CN102826514A - Method for preparing inorganic oxide aerogel by dehydrating and drying organic solvent - Google Patents
Method for preparing inorganic oxide aerogel by dehydrating and drying organic solvent Download PDFInfo
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- CN102826514A CN102826514A CN2012103256415A CN201210325641A CN102826514A CN 102826514 A CN102826514 A CN 102826514A CN 2012103256415 A CN2012103256415 A CN 2012103256415A CN 201210325641 A CN201210325641 A CN 201210325641A CN 102826514 A CN102826514 A CN 102826514A
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Abstract
The invention provides a method for preparing inorganic oxide aerogel by dehydrating and drying organic solvent for overcoming the defects of difficulty in controlling of the drying process, long time consumption, high price, low yield and the like in the preparation process of aerogel. According to the method, the organic solvent with small surface tension and special property is adopted and the characteristic that the organic solvent is easy to sublime, the organic solvent is dried in a vacuum drying chamber are utilized. With the rise of vacuum degree, the organic solvent is cured and sublimated during rapid evaporation, the damage to a three-dimensional network structure of the aerogel due to gas-liquid phase conversion is avoided and the inorganic oxide aerogel with a regular structure is further synthesized under vacuum conditions. The method has the advantages of simpleness and convenience in operation, short time consumption and low expenses; and the prepared aerogel has the characteristics of high porosity, small aperture, excellent heat insulating performance and excellent application values in the aspects such as heat insulating catalysis.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic oxide gas gel, specifically is the dry method for preparing the inorganic oxide gas gel of a kind of easy distillation dehydration of organic solvent.
Background technology
Gas gel is a kind ofly to assemble the nanoporous network structure of formation each other with the nanometer scale ultrafine particle, and in the network hole, has been full of the gaseous state dispersion medium, and porosity is the best solid material of the minimum heat-proof quality of present density up to 80%-99.8%.Gas gel also has unique character at aspects such as acoustics, mechanics, optics, for example as soundproofing lagging, refraction coating etc. good performance is arranged all.It also has the large development potentiality in fields such as information, environmental protection, electronics, metallurgy, aerospace simultaneously.The inorganic oxide gas gel is the focus place that people study always; Mainly be because the inorganic oxide gas gel at the peculiar property that many-sides such as heat, light, electricity, magnetic and chemical property have, makes it all have broad application prospects at aspects such as insulating refractory, silencing and damping material, catalyzer, dust grabber, gas and water purification agent.
Present stage gas gel preparing method's process in adopt supercritical technologies more, though can better be duplicated the desirable gel of wet gel network structure, it is high to equipment requirements; Condition control and operational difficulty; Whole drying process length consuming time, plant efficiency is low, danger is big, and gained gel poor mechanical property has greatly limited the application of gas gel; And liquid-solid phase transformation owing to take place in vacuum freeze-drying method in refrigerating process; Cause volume change inevitably, cause gel network structure to be destroyed in various degree, what obtain all is Powdered gas gel basically.Atmosphere pressure desiccation receives numerous investigators' favor day by day because of plurality of advantages such as simple to operate, that expense is low; But the contraction of gel in drying process, will inevitably occur and break; To this situation; Investigators adopt different means that gel is handled; As add the chemical seasoning control agent, increase the methods such as snappiness of gel skeleton, but see that from the situation of present report these technology all also are not very ripe, also exist a certain distance on the product performance that gas gel that makes and supercritical drying make.Therefore develop new dry technology, shorten the preparation time of gas gel and guarantee intact network structure, the minimizing power consumption reduces production costs and has crucial meaning for the industrial applications that advances gel.
Summary of the invention
Technical problem:The dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent that the present invention is intended to a kind of weak point easy and simple to handle, consuming time of the not enough proposition of prior art, cost is low, bulk is regular, superior performance is easy to realize suitability for industrialized production.
Technical scheme:The dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent of the present invention is: the organic solvent that adopts the easy distillation of one or more low toxicities high-solidification point is as drying medium; With the inorganic metal salt is raw material; Adopt Prepared by Sol Gel Method inorganic oxide gel precursor; After one or more low toxicities are prone to the replacement of distillation organic solvent, make the organic solvent distillation through vacuumizing, thermal treatment promptly gets the inorganic oxide gas gel; The preparation process of concrete inorganic oxide gas gel is following:
With the inorganic metal salt is presoma; Adopt sol-gel method and finishing technology to obtain wet gel; Adding one or more low toxicities is prone to the distillation organic solvent and is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation; The solvent replacing number of times is 2 ~ 4 times, and the gained gel is placed vacuum drying oven, is adjusted to 10
3~ 10
-1Pa, normal temperature keeps 0.5 ~ 48h, promptly gets the inorganic oxide gas gel through thermal treatment.
Used organic solvent is ethanol, the trimethyl carbinol or acetonitrile in the employing Prepared by Sol Gel Method inorganic oxide wet gel process.
The easy distillation of used low toxicity high-solidification point organic solvent is the trimethyl carbinol, acetonitrile, freonll-11 or hexamethyldisilazane in the solvent exchange process.
Used drying sublimation pressure is 10
3~ 10
-1Pa.
Beneficial effect:The dry method weak point easy and simple to handle, consuming time for preparing the inorganic oxide gas gel of dehydration of organic solvent provided by the invention, the organic solvent low toxicity is easy to distillation, and drying process only needs in vacuum drying oven, to accomplish, and required cost is low.Gained gel bulk is regular, porosity is high, the aperture is little, has excellent heat insulation property, thermostability and catalysis characteristics, and is easy to realize suitability for industrialized production.
Embodiment
The dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent of the present invention adopts low toxicity to be prone to distillation high-solidification point organic solvent as drying medium; Thereby low vacuum state can make the solvent distillation better duplicated the primary products of wet gel network structure down, obtains target product through thermal treatment.
The method steps of the dry preparation of dehydration of organic solvent of the present invention inorganic oxide gas gel is following:
(1) with the inorganic metal salt is presoma, adopts sol-gel method and finishing technology to obtain wet gel.
(2) adding the volatile organic solvent of one or more low toxicities is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 48h.
(3) the gained gel is placed vacuum drying oven, be adjusted to 10
3~ 10
-1Pa, normal temperature keeps 0.5 ~ 48h, promptly gets the inorganic oxide gas gel through thermal treatment.
Used organic solvent is ethanol, the trimethyl carbinol, acetonitrile etc. in the Prepared by Sol Gel Method inorganic oxide wet gel process.
Used organic replacement solvent is that low toxicity is prone to distillation high-solidification point organic solvent, the for example trimethyl carbinol, acetonitrile, freonll-11 or hexamethyldisilazane.
The dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent of the present invention is characterized in that if the solvent phase of Prepared by Sol Gel Method process reaction system employing organic solvent and solvent replacing together, can omit the solvent replacing operation.
Further describe characteristic of the present invention through instance below, but the present invention is not limited to following instance.
Embodiment 1
With the Aluminum Chloride Hexahydrate is presoma, adds ethanol, deionized water, methane amide, and the mol ratio of aluminium salt, ethanol, deionized water, methane amide is: 1:8:20:0.6 ~ 0.8, and normal temperature magnetic agitation to aluminium salt dissolves fully, and stir on the limit
The limit adds propylene oxide (mol ratio of aluminium salt and propylene oxide is 1:4 ~ 10) to mixing.Sealing and standing promptly gets wet gel behind 0.5 ~ 3h, wet gel normal temperature was worn out 1 ~ 2 day, and residual liquid inclines.Adding the organic solvent trimethyl carbinol is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 24h.The gained gel is placed vacuum drying oven, be adjusted to 10
3~ 10
-1Pa, normal temperature pressurize 0.5 ~ 24h.Then sample is placed retort furnace, in air atmosphere, regulating temperature rise rate is 1 ℃/min, is warming up to 500 ℃, and insulation 2 ~ 4h promptly gets block alumina aerogels behind the naturally cooling.
Embodiment 2
With the Aluminum Chloride Hexahydrate is presoma; Add ethanol, deionized water, methane amide; The mol ratio of aluminium salt, ethanol, deionized water, methane amide is: 1:8:20:0.6 ~ 0.8; Normal temperature magnetic agitation to aluminium salt dissolves fully, adds propylene oxide (mol ratio of aluminium salt and propylene oxide is 1:4 ~ 10) while stirring to mixing.Sealing and standing promptly gets wet gel behind 0.5 ~ 3h, wet gel normal temperature was worn out 1 ~ 2 day, and residual liquid inclines.Adding organic solvent acetonitrile is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 24h.The gained gel is placed vacuum drying oven, be adjusted to 10
3~ 10
-1Pa, normal temperature pressurize 0.5 ~ 24h.Then sample is placed retort furnace, in air atmosphere, regulating temperature rise rate is 1 ℃/min, is warming up to 500 ℃, and insulation 2 ~ 4h promptly gets block alumina aerogels behind the naturally cooling.
Embodiment 3
With the Aluminum Chloride Hexahydrate is presoma; Add ethanol, deionized water, methane amide; The mol ratio of aluminium salt, ethanol, deionized water, methane amide is: 1:8:20:0.6 ~ 0.8; Normal temperature magnetic agitation to aluminium salt dissolves fully, adds propylene oxide (mol ratio of aluminium salt and propylene oxide is 1:4 ~ 10) while stirring to mixing.Sealing and standing promptly gets wet gel behind 0.5 ~ 3h, wet gel normal temperature was worn out 1 ~ 2 day, and residual liquid inclines.Adding the organic solvent hexamethyldisilazane is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 24h.The gained gel is placed vacuum drying oven, be adjusted to 10
3~ 10
-1Pa, normal temperature pressurize 0.5 ~ 24h.Then sample is placed retort furnace, in air atmosphere, regulating temperature rise rate is 1 ℃/min, is warming up to 500 ℃, and insulation 2 ~ 4h promptly gets block alumina aerogels behind the naturally cooling.
Embodiment 4
Water glass solution with 10% is that raw material adds a certain amount of absolute ethyl alcohol; Obtain silicic acid through IX; The NaOH solution that adds 0.1mol/L is regulated pH value to 5; Be placed on that for some time obtains silica wet gel at last in 40 ~ 70 ℃ of oil baths, with aging 1 ~ 2 day of wet gel normal temperature, residual liquid inclined.Aging back wet gel is immersed put it into 40 ~ 60 ℃ of thermostatic drying chambers in the mixed solution of hexamethyldisilazane and the trimethyl carbinol of 1:1 and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 24h.The gained gel is placed vacuum
Loft drier is adjusted to 10
3~ 10
-1Pa, normal temperature pressurize 0.5 ~ 24h.Then sample is placed retort furnace, in air atmosphere, regulating temperature rise rate is 1 ℃/min, is warming up to 500 ℃, and insulation 2 ~ 4h promptly gets block silica aerogel behind the naturally cooling.
Embodiment 5
Water glass solution with 10% is that raw material adds a certain amount of absolute ethyl alcohol; Obtain silicic acid through IX; The NaOH solution that adds 0.1mol/L is regulated pH value to 5; Be placed on that for some time obtains silica wet gel at last in 40 ~ 70 ℃ of oil baths, with aging 1 ~ 2 day of wet gel normal temperature, residual liquid inclined.Aging back wet gel is immersed put it into 40 ~ 60 ℃ of thermostatic drying chambers in hexamethyldisilazane and the alcoholic acid mixed solution of 1:1 and carry out the solvent replacing operation.The solvent replacing number of times is 2 ~ 4 times, each 0.5 ~ 24h.The gained gel is placed vacuum drying oven, be adjusted to 10
3~ 10
-1Pa, normal temperature pressurize 0.5 ~ 24h.Then sample is placed retort furnace, in air atmosphere, regulating temperature rise rate is 1 ℃/min, is warming up to 500 ℃, and insulation 2 ~ 4h promptly gets block silica aerogel behind the naturally cooling.
Claims (4)
1. the dry method for preparing the inorganic oxide gas gel of a dehydration of organic solvent; The organic solvent that it is characterized in that adopting one or more low toxicities to be prone to the distillation high-solidification point is as drying medium; With the inorganic metal salt is raw material, adopts Prepared by Sol Gel Method inorganic oxide gel precursor, after one or more low toxicities are prone to the replacement of distillation organic solvent; Make the organic solvent distillation through vacuumizing, thermal treatment promptly gets the inorganic oxide gas gel; The preparation process of concrete inorganic oxide gas gel is following:
With the inorganic metal salt is presoma; Adopt sol-gel method and finishing technology to obtain wet gel; Adding one or more low toxicities is prone to the distillation organic solvent and is about to it and puts into 40 ~ 60 ℃ of thermostatic drying chambers and carry out the solvent replacing operation; The solvent replacing number of times is 2 ~ 4 times, and the gained gel is placed vacuum drying oven, is adjusted to 10
3~ 10
-1Pa, normal temperature keeps 0.5 ~ 48h, promptly gets the inorganic oxide gas gel through thermal treatment.
2. the dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent as claimed in claim 1 is characterized in that adopting that used organic solvent is ethanol, the trimethyl carbinol or acetonitrile in the Prepared by Sol Gel Method inorganic oxide wet gel process.
3. the dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent as claimed in claim 1 is characterized in that the easy distillation of used low toxicity high-solidification point organic solvent is the trimethyl carbinol, acetonitrile, freonll-11 or hexamethyldisilazane in the solvent exchange process.
4. the dry method for preparing the inorganic oxide gas gel of dehydration of organic solvent as claimed in claim 1 is characterized in that used drying sublimation pressure is 10
3~ 10
-1Pa.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103157410A (en) * | 2013-03-13 | 2013-06-19 | 中国科学院化学研究所 | Aerogel preparation method |
| CN104046357A (en) * | 2014-05-26 | 2014-09-17 | 浙江大学 | YAG fluorescent powder used in semiconductor illumination and preparation method thereof |
| WO2014180299A1 (en) * | 2013-05-07 | 2014-11-13 | Li Guangwu | Method and device for preparing aerogel by drying under reduced pressure |
| CN109650395A (en) * | 2019-02-28 | 2019-04-19 | 淮阴工学院 | The method that sublimed method prepares aerosil |
| CN114180540A (en) * | 2021-11-25 | 2022-03-15 | 中国科学院金属研究所 | Method for adjusting properties of boron nitride aerogel by utilizing atmosphere |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102642841A (en) * | 2012-04-25 | 2012-08-22 | 陕西得波材料科技有限公司 | Method for preparing low-density high-performance SiO2 aerogel at constant pressure |
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2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102642841A (en) * | 2012-04-25 | 2012-08-22 | 陕西得波材料科技有限公司 | Method for preparing low-density high-performance SiO2 aerogel at constant pressure |
Non-Patent Citations (3)
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| 吴志坚: "无机气凝胶研究进展", 《无机气凝胶研究进展》 * |
| 林高用 等: "非超临界干燥法制备块状SiO2气凝胶", 《中南大学学报(自然科学版)》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103157410A (en) * | 2013-03-13 | 2013-06-19 | 中国科学院化学研究所 | Aerogel preparation method |
| WO2014180299A1 (en) * | 2013-05-07 | 2014-11-13 | Li Guangwu | Method and device for preparing aerogel by drying under reduced pressure |
| US9731264B2 (en) | 2013-05-07 | 2017-08-15 | Hong Da Technology (Bei Jing) Co. Ltd. | Method and apparatus for preparing aerogel by drying under reduced pressure |
| KR101803765B1 (en) * | 2013-05-07 | 2017-12-01 | 광우 리 | Method and device for preparing aerogel by drying under reduced pressure |
| CN104046357A (en) * | 2014-05-26 | 2014-09-17 | 浙江大学 | YAG fluorescent powder used in semiconductor illumination and preparation method thereof |
| CN104046357B (en) * | 2014-05-26 | 2015-07-15 | 浙江大学 | YAG fluorescent powder used in semiconductor illumination and preparation method thereof |
| CN109650395A (en) * | 2019-02-28 | 2019-04-19 | 淮阴工学院 | The method that sublimed method prepares aerosil |
| CN114180540A (en) * | 2021-11-25 | 2022-03-15 | 中国科学院金属研究所 | Method for adjusting properties of boron nitride aerogel by utilizing atmosphere |
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| CN102826514B (en) | 2014-06-11 |
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