CN107365497A - A kind of polyimide-based composite aerogel with high flame resistance and its preparation method and application - Google Patents
A kind of polyimide-based composite aerogel with high flame resistance and its preparation method and application Download PDFInfo
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- CN107365497A CN107365497A CN201610316005.4A CN201610316005A CN107365497A CN 107365497 A CN107365497 A CN 107365497A CN 201610316005 A CN201610316005 A CN 201610316005A CN 107365497 A CN107365497 A CN 107365497A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a kind of preparation method and product of polyimide-based composite aerogel, and in particular to one kind strengthens polyimide-based composite aerogel and its preparation method and application using graphene.Its composition includes：The mass ratio of graphene and polyimides, the graphene and the polyimides is 6：100~20：100.Its preparation process includes：Graphene oxide is well mixed with the water-soluble precursor polyamic acid of polyimides, by sol-gel process and Freeze Drying Technique, prepares graphene oxide polyamic acid composite aerogel；Again by the sub- amidation process of heat, graphene polyimides composite aerogel is prepared.Polyimide-based composite aerogel prepared by the present invention is using a kind of preparation method of Green Chemistry, the use of no phosphonium flame retardant or halogen-containing flame retardant.In addition, the mechanical property of prepared polyimide-based composite aerogel, heat resistance and excellent in flame retardance, thus be a kind of preferably heat-insulated and fire proofing.
Description
Technical field
The invention belongs to the technical field of novel nano-material-polymer-based porous composite aerogel, it is related to a kind of graphite
Polyimide-based aerogel composite of alkene enhancing and its preparation method and application.
Background technology
Aeroge is a kind of porous gel-like substance with three-dimensional net structure using gas as decentralized medium, hole
Rate is generally 80~99.8%, and specific surface area is generally 200~1000m2g-1, density is typically smaller than 0.1g cm-3.Just because of
This unique loose structure of aeroge so that aeroge has many excellent property in mechanics, acoustics, calorifics etc.
Can, such as low bulk density, low acoustic impedance, lower thermal conductivity.Therefore, aeroge has wide in heat-insulated, fire-retardant, sound insulation etc.
Application prospect.
Compared with traditional silica (SiO2) aeroge, polymer-based aeroge due to cost is low, easy-formation,
The special performances such as porosity is high, density is low, thermal conductivity is low and be used as the matrix of the material such as fire-retardant, heat-insulated.At present, it is polymer-based
Fire-retardant aeroge is generally using the water miscible high polymer material such as polyvinyl alcohol as matrix, with environmentally friendly nano material, such as
Clay, SiO2 etc. are fire retardant, and freeze-dried technology is prepared.However, polymer-based fire-retardant aeroge generally existing power
Learn poor performance (modulus of compressibility is usually 0.3~5.8MPa), heat decomposition temperature low (190~270 DEG C), the poor flame retardant properties (limit
Oxygen index (OI), LOI<34) the problems such as, thus its application is restricted.To find out its cause, on the one hand it is the power by polymeric matrix in itself
Learn poor performance and heat decomposition temperature is low caused；On the other hand it is due to that flame retardant-nanofiller is easily reunited, in macromolecule matrix
It is difficult to scattered caused.It is thus achieved that the polymer-based aeroge of high flame resistance need to select with excellent mechanical performances and
The water soluble polymer matrix of high decomposition temperature, while need solve the scattering problem of fire-retardant filler in the base.
The content of the invention
The present invention be directed to using water-soluble polymers such as polyvinyl alcohol as main base, clay etc. is the height of main fire retardant
There are mechanics, calorifics, poor flame retardant properties in molecule base composite aerogel, the problems such as using being restricted, propose one kind with graphene
For fire retardant strengthen polyimide aerogels material with and its preparation method and application.
The present invention provides a kind of polyimide-based composite aerogel with high flame resistance, described polyimide-based compound
Aeroge includes graphene and polyimides, and the mass ratio of the graphene and the polyimides is 6:100~20:100.Stone
The cross-linked structure that black alkene is formed with polyamic acid, improve mechanical property, the heat endurance of composite aerogel.
Further, the mass ratio of the graphene and described polyimides is 10:100~18:100.
Further, the polyimide-based composite aerogel also includes montmorillonite.
The graphene and the mass ratio of described montmorillonite are not less than 0.3:1.
Preferably, the graphene and the mass ratio of described montmorillonite are 0.6:1~1.2:1.
The present invention also provides a kind of method for preparing the polyimide-based composite aerogel, comprises the following steps：
Graphene oxide is scattered in deionized water, ultrasound obtains the graphene oxide dispersion of stable dispersion, aoxidizes
The mass concentration of graphene dispersion solution is 2-10mg/mL；
Water-soluble polyamic acid is dissolved in the stable graphene oxide dispersion and obtains graphene oxide-polyamic acid
Solution；
12-24 hours will be placed after the graphene oxide-polyamic acid solution ultrasound, obtained by sol-gel process
To graphene oxide-polyamic acid hydrogel；
It is solid that the graphene oxide-polyamic acid hydrogel is freezed in refrigerator or liquid nitrogen, then dry in freezing
12-64 hours are freeze-dried in dry machine, graphene oxide-polyamic acid aeroge is obtained, is denoted as PAA/GO；
The sub- amidatioon of heat is carried out to the graphene oxide-polyamic acid aeroge in nitrogen atmosphere, prepares graphite
Alkene-polyimide aerogels, is denoted as PI/G.The abundant oxy radical of surface of graphene oxide can be with polyamic acid in fire-bar
Cross-linking reaction occurs under part, improves mechanical property, the heat endurance of composite aerogel.
Further, the preparation method comprises the following steps：
Graphene oxide is scattered in deionized water, ultrasound obtains the graphene oxide dispersion of stable dispersion, aoxidizes
The mass concentration of graphene dispersion solution is 2-10mg/mL；
The montmorillonite of stripping is scattered in deionized water, mechanical agitation obtains scattered montmorillonite dispersions；
Graphene oxide and the montmorillonite after peeling off are scattered in deionized water according to certain ratio, ultrasound obtains surely
Surely scattered graphene oxide/montmorillonite dispersions, wherein the ratio of graphene oxide and the montmorillonite after stripping is more than etc.
In 1:2.Surface of graphene oxide contains the oxy radicals such as abundant carboxyl, hydroxyl, carbonyl, and with negative electrical charge, these groups can
Effectively to be combined with the montmorillonite layer containing positive charge, play graphene oxide and scattered effect is cooperateed with montmorillonite.
Water-soluble polyamic acid is dissolved in described graphene oxide/montmorillonite dispersions and obtains graphene oxide/illiteracy
De- soil-polyamic acid solution；
12-24 hours will be placed after graphene oxide/montmorillonite-polyamic acid solution ultrasound, pass through sol-gel process
Obtain graphene oxide/montmorillonite-polyamic acid hydrogel；
It is solid that graphene oxide/montmorillonite-polyamic acid hydrogel is freezed in refrigerator or liquid nitrogen, is then being freezed
12-64 hours are freeze-dried in drying machine, graphene oxide/montmorillonite-polyamic acid aeroge is obtained, is denoted as PAA/GO/M；
The sub- amidatioon of heat is carried out to graphene oxide/montmorillonite-polyamic acid aeroge in nitrogen atmosphere, prepares stone
Black alkene/montmorillonite-polyimide aerogels, are denoted as PI/GO/M.
Further, the montmorillonite of described stripping is prepared by following steps：Original montmorillonite is scattered in a certain amount of
In deionized water, control temperature heats while stirring at least 0.5h at 70-95 DEG C, through ultrasound at least 1h, filtering, drying standby
With.
Further, described hot sub- amidation process is：By resulting polyamide acidic group composite aerogel in tubular type
Heat stepwise is incubated in nitrogen atmosphere in stove, i.e., 100 DEG C, 200 DEG C and 300 DEG C are incubated 0.5 to 2h respectively.Polyamic acid is dividing
The comparison reacted under Duan Baowen is abundant, and the cross-linked network of the polyamide formed is advantageous to the lifting of follow-up performance than comparatively dense.
The present invention also provides a kind of application of the polyimide-based composite aerogel as heat-barrier material, fire proofing, institute
State polyimide-based composite aerogel and include graphene and polyimides, the mass ratio of the graphene and the polyimides is
6:100~20:100.
The beneficial effects of the present invention are：
(1) mechanical property of the polyimide aerogels strengthened using graphene as fire retardant, heat resistance and anti-flammability obtain
Significant improvement, making it, fire proofing is more widely used as heat-insulated.
(2) due to cooperateing with peptizaiton between graphene oxide and montmorillonite well, it is easy to solve flame retardant-nanofiller
The problem of reunion so that the mechanical property of the polyimide aerogels strengthened using graphene/montmorillonite as fire retardant, heat resistance and
Anti-flammability has obtained further improvement.
(3) mentality of designing of the present invention is ingenious, and the preparation technology that use is simple and convenient, green is by two-dimensional nano lamella material
It is effectively compound to expect that graphene or graphene/montmorillonite are carried out with the polymeric matrix material with excellent properties, directly constructs
Three-dimensional aerogel material with excellent fire-retardancy.
Brief description of the drawings
Fig. 1 is graphene oxide and the sedimentation experiment figure of the scattered ratio of montmorillonite collaboration in the present invention；
Fig. 2-a are the scanning electron microscope (SEM) photograph of polyimide-based composite aerogel PI in the present invention；
Fig. 2-b are polyimide-based composite aerogel PI/G in the present invention100:6 scanning electron microscope (SEM) photograph；
Fig. 2-c are polyimide-based composite aerogel PI/G in the present invention100:6/ M scanning electron microscope (SEM) photograph.
Embodiment
With reference to instantiation, the present invention is described in further detail.
Embodiment 1
Can using DMA as solvent, by equimolar than 4,4 '-diaminodiphenyl ether and equal benzene four
Formic anhydride 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：
At room temperature, first by 8g 4,4 '-diaminodiphenyl ether is substantially soluble in 95g DMAs, is clarified, loseed with solution
Particle is defined, and the pyromellitic dianhydride of the amount of material such as is then added portionwise, is i.e. 8.85g, then moves to reaction in ice-water bath
React 2h.Then the triethylamine of the amount of substance such as addition and diamines, continues stirring reaction about 2h, and it is 15% that solid content, which is prepared,
Polyamic acid solution.Prepared polyamic acid solution is sealed, standing is poured slowly into frozen water two days later, scrubbed,
Freezing, it is standby to obtain water-soluble polyamic acid after drying.
30mL deionized waters are taken, 2g polyamic acids and 1g triethylamines is added, ultrasonic 1h, stirs 0.5h, make polyamic acid molten
Solve and be uniformly dispersed, obtain the polyamic acid aqueous solution.Triethylamine can be coated on the terminal carboxyl function of polyamic acid, made
Polyamic acid is soluble in deionized water.It is then transferred in mould, and ultrasonic 0.5h, mould is then transferred to 4 DEG C of left sides
Precooling 5h in right refrigerator, placing into liquid nitrogen makes its quick freeze be solid, is then freezed under 10~20Pa vacuums dry
Dry 48h, obtain 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 heating 30min, 1h is incubated；100 DEG C to 200 DEG C, heat up 30min, is incubated 1h；200 DEG C to 300 DEG C, heat up 30min,
It is incubated 1h, you can obtain polyimide aerogels, be designated as PI.
Embodiment 2
The step of preparing water-soluble polyamic acid is the same as embodiment 1.
It is as follows to prepare the step of graphene strengthens polyimide-based composite aerogel：
Take 30mL 5mg mL-1Graphene oxide dispersion, add 2g polyamic acids and 1g triethylamines, ultrasonic 1h, stirring
0.5h, polyamic acid is dissolved and is uniformly dispersed, obtain the polyamic acid aqueous solution.Remaining step is the same as embodiment 1.Obtain graphene
The polyimide-based composite aerogel of enhancing.Through thermogravimetic analysis (TGA) (TGA), the polyimide-based composite aerogel of graphene enhancing
In, the mass ratio of graphene and polyimides is 6：100.Therefore, the graphene obtained in embodiment 2 strengthens polyimide-based
Composite aerogel is designated as PI/G100:6。
Embodiment 3
The step of preparing water-soluble polyamic acid is the same as embodiment 1.
The step of preparing the polyimide-based composite aerogel of graphene/montmorillonite collaboration enhancing is as follows：
Take the 5mg mL that 30mL is prepared-1Graphene oxide dispersion, add 300mg montmorillonites, stir 0.5h, ultrasound
1h.Remaining step is the same as embodiment 1.The polyimide-based aerogel composite of graphene/montmorillonite collaboration enhancing is obtained, is designated as
PI/G100:6/M。
The polyimide-based aerogel composite obtained in embodiment 1,2,3, PI, PI/G100:6, and PI/G100:6/ M's
The result that properties are tested respectively is shown in table 1.Wherein, heat decomposition temperature is thermal weight loss temperature of the sample in 10wt%.Knot
Fruit shows relative to PI, PI/G100:6Modulus of compressibility, density, specific modulus and decomposition temperature be obviously improved, i.e., poly-
The mechanical property and heat resistance of acid imide aeroge improve substantially under the enhancing of graphene.And relative to PI, PI/G100:6/ M's
Modulus of compressibility, density, specific modulus, decomposition temperature and limited oxygen index are also obtained for lifting.Also, PI/G100:6/ M compression
Modulus, specific modulus, and limited oxygen index are relative to PI/G100:6It is more excellent.
Table 1：The performance of graphene or the polyimide-based composite aerogel of graphene/montmorillonite enhancing
Embodiment 4
Strengthen the method for polyimide-based composite aerogel according to graphene is prepared in embodiment 2, prepare respectively containing stone
Black alkene and polyimides ratio is 40:100,20:100,18:100,13:100 and 10:The polyimides of 100 graphene enhancing
Base composite aerogel, is designated as PI/G respectively100:40, PI/G100:20, PI/G100：18, PI/G100:13, PI/G100:10。
PI/G100:40, PI/G100:20, PI/G100：18, PI/G100:13, PI/G100:10, PI/G100:6Performance test results show
It is shown in table 2.As a result PI/G is shown100:20, PI/G100：18, PI/G100:13, PI/G100:10, PI/G100:6Mechanical property, heat resistance
It is good with anti-flammability.
Table 2：Composite aerogel performance containing different graphenes Yu polyimides mass ratio
Embodiment 5
As shown in figure 1, take 5mg mL-1Graphene oxide be decentralized medium, be separately added into from left to right isometric 0,
2.5th, 5,10,20 and 30mg mL-1Montmorillonite, stir 0.5h, ultrasonic 1h, shape evenly browned dispersion liquid respectively.Then stand
24 hours.As addition 20mg mL-1Montmorillonite when, dispersion liquid starts obvious flocculent deposit occur.And as addition 30mg
mL-1Montmorillonite when, dispersion liquid then completely precipitate.Sedimentation experiment result shows that graphene oxide is at most dispersible
The montmorillonite of twice of mass concentration.It is highly preferred that when the graphene oxide and the mass ratio of described montmorillonite are 1:1~2:
When 1, the collaboration dispersion effect of graphene oxide and montmorillonite is more preferable.
When graphene oxide disperses the montmorillonite of twice mass concentration, according to the method in embodiment 3 prepare graphene/
The polyimide-based composite aerogel of montmorillonite collaboration enhancing, through thermogravimetic analysis (TGA) (TGA), the polyimide-based compound gas of gained
In gel graphene and montmorillonite mass ratio be 0.3:1.When graphene oxide and the mass ratio of described montmorillonite are 1:1
~2:When 1, the polyimide-based compound airsetting of graphene oxide/montmorillonite collaboration enhancing is prepared according to the method in embodiment 3
Glue, through thermogravimetic analysis (TGA) (TGA), in the polyimide-based composite aerogel of gained graphene and the mass ratio of montmorillonite be
0.6:1~1.2:1.
Embodiment 6
Fig. 2 is the scanning electron microscope (SEM) photograph of polyimide-based composite aerogel in the present invention.SEM shows：Institute in the present invention
The PI/G of preparation100:6And PI/G100:6/ M, compared to PI, its inner void more uniform compact, also further more intuitively
Explain PI/G100:6And PI/G100:6/ M mechanical properties, heat resistance and fire resistance it is excellent.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that
After the content of the invention lectured has been read, those skilled in the art can make various changes or modification to the present invention, these
The equivalent form of value equally falls within the application appended claims limited range.
Claims (10)
1. a kind of polyimide-based composite aerogel with high flame resistance, it is characterised in that described polyimide-based compound
Aeroge includes graphene and polyimides, and the mass ratio of the graphene and the polyimides is 6:100~20:100.
2. polyimide-based composite aerogel according to claim 1, it is characterised in that the graphene gathers with described
Imido mass ratio is 10:100~18:100.
3. polyimide-based composite aerogel according to claim 1, it is characterised in that the polyimide-based compound gas
Gel also includes montmorillonite.
4. polyimide-based composite aerogel according to claim 3, it is characterised in that the graphene and described illiteracy
The mass ratio for taking off soil is not less than 0.3:1.
5. polyimide-based composite aerogel according to claim 4, it is characterised in that the graphene and described illiteracy
The mass ratio for taking off soil is 0.6:1~1.2:1.
6. a kind of preparation method of the polyimide-based composite aerogel with high flame resistance, it is characterised in that comprising as follows
Step：
Graphene oxide is scattered in deionized water, ultrasound obtains the graphene oxide dispersion of stable dispersion, graphite oxide
The mass concentration of alkene dispersion soln is 2-10mg/mL；
Water-soluble polyamic acid is dissolved in the stable graphene oxide dispersion to obtain graphene oxide-polyamic acid molten
Liquid；
12-24h will be placed after the graphene oxide-polyamic acid solution ultrasound, obtain aoxidizing stone by sol-gel process
Black alkene-polyamic acid hydrogel；
It is solid that the graphene oxide-polyamic acid hydrogel is freezed in refrigerator or liquid nitrogen, then in freeze drier
Middle freeze-drying 12-64h, graphene oxide-polyamic acid aeroge is obtained, is denoted as PAA/GO；
The sub- amidatioon of heat is carried out to the graphene oxide-polyamic acid aeroge in nitrogen atmosphere, prepares graphene-poly-
Acid imide aeroge, is denoted as PI/G.
7. the preparation method of polyimide-based composite aerogel according to claim 6, it is characterised in that include following step
Suddenly：
Graphene oxide is scattered in deionized water, ultrasound obtains the graphene oxide dispersion of stable dispersion, graphite oxide
The mass concentration of alkene dispersion soln is 2-10mg/mL；
The montmorillonite of stripping is scattered in deionized water, mechanical agitation obtains scattered montmorillonite dispersions, and montmorillonite disperses
The mass concentration of solution is 2-50mg/mL；
Graphene oxide and the montmorillonite after peeling off are scattered in deionized water according to certain ratio, ultrasound obtains stable point
Scattered graphene oxide/montmorillonite dispersions, wherein graphene oxide and the ratio of the montmorillonite after stripping are more than or equal to 1:2；
Water-soluble polyamic acid is dissolved in described graphene oxide/montmorillonite dispersions obtain graphene oxide/montmorillonite-
Polyamic acid solution；
12-24h will be placed after graphene oxide/montmorillonite-polyamic acid solution ultrasound, oxygen is obtained by sol-gel process
Graphite alkene/montmorillonite-polyamic acid hydrogel；
It is solid that graphene oxide/montmorillonite-polyamic acid hydrogel is freezed in refrigerator or liquid nitrogen, is then being freeze-dried
12-64h is freeze-dried in machine, graphene oxide/montmorillonite-polyamic acid aeroge is obtained, is denoted as PAA/GO/M；
The sub- amidatioon of heat is carried out to graphene oxide/montmorillonite-polyamic acid aeroge in nitrogen atmosphere, prepares graphite
Alkene/montmorillonite-polyimide aerogels, is denoted as PI/G/M.
8. the preparation method of polyimide-based composite aerogel according to claim 7, the montmorillonite of described stripping by
It is prepared by following steps：Original montmorillonite is scattered in deionized water, control temperature heats while stirring at least at 70-95 DEG C
0.5h, it is standby after drying through ultrasound at least 1h, filtering.
9. the preparation method of the polyimide-based aeroge according to claim 6 or 7, it is characterised in that described heat is sub-
Amidation process is：By resulting polyamide acidic group composite aerogel in tube furnace in nitrogen atmosphere heat stepwise protect
Temperature, i.e., 100 DEG C, 200 DEG C and 300 DEG C are incubated 0.5 to 2 hour respectively.
10. a kind of application of polyimide-based composite aerogel with high flame resistance as heat-barrier material, fire proofing, its
It is characterised by, the polyimide-based composite aerogel includes graphene and polyimides, and the graphene is sub- with the polyamides
The mass ratio of amine is 6:100~20:100.
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| CN109453743A (en) * | 2018-12-12 | 2019-03-12 | 郑州大学 | A kind of graphene oxide/bentonite nano piece aeroge, preparation method and application |
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