CN104610550B - Method for preparing polysiloxane aerogel - Google Patents
Method for preparing polysiloxane aerogel Download PDFInfo
- Publication number
- CN104610550B CN104610550B CN201510068291.2A CN201510068291A CN104610550B CN 104610550 B CN104610550 B CN 104610550B CN 201510068291 A CN201510068291 A CN 201510068291A CN 104610550 B CN104610550 B CN 104610550B
- Authority
- CN
- China
- Prior art keywords
- polysiloxanes
- aeroge
- supercritical
- catalyst
- fluid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for preparing polysiloxane aerogel. The preparation method comprises the following steps: carrying out a cross-linking reaction between hydrogen-containing polysiloxane and vinyl polysiloxane in a supercritical fluid in the presence of a catalyst, thereby obtaining the polysiloxane aerogel. The supercritical fluid can be any one of supercritical carbon dioxide fluid, supercritical methane fluid and supercritical nitrogen dioxide fluid, and the catalyst can be a Karstedt's catalyst or chloroplatinic acid. By utilizing a green solvent, a flexible cuttable knittable super-hydrophobic silica aerogel material is prepared in the supercritical fluid by virtue of a simple one-step method; the obtained silica aerogel has high flexibility and ultrahigh hydrophobicity and can perform cutting and knitting, and the application requirements on different shapes, different conditions and different needs are met; and moreover, the production cost is low, the production process is simple and environment-friendly, and industrial production is easily realized.
Description
Technical field
The present invention relates to a kind of preparation method of polysiloxanes aeroge, can weave super-hydrophobic poly- particularly to a kind of flexibility
The preparation method of siloxanes aeroge.
Background technology
When most of solvent sloughed by gel, in gel content liquid than solids content much less, or space networks of gel
Gassy in shape structure, appearance is in solid-like, referred to as aeroge.The species of aeroge is a lot, has silicon systems, carbon system, sulphur system, gold
Belong to oxide system or metal system etc..Typically common aeroge is silica aerogel, earliest by American science worker Kistler
It was obtained in 1931.Due to its nanometer of loose porous characteristic, aeroge is in high-tech light laser low density target material, effectively insulating
The aspects such as material, acoustical delay material, high performance catalyst are all widely used.
Silica aerogel has nanoporous three-dimensional net structure, high porosity, low-density, high-specific surface area and high pore volume
The feature of rate, has important using value, such as：The three-dimensional manometer network structure having can limit local thermal excitation effectively
Propagation, therefore can apply to heat-insulated field；The low acoustic-velocity characteristic having, therefore can be used for acoustical delay or high temperature acoustic；
There is high specific surface area, therefore can be used as new catalyst or catalyst carrier.
The method preparing polysiloxanes aeroge commonly used at present is sol-gal process, and the method is usually alkoxy silane
Si(OR)4/SiR1(OR2)3Realize through processes such as collosol and gel, aging and dried process in organic solvent.In the method,
In sol-gel process, by controlling Si (OR)4/SiR1(OR2)3Poly-condensation and hydrolysis condition, formed different in system
The nanocluster of structure, the inter-adhesive formation gelinite between cluster, and be then filled with around the solid-state skeleton of gelinite
Machine liquid reagent；Form three-dimensional net structure through ageing process so as to be condensed further；In order to anti-in follow-up dry run
Only the surface tension in gel pore hole leads to the destruction of material structure, generally adopt supercritical drying, environmental pressure to be dried and
The methods such as vacuum drying.However, the method processing step is numerous, waste time and energy, and it is dirty to introduce a large amount of solvents in preparation process
Dye, the feature of environmental protection is poor, and the aerogel products pliability prepared is poor, mechanical strength low it is impossible to opposing repeatedly circulate with substantially
Overstock contracting it is impossible to meet extensive commercial Application demand.
Content of the invention
It is an object of the invention to provide a kind of preparation method of polysiloxanes aeroge, this preparation method solution poly- silicon at present
The loaded down with trivial details time-consuming, feature of environmental protection of oxygen alkane aeroge preparation process is poor and the problems such as bad mechanical property.
A kind of preparation method of polysiloxanes aeroge that the present invention provides, comprises the steps：
In supercritical fluid, under conditions of catalyst exists, hydrogen containing siloxane and vinyl polysiloxane are through handing over
Connection reaction can get described polysiloxanes aeroge.
Polysiloxanes in the present invention refers to that main chain isPolymer, R1-R4Represent organic group, its
Middle R1、R2、R3And R4Can be identical, can be different, n, m are natural number, m with n can be identical, can be different.Described hydrogeneous poly- silicon
Oxygen alkane refers to the R in chain1-R4At least one is the polysiloxanes of hydrogen, or the end of the chain at least one end is the polysiloxanes of hydrogen；Described
Vinyl polysiloxane is the R in chain1-R4At least one is the polysiloxanes of vinyl, or in the end of the chain, at least one end is ethene
The polysiloxanes of base.
Described hydrogen containing siloxane concretely methyl hydrogen polysiloxanes, R in its repetitive1-R4One of be
Hydrogen, remaining is methyl, and end group is methyl.
Described vinyl polysiloxane concretely end-vinyl dimethyl polysiloxane, the R in its repetitive1-R4All
For methyl, two end groups are vinyl.
Described hydrogen containing siloxane and the crosslinked reaction of described vinyl polysiloxane can generate three-dimensional net structure
Aeroge, i.e. described polysiloxanes aeroge.
In above-mentioned preparation method, described supercritical fluid is supercritical carbon dioxide fluid, supercritical methane fluid and super
Any one in critical nitrogen dioxide fluid.
In above-mentioned preparation method, the addition of described catalyst is described hydrogen containing siloxane and the poly- silica of described vinyl
The 0.01%～1% of alkane quality sum, concretely 0.01%～0.1%, 0.01%～0.05%, 0.05%～0.1%,
0.01%th, 0.05% or 0.1%.
Described catalyst is catalyst made from platonic, and described catalyst made from platonic is Karstedt ' s catalyst or chloroplatinic acid.
In above-mentioned preparation method, in the molal quantity of the Si-H in described hydrogen containing siloxane and described vinyl polysiloxane
The molal quantity of vinyl ratio be 1.4～0.7：1.0, concretely 1.4～1.0：1.0,0.7～1.0：1.0、1.4：
1.0、1.0：1.0 or 0.7：1.0；
In described hydrogen containing siloxane, the quality (H in Si-H) of hydrogen atom can be the quality of described hydrogen containing siloxane
0.1%～1.4% (hydrogen content), concretely 0.2% or 0.4%；The molecular weight of described hydrogen containing siloxane can be 1000
～15000g/mol, concretely 1500～3000g/mol, 4000～8000g/mol or 10000～15000g/mol；
The molecular weight of described vinyl polysiloxane can be 1000～20000g/mol, concretely 1500～13000g/
Mol, 1500～3000g/mol, 5000～8000g/mol or 9000～13000g/mol.
In above-mentioned preparation method, the temperature of described cross-linking reaction can be 40～120 DEG C, concretely 40～80 DEG C, 40～
60 DEG C, 60～80 DEG C, 40 DEG C, 60 DEG C or 80 DEG C；Pressure can be 7MPa～60MPa, concretely 16～25MPa, 16MPa or
25MPa；
The time of described cross-linking reaction is 1～24h, concretely 1～4h, 4～24h, 1h, 4h or 24h.
In above-mentioned preparation method, when described supercritical fluid is supercritical carbon dioxide fluid, described overcritical dioxy
After change carbon flow body can be by being filled with carbon dioxide in reactor, obtain at described temperature and described pressure.
Invention further provides a kind of polysiloxanes aeroge being prepared using above-mentioned preparation method, this poly- silicon
Oxygen alkane aeroge has high flexibility and superelevation hydrophobicity, can carry out cutting and weave processing again, can meet different shape, different bar
The application demand such as part and different requirement.
The preparation method of polysiloxanes aeroge of the present invention has the advantage that：
1st, the present invention uses green solvent, is prepared flexible cleavable in supercritical carbon dioxide by simple one-step method
Super-hydrophobic silicon aerogel material can be woven.
2nd, the silica aerogel of gained of the present invention has high flexibility and superelevation hydrophobicity, can carry out cutting and weave processing again,
Meet the application demands such as different shape, different condition and different requirement.
3rd, low production cost of the present invention, production process simple and environmentally-friendly it is easy to industrialized production.
Brief description
Fig. 1 is the electron scanning micrograph of the polysiloxanes aeroge preparing in embodiment 1.
Fig. 2 is the transmission electron microscope photo of the polysiloxanes aeroge preparing in embodiment 1.
Fig. 3 is the contact angle to water for the polysiloxanes aeroge preparing in embodiment 1.
Fig. 4 is the mechanical experimental results of polysiloxanes aeroge, wherein Fig. 4 a) make in embodiment 1 and embodiment 4
The uniaxial compression curve of the standby polysiloxanes aeroge obtaining；Fig. 4 b)～Fig. 4 d) it is the poly- silica preparing in embodiment 1
Uniaxial cycling compresses the load-deformation curve of 100 times, Fig. 4 b to alkane aeroge at different temperatures)：Room temperature, Fig. 4 c)：150 DEG C,
Fig. 4 d)：-50℃.
Fig. 5 is the photo of the polysiloxanes aeroge preparing in embodiment 1.
Fig. 6 is the cutting of polysiloxanes aeroge and suture figure preparing in embodiment 1, and wherein, Fig. 6 (a) is to cut
Cut figure, Fig. 6 (b) is suture figure.
Specific embodiment
Experimental technique used in following embodiments if no special instructions, is conventional method.
Material used, reagent etc. in following embodiments, if no special instructions, all commercially obtain.
Embodiment 1, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 5.12g are 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.05% of based polysiloxane quality sum) it is added in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2It is in Supercritical Conditions, reaction released CO after 4 hours2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
As depicted in figs. 1 and 2, be the polysiloxanes aeroge that said method prepares SEM
(SEM) photo and transmission electron microscope (TEM) photo, as seen from the figure, this polysiloxanes aeroge is loose porous
Three-dimensional net structure, the aperture that can be seen that hole from SEM in figure is 8 μm, can be seen that this aeroge also exists from TEM in figure
Aperture is the hole of 30～180nm.
Embodiment 2, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 0.71g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 4.06g are 5000-8000g/mol (mean molecule quantity is 6000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.05% of based polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2It is in Supercritical Conditions, reaction released CO after 4 hours2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 1.0：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 3, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 0.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (its hydrogen content is 0.2wt%), the molecular weight of 7.80g are that (mean molecule quantity is 10000g/ to 9000-13000g/mol
Mol (quality is methyl hydrogen polysiloxanes and end ethene for end-vinyl dimethyl polysiloxane) and Karstedt ' s catalyst
The 0.05% of base dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with the pressure making system
Reach 16MPa, simultaneously CO2In a supercritical state, release CO after heat-insulation pressure keeping 4h2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 1.0：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 4, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 4000-8000g/mol (mean molecule quantity is 6000g/mol)
Oxygen alkane (hydrogen content is 0.4wt%), the molecular weight of 10.24g are 1500-3000g/mol (mean molecule quantity is 2900g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.05% of based polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2In a supercritical state, release CO after heat-insulation pressure keeping 4h2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 1.0：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 5, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The methyl hydrogen that the molecular weight of 0.62g is 10000～15000g/mol (mean molecule quantity is 12000g/mol)
Polysiloxanes (hydrogen content is 0.4wt%), the molecular weight of 2.56g are that (mean molecule quantity is 2900g/ to 1500～3000g/mol
Mol (quality is methyl hydrogen polysiloxanes and end ethene for end-vinyl dimethyl polysiloxane) and Karstedt ' s catalyst
The 0.05% of base dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with the pressure making system
Reach 16MPa, simultaneously CO2In a supercritical state, release CO after heat-insulation pressure keeping 4h2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 1.4：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 6, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silica of methyl hydrogen that the molecular weight of 0.9g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Alkane (hydrogen content is 0.2wt%), the molecular weight of 2.56g are the end of 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl dimethyl for Vinyl Dimethicone and Karstedt ' s catalyst
The 0.05% of polysiloxanes quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2In a supercritical state, release CO after heat-insulation pressure keeping 4h2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 7, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 5.12g are 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.05% of based polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
25MPa, CO simultaneously2In a supercritical state, release CO after heat-insulation pressure keeping 4h2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 8, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 5.12g are 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.01% of based polysiloxane quality sum) it is added in 50mL reactor, CO at 40 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2It is in Supercritical Conditions, after heat-insulation pressure keeping 24h, release CO2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 9, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 5.12g are 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.01% of based polysiloxane quality sum) it is added in 50mL reactor, CO at 80 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2It is in Supercritical Conditions, after heat-insulation pressure keeping 4h, release CO2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
Embodiment 10, the preparation of polysiloxanes aeroge
The preparation method of polysiloxanes aeroge, comprises the steps：
The poly- silicon of methyl hydrogen that the molecular weight of 1.80g is 1500-3000g/mol (mean molecule quantity is 1700g/mol)
Oxygen alkane (hydrogen content is 0.2wt%), the molecular weight of 5.12g are 1500-3000g/mol (mean molecule quantity is 2000g/mol)
(quality is methyl hydrogen polysiloxanes and end-vinyl diformazan for end-vinyl dimethyl polysiloxane and Karstedt ' s catalyst
The 0.1% of based polysiloxane quality sum) it is added in 50mL reactor, CO at 60 DEG C2It is filled with and so that the pressure of system is reached
16MPa, CO simultaneously2It is in Supercritical Conditions, after heat-insulation pressure keeping 1h, release CO2Directly obtain Monolithic aerogel.
Vinyl in the molal quantity of Si-H and vinyl polysiloxane in methyl hydrogen polysiloxanes in the present embodiment
The ratio of molal quantity is 0.7：1.0.
SEM (SEM) photo of the polysiloxanes aeroge preparing in the present embodiment and transmitted electron
Microscope (TEM) photo and Fig. 1 and Fig. 2 no significant difference.
The performance test of the polysiloxanes aeroge preparing in embodiment 1-10
(1) hydrophobicity test：
Measure the contact angle of the polysiloxanes aeroge preparing in embodiment 1 and water, knot using contact angle visualizer
, as shown in figure 3, its contact angle is 152 °, the obtained contact angle of polysiloxanes aeroge in other embodiments is with Fig. 1 no for fruit
Significantly difference, shows that the polysiloxanes aerosol that the inventive method prepares has good hydrophobicity.
(2) Mechanics Performance Testing：
Fig. 4 is the mechanical experimental results of polysiloxanes aeroge, wherein Fig. 4 a) make in embodiment 1 and embodiment 4
The uniaxial compression curve of the standby polysiloxanes aeroge obtaining, as seen from the figure, the polysiloxanes aeroge that the present invention prepares
Flexibility good, wherein, in uniaxial compression curve the Young's modulus of embodiment 4 be higher than embodiment 1 Young's modulus, embodiment
The aeroge of 1 aeroge relatively embodiment 4 is soft, this is because the friendship of the polysiloxanes preparing in embodiment 1
Connection density is less than the crosslink density of the polysiloxanes prepare in embodiment 4.
Fig. 4 b)～Fig. 4 d) it is the polysiloxanes aeroge uniaxial cycling pressure at different temperatures preparing in embodiment 1
The load-deformation curve that contracting is 100 times, wherein, Fig. 4 b) it is room temperature, Fig. 4 c) it is 150 degree, Fig. 4 d) spend for -50, permissible by this figure
Find out, the polysiloxanes aeroge that the present invention prepares has good resistance against compression within the scope of wider temperature, and this is
Because the main chain of the aeroge that the present invention prepares is flexible high, heat-resist, low temperature resistant O-Si-O chain, and such gas
Gel has three-dimensional net structure.
Fig. 5 is the photo of the polysiloxanes aeroge preparing in embodiment 1, obtained poly- silicon in other embodiments
Oxygen alkane aeroge and Fig. 5 no significant difference, from this figure it is also seen that the polysiloxanes aerosol that the present invention prepares has
Excellent flexibility.
(3) cuttability and stitchability：
In embodiment 1, any one prepared flexible aerogel material all can carry out arbitrary shape and cuts out, cuts and stitch
Close, as shown in fig. 6, Fig. 6 (a) is cutting drawing, Fig. 6 (b) is suture figure.
(4) heat-proof quality test：
Respectively the heat-proof quality of the polysiloxanes aeroge preparing in embodiment 1-10 is tested, result is such as
Under：
The heat-proof quality test result of the polysiloxanes aeroge preparing in table 1 embodiment 1-10
| Sample | Thermal conductivity W/ (m K) |
| Embodiment 1 | 0.021 |
| Embodiment 2 | 0.027 |
| Embodiment 3 | 0.034 |
| Embodiment 4 | 0.028 |
| Embodiment 5 | 0.029 |
| Embodiment 6 | 0.022 |
| Embodiment 7 | 0.025 |
| Embodiment 8 | 0.033 |
| Embodiment 9 | 0.034 |
| Embodiment 10 | 0.037 |
As can be seen from Table 1, using the polysiloxanes aeroge that the inventive method prepares, there is superinsulation performance.
Claims (6)
1. a kind of preparation method of polysiloxanes aeroge, comprises the steps：
In supercritical fluid, under conditions of catalyst exists, hydrogen containing siloxane and vinyl polysiloxane are crosslinked anti-
Described polysiloxanes aeroge should be can get；
The ratio of the molal quantity of the molal quantity of Si-H and described vinyl polysiloxane medium vinyl in described hydrogen containing siloxane
For 1.4～0.7：1.0；
In described hydrogen containing siloxane, the molal quantity of hydrogen atom be the molal quantity of described hydrogen containing siloxane 0.1%～
1.4%, molecular weight is 1000～15000g/mol；
The molecular weight of described vinyl polysiloxane is 1000～20000g/mol；
The temperature of described cross-linking reaction is 40～120 DEG C, and pressure is 7MPa～60MPa；
The time of described cross-linking reaction is 1～24h.
2. preparation method according to claim 1 it is characterised in that：Described supercritical fluid is stream of supercritical carbon dioxide
Any one in body, supercritical methane fluid and overcritical nitrogen dioxide fluid.
3. preparation method according to claim 1 and 2 it is characterised in that：The addition of described catalyst is described hydrogeneous
The 0.01%～1.0% of the quality sum of polysiloxanes and described vinyl polysiloxane；
Described catalyst is catalyst made from platonic, and described catalyst made from platonic is Karstedt ' s catalyst or chloroplatinic acid.
4. preparation method according to claim 1 it is characterised in that：When described supercritical fluid is supercritical carbon dioxide
During fluid, after described supercritical carbon dioxide fluid is by being filled with carbon dioxide in reactor, in described temperature and described pressure
Obtain under power.
5. the polysiloxanes aeroge that the preparation method any one of claim 1-4 prepares.
6. polysiloxanes aeroge according to claim 5 it is characterised in that：Described polysiloxanes aeroge is clipped,
Obtain after cutting or braiding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510068291.2A CN104610550B (en) | 2015-02-10 | 2015-02-10 | Method for preparing polysiloxane aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510068291.2A CN104610550B (en) | 2015-02-10 | 2015-02-10 | Method for preparing polysiloxane aerogel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104610550A CN104610550A (en) | 2015-05-13 |
| CN104610550B true CN104610550B (en) | 2017-02-22 |
Family
ID=53145219
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510068291.2A Expired - Fee Related CN104610550B (en) | 2015-02-10 | 2015-02-10 | Method for preparing polysiloxane aerogel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104610550B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107922738A (en) * | 2015-09-01 | 2018-04-17 | 日立化成株式会社 | Sol composition and aeroge |
| CN105236420A (en) * | 2015-09-06 | 2016-01-13 | 湖南上懿丰新材料科技有限公司 | Method of preparing regular-shaped SiO2 aerogel granules through mechanical cutting |
| CN106242610A (en) * | 2016-08-17 | 2016-12-21 | 哈尔滨工业大学 | A kind of preparation method of SiOC ceramic aerogel |
| CN106398215A (en) * | 2016-08-19 | 2017-02-15 | 青岛科技大学 | Preparation method of flexible polysiloxane electronic packaging material |
| CN110437496B (en) * | 2019-07-19 | 2020-10-27 | 淮阴工学院 | Polysiloxane aerogel composite material for efficient water evaporation and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974384A (en) * | 2006-12-19 | 2007-06-06 | 中国人民解放军国防科学技术大学 | High temperature and high pressure prepn process of SiO2 aerogel |
| CN101948297A (en) * | 2010-09-28 | 2011-01-19 | 航天特种材料及工艺技术研究所 | Autocatalytic aerogel heat insulation composite material and preparation method thereof |
| CN103708476A (en) * | 2014-01-07 | 2014-04-09 | 厦门大学 | Preparation method of flexible silica aerogel |
-
2015
- 2015-02-10 CN CN201510068291.2A patent/CN104610550B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974384A (en) * | 2006-12-19 | 2007-06-06 | 中国人民解放军国防科学技术大学 | High temperature and high pressure prepn process of SiO2 aerogel |
| CN101948297A (en) * | 2010-09-28 | 2011-01-19 | 航天特种材料及工艺技术研究所 | Autocatalytic aerogel heat insulation composite material and preparation method thereof |
| CN103708476A (en) * | 2014-01-07 | 2014-04-09 | 厦门大学 | Preparation method of flexible silica aerogel |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104610550A (en) | 2015-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104610550B (en) | Method for preparing polysiloxane aerogel | |
| CN108727818B (en) | Hydrophobic silicon dioxide/polyimide aerogel composite material and preparation method thereof | |
| Durães et al. | Effect of the drying conditions on the microstructure of silica based xerogels and aerogels | |
| CN108530673B (en) | Linear polyimide aerogel and preparation method thereof | |
| Ding et al. | Flexible, Mechanically Stable, Porous Self‐Standing Microfiber Network Membranes of Covalent Organic Frameworks: Preparation Method and Characterization | |
| Zheng et al. | Assembly of silica aerogels within silica nanofibers: towards a super-insulating flexible hybrid aerogel membrane | |
| TW201710086A (en) | Aerogel composite material | |
| Si et al. | Silicone-based tough hydrogels with high resilience, fast self-recovery, and self-healing properties | |
| JP6329632B2 (en) | Vacuum insulation board with organic airgel | |
| CN104030715A (en) | Preparation method of Cf/BN-SiC composite material | |
| KR102583729B1 (en) | Coating solution, coating film manufacturing method and coating film | |
| US9869422B2 (en) | Method for preparing bulk C—AlN composite aerogel with high strength and high temperature resistance | |
| CN101698591A (en) | Fiber composite carbon aerogel material and preparation method thereof | |
| CN110628217B (en) | Nanofiber modified polyimide aerogel material and preparation method thereof | |
| KR20160101967A (en) | Thermally insulative expanded polytetrafluoroethylene articles | |
| CN106750493A (en) | A kind of preparation method of polyimide aerogels | |
| CN112934128A (en) | Core-shell structure organic-inorganic hybrid nanofiber aerogel elastomer and preparation and application thereof | |
| CN111004541B (en) | 3D printing ink for silicon dioxide aerogel fibers and 3D printing preparation method | |
| CN110372907B (en) | Nanofiber reinforced polyimide aerogel material and preparation method thereof | |
| CN108265517B (en) | Preparation method of folding-resistant polytetrafluoroethylene/glass fiber membrane material | |
| CN105131221B (en) | A kind of preparation method of resorcinol formaldehyde/aerosil | |
| CN114715896B (en) | Preparation method of silicon carbide nanotube aerogel | |
| KR102563187B1 (en) | Crosslinked polymeric membrane and method for producing the same | |
| WO2021146733A1 (en) | Organosilica membranes, methods of making same, and uses thereof | |
| JP7163967B2 (en) | airgel composite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170222 Termination date: 20210210 |