CN109320882A - Silica modified PVDF aeroge, preparation method and the aerogel product including it - Google Patents
Silica modified PVDF aeroge, preparation method and the aerogel product including it Download PDFInfo
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- CN109320882A CN109320882A CN201811310277.9A CN201811310277A CN109320882A CN 109320882 A CN109320882 A CN 109320882A CN 201811310277 A CN201811310277 A CN 201811310277A CN 109320882 A CN109320882 A CN 109320882A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention provides a kind of silica modified PVDF aeroge, preparation method and including its aerogel product, it is related to dielectric material technical field.The preparation method of the silica modified PVDF aeroge is that vinylidene is dissolved in organic solution, and presoma silicon source is added and mixes obtained precursor solution, then obtained precursor sol and still aging is hydrolyzed in precursor solution, solvent displacement and drying then are carried out to the precursor sol after ageing, silica modified PVDF aeroge is made.The aeroge is during the preparation process due to joined vinylidene, the structure of PVDF (Kynoar) is formd in the internal structure of aeroge, since Kynoar has extraordinary high temperature resistant and resistance to acid and alkali, high temperature resistant, the acid-proof alkaline of the application aerogel material can be significantly improved, and then meets existing the needs of applying aeroge in the environment of high temperature and complex chemical composition as heat-insulating heat-preserving material.
Description
Technical field
The present invention relates to dielectric material technical fields, more particularly, to a kind of silica modified PVDF aeroge, preparation
Method and aerogel product including it.
Background technique
Aeroge has the characteristics that low-density, high-specific surface area, high porosity, is known as " changing the magical material in the world
Material ".Since there are a large amount of nanoscale hole holes in aeroge, brilliant thermal and insulating performance is made it have, is thermal coefficient pole
Low solid material, thermal coefficient is about 0.013W/ (mK) at normal temperature, also lower than still air.Aeroge simultaneously
Also have the characteristics that stability is high, environmentally protective, there is good hydrophobic effect later by modified, in liquefied natural gas
(LNG) all there is huge application prospect in the low temperature cold insulation such as pipeline, storage tank and ship field.
But the very low only 0.03-0.38g/cc of the density of aeroge, in addition it also has the porosity more than 95%, receives
Meter level is filled with gas in aperture, these design features are especially suitable for heat-insulated and heat preservation, in which: low-density and full of air
Micropore can reduce conduction bring energy loss, and curved small nano-size pores can minimize convection current.Although aeroge has upper
Excellent performance is stated, the low-density and high porosity of itself but cause the mechanical strength of aeroge very low, and it is easily broken, from
And limit its scope of application among small scale experiments and basic research, such as want in special dimension using aeroge as heat-insulated
And thermal insulation material, high temperature resistant, acid-proof alkaline must be improved.
Therefore, one kind is researched and developed while keeping aeroge excellent properties, and can significantly improve aerogel material
High temperature resistant, acid-proof alkaline aerogel products, using meet it is existing by aeroge as heat-insulating heat-preserving material in high temperature and
The demand applied in the environment of complex chemical composition becomes very necessary and urgent.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of silica modified PVDF aeroge, the airsetting
Due to joined vinylidene in the preparation process of glue, form PVDF's (Kynoar) in the internal structure of aeroge
Structure can significantly improve the application aeroge since Kynoar has extraordinary high temperature resistant and resistance to acid and alkali
The high temperature resistant of material, acid-proof alkaline, so meet it is existing using aeroge as heat-insulating heat-preserving material in high temperature and chemical component
The demand applied under complex environment.
The second object of the present invention is to provide a kind of silica modified PVDF aeroge, and the aeroge is by above-mentioned dioxy
The preparation method of the modified PVDF aeroge of SiClx is made, and silica modified PVDF aeroge prepared by the above method is resistance to
High-temperature behavior can achieve >=300 DEG C, and specific surface area is in 300~700m2/ g, thermal coefficient is in≤0.03W/ (mK), simultaneously
Also there is good acid-proof alkaline.
The third object of the present invention is to provide a kind of aerogel product, which includes that above-mentioned silica changes
Property PVDF aeroge, the aerogel product includes but is not limited to aerogel blanket etc..
A kind of preparation method of silica modified PVDF aeroge provided by the invention, the preparation method includes following
Step:
Firstly, vinylidene is dissolved in organic solution, and presoma silicon source is added and mixes obtained precursor solution, so
Obtained precursor sol and still aging is hydrolyzed in precursor solution afterwards, then the precursor sol after ageing is carried out molten
Agent displacement and drying, are made silica modified PVDF aeroge.
Further, the organic solution is any in dimethylformamide, dimethyl acetamide or dimethyl sulfoxide
It is a kind of.
Preferably, the presoma silicon source is ethyl orthosilicate or sodium silicate solution.
Further, the mass ratio of the vinylidene, organic solution and presoma silicon source is 1:(5~8): (1~
1.5)。
Further, the method that the precursor solution is hydrolyzed are as follows: under stirring conditions, the side that water is added dropwise
Formula is added in precursor solution；
Further, the mass ratio of the precursor solution and water is 4~6:1；
Preferably, the rate of the dropwise addition is 6~8ml/min.
Further, the still aging temperature is 10~30 DEG C, 20~30min of time.
Further, the solvent is replaced into be aged precursor sol after molding and be placed in alcohol or deionized water and carry out
Solvent displacement；
Preferably, the number of the solvent displacement is 4~8 times, and each time swap is 8~10h.
Further, the temperature of the drying is 120~200 DEG C.
A kind of silica modified PVDF aeroge provided by the invention, the aeroge is by above-mentioned silica modified
The preparation method of PVDF aeroge is made.
A kind of aerogel product provided by the invention, including above-mentioned silica modified PVDF aeroge.
Compared with prior art, the invention has the benefit that
The preparation method of silica modified PVDF aeroge provided by the invention is organic molten for vinylidene to be dissolved in
In liquid, and presoma silicon source is added and mixes obtained precursor solution, it is molten that obtained presoma then is hydrolyzed in precursor solution
Glue is simultaneously still aging, then carries out solvent displacement and drying to the precursor sol after ageing, silica modified PVDF is made
Aeroge.The aeroge forms PVDF in the internal structure of aeroge during the preparation process due to joined vinylidene
The structure of (Kynoar) can be mentioned significantly since Kynoar has extraordinary high temperature resistant and resistance to acid and alkali
The high temperature resistant of high the application aerogel material, acid-proof alkaline, and then meet and existing exist aeroge as heat-insulating heat-preserving material
The demand applied in the environment of high temperature and complex chemical composition.
Silica modified PVDF aeroge provided by the invention, the aeroge is by above-mentioned silica modified PVDF airsetting
The preparation method of glue is made, and silica modified PVDF aeroge prepared by the above method, high temperature resistance can achieve
>=300 DEG C, specific surface area is in 300~700m2/ g, thermal coefficient also have acidproof well in≤0.03W/ (mK)
Alkaline energy.
Aerogel product provided by the invention includes above-mentioned silica modified PVDF aeroge, the aerogel product packet
Include but be not limited to aerogel blanket etc..
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
According to an aspect of the present invention, a kind of preparation method of silica modified PVDF aeroge, the preparation side
Method the following steps are included:
Firstly, vinylidene is dissolved in organic solution, and presoma silicon source is added and mixes obtained precursor solution, so
Obtained precursor sol and still aging is hydrolyzed in precursor solution afterwards, then the precursor sol after ageing is carried out molten
Agent displacement and drying, are made silica modified PVDF aeroge.
The preparation method of silica modified PVDF aeroge provided by the invention is organic for that will be dissolved in vinylidene
In solution, and presoma silicon source is added and mixes obtained precursor solution, obtained presoma then is hydrolyzed in precursor solution
Colloidal sol is simultaneously still aging, then carries out solvent displacement and drying to the precursor sol after ageing, is made silica modified
PVDF aeroge.The aeroge forms in the internal structure of aeroge during the preparation process due to joined vinylidene
The structure of PVDF (Kynoar) can be shown since Kynoar has extraordinary high temperature resistant and resistance to acid and alkali
The high temperature resistant for improving the application aerogel material, acid-proof alkaline are write, and then is met existing using aeroge as heat-insulation and heat-preservation material
Expect the demand applied in the environment of high temperature and complex chemical composition.
In the preferred embodiment of the present invention, the organic solution is dimethylformamide, dimethyl acetamide
Or any one in dimethyl sulfoxide.
As a preferred embodiment, above-mentioned dimethylformamide, dimethyl acetamide or dimethyl sulfoxide can be with
It is completely dissolved in vinylidene in organic solution, and then in the hydrolytic process in later period, the application is made by polymerization reaction
The inside of aeroge forms the structure of PVDF (Kynoar).
In the preferred embodiment of the present invention, the presoma silicon source is ethyl orthosilicate or sodium silicate solution.
As a preferred embodiment, above-mentioned ethyl orthosilicate or sodium silicate solution are as presoma silicon source to be formed
Aerosil.
Preferably, the solvent of the sodium silicate solution is ethyl alcohol, and the content of sodium metasilicate is 10~20wt%.
In the preferred embodiment of the present invention, the vinylidene, organic solution and presoma silicon source quality
Than for 1:(5~8): (1~1.5).
In the preferred embodiment of the present invention, the method that the precursor solution is hydrolyzed are as follows: in stirring
Under the conditions of, water is added in precursor solution in a manner of being added dropwise；
In above-mentioned preferred embodiment, the mass ratio of the precursor solution and water is 5:1；
It is furthermore preferred that the rate of the dropwise addition is 6~8ml/min.
In the preferred embodiment of the present invention, the still aging temperature is 10~30 DEG C, the time 20~
30min。
In the present invention, it is 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C and 30 DEG C that still aging temperature is typical but non-limiting.
In the preferred embodiment of the present invention, the solvent is replaced into and will be aged precursor sol after molding and set
Solvent displacement is carried out in alcohol or deionized water；
Preferably, the number of the solvent displacement is 4~8 times, and each time swap is 8~10h.
In the preferred embodiment of the present invention, the temperature of the drying is 120~200 DEG C.
According to an aspect of the present invention, a kind of silica modified PVDF aeroge, the aeroge is by above-mentioned dioxy
The preparation method of the modified PVDF aeroge of SiClx is made.
Silica modified PVDF aeroge provided by the invention, the aeroge is by above-mentioned silica modified PVDF airsetting
The preparation method of glue is made, and silica modified PVDF aeroge prepared by the above method, high temperature resistance can achieve
>=300 DEG C, specific surface area is in 300~700m2/ g, thermal coefficient also have acidproof well in≤0.03W/ (mK)
Alkaline energy.
According to an aspect of the present invention, a kind of aerogel product, including above-mentioned silica modified PVDF aeroge.
Aerogel product provided by the invention includes above-mentioned silica modified PVDF aeroge, the aerogel product packet
Include but be not limited to aerogel blanket etc..
Technical solution of the present invention is described further below in conjunction with embodiment and comparative example.
Embodiment 1
A kind of preparation method of silica modified PVDF aeroge, the preparation method comprises the following steps:
(1), vinylidene is dissolved in dimethylformamide first, and ethyl orthosilicate is added and mixes obtained presoma
Solution, the mass ratio of the vinylidene, dimethylformamide and ethyl orthosilicate are 1:5:1.
(2), under stirring conditions, water is added in precursor solution in a manner of being added dropwise, obtained forerunner is hydrolyzed
The mass ratio of body colloidal sol, the precursor solution and water is 5:1, and the rate of the dropwise addition is 6ml/min.
(3), by precursor sol under conditions of 10 DEG C, still aging 20min will then be aged presoma after molding
Colloidal sol, which is placed in deionized water, carries out solvent displacement 4 times, and each time swap is 8h, is finally dried at 120 DEG C, is made
Silica modified PVDF aeroge.
Embodiment 2
A kind of preparation method of silica modified PVDF aeroge, the preparation method comprises the following steps:
(1), vinylidene is dissolved in dimethyl acetamide first, and sodium silicate solution is added and mixes obtained presoma
Solution,
The mass ratio of the vinylidene, dimethyl acetamide and sodium silicate solution is 1:8:1.5；
The solvent of the sodium silicate solution is ethyl alcohol, and the content of sodium metasilicate is 10wt%.
(2), under stirring conditions, water is added in precursor solution in a manner of being added dropwise, obtained forerunner is hydrolyzed
The mass ratio of body colloidal sol, the precursor solution and water is 5:1, and the rate of the dropwise addition is 8ml/min.
(3), by precursor sol under conditions of 30 DEG C, still aging 30min will then be aged presoma after molding
Colloidal sol, which is placed in deionized water, carries out solvent displacement 8 times, and each time swap is 10h, is finally dried at 200 DEG C, is made
Obtain silica modified PVDF aeroge.
Embodiment 3
A kind of preparation method of silica modified PVDF aeroge, the preparation method comprises the following steps:
(1), vinylidene is dissolved in dimethyl sulfoxide first, and it is molten that the obtained presoma of ethyl orthosilicate mixing is added
Liquid, the mass ratio of the vinylidene, dimethyl sulfoxide and ethyl orthosilicate are 1:6:1.2.
(2), under stirring conditions, water is added in precursor solution in a manner of being added dropwise, obtained forerunner is hydrolyzed
The mass ratio of body colloidal sol, the precursor solution and water is 5:1, and the rate of the dropwise addition is 7ml/min.
(3), by precursor sol under conditions of 15 DEG C, still aging 22min will then be aged presoma after molding
Colloidal sol, which is placed in deionized water, carries out solvent displacement 5 times, and each time swap is 9h, is finally dried at 150 DEG C, is made
Silica modified PVDF aeroge.
Embodiment 4
A kind of preparation method of silica modified PVDF aeroge, the preparation method comprises the following steps:
(1), vinylidene is dissolved in dimethylformamide first, and sodium silicate solution is added and mixes obtained presoma
Solution, the mass ratio of the vinylidene, dimethylformamide and sodium silicate solution are 1:7:1.4.
The solvent of the sodium silicate solution is ethyl alcohol, and the content of sodium metasilicate is 20wt%.
(2), under stirring conditions, water is added in precursor solution in a manner of being added dropwise, obtained forerunner is hydrolyzed
The mass ratio of body colloidal sol, the precursor solution and water is 5:1, and the rate of the dropwise addition is 6ml/min.
(3), by precursor sol under conditions of 18 DEG C, still aging 28min will then be aged presoma after molding
Colloidal sol, which is placed in deionized water, carries out solvent displacement 7 times, and each time swap is 10h, is finally dried at 180 DEG C, is made
Obtain silica modified PVDF aeroge.
Embodiment 5
A kind of preparation method of silica modified PVDF aeroge, the preparation method comprises the following steps:
(1), vinylidene is dissolved in dimethyl acetamide first, and sodium silicate solution is added and mixes obtained presoma
Solution, the mass ratio of the vinylidene, dimethyl acetamide and sodium silicate solution are 1:6:1.3；
The solvent of the sodium silicate solution is ethyl alcohol, and the content of sodium metasilicate is 15wt%.
(2), under stirring conditions, water is added in precursor solution in a manner of being added dropwise, obtained forerunner is hydrolyzed
The mass ratio of body colloidal sol, the precursor solution and water is 5:1, and the rate of the dropwise addition is 7ml/min.
(3), by precursor sol under conditions of 20 DEG C, still aging 25min will then be aged presoma after molding
Colloidal sol, which is placed in deionized water, carries out solvent displacement 6 times, and each time swap is 9h, is finally dried at 160 DEG C, is made
Silica modified PVDF aeroge.
Comparative example 1
This comparative example is not in addition to including vinylidene in preparation process, remaining is the same as embodiment 5.
Comparative example 2
Quality of this comparative example except vinylidene, dimethylformamide and sodium silicate solution in step (1) precursor solution
Outside for 0.8:6:1.3, remaining is the same as embodiment 5.
Comparative example 3
This comparative example is in addition to the mass ratio of step (2) precursor solution and water is 3:1, remaining is the same as embodiment 5.
Experimental example 1
In order to show that the silica modified PVDF aeroge that is prepared of the present invention has high temperature resistant, acid and alkali-resistance, compares table
The advantage that area is big, thermal conductivity is good, existing spy will prepare silica modified in the embodiment of the present invention 1~5 and comparative example 1~3
PVDF aeroge carries out the detection of high temperature resistant, acid and alkali-resistance, specific surface area, thermal coefficient, and the results are shown in following table 1.
(1) high temperature resistant is tested
Aeroge is placed on a test board, the test board is placed 10 days in the environment of 300 DEG C, observes airsetting
The situation of change of glue.
(2) resistance to acid and alkali is tested:
Aeroge is placed on a test board, by the test board 25 DEG C acid, place 30 days in aqueous slkali, observe
The case where aeroge weathers.
(3) specific surface area (m2/g)
It is measured using the SPECTOMETER1990 type specific surface pore size determination instrument that company of power & light company of the U.S. produces.
(4) thermal coefficient [W/ (mK)]
Using STA449C type heat conduction coefficient tester to measuring thermal coefficient.Operating method are as follows: grind prepared gas
Gel can be measured and be led in pop one's head in upper laying about 1cm thickness powder (using sample holder small size, not be compacted) to superfine powder
Hot coefficient.
Table 1: the performance test results of the silica modified PVDF aeroge of embodiment and comparative example preparation
As above-mentioned table 1 it is found that silica modified PVDF aeroge, heat-resisting quantity made from the embodiment of the present invention 1~5
>=300 DEG C can be can achieve, placed in the environment of 300 DEG C 10 days it is unchanged, specific surface area is in 300~700m2/g, thermally conductive system
Number in≤0.03W/ (mK), while also have good acid-proof alkaline, high temperature resistant, acid-proof alkaline, specific surface area and
Thermal coefficient is superior to the silica modified PVDF aeroge that comparative example 1~3 is prepared
The silica modified PVDF aeroge that comparative example 1 does not include vinylidene does not have the property of high temperature resistant and acid and alkali-resistance
Energy；Comparative example 2 leads to silica modified PVDF aeroge obtained since the content of vinylidene in precursor solution is lower
High temperature resistant and the performance of acid and alkali-resistance are poor, while specific surface area and thermal coefficient performance are also poor；During comparative example 3 hydrolyzes
Since the quality of precursor solution and water is relatively low, causes to hydrolyze and be not thorough, silica modified PVDF aeroge obtained
Properties corresponding requirement is also not achieved.
In conclusion the preparation method of silica modified PVDF aeroge provided by the invention is to dissolve vinylidene
In organic solution, and presoma silicon source is added and mixes obtained precursor solution, then precursor solution is hydrolyzed obtained
Precursor sol then successively carries out still aging, solvent displacement and drying to precursor sol, is made silica modified
PVDF aeroge.The aeroge forms in the internal structure of aeroge during the preparation process due to joined vinylidene
The structure of PVDF (Kynoar) can be shown since Kynoar has extraordinary high temperature resistant and resistance to acid and alkali
The high temperature resistant for improving the application aerogel material, acid-proof alkaline are write, and then is met existing using aeroge as heat-insulation and heat-preservation material
Expect the demand applied in the environment of high temperature and complex chemical composition.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of preparation method of silica modified PVDF aeroge, which is characterized in that the preparation method includes following step
It is rapid:
Firstly, vinylidene is dissolved in organic solution, and presoma silicon source is added and mixes obtained precursor solution, then will
Obtained precursor sol and still aging is hydrolyzed in precursor solution, then carries out solvent to the precursor sol after ageing and sets
It changes and dries, silica modified PVDF aeroge is made.
2. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that described organic
Solution is any one in dimethylformamide, dimethyl acetamide or dimethyl sulfoxide；
Preferably, the presoma silicon source is ethyl orthosilicate or sodium silicate solution.
3. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that the inclined fluorine
The mass ratio of ethylene, organic solution and presoma silicon source is 1:(5~8): (1~1.5).
4. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that the forerunner
The method that liquid solution is hydrolyzed are as follows: under stirring conditions, water is added in precursor solution in a manner of being added dropwise.
5. the preparation method of silica modified PVDF aeroge according to claim 4, which is characterized in that the forerunner
The mass ratio of liquid solution and water is 4~5:1；
Preferably, the rate of the dropwise addition is 6~8ml/min.
6. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that the standing
The temperature of ageing is 10~30 DEG C, 20~30min of time.
7. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that the solvent
Precursor sol after molding will be aged by, which being replaced into, is placed in progress solvent displacement in alcohol or deionized water；
Preferably, the number of the solvent displacement is 4~8 times, and each time swap is 8~10h.
8. the preparation method of silica modified PVDF aeroge according to claim 1, which is characterized in that the drying
Temperature be 120~200 DEG C.
9. a kind of silica modified PVDF aeroge, which is characterized in that the aeroge is by any one of claim 1~8 institute
The preparation method for the silica modified PVDF aeroge stated is made.
10. a kind of aerogel product, which is characterized in that including silica modified PVDF aeroge as claimed in claim 9.
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| CN112852079A (en) * | 2021-01-18 | 2021-05-28 | 陕西科技大学 | Super-hydrophobic self-cleaning radiation self-cooling material and preparation method thereof |
| CN112852079B (en) * | 2021-01-18 | 2022-09-06 | 陕西科技大学 | Super-hydrophobic self-cleaning radiation self-cooling material and preparation method thereof |
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