CN109721760A - Preparation method of polymer aerogel - Google Patents
Preparation method of polymer aerogel Download PDFInfo
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- CN109721760A CN109721760A CN201811608427.4A CN201811608427A CN109721760A CN 109721760 A CN109721760 A CN 109721760A CN 201811608427 A CN201811608427 A CN 201811608427A CN 109721760 A CN109721760 A CN 109721760A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920000642 polymer Polymers 0.000 title claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 11
- 230000001112 coagulating effect Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004814 polyurethane Substances 0.000 claims description 9
- 229920002635 polyurethane Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004800 polyvinyl chloride Substances 0.000 claims description 5
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012779 reinforcing material Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 2
- 229940113088 dimethylacetamide Drugs 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 1
- 239000001569 carbon dioxide Substances 0.000 claims 1
- MJEMIOXXNCZZFK-UHFFFAOYSA-N ethylone Chemical compound CCNC(C)C(=O)C1=CC=C2OCOC2=C1 MJEMIOXXNCZZFK-UHFFFAOYSA-N 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- 238000009413 insulation Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 3
- 238000001879 gelation Methods 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention belongs to the field of new material preparation, and relates to a preparation method of polymer aerogel. The method adopts high molecular powder as a precursor, firstly prepares a high molecular solution, then immerses a high molecular liquid film in a coagulating bath for gelation, and finally dries the gel to obtain the polymer aerogel. The polymer aerogel prepared by the invention has good flexibility, and can be used in the fields of heat insulation and preservation, water treatment, gas separation and the like in a low-temperature humid environment.
Description
Technical field
The invention belongs to the preparation fields of new material, and in particular to a kind of preparation method of polymeric aerogels.
Background technique
Aeroge has three-D nano-porous network structure, assigns the spies such as its low-density, high-specific surface area, macroporosity
Property, heat-insulation and heat-preservation, absorption, catalyst and in terms of show excellent properties.Silica aerogel has realized commercialization
And industrialization, but silica aerogel intensity is low, does not tolerate to water and organic solvent.High molecular material has good flexibility
And solvent tolerance, also there is good solvent tolerance and flexibility using polymeric aerogels prepared by polymeric powder.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of polymeric aerogels, can be prepared using this method flexible
Polymeric aerogels material of good performance, and the thickness of polymeric aerogels is adjustable.
The technical solution of the present invention is as follows: a kind of preparation method of polymeric aerogels, the specific steps of which are as follows:
(1) reinforcing material that addition mass fraction is 0~10% in organic solvent, dispersion 10~after sixty minutes, it is added
The polymeric powder for being 5~15% relative to organic solvent mass fraction, then stirs to get Polymer Solution, and macromolecule is molten
Liquid is stood；
(2) Polymer Solution after standing is scraped to 100~2000 microns of thickness of liquid film in substrate surface, it is then quiet
It sets, then immerses substrate in coagulating bath 1~30 minute, liquid film forming gel；
(3) then the soak described in is dried to obtain polymeric aerogels 1~3 day in Ageing solution.
Organic solvent described in preferred steps (1) is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N- methyl
One of pyrrolidones or dimethyl sulfoxide.
Reinforcing material described in preferred steps (1) is graphene, carbon nanotube, chopped strand, whisker or attapulgite
One of.
Preferred steps are separated into one of mechanical dispersion or ultrasonic disperse described in (1).
Polymeric powder described in preferred steps (1) is one of Kynoar, polyvinyl chloride or polyurethane.
Stirring described in preferred steps (1) is to stir 1~10 hour at 60~120 DEG C of 200~600r/min of revolving speed.
Standing described in preferred steps (1) is to stand 2~24 hours at 20~60 DEG C.
Standing described in preferred steps (2) is to stand 10~120 seconds at 0~60 DEG C.
Ageing solution described in preferred steps (3) is one of ethyl alcohol, methanol or water
Drying described in preferred steps (3) is that dry CO 2 supercritical, freeze-drying, constant pressure and dry or vacuum are dry
It is one of dry.
The utility model has the advantages that
Polymeric aerogels preparation method provided by the present invention is simple and environmentally-friendly, does not need using any acid or base catalysis
Agent, prepared polymeric aerogels are good to water and organic solvent tolerance, have preferable flexibility, can be used for Shui Chu
The fields such as reason, the heat-insulation and heat-preservation under low temperature environment, special dress clothes.
Detailed description of the invention
Fig. 1 is the photo in kind of polymeric aerogels made from example 1.
Specific embodiment
Example 1
The Kynoar powder that mass fraction is 5%, 120 DEG C of revolving speed 300r/min are added in n,N-Dimethylformamide
Lower stirring obtains Kynoar solution for 1 hour, and Kynoar solution scrapes after standing 24 hours at 20 DEG C in planar surface
The liquid film that 2000 microns of thickness after 0 DEG C stands 120 seconds, at room temperature immerses plate in coagulating bath 30 minutes, the liquid film on plate
Gel is formed, CO 2 supercritical is dried to obtain specific surface area 202m after gel impregnates 3 days in ethanol2/ g, thermal conductivity
The Kynoar aeroge of 0.034W/ (mK).Fig. 1 is the sample photo of Kynoar aeroge made from example 1.Institute
The polymeric aerogels of preparation are flaky material, and bendable is but, and flexibility is good.
Spectrophotometer method measures polymeric aerogels to heavy metal ion Cu in 1g/L heavy metallic salt solution2+、Ni2+With
Cr3+Adsorbance is respectively 220,109 and 69mg/g.
Example 2
Attapulgite of the addition relative to solvent quality score 10% in n,N-dimethylacetamide, mechanical dispersion 60 minutes
The polyvinyl chloride powder for being 15% relative to solvent quality score is added afterwards, after being stirred 3 hours under 100 DEG C of revolving speed 400r/min
To polyvinyl chloride solution, polyvinyl chloride solution in planar surface scrapes 1000 microns of thickness of liquid after standing 12 hours at 40 DEG C
Film after 20 DEG C stand 60 seconds, at room temperature immerses plate in coagulating bath 20 minutes, the liquid film forming gel on plate, gel exists
Constant pressure and dry obtains specific surface area 26m after impregnating 2 days in methanol2The polychlorostyrene second of the bendable of/g, thermal conductivity 0.036W/ (mK) but
Alkene aeroge.Spectrophotometer method measures polymeric aerogels to heavy metal ion Cu in 1g/L heavy metallic salt solution2+、Ni2+With
Cr3+Adsorbance is respectively 98,59 and 37mg/g.
Example 3
The whisker that mass fraction is 5% is added in N-Methyl pyrrolidone, mechanical dispersion is added after sixty minutes relative to molten
The polyurethane powder that agent mass fraction is 10% obtains polyurethane solutions, poly- ammonia after stirring 5 hours under 80 DEG C of revolving speed 200r/min
Ester solution in planar surface scrapes 500 microns of thickness of liquid film after standing 2 hours at 60 DEG C, after 40 DEG C stand 30 seconds, at room temperature
Plate is immersed in coagulating bath 10 minutes, the liquid film forming gel on plate, gel is freeze-dried after impregnating in water 3 days and obtains
Specific surface area 80m2The polyurethane aeroge of the bendable of/g, thermal conductivity 0.030W/ (mK) but.Spectrophotometer method measures polymerization
Object aeroge is to heavy metal ion Cu in 1g/L heavy metallic salt solution2+、Ni2+And Cr3+Adsorbance is respectively 186,101 and 64mg/
g。
Example 4
The carbon nanotube that mass fraction is 1% is added in dimethyl sulfoxide, and ultrasonic disperse is added after ten minutes relative to solvent
The polyurethane powder that mass fraction is 7% obtains polyurethane solutions, polyurethane after stirring 10 hours under 60 DEG C of revolving speed 600r/min
Solution in planar surface scrapes 100 microns of thickness of liquid film after standing 4 hours at 40 DEG C, after 60 DEG C stand 10 seconds, at room temperature will
Plate immerses in coagulating bath 5 minutes, and the liquid film forming gel on plate, gel is dried in vacuo after impregnating in ethanol 1 day and obtains
Specific surface area 67m2The polyurethane aeroge of the bendable of/g, thermal conductivity 0.033W/ (mK) but.Spectrophotometer method measures polymerization
Object aeroge is to heavy metal ion Cu in 1g/L heavy metallic salt solution2+、Ni2+And Cr3+Adsorbance is respectively 200,107 and 70mg/
g。
Example 5
The graphene that mass fraction is 0.1% is added in n,N-Dimethylformamide, is added after ultrasonic disperse 30 minutes opposite
The Kynoar powder for being 12% in solvent quality score obtains gathering inclined fluorine after stirring 3 hours under 90 DEG C of revolving speed 500r/min
Vinyl solution, Kynoar solution in planar surface scrape 1500 microns of thickness of liquid film after standing 16 hours at 20 DEG C, and 30
After DEG C standing 90 seconds, plate is immersed in coagulating bath 1 minute at room temperature, liquid film forming gel on plate, gel is in methyl alcohol
Constant pressure and dry obtains specific surface area 31m after impregnating 1 day2The Kynoar gas of the bendable of/g, thermal conductivity 0.034W/ (mK) but
Gel.Spectrophotometer method measures polymeric aerogels to heavy metal ion Cu in 1g/L heavy metallic salt solution2+、Ni2+And Cr3+
Adsorbance is respectively 97,63 and 48mg/g.
Claims (10)
1. a kind of preparation method of polymeric aerogels, the specific steps of which are as follows:
(1) reinforcing material that addition mass fraction is 0~10% in organic solvent, dispersion 10~after sixty minutes, it is added opposite
The polymeric powder for being 5~15% in organic solvent mass fraction, then stirs to get Polymer Solution, and Polymer Solution is quiet
It sets；
(2) liquid film that the Polymer Solution after standing is scraped to 100~2000 microns of thickness in substrate surface, is then allowed to stand, with
Substrate is immersed in coagulating bath 1~30 minute afterwards, liquid film forming gel；
(3) then the soak described in is dried to obtain polymeric aerogels 1~3 day in Ageing solution.
2. preparation method according to claim 1, it is characterised in that organic solvent described in step (1) is N, N- diformazan
One of base formamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone or dimethyl sulfoxide.
3. preparation method according to claim 1, it is characterised in that reinforcing material described in step (1) be graphene,
One of carbon nanotube, chopped strand, whisker or attapulgite.
4. preparation method according to claim 1, it is characterised in that be separated into mechanical dispersion or super described in step (1)
One of sound dispersion.
5. preparation method according to claim 1, it is characterised in that polymeric powder described in step (1) is to gather inclined fluorine
One of ethylene, polyvinyl chloride or polyurethane.
6. preparation method according to claim 1, it is characterised in that stirring described in step (1) is at 60~120 DEG C
It is stirred 1~10 hour under 200~600r/min of revolving speed.
7. preparation method according to claim 1, it is characterised in that standing described in step (1) is quiet at 20~60 DEG C
It sets 2~24 hours.
8. preparation method according to claim 1, it is characterised in that standing described in step (2) is quiet at 0~60 DEG C
It sets 10~120 seconds.
9. preparation method according to claim 1, it is characterised in that Ageing solution described in step (3) is ethyl alcohol, methanol
Or one of water
10. preparation method according to claim 1, it is characterised in that drying described in step (3) is super for carbon dioxide
One of critical drying, freeze-drying, constant pressure and dry or vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811608427.4A CN109721760A (en) | 2018-12-27 | 2018-12-27 | Preparation method of polymer aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811608427.4A CN109721760A (en) | 2018-12-27 | 2018-12-27 | Preparation method of polymer aerogel |
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| CN109721760A true CN109721760A (en) | 2019-05-07 |
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| CN201811608427.4A Pending CN109721760A (en) | 2018-12-27 | 2018-12-27 | Preparation method of polymer aerogel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024040690A1 (en) * | 2022-08-26 | 2024-02-29 | 电子科技大学长三角研究院(湖州) | Composite-aperture radiation refrigeration film with high mechanical properties, preparation method and use thereof |
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| CN103205015A (en) * | 2012-01-17 | 2013-07-17 | 中国科学院化学研究所 | Transparent and flexible cellulose aerogel and preparation method thereof |
| CN104117291A (en) * | 2014-07-21 | 2014-10-29 | 上海应用技术学院 | TiO2/C hybrid aerogel modified polyvinylidene fluoride membrane and preparation method thereof |
| CN104258745A (en) * | 2014-10-24 | 2015-01-07 | 南京水思环保科技有限公司 | Preparation method of hydrophilic polyethersulfone microfiltration membrane |
| CN105017555A (en) * | 2014-04-29 | 2015-11-04 | 中国科学院化学研究所 | Cellulose aerogel and preparation method for hybrid aerogel thereof |
| CN106636055A (en) * | 2016-12-09 | 2017-05-10 | 福建农林大学 | Preparation method and application of cellulose-SiO2 composite carrier |
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2018
- 2018-12-27 CN CN201811608427.4A patent/CN109721760A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205015A (en) * | 2012-01-17 | 2013-07-17 | 中国科学院化学研究所 | Transparent and flexible cellulose aerogel and preparation method thereof |
| CN105017555A (en) * | 2014-04-29 | 2015-11-04 | 中国科学院化学研究所 | Cellulose aerogel and preparation method for hybrid aerogel thereof |
| CN104117291A (en) * | 2014-07-21 | 2014-10-29 | 上海应用技术学院 | TiO2/C hybrid aerogel modified polyvinylidene fluoride membrane and preparation method thereof |
| CN104258745A (en) * | 2014-10-24 | 2015-01-07 | 南京水思环保科技有限公司 | Preparation method of hydrophilic polyethersulfone microfiltration membrane |
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| Title |
|---|
| STEFANO CARDEA ET AL.: ""Comparative study of PVDF-HFP-curcumin porous structures produced by supercritical assisted processes"", 《THE JOURNAL OF SUPERCRITICAL FLUIDS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024040690A1 (en) * | 2022-08-26 | 2024-02-29 | 电子科技大学长三角研究院(湖州) | Composite-aperture radiation refrigeration film with high mechanical properties, preparation method and use thereof |
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Application publication date: 20190507 |