CN102674374A - Preparation method of silica aerogel - Google Patents
Preparation method of silica aerogel Download PDFInfo
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- CN102674374A CN102674374A CN201210123526XA CN201210123526A CN102674374A CN 102674374 A CN102674374 A CN 102674374A CN 201210123526X A CN201210123526X A CN 201210123526XA CN 201210123526 A CN201210123526 A CN 201210123526A CN 102674374 A CN102674374 A CN 102674374A
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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, being specifically related to a kind of is raw material with the alkaline silica sol, prepares the method for nano porous silicon dioxide aerogel.
Background technology:
Silicon-dioxide (SiO
2) gas gel is to form a kind of the gathering each other by nano_scale particle, is the novel light porous material of dispersion medium with the air.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 advantage such as absorption property is strong; Show peculiar property at aspects such as chemistry, calorifics, optics, acoustics, electricity, have wide and great application prospect in various fields such as space flight, military project, communication, medical, building materials, electronics, metallurgy.Britain ' The Times ' highly praise SiO in 2007
2Gas gel is " the magical material that can change the world ".
Comprehensive existing patented technology and bibliographical information, existing SiO
2It is raw material that the gas gel working 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 gas gel and application.
Produce SiO through using water glass as raw material
2Gas gel has obviously reduced cost, but often by means of a kind of ion exchange resin, thereby make silicate solution, add a kind of alkalescence again and become gel, for example patent DE-A-4342548, EP-A-0658513, CN1636871B.Patent CN1241953B adopts the water glass hydrolysis method to prepare gel, uses the gel of hot water repetitive scrubbing gained then, makes SiO through normal pressure after organic solvent displacement and the surperficial silylation reactive again
2Gas gel.It is the silicon source that patent CN102167337AA discloses with alkaline silicate (water glass, potassium silicate); Add the dilution of entry and terepthaloyl moietie; Adding mineral acid then 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 quick dewatering drying at last.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 feedstock production SiO that the researchist adopts silicon sol
2Gas gel.For example patent CN101468798A with colloidal particle size about 8nm or lower silicon sol be the silicon source; With volume ratio is to form performed polymer in silicon sol 5-50 alcohol or ketone or the alcohol ketone mixtinite doubly; 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 dry down 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 big, is not suitable for industrial mass production.Patent CN1724354A utilizes silicon sol, ethanol, nitric acid mixing to get alcogel; After 50 ℃ of following constant temperature 12-24h are aging; With soaked in absolute ethyl alcohol 1-2 time, using concentration then is 80% alcohol immersion 24h, uses tetraethoxy and the alcoholic acid mixed liquid dipping 48h of volume ratio as 1:1 again; The gained gel places 70 ℃ of freeze-day with constant temperature 72h to make silica aerogel, soaks the thermostability that improves gas gel with iron nitrate solution then.This method directly makes alcogel through in silicon sol, adding ethanol; But behind gel, still need use Different concentrations of alcohol solution soaking gained gel, 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 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, technology is simple, with short production cycle, reaction process is controlled, and the SiO that can be continuously produced
2The preparation method of gas gel.
The technical scheme that the present invention takes is following:
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, adds acid then and makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of following ageing 0-72h;
Among the step ⑴:
Described alkaline silica sol is an 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;
Saidly add acid and make the colloidal sol polycondensation become SiO
2Hydrogel is 4.0-9.0 until the pH of latex gel value, preferred pH value 5.0-8.0.
Saidly add acid and make the colloidal sol polycondensation become SiO
2Hydrogel, preferably under room temperature or 30-90 ℃ of temperature, 15s-48h forms gel.
Preferred ageing 0-72h under room temperature or 30-90 ℃ of temperature, preferred especially temperature 60-80 ℃ of following ageing 0.5-10h.
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), the water cut in gel≤50 wt%.
Said 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 handled:
Resulting gel among the step ⑵ is carried out surperficial silylanizing handle, to obtain hydrophobic surface.
Said surperficial silylanizing is handled 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 Wasserstoffatoms or nonactive organic straight chain, straight chain, side chain, ring-type is saturated or unsaturated aromatics or heteroaromatic group;
Further, 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
2Gas gel.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, technology of the present invention is simple, and is with low cost.Because the raw material that the present invention selects for use is an alkaline silica sol; This silicon sol is the ability stable existence in 1 year; Saved use organosilicon (like methyl silicate, tetraethoxy, multi-polysiloxane) feedstock production wet gel the hydrolytic process of essential experience; Help the control of wet gel structure more, thereby make SiO of the present invention
2The producing to become of gas gel 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 is feedstock production SiO with the alkaline silica sol
2The technology of gas gel is compared for the technology of raw material with adopting organosilicon (like methyl silicate, tetraethoxy, multi-polysiloxane) at present, 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 influence to 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 improves the security of producing.
4, the present invention and traditional water glass prepare SiO
2Gas gel technology is compared, and has avoided the process of spent ion exchange resin treating water glass solution, or the water glass hydrolysis method prepares the process of repeated water 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.Through under acid, base catalysis condition, polycondensation takes place rapidly make wet gel, raw material is easy to get, and is cheap, and flow process is short, has shortened producing the time of gel greatly.
6, the SiO that makes of the inventive method
2Gas gel shows through the product test analysis: the SiO of the present invention's preparation
2The density of gas gel 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, water reaches 125-145 ° at the contact angle on gas gel surface.
Further specify method of the present invention by means of embodiment below, but be not restricted to this.
Embodiment:
Embodiment 1:
The alkaline silica sol 100ml that gets dioxide-containing silica and be 30% (wt) contains in the 500ml beaker, measures 200ml water and adds in the beaker alkaline silica sol is diluted, and after normal temperature fully stirs, slowly splashes in the silica aqueous solution that configures with the NaOH solution of 2mol/L; Stir while dripping, reach 11.4, with the HCl solution titration silica aqueous solution of 2mol/L, stir then while dripping until silica aqueous solution pH value; Reach 6.5 until the pH value, place 80 ℃ of water-baths with dripping good solution, solution forms hydrogel behind the 2h; Continuation is taken out gel at the aging 2h of 60 ℃ of water-bath atmosphere, places 95% (wt) ethanol displace; The volume ratio of ethanol and hydrogel is 5:1, and the displacement temperature is 60 ℃, and time swap is 3h; Replace altogether 3 times, obtain alcogel, be drying to obtain wetting ability SiO through CO 2 supercritical
2Gas gel.
Embodiment 2:
The alkaline silica sol 50ml that gets dioxide-containing silica and be 30% (wt) contains in the 500ml beaker, measures 150ml water and adds in the beaker alkaline silica sol is diluted, after normal temperature fully stirs; Slowly splash in the silica aqueous solution that configures with 10% (wt) sodium silicate solution, stir, reach 11.2 until silica aqueous solution pH value while dripping; With the HCl solution titration silica aqueous solution of 2mol/L, stir then, reach 7.2 until the pH value while dripping; Place 60 ℃ of water-baths with dripping good solution, solution forms hydrogel behind the 2min15s, continues at the aging 3h of 60 ℃ of water-bath atmosphere; Gel is taken out, place 95% (wt) ethanol displace, 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 surface processings that methylate, 60 ℃ of immersion 3h promptly get hydrophobicity SiO through the ethanol supercritical drying
2Gas gel.
Embodiment 3:
The alkaline silica sol 50ml that gets dioxide-containing silica and be 30% (wt) contains in the 1000ml beaker; Measure in the 200ml water adding beaker alkaline silica sol is diluted; After normal temperature fully stirs, slowly splash in the silica aqueous solution that configures, stir while dripping with 10% (wt) sodium silicate solution; Reach 11.0 until silica aqueous solution pH value, then with the H of 3mol/L
2SO
4Solution titration silica aqueous solution stirs while dripping, and reaches 6.4 until the pH value, places 60 ℃ of water-baths with dripping good solution; Solution forms hydrogel behind the 7min15s, continues at the aging 2.5h of 60 ℃ of water-bath atmosphere gel to be taken out; Place 95% (wt) ethanol displace, the volume ratio of ethanol and hydrogel is 5:1, and 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; Behind 60 ℃ of immersion 3h, place 100 ℃ of following constant pressure and dry 2h, promptly get hydrophobicity SiO
2Gas gel.
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 (9)
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, adds acid then and makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of following ageing 0-72h;
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), the water cut in gel≤50 wt%; Said organic solvent is at least a in alcohol, ether, ester, ketone, aliphatic series or the aromatic hydrocarbon;
⑶, surperficial silylanizing are handled:
Resulting gel among the step ⑵ is carried out surperficial silylanizing handle, 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
2Gas gel.
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, adds acid then and makes the colloidal sol polycondensation become SiO
2Hydrogel is at temperature 0-90 ℃ of following ageing 0-72h;
⑵, solvent exchange:
Adopt the hydrogel after the ageing in the organic solvent displacement step (1), the water cut in gel≤50 wt%; Said 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
2Gas gel.
3. the preparation method of a kind of aerosil according to claim 1 and 2, it is characterized in that: the preparation of said gel: alkaline silica sol is an industrial raw material, and pH is 8.5-10.5, and density is 25 ℃ of following 1.10-1.30g/cm
3, SiO
2Content 20%-42%, the content of NaO are 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 is characterized in that: the preparation of said gel: describedly add alkali to regulate the pH value of silica aqueous solution be 11.0-12.0, alkali is NaOH, NH
3H
2At least a in O, KOH, CaOH, LiOH, sodium silicate solution, potassium silicate solution, the lithium silicate solution.
5. the preparation method of a kind of aerosil according to claim 1 and 2 is characterized in that: the preparation of said gel: saidly add acid and make the colloidal sol polycondensation become SiO
2Hydrogel, under room temperature or 30-90 ℃ of temperature, 15s-48h forms gel, is 4.0-9.0 until the pH of latex gel value; 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.
6. the preparation method of a kind of aerosil according to claim 1 and 2, it is characterized in that: said solvent exchange: organic solvent is ethanol, methyl alcohol, acetone, normal hexane or hexanaphthene.
7. the preparation method of a kind of aerosil according to claim 1 is characterized in that: during surperficial silylanizing is handled: said 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 Wasserstoffatoms or nonactive organic straight chain, straight chain, side chain, ring-type is saturated or unsaturated aromatics or heteroaromatic group.
8. the preparation method of a kind of aerosil according to claim 7 is characterized in that: preferred trimethylchlorosilane of sillylation reagent or hexamethyldisilazane.
9. the preparation method of a kind of aerosil according to claim 1 and 2; It is characterized in that: said 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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| CN113716573A (en) * | 2021-09-08 | 2021-11-30 | 宁波卿甬新材料科技有限公司 | Preparation method of asymmetric porous silicon dioxide two-dimensional material |
| CN116425169A (en) * | 2023-04-10 | 2023-07-14 | 山东科翰硅源新材料有限公司 | Method for preparing silicon dioxide aerogel by using ammonia silica sol |
| CN116425169B (en) * | 2023-04-10 | 2024-02-02 | 山东科翰硅源新材料有限公司 | Method for preparing silicon dioxide aerogel by using ammonia silica sol |
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