CN106009665A - Polyimide film with low thermal expansion coefficient and preparation method thereof - Google Patents

Polyimide film with low thermal expansion coefficient and preparation method thereof Download PDF

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Publication number
CN106009665A
CN106009665A CN201610226102.4A CN201610226102A CN106009665A CN 106009665 A CN106009665 A CN 106009665A CN 201610226102 A CN201610226102 A CN 201610226102A CN 106009665 A CN106009665 A CN 106009665A
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CN
China
Prior art keywords
kapton
expansion
znow
thermal coefficient
low
Prior art date
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Pending
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CN201610226102.4A
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Chinese (zh)
Inventor
王超
吴小杰
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ANHUI XINBAIGE ELECTRONICS Co Ltd
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ANHUI XINBAIGE ELECTRONICS Co Ltd
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Priority to CN201610226102.4A priority Critical patent/CN106009665A/en
Publication of CN106009665A publication Critical patent/CN106009665A/en
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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
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/08—Oxygen-containing compounds
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/004—Additives being defined by their length
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00—Crosslinking

Abstract

The invention discloses a polyimide film with low thermal expansion coefficient and a preparation method thereof; the polyimide film comprises the following components by the mass percentage: 7%-17% of 1,2,4,5-benzenetetracarboxylic dianhydride, 4%-12% of diaminodiphenyl ether, 70%-88% of dimethylacetamide and 1%-9% of zinc oxide crystal whiskers. The preparation method comprises the steps: adding dimethylacetamide and diaminodiphenyl ether into a reaction kettle, stirring for 25 min-55 min, adding 1,2,4,5-benzenetetracarboxylic dianhydride into the reaction kettle, stirring for 25 min-55 min, finally, adding the zinc oxide crystal whiskers into the reaction kettle, stirring for 25 min-55 min, and thus obtaining a glue liquid after the stirring is completed; making the glue liquid into a gel film by a casting machine; and peeling the gel film from the surface of a mirror steel band of the casting machine, firstly, longitudinally stretching the gel film by using a longitudinal stretching machine, then transversely stretching the gel film by using a transverse stretching machine, and thus obtaining the polyimide film. The polyimide film has the advantages of low thermal expansion coefficient and the like.

Description

Kapton that a kind of thermal coefficient of expansion is low and preparation method thereof
Technical field
The present invention relates to Kapton production and processing field, Kapton that a kind of thermal coefficient of expansion is low and preparation method thereof.
Background technology
Kapton has heat stability, chemical resistance and the mechanical performance of excellence, and usually crocus, the bending strength of the polyimides of graphite or glass fiber reinforcement can reach 345 MPa, composite bending modulus reaches 20GPa, wherein, Kapton is widely used in the field such as Aero-Space, electric, machinery, microelectronics, chemical industry, but the thermal coefficient of expansion of existing Kapton is higher, therefore Kapton is not particularly suited for the field that some are special, needs to make existing Kapton further improvement.
Summary of the invention
The invention aims to solve the defect that Kapton thermal coefficient of expansion of the prior art is high, it is provided that Kapton that a kind of thermal coefficient of expansion is low and preparation method thereof solves the problems referred to above.
The invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 7%-17%, diaminodiphenyl ether 4%-12%, dimethyl acetylamide 70%-88%, ZnOw 1%-9%.
As preferably, the invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 8%-16%, diaminodiphenyl ether 5%-11%, dimethyl acetylamide 71%-87%, ZnOw 2%-8%.
As preferably, the invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 9%-15%, diaminodiphenyl ether 6%-10%, dimethyl acetylamide 72%-86%, ZnOw 3%-7%.
As preferably, the invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 75.1%, ZnOw 5%.
As preferably, the invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 76.1%, ZnOw 4%.
As preferably, the invention discloses the Kapton that a kind of thermal coefficient of expansion is low, according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 79.1%, ZnOw 1%.
As preferably, a length of 1-5 μm of described ZnOw.
As preferably, the present invention also provides for the preparation method of the low Kapton of a kind of above-mentioned thermal coefficient of expansion, specifically comprises the following steps that
Step one: according to above-mentioned mass percent, dimethyl acetylamide and diaminodiphenyl ether are joined in reactor, after stirring 25min-55min, then pyromellitic acid anhydride is joined in reactor, stir 25min-55min, finally ZnOw is joined in reactor, stirring 25min-55min, i.e. preparing glue after having stirred, the temperature in reactor is 22 DEG C-24 DEG C, and the pressure in reactor is 0.1MPa-0.2MPa；
Step 2: by glue on spraying die drool to the minute surface steel strip surface of casting machine, under conditions of 140 DEG C-180 DEG C, glue is prepared as gel film by casting machine；
Step 3: gel film is peeled off from the minute surface steel strip surface of casting machine, under conditions of 340 DEG C-560 DEG C, first use longitudinal stretching machine that gel film is carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-use transverse drawing mill and gel film is carried out cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton, then Kapton is cooled to 20 DEG C-30 DEG C.
The present invention has the advantage that ZnOw is the whisker uniquely possessing regular three-D space structure in current whisker family compared to existing technology, its whisker structure is complete, its strength modulus is the highest, ZnOw is due to solid four acicular texture of its uniqueness, can isotropically improve material mechanical performance, simultaneously because its heat-resisting quantity and low-expansion coefficient, cross-linked network is formed with polyimide resin matrix by each acicular texture, when variations in temperature is violent, can be as size backing material, material chemistry at high temperature and dimensional stability can be improved, therefore after the present invention is by adding ZnOw, the thermal coefficient of expansion ratio of obtained Kapton is relatively low, effectiveness comparison is good.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
Step one: according to mass percent, dimethyl acetylamide 75.1% and diaminodiphenyl ether 9.5% are joined in reactor, after stirring 55min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 55min, finally the ZnOw 5% of a length of 4 μm is joined in reactor, stirring 55min, i.e. preparing glue after having stirred, the temperature in reactor is 23 DEG C, and the pressure in reactor is 0.2MPa；
Step 2: by glue on spraying die drool to the minute surface steel strip surface of casting machine, under conditions of 180 DEG C, glue is prepared as gel film by casting machine；
Step 3: gel film is peeled off from the minute surface steel strip surface of casting machine, under conditions of 500 DEG C, first use longitudinal stretching machine that gel film is carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-use transverse drawing mill and gel film is carried out cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton, then Kapton is cooled to 30 DEG C.
Embodiment 2
Step one: according to mass percent, dimethyl acetylamide 76.1% and diaminodiphenyl ether 9.5% are joined in reactor, after stirring 45min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 45min, finally the ZnOw 4% of a length of 2 μm is joined in reactor, stirring 45min, i.e. preparing glue after having stirred, the temperature in reactor is 24 DEG C, and the pressure in reactor is 0.1MPa；
Step 2: by glue on spraying die drool to the minute surface steel strip surface of casting machine, under conditions of 160 DEG C, glue is prepared as gel film by casting machine；
Step 3: gel film is peeled off from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C, first use longitudinal stretching machine that gel film is carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-use transverse drawing mill and gel film is carried out cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton, then Kapton is cooled to 25 DEG C.
Embodiment 3
Step one: according to mass percent, dimethyl acetylamide 79.1% and diaminodiphenyl ether 9.5% are joined in reactor, after stirring 35min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 35min, finally the ZnOw 1% of a length of 1 μm is joined in reactor, stirring 35min, i.e. preparing glue after having stirred, the temperature in reactor is 24 DEG C, and the pressure in reactor is 0.1MPa；
Step 2: by glue on spraying die drool to the minute surface steel strip surface of casting machine, under conditions of 160 DEG C, glue is prepared as gel film by casting machine；
Step 3: gel film is peeled off from the minute surface steel strip surface of casting machine, under conditions of 450 DEG C, first use longitudinal stretching machine that gel film is carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-use transverse drawing mill and gel film is carried out cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton, then Kapton is cooled to 20 DEG C.
Table 1 is the Performance comparision that the Kapton that thermal coefficient of expansion that embodiment 1, embodiment 2 and embodiment 3 prepare is low is carried out with conventional polyimide thin film in the market, and result is as follows:
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Conventional polyimide thin film
Thermal coefficient of expansion (ppm/K) 9 26 32 49
Mechanical strength (MPa) 260 235 255 170
Electrical strength (MV/m) 270 243 250 180
Dimensional stability (‰) 0.1 0.5 0.3 1.0
The Kapton that thermal coefficient of expansion obtained by the present invention is low as shown in Table 1 has, relative to conventional polyimide thin film on market, the advantage that thermal coefficient of expansion is low, mechanical strength good, electrical strength is good and dimensional stability is strong, and as shown in Table 1, embodiment 1 is the optimum selection of the Kapton that a kind of thermal coefficient of expansion of the present invention is low and preparation method thereof.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle of the simply present invention described in above-described embodiment and description; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements both fall within the range of claimed invention.The protection domain of application claims is defined by appending claims and equivalent thereof.

Claims (8)

1. the Kapton that a thermal coefficient of expansion is low, it is characterised in that: according to mass percent, including following components: pyromellitic acid anhydride 7%-17%, diaminodiphenyl ether 4%-12%, dimethyl acetylamide 70%-88%, ZnOw 1%-9%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterized in that: according to mass percent, including following components: pyromellitic acid anhydride 8%-16%, diaminodiphenyl ether 5%-11%, dimethyl acetylamide 71%-87%, ZnOw 2%-8%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterized in that: according to mass percent, including following components: pyromellitic acid anhydride 9%-15%, diaminodiphenyl ether 6%-10%, dimethyl acetylamide 72%-86%, ZnOw 3%-7%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterized in that: according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 75.1%, ZnOw 5%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterized in that: according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 76.1%, ZnOw 4%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterized in that: according to mass percent, including following components: pyromellitic acid anhydride 10.4%, diaminodiphenyl ether 9.5%, dimethyl acetylamide 79.1%, ZnOw 1%.
The Kapton that a kind of thermal coefficient of expansion the most according to claim 1 is low, it is characterised in that: a length of 1-5 μm of described ZnOw.
8. according to the preparation method of the low Kapton of the arbitrary described a kind of thermal coefficient of expansion of claim 1-7, it is characterised in that: specifically comprise the following steps that
Step one: according to above-mentioned mass percent, dimethyl acetylamide and diaminodiphenyl ether are joined in reactor, after stirring 25min-55min, then pyromellitic acid anhydride is joined in reactor, stir 25min-55min, finally ZnOw is joined in reactor, stirring 25min-55min, i.e. preparing glue after having stirred, the temperature in reactor is 22 DEG C-24 DEG C, and the pressure in reactor is 0.1MPa-0.2MPa；
Step 2: by glue on spraying die drool to the minute surface steel strip surface of casting machine, under conditions of 140 DEG C-180 DEG C, glue is prepared as gel film by casting machine；
Step 3: gel film is peeled off from the minute surface steel strip surface of casting machine, under conditions of 340 DEG C-560 DEG C, first use longitudinal stretching machine that gel film is carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-use transverse drawing mill and gel film is carried out cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton, then Kapton is cooled to 20 DEG C-30 DEG C.
CN201610226102.4A 2016-04-13 2016-04-13 Polyimide film with low thermal expansion coefficient and preparation method thereof Pending CN106009665A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108264766A (en) * 2018-01-25 2018-07-10 无锡创彩光学材料有限公司 A kind of preparation method of Kapton

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090092800A1 (en) * 2007-10-08 2009-04-09 Samsung Electronics Co., Ltd. Composition for preparing modified polyimide/clay nanocomposites and preparation method of modified polymide/clay nanocomposites using the same
CN103275448A (en) * 2013-06-25 2013-09-04 孟红琳 Preparation method of modified packing ion enhanced polytetrafluoroethylene composite
CN103665544A (en) * 2013-11-20 2014-03-26 天津金发新材料有限公司 Isotropic polypropylene composition with low linear expansion coefficient and preparation method thereof
CN105111476A (en) * 2015-09-16 2015-12-02 安徽鑫柏格电子股份有限公司 Preparation method for polyimide film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090092800A1 (en) * 2007-10-08 2009-04-09 Samsung Electronics Co., Ltd. Composition for preparing modified polyimide/clay nanocomposites and preparation method of modified polymide/clay nanocomposites using the same
CN103275448A (en) * 2013-06-25 2013-09-04 孟红琳 Preparation method of modified packing ion enhanced polytetrafluoroethylene composite
CN103665544A (en) * 2013-11-20 2014-03-26 天津金发新材料有限公司 Isotropic polypropylene composition with low linear expansion coefficient and preparation method thereof
CN105111476A (en) * 2015-09-16 2015-12-02 安徽鑫柏格电子股份有限公司 Preparation method for polyimide film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108264766A (en) * 2018-01-25 2018-07-10 无锡创彩光学材料有限公司 A kind of preparation method of Kapton

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Application publication date: 20161012