CN107722272B - Preparation method of polyimide film - Google Patents
Preparation method of polyimide film Download PDFInfo
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- CN107722272B CN107722272B CN201711009356.1A CN201711009356A CN107722272B CN 107722272 B CN107722272 B CN 107722272B CN 201711009356 A CN201711009356 A CN 201711009356A CN 107722272 B CN107722272 B CN 107722272B
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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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- 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
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
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- 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
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
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- 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
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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 invention discloses a preparation method of a polyimide film, which comprises the following steps: s1, dividing pyromellitic dianhydride into two equal parts, simultaneously adding the two equal parts into a reactor filled with an N-methyl pyrrolidone solution containing fluorine-containing diamine from different feed inlets for reaction for 3-7 h, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.05-1.15; s2, adding a dehydrating agent, and fully stirring at 4-10 ℃ to obtain a fluorine-containing polyamic acid solution; s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain the polyimide film. According to the invention, through a large-amplitude circular heating mode, the difficult volatile substances are fully volatilized by repeatedly heating and cooling, and the high-quality thin film material without pores, with better heat resistance and thermal stability is obtained.
Description
Technical Field
The invention relates to the technical field of high polymer materials. More particularly, the present invention relates to a method for preparing a polyimide film.
Background
The polyimide has excellent mechanical property, heat resistance, low temperature resistance, flame retardance, solvent resistance and electrical property, can be used as a structural composite material, and is widely applied to aerospace, aviation, precision machinery, microelectronic devices and transparent conductive films thereof, TFT (thin film transistor) substrates, flexible printed circuit substrates and the like.
Polyimides are typically synthesized in a two-step process: the first step is dianhydride and diamine in polar aprotic reaction solvent to form polyamic acid (PAA); the second step is the imidization of hot PAA to polyimide, which mainly has the following problems during the preparation process: in the preparation process, the high-boiling point proton solvent is difficult to volatilize completely, and volatile matters are also released during the cyclization (imidization) of the polyamic acid, so that pores are easy to generate in a composite material product, and a high-quality composite material without pores is difficult to obtain; polyimide has higher melting temperature due to the characteristic of a rigid chain, is not easy to process and form, and a film prepared from the traditional polyimide is generally hard and brittle and has insufficient strength, so that the polyimide has the defect that the linear expansion coefficient and the mechanical strength are difficult to be considered when the polyimide is used in the microelectronic industry; because of the formation of intramolecular and intermolecular Charge Transfer Complexes (CTC) and electronic polarization, the traditional PI film is often yellow or dark brown, and cannot meet the requirements of optical waveguide materials, orientation films of liquid crystal displays, flexible transparent conductive substrates and the like in the communication field on the transparency of the PI film in the optical field.
Meanwhile, the raw materials are expensive, so that the preparation cost of the polyimide is always high. In view of the above disadvantages of polyimides, it is necessary to investigate modification of polyimide molecular structures to continuously adapt to the performance requirements of new products.
Disclosure of Invention
An object of the present invention is to solve the above-described problems and provide advantages which will be described later.
Still another object of the present invention is to provide a method for preparing a polyimide film, which uses a large-scale loop-type heating method and repeated heating and cooling to ensure sufficient volatilization of volatile matters, thereby obtaining a high-quality film material without voids and with better heat resistance and thermal stability.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a polyimide film, comprising the steps of:
s1, dividing pyromellitic dianhydride into two equal parts, and simultaneously adding the two equal parts into a reactor filled with a fluorine-containing diamine N-methyl pyrrolidone solution from different feed inlets for reaction for 3-7 h, wherein the molar ratio of pyromellitic dianhydride to fluorine-containing diamine is 1: 1.05-1.15;
s2, adding a dehydrating agent, and fully stirring at 4-10 ℃ to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain the polyimide film.
Preferably, the dehydrating agent in step S2 is acetic anhydride, and the molar ratio of acetic anhydride to pyromellitic dianhydride is 3-6: 1.
Preferably, in the N-methylpyrrolidone solution of fluorine-containing diamine in step S1, the molar ratio of the aromatic diamine to the aliphatic diamine is 3 to 7:1, and the aromatic diamine is 2,2' -bis (trifluoromethyl) -biphenyldiamine.
Preferably, the aliphatic diamine is a silicone-containing diamine.
Preferably, the N-methylpyrrolidone solution of the fluorine-containing diamine in step S1 is obtained by dissolving the aromatic diamine and the siloxane diamine in the N-methylpyrrolidone-containing solvent after sufficiently stirring them in an argon atmosphere.
Preferably, the solvent further contains tetrahydrofuran, and the molar ratio of the N-methylpyrrolidone to the tetrahydrofuran is 4-6: 1.
Preferably, the thickness of the film coated on the glass plate in the step S3 is 120 to 200 μm, and the polyimide film is obtained after drying in an argon oven, cooling to room temperature and peeling.
The invention at least comprises the following beneficial effects:
the invention provides a preparation method of a polyimide film, which has the advantages of simple process, energy conservation, environmental protection, high economic benefit and easy long-term storage, and compared with the prior art, the method aims at the problems that N-methyl pyrrolidone and the like are difficult to volatilize cleanly and volatile matters are discharged during imidization, adopts a large-span heating mode of rapidly heating from 50 ℃ to 150 ℃ to 250 ℃ to form a fluorine-containing polyamide acid solution in advance, and then quickly awakens and then dries and dehydrates. The thermal imidization process generally starts rapid cyclodehydration at 120-150 ℃, imidization reaction is basically completed when the temperature reaches 250 ℃, the temperature is slightly reduced to 200 ℃, the temperature is increased to 250 ℃ and 300 ℃ to 400 ℃ again in a 'loop type' heating mode, and the difficult volatile substances such as N-methyl pyrrolidone, other solvents and the like are heated repeatedly at 200 ℃, namely near the boiling point, so that the difficult volatile substances are fully volatilized in the previous period, the imidization reaction is more complete, pores in the film forming process are fewer, the heat resistance and the thermal stability are better, and the uniformity is better.
By dividing the pyromellitic dianhydride into two equal parts and adding the two equal parts into the fluorine-containing diamine from different feeding ports, a large amount of fluorine-containing diamine molecules on the contact surfaces at different positions of the reactor are ensured to attack each equal part of the pyromellitic dianhydride in a very short time, and the polymerization reaction is rapidly carried out, so that the condition that the ratio of the pyromellitic dianhydride to the fluorine-containing diamine is damaged due to the consumption of complexing with a solvent is avoided, and a high-concentration and stable solution is generated. Meanwhile, in the polyimide, the fluorine-containing diamine is used as a raw material, and the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is controlled to be 1: 1.05-1.15, so that the solubility and the transparency of the polyimide are increased. Furthermore, the solvent contains tetrahydrofuran, and the proportion of the N-methyl pyrrolidone and the tetrahydrofuran is controlled, so that the dissolving efficiency is improved, the using amount of the N-methyl pyrrolidone is reduced, and the formed film has less pores.
Furthermore, two structures of 2,2' -bis (trifluoromethyl) -biphenyldiamine and aliphatic diamine are adopted, the molar ratio is controlled to be 3-7: 1, the inter-chain molecular distance is increased, small solvent molecules can better enter gaps, the solubility of the small solvent molecules is increased, the CTC (charge transfer complex) effect is eliminated, and the transparency of the polyimide film is improved. On the basis, the aliphatic diamine is siloxane-containing diamine, and by introducing a flexible siloxane structure, the solubility of the polyimide is increased, the processability is improved, and the air permeability, the tensile strength, the impact resistance and other mechanical properties are obviously enhanced.
The prepared polyimide prepolymer glue solution is used for coating, the prepared film has few pores, good mechanical property, thermal property and transparency, and the production process is energy-saving and environment-friendly and has great economic benefit. The polyimide film of the present invention is very promising as, for example, a TFT substrate material, an ITO substrate material, a flexible display substrate, an optical member, or other display devices.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention will be described in further detail with reference to examples, which enable those skilled in the art to practice the invention with reference to the accompanying text.
Example 1
S1, dividing pyromellitic dianhydride into two equal parts, and simultaneously adding the two equal parts into a reactor filled with a fluorine-containing diamine N-methyl pyrrolidone solution from different feed inlets for reaction for 3 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.05;
s2, adding a dehydrating agent, and fully stirring at 4 ℃ to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain the polyimide film.
Example 2
S1, dividing pyromellitic dianhydride into two equal parts, and simultaneously adding the two equal parts into a reactor filled with a fluorine-containing diamine N-methyl pyrrolidone solution from different feed inlets for reaction for 5 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.10;
s2, adding a dehydrating agent, and fully stirring at 7 ℃ to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain the polyimide film.
Example 3
S1, dividing pyromellitic dianhydride into two equal parts, and simultaneously adding the two equal parts into a reactor filled with a fluorine-containing diamine N-methyl pyrrolidone solution from different feed inlets for reaction for 7 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.15;
s2, adding a dehydrating agent, and fully stirring at 10 ℃ to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain the polyimide film.
Example 4
S1, dividing pyromellitic dianhydride into two equal parts, simultaneously adding the two equal parts into a reactor filled with N-methylpyrrolidone solution containing fluorine-containing diamine from different feed inlets, and reacting for 3 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.05.
The N-methylpyrrolidone solution containing the fluorine-containing diamine is obtained by fully stirring 2,2' -bis (trifluoromethyl) -biphenyldiamine and siloxane diamine at a molar ratio of 3:1 in an argon atmosphere and dissolving the two in a solvent containing N-methylpyrrolidone and tetrahydrofuran, wherein the molar ratio of the N-methylpyrrolidone to the tetrahydrofuran is 4: 1.
S2, adding a dehydrating agent acetic anhydride, wherein the molar ratio of acetic anhydride to pyromellitic dianhydride is 3-6: 1, and fully stirring at 4-10 ℃ to obtain the fluorine-containing polyamic acid solution.
S3, coating the fluorine-containing polyamic acid solution on a glass plate, wherein the thickness of the film coated on the glass plate is 120 mu m, drying the glass plate in an argon oven at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ for 1h each time, cooling to room temperature after drying, and stripping to obtain the polyimide film.
Example 5
S1, dividing pyromellitic dianhydride into two equal parts, simultaneously adding the two equal parts into a reactor filled with N-methylpyrrolidone solution containing fluorine-containing diamine from different feed inlets, and reacting for 7 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.10.
The N-methylpyrrolidone solution containing the fluorine-containing diamine is obtained by fully stirring 2,2' -bis (trifluoromethyl) -biphenyldiamine and siloxane diamine at a molar ratio of 5:1 in an argon atmosphere and dissolving the two in a solvent containing N-methylpyrrolidone and tetrahydrofuran at a molar ratio of 5: 1.
S2, adding acetic anhydride as a dehydrating agent, wherein the molar ratio of the acetic anhydride to the pyromellitic dianhydride is 5:1, and fully stirring at 7 ℃ to obtain the fluorine-containing polyamic acid solution.
S3, coating the fluorine-containing polyamic acid solution on a glass plate, wherein the thickness of the film coated on the glass plate is 150 μm, drying the glass plate in an argon oven at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ for 1h each time, cooling to room temperature after drying, and stripping to obtain the polyimide film.
Example 6
S1, dividing pyromellitic dianhydride into two equal parts, simultaneously adding the two equal parts into a reactor filled with N-methylpyrrolidone solution containing fluorine-containing diamine from different feed inlets, and reacting for 5 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.15.
The N-methylpyrrolidone solution containing the fluorine-containing diamine is obtained by fully stirring 2,2' -bis (trifluoromethyl) -biphenyldiamine and siloxane diamine at a molar ratio of 7:1 in an argon atmosphere and dissolving the two in a solvent containing N-methylpyrrolidone and tetrahydrofuran, wherein the molar ratio of the N-methylpyrrolidone to the tetrahydrofuran is 6: 1.
S2, adding acetic anhydride as a dehydrating agent, wherein the molar ratio of the acetic anhydride to the pyromellitic dianhydride is 6:1, and fully stirring at 10 ℃ to obtain the fluorine-containing polyamic acid solution.
S3, coating the fluorine-containing polyamic acid solution on a glass plate, wherein the thickness of the film coated on the glass plate is 200 μm, drying the glass plate in an argon oven at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ for 1h each time, cooling to room temperature after drying, and stripping to obtain the polyimide film.
Comparative example 1
S1, adding pyromellitic dianhydride into a reactor filled with a fluorine-containing diamine N-methyl pyrrolidone solution to react for 5 hours, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.10;
s2, adding a dehydrating agent, and fully stirring at normal temperature to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃ and 400 ℃ in sequence to obtain the polyimide film.
In order to illustrate the effects of the present invention, the inventors performed performance tests on the polyimide films prepared in the above examples and comparative examples, and compared the transparency, thermal properties, mechanical properties and solubility of each group of polyimide films, respectively, and the results are shown in table 1.
TABLE 1 polyimide film Properties
As can be seen from the test results in Table 1, since the conditions of example 2 are the same as those of comparative example 1 except that the heating manner of the "loop type" and the divided charging manner of pyromellitic dianhydride are different, the glass transition temperature Tg and the thermal weight loss temperature Td of example 2 are significantly higher than those of comparative example 1 in comparison with comparative example 1 in the case of the polyimide film prepared in example 2, i.e., the polyimide film obtained by the "loop type" heating manner and the divided charging manner of pyromellitic dianhydride has better heat resistance and thermal stability, and the solubility is also enhanced. Meanwhile, in examples 4 to 6, compared with examples 1 to 3, the two structures of 2,2' -bis (trifluoromethyl) -biphenyldiamine and siloxane diamine are adopted, so that the transparency and the tensile strength are obviously enhanced, particularly the tensile strength is obviously enhanced, and the thermal stability is also enhanced to a certain extent.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (4)
1. The preparation method of the polyimide film is characterized by comprising the following steps:
s1, dividing pyromellitic dianhydride into two equal parts, simultaneously adding the parts into a reactor filled with an N-methyl pyrrolidone solution containing fluorine-containing diamine from different feed inlets, and reacting for 3-7 h, wherein the molar ratio of the pyromellitic dianhydride to the fluorine-containing diamine is 1: 1.05-1.15;
s2, adding a dehydrating agent, and fully stirring at 4-10 ℃ to obtain a fluorine-containing polyamic acid solution;
s3, coating the fluorine-containing polyamic acid solution on a glass plate, and heating the glass plate in an argon oven for 1h at 50 ℃, 150 ℃, 250 ℃, 200 ℃, 250 ℃, 300 ℃ and 400 ℃ in sequence to obtain a polyimide film;
in the step S1, the molar ratio of the aromatic diamine to the aliphatic diamine in the N-methylpyrrolidone solution of the fluorine-containing diamine is 5:1, the aromatic diamine is 2,2' -bis (trifluoromethyl) -biphenyldiamine, and the aliphatic diamine is siloxane-containing diamine;
the N-methyl pyrrolidone solution also contains tetrahydrofuran, and the molar ratio of the N-methyl pyrrolidone to the tetrahydrofuran is 4-6: 1.
2. The method of claim 1, wherein the dehydrating agent in step S2 is acetic anhydride, and the molar ratio of acetic anhydride to pyromellitic dianhydride is 3-6: 1.
3. The method for producing a polyimide film according to claim 1, wherein the N-methylpyrrolidone solution containing a fluorine-containing diamine in step S1 is obtained by dissolving an aromatic diamine and a siloxane diamine in a solvent containing N-methylpyrrolidone and tetrahydrofuran under an argon atmosphere with sufficient stirring.
4. The method for preparing the polyimide film according to claim 1, wherein the thickness of the film coated on the glass plate in the step S3 is 120 to 200 μm, the film is dried in an argon oven and then cooled to room temperature, and the polyimide film is obtained after peeling.
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| JP2001152013A (en) * | 1999-11-26 | 2001-06-05 | Gunze Ltd | Thermally stable semiconductive polyamic acid composition and its use |
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