and accordingly dangers in sol formation are eliminated. The complex process of sol preparation by organosilicone and desalination by sodium silicate is omitted from the aerogel preparation, the alkaline silica sol low in cost and stable in performance is used as raw material, process is simple, production cycle is short, reaction process is controllable, equipment requirements and investment are low, and industrial production of SiO2 aerogel is achieved.
Description
Technical field:
The invention belongs to the inorganic porous material preparation field, be specifically related to a kind ofly take alkaline silica sol as raw material, prepare the method for nano porous silicon dioxide aerogel.
Background technology:
Silicon-dioxide (SiO
2) aerogel is a kind of mutually the gathering by nano_scale particle to form the novel light porous material take air as dispersion medium.Its hole ratio is up to 80%-99%, the typical sizes of hole is 1-100nm, have that specific refractory power is low, Young's modulus is little, specific acoustic resistance is low, thermal conductivity is low and the advantage such as absorption property is strong, show peculiar property at aspects such as chemistry, calorifics, optics, acoustics, electricity, in various fields such as space flight, military project, communication, medical, building materials, electronics, metallurgy wide and huge application prospect is arranged.Britain ' The Times ' highly praise SiO in 2007
2Aerogel is " the magical material that can change the world ".
Comprehensive existing patented technology and bibliographical information, existing SiO
2It is raw material that the aerogel production method adopts organosilicon (tetraethoxy, methyl silicate, multi-polysiloxane) more, with supercritical drying or the preparation of constant pressure and dry method.As open among patent EP-A-0396076, WO92/03378, WO94/25149, WO92/20623, the CN1557778.These methods exist raw material very expensive, and have toxicity, complex process, and security is low etc., and problem has seriously restricted SiO
2The large-scale production of aerogel and application.
By using water glass as waste SiO
2Aerogel has obviously reduced cost, but often by means of a kind of ion exchange resin, thereby make silicate solution, add again a kind of alkalescence and become gel, for example patent DE-A-4342548, EP-A-0658513, CN1636871B.Patent CN1241953B adopts the water glass hydrolysis method to prepare gel, then uses the gel of hot water repetitive scrubbing gained, makes SiO by normal pressure after organic solvent displacement and the surperficial silylation reactive again
2Aerogel.Patent CN102167337AA discloses take alkaline silicate (water glass, potassium silicate) as the silicon source, add the dilution of entry and ethylene glycol, then adding mineral acid fully reacts after 1-5 hour and adjusts pH2-4, repeatedly water alcohol or its mixture wash to sodium ion or potassium content be below 0.1%, under 100-400 ℃, carry out at last quick dewatering drying.This class methods complex operation, the production cycle is long, and efficient is low, and can produce a large amount of brine wastes among the preparation technology.
Because contain more impurity in the service water glass, for avoiding interference, it is that raw material prepares SiO that the researchist adopts silicon sol
2Aerogel.For example patent CN101468798A take colloidal particle size about 8nm or lower silicon sol as the silicon source, with volume ratio be silicon sol 5-50 doubly alcohol or ketone or alcohol ketone mixture in form performed polymer, sealed vessel is dehydrating gel under 100-200 ℃ of condition, and aging 3-15 days formation wet gels, unlimited sealing is placed on the 30-80 ℃ of lower dry ultra-low density silicon dioxide aerogel that forms, and this gel is kept 1-3 hour purified gas gel in 400-500 ℃.This method is strict to the silicon sol particle diameter, and the production cycle is long, and equipment requirements is high, and energy consumption is large, is not suitable for industrial mass production.Patent CN1724354A utilizes silicon sol, ethanol, nitric acid mixing to get alcogel, after 50 ℃ of lower constant temperature 12-24h are aging, with soaked in absolute ethyl alcohol 1-2 time, then be 80% alcohol immersion 24h with concentration, be the tetraethoxy of 1:1 and the mixed liquid dipping 48h of ethanol with volume ratio again, the gained gel places 70 ℃ of freeze-day with constant temperature 72h to make silica aerogel, then soaks to improve the thermostability of aerogel with iron nitrate solution.This method directly makes alcogel by add ethanol in silicon sol, but behind gel, still need use the alcohol solution dipping gained gel of different concns, concerning suitability for industrialized production, introduce organic solvent in the preparation gelation process, process is loaded down with trivial details, and introduce organic solvent in the preparation gelation process, increased the requirements such as stopping property to equipment, explosion-proof, anti-electrostatic, not only increased cost and also reduced the security of producing.
Summary of the invention:
The object of the present invention is to provide a kind of with low cost, technique is simple, with short production cycle, reaction process is controlled, and the SiO that can be continuously produced
2The preparation method of aerogel.
The technical scheme that the present invention takes is as follows:
A kind of preparation method of aerosil is characterized in that, may further comprise the steps:
⑴ the preparation of, gel:
The alkaline silica sol thin up is become silica aqueous solution, and adding alkali adjusting silica aqueous solution pH is 11.0-12.0, and then acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of lower ageing 0-72h;
Among the step ⑴:
Described alkaline silica sol is industrial raw material, and pH is 8.5-10.5, and density is 1.10-1.30g/cm3(25 ℃), SiO
2Content 20%-42%, the content of NaO are 0-0.6%, SiO
2The particle diameter of micelle concentrates between the 4-24nm;
Described alkali is NaOH, NH
3H
2At least a in O, KOH, CaOH, LiOH, sodium silicate solution, potassium silicate solution, the lithium silicate solution;
The pH value that adds alkali adjusting silica aqueous solution is 11.0-12.0, preferred pH value 11.2-11.5.
Described acid is HCl, H
2SO
4, HNO
3, H
3PO
4, HF, HBr, H
2SeO
4, HClO
4, H
2SO
3In at least a;
Described acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel, until the pH of latex gel value is 4.0-9.0, preferred pH value 5.0-8.0.
Described acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel, preferably under room temperature or 30-90 ℃ of temperature, 15s-48h forms gel.
Preferably ageing 0-72h, particularly preferably temperature 60-80 ℃ of lower ageing 0.5-10h under room temperature or 30-90 ℃ of temperature.
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), until the water content in the gel≤50 wt%.
Described organic solvent is at least a in alcohol, ether, ester, ketone, aliphatic series or the aromatic hydrocarbon, is preferably ethanol, methyl alcohol, acetone, normal hexane or hexanaphthene.
⑶, surperficial silylanizing are processed:
Resulting gel among the step ⑵ is carried out surperficial silylanizing process, to obtain hydrophobic surface.
Described surperficial silylanizing is processed and is adopted sillylation reagent R1
4-nSiCln, R1
4-nSi (OR2) n or R3Si-N (H)-SiR3, n=1 in the above-mentioned formula～3, R1, R2 and R3 are separate, identical or different, and R1, R2 and R3 are selected from hydrogen atom or nonactive organic straight chain, straight chain, side chain, ring-type is saturated or unsaturated aromatics or heteroaromatic group;
Further, the preferred trimethylchlorosilane of sillylation reagent or hexamethyldisilazane.
⑷, overcritical or constant pressure and dry:
Step ⑵ or the resulting gel of ⑶ are carried out overcritical or constant pressure and dry, obtain SiO
2Aerogel.Wherein: the constant pressure and dry temperature is 50 ℃-200 ℃.The supercritical drying solvent is any one in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane, is preferably carbonic acid gas or ethanol.
The present invention compared with prior art has the following advantages:
1, technique of the present invention is simple, and is with low cost.Because the raw material that the present invention selects is alkaline silica sol, this silicon sol is the energy stable existence in 1 year, saved use organosilicon (such as methyl silicate, tetraethoxy, multi-polysiloxane) raw material prepare wet gel the hydrolytic process of essential experience, more be conducive to the control of wet gel structure, thereby make SiO of the present invention
2The producing to become of aerogel is more prone to.Because the alkaline silica sol source is very extensive, the domestic production technology is very ripe simultaneously, and product is stable, and is functional, cheap, and the content of the silicon-dioxide in the raw material can be up to 42%, so the present invention prepares SiO take alkaline silica sol as raw material
2The technique of aerogel is compared for the technique of raw material with adopting at present organosilicon (such as methyl silicate, tetraethoxy, multi-polysiloxane), and operational condition is simplified more, and preparation efficiency improves greatly, and product cost obviously reduces.
2, the alkaline silica sol of the present invention's use is the dispersion liquid of nano level silica dioxide granule in water, and odorless, nontoxic reduces the impact on HUMAN HEALTH and environmental pollution.
3, not with an organic solvent, there is not organic solvent evaporates problem in the present invention in the process of sol-gel, and equipment requirements and drop into lowly in the suitability for industrialized production had not only reduced cost but also improved the security of production.
4, the present invention and traditional water glass prepare SiO
2Aerogel technique is compared, and avoided spent ion exchange resin to process the process of water glass solution, or the water glass hydrolysis method prepares the process of repeatedly washing desalination behind the gel, has improved working efficiency, has reduced technical process.
5, reaction conditions of the present invention is easy and controlled, and the cycle is short.By under acid, base catalysis condition, polycondensation occurs rapidly make wet gel, raw material is easy to get, and is cheap, and flow process is short, has greatly shortened producing the time of gel.
6, the SiO that makes of the inventive method
2Aerogel shows through the product test analysis: the SiO of the present invention's preparation
2The density of aerogel is at 0.04-0.4g/cm
3Between controlled, specific surface area is at 400-800m
2/ g, mean pore size 10-70nm, under the room temperature, the contact angle of water on the aerogel surface reaches 125-145 °.
The below further specifies method of the present invention by means of embodiment, but is not restricted to this.
Embodiment:
Embodiment 1:
Getting dioxide-containing silica is 30%(wt) alkaline silica sol 100ml be contained in the 500ml beaker, measure in the 200ml water adding beaker alkaline silica sol is diluted, after normal temperature fully stirs, NaOH solution with 2mol/L slowly splashes in the silica aqueous solution that configures, stir while dripping, until silica aqueous solution pH value reaches 11.4, then with the HCl solution titration silica aqueous solution of 2mol/L, stir while dripping, until the pH value reaches 6.5, place 80 ℃ of water-baths with dripping good solution, solution forms hydrogel behind the 2h, continues at the aging 2h of 60 ℃ of water-bath atmosphere, gel is taken out, placing 95%(wt) ethanol replaces, and the volume ratio of ethanol and hydrogel is 5:1, and the displacement temperature is 60 ℃, time swap is 3h, altogether replace 3 times, obtain alcogel, be drying to obtain wetting ability SiO by CO 2 supercritical
2Aerogel.
Embodiment 2:
Getting dioxide-containing silica is 30%(wt) alkaline silica sol 50ml be contained in the 500ml beaker, measure in the 150ml water adding beaker alkaline silica sol is diluted, after normal temperature fully stirs, with 10%(wt) sodium silicate solution slowly splashes in the silica aqueous solution that configures, stir while dripping, until silica aqueous solution pH value reaches 11.2, then with the HCl solution titration silica aqueous solution of 2mol/L, stir while dripping, until the pH value reaches 7.2, place 60 ℃ of water-baths with dripping good solution, solution forms hydrogel behind the 2min15s, continuation is at the aging 3h of 60 ℃ of water-bath atmosphere, gel being taken out, places 95%(wt) ethanol replaces, and the volume ratio of ethanol and hydrogel is 5:1, the displacement temperature is 60 ℃, time swap is 3h, replaces 1 time, gel is taken out put into trimethylchlorosilane solution and carry out the surface processing that methylates, 60 ℃ are soaked 3h, namely get hydrophobicity SiO by ethanol supercritical drying
2Aerogel.
Embodiment 3:
Getting dioxide-containing silica is 30%(wt) alkaline silica sol 50ml be contained in the 1000ml beaker, measure in the 200ml water adding beaker alkaline silica sol is diluted, after normal temperature fully stirs, with 10%(wt) sodium silicate solution slowly splashes in the silica aqueous solution that configures, stir while dripping, until silica aqueous solution pH value reaches 11.0, then with the H of 3mol/L
2SO
4Solution titration silica aqueous solution, stir while dripping, until the pH value reaches 6.4, place 60 ℃ of water-baths with dripping good solution, solution forms hydrogel behind the 7min15s, continuation is taken out gel at the aging 2.5h of 60 ℃ of water-bath atmosphere, places 95%(wt) ethanol replaces, the volume ratio of ethanol and hydrogel is 5:1, the displacement temperature is 60 ℃, and time swap is 3h, replaces 1 time, gel taken out put into trimethylchlorosilane solution and carry out the surface processing that methylates, behind 60 ℃ of immersion 3h, place 100 ℃ of lower constant pressure and dry 2h, namely get hydrophobicity SiO
2Aerogel.
Embodiment 4: product detects
The product test of embodiment 1-3 preparation is analyzed as follows:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Raw material | Alkaline silica sol | Alkaline silica sol | Alkaline silica sol |
| Density (Kg/m 3) | 120 | 90 | 63 |
| Specific surface area (m 2/g) | 426.54 | 503.73 | 712.68 |
| Mean pore size (nm) | 48 | 64 | 70 |
| To the contact angle of water (°) | / | 141 | 137 |
Claims (7)
1. the preparation method of an aerosil is characterized in that, may further comprise the steps:
⑴ the preparation of, gel:
The alkaline silica sol thin up is become silica aqueous solution, and adding alkali adjusting silica aqueous solution pH is 11.0-12.0, and then acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of lower ageing 0-72h;
The described pH value that adds alkali adjusting silica aqueous solution is 11.0-12.0, and alkali is NaOH, NH
3H
2At least a in O, KOH, LiOH, sodium silicate solution, potassium silicate solution, the lithium silicate solution;
Described acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel, under room temperature or 30-90 ℃ of temperature, 15s-48h forms gel, until the pH of latex gel value is 4.0-9.0; Described acid is HCl, H
2SO
4, HNO
3, H
3PO
4, HF, HBr, H
2SeO
4, HClO
4, H
2SO
3In at least a;
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), until the water content in the gel≤50 wt%; Described organic solvent is at least a in alcohol, ether, ester, ketone, aliphatic series or the aromatic hydrocarbon;
⑶, surperficial silylanizing are processed:
Resulting gel among the step ⑵ is carried out surperficial silylanizing process, to obtain hydrophobic surface;
⑷, overcritical or constant pressure and dry:
The resulting gel of step ⑶ is carried out overcritical or constant pressure and dry, obtain SiO
2Aerogel.
2. the preparation method of an aerosil is characterized in that, may further comprise the steps:
⑴ the preparation of, gel:
The alkaline silica sol thin up is become silica aqueous solution, and adding alkali adjusting silica aqueous solution pH is 11.0-12.0, and then acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of lower ageing 0-72h;
The described pH value that adds alkali adjusting silica aqueous solution is 11.0-12.0, and alkali is NaOH, NH
3H
2At least a in O, KOH, LiOH, sodium silicate solution, potassium silicate solution, the lithium silicate solution;
Described acid adding makes the colloidal sol polycondensation become SiO
2Hydrogel, under room temperature or 30-90 ℃ of temperature, 15s-48h forms gel, until the pH of latex gel value is 4.0-9.0; Described acid is HCl, H
2SO
4, HNO
3, H
3PO
4, HF, HBr, H
2SeO
4, HClO
4, H
2SO
3In at least a;
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), until the water content in the gel≤50 wt%; Described organic solvent is at least a in alcohol, ether, ester, ketone, aliphatic series or the aromatic hydrocarbon;
⑶, overcritical or constant pressure and dry:
The gel that step ⑵ is obtained carries out overcritical or constant pressure and dry, obtains SiO
2Aerogel.
3. the preparation method of a kind of aerosil according to claim 1 and 2, it is characterized in that: the preparation of described gel: alkaline silica sol is industrial raw material, and pH is 8.5-10.5, and density is 25 ℃ of lower 1.10-1.30g/cm
3, SiO
2Content 20%-42%, Na
2The content of O is 0-0.6%, SiO
2The particle diameter of micelle concentrates between the 4-24nm.
4. the preparation method of a kind of aerosil according to claim 1 and 2, it is characterized in that: described solvent exchange: organic solvent is ethanol, methyl alcohol, acetone, normal hexane or hexanaphthene.
5. the preparation method of a kind of aerosil according to claim 1 is characterized in that: during surperficial silylanizing is processed: described surperficial silylanizing processing employing sillylation reagent R1
4-nSiCln, R1
4-nSi (OR2) n or R3Si-N (H)-SiR3, n=1 in the above-mentioned formula～3, R1, R2 and R3 are separate, identical or different, and R1, R2 and R3 are selected from hydrogen atom or nonactive organic straight chain, straight chain, side chain, ring-type is saturated or unsaturated aromatics or heteroaromatic group.
6. the preparation method of a kind of aerosil according to claim 5 is characterized in that: the preferred trimethylchlorosilane of sillylation reagent or hexamethyldisilazane.
7. the preparation method of a kind of aerosil according to claim 1 and 2, it is characterized in that: described overcritical or constant pressure and dry: the constant pressure and dry temperature is 50 ℃-200 ℃, and the supercritical drying solvent is any one in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane.
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| CN102674374B true CN102674374B (en) | 2013-10-30 |
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| CN101318659A (en) * | 2008-07-04 | 2008-12-10 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for preparing silicon dioxide silica aerogel composite material by drying in atmosphere pressure |
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| EP3219670A4 (en) * | 2015-11-03 | 2018-02-28 | LG Chem, Ltd. | Method for preparing hydrophobic metal oxide-silica composite aerogel, and hydrophobic metal oxide-silica composite aerogel prepared thereby |
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