CN1865136A - Surface activity adjustable nano porous silicon dioxide aerogel and its preparation method - Google Patents
Surface activity adjustable nano porous silicon dioxide aerogel and its preparation method Download PDFInfo
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- CN1865136A CN1865136A CN 200510025992 CN200510025992A CN1865136A CN 1865136 A CN1865136 A CN 1865136A CN 200510025992 CN200510025992 CN 200510025992 CN 200510025992 A CN200510025992 A CN 200510025992A CN 1865136 A CN1865136 A CN 1865136A
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Abstract
This invention relates to a silica dioxide aerogel and the preparation method thereof. Said silica dioxide aerogel is surface activity adjustable and nanometer porous. The preparation procedures comprise: use polysiloxane, water, solvent and catalyst as raw material to make wet gel by sol-gel processing, wherein the volume ration of polysiloxane, water, solvent and catalyst is 1:3-15:0.5-1.0:0.02-0.1; conduct surface conditioning of the wet gel, wherein the volume ratio of the coating material and the conditioning solvent is 1:5-15; take out the wet gel to conduct normal pressure drying and sectional thermal treatment, with the temperature range between 100 and 600Deg C. This invention can transform the original hydrophobic state of the aerogel particle to hydrophilic state according to the practical need, suitable for different application requirement. It also has benefits of low cost and simple process, which makes it much qualified for industrial production.
Description
Technical field
The present invention relates to a kind of aerosil and preparation method thereof field.
Background technology
SiO
2Aerogel is a kind of high-specific surface area, low-density porous material, because the existence of nanometer network structure, caused this material itself to have special nature, have a wide range of applications in various fields such as optics, electricity, acoustics, environmental protection, metallurgy, classified as the world's ten big hot topic science and technology by U.S.'s the 250th phase " science ".Inorganic SiO
2Aerogel is because of itself having the three-dimensional porous nano network structure of high-permeability, thereby has very low solid thermal conduction and have and can stop the heat conducting nano aperture structure of convection of air, and utilizes and mix the reflection-absorption ir radiation, thereby makes SiO
2Aerogel material becomes a kind of efficient and light weight heat-insulation material with utmost point lower thermal conductivity; Also be a kind of outstanding sound insulation, absorption, catalyst support material simultaneously, have wide application prospects.
In view of the elite clone characteristic and the application prospects of aerogel, there are many people that the preparation of material is studied.Preparation SiO
2It is raw material that aerogel generally adopts organosilicon, prepares in conjunction with supercritical drying by Sol-Gel technology.Because supercritical drying needs the High Temperature High Pressure process, energy consumption is big, and technology is loaded down with trivial details, has certain risk, and product amounts is limited, is unfavorable for suitability for industrialized production, thereby cost is also high.The physical strength of aerogel own is very low in addition, generally need just can be put to practicality with other materials is compound, therefore must carry out suitable adjusting to the surface tissue of aerogel, and making it to have good surfactivity could mate with corresponding matrix material.Like this about aerogel in numerous application possibility such as insulation, sound insulation, absorption, porousness, specific surface area, surfactivity, manufacturing cost and can whether possess the technology of be fit to producing in batches be the important factor that realize on a large scale to marketing.
The silicon source that Chinese patent 97195616.2 (" method for preparing organically-modified aerogel ") adopts is a water glass solution, technical process is at first obtaining the lyogel of silicate, back binary ether organic solvent washing, make the gel surface silylanizing of acquisition then, the final drying gel obtains aerogel, and surperficial silylanizing solvent is the formula R of n=1～3
1 4-nSiCl
nOr R
1 4-nSi (OR
2)
nThe silicon source that Chinese patent 97181109.1 (" method for preparing aerogel organically-modified, permanently hydrophobic ") adopts is respectively a water glass solution, and technical process is with patent 97195616.2, and silylating agent is R
3Si-o-SiR
3Sily oxide.The silicon source that Chinese patent 98811584.0 (" producing the method for silicon tetrachloride-based organically-modified aerogel ") adopts is respectively a silicon tetrachloride, technical process is for to obtain hydrogel with tetrazotization silicon and water direct reaction, carry out surface modification then, final drying obtains organically-modified aerogel.Employed silylanizing medium is R
1 4-nSiCl
nOr R
1 4-nSi (OR
2)
nAt least a silane.The organically-modified aerogel that these several patents are prepared all only has hydrophobic function, can not realize that hydrophobic, water-wetted surface is active adjustable, and restriction is received in the selection of matrix material.
Summary of the invention
It is adjustable to the purpose of this invention is to provide a kind of surfactivity, can with the nano porous silicon dioxide aerogel of corresponding matrix material coupling.
Another object of the present invention provides the preparation method of the adjustable nano porous silicon dioxide aerogel of above-mentioned surfactivity.
Nano porous silicon dioxide aerogel of the present invention, its mean pore size are 5～30nm, and the BET specific surface area is 600～1000m
2/ g, hole ratio＞80%, 1000 ℃ of high-temperature resistants, and surfactivity is adjustable.
The nano porous silicon dioxide aerogel that surfactivity of the present invention is adjustable, its preparation methods steps is as follows:
A, be that raw material makes wet gel through sol-gel processing with multi-polysiloxane, water, solvent and catalyzer, wherein multi-polysiloxane, water, solvent and catalyst volume ratio are 1: 3～15: 0.5～1.0: 0.02～0.1;
B, the wet gel that step a is obtained carry out finishing, and the volume ratio of finishing liquid and decorating liquid solvent is 1: 5～15;
Carry out constant pressure and dry segmentation thermal treatment behind c, the taking-up wet gel, temperature range is at 100～600 ℃.
The preparation method of the nano porous silicon dioxide aerogel that surfactivity of the present invention is adjustable, wherein the described multi-polysiloxane of step a can be methyl silicate, tetraethoxy, industrial raw material E-40, E32 or E28 etc., described solvent can be ethanol, Virahol, acetone, butanone or acetonitrile etc., and described catalyzer can be sulfuric acid, nitric acid, hydrofluoric acid, hydrochloric acid, oxalic acid or ammoniacal liquor etc.
The preparation method of the nano porous silicon dioxide aerogel that surfactivity of the present invention is adjustable, wherein the described finishing liquid of step b is a kind of in trimethylchlorosilane, hexamethyldisiloxane, dimethyldiethoxysilane, Union carbide A-162 or the fluoro silane, and the decorating liquid solvent is hexamethyldisiloxane, hexanaphthene, normal hexane, Virahol, hexamethyldisiloxane hexanaphthene mixed solution, normal hexane Virahol mixed solution or hexamethyldisiloxane normal hexane mixed solution.
The preparation method of the nano porous silicon dioxide aerogel that surfactivity of the present invention is adjustable, wherein the described segmentation thermal treatment of step c is meant at 100～200 ℃ and handled 2～5 hours down, handled 3～7 hours down at 300～350 ℃ then, handled 8～15 hours down at 500～600 ℃ again.
With the prepared nano porous silicon dioxide aerogel of the preparation method of above-mentioned nano porous silicon dioxide aerogel is the adjustable nano porous silicon dioxide aerogel of surfactivity of the present invention.
Beneficial effect of the present invention: the present invention by to the nano porous silicon dioxide aerogel surface group modification regulate the aerogel activity, can according to actual needs aerogel particle be changed over hydrophily by original hydrophobic state like this, to be applicable to different application requiring.The present invention prepares aerosil by the method for constant pressure and dry, and preparation cost is low, technology is simple, can carry out suitability for industrialized production.
Embodiment
Embodiment 1
Is 1: 10: 1 with methyl silicate and water, ethanol, hydrochloric acid by the room temperature volume ratio: 0.1 hybrid reaction obtained wet gel after 3 hours.Wet gel is immersed in the normal hexane Virahol mixed solution (the room temperature volume ratio is: 1: 10) of finishing liquid trimethylchlorosilane, normal temperature soaks down.Take out wet gel after 30 hours,, carry out 100 ℃ of thermal treatments of constant pressure and dry 5 hours, obtain the aerogel small-particle of hydrophobic type through suitably oven dry pulverizing arrangement.300 ℃ of following thermal treatments 3 hours and 600 ℃ of following thermal treatment 8 hours, obtain the aerogel small-particle of hydrophilic then.
Detect aerogel hole rate 85% in the material, aperture size 5nm, volume density 200kg/m through ASAP-2000 type physical adsorption appearance
3, specific surface area 600m
2/ g.Detect through quiet contact angle measurement, the contact angle of the aerogel of hydrophobic type is 130 °, demonstrates hydrophobicity.The aerogel of hydrophilic is infiltrated in the water, demonstrates wetting ability.
Embodiment 2
Is 1: 15: 0.8 with E-40 and water, ethanol, hydrofluoric acid by the room temperature volume ratio: 0.05 hybrid reaction obtained wet gel after 3 hours.Wet gel is immersed in the hexamethyldisiloxane hexanaphthene mixed solution (the room temperature volume ratio is: 1: 5) of finishing liquid fluorine for silane, and normal temperature soaks down.Take out wet gel after 48 hours,, carry out 150 ℃ of thermal treatments of constant pressure and dry 3 hours, obtain the aerogel small-particle of hydrophobic type through suitably oven dry pulverizing arrangement.300 ℃ of following 5 hours and 500 ℃ of following thermal treatments 12 hours, obtain the aerogel small-particle of hydrophilic then.
Detect aerogel hole rate 90% in the material, aperture size 15nm, volume density 150kg/m through ASAP-2000 type physical adsorption appearance
3, specific surface area 700m
2/ g.Detect through quiet contact angle measurement, the contact angle of aerogel is 130 °, demonstrates hydrophobicity.The aerogel of hydrophilic is infiltrated in the water, demonstrates wetting ability.
Embodiment 3
Is 1: 3: 0.5 with E-32 and water, ethanol, sulfuric acid by the room temperature volume ratio: 0.02 hybrid reaction obtained wet gel after 3 hours.Wet gel is immersed in the aqueous isopropanol (the room temperature volume ratio is: 1: 15) of finishing liquid dimethyldiethoxysilane, normal temperature soaks down.Take out wet gel after 36 hours,, carry out 200 ℃ of thermal treatments of constant pressure and dry 2 hours, obtain the aerogel small-particle of hydrophobic type through suitably oven dry pulverizing arrangement.350 ℃ of following 7 hours and 550 ℃ of following thermal treatments 15 hours, obtain the aerogel small-particle of hydrophilic then.
Detect aerogel hole rate 93% in the material, aperture size 25nm, volume density 100kg/m through ASAP-2000 type physical adsorption appearance
3, specific surface area 800m
2/ g.Detect through quiet contact angle measurement, the contact angle of aerogel is 120 °, demonstrates hydrophobicity.The aerogel of hydrophilic is infiltrated in the water, demonstrates wetting ability.
Claims (8)
1, the preparation method of the adjustable nano porous silicon dioxide aerogel of a kind of surfactivity, its step is as follows:
A, be that raw material makes wet gel through sol-gel processing with multi-polysiloxane, water, solvent and catalyzer, wherein multi-polysiloxane, water, solvent and catalyst volume ratio are 1: 3～15: 0.5～1.0: 0.02～0.1;
B, the wet gel that step a is obtained carry out finishing, and the volume ratio of finishing liquid and decorating liquid solvent is 1: 5～15;
Carry out constant pressure and dry segmentation thermal treatment behind c, the taking-up wet gel, temperature range is at 100～600 ℃.
2, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 1, it is characterized in that the described segmentation thermal treatment of step c is meant 100～200 ℃ of following processing 2～5 hours, handled 3～7 hours down at 300～350 ℃ then, handled 8～15 hours down at 500～600 ℃ again.
3, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 2 is characterized in that the described multi-polysiloxane of step a is meant methyl silicate, tetraethoxy, industrial raw material E-40, E32 or E28.
4, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 2 is characterized in that the described solvent of step a is meant ethanol, Virahol, acetone, butanone or acetonitrile.
5, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 2 is characterized in that the described catalyzer of step a is sulfuric acid, nitric acid, hydrofluoric acid, hydrochloric acid, oxalic acid or ammoniacal liquor.
6, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 2 is characterized in that the described finishing liquid of step b is a kind of in trimethylchlorosilane, hexamethyldisiloxane, dimethyldiethoxysilane, Union carbide A-162 or the fluoro silane.
7, the preparation method of the adjustable nano porous silicon dioxide aerogel of surfactivity as claimed in claim 2 is characterized in that the described decorating liquid solvent of step b is hexamethyldisiloxane, hexanaphthene, normal hexane, Virahol, hexamethyldisiloxane hexanaphthene mixed solution, normal hexane Virahol mixed solution or hexamethyldisiloxane normal hexane mixed solution.
8, the adjustable nano porous silicon dioxide aerogel of the prepared surfactivity of preparation method of the adjustable nano porous silicon dioxide aerogel of the arbitrary surfactivity of claim 1～7.
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| CN110354808B (en) * | 2019-07-18 | 2022-03-01 | 浙江工业大学 | By SiO2Method for removing thiophene sulfides in fuel oil by using-MTES hybrid aerogel as adsorbent |
| CN111005231A (en) * | 2019-11-20 | 2020-04-14 | 上海工程技术大学 | Preparation method of durable photocatalytic self-repairing super-amphiphobic ultraviolet-proof textile |
| CN111005231B (en) * | 2019-11-20 | 2022-08-26 | 上海工程技术大学 | Preparation method of durable photocatalytic self-repairing super-amphiphobic ultraviolet-proof textile |
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