CN106633169A - Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof - Google Patents
Carbon-black-filled polyimide-based compound aerogel material and preparation method thereof Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- 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
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Abstract
The invention belongs to the technical field of compound aerogel, and in particular relates to a carbon-black-filled polyimide-based compound aerogel material and a preparation method thereof. The compound aerogel is prepared from the following raw materials: one or more water-soluble polyimide precursor-polyamide acids and one or more carbon black. The preparation method comprises the steps of preparing oxidized carbon black dispersion liquid; preparing polyamide acid-oxidized carbon black hydrogel by means of a sol-gel process; preparing polyamide acid-oxidized carbon black aerogel by means of freeze drying; preparing polyimide-carbon black compound aerogel by means of hot imidization. The raw materials for preparing the polyimide-based compound aerogel are low-cost, and the preparation method is simple and easy to implement; the prepared compound aerogel is uniform in micro-morphology. Furthermore, the prepared polyimide-based compound aerogel has excellent mechanical strength and heat resistance, and a lower dielectric constant, thus being an ideal high-temperature dielectric material.
Description
Technical field
The invention belongs to the technical field of composite aerogel, and in particular to a kind of carbon black filled polyimide-based compound gas
Gel rubber material and preparation method thereof.
Background technology
Polymer aerogel is porous gel class material of the class based on naturally occurring or synthetic macromolecule, with easily into
The characteristics such as type, high porosity, high-specific surface area, low-density, lower thermal conductivity.Thus, polymer aerogel is gradually in heat-insulated, sound insulation
Be used as matrix material in dielectric material.However, polymer aerogel generally existing poor mechanical property, thermal stability are poor, easy
The problems such as combustion.Trace it to its cause, mainly caused by polymeric matrix poor mechanical property and heat decomposition temperature are low.
Polyimides, as a kind of engineering plastics, is a kind of preferable height with good mechanical property and heat endurance
Molecule aeroge matrix material.Polyimide-based aeroge compared with other polymer-based aeroges, in addition to above-mentioned advantage,
The features such as also having high mechanical strength and good heat endurance, is the preferable high performance turbine application material of a class.Generally, polyamides is sub-
Amine aeroge needs the contraction that aeroge is reduced using crosslinking agent in preparation process.However, being applied to polyimides at present
Most of crosslinking agent in aeroge preparation process is expensive and is not yet commercialized, and limits its large-scale use.So that
A kind of wide material sources, mode with low cost solve the problems, such as contraction of the polyimide aerogels in preparation process.Wherein, nanometer
Particle is widely used in strengthening composite because of its unique performance.But nano-particle is easily reunited, in polymeric matrix
In be difficult dispersion, cause the performance boost of composite not notable.
The content of the invention
The present invention be directed to the crosslinking agent at present used in polyimide aerogels preparation process is expensive, using limited
Problem, propose one kind with carbon black as crosslinking agent, and by prepare oxidized black method improve carbon black dispersiveness, prepare charcoal
The method of the polyimides composite aerogel of black filling.
The present invention provides a kind of preparation method of carbon black filled polyimides aerogel composite, its raw material composition bag
Containing one or more water-soluble polyimide precursor-polyamic acid, one or more carbon black, one or more graphite oxide
Alkene, wherein polyamic acid are 100 with the mass ratio of carbon black: 0.2-100:10, preparation is concretely comprised the following steps：
（1）Stir after carbon black is mixed with sodium nitrate, add the concentrated sulfuric acid, continue to stir, obtain carbon black-sodium nitrate-sulfuric acid
Mixed liquor；
（2）Potassium permanganate is slowly added in the mixed liquor of carbon black-sodium nitrate-sulfuric acid, stirring obtains the mixed liquor of carbon black；
（3）Deionized water is slowly added in the mixed liquid of carbon black, hydrogen peroxide is added, oxidized black dispersion liquid is obtained；
（4）Oxidized black dispersion liquid is filtered, and uses salt acid elution, until can't detect sulfate ion, obtain oxidized black
Filter cake；
（5）By oxidized black filtration cakes torrefaction, oxidized black solid is obtained；
（6）Oxidized black is scattered in deionized water, ultrasound obtains the oxidized black dispersion liquid of stable dispersion；
（7）Water-soluble polyamic acid is dissolved in oxidized black dispersion liquid, polyamic acid-oxidized black solution is obtained；
（8）Polyamic acid-oxidized black solution is placed into a period of time, polyamic acid-oxidation is obtained by sol-gel process
Carbon black hydrogel；
（9）By polyamic acid-oxidized black hydrogel precooling for a period of time, then to transfer them in refrigerator or liquid nitrogen freezing be solid
Body, the subsequently freeze-drying in freeze drier obtains polyamic acid-oxidized black aeroge；
（10）Hot Asia amidatioon is carried out to polyamic acid-oxidized black aeroge in nitrogen atmosphere, polyimides-charcoal is prepared
Black aeroge.
Further, step（1）In carbon black be selected from color black, rubber grade carbon black, conductive black and black carbon special.
Further, step（1）Middle carbon black is 1.5 with the mass ratio of sodium nitrate: 1-1.2: 1.
Further, step（1）The middle concentrated sulfuric acid is 60 with the mass ratio of carbon black: 1-45: 1.
Further, step（2）Middle potassium permanganate is 5 with the mass ratio of carbon black: 1-3:1, mixing time is 10-30
h。
Further, step（3）Middle deionization consumption is 400-600 mL.
Further, step（3）The concentration of middle hydrogen peroxide is 10-30%, and consumption is 30-90 mL.
Further, step（4）The concentration of middle hydrochloric acid is 5-10%.
Further, step（5）Middle baking temperature is 50-80 DEG C.
Further, step（6）The concentration of middle oxidized black dispersion liquid is 0.1-10 mg/mL.
Further, step（7）The mass fraction of middle polyamic acid is 4-15%.
Further, step（8）Middle time of repose is 2-24 h.
Further, step（9）Described in pre-coo time be 5-24 h, precooling temperature be 1-5 DEG C, in freeze drier
Middle drying time is 24-72 h.
Further, step（10）Described in heat Asia amidation process be：By the compound gas of resulting polyamide acidic group
Gel is placed in tube furnace and 290-300 DEG C is warmed up in nitrogen atmosphere, insulation 0.5-6 h.
Further, the temperature-rise period divides to be progressively warming up to 90-100 DEG C, 190-200 DEG C and 290-300 DEG C
Bao Wen not 0.5-1.5 h.
The low raw-material cost of polyimides composite aerogel prepared by the present invention, method is simple, and prepared answers
Close aeroge microscopic appearance homogeneous.Additionally, prepared polyimide-based composite aerogel has excellent mechanical strength, heat-resisting
Property and relatively low dielectric constant, are a kind of preferable high-temperature dielectric materials.
Description of the drawings
Fig. 1 is the infared spectrum of oxidized black and untreated carbon black in the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of polyimide aerogels PI in the present invention.
Fig. 3 is polyimide-based composite aerogel PI/CB in the present invention2%Scanning electron microscope (SEM) photograph.
Fig. 4 is polyimide-based composite aerogel PI/CB in the present invention4%Scanning electron microscope (SEM) photograph.
Fig. 5 is polyimide-based composite aerogel PI/CB in the present invention6%Scanning electron microscope (SEM) photograph.
Specific embodiment
With reference to instantiation, the present invention is described in further detail, it should be appreciated that these embodiments are merely to illustrate
The present invention rather than restriction the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, this area
Technical staff can make various changes or modification to the present invention, and these equivalent form of values equally fall within the application appended claims
Limited range.
Embodiment 1
The present embodiment is comprised the steps of：
WithN,N- dimethyl acetamide is solvent, 4,4 '-diaminodiphenyl ether and pyromellitic dianhydride are monomer in ice-water bath
Condensation polymerization reaction is carried out, polyamic acid filiform is prepared.Detailed process is as follows：Under room temperature, first by 8 g（0.04 mol）4,
4 '-diaminodiphenyl ether is substantially soluble in 95 gN,N- dimethyl acetamide, by solution clarification, loses particle and is defined.Then it is slow
Add 8.85 g（0.046 mol）Pyromellitic dianhydride, reaction is subsequently moved to stir in ice-water bath 2 h.Be subsequently adding with
0.04 mol triethylamines, continue the h of stirring reaction about 2, prepare the polyamic acid solution that solid content is 15%.Will be prepared
Polyamic acid solution sealing preserve, standing is poured slowly into two days later in frozen water, scrubbed, freezing, and after being dried water-soluble poly is obtained
Amic acid filiform is standby.
30 mL deionized waters are taken, adds 2 g polyamic acids filiforms and 1 g triethylamines, ultrasonic 1 h to stir 0.5 h, make
Polyamic acid dissolves and is uniformly dispersed, and obtains the polyamic acid aqueous solution.Triethylamine can be coated on the terminal carboxyl group of polyamic acid
In functional group, polyamic acid is set to be soluble in deionized water.In being then transferred to mould, and ultrasonic 0.5 h, subsequently by mould
The h of precooling 5 in 4 DEG C or so of refrigerator is transferred to, it is solid to place into and make in liquid nitrogen its quick freeze, then in 10 ~ 20 Pa
The h of freeze-drying 48 under vacuum, obtains polyamic acid aeroge.
Resulting polyamic acid aeroge is placed in tube furnace, heating schedule, i.e. room temperature are controlled in nitrogen atmosphere
To 100 DEG C of 30 min of intensification, 1 h is incubated；100 DEG C to 200 DEG C, heat up 30 min, is incubated 1 h；200 DEG C to 300 DEG C, intensification 30
Min, is incubated 1 h, you can obtain polyimide aerogels, be designated as PI.
Embodiment 2
The present embodiment is comprised the steps of：
The step of preparing water-soluble polyamic acid is with embodiment 1.
The step of preparing oxidized black is as follows：
With acetylene black（The m of specific surface area 752/ g, apparent density 90-120 g/L）As a example by, prepare oxidized black.5 g carbon blacks are added
Enter in 1000 mL beakers, add 3.75 g sodium nitrate, stir 10 min；The 150 mL concentrated sulfuric acids are added, 0.5 h is stirred；
20 g potassium permanganate are slowly added to, 0.5 h additions are finished, and stir 20 h；500 mL deionized waters are slowly added to, are added after cooling
The hydrogen peroxide of 50 mL 30%, stirs 1 h；Mixing is also carried out into suction filtration, and is washed with 10% hydrochloric acid, until inspection is not measured
Sulfate ion, obtains oxidized black wet cake；Then in 70 DEG C of h of drying 5, oxidized black solid is obtained.
The step of preparing polyimides-carbon black composite aerogel is as follows：
Take 40 mg oxidized blacks to be added in 30 mL deionized waters, ultrasonic 0.5 h makes oxidized black be uniformly dispersed.Obtaining
Oxidized black dispersion liquid in add 2 g polyamic acids and 1 g triethylamines, ultrasonic 1 h stirs 0.5 h, disperses polyamic acid
Uniformly, polyamic acid-oxidized black aqueous solution is obtained.Remaining step is with embodiment 2.Obtain the compound airsetting of polyimides-carbon black
Glue, is designated as PI/CB2%。
Embodiment 3
The present embodiment is comprised the steps of：
The step of preparing water-soluble polyamic acid with embodiment 1, with embodiment 2 the step of prepare oxidized black.
The step of preparing polyimides-carbon black composite aerogel is as follows：
Take 80 mg oxidized blacks to be added in 30 mL deionized waters, ultrasonic 0.5 h makes oxidized black be uniformly dispersed.Remaining is same
Embodiment 3.Polyimides-carbon black composite aerogel is obtained, PI/CB is designated as4%。
Embodiment 4
The present embodiment is comprised the steps of：
The step of preparing water-soluble polyamic acid with embodiment 1, with embodiment 2 the step of prepare oxidized black.
The step of preparing polyimides-carbon black composite aerogel is as follows：
Take 120 mg oxidized blacks to be added in 30 mL deionized waters, ultrasonic 0.5 h makes oxidized black be uniformly dispersed.Remaining is same
Embodiment 3.Polyimides-carbon black composite aerogel is obtained, PI/CB is designated as6%。
The component and performance of the polyimide-based composite aerogel of table 1
。
Claims (10)
1. a kind of preparation method of carbon black filled polyimide-based aerogel composite, it is characterised in that raw material includes：
One or more water-soluble polyimide precursor-polyamic acid, one or more carbon black, the wherein matter of polyamic acid and carbon black
Amount is than being 100: 0.2-100:10, preparation is concretely comprised the following steps：
（1）Stir after carbon black is mixed with sodium nitrate, add the concentrated sulfuric acid, continue to stir, obtain carbon black-sodium nitrate-sulfuric acid
Mixed liquor；
（2）Potassium permanganate is slowly added in the mixed liquor of carbon black-sodium nitrate-sulfuric acid, stirring obtains the mixed liquor of carbon black；
（3）Deionized water is slowly added in black dispersion liquid, hydrogen peroxide is added, oxidized black dispersion liquid is obtained；
（4）Oxidized black dispersion liquid is filtered and used salt acid elution, until can't detect sulfate ion, oxidized black filter is obtained
Cake；
（5）By oxidized black filtration cakes torrefaction, oxidized black solid is obtained；
（6）Oxidized black is scattered in deionized water, ultrasound obtains the oxidized black dispersion liquid of stable dispersion；
（7）Water-soluble polyamic acid is dissolved in into oxidized black dispersion liquid, polyamic acid-oxidized black solution is obtained；
（8）Polyamic acid-oxidized black solution is placed into a period of time, polyamic acid-oxidation is obtained by sol-gel process
Carbon black hydrogel；
（9）By polyamic acid-oxidized black hydrogel precooling for a period of time, then to transfer them in refrigerator or liquid nitrogen freezing be solid
Body, the subsequently freeze-drying in freeze drier obtains polyamic acid-oxidized black aeroge；
（10）Hot Asia amidatioon is carried out to polyamic acid-oxidized black aeroge in nitrogen atmosphere, polyimides-charcoal is prepared
Black aeroge.
2. preparation method according to claim 1, it is characterised in that step（1）Described in carbon black selected from coloring charcoal
Black, rubber grade carbon black, conductive black and black carbon special；Carbon black is 1.5 with the mass ratio of sodium nitrate: 1-1.2: 1；The concentrated sulfuric acid with
The mass ratio of carbon black is 60: 1-45: 1.
3. preparation method according to claim 1 and 2, it is characterised in that step（2）Described in potassium permanganate and carbon black
Mass ratio be 5: 1-3:1, mixing time is 10-30 h.
4. preparation method according to claim 3, it is characterised in that step（3）Middle deionization consumption is 400-600
mL；The concentration of hydrogen peroxide is 10-30%, and consumption is 30-90 mL.
5. the preparation method according to claim 1,2 or 4, it is characterised in that step（4）The concentration of middle hydrochloric acid is 5-
10%；Step（5）Middle baking temperature is 50-80 DEG C.
6. preparation method according to claim 5, it is characterised in that step（6）The concentration of middle oxidized black dispersion liquid is
0.1-10 mg/mL；Step（7）The mass fraction of middle polyamic acid is 4-15%.
7. the preparation method according to claim 1,2,4 or 6, it is characterised in that step（8）Middle time of repose is 2-24
h。
8. preparation method according to claim 7, it is characterised in that step（9）Described in pre-coo time be 5-24
H, precooling temperature is 1-5 DEG C, and drying time is 24-72 h in freeze drier.
9. the preparation method according to claim 1,2,4,6 or 8, it is characterised in that step（10）Described in heat Asia acyl
Aminating process is：Resulting polyamide acidic group composite aerogel is placed in tube furnace and is warmed up in nitrogen atmosphere 290-
300 DEG C, it is incubated 0.5-6 h.
10. a kind of carbon black filled polyimide-based compound gas prepared by one of claim 1-9 preparation method
Gel rubber material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107417961A (en) * | 2017-07-28 | 2017-12-01 | 四川大学 | A kind of anisotropy polyimide aerogels material and preparation method thereof |
| CN108359238A (en) * | 2018-02-28 | 2018-08-03 | 佛山慧创正元新材料科技有限公司 | The preparation method of high temperature resistant compound polyimide dielectric material |
| CN115028997A (en) * | 2022-06-30 | 2022-09-09 | 武汉工程大学 | Biomass-derived carbon/polyimide super-hydrophobic composite aerogel and preparation method and application thereof |
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| CN105110313A (en) * | 2015-07-25 | 2015-12-02 | 复旦大学 | Polyimide-based composite carbon aerogel and preparation method therefor |
| US9309369B1 (en) * | 2009-09-30 | 2016-04-12 | The United States Of America, As Represented By The Administrator Of The National Aeronautics And Space Administration | Polyimide aerogels with three-dimensional cross-linked structure |
| CN106082190A (en) * | 2016-06-13 | 2016-11-09 | 浙江极力动力新能源有限公司 | Graphene/carbon black composite granule Low Temperature Thermal expands ball-milling preparation method |
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| CN104355302A (en) * | 2014-10-21 | 2015-02-18 | 复旦大学 | Preparation method of graphene/polyimide-based carbon aerogel |
| CN105110313A (en) * | 2015-07-25 | 2015-12-02 | 复旦大学 | Polyimide-based composite carbon aerogel and preparation method therefor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107417961A (en) * | 2017-07-28 | 2017-12-01 | 四川大学 | A kind of anisotropy polyimide aerogels material and preparation method thereof |
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| CN108359238A (en) * | 2018-02-28 | 2018-08-03 | 佛山慧创正元新材料科技有限公司 | The preparation method of high temperature resistant compound polyimide dielectric material |
| CN115028997A (en) * | 2022-06-30 | 2022-09-09 | 武汉工程大学 | Biomass-derived carbon/polyimide super-hydrophobic composite aerogel and preparation method and application thereof |
| CN115028997B (en) * | 2022-06-30 | 2024-01-23 | 武汉工程大学 | Biomass-derived carbon/polyimide super-hydrophobic composite aerogel and preparation method and application thereof |
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Application publication date: 20170510 |