CN110452480B - Preparation method of ultra-light heat-insulating flexible aerogel - Google Patents
Preparation method of ultra-light heat-insulating flexible aerogel Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08J2203/06—CO2, N2 or noble gases
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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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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C08K3/20—Oxides; Hydroxides
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Abstract
The invention discloses a preparation method of ultra-light heat-insulating flexible aerogel, which comprises the steps of taking fluororubber as a raw material, dissolving the fluororubber in an organic solvent to form sol, adding a filler and a vulcanization system into the sol to crosslink the fluororubber sol, gradually changing the sol into gel after the sol is crosslinked to obtain fluororubber wet gel, putting the wet gel into a reaction kettle, introducing supercritical gas, and performing supercritical drying and foaming to obtain the fluororubber aerogel material. According to the invention, the fluororubber material is crosslinked in the solvent for the first time, and the gel material is subjected to supercritical drying and foaming, so that the prepared fluororubber aerogel material has extremely low density and heat conductivity coefficient and has good flexibility.
Description
Technical Field
The invention relates to an aerogel material, in particular to an organic polymer aerogel material, and belongs to the technical field of new materials.
Background
Aerogel is a novel nanoscale porous material, and is mainly prepared from molecular precursors by a sol-gel method, and then a solvent used in the process of removing sol from wet gel by a drying (freezing or supercritical) technology, wherein the interior of the material is filled with air, and the microstructure can be observed by using a scanning electron microscope, so that the material has a porous nano structure, a very high surface area, adjustable porosity and a large pore volume. Earlier, the understanding of aerogel definition was also limited to one material of three-dimensional network structure prepared by supercritical drying. With the continued intensive research by researchers, it is considered that as long as the liquid dispersion is changed to a solid dispersion, the aerogel can be formed with a three-dimensional network structure. At present, graphene aerogel mainly exists according to different matrixes, and can be used in various functional material fields; organic aerogel, the precursor is resorcinol-formaldehyde; inorganic aerogels, mainly silica aerogel and metal oxide aerogel. Aerogels have many excellent properties due to their special structure, such as high specific surface area, high porosity, low density, high insulation value, ultra low dielectric constant, low refractive index, etc. These excellent properties enable the aerogel to be used in many high-end applications, such as in the laser field, aerospace, thermal insulation, energy storage devices, and the like. However, the high porosity and low solid content of the aerogel generally make the mechanical properties of the aerogel worse, the aerogel is easy to crush and not easy to bend, which has great influence on the processing and application of the aerogel, so that many researchers focus on the development and preparation of the ultra-light flexible aerogel.
Disclosure of Invention
The invention develops a preparation method of ultra-light heat-insulating flexible aerogel, which takes fluororubber as a raw material, adds solvent to dissolve the fluororubber to form sol, then adds filler and bisphenol vulcanization system, continuously stirs the sol to a wet gel state, puts the wet gel into a reaction kettle, and lets in gas to reach a supercritical state, after saturation for a certain period, slowly releases pressure to complete the processes of supercritical drying and supercritical foaming, thus obtaining the fluororubber-based aerogel material.
In order to achieve the above object, the present invention is achieved by the following technical scheme. Wherein, the mass ratio of each raw material is as follows: 100 parts of fluororubber, 1-2.5 parts of vulcanizing agent bisphenol AF, 0.4-1.6 parts of accelerator BPP, 3-10 parts of acid absorber, 6-20 parts of calcium hydroxide, 0.1-20 parts of filler and 600-1200 parts of solvent.
The method comprises the following specific steps:
(1) Preparation of fluororubber wet gel
Firstly, taking a beaker to dissolve fluororubber in ethyl acetate to form uniform sol, adding a vulcanizing agent and an accelerator into the sol, and continuing stirring for 1h and then performing ultrasonic dispersion for 1h; taking another beaker, filling an organic solvent, adding filler, magnesium oxide and calcium hydroxide into the beaker, carrying out ultrasonic dispersion uniformly, pouring dispersion liquid containing the filler, the magnesium oxide and the calcium hydroxide into fluororubber sol, continuously stirring uniformly, and standing to form fluororubber wet gel.
(2) Preparation of fluororubber aerogel
Cutting out the prepared fluororubber wet gel to a certain size, putting the fluororubber wet gel into a supercritical reaction kettle, heating the reaction kettle, introducing gas for pressurizing, preserving heat and pressure, discharging gas in the kettle, opening the reaction kettle to obtain fluororubber aerogel material, and standing for 24 hours at normal temperature to perform performance test.
Wherein the vulcanizing agent is any one of bisphenol AF vulcanizing agent or peroxide vulcanizing agent.
Wherein the accelerator is any one of benzyl triphenyl phosphorus chloride (BPP) or triallyl isocyanurate (TAIC).
Wherein the solvent is one or more of ethyl acetate, dimethylformamide, toluene and chloroform.
Wherein the filler is SiO 2 Any one of aerogel, graphene, carbon nanotubes, carbon fibers, metal fibers.
Wherein the gas introduced into the supercritical reaction kettle is N 2 Or CO 2 Any of the above.
Wherein, the technological parameters of the supercritical drying and foaming process are as follows: the temperature of the supercritical reaction kettle is 20-80 ℃, the saturation time is 2-8h, the saturation pressure is 8-25Mpa, and the pressure relief time is 1-15 s.
The invention has the beneficial effects that the fluororubber aerogel is prepared for the first time, and the prepared rubber-based ultra-light and soft aerogel material solves the problems of easy crushing, powder falling and the like in the folding and bending processes of the traditional inorganic aerogel composite material, and the product has excellent flexibility and elasticity, and simultaneously has the performances of ultra-light, heat insulation, temperature resistance and the like.
Drawings
FIG. 1 is a schematic diagram of the flow chart of the preparation of the wet fluororubber gel of the present invention.
FIG. 2 shows the aerogel of example 1 in a state supported by young leaves of plants in the preparation method of the present invention.
FIG. 3 is a scanning electron micrograph of an aerogel cell of example 2 in a method of making the invention.
FIG. 4 shows the aerogel of example 2 in a core supported state in the preparation method of the present invention.
FIG. 5 is a flexible view of an aerogel of example 2 in the method of making the invention.
FIG. 6 is a graph showing the variation in cell size of aerogels of examples 2 to 6 in the production process of the present invention.
FIG. 7 shows the density change pattern of the aerogels of examples 2 to 6 in the production process of the present invention.
FIG. 8 is a graph showing the compression properties of the aerogels of examples 2 to 6 in the production process of the present invention.
FIG. 9 shows the thermal conductivity of aerogels of examples 2 to 6 according to the process of the present invention.
The specific embodiment is as follows:
the invention is further illustrated by the following examples:
example 1
The formula comprises the following components: 100 parts of fluororubber, 1.5 parts of bisphenol AF, 0.6 part of accelerator BPP, 6 parts of magnesium oxide, 12 parts of calcium hydroxide and SiO 2 Aerogel powder 4 parts, ethyl acetate 800 parts.
The process comprises the following steps: adding fluororubber into 600 parts of organic solvent, mechanically stirring until the fluororubber is completely dissolved, adding bisphenol AF and BPP into the sol, continuously stirring for 1h, and then performing ultrasonic dispersion for 1h; magnesium oxide, calcium hydroxide and SiO 2 Adding aerogel powder into 200 parts of ethyl acetate, mechanically stirring for 1h, performing ultrasonic dispersion for 1h, adding the dispersed suspension into fluororubber sol, placing in an environment with the temperature not higher than 5 ℃ for continuous stirring for 1h, performing ultrasonic dispersion for 1h, placing the mixed solution in an environment with the temperature of 25-35 ℃ to enable the mixed solution to start to perform a crosslinking reaction to form gel, standing for 6h, and waiting for the gel to completely form fluororubber wet gel; cutting the wet gel, placing into supercritical reaction kettle, setting the temperature of the reaction kettle to 50deg.C, introducing nitrogen, pressurizing to 16MPa, and maintaining the stripDecompression after 4h, opening the reaction kettle, taking out the material, placing the material in the air, and standing for 24h to obtain the fluororubber aerogel material, wherein the density of the fluororubber aerogel material is 9mg/cm 3 The cell size was 800um; the thermal conductivity was 0.015W/mK, and the stress at a compression ratio of 0.7 was about 48kPa.
Example 2-example 6
The process comprises the following steps: adding fluororubber into ethyl acetate, mechanically stirring until the fluororubber is dissolved to form sol, adding bisphenol AF and BPP into the sol, continuously stirring for 1h, and then performing ultrasonic dispersion for 1h; adding magnesium oxide, calcium hydroxide and graphene into DMF in another beaker, mechanically stirring for 1h, performing ultrasonic dispersion for 1h to enable the graphene to be completely dispersed, adding a dispersed DMF filler suspension into ethyl acetate sol containing fluororubber, placing the mixture in an environment with the temperature not exceeding 5 ℃ to continuously stir for 1h, performing ultrasonic dispersion for 1h, repeating the operation for 3 times, then placing the mixed solution in the environment with the temperature of 25-35 ℃ to slowly stir at the rotating speed of 150r/min, observing that the mixed solution is stopped to stir after gel starts, standing for 6h, and waiting for the gel to completely form fluororubber wet gel; placing the fluororubber wet gel in a supercritical foaming reaction kettle, introducing nitrogen, setting the temperature of the reaction kettle to 60 ℃, pressurizing to 18MPa, maintaining the condition for 4 hours, then decompressing for 2 seconds, taking out the material, placing the material in the air, standing for 24 hours, and obtaining fluororubber aerogel materials, and carrying out various tests.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the foregoing embodiments have been described in detail for the purpose of illustration, those skilled in the art may still make modifications to the technical solutions of the foregoing embodiments or make equivalent substitutions of some of the technical features thereof; such modifications and substitutions do not depart from the spirit of the invention.
Claims (5)
1. The preparation method of the ultra-light heat-insulating flexible aerogel is characterized by comprising 100 parts of fluororubber, 1-2.5 parts of vulcanizing agent, 0.2-1.6 parts of accelerator, 3-20 parts of magnesium oxide, 5-40 parts of calcium hydroxide, 0.1-30 parts of filler and 600-1200 parts of solvent; the vulcanizing agent is bisphenol AF, the accelerator is benzyl triphenyl phosphorus chloride (BPP), and the specific preparation steps are as follows:
(1) Preparation of fluororubber wet gel
Firstly, taking a beaker to dissolve fluororubber in ethyl acetate to form uniform sol, adding a vulcanizing agent and an accelerator into the sol, and continuing stirring for 1h and then performing ultrasonic dispersion for 1h; taking another beaker, filling an organic solvent, adding filler, magnesium oxide and calcium hydroxide into the beaker, carrying out ultrasonic dispersion uniformly, pouring dispersion liquid containing the filler, the magnesium oxide and the calcium hydroxide into fluororubber sol, continuously stirring uniformly, and standing to form fluororubber wet gel;
(2) Preparation of fluororubber aerogel
Cutting out the prepared fluororubber wet gel to a certain size, putting the fluororubber wet gel into a supercritical reaction kettle, heating the reaction kettle, introducing gas for pressurizing, preserving heat and pressure, discharging gas in the kettle, and opening the reaction kettle to obtain the ultra-light and heat-insulating fluororubber aerogel material.
2. The method for preparing the ultra-light heat-insulating flexible aerogel according to claim 1, wherein the solvent is one or a mixture of more of ethyl acetate, dimethylformamide, toluene and chloroform.
3. The method for preparing ultra-light adiabatic flexible aerogel according to claim 1, wherein said filler is SiO 2 Any one of aerogel, graphene, carbon nanotubes, carbon fibers, metal fibers.
4. The method for preparing ultra-light adiabatic flexible aerogel according to claim 1, wherein the gas introduced into said supercritical reaction vessel is N 2 Or CO 2 Any of the above.
5. The method for preparing the ultra-light heat-insulating flexible aerogel according to claim 1, wherein the process parameters of the supercritical drying and foaming process are as follows: the temperature of the supercritical reaction kettle is 20-80 ℃, the saturation time is 2-8h, the saturation pressure is 8-25MPa, and the pressure relief time is 1-15 s.
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| CN105536655A (en) * | 2015-12-11 | 2016-05-04 | 中国科学院兰州化学物理研究所 | Rapid preparation method for aerogel material |
| JP2016074841A (en) * | 2014-10-08 | 2016-05-12 | 株式会社イノアックコーポレーション | Flexible aerogel composite and production process therefor |
| CN108047485A (en) * | 2017-12-13 | 2018-05-18 | 西华大学 | A kind of aerogel material and preparation method thereof |
| CN108192129A (en) * | 2017-11-30 | 2018-06-22 | 南京工业大学 | A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof |
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| US20100160472A1 (en) * | 2005-11-28 | 2010-06-24 | Aspen Aerogels, Inc. | Polyolefin aerogels and composites |
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| JP2016074841A (en) * | 2014-10-08 | 2016-05-12 | 株式会社イノアックコーポレーション | Flexible aerogel composite and production process therefor |
| CN105536655A (en) * | 2015-12-11 | 2016-05-04 | 中国科学院兰州化学物理研究所 | Rapid preparation method for aerogel material |
| CN108192129A (en) * | 2017-11-30 | 2018-06-22 | 南京工业大学 | A kind of ultra-hydrophobic polyvinylidene fluoride aerogel material and preparation method thereof |
| CN108047485A (en) * | 2017-12-13 | 2018-05-18 | 西华大学 | A kind of aerogel material and preparation method thereof |
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