CN101289191B - Transparent meso-porousearth silicon gel monolithi material - Google Patents
Transparent meso-porousearth silicon gel monolithi material Download PDFInfo
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- CN101289191B CN101289191B CN2008100550595A CN200810055059A CN101289191B CN 101289191 B CN101289191 B CN 101289191B CN 2008100550595 A CN2008100550595 A CN 2008100550595A CN 200810055059 A CN200810055059 A CN 200810055059A CN 101289191 B CN101289191 B CN 101289191B
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- porousearth
- monolithi
- aperture
- meso
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Abstract
The invention relates to a transparent mesoporous silicon dioxide gel monolith material which pertains to the technical field of inorganic porous material, in particular to an ordered mesoporous silicon dioxide gel monolith material with large size, no crackle and optical transparentness. The material is characterized in that direct conversion of sol, gel, aging and drying can be realized at high temperature by adjusting synthesis ratio without any special protective means or complicated operation procedures. The method has a short synthesis period and simple operation steps and is easy to control. The material generated by the method has an ordered hexagonal phase mesoporous structure with 2nm to 10nm of aperture, 0.2cm<3>/g to 0.8cm<3>/g of pore volume, 450m<2>/g to 850m<2>/g of the specific area and 2.2nm of wall thickness, and the wall thickness of the structure is larger than the aperture. The transmissivity of visible light of the structure is similar to optical glass with the same thickness, thereby having wide application value in the research aspect of novel optical units, electrical units and magnetic units.
Description
Technical field
A kind of transparent meso-porousearth silicon gel monolithi material of the present invention belongs to the inorganic porous material technical field, is specifically related to a kind of large size, leakless, transparent meso-porousearth silicon gel monolithi material and preparation method simply, fast and efficiently.
Background technology
Mesoporous silicon oxide is that a class is made the novel porous material of template synthetic with tensio-active agent, because of it has big specific surface area, high pore volume, regular and multifarious pore passage structure and the characteristics such as adjustable sex change of pore distribution in relative broad range thereof, and in fields such as absorption, separation and catalysis, demonstrated wide application prospect.The more important thing is that orderly tissue and the periodic arrangement of this meso-hole structure on molecular level also is the guest molecule of nanoscale such as dye molecule; photosensitive molecular; Heterogeneous Composite in mesoporous such as semiconductor grain or conducting nanowires provides a kind of effective confinement place, and then provides new opportunity for the development field of new optical devices such as lens, chromatophore, Laser Devices, photochromics and nonlinear optical material etc.
Compare with common synthetic mesoporous silicon dioxide powder material, the large size transparent meso-porousearth silicon gel monolithi material has better operability.The fine and close ratio of glassy phase mutually with traditional sol-gel method preparation, because its distinctive meso-hole structure can make organic guest molecule embed matrix and intermolecular mutual gathering does not take place with higher concentration, therefore has more wide industrial application prospect than the conventional gel glass material.At present, the synthetic of transparent meso-porousearth silicon gel monolithi material adopts solvent evaporation method or microemulsion method under the different templates agent is induced to be prepared usually.Produce cracking phenomena for fear of synthetic materials in drying process, slow evaporation, supercritical extraction, vacuum-drying, the introducing inert media of general employing control solvent makes the pattern protective material or employing vacuumizes the methods such as multistep operating process that combine with hydrothermal treatment consists.These methods are generally to the equipment requirements harshness, and energy consumption height, required time are grown (about 8-12 week) very much, or the operation steps complexity is unfavorable for the suitability for industrialized production of this type of material.We find under study for action, proportioning when synthesizing by control material, and to synthesizing wet gel after suitable burin-in process, can under higher temperature, directly carry out uncovered drying, thereby obtain large size, the transparent ordered mesoporous silica dioxide gel monolith of flawless material in the short period of time wet gel.(patent No.: ZL 200310108844.X) compare, our method need not introduced inert media as the pattern protective material, has simplified operational means with prior art.(patent No.: ZL200410061428.3) compare, our method need not vacuumize and hydro-thermal gelation treating processes, and template concentration is relatively low, has simplified synthesis program, has shortened generated time and has saved the template consumption and with prior art.
Summary of the invention
The purpose of a kind of transparent meso-porousearth silicon gel monolithi material of the present invention is at above-mentioned the deficiencies in the prior art, propose a kind of large size, flawless, optically transparent ordered mesoporous silica dioxide gel monolith material and simply, efficiently, preparation method's technical scheme fast, easily.
A kind of transparent meso-porousearth silicon gel monolithi material of the present invention, it is characterized in that it being a kind of large size, flawless, optically transparent ordered mesoporous silica dioxide gel monolith material that is applied to novel light, electricity, magnetic device aspect, have six orderly side's phase meso-hole structures, the aperture is 2-10nm, pore volume 0.20.8cm
3/ g, specific surface area 450-850m
2/ g, the thickness of hole wall is greater than 2.2nm, and pore wall thickness is all greater than the aperture, and apparent size is greater than 1 * 1 * 0.2cm, opticglass to the transmitance of visible light and same thickness is suitable, its shape by changing container shape and the consumption of reactant can adjust variation.
The preparation method of above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material, it is characterized in that: at first nonionogenic tenside is dissolved in alcohol, in the mixing solutions that water and acid are formed, wait to dissolve the back and add the silicon source, the mol ratio of its initial reactant is: silicon source: nonionogenic tenside: alcohol: water: acid=1: (0.01-0.07): (7-12): (2-4): (0.01-0.02), after the stirring at room 1～2 hour, with the plastics film that has 3～5 pin holes with container sealing, under 55～80 ℃, left standstill 6～48 hours, make wet gel, pin hole is sealed, it was further fully worn out 24～72 hours, directly uncoveredly then no longer produce weight loss at 55～65 ℃ of following freeze-day with constant temperature 18～72 hours to gel, make optically transparent flawless ordered mesoporous silica dioxide gel monolith material, synthesis cycle is 2～8 days.
The preparation method of above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material is characterized in that described silicon source is methyl silicate (TMOS), tetraethoxy (TEOS) or positive silicic acid propyl ester (TPOS).
The preparation method of above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material is characterized in that described nonionogenic tenside is P123, Brij56 or F127.
The preparation method of above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material is characterized in that described alcohol is methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol or Pentyl alcohol.
The preparation method of above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material is characterized in that described acid is hydrochloric acid, sulfuric acid or nitric acid.
The above-mentioned a kind of transparent meso-porousearth silicon gel monolithi material of the present invention, its advantage is:
I, different at the consumption of the shape of container and reactant, the time of its gelation, gel seal aged time and the final uncovered exsiccant asynchronism(-nization) of gel, are worn out and the exsiccant time is directly proportional at the size of the consumption of reactant and preparation gelinite and required gelation.
II, by aperture and pore passage structure that the character and the concentration of reconciliation statement surface-active agent are regulated the gained mesoporous material, the thickness of this material hole wall is greater than 2.2nm, and pore wall thickness is all greater than the aperture.
III, realization can be passed through direct doped metal salt: FeCl when synthetic to the regulation and control of preparation optical properties of materials
36H
2O, CuSO
46H
2O and laser dyes: rhodamine B, rhodamine 6G, acquisitions such as tonka bean camphor or methylene blue.
IV, not only can synthesize transparent meso-porousearth silicon gel monolithi material, be equally applicable to the synthetic mesoporous gel monolith material of other non-silicon.
V, by regulating synthetic ratio, need not adopt special protective devices and complicated operations program can be implemented in direct conversion between colloidal sol under the comparatively high temps, gel, aging and drying process.This method synthesis cycle is short, operation steps is simple, and be easy to control, reduced the synthetic difficulty of large size, leakless, optically transparent ordered mesoporous silica dioxide gel monolith material, the meso-porousearth silicon gel monolithi material regular shape that contains tensio-active agent that makes, controllable size, the thermostability and the transparency are good, are suitable for making optical material; Removing the meso-porousearth silicon gel monolithi material that obtains behind the tensio-active agent is having a wide range of applications aspect catalysis, the separation.
Embodiment
Embodiment 1:
With 0.5 gram Pluronic 123 (P123, EO
20PO
70EO
20) be dissolved in 2.32 gram ethanol, in the solution that 0.27 gram water and 0.1 gram 1mol/L hydrochloric acid are formed, stir and make its dissolving, add 1.04 gram TEOS then, continued stir about 60 minutes.The colloidal sol immigration of preparation is had in the container of definite shape, with the plastics film that has 3 pin holes with container sealing, leave standstill at 60 ℃ of following constant temperature and to make the system gelation in 42 hours, pin hole is sealed, continuation was left standstill under 60 ℃ aging 1 day, 60 ℃ of lower open mouth dryings, obtain complete transparent meso-porousearth silicon gel monolithi material after 3 days then.Be warming up to 550 ℃ and roasting 6 hours to remove the surfactant templates agent fully with the speed of 2 ℃/min again, obtain the only stone material of orderly mesoporous silicon oxide.Through XRD, N
2Isothermal adsorption etc. are analyzed test shows, and the gained material has high-quality six side's phase structures, and its specific surface area is 608.66m
2/ g, pore volume are 0.47cm
3/ g, the aperture is 3.6nm, pore wall thickness is 4.02nm.
Embodiment 2:
With 0.5 gram Pluronic 123 (P123, EO
20PO
70EO
20) be dissolved in 2.32 gram ethanol, in the solution that 0.27 gram water and 0.1 gram 1mol/L hydrochloric acid are formed, stir and make its dissolving, add 1.04 gram TEOS then, continued stir about 90 minutes.The colloidal sol immigration is had in the container of definite shape, with the plastics film that has 5 pin holes with container sealing, leave standstill at 80 ℃ of following constant temperature and to make its gelation in 20 hours, pin hole is sealed, being cooled to 60 ℃ subsequently continued to leave standstill aging 1 day, 60 ℃ of lower open mouth dryings, obtain complete transparent meso-porousearth silicon gel monolithi material after 3 days then.Be warming up to 550 ℃ and roasting 6 hours to remove the surfactant templates agent fully with the speed of 2 ℃/min again, other is with embodiment 1.
Embodiment 3:
With 1.156 gram F127 (EO
106PO
70EO
106) be dissolved in 2.32 gram ethanol, in the solution that 0.27 gram water and 0.1 gram 1mol/L hydrochloric acid are formed, stir and make its dissolving, add 1.04 gram TEOS then, continued stir about 120 minutes.The colloidal sol immigration of preparation is had in the container of definite shape, with the plastics film that has 4 pin holes with container sealing, leave standstill at 55 ℃ of following constant temperature and to make the system gelation in 48 hours, pin hole is sealed, continuation was left standstill under 55 ℃ aging 2 days, 55 ℃ of lower open mouth dryings, obtain complete transparent meso-porousearth silicon gel monolithi material after 3 days then.Be warming up to 550 ℃ and roasting 6 hours to remove the surfactant templates agent fully with the speed of 2 ℃/min again, obtain the only stone material of orderly mesoporous silicon oxide.Through XRD, N
2Isothermal adsorption etc. are analyzed test shows, and the gained material has high-quality six side's phase structures, and its specific surface area is 500.17m
2/ g, pore volume are 0.42cm
3/ g, the aperture is 3.6nm, pore wall thickness is 7.14nm.
Embodiment 4:
With 0.5 gram Brij56 (C
16EO
10) be dissolved in 2.32 gram ethanol, in the solution that 0.27 gram water and 0.1 gram 1mol/L hydrochloric acid are formed, stir and make its dissolving, add 1.04 gram TEOS then, continued stir about 90 minutes.The colloidal sol immigration of preparation is had in the container of definite shape, with the plastics film that has 3 pin holes with container sealing, leave standstill at 65 ℃ of following constant temperature and to make the system gelation in 37 hours, pin hole is sealed, continuation was left standstill under 65 ℃ aging 1 day, 65 ℃ of lower open mouth dryings, obtain complete transparent meso-porousearth silicon gel monolithi material after 3 days then.Be warming up to 550 ℃ and roasting 6 hours to remove the surfactant templates agent fully with the speed of 2 ℃/min again, obtain the only stone material of orderly mesoporous silicon oxide.Through XRD, N
2Isothermal adsorption etc. are analyzed test shows, and the gained material has high-quality six side's phase structures, and its specific surface area is 450.48m
2/ g, pore volume are 0.26cm
3/ g, the aperture is 2.0nm, pore wall thickness is 2.22nm.
Claims (1)
1. transparent meso-porousearth silicon gel monolithi material, it is characterized in that it being a kind of large size, flawless, optically transparent ordered mesoporous silica dioxide gel monolith material that is applied to novel light, electricity, magnetic device aspect, have six orderly side's phase meso-hole structures, the aperture is 2-10nm, pore volume 0.2-0.8cm
3/ g, specific surface area 450-850m
2/ g, the thickness of hole wall is greater than 2.2nm, and pore wall thickness is all greater than the aperture, and apparent size is greater than 1 * 1 * 0.2cm, opticglass to the transmitance of visible light and same thickness is suitable, its shape by changing container shape and the consumption of reactant can adjust variation.
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| CN2008100550595A CN101289191B (en) | 2008-06-05 | 2008-06-05 | Transparent meso-porousearth silicon gel monolithi material |
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| CN2008100550595A CN101289191B (en) | 2008-06-05 | 2008-06-05 | Transparent meso-porousearth silicon gel monolithi material |
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| CN101289191A CN101289191A (en) | 2008-10-22 |
| CN101289191B true CN101289191B (en) | 2011-04-13 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804989B (en) * | 2010-04-16 | 2012-05-09 | 太原理工大学 | Preparation method of transparent mesoporous silica gel monolith |
| CN101811702B (en) * | 2010-04-16 | 2013-07-10 | 太原理工大学 | Preparation method of double-mesopore silicon dioxide transparent gel monolith |
| CN102285659B (en) * | 2010-06-17 | 2013-04-03 | 国家纳米科学中心 | Ordered mesoporous silicon-dioxide material and preparation method thereof |
| CN103159221B (en) * | 2013-03-07 | 2014-12-10 | 太原理工大学 | Preparation method of double-groups modified transparent meso pore silica gel monolith |
| CN103193246B (en) * | 2013-03-07 | 2015-04-29 | 太原理工大学 | Preparation method of transparent mesoporous gel monolith with dual-functional-modified hole walls |
| CN103145141B (en) * | 2013-03-07 | 2014-11-05 | 太原理工大学 | Preparation method of organic-inorganic hybrid transparent mesoporous gel monolith |
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