CN110358085A - A kind of preparation method of silica aerogel/polyimides compound heat-insulation film - Google Patents
A kind of preparation method of silica aerogel/polyimides compound heat-insulation film Download PDFInfo
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- CN110358085A CN110358085A CN201810317983.XA CN201810317983A CN110358085A CN 110358085 A CN110358085 A CN 110358085A CN 201810317983 A CN201810317983 A CN 201810317983A CN 110358085 A CN110358085 A CN 110358085A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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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Abstract
The present invention relates to a kind of silica aerogel/polyimides compound heat-insulation film preparation methods.Excellent with mechanical performance, chemical stability is high, and the polyimides of fine heat-resisting performance is matrix, the homemade SiO in laboratory2Aeroge is that reinforcement prepares effectively insulating composite material.It is non-uniform to solve the problems, such as that aeroge disperses using a kind of novel preparation method, and effectively remains the hole configurations of aeroge.Compare influence of the aeroge volume to polyimides heat-proof quality and high temperature resistance, obtain increasing with silica aerogel content, the thermal coefficient of polyimides gradually decreases；Meanwhile although with aeroge addition, the tensile strength of polyimides decreases, and elongation also increases significantly.Illustrate that silica aerogel can significantly improve the heat-proof quality of polyimides, and its mechanical performance can be enhanced to a certain extent.Thus silica aerogel/composite polyimide material of preparation can be extensive, effectively applies in heat-insulated field.
Description
Technical field
The invention belongs to technical field of composite preparation, are related to a kind of silica aerogel/polyimides compound heat-insulation
The method of film.
Background technique
With the development of science and technology and people's environmental consciousness increasingly improves, and the application field of heat-barrier material becomes increasingly wider
General, existing heat-barrier material is mostly insulating mold coating for construction, thermal insulation board, heat insulation felt etc., and in aerospace, automobile, electronic device etc.
Battery, electronic component etc. in field then need a kind of frivolous, soft, convenient thermal insulation film.
Kapton is the flexible material of excellent combination property, and high temperature resistant is up to 400 DEG C, long-term use temperature range-
200~300 DEG C, no sharp melting point, high insulating property, excellent mechanical performances are basis material of the invention.
SiO2Aeroge is a kind of light nanoporous amorphous solid material that heat-proof quality is very excellent, and porosity is reachable
99%, the extremely low (3mg/cm of density3), specific surface area (up to 1600m2/ g), thermal coefficient is low (0.012W/mK), at 700 DEG C
It is able to maintain complete pore structure, high temperature resistance is good；(research [ D ] of high infrared reflection rate insulating moulding coating is breathed out Wang Demin et al.
Your shore: Harbin Engineering University, 2008.) by functional stuffing of SiO2 aeroge it is prepared for insulating moulding coating, YUAN B et al.
(Heat Insulation Properties of silica Aerogel/Glass Fiber Composites
Fabricated by Press Forming [ J ] .Materials Letters, 2012,75:204-206.) it has studied
SiO2 aeroge and glass fibre take punch forming to prepare laminated film, all show SiO2The excellent thermal insulation of aeroge
Can, but it is fewer in aeroge/composite polyimide material field report.
The high porosity of aeroge is one of its performance excellent thermal insulation performance-critical factor, however when aeroge exclusive use
Brittleness is big, it is difficult to form a film；Compound with polymer is easy to block hole, it is difficult to prepare the significant laminated film of heat insulation；
Simultaneously because aeroge density is extremely low, it is not easy to be uniformly dispersed in a polymer matrix；The present invention is to overcome above-mentioned difficulties, and design is closed
At a kind of silica aerogel/polyimides compound heat-insulation film；It is highly polar by the way that aerosil to be added to first
In aprotic organic solvent, aeroge hole is filled using solvent；Further volatilized in polyamic acid heat treatment by solvent
The high porosity of aeroge is kept, so that the aeroge with high porosity is dispersed in polyimide matrix.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of novel SiO2Aeroge/polyimides compound heat-insulation film
Preparation method met the demands of production and living with making up shortcomings and deficiencies of the prior art.
To achieve the above object of the invention, the technical solution adopted by the present invention is that: a kind of SiO that heat-proof quality is excellent2Airsetting
Glue/polyimide composite film preparation method, is made in the steps below:
Step 1: by ethyl orthosilicate, oxalic acid solution, ethyl alcohol hydrolyzes for 24 hours according to a certain percentage, utilizes suitable ammonia spirit tune
PH value is saved to 3 ~ 5, obtains wet gel.
Step 2: wet gel is placed in ethyl alcohol and is replaced；Wet gel is placed in supercritical reaction kettle after displacement and is surpassed
It is critical to be dried to obtain SiO2Aerogel block body；By SiO2Aerogel block body ball mill grinding in the ball mill, obtaining partial size is 30 ~ 60
The aerogel powder of micron.
Step 3: aerogel powder is added in highly polar aprotic organic solvent, is stirred certain time, is made aeroge
It is uniformly dispersed.
Step 4: diamines is added in the mixed liquor of step 3, and dianhydride is added after completely dissolution to it in nitrogen atmosphere
Middle carry out polymerization reaction, diamines and dianhydride molar ratio be 1:0.95 ~ 1.01, reaction temperature be 0 ~ 30 DEG C, the reaction time be 0.5h ~
12h obtains the sticky polyamic acid solution that solid content by weight is 5% ~ 25%.
Step 5: step 4 polyamic acid solution is coated uniformly on clean glass plate, 60 ~ 80 in vacuum drying oven
1h ~ 10h is kept the temperature at DEG C removes solvent；Hot-imide is further carried out using gradient increased temperature mode, SiO is made2Aeroge/poly-
Acid imide compound heat-insulation film.
Ethyl orthosilicate described in step 1, the ratio between volume of ethyl alcohol are preferably 1:1 ~ 1:4, ethyl alcohol and oxalic acid volume ratio
Preferably 8:1 ~ 2:1, ammonia concn are preferably 0.01 ~ 2mol/L, and the concentration of oxalic acid is preferably 0.01 ~ 1mol.
Organic solvent is one of methanol, ethyl alcohol, isopropanol, butanol, the hole of aerogel powder after ball milling in step 2
Diameter is preferably 10 ~ 300 μm.
The optional n,N-Dimethylformamide of highly polar aprotic organic solvent in step 3, n,N-dimethylacetamide,
One kind of N- methyl -2- pyrrolidines.
Diamines described in step 4 selects m-phenylene diamine (MPD), o-phenylenediamine, p-phenylenediamine, 3,3 '-dimethyl -4,4 '-diaminos
Base biphenyl, 3,3 '-dimethoxy-4 's, 4 '-benzidines, 4,4 '-diaminodiphenylmethane, 3,3 '-dimethyl -4,4 '-two
Diaminodiphenylmethane, 4,4 '-diaminodiphenyl ethers, 3,4 '-diaminodiphenyl ethers, 3,3 '-diaminodiphenyl ethers, 4,4 '-diaminos
Base diphenyl sulfide, 4,4 '-diaminodiphenylsulfones, 3,3 '-diaminodiphenylsulfones, 4,4 '-diamino Ketene dimethyls, 3,3 '-diamino
One of diamines such as Ketene dimethyl.
The dianhydride selects pyromellitic acid anhydride, 3,3 ', 4,4 '-tetracarboxylic acid diphenyl ether dianhydrides, 3,3 ', 4 '-tetracarboxylic acids
Diphenyl ether dianhydride, 2,2 ', 3,3 '-tetramethyl diphenyl ether dianhydrides, 3,3 ', 4,4 '-tetracarboxylic acid benzophenone dianhydrides, 3,3 ', 4,4 '
Tetracarboxylic acid biphenyl dianhydride, 2,3,3 ', 4 '-tetracarboxylic acid biphenyl dianhydrides, 2,2 ', 3,3 '-tetracarboxylic acid biphenyl dianhydrides, 3,3 ', 4,4 '-
Tetracarboxylic acid diphenyl ether dianhydride, 2,3,3 ', 4 '-tetracarboxylic acid diphenyl ether dianhydrides, 2,2 ', 3,3 '-tetracarboxylic acid diphenyl ether dianhydrides
One of equal dianhydrides.
Preferred temperature program is as follows in step 5: 120 DEG C of heat preservation 2h are warming up to 250 DEG C of heat preservation 2h, it is Celsius to be warming up to 300
Degree heat preservation 2h.
Detailed description of the invention
Attached drawing 1 is the scanning of silica aerogel prepared by the present invention/polyimides compound heat-insulation film high-amplification-factor
Electron micrograph, attached drawing 2 are silica aerogel prepared by the present invention/polyimides compound heat-insulation film low magnification
Scanning electron micrograph.
Specific embodiment
Embodiment 1
30ml n,N-dimethylacetamide (DMAc) solution is placed in 100ml three-necked flask, 1.822g 4,4 '-two is added
Amino-diphenylethers (ODA) is passed through nitrogen, and ice-water bath is cooled to 0 DEG C, and stirring to ODA is completely dissolved, and it is equal that 2.00g is added in three times
Pyromellitic dianhydride (PMDA) obtains thick polyamic acid solution after being stirred to react 1 hour；It is coated uniformly on glass plate
On, it is placed in vacuum drying oven, under conditions of 80 DEG C, dry 6h removes solvent；Then it according to 120 DEG C of heat preservation 2h, is warming up to
250 DEG C of heat preservation 2h, the gradient increased temperature mode for being warming up to 300 DEG C of heat preservation 2h carry out hot pressing amidation, finally obtain pure polyimides
Film.
Obtained pure Kapton thermal coefficient is 0.5437W/(mK), tensile strength 95.35MPa breaks
Splitting elongation is 6.62%.
Embodiment 2
By ethyl orthosilicate, oxalic acid solution, ethyl alcohol hydrolyzes for 24 hours according to 4:1:8 volume ratio, utilizes the ammonia spirit tune of 0.1mol/L
PH value is saved to 3 ~ 5, wet gel is obtained, wet gel is placed in ethyl alcohol and replaces 3d；Wet gel is placed in supercritical reaction after displacement
Supercritical drying is carried out in kettle, obtains SiO2Aerogel block body；By the ball mill grinding in the ball mill of SiO2 aerogel block body, obtain
The aerogel powder that partial size is 30 ~ 60 microns.
Accounting for Solute mass ratio according to aerogel powder is 1%, weighs 0.038g aeroge and is added to 30ml N, N- dimethyl
In acetamide (DMAc), 30min is stirred with the speed of 200r/min, silica aerogel is enabled to evenly spread to DMAc solution
In, mixed solution is placed in three mouthfuls of 100ml flasks, 4,4 '-diaminodiphenyl ether (ODA) of 1.822g is added, is passed through nitrogen,
Ice-water bath is cooled to 0 DEG C, and stirring to ODA is completely dissolved, and 2.00g pyromellitic acid anhydride (PMDA) is added in three times, and stirring is anti-
It obtains after answering 1 hour mixed with SiO2The thick polyamic acid solution of aeroge；It is coated uniformly on glass plate, is placed in true
In empty baking oven, under conditions of 80 DEG C, dry 6h removes solvent；Then according to 120 DEG C of heat preservation 2h, 250 DEG C of heat preservations are warming up to
2h, the gradient increased temperature mode mode for being warming up to 300 DEG C of heat preservation 2h carry out hot pressing amidation, finally obtain silica aerogel/poly-
Acid imide thermal insulation film.
Obtained aeroge/polyimide composite film thermal coefficient is 0.4830W/(mK), tensile strength is
92.14MPa, elongation at break 6.925%.
Embodiment 3
Aeroge preparation method follows embodiment 2, and accounting for Solute mass ratio according to aerogel powder is 2%, weighs 0.076g aeroge
It is added in 30ml n,N-dimethylacetamide (DMAc), 30min is stirred with the speed of 200r/min, enable silica aerogel
It enough evenly spreads in DMAc solution, mixed solution is placed in three mouthfuls of 100ml flasks, 4,4 '-diamino of 1.822g is added
Diphenyl ether (ODA) is passed through nitrogen, and ice-water bath is cooled to 0 DEG C, and stirring to ODA is completely dissolved, and the equal benzene four of 2.00g is added in three times
Formic acid dianhydride (PMDA), obtains after being stirred to react 1 hour mixed with SiO2The thick polyamic acid solution of aeroge；Uniformly by it
Coating on a glass, is placed in vacuum drying oven, and under conditions of 80 DEG C, dry 6h removes solvent；Then it is protected according to 120 DEG C
Warm 2h is warming up to 250 DEG C of heat preservation 2h, and the gradient increased temperature mode mode for being warming up to 300 DEG C of heat preservation 2h carries out hot pressing amidation, finally
Obtain silica aerogel/polyimides thermal insulation film.
Obtained aeroge/polyimide composite film room temperature thermal coefficient is 0.3392W/ (mK), tensile strength
For 90.14MPa, elongation at break 7.435%.
Embodiment 4
Aeroge preparation method follows embodiment 2, and accounting for Solute mass ratio according to aerogel powder is 5%, weighs 0.1911g airsetting
Glue is added in 30ml n,N-dimethylacetamide (DMAc), 30min is stirred with the speed of 200r/min, so that silica aerogel
It can evenly spread in DMAc solution, mixed solution is placed in three mouthfuls of 100ml flasks, 4,4 '-diamino of 1.822g is added
Yl diphenyl ether (ODA) is passed through nitrogen, and ice-water bath is cooled to 0 DEG C, and stirring to ODA is completely dissolved, and the equal benzene of 2.00g is added in three times
Tetracarboxylic acid dianhydride (PMDA), obtains after being stirred to react 1 hour mixed with SiO2The thick polyamic acid solution of aeroge；By it
Even coating on a glass, is placed in vacuum drying oven, and under conditions of 80 DEG C, dry 6h removes solvent；Then according to 120 DEG C
2h is kept the temperature, 250 DEG C of heat preservation 2h are warming up to, the gradient increased temperature mode mode for being warming up to 300 DEG C of heat preservation 2h carries out hot pressing amidation, most
Silica aerogel/polyimides thermal insulation film is obtained eventually.
Obtained aeroge/polyimide composite film room temperature thermal coefficient is 0.2243W/ (mK), tensile strength
For 81.46MPa, elongation at break 9.217%.
Embodiment 5
Aeroge preparation method follows embodiment 2, and accounting for Solute mass ratio according to aerogel powder is 10%, weighs 0.3822g airsetting
Glue is added in 30ml n,N-dimethylacetamide (DMAc), 30min is stirred with the speed of 200r/min, so that silica aerogel
It can evenly spread in DMAc solution, mixed solution is placed in three mouthfuls of 100ml flasks, 4,4 '-diamino of 1.822g is added
Yl diphenyl ether (ODA) is passed through nitrogen, and ice-water bath is cooled to 0 DEG C, and stirring to ODA is completely dissolved, and the equal benzene of 2.00g is added in three times
Tetracarboxylic acid dianhydride (PMDA), obtains after being stirred to react 1 hour mixed with SiO2The thick polyamic acid solution of aeroge；By it
Even coating on a glass, is placed in vacuum drying oven, and under conditions of 80 DEG C, dry 6h removes solvent；Then according to 120 DEG C
2h is kept the temperature, 250 DEG C of heat preservation 2h are warming up to, the gradient increased temperature mode mode for being warming up to 300 DEG C of heat preservation 2h carries out hot pressing amidation, most
Silica aerogel/polyimides thermal insulation film is obtained eventually.
Obtained aeroge/polyimide composite film thermal coefficient is 0.1026W/ (mK), and tensile strength is
78.97MPa, elongation at break 12.794%.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent variation or replacement on the premise of without prejudice to spirit of the invention,
These equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (7)
1. a kind of high temperature resistant SiO2The preparation method of the heat-insulated laminated film of aeroge/polyimides, it is characterised in that in the steps below
It is prepared:
Step 1: by ethyl orthosilicate, oxalic acid solution, ethyl alcohol hydrolyzes for 24 hours according to a certain percentage, utilizes suitable ammonia spirit tune
PH value is saved to 3 ~ 5, obtains wet gel；
Step 2: wet gel is placed in ethyl alcohol and is replaced；Wet gel is placed in supercritical reaction kettle after displacement carry out it is overcritical
It is dry, obtain SiO2 aerogel block body；By the ball mill grinding in the ball mill of SiO2 aerogel block body, obtaining partial size is 30 ~ 60 micro-
The aerogel powder of rice；
Step 3: aerogel powder is added in highly polar aprotic organic solvent in solvent, is stirred certain time, is made airsetting
Glue is uniformly dispersed；
Step 4: diamines is added in the mixed liquor of step 3, be added after completely dissolution to it dianhydride in nitrogen atmosphere into
Row polymerization reaction, diamines and dianhydride molar ratio are 1:0.95 ~ 1.01, and reaction temperature is 0 ~ 30 DEG C, and the reaction time is 0.5h ~ 12h,
Obtain the sticky polyamic acid solution that solid content by weight is 5% ~ 25%；
Step 5: step 4 polyamic acid solution is coated uniformly on clean glass plate, in vacuum drying oven at 60 ~ 80 DEG C
1h ~ 10h is kept the temperature, to remove solvent, it is heat-insulated that SiO2 aeroge/polyimides is made using the hot-imide method of gradient increased temperature
Composite material.
2. the preparation method of silica aerogel/composite polyimide material according to claim 1, it is characterised in that on
Ethyl orthosilicate described in step 1 is stated, the ratio between volume of ethyl alcohol is preferably 1:1 ~ 1:4, and ethyl alcohol is preferably with oxalic acid volume ratio
8:1 ~ 2:1, ammonia concn are preferably 0.01 ~ 2mol/L, and the concentration of oxalic acid is preferably 0.01 ~ 1mol.
3. the preparation method of high temperature oxidation resisting silica aerogel/composite polyimide material according to claim 1, feature
It is in above-mentioned steps two that organic solvent is one of methanol, ethyl alcohol, isopropanol, butanol, the hole of aerogel powder after ball milling
Diameter is preferably 10 ~ 300 μm.
4. the preparation method of silica aerogel/composite polyimide material according to claim 1, it is characterised in that on
State highly polar aprotic organic solvent selection n,N-Dimethylformamide, n,N-dimethylacetamide, N- methyl -2- in step 3
Pyrrolidines is one of.
5. the preparation method of silica aerogel/composite polyimide material according to claim 1, it is characterised in that on
State diamines described in step 4 selection m-phenylene diamine (MPD), o-phenylenediamine, p-phenylenediamine, 3,3 '-dimethyl -4,4 '-benzidines,
3,3 '-dimethoxy-4 's, 4 '-benzidines, 4,4 '-diaminodiphenylmethane, 3,3 '-dimethyl -4,4 '-diamino hexichol
Methane, 4,4 '-diaminodiphenyl ethers, 3,4 '-diaminodiphenyl ethers, 3,3 '-diaminodiphenyl ethers, 4,4 '-diamino diphenyl sulfides
Ether, 4,4 '-diaminodiphenylsulfones, 3,3 '-diaminodiphenylsulfones, 4,4 '-diamino Ketene dimethyls, 3,3 '-diamino Ketene dimethyls etc.
One of diamines.
6. the preparation method of silica aerogel/composite polyimide material according to claim 1, it is characterised in that on
State dianhydride described in step 4 selection pyromellitic acid anhydride, 3,3 ', 4,4 '-tetracarboxylic acid diphenyl ether dianhydrides, 3,3 ', 4 '-tetramethyls
Sour diphenyl ether dianhydride, 2,2 ', 3,3 '-tetramethyl diphenyl ether dianhydrides, 3,3 ', 4,4 '-tetracarboxylic acid benzophenone dianhydrides, 3,3 ', 4,
4 '-tetracarboxylic acid biphenyl dianhydrides, 2,3,3 ', 4 '-tetracarboxylic acid biphenyl dianhydrides, 2,2 ', 3,3 '-tetracarboxylic acid biphenyl dianhydrides, 3,3 ',
4,4 '-tetracarboxylic acid diphenyl ether dianhydrides, 2,3,3 ', 4 '-tetracarboxylic acid diphenyl ether dianhydrides, 2,2 ', 3,3 '-tetracarboxylic acid hexichol
One of dianhydrides such as thioether dianhydride.
7. the preparation method of silica aerogel/composite polyimide material according to claim 1, it is characterised in that on
It is as follows to state preferred temperature program in step 5: 120 DEG C of heat preservation 2h are warming up to 250 DEG C of heat preservation 2h, are warming up to 300 degrees Celsius of heat preservations
2h。
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070259979A1 (en) * | 2006-05-03 | 2007-11-08 | Aspen Aerogels, Inc. | Organic aerogels reinforced with inorganic aerogel fillers |
| CN103432968A (en) * | 2013-09-06 | 2013-12-11 | 常州循天节能科技有限公司 | Preparation method for aerogel particle in cavity structure |
| WO2015152178A1 (en) * | 2014-03-31 | 2015-10-08 | 日産化学工業株式会社 | Method for producing resin thin film, and composition for forming resin thin film |
| JP2015199845A (en) * | 2014-04-09 | 2015-11-12 | ユニチカ株式会社 | Polyimide-silica composite porous body and manufacturing method therefor |
| CN105802220A (en) * | 2016-04-06 | 2016-07-27 | 同济大学 | Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material |
| CN105835498A (en) * | 2016-03-23 | 2016-08-10 | 中国空间技术研究院 | One-side atomic oxygen resistant polyimide composite film and preparation method thereof |
| US20170183470A1 (en) * | 2015-12-25 | 2017-06-29 | Taiwan Textile Research Institute | Amino-containing silica particle, composition for forming polyimide aerogel, polyimide aerogel and method of fabricating the same, polyimide aerogel-containing composite material |
| CN107304053A (en) * | 2016-04-22 | 2017-10-31 | 北京化工大学 | A kind of method of aerosil impregnation process |
| CN107523198A (en) * | 2017-07-26 | 2017-12-29 | 贵州省漆彩金州涂料有限公司 | A kind of aerosil coating manufacture craft |
-
2018
- 2018-04-10 CN CN201810317983.XA patent/CN110358085A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070259979A1 (en) * | 2006-05-03 | 2007-11-08 | Aspen Aerogels, Inc. | Organic aerogels reinforced with inorganic aerogel fillers |
| CN103432968A (en) * | 2013-09-06 | 2013-12-11 | 常州循天节能科技有限公司 | Preparation method for aerogel particle in cavity structure |
| WO2015152178A1 (en) * | 2014-03-31 | 2015-10-08 | 日産化学工業株式会社 | Method for producing resin thin film, and composition for forming resin thin film |
| JP2015199845A (en) * | 2014-04-09 | 2015-11-12 | ユニチカ株式会社 | Polyimide-silica composite porous body and manufacturing method therefor |
| US20170183470A1 (en) * | 2015-12-25 | 2017-06-29 | Taiwan Textile Research Institute | Amino-containing silica particle, composition for forming polyimide aerogel, polyimide aerogel and method of fabricating the same, polyimide aerogel-containing composite material |
| CN105835498A (en) * | 2016-03-23 | 2016-08-10 | 中国空间技术研究院 | One-side atomic oxygen resistant polyimide composite film and preparation method thereof |
| CN105802220A (en) * | 2016-04-06 | 2016-07-27 | 同济大学 | Preparation method of polyimide/silicon dioxide aerogel powder composite aerogel material |
| CN107304053A (en) * | 2016-04-22 | 2017-10-31 | 北京化工大学 | A kind of method of aerosil impregnation process |
| CN107523198A (en) * | 2017-07-26 | 2017-12-29 | 贵州省漆彩金州涂料有限公司 | A kind of aerosil coating manufacture craft |
Non-Patent Citations (2)
| Title |
|---|
| SEONG YUN KIM等: ""Silica Aerogel/Polyimide Composites with Preserved Aerogel Pores Using Multi-Step Curing"", 《MACROMOLECULAR RESEARCH》 * |
| 陈晓红等: ""ＳｉＯ2 气凝胶常压干燥工艺与隔热应用进展"", 《宇航材料工艺》 * |
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