CN104003406A - Preparation method and applications of super-hydrophobic SiO2 aerogel powder - Google Patents
Preparation method and applications of super-hydrophobic SiO2 aerogel powder Download PDFInfo
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- CN104003406A CN104003406A CN201410235770.4A CN201410235770A CN104003406A CN 104003406 A CN104003406 A CN 104003406A CN 201410235770 A CN201410235770 A CN 201410235770A CN 104003406 A CN104003406 A CN 104003406A
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Abstract
The invention relates to a preparation method and applications of super-hydrophobic SiO2 aerogel powder. The method is implemented through the following steps: preparing a silicon source solution, an oil phase, a surfactant and a surfactant aid into a microemulsion; then, neutralizing the microemulsion until the pH value is 6-10 so as to form wet microgel particles; sequentially carrying out ageing, washing and solvent exchange on the wet microgel particles; finally, modifying the obtained product by using a silane modifier, and drying gel at normal pressure and temperature so as to obtain aerogel powder. The method is capable of preparing aerogel powder by using a microemulsion, the particle size of aerogel powder prepared by using the method is uniformly distributed, and prepared aerogel powder has the characteristics of controllable particle size distribution, short preparation period, and capability of being dried at normal pressure and temperature.
Description
Technical field
The invention belongs to the preparing technical field of ceramic, particularly a kind of super-hydrophobicity SiO
2the preparation method of aerogel powder and application.
Background technology
SiO
2aerogel be a kind of uniqueness by the porous solid material of having of the highly cross-linked gathering of nano_scale particle, there is continuous three-dimensional net structure, it forms by more than 90% air with less than 10% solid.SiO
2the structural performance of aerogel, makes it have the special property of the aspects such as mechanics, calorifics, acoustics, optics, electricity, such as it has ultralow apparent density (0.03g/cm
3left and right), ultralow thermal conductivity (0.03W/mK is following), high-specific surface area (600~1200m
2/ g), low-refraction, low acoustic resistance, strong absorption property etc.SiO
2aerogel is as a kind of novel material, and because of its special property, it will inevitably have broad application prospects in fields such as heat insulation thermal insulation, medicine, environmental protection, chemical catalysis, building energy conservation, aerospace.
At present, SiO
2the preparation of aerogel powder is generally to adopt to prepare aerogel block body and clay into power or adopt spray method or emulsion method.It is long that constant pressure and dry is prepared aerogel block body fabrication cycle, easily occurs the incomplete situation of modification, makes the aerogel powder bad preparing; The aerogel powder that spray method prepares is easily drop generation adhesion reunion in the process of spraying, thereby occurs that particle diameter surpasses the powder of 1mm; The aerogel that emulsion method prepares is due to emulsion droplet size heterogeneity, and the aerogel powder particle size distribution range preparing is wide.
Microemulsion is Thermodynamically stable, transparent water droplet (W/O) or the oil droplet monodisperse system that (O/W) forms in water in oil, and the particle diameter of its microstructure is 5~70nm, is that surfactant molecule is at the organized assembles of oil/water interface formation.The difference of microemulsion and emulsion is that microemulsion is that the drop that formed under the effect of tensio-active agent and cosurfactant by water oil phase is at the liquid of the character homogeneous of 5~10nm, emulsion is that liquid particle diameter is more than μ m, so emulsion can be in gravity or centrifugal effect lower leaf, microemulsion can be not stratified at long-time standing or centrifugal lower water oil phase.
In microemulsion system, two kinds of immiscible continuums are divided into short space by tensio-active agent parents molecule, form microreactor, w/o type microemulsion particularly, can form microreactor (micro-pond) thus be used for preparing nano material, its size can be controlled in nano level scope to micron order, and reactant reacts and generates solid phase particles in system.Microemulsion can regulate and control the particle diameter of nano material and stability, the processes such as the nucleation, growth of restriction nanoparticle, coalescent, reunion, thus the grain diameter forming can regulate and control.Therefore, be badly in need of finding a kind of preparation method that can make aerogel powder particle size distribution evenly and at normal temperatures and pressures can be dry.
Summary of the invention
The object of the present invention is to provide a kind of super-hydrophobicity SiO
2the preparation method of aerogel powder and application, the method adopts microemulsion method preparation, can make aerogel powder particle size distribution evenly and at normal temperatures and pressures can be dried.
For achieving the above object, technical scheme of the present invention is:
A kind of super-hydrophobicity SiO
2the preparation method of aerogel powder, it is characterized in that: the microemulsion that adopts silicon source solution, oil phase, tensio-active agent and cosurfactant to prepare is prepared wet gel, through ageing, washing, solvent replacing, surface modification treatment, after being dried under normal pressure and temperature, obtain described super-hydrophobicity SiO
2aerogel powder.
In such scheme, the step of preparing microemulsion is: silicon source solution, tensio-active agent, cosurfactant and oil phase mixing liquid are stirred under 200~500r/min rotating speed change into and stablize not stratified clear microemulsion, the quality of described tensio-active agent is 5%~25% of silicon source solution and oil phase total mass; The quality of described cosurfactant is 15%~50% of silicon source solution and oil phase total mass.The volume ratio of silicon source solution and oil phase is preferably 1:20~1:1.
In such scheme, described silicon source is water glass solution or silicic acid sol.The massfraction of described silicic acid sol is preferably 10%~50%.Described water glass solution is that modulus is 1.0~4.0 sodium silicate or the mixing solutions of potash water glass solution and water.
In such scheme, described oil phase is heptane, octane or kerosene.
In such scheme, described tensio-active agent is cetyl trimethylammonium bromide (CTAB) or sodium lauryl sulphate (SDS).
In such scheme, described cosurfactant is propyl carbinol or 2,4-hexylene glycol.
In such scheme, the dry 0.5~4h under 15 ℃~35 ℃ and condition of normal pressure of the wet gel powder after modification forms aerogel powder.Temperature is preferably at 25 ℃ of room temperatures.
In such scheme, the step of preparing wet gel is the aforementioned microemulsion obtaining to be neutralized to pH 6~10 obtain SiO
2wet gel.In and microemulsion acid solution used be sulfuric acid, hydrochloric acid or nitre aqueous acid; Acid solutions is 0.5~2.5mol/L; Alkaline solution is the aqueous solution of ammoniacal liquor, sodium hydroxide or potassium hydroxide, and its concentration is 0.5~5mol/L.When silicon source is water glass solution, adopt in acid solution and microemulsion; When silicon source is silicic acid sol, adopt in alkaline solution and microemulsion, the positively charged ion that silicic acid sol can be used commercially available silicic acid sol or spent ion exchange resin to remove in water glass makes.
In such scheme, described surface modification treatment step is the wet gel after solvent replacing to be mixed and soaked with organic solvent and surface-modifying agent, modification 1h~48h.Described organic solvent is normal hexane, hexanaphthene, heptane or octane.
In such scheme, described surface-modifying agent is trimethylchlorosilane (TMCS) or hexamethyldisilazane (HMDS).
In such scheme, described aging step is ageing 1~48h at 15~80 ℃.
In such scheme, described washing step is alternately to rinse wet gel after ageing 2~15 times with dehydrated alcohol and deionized water, removes oil phase wherein and unnecessary Na
+deng foreign ion.
In such scheme, described solvent replacing step is the moisture in the wet gel after washing to be replaced out at 15~80 ℃ with the organic solvent of low surface tension, with 2~4 kinds of organic solvents, replaces step by step, and replacing number of times is 2~5 times, and the replacement time is 2~12h at every turn.The ultrasonic wave that is 20Hz~30Hz by frequency during each replacement is carried out ultrasonic dispersion 10min~1h or by 500r/min revolution dispersed with stirring.
The invention has the beneficial effects as follows:
1) adopt microemulsion method to prepare aerogel powder, can effectively control the size distribution of powder, can also be dried and be prepared into aerogel powder at normal temperatures and pressures, reduced production energy consumption.Microemulsion method is compared with traditional preparation method, has obvious advantage and advance.There is the feature that size distribution can regulate and control, preparation cycle is short, at normal temperatures and pressures can be dry simultaneously.
2) the standby aerogel powder particle size distribution of this legal system is even, its grain diameter is little, narrow diameter distribution, produces one deck super-hydrophobicity aerogel powder coating thereby can adhere to preferably on substrate material surface, can reach super-hydrophobic, self-cleaning effect.
Accompanying drawing explanation
Fig. 1 is the prepared SiO of embodiment 1
2the SEM figure of aerogel powder.
Fig. 2 is the prepared SiO of embodiment 1
2the XRD figure of aerogel powder.
Fig. 3 is the prepared SiO of embodiment 1
2the FT-IR figure of aerogel powder.
Fig. 4 is the prepared SiO of embodiment 1
2the contact angle test result figure of aerogel powder.
Fig. 5 is the prepared SiO of embodiment 2
2the SEM figure of aerogel powder.
Fig. 6 is the prepared SiO of embodiment 2
2the contact angle test result figure of aerogel powder.
Fig. 7 is the prepared SiO of embodiment 3
2the size distribution figure of aerogel powder.
Fig. 8 is the design sketch of the prepared super-hydrophobicity aerogel powder of embodiment 4 coating.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment and accompanying drawing, further illustrate content of the present invention, but content of the present invention is not only confined to the following examples.
Embodiment 1
The silicic acid sol of 20% massfraction of take is raw material, adds 10ml kerosene and 2ml silicic acid sol, and add 0.8g cetyl trimethylammonium bromide (CTAB) and 2.8g cosurfactant propyl carbinol in container.Use 250rpm magnetic stirrer to stir, treat that liquid in containers becomes the microemulsion of clear from milky emulsion.Drip while stirring the ammonia soln of pH~12, treat that microemulsion is sticky, reaction completes, and forms trickle wet gel particle in container.In container, add deionized water, soak 6h ageing and with absolute ethanol washing, suction filtration, to remove kerosene and unnecessary CTAB.Wet gel after suction filtration, makes solvent with alcohol and normal hexane respectively and respectively replaces 2 hours and disperse 1h under the ultrasonic wave of 25Hz frequency.With the solution that normal hexane and trimethylchlorosilane (TMCS) ratio are 2:1, carry out hydrophobically modified, after question response is complete, with normal hexane, wash unreacted TMCS, drying at room temperature 1h can obtain silicon dioxide aerogel powder.Fig. 1 is the SEM figure of the aerogel powder that obtains, as can be seen from the figure SiO
2aerogel powder particle is more even, between 1 μ m~3 μ m.Fig. 2 is the XRD figure of resulting aerogel powder, illustrates that this aerogel powder is a kind of unsetting thing.Fig. 3 is the FT-IR figure of resulting super-hydrophobicity aerogel powder, and in figure, wave number is 2846cm
-1, 1197cm
-1, 871cm
-1for-Si-CH
3the vibration absorption peak of group, illustrates that prepared aerogel powder is for having hydrophobic property.Fig. 4 is that super-hydrophobicity aerogel powder is tested at the contact angle of slide surface coating, and contact angle reaches 161.5 °, illustrates that this aerogel powder is Ultrahydrophobic powder.
Embodiment 2
By water: the sodium silicate that water glass volume ratio (3:1) dilution modulus is 3.0, and the filtration that stirs obtains water glass solution, in container, add 10ml kerosene and 4ml water glass solution, add 4g sodium lauryl sulphate (SDS) and 3.5g cosurfactant 2,4-hexylene glycol.Under 200rpm revolution stirs, liquid in containers becomes the microemulsion of clear from milky emulsion.Drip while stirring the sulphuric acid soln of 2mol/L, treat that microemulsion is sticky, reaction completes, and forms wet gel particle in container.In container, add deionized water, soak ageing in 8 hours and replace washing, suction filtration 8 times with dehydrated alcohol and deionized water, to remove kerosene and unnecessary SDS and Na
+.Wet gel after suction filtration, makes solvent with alcohol and octane and respectively replaces 12 hours.With the solution of octane: TMCS (1:2) ratio, carry out solvent replacing and hydrophobically modified, the completely rear suction filtration of question response obtains gel powder, and drying at room temperature 3h obtains aerogel powder.Fig. 5 is the particle size analysis figure of the aerogel powder that obtains, the as can be seen from the figure prepared SiO of embodiment 2
2aerogel powder particle is 24 μ m, and size distribution is 9 μ m~69 μ m.Fig. 6 is that super-hydrophobicity aerogel powder is tested at the contact angle of slide surface coating, and contact angle reaches 154 °, illustrates that this aerogel powder is Ultrahydrophobic powder.
Embodiment 3
By water: the sodium silicate that water glass volume ratio (4:1) dilution modulus is 3.2 also stirs, by dilution water glass by 732 sodium type strong acid type vinylbenzene ion exchange resin to remove Na
+, obtain silicic acid sol.Get 20ml heptane and 4ml silicic acid sol, and add 1.6g cetyl trimethylammonium bromide (CTAB) and 3.0g cosurfactant propyl carbinol.Use magnetic stirrer stirs, and treats that liquid in containers becomes the microemulsion of clear from milky emulsion.Drip while stirring the sodium hydroxide solution of 2mol/L, treat that microemulsion is sticky, reaction completes, and forms trickle wet gel particle in container.After soaking ageing 8h with deionized water, use deionized water wash to remove CTAB.Wet gel after suction filtration, minute makes solvent with alcohol and heptane respectively replace 4 hours and disperse 30min under the ultrasonic wave of 25KHz frequency.With the mixing solutions that heptane and hexamethyldisilazane (HMDZ) ratio are 1:1, wet gel particle is carried out to hydrophobically modified, question response is completely rear with the unreacted hexamethyldisilazane of heptane wash (HMDZ), and drying at room temperature 0.5h can obtain silicon dioxide aerogel powder.Fig. 7 is the particle size analysis figure for preparing aerogel powder, the SiO that embodiment 3 is prepared
2aerogel powder particle 36 μ m, size distribution is 15 μ m~91 μ m.
Embodiment 4
The aerogel particle particle diameter of preparing due to the present invention is little, and particle size distribution range is narrow, is easily adsorbed on base material, therefore super-hydrophobicity aerogel powder prepared by the present invention can be applicable to super-hydrophobic coat field.Aerogel powder prepared by the embodiment 3 of take is example, press aerogel powder: acetone ratio disperses aerogel powder for (0.3g:5ml), and being painted on concrete surface, after acetone volatilization, aerogel powder is adsorbed in concrete surface and forms super-hydrophobic coat.Fig. 8 is the super-hydrophobic effect of super-hydrophobic coat.
Claims (10)
1. a super-hydrophobicity SiO
2the preparation method of aerogel powder, it is characterized in that: the microemulsion that adopts silicon source solution, oil phase, tensio-active agent and cosurfactant to prepare is prepared wet gel, through ageing, washing, solvent replacing, surface modification treatment, after being dried under normal pressure and temperature, obtain described super-hydrophobicity SiO
2aerogel powder.
2. preparation method according to claim 1, it is characterized in that, the step of preparing microemulsion is: silicon source solution, tensio-active agent, cosurfactant and oil phase mixing liquid are stirred under 200~500r/min rotating speed change into and stablize not stratified clear microemulsion, the quality of described tensio-active agent is 5%~25% of silicon source solution and oil phase total mass; The quality of described cosurfactant is 15%~50% of silicon source solution and oil phase total mass.
3. preparation method according to claim 1, is characterized in that, described silicon source is water glass solution or silicic acid sol.
4. preparation method according to claim 1, is characterized in that, described oil phase is heptane, octane or kerosene.
5. preparation method according to claim 1, is characterized in that, described tensio-active agent is cetyl trimethylammonium bromide or sodium lauryl sulphate; Described cosurfactant is propyl carbinol or 2,4-hexylene glycol.
6. preparation method according to claim 1, is characterized in that, the dry 0.5~4h under 15 ℃~35 ℃ and condition of normal pressure of the wet gel powder after modification forms aerogel powder.
7. preparation method according to claim 1, is characterized in that, the step of preparing wet gel is the aforementioned microemulsion obtaining to be neutralized to pH 6~10 obtain SiO
2wet gel.
8. preparation method according to claim 1, is characterized in that, described surface modification treatment step is the wet gel after solvent replacing to be mixed and soaked with organic solvent and surface-modifying agent, modification 1h~48h.
9. preparation method according to claim 8, is characterized in that, described surface-modifying agent is trimethylchlorosilane or hexamethyldisilazane.
10. the super-hydrophobicity SiO that preparation method according to claim 1 prepares
2the application of aerogel powder in super-hydrophobic coat.
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