CN110423465A - A kind of preparation method and product of the Kapton of biaxial oriented stretch in length and breadth - Google Patents
A kind of preparation method and product of the Kapton of biaxial oriented stretch in length and breadth Download PDFInfo
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- CN110423465A CN110423465A CN201910706009.7A CN201910706009A CN110423465A CN 110423465 A CN110423465 A CN 110423465A CN 201910706009 A CN201910706009 A CN 201910706009A CN 110423465 A CN110423465 A CN 110423465A
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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
-
- 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
-
- 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
- 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
- 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
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
Abstract
The invention discloses the preparation methods and product of a kind of biaxial oriented stretch Kapton in length and breadth.It is made of the raw material of following parts by weight: 1200-1600 parts of diamines, 1200-1600 parts of dianhydride, 15-25 parts of catalyst, 30-50 parts of ferritungstiite.Kapton prepared by the present invention, biaxial oriented stretch orientation in length and breadth is carried out in preparation process, and it is added to ferritungstiite, considerably increase the heat resistance and resistance to shrinkage of Kapton, it is able to satisfy the high-end requirement of electric apparatus insulation and the common requirement in lapping electromagnetic wire field and flexible circuit preparation.
Description
Technical field
The invention belongs to imide membrane preparation technical fields, and in particular to a kind of biaxial oriented stretch polyimides in length and breadth
The preparation method and product of film.
Background technique
Polyimides is a kind of with high-modulus, the engineering plastics of low water absorption and resistance to thermo oxidative stability.Currently, polyamides
Imines has increasingly received the attention and exploitation of people.It is taken the lead by former Machinery Ministry and the Ministry of Chemical Industry in the seventies, researches and develops this in China
Kind material, is used for electric insulation.The main application fields of domestic Kapton are electric apparatus insulation and lapping electromagnetic wire.
Kapton is the key that electric apparatus insulating materials, is widely used in equipment for power transmission and distribution, wind power plant, variable-frequency electric
The manufacture of machine, high-speed pulling motor and high-tension transformer etc. occupies unique status in currently used electric insulation film.With
China's digital product, intelligent appliance, the fast development of automotive electronics etc. pushed the rapid growth in flexible circuit board market.
Such as Mobile Industry, 1 conventional mobile phone demand about 2-3 piece flexible circuit board, high-grade mobile phone 5-6 piece, smart phone is then 6-8
Piece.The Kapton demand in China flexible circuit field is up to 5000 tons, and cumulative year after year, China's Kapton
Product scale is annual up to 4700 tons, but most of product low side, is mainly used in insulating materials field, the application of flexible circuit field
85% or more Kapton rely on import.
Using Kapton as substrate, in its single side or two-sided painting perfluoroethylene-propylene emulsion, adhesive tape is made can
Surround on bare copper wire, heat-resist, thickness of insulating layer is uniform and thin, good airproof performance, improves the humidity resistance of conducting wire.But
It is that current Kapton is flexible poor, and heat resistance is poor, physical property and sealing performance decline under the high temperature conditions, no
It is suitble to the preparation of high-end product such as flexible circuit board.
Summary of the invention
The purpose of the present invention is to provide the preparation methods and product of a kind of biaxial oriented stretch Kapton in length and breadth.
A kind of biaxial oriented stretch Kapton in length and breadth, is made: diamines 1200- of the raw material of following parts by weight
1600 parts, 1200-1600 parts of dianhydride, 15-25 parts of catalyst, 30-50 parts of ferritungstiite.
The diamines is 3,4 '-diaminodiphenyl ethers, 4,4 '-diaminodiphenyl-methanes, 9,9- bis- (fluoro- 4- amino of 3-
Phenyl) fluorenes, one of bis- (the fluoro- 4- aminophenyl of 2-) terephthalates or more than one.
The dianhydride be pyromellitic acid anhydride, bisphenol A dianhydride, bis- (3, the 4- dicarboxyphenyi) hexafluoropropane dianhydrides of 2-,
One of bis- (trimellitic anhydride) phenyl esters of methyl-or more than one.
The catalyst is triethylamine, pyridine or isoquinolin.
A kind of preparation method of the Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst are added, be heated to 70-100 DEG C of initiated polymerization, stir 12-36h,
Slurry is made；
(2) ferritungstiite is crushed, is milled, cross 120-180 mesh, be put into the slurry of step (1) preparation, stir evenly,
Coating liquid is made；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products.
The longitudinal stretching multiplying power of the orientation of biaxial oriented stretch in length and breadth is 1.5-2.5, cross directional stretch multiplying power 6.0-
9.5。
Beneficial effects of the present invention: Kapton prepared by the present invention carries out in preparation process biaxially oriented in length and breadth
Orientation is stretched, and is added to ferritungstiite, the heat resistance and resistance to shrinkage of Kapton is considerably increased, is able to satisfy
The high-end requirement of electric apparatus insulation and the common requirement in lapping electromagnetic wire field and flexible circuit preparation.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
A kind of biaxial oriented stretch Kapton in length and breadth, is made: 3,4 '-diamino of the raw material of following parts by weight
1400 parts of diphenyl ether, 1400 parts of pyromellitic acid anhydride, 20 parts of triethylamine, 40 parts of ferritungstiite.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) 3,4 '-diaminodiphenyl ethers and pyromellitic acid anhydride are mixed, catalyst is added, be heated to 90 DEG C of initiations
Polymerization reaction stirs 28h, and slurry is made；
(2) ferritungstiite is crushed, is milled, cross 160 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products；The longitudinal stretching of the orientation of biaxial oriented stretch in length and breadth
Multiplying power is 1.8, cross directional stretch multiplying power 7.5.
Embodiment 2
A kind of biaxial oriented stretch Kapton in length and breadth, is made: 4,4 '-diamino of the raw material of following parts by weight
1300 parts of diphenyl methane, 1300 parts of bisphenol A dianhydride, 18 parts of isoquinolin, 35 parts of ferritungstiite.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) 4,4 '-diaminodiphenyl-methanes and bisphenol A dianhydride are mixed, isoquinolin is added, it is poly- to be heated to 80 DEG C of initiations
Reaction is closed, for 24 hours, slurry is made in stirring；
(2) ferritungstiite is crushed, is milled, cross 140 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products；The longitudinal stretching of the orientation of biaxial oriented stretch in length and breadth
Multiplying power is 1.5, cross directional stretch multiplying power 6.0.
Embodiment 3
A kind of biaxial oriented stretch Kapton in length and breadth, is made: 9,9- bis- (3- of the raw material of following parts by weight
Fluoro- 4- aminophenyl) 1500 parts of fluorenes, 1500 parts of hexafluoropropane dianhydride of 2- bis- (3,4- dicarboxyphenyis), 25 parts of pyridine, ferritungstiite
45 parts.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) bis- (the fluoro- 4- aminophenyl of the 3-) fluorenes of 9,9- and bis- (3, the 4- dicarboxyphenyi) hexafluoropropane dianhydrides of 2- are mixed,
Pyridine is added, is heated to 90 DEG C of initiated polymerizations, stirs 18h, slurry is made；
(2) ferritungstiite is crushed, is milled, cross 120 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products；The longitudinal stretching of the orientation of biaxial oriented stretch in length and breadth
Multiplying power is 2.2, cross directional stretch multiplying power 8.5.
Embodiment 4
A kind of biaxial oriented stretch Kapton in length and breadth, is made: bis- (fluoro- 4- of 2- of the raw material of following parts by weight
Aminophenyl) 1300 parts of terephthalate, bis- 1300 parts of (trimellitic anhydride) phenyl ester of methyl-, 18 parts of isoquinolin, ferritungstiite 38
Part.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 75 DEG C of initiated polymerizations, stir 32h, slurry is made
Material；
(2) ferritungstiite is crushed, is milled, cross 170 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products；The longitudinal stretching of the orientation of biaxial oriented stretch in length and breadth
Multiplying power is 2.1, cross directional stretch multiplying power 7.8.
Comparative example 1
A kind of biaxial oriented stretch Kapton in length and breadth, is made: 3,4 '-diamino of the raw material of following parts by weight
1400 parts of diphenyl ether, 1400 parts of pyromellitic acid anhydride, 20 parts of triethylamine.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) 3,4 '-diaminodiphenyl ethers and pyromellitic acid anhydride are mixed, catalyst is added, be heated to 90 DEG C of initiations
Polymerization reaction stirs 28h, and slurry is made；
(2) slurry made of step (1) is sent into extrusion coating machine, is coated with polyimide resin liquid by extrusion die
Onto steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(3) polyimide film by step (2) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and obtains final products；The longitudinal stretching of the orientation of biaxial oriented stretch in length and breadth
Multiplying power is 1.8, cross directional stretch multiplying power 7.5.
Comparative example 2
A kind of biaxial oriented stretch Kapton in length and breadth, is made: 3,4 '-diamino of the raw material of following parts by weight
1400 parts of diphenyl ether, 1400 parts of pyromellitic acid anhydride, 20 parts of triethylamine, 40 parts of ferritungstiite.
The preparation method of the above-mentioned Kapton of biaxial oriented stretch in length and breadth carries out in accordance with the following steps:
(1) 3,4 '-diaminodiphenyl ethers and pyromellitic acid anhydride are mixed, catalyst is added, be heated to 90 DEG C of initiations
Polymerization reaction stirs 28h, and slurry is made；
(2) ferritungstiite is crushed, is milled, cross 160 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied polyimide resin liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Obtain final products.
Experimental example
Referring to the requirement of international standard IEC 60674-3-4/6:1993: 150 DEG C, 400 DEG C of shrinking percentage≤0.06%, volume
Resistivity >=1012Ω .m, surface resistivity >=1014Ω.150 DEG C for detecting 1-4 of the embodiment of the present invention and comparative example 1-2,400
DEG C shrinking percentage, volume resistivity and surface resistivity, testing result are as shown in Table 1 and Table 2.
Table 1
Note: * represents P < 0.05 compared with embodiment 1.
Table 2
Note: * represents P < 0.05 compared with embodiment 1.
Claims (6)
1. a kind of biaxial oriented stretch Kapton in length and breadth, which is characterized in that be made of the raw material of following parts by weight: two
1200-1600 parts of amine, 1200-1600 parts of dianhydride, 15-25 parts of catalyst, 30-50 parts of ferritungstiite.
2. biaxial oriented stretch Kapton in length and breadth according to claim 1, which is characterized in that the diamines is 3,
4 '-diaminodiphenyl ethers, 4,4 '-diaminodiphenyl-methanes, 9,9- bis- (the fluoro- 4- aminophenyl of 3-) fluorenes, bis- (fluoro- 4- ammonia of 2-
Base phenyl) one of terephthalate or more than one.
3. biaxial oriented stretch Kapton in length and breadth according to claim 1, which is characterized in that the dianhydride is equal benzene
Tetracarboxylic acid dianhydride, bisphenol A dianhydride, bis- (3, the 4- dicarboxyphenyi) hexafluoropropane dianhydrides of 2-, bis- (trimellitic anhydride) phenyl esters of methyl-
One of or more than one.
4. biaxial oriented stretch Kapton in length and breadth described in -4 according to claim 1, which is characterized in that the catalyst is
Triethylamine, pyridine or isoquinolin.
5. a kind of preparation method of biaxial oriented stretch Kapton in length and breadth, which is characterized in that carry out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 70-100 DEG C of initiated polymerization, stir 12-36h, be made
Slurry；
(2) ferritungstiite is crushed, is milled, cross 120-180 mesh, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid made of step (2) is sent into extrusion coating machine, is applied to polyimide resin liquid by extrusion die
On steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, simultaneously
It carries out biaxial oriented stretch in length and breadth to be orientated, obtains final products.
6. the preparation method of biaxial oriented stretch Kapton in length and breadth according to claim 5, which is characterized in that described
The longitudinal stretching multiplying power of biaxial oriented stretch orientation is 1.5-2.5, cross directional stretch multiplying power 6.0-9.5 in length and breadth.
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| CN201910706009.7A CN110423465A (en) | 2019-08-01 | 2019-08-01 | A kind of preparation method and product of the Kapton of biaxial oriented stretch in length and breadth |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910706009.7A CN110423465A (en) | 2019-08-01 | 2019-08-01 | A kind of preparation method and product of the Kapton of biaxial oriented stretch in length and breadth |
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Citations (4)
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| CN104845367A (en) * | 2015-01-14 | 2015-08-19 | 无锡龙舜实业有限公司 | Plastic agricultural film |
| CN107652679A (en) * | 2017-09-29 | 2018-02-02 | 安徽国风塑业股份有限公司 | A kind of Inverter fed motor PI films and preparation method thereof |
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-
2019
- 2019-08-01 CN CN201910706009.7A patent/CN110423465A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845367A (en) * | 2015-01-14 | 2015-08-19 | 无锡龙舜实业有限公司 | Plastic agricultural film |
| CN104845368A (en) * | 2015-04-01 | 2015-08-19 | 无锡龙舜实业有限公司 | Preparation process of shield plastic film |
| CN107652679A (en) * | 2017-09-29 | 2018-02-02 | 安徽国风塑业股份有限公司 | A kind of Inverter fed motor PI films and preparation method thereof |
| CN109400875A (en) * | 2018-10-31 | 2019-03-01 | 江苏亚宝绝缘材料股份有限公司 | A method of with bis- [4-(3- amino-benzene oxygen) benzoyl] the benzene synthesizing polyamides acid resins of 1,3- |
Non-Patent Citations (2)
| Title |
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| 印协世: "《钨丝生产原理、工艺及其性能》", 31 May 1998, 冶金工业出版社 * |
| 王文广等: "《塑料改性实用技术》", 31 March 2000, 中国轻工业出版社 * |
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Application publication date: 20191108 |