CN106629752A - Preparation method of elastic aerogel - Google Patents
Preparation method of elastic aerogel Download PDFInfo
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- CN106629752A CN106629752A CN201611092125.7A CN201611092125A CN106629752A CN 106629752 A CN106629752 A CN 106629752A CN 201611092125 A CN201611092125 A CN 201611092125A CN 106629752 A CN106629752 A CN 106629752A
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- preparation
- elastic
- mixed solution
- elastic aeroge
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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
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
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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
- C01P2006/10—Solid density
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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
- C01P2006/12—Surface area
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- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of elastic aerogel. The preparation method comprises the following steps: (S1) dissolving a surface modifier in methanol and mixing uniformly; dropwise adding a mixed solution of ethyl orthosilicate and methyl trimethoxy silane and stirring uniformly; and adding 0.01-0.5mol/L oxalic acid, and stirring till complete hydrolysis to obtain stable alcosol; (S2) dropwise adding 1-10mol/L ammonia water into the alcosol prepared in the step (S1), stirring and aging to obtain wet gel; and (S3) performing hydrophobic modification of the wet gel obtained in the step (S2) through the mixed solution, drying in a drying oven, and naturally cooling to obtain elastic aerosol. The preparation method disclosed by the invention has the following advantages: the whole preparation flow is easily controlled, elastic aerosol different in elasticity coefficient can be prepared according to the requirements, and mass production is promoted; and moreover, the specific surface area of the aerosol prepared by the method is 800-1,000m<2>/g, the density is 0.1-0.15g/cm<3>, the porosity is greater than or equal to 90%, the mechanical property is good, and the defect that aerogel is easily broken is improved.
Description
Technical field
The invention belongs to aerogel material technical field, specifically a kind of preparation method of elastic aeroge.
Background technology
At present, because the fire safety problem of insulation material is increasingly taken seriously, the growth momentum of state's inside thermal conservation material is all the more
Rapidly.And aeroge has the advantages that high temperature resistant, anti-pressure ability are strong, usually it is used in heat preservation fireproofing material by the people, but will
It is prepared into product as raw material, and the preparation process of prior art is complicated, and volume production is little, and causes the product mechanical performance for preparing
It is poor, frangible.
The content of the invention
In order to solve above-mentioned technological deficiency, the present invention prepares a kind of preparation method of elastic aeroge so that the product of acquisition
Product have elasticity, and mechanical performance is strong, non-friable, and preparation process is simple, beneficial to volume production.
A kind of preparation method of elastic aeroge, comprises the steps：
S1：Coating material is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and methyl trimethoxy epoxide
Stir after the mixed solution of silane, add the oxalic acid that concentration is 0.01～0.5mol/L, stirring makes its hydrolysis complete, obtains
To stable alcosol；
S2：It is added dropwise in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, stirring is aging, obtains wet
Gel；
S3：Hydrophobically modified is carried out to the wet gel that step S2 is obtained by mixed solution, is put into after being dried in drying box, extremely
Natural cooling obtains elastic aeroge.
A kind of preparation method of elastic aeroge, its advantage is：Whole preparation flow of the invention is easily controlled, can be according to need
Ask and prepare the different elastic aeroge of coefficient of elasticity, and beneficial to volume production；Furthermore, adopt a process for preparing aeroge specific surface
Product is 800～1000 ㎡/g, and density is 0.1～0.15g/cm3, porosity of=90%, good mechanical property, while improving airsetting
The frangible shortcoming of glue.
Specific embodiment
The present invention is further illustrated, concrete preparation process is as follows：
S1：Coating material is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and methyl trimethoxy epoxide
Stir after the mixed solution of silane, add the oxalic acid that concentration is 0.01～0.5mol/L, stirring makes its hydrolysis complete, obtains
To stable alcosol；
Preferably, in step S1, coating material is octyl phenyl polyoxyethylene ether, TPAOH, dodecane
Base trimethylammonium bromide, P123, polyethylene glycol 200, PEG400, Macrogol 600, in lauryl sodium sulfate at least
A kind of mixture of material；
Preferably, in step S1, in the mixed solution of tetraethyl orthosilicate and MTMS, tetraethyl orthosilicate and
The molal volume ratio of MTMS is 1:1～10；
Preferably, in step S1, mixing speed is 500～1500r/min；
Preferably, in step S1, under the conditions of 25～35 DEG C oxalic acid is added；
Preferably, in step S1, the amount for adding oxalic acid causes solution PH for 2～4；
Preferably, in step S1, tetraethyl orthosilicate is 1 with the mol ratio of methyl alcohol:1～20；
S2：It is added dropwise in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, stirring is aging, obtains wet
Gel；
Preferably, in step S2, under stirring ammoniacal liquor is added；
Preferably, in step S2, the amount for adding ammoniacal liquor causes solution PH for 5～7；
Preferably, in step S2, mixing time is 8～20min；
Preferably, in step S2, aging 12～72h under the conditions of 45～100 DEG C；
S3：Hydrophobically modified is carried out to the wet gel that step S2 is obtained by mixed solution, is put into after being dried in drying box, extremely
Natural cooling obtains elastic aeroge；
Preferably, in step S3, mixed solution is 0.05～1 with wet gel mass ratio：1；
Preferably, in step S3, mixed solution is ethanol, and hexamethylene, toluene, n-hexane, dimethylbenzene, isobutanol is different pungent
Alkane, HMDS, HMDO, MTES, trim,ethylchlorosilane, methyl trimethoxy epoxide silicon
The mixture of two or more material in alkane；
Preferably, in step S3, the hydrophobically modified time is 5～24h；
Preferably, in step S3, four temperature stages are divided into from low to high carries out heat preservation and dryness, and each stage insulation is dry
The dry time is 1～3h；Further, four temperature stages are followed successively by：45～70 DEG C, 70～100 DEG C, 100～120 DEG C, 120 DEG C
～150 DEG C.
Hereinafter with regard to specific embodiment, the present invention will be further described
Embodiment one
S1：Lauryl sodium sulfate is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and methyl trimethoxy
The mixed solution of TMOS, and in mixed solution, the molal volume ratio of tetraethyl orthosilicate and MTMS is 1:
10 (and tetraethyl orthosilicate and the mol ratio of methyl alcohol are 1:20), stir under the conditions of 1500r/min, then under the conditions of 30 DEG C
The oxalic acid that concentration is 0.01～0.5mol/L is added, and adds the amount of oxalic acid to cause solution PH for 2；Speed is stirred with 1100r/min to stir
Mixing makes its hydrolysis complete, obtains stable alcosol；
S2：It is added dropwise under stirring in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, and adds
Enter the amount of ammoniacal liquor so that solution PH be 6, stir 8min, aging 12～72h under the conditions of 45 DEG C, obtain wet gel；
S3：Hydrophobically modified, and mixed solution and wet gel matter are carried out to the wet gel that step S2 is obtained by mixed solution
Amount is than being 0.5：1, be put into drying box, be divided into from low to high 45 DEG C, 70 DEG C, 100 DEG C, 120 DEG C of four temperature stages are protected
Temperature is dried, and each heat preservation and dryness time in stage is 3h；After drying, to natural cooling elastic aeroge is obtained.
Embodiment two
S1：Octyl phenyl polyoxyethylene ether is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and methyl
The mixed solution of trimethoxy silane, and in mixed solution, the molal volume ratio of tetraethyl orthosilicate and MTMS
For 1:5 (and tetraethyl orthosilicate and the mol ratio of methyl alcohol are 1:10), stir under the conditions of 500r/min, then in 25 DEG C of conditions
It is lower to add the oxalic acid that concentration is 0.01～0.5mol/L, and add the amount of oxalic acid to cause solution PH for 3；Speed is stirred with 1500r/min
Stirring makes its hydrolysis complete, obtains stable alcosol；
S2：It is added dropwise under stirring in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, and adds
Enter the amount of ammoniacal liquor so that solution PH be 7, stir 20min, aging 12～72h under the conditions of 75 DEG C, obtain wet gel；
S3：Hydrophobically modified, and mixed solution and wet gel matter are carried out to the wet gel that step S2 is obtained by mixed solution
Amount is than being 1：1, be put into drying box be divided into from low to high 55 DEG C, 85 DEG C, 110 DEG C, that 135 DEG C of four temperature stages carry out insulation is dry
It is dry, and each heat preservation and dryness time in stage is 2h；After drying, to natural cooling elastic aeroge is obtained.
Embodiment three
S1：Macrogol 600 is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and methyl trimethoxy epoxide
The mixed solution of silane, and in mixed solution, the molal volume ratio of tetraethyl orthosilicate and MTMS is 1:1 (and
Tetraethyl orthosilicate is 1 with the mol ratio of methyl alcohol:1), stir under the conditions of 1000r/min, then add under the conditions of 35 DEG C dense
The oxalic acid for 0.01～0.5mol/L is spent, and adds the amount of oxalic acid to cause solution PH for 4；Stirring speed stirring with 1500r/min makes it
Hydrolysis is complete, obtains stable alcosol；
S2：It is added dropwise under stirring in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, and adds
Enter the amount of ammoniacal liquor so that solution PH be 5, stir 14min, aging 12～72h under the conditions of 100 DEG C, obtain wet gel；
S3：Hydrophobically modified, and mixed solution and wet gel matter are carried out to the wet gel that step S2 is obtained by mixed solution
Amount is than being 0.05：1, be put into drying box be divided into from low to high 70 DEG C, 100 DEG C, 120 DEG C, 150 DEG C of four temperature stages are protected
Temperature is dried, and each heat preservation and dryness time in stage is 1h；After drying, to natural cooling elastic aeroge is obtained.
The foregoing is only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of elastic aeroge, it is characterised in that：Comprise the steps：
S1：Coating material is dissolved in methyl alcohol and is well mixed, then be added dropwise over tetraethyl orthosilicate and MTMS
Mixed solution after stir, add the oxalic acid that concentration is 0.01～0.5mol/L, stirring makes its hydrolysis complete, obtains steady
Fixed alcosol；
S2：It is added dropwise in the alcosol that the ammoniacal liquor that concentration is 1～10mol/L is prepared to step S1, stirring is aging, obtains wet gel；
S3：Hydrophobically modified is carried out to the wet gel that step S2 is obtained by mixed solution, is put into after being dried in drying box, to nature
Cooling obtains elastic aeroge.
2. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1, surface modification
Agent is octyl phenyl polyoxyethylene ether, TPAOH, DTAB, P123, polyethylene glycol 200,
The mixture of at least one of PEG400, Macrogol 600, lauryl sodium sulfate material.
3. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1, positive silicic acid second
In the mixed solution of ester and MTMS, the molal volume ratio of tetraethyl orthosilicate and MTMS is 1:
1～10.
4. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1, mixing speed
It is 500～1500r/min.
5. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1,25～35
Oxalic acid is added under the conditions of DEG C.
6. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1, oxalic acid is added
Amount cause solution PH be 2～4.
7. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S1, positive silicic acid second
Ester is 1 with the mol ratio of methyl alcohol:1～20.
8. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S2, in stirring shape
Ammoniacal liquor is added under state；The amount for adding ammoniacal liquor causes solution PH for 5～7.
9. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S3, mixed solution
It is 0.05～1 with wet gel mass ratio：1.
10. a kind of preparation method of elastic aeroge according to claim 1, it is characterised in that：In step S3, mixed solution
It is ethanol, hexamethylene, toluene, n-hexane, dimethylbenzene, isobutanol, isooctane, HMDS, HMDO,
MTES, trim,ethylchlorosilane, the mixture of two or more material in MTMS.
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| CN201611092125.7A CN106629752A (en) | 2016-12-01 | 2016-12-01 | Preparation method of elastic aerogel |
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| CN201611092125.7A CN106629752A (en) | 2016-12-01 | 2016-12-01 | Preparation method of elastic aerogel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112592655A (en) * | 2020-12-01 | 2021-04-02 | 国网湖南省电力有限公司 | Fireproof anti-condensation material and preparation method thereof |
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Cited By (1)
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| CN112592655A (en) * | 2020-12-01 | 2021-04-02 | 国网湖南省电力有限公司 | Fireproof anti-condensation material and preparation method thereof |
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Application publication date: 20170510 |