CN108046274A - SiO2Aeroge and preparation method thereof - Google Patents
SiO2Aeroge and preparation method thereof Download PDFInfo
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- CN108046274A CN108046274A CN201810042132.9A CN201810042132A CN108046274A CN 108046274 A CN108046274 A CN 108046274A CN 201810042132 A CN201810042132 A CN 201810042132A CN 108046274 A CN108046274 A CN 108046274A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention provides a kind of SiO2Aeroge and preparation method thereof is related to aeroge field, the SiO2The preparation method of aeroge, using supercritical drying drying method to using the SiO that sol-gal process is prepared2Wet gel obtains SiO after being dried2Aeroge, the supercritical drying include：Progressively boosting carries out gradient stage drying under an inert atmosphere and in the pressure limit of 2 7MPa, and pressure then is risen to 11 12MPa carries out Constant pressure drying, and Constant pressure drying temperature is 270 280 DEG C.It can alleviate the technical issues of existing preparation method is easy to cause aeroge framework shrinkage cracking and void collapse using the preparation method, achieve the purpose that improve porosity and prevent aeroge from cracking.
Description
Technical field
The present invention relates to aeroge field, more particularly, to a kind of SiO2Aeroge and preparation method thereof.
Background technology
Aerosil is a kind of nanoporous light inorganic material, and porosity is up to 80-99.8%, hole
Typical sizes are 1-100nm, specific surface area 200-1000m2/ g, and density can be down to 3kg/m3, room temperature thermal conductivity factor can be down to
0.012W/ (mk) is one kind that heat-proof quality is best in current solid-state material.Meanwhile aerosil also has well
Heat resistance, can tolerate 600-900 DEG C of highest high temperature, low temperature use scope is a kind of function admirable close to absolute zero
Thermal insulation material.
Aerosil is mainly prepared using sol-gel method at present, in the drying process in later stage, due to
Wet gel after drying, is easily generating framework shrinkage cracking and the problems such as void collapse, so as to drop under the action of interfacial tension
Its low power resistance strength and heat preservation and insulation.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of SiO2The preparation method of aeroge, to alleviate existing preparation method
The technical issues of being easy to cause aeroge framework shrinkage cracking and void collapse.
The second object of the present invention is to provide a kind of SiO2Aeroge, the SiO2Aeroge has complete three-dimensional network
Structure has higher tensile strength and preferable heat-insulating property.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of SiO2The preparation method of aeroge, using supercritical drying drying method to being prepared using sol-gel method
SiO2Wet gel obtains SiO after being dried2Aeroge, the supercritical drying include：Under an inert atmosphere and in 2-
Progressively boosting carries out gradient stage drying in the pressure limit of 7MPa, and pressure then is risen to 11-12MPa carries out Constant pressure drying,
Constant pressure drying temperature is 270-280 DEG C.
Further, the hop count during ladder stage drying is no less than four.
Further, the hop count during ladder stage drying is 4~10.
Further, the first dry 40-50min in the pressure limit of 2-3MPa, then done in the pressure limit of 3-4MPa
Then dry 50-60min dries 50-60min in the pressure limit of 4-5MPa again, done afterwards in the pressure limit of 5-6MPa
Dry 60-80min finally dries 30-40min in the pressure limit of 6-7MPa again, completes gradient stage drying.
Further, the Constant pressure drying time is 80-100min during the Constant pressure drying.
Further, SiO is prepared using sol-gel method2Wet gel comprises the following steps：Hydrochloric acid is added dropwise in waterglass
Catalytic reaction is carried out, obtains SiO through aging, alcohol displacement and modification after reaction2Wet gel.
Further, the concentration of the hydrochloric acid is 0.02-0.05mol/L.
Further, aging temperature is 45-60 DEG C, ageing time 20-24h.
Further, the weight ratio of sodium metasilicate and water is in waterglass：1：(3-4).
A kind of SiO2Aeroge is obtained according to above-mentioned preparation method.
Compared with the prior art, the present invention has the advantages that：
SiO provided by the invention2It is with the supercritical drying side that is dried of progressively pressurizeing in the preparation method of aeroge
Method is to SiO2Processing is dried in wet gel, so that SiO2Ethyl alcohol in wet gel is fully evaporated, and prevents SiO2Wet gel exists
It is cracking in drying process.The drying method will not damage SiO2The three-dimensional net structure of aeroge, to prevent airsetting
Hole in glue collapses.The SiO with complete network structure can be obtained using drying method provided by the invention2
Aeroge.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
One aspect of the present invention provides a kind of SiO2The preparation method of aeroge, using supercritical drying drying method to adopting
The SiO being prepared with sol-gel method2Wet gel obtains SiO after being dried2Aeroge, the supercritical drying include：
Progressively boosting carries out gradient stage drying under an inert atmosphere and in the pressure limit of 2-7MPa, then rises to pressure
11-12MPa carries out Constant pressure drying, and drying temperature is 270-280 DEG C.
SiO provided by the invention2It is with the supercritical drying side that is dried of progressively pressurizeing in the preparation method of aeroge
Method is to SiO2Processing is dried in wet gel, so that SiO2Ethyl alcohol in wet gel is fully evaporated, and prevents SiO2Wet gel exists
It is cracking in drying process.The drying method will not damage SiO2The three-dimensional net structure of aeroge, to prevent airsetting
Hole in glue collapses.The SiO with complete network structure can be obtained using drying method provided by the invention2
Aeroge.
In certain embodiments of the present invention, the hop count during ladder stage drying is no less than four.
Wet gel is dried using rational segmented mode, the evaporation rate of ethyl alcohol can be slowed down, and then further
Reduce the generation of defect.
In certain embodiments of the present invention, the hop count during ladder stage drying is 4~10.
Wherein, hop count during ladder stage drying it is nonrestrictive for example can be 4,5,6,7,8,
9 or 10.
In certain embodiments of the present invention, the first dry 40-50min in the pressure limit of 2-3MPa, then in 3-
50-60min is dried in the pressure limit of 4MPa, 50-60min is then dried in the pressure limit of 4-5MPa again, afterwards in 5-
60-80min is dried in the pressure limit of 6MPa, finally dries 30-40min in the pressure limit of 6-7MPa again, completes gradient
Stage drying.
Using more fine gradient drying method, SiO can be further reduced2The generation of aeroge internal flaw.
In certain embodiments of the present invention, the Constant pressure drying time is 80-100min during the Constant pressure drying.
Wherein, drying time for example can be：80min, 85min, 90min, 95min or 100min.
In certain embodiments of the present invention, SiO is prepared using sol-gel method2Wet gel comprises the following steps：
Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, obtains SiO through aging, alcohol displacement and modification after reaction2Wet gel.
In certain embodiments of the present invention, the concentration of the hydrochloric acid is 0.02-0.05mol/L.
By the use of the hydrochloric acid of certain concentration as catalyst, hydrolysis-condensation reaction can be made fully to carry out, improve gelular ion
Between cross-link intensity, shorten gel time, improve the skeleton structure of gel.
In certain embodiments of the present invention, aging temperature is 45-60 DEG C, ageing time 20-24h.
Wherein, what aging temperature was nonrestrictive for example can be 45 DEG C, 47 DEG C, 50 DEG C, 52 DEG C, 55 DEG C, 57 DEG C or 60 DEG C；
Ageing time it is nonrestrictive for example can be 20h, 21h, 22h, 23h or for 24 hours.
In certain embodiments of the present invention, the weight ratio of sodium metasilicate and water is in waterglass：1：(3-4).
A kind of SiO2 aeroges, obtain according to above-mentioned preparation method.
Below in conjunction with embodiment and comparative example, the present invention will be further described in detail.
Embodiment 1
The present embodiment is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3, the concentration of hydrochloric acid is 0.03mol/L, aging temperature
For 50 DEG C, ageing time is for 24 hours；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in the present embodiment are：The first dry 40min under the pressure of 2.5MPa, then
Then the interior dry 50min under the pressure of 3.5MPa dries 50min, afterwards in the pressure of 5.5MPa under the pressure of 4.5MPa again
60min is dried under power, finally dries 30min under the pressure of 6MPa again, completes gradient stage drying；Gradient drying after the completion of
Constant pressure drying 80min under 11MPa；
Wherein, the supercritical drying temperature in step b) is 270 DEG C.
Embodiment 2
The present embodiment is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：4, the concentration of hydrochloric acid is 0.04mol/L, aging temperature
For 55 DEG C, ageing time 22h；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in the present embodiment are：The first dry 50min under the pressure of 3.5MPa, so
Dry 60min under the pressure of 5MPa again afterwards, the dry 40min under the pressure of 6MPa, completes gradient stage drying afterwards；Gradient
After the completion of drying under 11MPa Constant pressure drying 90min；
Wherein, the supercritical drying temperature in step b) is 280 DEG C.
Embodiment 3
The present embodiment is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3.5, the concentration of hydrochloric acid is 0.04mol/L, aging temperature
It spends for 55 DEG C, ageing time 23h；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in the present embodiment are：The first dry 50min under the pressure of 3MPa, then
Dry 50min under the pressure of 4.5MPa, the dry 40min under the pressure of 6MPa, completes gradient stage drying afterwards；Gradient is dried
The Constant pressure drying 80-100min under 12MPa after finishing；
Wherein, the supercritical drying temperature in step b) is 270 DEG C.
Embodiment 4
The present embodiment is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3, the concentration of hydrochloric acid is 0.003mol/L, aging temperature
For 50 DEG C, ageing time is for 24 hours；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in the present embodiment are：The first dry 40min under the pressure of 3MPa, then
50min is dried under the pressure of 4MPa, then dries 40min under the pressure of 7MPa again, completes gradient stage drying；Gradient is dried
The Constant pressure drying 100min under 11MPa after finishing；
Wherein, the supercritical drying temperature in step b) is 270 DEG C.
Comparative example 1
This comparative example is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3, the concentration of hydrochloric acid is 0.04mol/L, aging temperature
For 45 DEG C, ageing time 20h；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in this comparative example are：The dry 2h at a temperature of 12MPa pressure and 280 DEG C.
Comparative example 2
This comparative example is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：4, the concentration of hydrochloric acid is 0.05mol/L, aging temperature
For 50 DEG C, ageing time is for 24 hours；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in this comparative example are：The dry 3h at a temperature of 11MPa pressure and 270 DEG C.
Comparative example 3
This comparative example is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3, the concentration of hydrochloric acid is 0.02mol/L, aging temperature
For 45 DEG C, ageing time 20h；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in this comparative example are：The dry 3h at a temperature of 11MPa pressure and 270 DEG C.
Comparative example 4
This comparative example is a kind of SiO2The preparation method of aeroge, comprises the following steps：
Step a) prepares SiO using sol-gel method2Wet gel：Hydrochloric acid is added dropwise in waterglass and carries out catalytic reaction, instead
After should terminating SiO is obtained through aging, alcohol displacement and modification2Wet gel；
Wherein, the weight ratio of sodium metasilicate and water is in waterglass：1：3, the concentration of hydrochloric acid is 0.02mol/L, aging temperature
For 45 DEG C, ageing time 20h；
Step b) is using supercritical drying drying method to using the SiO that sol-gel method is prepared2Wet gel is dried
After obtain SiO2Aeroge, the supercritical drying drying method in this comparative example are：The first dry 50min under the pressure of 8MPa, then
Dry 50min, completes gradient stage drying under the pressure of 9MPa；Gradient drying after the completion of under 11MPa Constant pressure drying 100min；
Wherein, the supercritical drying temperature in step b) is 270 DEG C.
The SiO provided respectively embodiment 1-4 and comparative example 1-42Aeroge is tested for the property, and tests leading under room temperature
Hot coefficient and porosity and apparent form.Test result is listed in table 1.
1 the performance test results of table
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of SiO2The preparation method of aeroge is prepared using supercritical drying drying method to using sol-gel method
SiO2Wet gel obtains SiO after being dried2Aeroge, which is characterized in that the supercritical drying includes：Under an inert atmosphere
And progressively boosting carries out gradient stage drying in the pressure limit of 2-7MPa, and pressure then is risen to 11-12MPa carries out perseverance
Press dry it is dry, drying temperature be 270-280 DEG C.
2. SiO according to claim 12The preparation method of aeroge, which is characterized in that during ladder stage drying
Hop count is no less than four.
3. SiO according to claim 22The preparation method of aeroge, which is characterized in that during ladder stage drying
Hop count is 4~10.
4. SiO according to claim 22The preparation method of aeroge, which is characterized in that first in the pressure limit of 2-3MPa
Interior dry 40-50min, then the dry 50-60min in the pressure limit of 3-4MPa, then again in the pressure limit of 4-5MPa
50-60min is dried, afterwards the dry 60-80min in the pressure limit of 5-6MPa, finally again in the pressure limit of 6-7MPa
Dry 30-40min, completes gradient stage drying.
5. according to claim 1-4 any one of them SiO2The preparation method of aeroge, which is characterized in that the Constant pressure drying
The Constant pressure drying time is 80-100min in the process.
6. according to claim 1-4 any one of them SiO2The preparation method of aeroge, which is characterized in that using sol-gel
Method prepares SiO2Wet gel comprises the following steps：In waterglass be added dropwise hydrochloric acid carry out catalytic reaction, after reaction through aging,
Alcohol is replaced and modification obtains SiO2Wet gel.
7. SiO according to claim 62The preparation method of aeroge, which is characterized in that the concentration of the hydrochloric acid is 0.02-
0.05mol/L。
8. SiO according to claim 62The preparation method of aeroge, which is characterized in that aging temperature is 45-60 DEG C, always
The change time is 20-24h.
9. SiO according to claim 62The preparation method of aeroge, which is characterized in that sodium metasilicate and water in waterglass
Weight ratio is：1：(3-4).
10. a kind of SiO2Aeroge, which is characterized in that obtained according to claim 1-9 any one of them preparation methods.
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| CN201810042132.9A CN108046274A (en) | 2018-01-16 | 2018-01-16 | SiO2Aeroge and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640641A (en) * | 2018-05-28 | 2018-10-12 | 天津摩根坤德高新科技发展有限公司 | Aerogel heat-insulating felt and preparation method thereof made from organic solvent supercritical drying |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0409082A1 (en) * | 1989-07-21 | 1991-01-23 | Henkel Kommanditgesellschaft auf Aktien | Process for the preparation of SiO2 aerogels |
| US20060178496A1 (en) * | 2005-02-07 | 2006-08-10 | Industrial Technology Research Institute | Silica aerogels with high-temperature hydrophobation synthesized by using co-precursor solutions |
| CN101646622A (en) * | 2007-03-27 | 2010-02-10 | Neb株式会社 | The method and the hydrophobic aerogel prepared therefrom that prepare hydrophobic aerogel |
| CN106395837A (en) * | 2016-08-31 | 2017-02-15 | 刘朝辉 | Method for preparing silicon dioxide aerogel |
-
2018
- 2018-01-16 CN CN201810042132.9A patent/CN108046274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0409082A1 (en) * | 1989-07-21 | 1991-01-23 | Henkel Kommanditgesellschaft auf Aktien | Process for the preparation of SiO2 aerogels |
| US20060178496A1 (en) * | 2005-02-07 | 2006-08-10 | Industrial Technology Research Institute | Silica aerogels with high-temperature hydrophobation synthesized by using co-precursor solutions |
| CN101646622A (en) * | 2007-03-27 | 2010-02-10 | Neb株式会社 | The method and the hydrophobic aerogel prepared therefrom that prepare hydrophobic aerogel |
| CN106395837A (en) * | 2016-08-31 | 2017-02-15 | 刘朝辉 | Method for preparing silicon dioxide aerogel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640641A (en) * | 2018-05-28 | 2018-10-12 | 天津摩根坤德高新科技发展有限公司 | Aerogel heat-insulating felt and preparation method thereof made from organic solvent supercritical drying |
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Application publication date: 20180518 |