CN112280036A - Processing technology of polyimide film - Google Patents
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- 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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- 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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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/38—Boron-containing compounds
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- 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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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention belongs to the field of polyimide films, in particular to a processing technology of a polyimide film, aiming at the problems that the prior nano particles have large specific surface area and surface energy, strong interaction exists among the particles, agglomeration is easy to generate, ideal nano-scale compounding is difficult to achieve between the nano particles and polymers with large viscosity, and the comprehensive performance of a composite material is influenced, the following scheme is proposed, which comprises the following steps: s1: preparing 1-10 parts of 4,4' -diaminodiphenyl ether and 1-10 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride, preparing 5-10 parts of N, N-dimethylformamide and preparing 10-20 parts of aluminum oxide, silicon dioxide and boron nitride; s2: a reactor with nitrogen blanket was prepared. The processing technology of the polyimide film is more perfect, the corona resistance of the polyimide film is stronger, the tensile resistance is better, and the service life is longer.
Description
Technical Field
The invention relates to the technical field of polyimide films, in particular to a processing technology of a polyimide film.
Background
The polyimide film is a novel high-temperature-resistant organic polymer film, has high modulus, low shrinkage, high strength, low water absorption, hydrolysis resistance, radiation resistance, no toxicity, excellent insulativity and thermal oxidation resistance, is called as a gold film because the polyimide film is one of the most expensive film materials in the world at present, is a key insulating material of power electrical appliances and is also a key material for manufacturing and packaging microelectronics;
however, the existing nanoparticles have large specific surface area and large surface energy, strong interaction exists among the particles, agglomeration is easy to generate, ideal nanoscale compounding is difficult to achieve between the nanoparticles and polymers with large viscosity, and the comprehensive performance of the composite material is influenced.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a processing technology of a polyimide film.
In order to achieve the purpose, the invention adopts the following technical scheme:
a processing technology of a polyimide film comprises the following steps:
s1: preparing 1-10 parts of 4,4' -diaminodiphenyl ether and 1-10 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride, preparing 5-10 parts of N, N-dimethylformamide and preparing 10-20 parts of aluminum oxide, silicon dioxide and boron nitride;
s2: preparing a reactor with nitrogen protection, putting 6-8 parts of N, N-dimethylformamide into the reactor, opening the reactor, stirring the N, N-dimethylformamide by a stirring device in the reactor in advance, and then adding 2-5 parts of 4,4' -diaminodiphenyl ether for stirring;
s3: adding 2-5 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride in batches, stirring, and continuously adding nitrogen in the stirring process;
s4: sequentially adding 12-16 parts of aluminum oxide, silicon dioxide and boron nitride into a reactor for stirring to form a polyamic acid solution, and defoaming the polyamic acid solution in a defoaming machine;
s5: conveying the defoamed polyamic acid solution to a storage tank of a casting nozzle from a stainless steel tank through a pipeline, taking away the solution in the storage tank through a scraper in front of the casting nozzle, preparing a film with a certain specification and thickness by using a film spreading machine, conveying the film into a drying channel for drying, gradually raising the temperature of the film during drying, gradually volatilizing a solvent, carrying out programmed temperature rise in a drying oven, and carrying out imidization film forming by adopting thermal imidization;
s6: conveying the polyamide acid film on a steel belt, evaporating a solvent to form a solid film, guiding the film stripped from the steel belt to an imidization furnace through a guide roller, imidizing at high temperature, and winding by a winding machine;
s7: and carrying out various performance tests on the corona resistance of the finished film and other detection items.
Preferably, in the S2, the N, N-dimethylformamide is stirred in advance for 5-10 minutes at the temperature of 8-10 ℃ and at the stirring speed of 100-200 r/min.
Preferably, in the S2, the stirring time of the 4,4' -diaminodiphenyl ether is 20-40 minutes, the temperature is 8-15 ℃, and the stirring speed is 200-500 r/min.
Preferably, in the S3, the stirring time of the 3,3',4,4' -benzophenone tetracarboxylic dianhydride is 30-60 minutes, the temperature is 8-15 ℃, and the stirring speed is 300-400 r/min.
Preferably, in the S4, the stirring time of the aluminum oxide, the silicon dioxide and the boron nitride is 60-130 minutes, the temperature is 8-15 ℃, and the stirring speed is 400-500 r/min.
Preferably, in S7, the performance testing equipment is a high-voltage testing transformer, a projection vertical optical meter and a micro-control electronic universal testing machine, and the performance testing equipment can respectively test the electrical strength, the thickness and the tensile strength of the polyimide film.
Compared with the prior art, the invention has the beneficial effects that:
according to the scheme, aluminum oxide, silicon dioxide, boron nitride and other inorganic particles are added in a composite mode in the PAA synthesis process to improve corona resistance of the product, the excellent electrical conductivity of the aluminum oxide is utilized, dissipation of charges can be achieved rapidly, accumulation of the charges after corona discharge is prevented, the excellent thermal conductivity of the boron nitride is utilized, the heat transfer effect of a film surface can be enhanced, heat can be dissipated rapidly, and thermal degradation of molecular chains caused by local overheating is prevented; silicon dioxide, titanium dioxide and the like form micro-traps, a multi-core shielding effect and the like, the uniform dispersion of inorganic nanoparticles is realized by researching the size, the addition proportion, the dispersion condition and a film structure model, the corona resistance is effectively prevented from being broken down, the corona resistance service life is obviously prolonged, the combination of materials with different properties and particle sizes is adopted, the materials can be uniformly distributed in the polyimide film, the corona resistance effect is finally realized, and the corona resistance type polyimide film with better performance is obtained by salivation, bidirectional stretching and thermal imidization to form a film and rolling;
the processing technology of the polyimide film is more perfect, the corona resistance of the polyimide film is stronger, the tensile resistance is better, and the service life is longer.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Implement method
A processing technology of a polyimide film comprises the following steps:
s1: preparing 1-10 parts of 4,4' -diaminodiphenyl ether and 1-10 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride, preparing 5-10 parts of N, N-dimethylformamide and preparing 10-20 parts of aluminum oxide, silicon dioxide and boron nitride;
s2: preparing a reactor with nitrogen protection, putting 6-8 parts of N, N-dimethylformamide into the reactor, opening the reactor, stirring the N, N-dimethylformamide by a stirring device in the reactor in advance, and then adding 2-5 parts of 4,4' -diaminodiphenyl ether for stirring;
s3: adding 2-5 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride in batches, stirring, and continuously adding nitrogen in the stirring process;
s4: sequentially adding 2-6 parts of aluminum oxide, silicon dioxide and boron nitride into a reactor for stirring to form a polyamic acid solution, and defoaming the polyamic acid solution in a defoaming machine;
s5: conveying the defoamed polyamic acid solution to a storage tank of a casting nozzle from a stainless steel tank through a pipeline, taking away the solution in the storage tank through a scraper in front of the casting nozzle, preparing a film with a certain specification and thickness by using a film spreading machine, conveying the film into a drying channel for drying, gradually raising the temperature of the film during drying, gradually volatilizing a solvent, carrying out programmed temperature rise in a drying oven, and carrying out imidization film forming by adopting thermal imidization;
s6: conveying the polyamide acid film on a steel belt, evaporating a solvent to form a solid film, guiding the film stripped from the steel belt to an imidization furnace through a guide roller, imidizing at high temperature, and winding by a winding machine;
s7: and carrying out various performance tests on the corona resistance of the finished film and other detection items.
In this embodiment, in S2, the N, N-dimethylformamide is pre-stirred for 5-10 minutes at 8-10 deg.C and at a stirring speed of 100-200 r/min.
In this example, in S2, 4' -diaminodiphenyl ether was stirred for 20-40 minutes at 8-15 ℃ and at a stirring speed of 200-500 r/min.
In this embodiment, in S3, 3',4,4' -benzophenone tetracarboxylic dianhydride is stirred for 30-60 minutes at 8-15 ℃ and at a stirring speed of 300-400 r/min.
In this embodiment, in S4, the stirring time for alumina, silica and boron nitride is 60-130 minutes, the temperature is 8-15 ℃, and the stirring speed is 400-500 r/min.
In this embodiment, in S7, the performance testing equipment includes a high-voltage testing transformer, a projection vertical optical meter, and a micro-control electronic universal testing machine, and can respectively test the electrical strength, the thickness, and the tensile strength of the polyimide film.
Implementation of the second embodiment
A processing technology of a polyimide film comprises the following steps:
s1: preparing 1-10 parts of 4,4' -diaminodiphenyl ether and 1-10 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride, preparing 5-10 parts of N, N-dimethylformamide and preparing 10-20 parts of aluminum oxide, silicon dioxide and boron nitride;
s2: preparing a reactor with nitrogen protection, putting 7 parts of N, N-dimethylformamide into the reactor, opening the reactor, stirring the N, N-dimethylformamide by using stirring equipment in the reactor in advance, and then adding 4 parts of 4,4' -diaminodiphenyl ether for stirring;
s3: adding 4.2 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride in batches, stirring, and continuously adding nitrogen in the stirring process;
s4: adding 15 parts of aluminum oxide, silicon dioxide and boron nitride into a reactor in sequence, stirring to form a polyamic acid solution, and defoaming the polyamic acid solution in a defoaming machine;
s5: conveying the defoamed polyamic acid solution to a storage tank of a casting nozzle from a stainless steel tank through a pipeline, taking away the solution in the storage tank through a scraper in front of the casting nozzle, preparing a film with a certain specification and thickness by using a film spreading machine, conveying the film into a drying channel for drying, gradually raising the temperature of the film during drying, gradually volatilizing a solvent, carrying out programmed temperature rise in a drying oven, and carrying out imidization film forming by adopting thermal imidization;
s6: conveying the polyamide acid film on a steel belt, evaporating a solvent to form a solid film, guiding the film stripped from the steel belt to an imidization furnace through a guide roller, imidizing at high temperature, and winding by a winding machine;
s7: and carrying out various performance tests on the corona resistance of the finished film and other detection items.
In this example, in S2, N-dimethylformamide was stirred for 8 minutes at 10 ℃ and at 170 r/min.
In this example, in S2, 4' -diaminodiphenyl ether was stirred for 40 minutes at 11 ℃ and at a stirring speed of 300 r/min.
In this example, in S3, 3',4,4' -benzophenone tetracarboxylic dianhydride was stirred at 10 ℃ for 50 minutes and at 350 r/min.
In this embodiment, in S4, the alumina, the silicon dioxide, and the boron nitride are stirred for 120 minutes at 10 ℃ and at a stirring speed of 400 r/min.
In this embodiment, in S7, the performance testing equipment includes a high-voltage testing transformer, a projection vertical optical meter, and a micro-control electronic universal testing machine, and can respectively test the electrical strength, the thickness, and the tensile strength of the polyimide film.
In the embodiment, aluminum oxide, silicon dioxide, boron nitride and other inorganic particles are added in a composite manner in the PAA synthesis process to improve the corona resistance of the product, the excellent electrical conductivity of the aluminum oxide can be utilized to quickly dissipate charges, the accumulation of the charges after corona discharge is prevented, the excellent thermal conductivity of the boron nitride can be utilized to enhance the heat transfer effect of the film surface, the quick dissipation of heat is facilitated, and the thermal degradation of molecular chains caused by local overheating is prevented; the corona-resistant polyimide film with excellent performance is obtained by forming micro-traps, multi-core shielding effect and the like by silicon dioxide, titanium dioxide and the like, realizing the uniform dispersion of inorganic nano particles by researching the size, the addition proportion, the dispersion condition and a film structure model, effectively preventing corona breakdown, obviously prolonging the corona-resistant service life, adopting the combination of materials with different properties and particle sizes, achieving uniform distribution in the polyimide film, finally realizing the corona-resistant effect, and forming and winding a film after salivation, bidirectional stretching and thermal imidization.
Compared with the prior art, the invention has the technical progress that: the processing technology of the polyimide film is more perfect, the corona resistance of the polyimide film is stronger, the tensile resistance is better, and the service life is longer.
Claims (6)
1. The processing technology of the polyimide film is characterized by comprising the following steps of:
s1: preparing 1-10 parts of 4,4' -diaminodiphenyl ether and 1-10 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride, preparing 5-10 parts of N, N-dimethylformamide and preparing 10-20 parts of aluminum oxide, silicon dioxide and boron nitride;
s2: preparing a reactor with nitrogen protection, putting 6-8 parts of N, N-dimethylformamide into the reactor, opening the reactor, stirring the N, N-dimethylformamide by a stirring device in the reactor in advance, and then adding 2-5 parts of 4,4' -diaminodiphenyl ether for stirring;
s3: adding 2-5 parts of 3,3',4,4' -benzophenone tetracarboxylic dianhydride in batches, stirring, and continuously adding nitrogen in the stirring process;
s4: sequentially adding 12-16 parts of aluminum oxide, silicon dioxide and boron nitride into a reactor for stirring to form a polyamic acid solution, and defoaming the polyamic acid solution in a defoaming machine;
s5: conveying the defoamed polyamic acid solution to a storage tank of a casting nozzle from a stainless steel tank through a pipeline, taking away the solution in the storage tank through a scraper in front of the casting nozzle, preparing a film with a certain specification and thickness by using a film spreading machine, conveying the film into a drying channel for drying, gradually raising the temperature of the film during drying, gradually volatilizing a solvent, carrying out programmed temperature rise in a drying oven, and carrying out imidization film forming by adopting thermal imidization;
s6: conveying the polyamide acid film on a steel belt, evaporating a solvent to form a solid film, guiding the film stripped from the steel belt to an imidization furnace through a guide roller, imidizing at high temperature, and winding by a winding machine;
s7: and carrying out various performance tests on the corona resistance of the finished film and other detection items.
2. The process of claim 1, wherein in S2, the N, N-dimethylformamide is pre-stirred for 5-10 min at 8-10 ℃ and at a stirring speed of 100-200 r/min.
3. The process of claim 1, wherein in S2, the stirring time of 4,4' -diaminodiphenyl ether is 20-40 min, the temperature is 8-15 ℃, and the stirring speed is 200-500 r/min.
4. The process of claim 1, wherein in S3, the 3,3',4,4' -benzophenone tetracarboxylic dianhydride is stirred for 30-60 minutes at 8-15 ℃ and at a stirring speed of 300-400 r/min.
5. The process of claim 1, wherein in S4, the stirring time of alumina, silica and boron nitride is 60-130 min, the temperature is 8-15 ℃, and the stirring speed is 400-500 r/min.
6. The process of claim 1, wherein in step S7, the performance testing devices are a high voltage testing transformer, a projection vertical optical meter and a micro-control electronic universal testing machine, which can respectively test the electrical strength, thickness and tensile strength of the polyimide film.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113561589A (en) * | 2021-09-01 | 2021-10-29 | 许绝电工股份有限公司 | Polyimide film and preparation method thereof |
| CN113715236A (en) * | 2021-09-02 | 2021-11-30 | 江苏传艺科技股份有限公司 | Low-retardation polyimide film processing technology and production equipment thereof |
| CN114989466A (en) * | 2022-07-20 | 2022-09-02 | 潍坊弘润新材料有限公司 | Corona-resistant polyimide film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113561589A (en) * | 2021-09-01 | 2021-10-29 | 许绝电工股份有限公司 | Polyimide film and preparation method thereof |
| CN113561589B (en) * | 2021-09-01 | 2023-08-15 | 许绝电工股份有限公司 | Polyimide film and preparation method thereof |
| CN113715236A (en) * | 2021-09-02 | 2021-11-30 | 江苏传艺科技股份有限公司 | Low-retardation polyimide film processing technology and production equipment thereof |
| CN114989466A (en) * | 2022-07-20 | 2022-09-02 | 潍坊弘润新材料有限公司 | Corona-resistant polyimide film and preparation method thereof |
| CN114989466B (en) * | 2022-07-20 | 2022-10-21 | 潍坊弘润新材料有限公司 | Corona-resistant polyimide film and preparation method thereof |
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