CN110372908A - A kind of insulation polyimide nano-fiber aeroge and preparation method thereof - Google Patents
A kind of insulation polyimide nano-fiber aeroge and preparation method thereof Download PDFInfo
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- CN110372908A CN110372908A CN201910585660.3A CN201910585660A CN110372908A CN 110372908 A CN110372908 A CN 110372908A CN 201910585660 A CN201910585660 A CN 201910585660A CN 110372908 A CN110372908 A CN 110372908A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J9/286—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 the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
Abstract
The present invention relates to a kind of insulation polyimide nano-fiber aeroge and preparation method thereof, the raw material components include polyamic acid nanofiber, water-soluble polyamic acid；Wherein polyamic acid nanofiber, water-soluble polyamic acid mass ratio be 1-5:1.Polyimide nano-fiber aeroge prepared by the present invention, has good compression resilience, and thermal coefficient is low, and still having good heat-insulating capability under high temperature, compression, excellent combination property, preparation process is simple to operation, it is environmentally protective, it can be used for a variety of heat-insulated scenes.
Description
Technical field
The invention belongs to heat preserving and insulating material and its preparation field, in particular to a kind of insulation polyimide nano is fine
Tie up aeroge and preparation method thereof.
Background technique
Aeroge is the continuous three-dimensional framework network structure being made of solia particle, and dispersed phase is the high dispersive of gas
Solid-state material.Have the characteristics that density is low, specific surface area is high, thermal conductivity is low, in aerospace, petrochemical industry, auto industry, builds
The fields such as heat preservation are built to hold out broad prospects.
Aeroge has ultralow thermal conductivity and excellent heat-proof quality.Therefore, aeroge building, automobile, aerospace,
There is good application prospect in many fields such as household electrical appliance, petrochemical factory and outdoor sports.However, needing in practical applications
Aeroge has the other performance in addition to low heat conductivity.For example, in space shuttle and space exploration field, it is desirable that aeroge tool
Standby high-intensitive and good toughness, to resist the impact of external environment.In building field, then require aeroge with higher strong
Certain load is spent and be able to bear, while to have hydrophobicity also to prevent material from getting wet, or even have shape memory function
It can be applied to small space.Outdoor sports, such as shoes and tent, it is desirable that aeroge has flexibility, elasticity and hydrophobicity, can
To restore from deformation, various weather conditions are adapted to.However, designing and manufacturing with ultralow thermal conductivity, strong mechanical performance and Zhuo
The aeroge of more shape memory function is still a huge challenge.
Polyimides (Polyimide) is that a kind of have good moulding processability, high mechanical strength, thermal stability good etc. excellent
The special engineering plastics of point, are widely used in the every field of national economy.The present invention passes through the skills such as electrostatic spinning, freeze-drying
Art prepares polyimide nano-fiber aeroge, on the one hand, the polyimide nano-fiber prepared by electrostatic spinning is as gas
The basis material of gel, itself just possesses good mechanics and heat-proof quality；On the other hand, the polyamides formed as crosslinking agent
Imines lamellar structure is connected with polyimide nano-fiber, may make that being formed by polyimide nano-fiber aeroge has
Better stability and the stress concentration phenomenon for reducing aeroge, to enhance the mechanical property of aeroge, imparting aeroge is good
Good compression recovery performance.Polyimides is as basis material, and therefore, the aeroge is in aerospace, building heat preservation, outdoor fortune
It is dynamic that fields is waited to have good application prospect.
108864473 A of CN discloses the ultralight heat-insulated resilient polyimide nano-fiber aeroge of one kind and its preparation
Method, although the aeroge in this method also has good thermal and insulating performance, the aerogel structure is in extreme temperature
It is easy to be destroyed under the action of thermal stress when environment, to lose insulation ability.Nanofiber in aeroge of the present invention
Pore creating material is not added, ensure that its mechanical performance at a temperature of not having to, while still having good thermal and insulating performance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of insulation polyimide nano-fiber aeroge and its
Preparation method overcomes prior art aeroge to lose the defect of heat-insulating capability in extreme temperatures, uses polyamides sub- in the present invention
For amine nanofiber as basis material, raw material includes polyamic acid and polyimide precursor: water-soluble polyamic acid.
A kind of polyimide nano-fiber aeroge of the invention, which is characterized in that the raw material components include polyamide
Sour nanofiber, water-soluble polyamic acid；Wherein polyamic acid nanofiber, water-soluble polyamic acid mass ratio be 1-5:1,
Polystyrene is not contained in raw material components wherein.
Further, polyamic acid nanofiber, water-soluble polyamic acid mass ratio be 1:1,2:1 or 4:1.
The polyamic acid nanofiber is prepared by following method: diamine monomer being dissolved in polar solvent, adds two
First anhydride monomer reacts to obtain polyamic acid spinning solution, and electrostatic spinning is to get polyamic acid nanofiber；Wherein diamine monomer, two
The ratio of first anhydride monomer is 1:1, and spinning solution mass percentage concentration is 10-20%.
The voltage of the electrostatic spinning is 15~20kV.
The water-soluble polyamic acid are as follows: diamine monomer is dissolved in polar solvent, binary anhydride monomer is added, in ice water
Organic amine is added in bath after polymerization reaction, the reaction was continued, and water-soluble polyamic acid solution is made；The polyamic acid solution is slow
It pours into precipitating in deionized water and obtains polyamic acid, be freeze-dried to get water-soluble polyamic acid；Wherein diamine monomer, two
First anhydride monomer, organic amine ratio be 1:1:2.
The organic amine is triethylamine.
The diamine monomer is p-phenylenediamine or 4,4 '-diaminodiphenyl ethers；Binary anhydride monomer is Pyromellitic Acid two
Acid anhydride, biphenyltetracarboxylic dianhydride or diphenyl ether tetracarboxylic dianhydride；Polar solvent is dimethyl acetamide, N-Methyl pyrrolidone or two
Methylformamide.A kind of preparation method of polyimide nano-fiber aeroge of the invention, comprising:
(1) polyamic acid nanofiber, water-soluble polyamic acid, triethylamine are mixed in water, disperses, is dispersed
Liquid；
(2) above-mentioned dispersion liquid is placed in mold and freezed, then be freeze-dried, carried out hot imidization and received to get polyimides
Rice aeroge.
The preferred embodiment of above-mentioned preparation method is as follows:
It being separated into the step (1) and is dispersed using dispersion machine, the revolving speed of dispersing agent is 10000~13000r/min, point
Dissipating the time is 30-40min.
Freezing is to freeze in cryogenic thermostat reactive bath technique in the step (2), and the temperature of cryogenic thermostat reactive bath technique is -40~60
DEG C, the reaction time is 30~60min；Freeze-drying are as follows: carried out using freeze drier, drying temperature is -50 DEG C, and vacuum degree is
20Pa, drying time are 24~72h.
The technological parameter of hot imidization in the step (2) are as follows: carried out in tube furnace, from room temperature to 120~150
DEG C and keep the temperature 1~2h, then be warming up to 320~360 DEG C and keep the temperature 1.5~2.5h.
A kind of application of polyimide nano-fiber aeroge of the invention.
Beneficial effect
(1) preparation process of the present invention it is simple, it is low in cost, still have the poly- of good heat preservation and insulation under extreme conditions
Acid imide nanofiber aeroge；
(2) preparation process of the present invention is simple, easily operated, is a kind of preparation method of convenient and efficient；
(3) present invention can substantially reduce the quality of aeroge using polyimide nano-fiber as basis material, and
The thermal conductivity for reducing aeroge is crosslinked as crosslinking agent and nanofiber using water-soluble polyamic acid, can eliminate aeroge
Stress concentration phenomenon improves structural stability, while the three-dimensional interworking network structure formed after being crosslinked can reduce its thermal conductivity,
Material is set to have good insulation ability；
(4) polyimide nano-fiber aeroge provided by the invention has lower thermal conductivity, has in high temperature and low temperature
The advantages that standby insulation ability, gained polyimide nano-fiber aeroge thermal conductivity 30mWm-1·K-1, it is minimum can be extremely
27mW·m-1·K-1, and good insulation ability is all had in high temperature and low temperature, still have excellent guarantor under extreme condition
Warm heat-insulating capability is a kind of good heat preserving and insulating material with wide application prospect；
(5) the polyimide nano-fiber aeroge prepared by the present invention has good compression resilience, thermal coefficient
It is low, and still have good heat-insulating capability under high temperature, compression, excellent combination property, preparation process is simple to operation, green
Environmental protection can be used for a variety of heat-insulated scenes.
Detailed description of the invention
Fig. 1 is the electron microscopic picture of the polyimide nano-fiber aeroge of embodiment 1-3 preparation；Wherein A is embodiment 1；B
For embodiment 2；C is embodiment 3；
Fig. 2 is the heat-insulated infrared thermal imaging of the polyimide nano-fiber aeroge of the preparation of embodiment 2 at high temperature；Wherein
A, B, C are respectively the infrared thermal imaging figure that aeroge places different time in 300 DEG C of thermal station, its tip temperature is still after 20mins
So close to room temperature, its excellent thermal and insulating performance and structural stability at high temperature is illustrated；
Fig. 3 is heat preservation infrared thermal imaging of the polyimide nano-fiber aeroge of the preparation of embodiment 2 in low temperature；Wherein
A, B, C are respectively the infrared thermal imaging figure that aeroge places different time on -100 DEG C of cold sources, its tip temperature after 20mins
Still close to room temperature, its thermal and insulating performance and structural stability excellent in low temperature is illustrated.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.Drug is obtained from traditional Chinese medicines chemical reagent institutional purchase.
Embodiment 1
1, using n,N-dimethylacetamide as solvent, pass through 4,4 '-diaminodiphenyl ethers of equimolar ratio and terephthaldehyde
Acid anhydrides carries out condensation polymerization reaction in ice-water bath and the polyamic acid that solid content is 15% is prepared, and obtains polyamic acid mixing
Solution.Detailed process is as follows: 4,4 '-diaminodiphenyl ether of 8.0096g being dissolved in 95.57g n,N-dimethylacetamide, is added
8.8556g pyromellitic acid anhydride, reacts 5h in ice-water bath.Polyamic acid solution is prepared.By the polyamic acid of preparation
Syringe is added in mixed solution, carries out electrostatic spinning, obtains polyamic acid nano fibrous membrane.
2, using n,N-dimethylacetamide as solvent, pass through 4,4 '-diaminodiphenyl ethers of equimolar ratio and terephthaldehyde
Acid anhydrides carries out condensation polymerization reaction in ice-water bath and the polyamic acid that solid content is 15% is prepared.Detailed process is as follows: will
8.0096g4,4 '-diaminodiphenyl ethers are dissolved in 95.57g n,N-dimethylacetamide, and 8.8556g Pyromellitic Acid two is added
Acid anhydride reacts 5h in ice-water bath.Then, 4.0476g triethylamine is added, the reaction was continued 5h, it is 15% that solid content, which is prepared,
Water-soluble polyamic acid solution.By prepared water-soluble polyamic acid deionized water precipitating, then by washing and freezing
It is stand-by to be dried to obtain water-soluble polyamic acid.
3,50mL deionized water is taken, 0.3g nano fibrous membrane, 0.3g water-soluble polyamic acid, the mixing of 0.3g triethylamine,
After even dispersion, obtained dispersion liquid is placed in mold and is freezed in cryogenic thermostat reactive bath technique, it is freeze-dried, after hot imidization
Polyimide nano-fiber aeroge is obtained, PI1-1 is denoted as.
Embodiment 2
The present embodiment difference from example 1 is that: polyamic acid nano fibrous membrane and water-soluble polyamic acid
Mass ratio is 2:1.Take 50mL deionized water, 0.8g nano fibrous membrane, 0.4g water-soluble polyamic acid, 0.4g triethylamine is mixed
It closes, after evenly dispersed, obtained dispersion liquid is placed in mold and is freezed in cryogenic thermostat reactive bath technique, freeze-dried, heat is sub-
Polyimide nano-fiber aeroge is obtained after amination, is denoted as PI2-1.
Embodiment 3
The present embodiment difference from example 1 is that: polyamic acid nano fibrous membrane and water-soluble polyamic acid
Mass ratio is 2:1.Take 50mL deionized water, 0.96g nano fibrous membrane, 0.24g water-soluble polyamic acid, 0.24g triethylamine
Mixing, after evenly dispersed, be placed in mold for obtained dispersion liquid and freeze in cryogenic thermostat reactive bath technique, freeze-dried, heat
Polyimide nano-fiber aeroge is obtained after imidization, is denoted as PI4-1.
The electron microscopic picture of the polyimide nano-fiber aeroge of embodiment 1-3 preparation, as shown in Figure 1；
The heat-insulated infrared thermal imaging of polyimide nano-fiber aeroge prepared by embodiment 2 at high temperature, such as Fig. 2 institute
Show, it can be seen that placed after twenty minutes in 300 DEG C of thermal station, aeroge still has good heat-insulating capability；
The heat preservation infrared thermal imaging of polyimide nano-fiber aeroge prepared by embodiment 2 in low temperature, such as Fig. 3 institute
Show, it can be seen that when bottom is -100 DEG C, aeroge upper surface still has good insulating power.
Claims (10)
1. a kind of polyimide nano-fiber aeroge, which is characterized in that the raw material components include polyamic acid nanofiber,
Water-soluble polyamic acid；Wherein polyamic acid nanofiber, water-soluble polyamic acid mass ratio be 1-5:1, wherein raw material group
Polystyrene is not contained in point.
2. aeroge according to claim 1, which is characterized in that the polyamic acid nanofiber is prepared by following method:
Diamine monomer is dissolved in polar solvent, adds binary anhydride monomer, reacts to obtain polyamic acid spinning solution, electrostatic spinning to get
Polyamic acid nanofiber；Wherein diamine monomer, binary anhydride monomer molar ratio be 1:1, spinning solution mass percentage concentration is
10-20%.
3. aeroge according to claim 1, which is characterized in that the water-soluble polyamic acid are as follows: diamine monomer is molten
In polar solvent, binary anhydride monomer is added, organic amine is added after polymerization reaction in ice-water bath, the reaction was continued, is made water-soluble
Property polyamic acid solution；The polyamic acid solution is poured slowly into precipitating in deionized water and obtains polyamic acid, is freeze-dried, i.e.,
Obtain water-soluble polyamic acid；Diamine monomer, binary anhydride monomer, organic amine molar ratio be 1:1:2.
4. according to the aeroge of claim 2 and 3, which is characterized in that the diamine monomer be p-phenylenediamine or 4,4 '-two
Amino-diphenylethers；Binary anhydride monomer is pyromellitic acid anhydride, biphenyltetracarboxylic dianhydride or diphenyl ether tetracarboxylic dianhydride；Polarity is molten
Agent is dimethyl acetamide, N-Methyl pyrrolidone or dimethylformamide.
5. aeroge according to claim 3, which is characterized in that the organic amine is triethylamine.
6. a kind of preparation method of polyimide nano-fiber aeroge, comprising:
(1) polyamic acid nanofiber, water-soluble polyamic acid, triethylamine are mixed in water, disperses, obtains dispersion liquid；
(2) above-mentioned dispersion liquid is placed in mold and freezed, then be freeze-dried, carry out hot imidization to get polyimide nano gas
Gel.
7. preparation method according to claim 6, which is characterized in that it is separated into the step (1) and is dispersed using dispersion machine,
The revolving speed of dispersing agent is 10000~13000r/min, jitter time 30-40min.
8. preparation method according to claim 6, which is characterized in that freezing is cryogenic thermostat reactive bath technique in the step (2)
Middle freezing, the temperature of cryogenic thermostat reactive bath technique are -40~60 DEG C, and the reaction time is 30~60min；Freeze-drying are as follows: using cold
Lyophilizer carries out, and drying temperature is -50 DEG C, vacuum degree 20Pa, and drying time is 24~72h.
9. preparation method according to claim 6, which is characterized in that the technological parameter of hot imidization in the step (2) are as follows:
It is carried out in tube furnace, from room temperature to 120~150 DEG C and keeps the temperature 1~2h, then be warming up to 320~360 DEG C and keep the temperature 1.5
~2.5h.
10. the application of polyimide nano-fiber aeroge described in a kind of claim 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111116974A (en) * | 2019-12-30 | 2020-05-08 | 东华大学 | Nylon nanofiber aerogel material for air filtration and preparation method thereof |
| CN111116976A (en) * | 2019-12-30 | 2020-05-08 | 东华大学 | Nanofiber aerogel-based solar water evaporator and preparation method thereof |
| CN111533944A (en) * | 2020-05-08 | 2020-08-14 | 中国科学院空间应用工程与技术中心 | Preparation method of polyimide nanofiber aerogel with controllable microstructure |
| CN113088078A (en) * | 2021-04-08 | 2021-07-09 | 北京化工大学 | MXene/polyimide nanofiber aerogel and preparation method and application thereof |
| CN114775095A (en) * | 2022-05-13 | 2022-07-22 | 芯安健康科技(广东)有限公司 | Antibacterial, mildewproof, aldehyde-removing and odor-removing multifunctional soft chip and preparation method thereof |
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| CN110157035A (en) * | 2019-06-05 | 2019-08-23 | 东华大学 | A kind of heat-insulated anisotropy polyimide nano-fiber aeroge and preparation method thereof |
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| CN114775095B (en) * | 2022-05-13 | 2022-12-09 | 芯安健康科技(广东)有限公司 | Antibacterial, mildew-proof, aldehyde-removing and odor-removing multifunctional soft chip and preparation method thereof |
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Application publication date: 20191025 |