CN101844771A - Method for preparing super-hydrophobic silica aerogel at normal pressure - Google Patents
Method for preparing super-hydrophobic silica aerogel at normal pressure Download PDFInfo
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- CN101844771A CN101844771A CN 201010205734 CN201010205734A CN101844771A CN 101844771 A CN101844771 A CN 101844771A CN 201010205734 CN201010205734 CN 201010205734 CN 201010205734 A CN201010205734 A CN 201010205734A CN 101844771 A CN101844771 A CN 101844771A
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- silicon source
- silica aerogel
- normal pressure
- solvent
- hydrophobic silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 13
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 17
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N anhydrous n-heptane Natural products CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 230000002209 hydrophobic effect Effects 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000007171 acid catalysis Methods 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 239000003637 basic solution Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000006884 silylation reaction Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims 1
- 238000000352 supercritical drying Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000011240 wet gel Substances 0.000 abstract 3
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000499 gel Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000004964 aerogel Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
The invention discloses a method for preparing super-hydrophobic silica aerogel at the normal pressure by taking an inorganic silicon source or an organic silicon source as a raw material. The method comprises the following steps: taking the inorganic silicon source or the organic silicon source as the raw material, then mixing the raw material with a solvent and a catalyst, and obtaining wet gel through a process of sol-gel, and then carrying out ageing, solvent replacement, surface modification and ambient pressure drying on the obtained wet gel to obtain the silica aerogel with low-density, high specific table and super hydrophobicity. The invention realizes the ambient pressure drying of the wet gel, avoids the equipment investment when the conventional supercritical drying is adopted, greatly improves the safety of the production, has simple operation, good properties and controllability of the products, and is suitable for large-scale production.
Description
Technical field
The invention belongs to the chemical materials preparation field, relate to a kind of method of preparing super-hydrophobic silica aerogel at normal pressure.
Background technology
Aerosil is a kind of light porous material, has the logical structure in continuous random hole, its particular structure makes it have many good performances, its low density particularly, low thermal conductivity, and make it contain great application prospect in heat preservation and insulation field in performances such as visible region high-clarity.
Fricke etc. have studied the infrared emanation conduction of aerogel, and they find that the double thermal insulation window thermal conductivity of SiO2 aerogel preparation is lower than 0.002Wm
-1K
-1Jensen etc. are by charging into the SiO of 15mm in the middle of glass
2Aerogel makes the heat loss factor at center less than 0.7Wm
2K
-1, transmittance can reach 76%, but adopts this glass port for average family conserve energy in an every year 2300KWh in Denmark.SiO
2Aerogel also can be used as the lagging material of cryogenic systems such as refrigerator, and the common lagging material that is used for low temperature thermal insulation systems such as refrigerator is the polyurethane foam of fluorine Lyons system, and this material contains a large amount of fluorine Lyons gas.And SiO
2Aerogel discharges a large amount of Freon gases in the time of then avoiding the refrigerator work of traditional insulation materials and destroys atmospheric ozone layer, causes the danger of Greenhouse effect.
Compare nanoporous SiO with conventional insulation material
2Aerogel material has lighter quality, the littler higher temperature of volume, ability, makes it become the thermofin of aerospace craft coideal.For example the black box of record-setting flight status data has used this material as thermofin on the aircraft, and what the cabin thermofin of Britain " panther puma " air fighter adopted also is this material.U.S. NASA also used SiO in the design of " Mars Nomads "
2Aerogel material is used for keeping out Mars subzero very low temperature below 100 ℃ at night as thermal insulation layer.We also are successfully applied to this material on the high-energy particle accelerator at home, but also can make suit with this material, do civilian insulated cold wear, and its heat retention is better than common insulated cold wear.
At present, the preparation of aerosil comprises sol-gel and dry two processes, and drying process adopts supercritical drying usually.As Chinese patent CN1449997A the gel that makes is replaced through organic solvent and liquid carbon dioxide, obtain aerosil through the supercritical co drying again.But the supercritical drying complex process is had relatively high expectations to equipment material, and high pressure potential danger limited the process of aerosil suitability for industrialized production, has restricted it and has promoted the use of on a large scale.
Summary of the invention
The objective of the invention is to the deficiency at present aerosil technology of preparing, provide a kind of can be under normal pressure dry, technology is simple, is suitable for the method for preparing aerosil that industrialization is produced.
Technical scheme of the present invention is: a kind of method of preparing super-hydrophobic silica aerogel at normal pressure, this method is as raw material with inorganic silicon source or organosilicon source, at first prepare the mixing solutions of certain proportion silicon source and solvent, and then make gel with step acid catalysis or an acid, alkali two-step catalysis, the gained gel is after ageing for some time, through solvent exchange, the coating materials of silylation is modified and is made the silica dioxide gel face hydrophobic, obtain hydrophobic aerosil through constant pressure and dry again, this method may further comprise the steps:
(1) with inorganic silicon source or organosilicon source and solvent, the mass ratio of the shared mixing solutions in inorganic silicon source is in the 5-40% scope, and the mass ratio of the shared mixing solutions in organosilicon source adds acid then in the solution that mixes in the 2-30% scope, when adopting the inorganic silicon source, regulating the pH value is 1-6; When adopting the organosilicon source, it is 4-7 that mixed solution is regulated the pH value with basic solution again; Time of repose is 2-10 hour, and dwell temperature is 15-80 ℃;
(2) treat that above-mentioned solution becomes gel after, ageing 2-12 hour, add then that solvent is replaced and carry out finishing with coating materials;
(3) promptly get aerosil behind the constant pressure and dry, the constant pressure and dry temperature is 80-200 ℃.
Described organosilicon source is positive tetraethyl orthosilicate, and the inorganic silicon source is a water glass, and solvent is the second alcohol and water, and acid is hydrochloric acid, nitric acid or oxalic acid alkali; Solution is a kind of in ammonia soln, sodium carbonate solution or the ammonium bicarbonate solution; Solvent is ethanol, acetone, normal hexane or heptane; Coating materials is trimethylchlorosilane, hexamethyldisilazane, two (front three is silica-based) ethanamide, methoxytrimethylsilane, dimethoxy dimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxy silane, Union carbide A-162 or methyl trimethoxy oxygen base alkane.
When digestion time is 4-7 hour, when drying temperature is 80-110 ℃, prepare best results.
Effect of the present invention and benefit are: the method for preparing aerosil under a kind of normal pressure that provides, this method can adopt atmosphere pressure desiccation to prepare aerosil.The specific surface area of gained silica aerogel is 500～1000m
2/ g, pore volume is 1.5～3.9cm
3G
-1, the aperture is in the scope of 4～25nm.Prepare aerosil technology with traditional supercritical drying and compare, this method not only technology is simple, and energy consumption is low, and is dangerous low, and the parameter of product is adjustable, therefore is more suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the SEM figure of aerosil, shows that aerosil has abundant, the random pore texture of successive.
Fig. 2 shows that the aerosil of preparation has super-hydrophobicity
Fig. 3 is the nitrogen adsorption desorption curve of aerosil.
Fig. 4 is the pore size distribution curve of aerosil.
Embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme.
Example one
The preparation mass ratio is 23% sodium silicate aqueous solution, regulate pH value to 1 with concentrated hydrochloric acid then, obtain gel after in 50 ℃ of environment, leaving standstill 30 minutes, be that 20% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with deionized water, ethanol, normal hexane and volume ratio successively then, dry under 150 ℃ at last, obtain aerosil.The specific surface area of gained aerosil is 543m
2/ g, pore volume are 3.43cm
3G
-1, inner aperture is 25.3nm.
Example two
Get the 3.03g mass ratio and be 23% sodium silicate aqueous solution, regulate pH value to 1 with concentrated hydrochloric acid then, and then adding 2.08g deionized water, obtain gel after in 50 ℃ of environment, leaving standstill 3h, be that 20% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with deionized water, ethanol, normal hexane and volume ratio successively then, dry under 150 ℃ at last, obtain aerosil.The specific surface area of gained aerosil is 572m
2/ g, pore volume are 2.03cm
3G
-1, inner aperture is 14.1nm.
Example three
Get the 3.03g mass ratio and be 23% sodium silicate aqueous solution, regulate pH value to 1 with concentrated hydrochloric acid then, and then adding 4.16g deionized water, obtain gel after in 15 ℃ of environment, leaving standstill 40h, be that 20% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with deionized water, ethanol, normal hexane and volume ratio successively then, dry under 150 ℃ at last, obtain aerosil.The specific surface area of aerosil be 582m
2/ g, pore volume are 2.5cm
3G
-1, inner aperture is 17.3nm.
Example four
Positive tetraethyl orthosilicate, ethanol and deionized water are mixed by the room temperature volume ratio at 1.5: 10: 2, regulate pH value to 3 with HCl solution then, left standstill 8 hours, add ammonia soln then and regulate pH value to 6.5, leave standstill and obtained gel in 8 hours, be that 10% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with ethanol, normal hexane and volume ratio successively then, at last 150 ℃ dry down, obtain aerosil.The specific surface area of aerosil be 771m
2/ g, pore volume are 2.6cm
3G
-1Inner aperture is 8.6nm.
Example five
Positive tetraethyl orthosilicate, ethanol and deionized water are mixed by the room temperature volume ratio at 1.5: 10: 2, regulate pH value to 2 with HCl solution then, left standstill 4 hours, add ammonia soln then and regulate pH value to 7, leave standstill 1 and obtain gel after little, be that 20% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with ethanol, normal hexane and volume ratio successively then, at last 150 ℃ dry down, obtain aerosil.The specific surface area of aerosil be 792m
2/ g, pore volume are 2.5cm
3G
-1, inner aperture is 8.6nm.
Example six
Positive tetraethyl orthosilicate, ethanol and deionized water are mixed by the room temperature volume ratio at 0.5: 10: 2, regulate pH value to 3 with HCl solution then, left standstill 6 hours, add ammonia soln then and regulate pH value to 6, leave standstill and obtained gel in 8 hours, be that 20% the normal hexane and the mixing solutions of trimethylchlorosilane are respectively handled 24h with ethanol, normal hexane and volume ratio successively then, at last 150 ℃ dry down, obtain aerosil.The specific surface area of aerosil be 679m
2/ g, pore volume are 1.7cm
3G
-1Inner aperture is 12.6nm.
Claims (6)
1. the method for a preparing super-hydrophobic silica aerogel at normal pressure, it is characterized in that, this method is as raw material with inorganic silicon source or organosilicon source, at first prepare the mixing solutions of certain proportion silicon source and solvent, and then make gel with step acid catalysis or an acid, alkali two-step catalysis, the gained gel is after ageing for some time, through solvent exchange, the coating materials of silylation is modified and is made the silica dioxide gel surface hydrophobicity, obtain hydrophobic aerosil through constant pressure and dry again, this method may further comprise the steps:
(1) with inorganic silicon source or organosilicon source and solvent, the mass ratio of the shared mixing solutions in inorganic silicon source is in the 5-40% scope, and the mass ratio of the shared mixing solutions in organosilicon source adds acid then in the solution that mixes in the 2-30% scope, when adopting the inorganic silicon source, regulating the pH value is 1-6; When adopting the organosilicon source, it is 4-7 that mixed solution is regulated the pH value with basic solution again; Time of repose is 2-10 hour, and dwell temperature is 15-80 ℃;
(2) treat that above-mentioned solution becomes gel after, ageing 2-12 hour, add then that solvent is replaced and carry out finishing with coating materials;
(3) promptly get aerosil behind the constant pressure and dry, the constant pressure and dry temperature is 80-200 ℃.
2. the method for a kind of preparing super-hydrophobic silica aerogel at normal pressure according to claim 1 is characterized in that, described organosilicon source is positive tetraethyl orthosilicate, and the inorganic silicon source is a water glass, and solvent is the second alcohol and water, and acid is hydrochloric acid, nitric acid or oxalic acid.
3. the method for a kind of preparing super-hydrophobic silica aerogel at normal pressure according to claim 1 is characterized in that, described alkaline solution is a kind of in ammonia soln, sodium carbonate solution or the ammonium bicarbonate solution.
4. the method for a kind of preparing super-hydrophobic silica aerogel at normal pressure according to claim 1, its feature exists, and described solvent is ethanol, acetone, normal hexane or heptane.
5. the method for a kind of preparing super-hydrophobic silica aerogel at normal pressure according to claim 1, it is characterized in that described coating materials is trimethylchlorosilane, hexamethyldisilazane, two (front three is silica-based) ethanamide, methoxytrimethylsilane, dimethoxy dimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxy silane, Union carbide A-162 or methyl trimethoxy oxygen base alkane.
6. the method for a kind of preparing super-hydrophobic silica aerogel at normal pressure according to claim 1 is characterized in that, described digestion time is 4-7 hour, and drying temperature is 80-110 ℃.
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