CN102198943A - Method for preparing silicon-based aerogel with different contact angles by drying with low cost under normal pressure - Google Patents
Method for preparing silicon-based aerogel with different contact angles by drying with low cost under normal pressure Download PDFInfo
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- CN102198943A CN102198943A CN 201110100550 CN201110100550A CN102198943A CN 102198943 A CN102198943 A CN 102198943A CN 201110100550 CN201110100550 CN 201110100550 CN 201110100550 A CN201110100550 A CN 201110100550A CN 102198943 A CN102198943 A CN 102198943A
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Abstract
The invention relates to a method for preparing silicon-based aerogel with different contact angles by drying with low cost under normal pressure, and belongs to the technical field of novel material preparation. The method comprises the following steps of: mixing a certain amount of sodium metasilicate nonahydrate and deionized water in a breaker, arranging a rotor to seal the breaker, stirring in a water bath of 35 to 60 DEG C, cooling after 20 to 40 minutes, dropwise adding glacial acetic acid, regulating the pH to be acidic, ageing for 2 to 6 days after gel is formed, adding distilled water, soaking and cleaning for 24 hours in the water bath of 35 to 60 DEG C, immersing the wet gel into the modified n-hexane/trimethylchlorosilane solution, performing surface modification for 24 hours at the temperature of 50 DEG C, adding a certain amount of n-hexane to exchange the un-reacted modifier twice in 24 hours, sealing the breaker by using a preservative film with pin holes and an aluminum foil, performing graded drying under normal pressure, and finally cooling to room temperature to obtain the modified silicon-based aerogel. The method has the advantages of low cost, low energy consumption and easily controlled reaction.
Description
Technical field
The invention belongs to technical field of new material preparation, particularly a kind of low-cost constant pressure and dry prepares the method for silica-based aerogel, refers in particular to and adopts acid one step catalysis and constant pressure and dry to prepare the method for the silica-based aerogel of different contact angles.
Background technology
Silica-based aerogel is a kind of novel lightweight nano-porous materials, have many good performances, such as characteristics such as: specific surface area big (600～1000 m2g-1), porosity height (80%～99.8%), pore distribution are even, and its thermal conductivity, specific refractory power, Young's modulus, specific acoustic resistance are all very low, and this makes SiO
2Aerogel has boundless application prospect in fields such as specific acoustic resistance coupling material, heat-insulation and heat-preservation material, catalyzer and carriers thereof.At present, SiO
2The preparation of aerogel mainly uses tetraethoxy, multi-polysiloxane, poly-diethoxy siloxanes etc. as the silicon source, adopt sol-gel method to obtain vesicular structure by Supercritical Drying Technology, these silicon source great majority relatively costliness and Supercritical Drying Technology devices needed require high, energy consumption is very big and safety coefficient is low, has limited suitability for industrialized production and practical application.Therefore, adopt a kind of more cheap silicon source, the silica-based aerogel big by constant pressure and dry prepared specific surface area, that porosity is high is for realizing that silica-based aerogel scale operation and commercialization widespread use remain necessary.
This experiment adopts cheap silicon source-Starso as reactant, Glacial acetic acid is as acid regulator, obtain water glass solution by regulating the potential of hydrogen single stage method, adopt sol-gel method to make water glass solution be converted into silica-based wet gel, before constant pressure and dry, with the mixed and modified liquid of normal hexane/trimethylchlorosilane silica-based wet gel is carried out surface modification, the classification constant pressure and dry, finally obtain porous, with the silica-based aerogel of the different contact angles of water.
Summary of the invention
The objective of the invention is to have proposed the method that a kind of low-cost constant pressure and dry prepares silica-based aerogel in order to overcome above-mentioned the deficiencies in the prior art,
A kind of low-cost constant pressure and dry prepares the method for the silica-based aerogel of different contact angles, is undertaken by following step:
(1) gets a certain amount of non-hydrate sodium metasilicate and deionized water and be mixed in the beaker, add the good beaker of rotor seal, place 35-60 ℃ of stirred in water bath, behind the 20-40min, dropwise add Glacial acetic acid after the cooling, regulation and control pH is acid, after treating gel formation, aging 2-6 days
(2) add distilled water soaking and washing 24 h in 35-60 ℃ water-bath, add a certain amount of dehydrated alcohol, water in 48 h in the exchange gel (is used the alcohol immersion gel 2 times, 24 h change once), again with the ethanol in the exchange gel in a certain amount of normal hexane 48h 2 times, wet gel is immersed in modification liquid normal hexane/trimethylchlorosilane solution, a certain amount of normal hexane of adding exchanges twice of unreacted properties-correcting agent after carrying out surface modification 24h under 50 ℃ in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃, be cooled to room temperature at last, obtain the silica-based aerogel of modification.
Wherein the percentage composition of the non-hydrate sodium metasilicate described in the step (1) compares Na
2O:SiO
2=1.03; The mol ratio of non-hydrate sodium metasilicate and deionized water is 1:80.
Wherein the ratio of wet gel and normal hexane/trimethylchlorosilane solution described in the step (2) with wet gel in the molar ratio computing of silicone content and trimethylchlorosilane be Si: TMCS=1:1-9.
With the silica-based aerogel of this method preparation, advantage such as specific surface area is big, hydrophobicity is good.Present method has low, the less energy-consumption of cost, the advantage of easy control of reaction system.
Description of drawings
Fig. 1,2,3,4 is respectively different proportioning properties-correcting agent (trimethylchlorosilanes, mol ratio is respectively Si: TMCS=1:1, Si: TMCS=1:2, Si: TMCS=1:6, Si: TMCS=1:9), adopt the contact angle photo of the silica-based aerogel of an acid step and constant pressure and dry preparation;
Fig. 5,6,7 is respectively properties-correcting agent trimethylchlorosilane (mol ratio Si: TMCS=1:9), adopt stereoscan photograph, electron energy scattering spectra and the transmission electron microscope photo of the hydrophobic type aerosil of an acid step and constant pressure and dry preparation;
Fig. 8,9 is respectively properties-correcting agent trimethylchlorosilane (mol ratio Si: TMCS=1:9), adopt the N2 adsorption-desorption thermoisopleth and the pore size distribution curve of the hydrophobic type aerosil of an acid step and constant pressure and dry preparation.
Embodiment
The present invention will be further described below in conjunction with concrete embodiment.
Example 1
Take by weighing 3.8 g non-hydrate sodium metasilicates, join in the deionized water of 20 ml, at 60 ℃ of stirring in water bath 20 min, treat solution cooling after, to wherein dripping the 4ml glacial acetic acid solution, after treating all to drip off, it is acid that solution system shows, and leaves standstill in 60 ℃ of water-baths, and gelation took place after a few hours, obtain silica wet gel, aging 2 days; In 60 ℃ water-bath, add deionized water soaking and washing 24 h; Add 15-25 ml dehydrated alcohol, water in 48 h in the exchange gel (is used the alcohol immersion gel 2 times, 24 h change once), ethanol in the interior exchange of the normal hexane 48h gel of usefulness 15-25 ml is 2 times again, with wet gel immerse different proportionings (mol ratio of silicone content and trimethylchlorosilane is in the normal hexane/trimethylchlorosilane solution of Si: TMCS=1:1) in the wet gel, the normal hexane that carries out adding behind the surface modification 24h 15-25 ml under 50 ℃ exchanges twice of unreacted properties-correcting agent in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃, be cooled to room temperature at last, obtain the silica-based aerogel of modification.Its contact angle is 24.88 °
Example 2
Take by weighing 3.8 g non-hydrate sodium metasilicates, join in the deionized water of 20 ml, at 60 ℃ of stirring in water bath 20 min, treat solution cooling after, to wherein dripping the 4ml glacial acetic acid solution, after treating all to drip off, it is acid that solution system shows, and leaves standstill in 60 ℃ of water-baths, and gelation took place after a few hours, obtain silica wet gel, aging 2 days; In 60 ℃ water-bath, add deionized water soaking and washing 24 h; Add 15-25 ml dehydrated alcohol, water in 48 h in the exchange gel (is used the alcohol immersion gel 2 times, 24 h change once), ethanol in the interior exchange of the normal hexane 48h gel of usefulness 15-25 ml is 2 times again, with wet gel immerse different proportionings (mol ratio of silicone content and trimethylchlorosilane is in the normal hexane/trimethylchlorosilane solution of Si: TMCS=1:2) in the wet gel, the normal hexane that carries out adding behind the surface modification 24h 15-25 ml under 50 ℃ exchanges twice of unreacted properties-correcting agent in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃, be cooled to room temperature at last, obtain the silica-based aerogel of modification.Its contact angle is 32.24 °
Example 3
Take by weighing 3.8 g non-hydrate sodium metasilicates, join in the deionized water of 20 ml, at 60 ℃ of stirring in water bath 20 min, treat solution cooling after, to wherein dripping the 4ml glacial acetic acid solution, after treating all to drip off, it is acid that solution system shows, and leaves standstill in 60 ℃ of water-baths, and gelation took place after a few hours, obtain silica wet gel, aging 2 days; In 60 ℃ water-bath, add deionized water soaking and washing 24 h; Add 15-25 ml dehydrated alcohol, water in 48 h in the exchange gel (is used the alcohol immersion gel 2 times, 24 h change once), ethanol in the interior exchange of the normal hexane 48h gel of usefulness 15-25 ml is 2 times again, with wet gel immerse different proportionings (mol ratio of silicone content and trimethylchlorosilane is in the normal hexane/trimethylchlorosilane solution of Si: TMCS=1:6) in the wet gel, the normal hexane that carries out adding behind the surface modification 24h 15-25 ml under 50 ℃ exchanges twice of unreacted properties-correcting agent in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃, be cooled to room temperature at last, obtain the silica-based aerogel of modification.Its contact angle is 58.57 °
Example 4
Take by weighing 3.8 g non-hydrate sodium metasilicates, join in the deionized water of 20 ml, at 60 ℃ of stirring in water bath 20 min, treat solution cooling after, to wherein dripping the 4ml glacial acetic acid solution, after treating all to drip off, it is acid that solution system shows, and leaves standstill in 60 ℃ of water-baths, and gelation took place after a few hours, obtain silica wet gel, aging 2 days; In 60 ℃ water-bath, add deionized water soaking and washing 24 h; Add 15-25 ml dehydrated alcohol, water in 48 h in the exchange gel (is used the alcohol immersion gel 2 times, 24 h change once), ethanol in the interior exchange of the normal hexane 48h gel of usefulness 15-25 ml is 2 times again, with wet gel immerse different proportionings (mol ratio of silicone content and trimethylchlorosilane is in the normal hexane/trimethylchlorosilane solution of Si: TMCS=1:9) in the wet gel, the normal hexane that carries out adding behind the surface modification 24h 15-25 ml under 50 ℃ exchanges twice of unreacted properties-correcting agent in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃, be cooled to room temperature at last, obtain the silica-based aerogel of modification.Its contact angle is 144.45 °
Experiment one
Contact angle to the sample of different proportioning properties-correcting agent preparation is tested, and drawing best proportioning is Si: the silica-based aerogel contact angle of gained is 144.45 ° during TMCS=1:9, and the good hydrophobic performance is arranged; Scanning electron microscope and transmission electron microscope are shown as the standard construction (porous three-dimensional reticulated structure) of aerogel, and the electron energy scattering spectra shows in the prepared sample and do not contain other impurity; Often press dry dry making and have the silica-based aerogel of hydrophobicity.
Experiment two
(specific surface area of Si: TMCS=1:9) and pore size distribution (NOVA2000 type, U.S. Quntachrome company) are gone up and are measured, and temperature is 77 K, and adsorbate is N to take the BET method to measure silica-based aerogel
2Utilize pore size distribution and specific surface area tester to measure silica-based aerogel (pore size distribution and specific surface area and the adsorption-desorption collection of illustrative plates of Si: TMCS=1:9).(specific surface area of Si: TMCS=1:9) is respectively 892.44 m to record the silica-based aerogel of preparation
2/ g.(pore size distribution of Si: TMCS=1:9) is at 1.6 ~ 50.45nm, and mean pore size 1.759nm is typical nano-porous materials can obviously to find out silica-based aerogel from Fig. 6.Fig. 5 is silica-based aerogel (Si: TMCS=1:9) to N
2The adsorption-desorption thermoisopleth, this curve is typical V class thermoisopleth, silica-based aerogel is described, and (Si: TMCS=1:9) has vesicular structure.
Claims (3)
1. a low-cost constant pressure and dry prepares the method for the silica-based aerogel of different contact angles, it is characterized in that according to being undertaken by following step:
(1) gets a certain amount of non-hydrate sodium metasilicate and deionized water and be mixed in the beaker, add the good beaker of rotor seal, place 35-60 ℃ of stirred in water bath, behind the 20-40min, dropwise add Glacial acetic acid after the cooling, regulation and control pH is acid, after treating gel formation, aging 2-6 days
(2) add distilled water soaking and washing 24 h in 35-60 ℃ water-bath, add a certain amount of dehydrated alcohol, water in 48 h in the exchange gel 2 times, again with the ethanol in the exchange gel in a certain amount of normal hexane 48h 2 times, wet gel is immersed in modification liquid normal hexane/trimethylchlorosilane solution, a certain amount of normal hexane of adding exchanges twice of unreacted properties-correcting agent after carrying out surface modification 24h under 50 ℃ in 24h, preservative film and aluminium foil sealing beaker with the band pin hole, 6h when under normal pressure, carrying out dry 60 ℃ of classification, 4h in the time of 80 ℃, 2h in the time of 120 ℃ is cooled to room temperature at last, obtains the silica-based aerogel of modification.
2. a kind of low-cost constant pressure and dry according to claim 1 prepares the method for the silica-based aerogel of different contact angles, it is characterized in that wherein the percentage composition of the non-hydrate sodium metasilicate described in the step (1) compares Na
2O:SiO
2=1.03; The mol ratio of non-hydrate sodium metasilicate and deionized water is 1:80.
3. a kind of low-cost constant pressure and dry according to claim 1 prepares the method for the silica-based aerogel of different contact angles, it is characterized in that the ratio of wet gel and normal hexane/trimethylchlorosilane solution described in the step (2) wherein with wet gel in the molar ratio computing of silicone content and trimethylchlorosilane be Si: TMCS=1:1-9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003406A (en) * | 2014-05-30 | 2014-08-27 | 武汉理工大学 | Preparation method and applications of super-hydrophobic SiO2 aerogel powder |
| CN104071797A (en) * | 2014-05-21 | 2014-10-01 | 合肥科斯孚安全科技有限公司 | Method for preparing silicon dioxide aerogel coating with low density and large specific surface area by water glass at normal pressure and room temperature |
| CN106082244A (en) * | 2016-06-12 | 2016-11-09 | 常州天合光能有限公司 | A kind of method utilizing crystal silicon solar batteries cleaning waste liquid to prepare aeroge |
| CN106745003A (en) * | 2017-01-20 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of one-step method silicon dioxide aerogel powder normal pressure fast preparation method |
| CN112850723A (en) * | 2019-11-27 | 2021-05-28 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method of functional group modified aerogel particles for spinning and fiber spinning |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071797A (en) * | 2014-05-21 | 2014-10-01 | 合肥科斯孚安全科技有限公司 | Method for preparing silicon dioxide aerogel coating with low density and large specific surface area by water glass at normal pressure and room temperature |
| CN104071797B (en) * | 2014-05-21 | 2015-12-09 | 合肥科斯孚安全科技有限公司 | A kind of method preparing low density bigger serface aerosil coating with water glass atmospheric pressure at room |
| CN104003406A (en) * | 2014-05-30 | 2014-08-27 | 武汉理工大学 | Preparation method and applications of super-hydrophobic SiO2 aerogel powder |
| CN106082244A (en) * | 2016-06-12 | 2016-11-09 | 常州天合光能有限公司 | A kind of method utilizing crystal silicon solar batteries cleaning waste liquid to prepare aeroge |
| CN106745003A (en) * | 2017-01-20 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of one-step method silicon dioxide aerogel powder normal pressure fast preparation method |
| CN112850723A (en) * | 2019-11-27 | 2021-05-28 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method of functional group modified aerogel particles for spinning and fiber spinning |
| CN112850723B (en) * | 2019-11-27 | 2022-11-04 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method of functional group modified aerogel particles for spinning and fiber spinning |
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