CN104610550A - Method for preparing polysiloxane aerogel - Google Patents
Method for preparing polysiloxane aerogel Download PDFInfo
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- CN104610550A CN104610550A CN201510068291.2A CN201510068291A CN104610550A CN 104610550 A CN104610550 A CN 104610550A CN 201510068291 A CN201510068291 A CN 201510068291A CN 104610550 A CN104610550 A CN 104610550A
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- 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
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- 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 polysiloxane aerogel, particularly a kind of flexibility can weave the preparation method of super-hydrophobic polysiloxane aerogel.
Background technology
When most of solvent sloughed by gel, in gel, content liquid is than solids content much less, or aerification in the space net structure of gel, and appearance is solid state, is called aerogel.The kind of aerogel is a lot, has silicon system, carbon system, sulphur system, burning system or metal system etc.Generally common aerogel is silica aerogel, is obtained the earliest by American science worker Kistler in 1931.Due to the loose porous characteristic of its nanometer, aerogel is all widely used in hi-tech light laser low density target material, high efficiency heat insulation material, acoustical delay material, high performance catalyst etc.
Silica aerogel has the feature of nanoporous three-dimensional net structure, high porosity, low density, high-ratio surface sum height pore volume rate, there is important using value, as: the three-dimensional manometer network structure had can limit the propagation of local thermal excitation effectively, therefore can be applied to heat insulation field; The low acoustic-velocity characteristic had, 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 support of the catalyst.
The method preparing polysiloxane aerogel conventional is at present sol-gel method, and the method is generally organoalkoxysilane Si (OR)
4/ SiR
1(OR
2)
3in organic solvent through process implementations such as collosol and gel, aging and drying treatment.In the method, in sol-gel process, by control Si (OR)
4/ SiR
1(OR
2)
3poly-condensation and hydrolysis condition, in system, form the nanocluster of different structure, the inter-adhesive formation gelinite between cluster, is then full of organic liquid reagent around the solid-state skeleton of gelinite; Through weathering process, its further condensation is made to form three-dimensional net structure; Destruction in order to prevent the surface tension in gel pore hole from causing material structure in follow-up drying process, adopts the methods such as the drying of supercritical drying, environmental stress and vacuum-drying usually.But the method processing step is numerous, wastes time and energy, and in preparation process, introduce a large amount of solvent contamination, the feature of environmental protection is poor, and the aerogel products snappiness prepared is poor, physical strength is low, cannot resist repeatedly circulation and large volume compression, cannot meet industrial application demand widely.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polysiloxane aerogel, this preparation method solve current polysiloxane aerogel preparation process loaded down with trivial details time-consuming, the feature of environmental protection is poor and the problem such as bad mechanical property.
The preparation method of a kind of polysiloxane aerogel provided by the invention, comprises the steps:
In supercutical fluid, under catalyzer existent condition, hydrogen containing siloxane and vinyl polysiloxane can obtain described polysiloxane aerogel through crosslinking reaction.
Polysiloxane in the present invention refers to that main chain is
polymkeric substance, R
1-R
4represent organic group, wherein R
1, R
2, R
3and R
4can be identical, can be different, n, m are natural number, m with n can be identical, can be different.Described hydrogen containing siloxane refers to the R in chain
1-R
4at least one is the polysiloxane of hydrogen, or the end of the chain at least one end be the polysiloxane of hydrogen; Described vinyl polysiloxane is the R in chain
1-R
4at least one is the polysiloxane of vinyl, or in the end of the chain at least one end be the polysiloxane of vinyl.
Described hydrogen containing siloxane specifically can be methyl hydrogen polysiloxane, R in its repeating unit
1-R
4in one be hydrogen, all the other are methyl, and end group is methyl.
Described vinyl polysiloxane specifically can be end-vinyl dimethyl polysiloxane, the R in its repeating unit
1-R
4be methyl, two end groups are vinyl.
Described hydrogen containing siloxane and described vinyl polysiloxane can generate the aerogel of three-dimensional net structure through crosslinking reaction, i.e. described polysiloxane aerogel.
In above-mentioned preparation method, described supercutical fluid is any one in supercritical carbon dioxide fluid, supercritical methane fluid and overcritical nitrogen peroxide fluid.
In above-mentioned preparation method, the add-on of described catalyzer is 0.01% ~ 1% of described hydrogen containing siloxane and described vinyl polysiloxane quality sum, specifically can be 0.01% ~ 0.1%, 0.01% ~ 0.05%, 0.05% ~ 0.1%, 0.01%, 0.05% or 0.1%.
Described catalyzer is catalyst made from platonic, and described catalyst made from platonic is Karstedt ' s catalyzer or Platinic chloride.
In above-mentioned preparation method, the ratio of the mole number of the vinyl in the mole number of the Si-H in described hydrogen containing siloxane and described vinyl polysiloxane is 1.4 ~ 0.7:1.0, specifically can be 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 0.1% ~ 1.4% (hydrogen content) of the quality of described hydrogen containing siloxane, specifically can be 0.2% or 0.4%; The molecular weight of described hydrogen containing siloxane can be 1000 ~ 15000g/mol, specifically can be 1500 ~ 3000g/mol, 4000 ~ 8000g/mol or 10000 ~ 15000g/mol;
The molecular weight of described vinyl polysiloxane can be 1000 ~ 20000g/mol, specifically can be 1500 ~ 13000g/mol, 1500 ~ 3000g/mol, 5000 ~ 8000g/mol or 9000 ~ 13000g/mol.
In above-mentioned preparation method, the temperature of described crosslinking reaction can be 40 ~ 120 DEG C, specifically can be 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, specifically can be 16 ~ 25MPa, 16MPa or 25MPa;
The time of described crosslinking reaction is 1 ~ 24h, specifically can be 1 ~ 4h, 4 ~ 24h, 1h, 4h or 24h.
In above-mentioned preparation method, when described supercutical fluid is supercritical carbon dioxide fluid, described supercritical carbon dioxide fluid, by being filled with after in reactor by carbonic acid gas, obtains at described temperature and described pressure.
Invention further provides a kind of polysiloxane aerogel utilizing above-mentioned preparation method to prepare, this polysiloxane aerogel has high flexibility and superelevation hydrophobicity, cutting can be carried out and weave processing again, the application demands such as different shapes, different condition and different requirements can be met.
Preparation method's tool of polysiloxane aerogel of the present invention has the following advantages:
1, the present invention uses green solvent, prepares flexibility can cut and can weave super-hydrophobic silicon aerogel material by simple single stage method in supercritical co.
2, the silica aerogel of gained of the present invention has high flexibility and superelevation hydrophobicity, can carry out cutting and weave processing again, meets the application demands such as different shapes, different condition and different requirements.
3, production cost of the present invention is low, and the simple environmental protection of production process, is easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the polysiloxane aerogel prepared in embodiment 1.
Fig. 2 is the transmission electron microscope photo of the polysiloxane aerogel prepared in embodiment 1.
Fig. 3 is that the polysiloxane aerogel for preparing in embodiment 1 is to the contact angle of water.
Fig. 4 is the mechanical experimental results of polysiloxane aerogel, wherein the uniaxial compression curve of polysiloxane aerogel of Fig. 4 a) for preparing in embodiment 1 and embodiment 4; Fig. 4 b) ~ Fig. 4 d) for the polysiloxane aerogel for preparing in embodiment 1 at different temperatures uniaxial cycling compress the stress-strain curve of 100 times, Fig. 4 b): room temperature, Fig. 4 c): 150 DEG C, Fig. 4 d) :-50 DEG C.
Fig. 5 is the photo of the polysiloxane aerogel prepared in embodiment 1.
Fig. 6 is cutting and the stitching figure of the polysiloxane aerogel prepared in embodiment 1, and wherein, Fig. 6 (a) is cutting drawing, and Fig. 6 (b) is for sewing up figure.
Embodiment
The experimental technique used in following embodiment if no special instructions, is ordinary method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The preparation of embodiment 1, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 1.80g, the molecular weight of 5.12g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) join in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in Supercritical Conditions, react and release CO after 4 hours
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
As depicted in figs. 1 and 2, scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared for aforesaid method and transmission electron microscope (TEM) photo, as seen from the figure, this polysiloxane aerogel is loose porous three-dimensional net structure, can find out that from SEM figure the aperture of hole is 8 μm, can find out that from TEM figure this aerogel also exists the hole that aperture is 30 ~ 180nm.
The preparation of embodiment 2, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 0.71g, the molecular weight of 4.06g is that the end-vinyl dimethyl polysiloxane of 5000-8000g/mol (molecular-weight average is 6000g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in Supercritical Conditions, react and release CO after 4 hours
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 1.0:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 3, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (its hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 0.80g, the molecular weight of 7.80g is that the end-vinyl dimethyl polysiloxane of 9000-13000g/mol (molecular-weight average is 10000g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in supercritical state, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 1.0:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 4, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.4wt%) of 4000-8000g/mol (molecular-weight average is 6000g/mol) by the molecular weight of 1.80g, the molecular weight of 10.24g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2900g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in supercritical state, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 1.0:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 5, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.4wt%) of 10000 ~ 15000g/mol (molecular-weight average is 12000g/mol) by the molecular weight of 0.62g, the molecular weight of 2.56g is that the end-vinyl dimethyl polysiloxane of 1500 ~ 3000g/mol (molecular-weight average is 2900g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in supercritical state, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 1.4:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 6, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 0.9g, the molecular weight of 2.56g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in supercritical state, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 7, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 1.80g, the molecular weight of 5.12g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.05% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) add in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 25MPa, simultaneously CO
2be in supercritical state, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 8, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 1.80g, the molecular weight of 5.12g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.01% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) join in 50mL reactor, CO at 40 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in Supercritical Conditions, after heat-insulation pressure keeping 24h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 9, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 1.80g, the molecular weight of 5.12g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.01% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) join in 50mL reactor, CO at 80 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in Supercritical Conditions, after heat-insulation pressure keeping 4h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The preparation of embodiment 10, polysiloxane aerogel
The preparation method of polysiloxane aerogel, comprises the steps:
Be the methyl hydrogen polysiloxane (hydrogen content is 0.2wt%) of 1500-3000g/mol (molecular-weight average is 1700g/mol) by the molecular weight of 1.80g, the molecular weight of 5.12g is that the end-vinyl dimethyl polysiloxane of 1500-3000g/mol (molecular-weight average is 2000g/mol) and Karstedt ' s catalyzer (quality is 0.1% of methyl hydrogen polysiloxane and end-vinyl dimethyl polysiloxane quality sum) join in 50mL reactor, CO at 60 DEG C
2be filled with and make the pressure of system reach 16MPa, simultaneously CO
2be in Supercritical Conditions, after heat-insulation pressure keeping 1h, release CO
2directly obtain Monolithic aerogel.
The ratio of the mole number of the vinyl in the present embodiment in methyl hydrogen polysiloxane in the mole number of Si-H and vinyl polysiloxane is 0.7:1.0.
Scanning electronic microscope (SEM) photo of the polysiloxane aerogel prepared in the present embodiment and transmission electron microscope (TEM) photo and Fig. 1 and Fig. 2 are without significant difference.
The performance test of the polysiloxane aerogel prepared in embodiment 1-10
(1) hydrophobicity test:
Contact angle visualizer is adopted to measure the contact angle of polysiloxane aerogel and the water prepared in embodiment 1, result as shown in Figure 3, its contact angle is 152 °, the contact angle of the polysiloxane aerogel obtained in other embodiment and Fig. 1, without obvious difference, show that the polysiloxane aerosol that the inventive method prepares has good hydrophobicity.
(2) Mechanics Performance Testing:
Fig. 4 is the mechanical experimental results of polysiloxane aerogel, the wherein uniaxial compression curve of polysiloxane aerogel of Fig. 4 a) for preparing in embodiment 1 and embodiment 4, as seen from the figure, the flexibility of the polysiloxane aerogel that the present invention prepares is good, wherein, in uniaxial compression curve, the Young's modulus of embodiment 4 is higher than the Young's modulus of embodiment 1, the aerogel of the aerogel of embodiment 1 relatively embodiment 4 wants soft, this is because the cross-linking density of the polysiloxane prepared in embodiment 1 is lower than the cross-linking density of the polysiloxane prepared in embodiment 4.
Fig. 4 b) ~ Fig. 4 d) for the polysiloxane aerogel for preparing in embodiment 1 at different temperatures uniaxial cycling compress the stress-strain curve of 100 times, wherein, Fig. 4 b) be room temperature, Fig. 4 c) be 150 degree, Fig. 4 d) be-50 degree, as can be seen from this figure, the polysiloxane aerogel that the present invention prepares has good resistance against compression in wide temperature range, this is because the main chain of aerogel that the present invention prepares is flexible high, good heat resistance, low temperature resistant O-Si-O chain, and this aerogel-like has three-dimensional net structure.
Fig. 5 is the photo of the polysiloxane aerogel prepared in embodiment 1, from this figure, the polysiloxane aerogel obtained in other embodiment and Fig. 5, without significant difference, also can find out that the polysiloxane aerosol that the present invention prepares has excellent flexibility.
(3) can cutting and stitchability:
Any one flexible air gelatinous material prepared in embodiment 1 all can carry out arbitrary shape and cut out, cuts and sew up, and as shown in Figure 6, Fig. 6 (a) is cutting drawing, and Fig. 6 (b) is for sewing up figure.
(4) heat-proof quality test:
Test the heat-proof quality of the polysiloxane aerogel prepared in embodiment 1-10 respectively, result is as follows:
The heat-proof quality test result of the polysiloxane aerogel prepared in table 1 embodiment 1-10
| Sample | Thermal conductivity W/ (mK) |
| 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, the polysiloxane aerogel utilizing the inventive method to prepare has superinsulation performance.
Claims (8)
1. a preparation method for polysiloxane aerogel, comprises the steps:
In supercutical fluid, under catalyzer existent condition, hydrogen containing siloxane and vinyl polysiloxane can obtain described polysiloxane aerogel through crosslinking reaction.
2. preparation method according to claim 1, is characterized in that: described supercutical fluid is any one in supercritical carbon dioxide fluid, supercritical methane fluid and overcritical nitrogen peroxide fluid.
3. preparation method according to claim 1 and 2, is characterized in that: the add-on of described catalyzer is 0.01% ~ 1.0% of the quality sum of described hydrogen containing siloxane and described vinyl polysiloxane;
Described catalyzer is catalyst made from platonic, and described catalyst made from platonic is Karstedt ' s catalyzer or Platinic chloride.
4. the preparation method according to any one of claim 1-3, is characterized in that: in described hydrogen containing siloxane, the ratio of the mole number of Si-H and the mole number of described vinyl polysiloxane medium vinyl is 1.4 ~ 0.7:1.0;
In described hydrogen containing siloxane, the mole number of hydrogen atom is 0.1% ~ 1.4% of the mole number of described hydrogen containing siloxane, and molecular weight is 1000 ~ 15000g/mol;
The molecular weight of described vinyl polysiloxane is 1000 ~ 20000g/mol.
5. the preparation method according to any one of claim 1-4, is characterized in that: the temperature of described crosslinking reaction is 40 ~ 120 DEG C, and pressure is 7MPa ~ 60MPa;
The time of described crosslinking reaction is 1 ~ 24h.
6. preparation method according to claim 5, it is characterized in that: when described supercutical fluid is supercritical carbon dioxide fluid, described supercritical carbon dioxide fluid, by being filled with after in reactor by carbonic acid gas, obtains at described temperature and described pressure.
7. the polysiloxane aerogel that the preparation method according to any one of claim 1-6 prepares.
8. polysiloxane aerogel according to claim 7, is characterized in that: described polysiloxane aerogel obtains after cutting, cutting or braiding.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107922738A (en) * | 2015-09-01 | 2018-04-17 | 日立化成株式会社 | Sol composition and aeroge |
| CN110437496A (en) * | 2019-07-19 | 2019-11-12 | 淮阴工学院 | A kind of polysiloxanes aerogel composite and its preparation method and application for high-efficiency water evaporating |
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 |
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| CN106242610A (en) * | 2016-08-17 | 2016-12-21 | 哈尔滨工业大学 | A kind of preparation method of SiOC ceramic aerogel |
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| CN110437496A (en) * | 2019-07-19 | 2019-11-12 | 淮阴工学院 | A kind of polysiloxanes aerogel composite and its preparation method and application for high-efficiency water evaporating |
| 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 |
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