CN107652680A - A kind of nanometer alumina modified hybrid film of polyimide and preparation method thereof - Google Patents
A kind of nanometer alumina modified hybrid film of polyimide and preparation method thereof Download PDFInfo
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- CN107652680A CN107652680A CN201710916076.2A CN201710916076A CN107652680A CN 107652680 A CN107652680 A CN 107652680A CN 201710916076 A CN201710916076 A CN 201710916076A CN 107652680 A CN107652680 A CN 107652680A
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- Prior art keywords
- polyimide
- parts
- hybrid film
- modified hybrid
- nanometer alumina
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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
-
- 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
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to film fabrication techniques field, and in particular to a kind of nanometer alumina modified hybrid film of polyimide and preparation method thereof, includes the component of volumes below proportioning：98 108 parts of bibenzene tetracarboxylic dianhydride, 4.4 67 77 parts of diaminodiphenyl ethers, N, 600 620 parts of N dimethyl acetamides, 15 25 parts of the nano aluminium oxide of drying process, then nanometer alumina modified hybrid film of polyimide is made in special process, and this method can further improve blending effect, and heat endurance, the mechanical property of modified resin, which have, to be obviously improved.
Description
Technical field
The present invention relates to film fabrication techniques field, and in particular to a kind of nanometer alumina modified hybrid film of polyimide
And preparation method thereof.
Background technology
The filling-modified resin of inorganic nano-particle mainly passes through blending method, and it either physically or chemically will by different
Nano-particle fully mixes to form composite with resin.Due to nano effect group easily occurs during mixing for nano-particle
It is poly-, and the viscosity of resin is very big, causes modified effect not reach optimum efficiency.
The content of the invention
For shortcomings and deficiencies of the prior art, the present invention provides a kind of nanometer alumina modified hybrid film of polyimide
And preparation method thereof, this method can further improve blending effect, and heat endurance, the mechanical property of modified resin have
It is obviously improved.
Technical scheme is used by order to solve its technical problem：
A kind of nanometer alumina modified hybrid film of polyimide, include the component of volumes below proportioning：Bibenzene tetracarboxylic dianhydride
98-108 parts, 4.4- diaminodiphenyl ether 67-77 parts, DMA 600-620 parts, drying process it is nano oxidized
Aluminium 15-25 parts.
The preparation method of above-mentioned nanometer alumina modified hybrid film of polyimide, comprises the following steps：
A, polyimides compound resin processed：Protect in logical nitrogen, under the isoperibol that 0 DEG C of constant temperature, nano aluminium oxide is added to
In DMA solution, keep after persistently stirring 30 minutes, add 4.4- diaminodiphenyl ethers, continue to be kept stirring for
To being completely dissolved, bibenzene tetracarboxylic dianhydride is added, polyimides compound resin is made after 9 hours；
B, nanometer alumina modified hybrid film of polyimide is made：As for glass after obtained polyimides compound resin is filtered
On plate, with film-laying machine plastic film mulch, being put into baking oven makes its imidization, and nanometer alumina modified hybrid film of polyimide is made.
The beneficial effects of the invention are as follows：This method can further improve blending effect, the heat endurance of modified resin,
Mechanical property, which has, to be obviously improved, and is found by SEM, XRD and thermogravimetic analysis (TGA) and the contrast of other modified effects, mechanical property
Can it be significantly increased with thermal stability.
Embodiment
Embodiment 1：A kind of nanometer alumina modified hybrid film of polyimide, include the component of volumes below proportioning：Connection
98 parts of PMDA, 67 parts of 4.4- diaminodiphenyl ethers, 600 parts of DMA, the nano oxygen of drying process
Change 15 parts of aluminium.
The preparation method of above-mentioned nanometer alumina modified hybrid film of polyimide, comprises the following steps：
A, polyimides compound resin processed：Protect in logical nitrogen, under the isoperibol that 0 DEG C of constant temperature, nano aluminium oxide is added to
In DMA solution, keep after persistently stirring 30 minutes, add 4.4- diaminodiphenyl ethers, continue to be kept stirring for
To being completely dissolved, bibenzene tetracarboxylic dianhydride is added, polyimides compound resin is made after 9 hours；
B, nanometer alumina modified hybrid film of polyimide is made：As for glass after obtained polyimides compound resin is filtered
On plate, with film-laying machine plastic film mulch, being put into baking oven makes its imidization, and nanometer alumina modified hybrid film of polyimide is made.
Embodiment 2：A kind of nanometer alumina modified hybrid film of polyimide, include the component of volumes below proportioning：Connection
108 parts of PMDA, 77 parts of 4.4- diaminodiphenyl ethers, 620 parts of DMA, the nano oxygen of drying process
Change 25 parts of aluminium.
The preparation method of above-mentioned nanometer alumina modified hybrid film of polyimide, comprises the following steps：
A, polyimides compound resin processed：Protect in logical nitrogen, under the isoperibol that 0 DEG C of constant temperature, nano aluminium oxide is added to
In DMA solution, keep after persistently stirring 30 minutes, add 4.4- diaminodiphenyl ethers, continue to be kept stirring for
To being completely dissolved, bibenzene tetracarboxylic dianhydride is added, polyimides compound resin is made after 9 hours；
B, nanometer alumina modified hybrid film of polyimide is made：As for glass after obtained polyimides compound resin is filtered
On plate, with film-laying machine plastic film mulch, being put into baking oven makes its imidization, and nanometer alumina modified hybrid film of polyimide is made.
Embodiment 3：A kind of nanometer alumina modified hybrid film of polyimide, include the component of volumes below proportioning：Connection
93 parts of PMDA, 72 parts of 4.4- diaminodiphenyl ethers, 610 parts of DMA, the nano oxygen of drying process
Change 20 parts of aluminium.
The preparation method of above-mentioned nanometer alumina modified hybrid film of polyimide, comprises the following steps：
A, polyimides compound resin processed：Protect in logical nitrogen, under the isoperibol that 0 DEG C of constant temperature, nano aluminium oxide is added to
In DMA solution, keep after persistently stirring 30 minutes, add 4.4- diaminodiphenyl ethers, continue to be kept stirring for
To being completely dissolved, bibenzene tetracarboxylic dianhydride is added, polyimides compound resin is made after 9 hours；
B, nanometer alumina modified hybrid film of polyimide is made：As for glass after obtained polyimides compound resin is filtered
On plate, with film-laying machine plastic film mulch, being put into baking oven makes its imidization, and nanometer alumina modified hybrid film of polyimide is made.
Claims (2)
1. a kind of nanometer alumina modified hybrid film of polyimide, it is characterised in that include the component of volumes below proportioning：Connection
PMDA 98-108 parts, 4.4- diaminodiphenyl ether 67-77 parts, DMA 600-620 parts, dry at
Nano aluminium oxide 15-25 parts of reason.
2. a kind of preparation method of nanometer alumina modified hybrid film of polyimide, it is characterised in that comprise the following steps：
A, polyimides compound resin processed：Protect in logical nitrogen, under the isoperibol that 0 DEG C of constant temperature, nano aluminium oxide is added to
In DMA solution, keep after persistently stirring 30 minutes, add 4.4- diaminodiphenyl ethers, continue to be kept stirring for
To being completely dissolved, bibenzene tetracarboxylic dianhydride is added, polyimides compound resin is made after 9 hours；
B, nanometer alumina modified hybrid film of polyimide is made：As for glass after obtained polyimides compound resin is filtered
On plate, with film-laying machine plastic film mulch, being put into baking oven makes its imidization, and nanometer alumina modified hybrid film of polyimide is made.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710916076.2A CN107652680A (en) | 2017-09-25 | 2017-09-25 | A kind of nanometer alumina modified hybrid film of polyimide and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710916076.2A CN107652680A (en) | 2017-09-25 | 2017-09-25 | A kind of nanometer alumina modified hybrid film of polyimide and preparation method thereof |
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| CN107652680A true CN107652680A (en) | 2018-02-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776828A (en) * | 2019-02-15 | 2019-05-21 | 哈尔滨理工大学 | A kind of aluminum oxide nanoparticle/polyimides base energy storage medium and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786688A (en) * | 2012-08-06 | 2012-11-21 | 江苏南方贝昇光电材料有限公司 | Preparation method for aureole resistant polyimide film |
| CN103172859A (en) * | 2013-04-16 | 2013-06-26 | 株洲时代电气绝缘有限责任公司 | Polyamide acid dispersion liquid and preparation method thereof as well as polyimide film |
| CN105820366A (en) * | 2016-05-05 | 2016-08-03 | 南方电网科学研究院有限责任公司 | Surface modified nano polyimide film and preparation method thereof |
-
2017
- 2017-09-25 CN CN201710916076.2A patent/CN107652680A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786688A (en) * | 2012-08-06 | 2012-11-21 | 江苏南方贝昇光电材料有限公司 | Preparation method for aureole resistant polyimide film |
| CN103172859A (en) * | 2013-04-16 | 2013-06-26 | 株洲时代电气绝缘有限责任公司 | Polyamide acid dispersion liquid and preparation method thereof as well as polyimide film |
| CN105820366A (en) * | 2016-05-05 | 2016-08-03 | 南方电网科学研究院有限责任公司 | Surface modified nano polyimide film and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776828A (en) * | 2019-02-15 | 2019-05-21 | 哈尔滨理工大学 | A kind of aluminum oxide nanoparticle/polyimides base energy storage medium and preparation method thereof |
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Application publication date: 20180202 |