CN113980342B - Organosilicon polymer shape memory aerogel and preparation method thereof - Google Patents
Organosilicon polymer shape memory aerogel and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/04—Polythioethers from mercapto compounds or metallic derivatives thereof
- C08G75/045—Polythioethers from mercapto compounds or metallic derivatives thereof from mercapto compounds and unsaturated compounds
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- C—CHEMISTRY; METALLURGY
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- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
Abstract
The invention provides a preparation method of an organic silicon polymer shape memory aerogel, which adopts a sol-gel method, namely, a click reaction of a multi-sulfhydryl compound and an alkenyl-containing silicon compound quickly forms multi-siloxane micromolecules, then the multi-siloxane micromolecules are hydrolyzed and polymerized to form a cross-linked three-dimensional network structure under the action of a catalyst, and then the shape memory aerogel is obtained through supercritical drying. Compared with the prior art, the aerogel prepared by the method provided by the invention has the advantages of high porosity, high shape recovery rate, good fatigue resistance, adjustable deformation temperature and the like. The invention also provides the organosilicon polymer shape memory aerogel.
Description
Technical Field
The invention belongs to the technical field of aerogel, and particularly relates to an organic silicon polymer shape memory aerogel and a preparation method thereof.
Background
Aerogel is a nano porous material with a three-dimensional network structure, and since being discovered for the first time in 1931, the aerogel attracts people's attention due to the characteristics of high porosity, high specific surface area, low thermal conductivity coefficient and the like. Through the development of the last century, various types of aerogels have been prepared, and organic polymers, organic silicon aerogels and the like with different purposes are gradually developed from the initial inorganic oxide aerogels such as silicon oxide and the like. The organic silicon aerogel is formed by crosslinking organic silicon small molecules or polymers containing a plurality of reaction sites to form a three-dimensional network structure, and then the aerogel is formed. Due to the characteristics of excellent cold resistance, heat resistance, aging resistance and the like, the organic silicon aerogel gradually draws wide attention of researchers.
The thermotropic shape memory material is a solid material which can deform above room temperature, can be fixedly deformed at room temperature, can be stored for a long time, and can quickly restore the original shape of a workpiece when the temperature is raised to a certain specific response temperature. By endowing the aerogel material with the shape thermal memory effect, the intelligence and the diversity of the application of the aerogel can be improved, and a new direction is provided for the application of the aerogel. In order to expand the application range of the shape memory aerogel, the shape memory aerogel needs to be further modified, which is a problem to be solved in the field.
Disclosure of Invention
In view of the above, the invention aims to provide an organosilicon polymer shape memory aerogel, and the aerogel prepared by the method provided by the invention has the advantages of high porosity, high shape recovery rate, good fatigue resistance, adjustable deformation temperature and the like.
The invention provides a preparation method of an organic silicon polymer shape memory aerogel, which comprises the following steps:
reacting a multi-sulfhydryl compound, an alkenyl-containing silicon compound, benzoyl peroxide and N, N-dimethyl-p-toluidine in a solvent to obtain an aerogel precursor solution;
mixing the aerogel precursor solution, water and a catalyst, and then carrying out gel aging and solvent exchange to obtain wet gel;
and drying the wet gel to obtain the organic silicon polymer shape memory aerogel.
Preferably, the multi-mercapto compound is selected from one or more of pentaerythritol tetrakis (3-mercaptopropionate), tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate), trimethylolpropane-tris (3-mercaptopropionate), pentaerythritol tris (3-mercaptopropionate), and pentaerythritol bis (3-mercaptopropionate).
Preferably, the alkenyl-containing silicon compound is selected from one or more of vinyltrimethoxysilane, vinyltriethoxysilane, propenyl-trimethoxysilane, propenyl-triethoxysilane, vinyldimethylmethoxysilane, vinyldimethylethoxysilane, propenyl-dimethylmethoxysilane and propenyl-dimethylethoxysilane.
Preferably, the molar ratio of the multi-mercapto compound, the alkenyl-containing silicon compound, the N, N-dimethyl-p-toluidine and the benzoyl peroxide is 100:100: (3-10): (1-3).
Preferably, the solvent is one or more selected from acetonitrile, acetone, N-dimethylformamide, N-methylpyrrolidone, N-diethylformamide and dioxane.
Preferably, the catalyst is one or more selected from tetrabutylammonium hydroxide, tetramethylammonium hydroxide, ammonia water, hydrochloric acid, acetic acid and sulfuric acid.
Preferably, the solvent used in the solvent exchange process is selected from one of acetone, ethanol and acetonitrile.
Preferably, the time for the solvent exchange is 8 to 20 hours.
Preferably, the drying method is supercritical CO 2 And (5) drying.
The invention provides the organic silicon polymer shape memory aerogel prepared by the method in the technical scheme.
The method rapidly prepares the polysilicone organic compound with a plurality of cross-linking points through the click reaction of the polymercapto compound and the alkenyl-containing silicon compound, prepares the organic silicon polymer elastic wet gel through the hydrolytic polymerization of siloxane by adopting a sol-gel method, and prepares the shape memory aerogel under the condition of supercritical carbon dioxide. Compared with the traditional preparation method, the preparation method of the shape memory aerogel prepared by the invention mainly has the following advantages: the branching degree and the crosslinking degree of the hyperbranched organic silicon polymer are regulated and controlled by utilizing the number of reaction sites of different mercapto compounds and the number of alkoxy groups containing alkenyl siloxane, so that the fine and free regulation and control of the deformation temperature are realized; compared with the common organic polymer aerogel, the shape memory aerogel with the special silicon-containing compound as the precursor can effectively enhance the temperature adaptability, improve the cold resistance and the heat resistance and enhance the fatigue resistance of the shape memory aerogel.
The experimental results show that: the shape memory aerogel prepared by the invention has the porosity of 75-90 percent and the density of 0.03-0.5 g/cm 3 The glass transition temperature is 20-80 ℃, the hydrophobic angle is 95-135 degrees, the shrinkage rate is 7.3-16.1 percent, and the initial decomposition temperature is above 220 ℃.
Drawings
FIG. 1 is a picture of the appearance of an aerogel prepared in example 1 of the present invention;
FIG. 2 is a photograph of water contact angle of aerogel prepared in example 1 of the present invention;
FIG. 3 is an SEM picture of an aerogel prepared in example 3 of the present invention;
FIG. 4 is a diagram of the shape memory recovery process of the aerogel prepared in example 4 of the present invention;
FIG. 5 is a thermogravimetric and DSC curves of an aerogel prepared according to example 4 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of an organic silicon polymer shape memory aerogel, which comprises the following steps:
reacting a multi-sulfhydryl compound, an alkenyl-containing silicon compound, benzoyl peroxide and N, N-dimethyl-p-toluidine in a solvent to obtain an aerogel precursor solution;
mixing the aerogel precursor solution, water and a catalyst, and then carrying out gel aging and solvent exchange to obtain wet gel;
and drying the wet gel to obtain the organic silicon polymer shape memory aerogel.
In the present invention, the polymercapto compound is preferably one or more selected from the group consisting of pentaerythritol tetrakis (3-mercaptopropionate), tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate), trimethylolpropane-tris (3-mercaptopropionate), pentaerythritol tris (3-mercaptopropionate), and pentaerythritol bis (3-mercaptopropionate), and more preferably one or two selected from the group consisting of pentaerythritol tetrakis (3-mercaptopropionate) and tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate).
In the present invention, the alkenyl-containing silicon compound is preferably one or more selected from vinyltrimethoxysilane, vinyltriethoxysilane, propenyltrimethoxysilane, propenyltriethoxysilane, vinyldimethylmethoxysilane, vinyldimethylethoxysilane, propenyldimethylmethoxysilane and propenyldimethylethoxysilane, and more preferably one or two selected from vinyltrimethoxysilane and vinyldimethylmethoxysilane.
In the present invention, the molar ratio of the polymercapto compound, the alkenyl-containing silicon compound, N-dimethyl-p-toluidine, and benzoyl peroxide is preferably 100:100: (3-10): (1 to 3), more preferably 100:100: (4-6): (1-2), most preferably 100:100:5:1.5.
in the present invention, the solvent is preferably one or more selected from acetonitrile, acetone, N-dimethylformamide, N-methylpyrrolidone, N-diethylformamide and dioxane, and more preferably one or two selected from acetonitrile and acetone.
In the present invention, the solvent is used in an amount of preferably 70 to 95%, more preferably 75 to 90%, most preferably 80 to 85% of the total mass of the polymercapto compound, the alkenyl group-containing silicon compound, benzoyl peroxide and N, N-dimethyl-p-toluidine.
In the present invention, the temperature of the reaction is preferably room temperature, more preferably 20 to 30 ℃, more preferably 22 to 28 ℃, and most preferably 24 to 26 ℃; the reaction time is preferably 1 to 6 hours, more preferably 2 to 5 hours, and most preferably 3 to 4 hours.
In the present invention, the preparation method of the aerogel precursor solution preferably includes:
dissolving a multi-sulfhydryl compound and an alkenyl-containing silicon compound in a solvent, adding benzoyl peroxide and N, N-dimethyl-p-toluidine, and reacting for 1-6 h to obtain an aerogel precursor solution.
In the present invention, the water is preferably deionized water.
In the present invention, the ratio of the molar amount of water to the molar amount of siloxane in the alkenyl-containing silicon compound is preferably 1: (0.8 to 1.2), more preferably 1:1.
in the present invention, the catalyst is preferably an acid-base catalyst, and more preferably one or more selected from tetrabutylammonium hydroxide, tetramethylammonium hydroxide, ammonia water, hydrochloric acid, acetic acid and sulfuric acid; more preferably one or two selected from tetrabutylammonium hydroxide and tetramethylammonium hydroxide.
In the present invention, the ratio of the molar amount of the catalyst to the molar amount of the siloxane in the alkenyl-containing silicon compound is preferably (0.1 to 5): 100, more preferably (0.5 to 4): 100, more preferably (1 to 3): 100, most preferably 2:100.
in the present invention, the mixing is preferably performed under stirring; the stirring time is preferably 15 to 25min, more preferably 18 to 22min, and most preferably 20min.
In the present invention, the temperature of the gel aging is preferably 25 to 55 ℃, more preferably 30 to 50 ℃, and most preferably 35 to 45 ℃; the gel is preferably aged for a period of 18 to 40 hours, more preferably 25 to 35 hours, and most preferably 30 hours.
In the present invention, the solvent used in the solvent exchange process is preferably one selected from the group consisting of acetone, ethanol and acetonitrile, and more preferably acetone; the solvent is preferably the same as the solvent used in the preparation of the aerogel precursor solution.
In the present invention, the time for the solvent exchange is preferably 8 to 20 hours, more preferably 9 to 18 hours, and most preferably 10 to 12 hours.
In the present invention, the preparation method of the wet gel preferably includes:
adding deionized water and an acid-base catalyst into the aerogel precursor solution, stirring for 20min, pouring the solution into a mold, and performing gel aging and solvent exchange to obtain wet gel with certain elasticity.
In the present invention, the drying is preferably supercritical CO 2 Drying, wherein the drying temperature is preferably 35-45 ℃, more preferably 38-42 ℃, and most preferably 40 ℃; the drying pressure is preferably 8.5-14.5 MPa, preferably 9-12 MPa, and most preferably 10-11 MPa; the drying time is preferably 12 to 72 hours, more preferably 20 to 60 hours, more preferably 20 to 50 hours, more preferably 20 to 40 hours, more preferably 20 to 30 hours, and most preferably 25 hours.
The invention provides the organosilicon polymer shape memory aerogel prepared by the method in the technical scheme; the aerogel preferably has a porosity of 75 to 90% and a density of 0.03 to 0.5g/cm 3 The glass transition temperature is preferably 20 to 80 ℃, the hydrophobic angle is preferably 95 to 135 ℃, and the shrinkage rate is preferably 7.3 to 16.1 percent.
According to the invention, a multi-silicon organic compound with a plurality of cross-linking points is rapidly prepared through the click reaction of a multi-sulfhydryl compound and an alkenyl-containing silicon compound, an organosilicon polymer elastic wet gel is prepared through the hydrolytic polymerization of siloxane by adopting a sol-gel method, and the shape memory aerogel is prepared by drying under the supercritical carbon dioxide condition. Compared with the traditional preparation method, the preparation method of the shape memory aerogel prepared by the invention mainly has the following advantages: the branching degree and the crosslinking degree of the hyperbranched organic silicon polymer are regulated and controlled by utilizing the number of reaction sites of different mercapto compounds and the number of alkoxy groups containing alkenyl siloxane, so that the fine and free regulation and control of the deformation temperature are realized; compared with the common organic polymer aerogel, the shape memory aerogel with the special silicon-containing compound as the precursor can effectively enhance the temperature adaptability, improve the cold resistance and the heat resistance and enhance the fatigue resistance of the shape memory aerogel.
Example 1
Dissolving pentaerythritol tetrakis (3-mercaptopropionate) (2.44g, 5.0mmol), vinyldimethylmethoxysilane (1.32g, 10mmol), vinyltrimethoxysilane (1.49g, 10mmol) and benzoyl peroxide (24.2mg, 0.1mmol) in 80mL of acetone, stirring at room temperature for 20min, adding N, N-dimethyl-p-toluidine (68mg, 0.5mmol), and reacting at room temperature for 1h to obtain an organic silicon precursor solution;
adding deionized water (360mg, 20mmol) and a tetramethylammonium hydroxide aqueous solution (25%, 50 mu L) into the precursor solution, and stirring at room temperature for 30 minutes to form a uniform mixed solution;
pouring the mixed solution into a polypropylene plastic box mold, placing into a sealing bag, sealing, gelling at 40 ℃ for 20h, and continuously aging for 12h to obtain elastic wet gel;
soaking the wet gel in acetone for 12h for solvent exchange, and washing away small molecular substances which cannot participate in the reaction;
and (3) drying the soaked gel by supercritical carbon dioxide, wherein the drying condition is that the pressure is kept at 9MPa for 28h at 40 ℃, so as to obtain the shape memory aerogel.
Testing the porosity of the shape memory aerogel prepared in the embodiment 1 of the invention by a mercury intrusion method; the density of the shape memory aerogel prepared in example 1 of the present invention was tested using the mass to volume ratio; testing the glass transition temperature of the shape memory aerogel prepared in example 1 of the invention by using a dynamic thermomechanical analyzer; testing the hydrophobic angle of the shape memory aerogel prepared in the embodiment 1 of the invention by using a contact angle analyzer; the volume ratio is adopted to test the shrinkage rate of the shape memory aerogel prepared in the embodiment 1 of the invention; the initial decomposition temperature of the shape memory aerogel prepared in example 1 of the present invention was measured using a thermogravimetric analyzer.
As a result of the examination, the shape memory aerogel prepared in example 1 of the present invention had a porosity of 91% and a density of 0.032g/cm 3 The glass transition temperature was 42 ℃, the hydrophobic angle was 109 °, the shrinkage was 16.1%, and the initial decomposition temperature was 220 ℃.
Fig. 1 is a picture of a shape memory aerogel prepared in example 1 of the present invention, and fig. 2 is a photograph of a water contact angle of the shape memory aerogel prepared in example 1 of the present invention, from fig. 1, it can be seen that the aerogel has better block integrity, and from fig. 2, the water contact angle of the aerogel is 109 °.
Example 2
Dissolving pentaerythritol tetrakis (3-mercaptopropionate) (2.44g, 5.0 mmol), vinyltrimethoxysilane (2.96g, 20mmol) and benzoyl peroxide (24.2mg, 0.1mmol) in 50mL of acetonitrile, stirring at room temperature for 20min, adding N, N-dimethyl-p-toluidine (68mg, 0.5 mmol), and reacting at room temperature for 1h to obtain an organic silicon precursor solution;
deionized water (1.08g, 60mmol) and tetrabutylammonium hydroxide aqueous solution (25%, 70 μ L) were added to the precursor solution, and stirred at room temperature for 30 minutes to form a uniform mixed solution;
pouring the mixed solution into a polypropylene plastic box mold, putting into a sealing bag, sealing, gelling at 50 ℃ for 9 hours, and continuously aging for 12 hours to obtain elastic wet gel;
soaking the wet gel in acetone for 12h for solvent exchange, and washing away small molecular substances which cannot participate in the reaction;
and (3) drying the soaked gel by supercritical carbon dioxide, wherein the drying condition is that the pressure is kept at 12MPa for 48h at 35 ℃, so as to obtain the shape memory aerogel.
When the shape memory aerogel prepared in example 2 of the present invention was measured according to the method of example 1 of the present invention, the porosity was 83%, and the density was 0.037g/cm 3 The glass transition temperature was 73 ℃, the hydrophobic angle was 97 °, the shrinkage was 14.3%, and the initial decomposition temperature was 330 ℃.
Example 3
Dissolving tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate) (2.62g, 10mmol), pentaerythritol tetrakis (3-mercaptopropionate) (488mg, 11mmol), vinyltrimethoxysilane (1.48g, 10mmol) and benzoyl peroxide (24.2mg, 0.1mmol) in 30mL of acetonitrile, stirring at room temperature for 20min, adding N, N-dimethyl-p-toluidine (68mg, 0.5mmol), and reacting at room temperature for 1.5h to obtain a silicone precursor solution;
deionized water (540 mg, 30mmol) and tetrabutylammonium hydroxide aqueous solution (25%, 20 μ L) were added to the above precursor solution, and stirred at room temperature for 30 minutes to form a uniform mixed solution;
pouring the mixed solution into a polypropylene plastic box mold, placing the polypropylene plastic box mold into a sealing bag, sealing, gelling at 55 ℃ for 6 hours, and continuously aging for 12 hours to obtain elastic wet gel;
soaking the wet gel in acetone for 12h for solvent exchange, and washing away small molecular substances which cannot participate in the reaction;
and (3) drying the soaked gel by supercritical carbon dioxide under the condition of keeping the pressure of 9MPa at 50 ℃ for 25h to obtain the shape memory aerogel.
According to the method of the embodiment 1, the shape memory aerogel prepared in the embodiment 3 of the invention is detected, and the detection result is that the porosity is85% and the density is 0.037g/cm 3 The glass transition temperature was 66 ℃, the hydrophobic angle was 99 °, the shrinkage was 8.6%, and the initial decomposition temperature was 330 ℃.
Fig. 3 is an SEM picture of the aerogel prepared in example 3 of the present invention, and it can be seen from fig. 3 that the aerogel is connected by the nano-spheres to form a pearl necklace structure, and then a porous secondary structure is formed, and the pores are uniformly dispersed.
Example 4
Dissolving tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate) (524mg, 2mmol), vinyltrimethoxysilane (4.44g, 30mmol) and benzoyl peroxide (121mg, 0.5 mmol) in 80mL of acetonitrile, stirring at room temperature for 20min, adding N, N-dimethyl-p-toluidine (136mg, 1mmol), and reacting at room temperature for 1h to obtain an organosilicon precursor solution;
deionized water (1.08g, 60mmol) and tetrabutylammonium hydroxide aqueous solution (25%, 80 μ L) were added to the precursor solution, and stirred at room temperature for 30 minutes to form a uniform mixed solution;
pouring the mixed solution into a polypropylene plastic box mold, placing the polypropylene plastic box mold into a sealing bag, sealing, gelling at 50 ℃ for 8 hours, and continuously aging for 12 hours to obtain elastic wet gel;
soaking the wet gel in acetone for 12h for solvent exchange, and washing away small molecular substances which cannot participate in the reaction;
and (3) drying the soaked gel by supercritical carbon dioxide, wherein the drying condition is that the pressure is kept at 11MPa for 38h at 42 ℃, so as to obtain the shape memory aerogel.
According to the method of the embodiment 1, the shape memory aerogel prepared in the embodiment 4 of the invention is detected, and the detection result shows that the porosity is 87%, and the density is 0.041g/cm 3 The glass transition temperature was 58 ℃, the hydrophobic angle was 105 °, the shrinkage was 8.6%, and the initial decomposition temperature was 350 ℃.
Fig. 4 is a picture of a shape memory recovery process of the aerogel prepared in example 4 of the present invention, and it can be seen from fig. 4 that the aerogel prepared in the present invention has a better shape memory effect.
Fig. 5 is thermogravimetric and DSC curves of the aerogel prepared in example 4 of the present invention, and as can be seen from fig. 5, the initial decomposition temperature of the aerogel prepared in example 4 is 350 ℃.
From the above examples, the preparation method of the silicone polymer shape memory aerogel provided by the invention comprises the following steps: dissolving a multi-sulfhydryl compound and an alkenyl-containing silicon compound in a solvent, adding benzoyl peroxide and N, N-dimethyl-p-toluidine, and reacting for 1-6 h to obtain an aerogel precursor solution; adding deionized water and an acid-base catalyst into the precursor solution, stirring for 20min, pouring the solution into a mold, performing a gel aging step and a solvent exchange step to obtain a wet gel with certain elasticity, and drying the wet gel to obtain the shape memory aerogel. The experimental results show that: the shape memory aerogel prepared by the invention has the porosity of 75-90 percent and the density of 0.03-0.5 g/cm 3 The glass transition temperature is 20-80 ℃, the hydrophobic angle is 95-135 degrees, and the shrinkage rate is 7.3-16.1 percent.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A method for preparing a silicone polymer shape memory aerogel, comprising:
reacting a multi-sulfhydryl compound, an alkenyl-containing silicon compound, benzoyl peroxide and N, N-dimethyl-p-toluidine in a solvent to obtain an aerogel precursor solution;
mixing the aerogel precursor solution, water and a catalyst, and then carrying out gel aging and solvent exchange to obtain wet gel;
drying the wet gel to obtain the organic silicon polymer shape memory aerogel;
the molar ratio of the multi-sulfhydryl compound, the alkenyl-containing silicon compound, the N, N-dimethyl-p-toluidine and the benzoyl peroxide is 100:100: (3-10): (1-3).
2. The method according to claim 1, wherein the multi-mercapto compound is selected from one or more of pentaerythritol tetrakis (3-mercaptopropionate), tris (2-hydroxyethyl) isocyanurate-tris (mercaptopropionate), trimethylolpropane-tris (3-mercaptopropionate), pentaerythritol tris (3-mercaptopropionate), and pentaerythritol bis (3-mercaptopropionate).
3. The method according to claim 1, wherein the alkenyl silicon-containing compound is one or more selected from the group consisting of vinyltrimethoxysilane, vinyltriethoxysilane, propenyltrimethoxysilane, propenyltriethoxysilane, vinyldimethylmethoxysilane, vinyldimethylethoxysilane, propenyldimethylmethoxysilane, and propenyldimethylethoxysilane.
4. The method according to claim 1, wherein the solvent is selected from one or more of acetonitrile, acetone, N-dimethylformamide, N-methylpyrrolidone, N-diethylformamide and dioxane.
5. The method of claim 1, wherein the catalyst is selected from one or more of tetrabutylammonium hydroxide, tetramethylammonium hydroxide, aqueous ammonia, hydrochloric acid, acetic acid, and sulfuric acid.
6. The method according to claim 1, wherein the solvent used in the solvent exchange process is selected from one of acetone, ethanol and acetonitrile.
7. The process according to claim 6, characterized in that the time of the solvent exchange is between 8 and 20h.
8. The method of claim 1, wherein the drying method is supercritical CO 2 And (5) drying.
9. A silicone polymer shape memory aerogel prepared by the method of claim 1.
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| RU2659077C1 (en) * | 2017-12-13 | 2018-06-28 | Федеральное государственное бюджетное учреждение науки Институт элементоорганических соединений им. А.Н. Несмеянова Российской академии наук (ИНЭОС РАН) | Method for producing flexible siloxane aerogels |
| CN111019519A (en) * | 2018-10-09 | 2020-04-17 | 上海产业技术研究院 | Crosslinkable composition, preparation method and application thereof |
| CN109796018A (en) * | 2019-01-29 | 2019-05-24 | 同济大学 | A kind of preparation method of elasticity double cross connection aeroge |
| WO2020247743A2 (en) * | 2019-06-06 | 2020-12-10 | Blueshift Materials, Inc. | Aerogels having a core-spoke polymeric matrix, methods of making, and uses thereof |
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