CN105019047A - Low dielectric polyimide fiber and preparation method thereof - Google Patents

Low dielectric polyimide fiber and preparation method thereof Download PDF

Info

Publication number
CN105019047A
CN105019047A CN201510432142.XA CN201510432142A CN105019047A CN 105019047 A CN105019047 A CN 105019047A CN 201510432142 A CN201510432142 A CN 201510432142A CN 105019047 A CN105019047 A CN 105019047A
Authority
CN
China
Prior art keywords
preparation
fiber
polyimide fiber
polyamic acid
spinning
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510432142.XA
Other languages
Chinese (zh)
Inventor
俞建刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd
Original Assignee
JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd filed Critical JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd
Priority to CN201510432142.XA priority Critical patent/CN105019047A/en
Publication of CN105019047A publication Critical patent/CN105019047A/en
Pending legal-status Critical Current

Links

Landscapes

  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The present invention discloses a low dielectric polyimide fiber and a preparation method thereof, and belongs to the field of functional organic fibers. The fiber is prepared as follows: a copolymer polyamide acid spinning solution is prepared by condensation polymerization of hexafluorodianhydride (6FDA) and other dianhydride diamine; wet or dry-wet spinning process is used for spinning, poly amidoacid as-spun fiber is obtained by solidification and water washing; and the low dielectric polyimide fiber is prepared by thermal imidization and drawing processing of the fiber by gradient temperature, the tensile strength is up to 2.46GPa, initial modulus reaches 82.5GPa, and dielectric constant is as low as 2.55. The present invention provides a preparation method of the low dielectric polyimide fiber, has the characteristics of simple preparation method, low equipment requirements, extensive sources of raw materials, and continuous spinning production, and is suitable for industrial promotion.

Description

A kind of low dielectric polyimide fiber and preparation method thereof
Technical field:
The invention belongs to functional organic fiber technical field, be specifically related to a kind of low dielectric polyimide fiber and preparation method thereof.
Background technology:
Polyimide fiber contains the imide ring of rigidity due to molecular backbone, thus has the dielectric properties of high-strength and high-modulus, high-low temperature resistant, resistance to chemical attack, radiation hardness and excellence.As a kind of high performance functionality fiber, polyimide fiber has broad application prospects, and is mainly used in the fields such as Aero-Space, war industry, ocean development and fire-fighting, microelectronics, high-temperature medium at present.Particularly in electronics industry, polyimide material can be used as the shielding protection layer of insulation dielectric layer in large scale integrated circuit or integrated circuit.In order to reduce signal transmission delay, reduce the interference between line loss and unlike signal, need to adopt the material of more low-k to reduce capacity effect or Conduction coupling, therefore prepare one of polyimide material emphasis direction becoming research with more low-k.
In order to reduce the dielectric constant of polyimide material, the dianhydride diamine monomer with higher free volume can be adopted, or F atom is incorporated in molecular backbone.But so far, the research for Kapton dielectric properties is more, and mention about the technology reducing polyimide fiber dielectric constant is also rarely seen.In view of polyimide fiber is in the important application of various fields, in order to effectively reduce the dielectric constant of polyimide fiber, F atom can be introduced in molecular backbone.But add due to F atom the bulk density and interaction force that reduce strand, thus can sacrificial fiber intrinsic mechanics and thermal property etc., this patent passes through to regulate the process conditions such as hot imidization temperature and draw ratio in fiber manufacturing process, strand is arranged more in order regular, thus the polyimide fiber simultaneously had compared with high-mechanical property and low-k can be obtained.
Summary of the invention:
The object of the invention is to prepare a kind of low dielectric polyimide fiber, it is characterized in that the dielectric constant range of described polyimide fiber is 2.55-3.3.
Present invention also offers the preparation method of described low dielectric polyimide fiber, it is characterized in that, comprise the following steps:
A: by hexafluorodianhydride (6FDA) (6FDA) and other dianhydrides, diamines, carries out proportioning by dianhydride and the total mol ratio 1: 1-1: 1.05 of diamines.
B: at N 2under protection, diamines is added in metering solvent and dissolve, then add dianhydride in batches, make the solid content of solution be 5-20wt%, fully obtain polyamic acid spinning solution after reaction.
C: polyamic acid spinning solution is carried out spinning according to wet method or dry-wet spinning technique, gained polyamic acid as-spun fibre obtains the polyimide fiber with low-dielectric energy through hot imidization and draft process.
Other dianhydrides adopted in steps A are 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA), pyromellitic acid anhydride (PMDA), 3,3 ', 4,4 '-Biphenyl Ether dianhydride (ODPA) and 3,3 ', 4, at least one in 4 '-benzophenone tetracarboxylic dianhydride (BTDA).
Other diamines adopted in steps A are p-phenylenediamine (PPD) (p-PDA), 4, and 4 '-diaminodiphenyl ether (ODA), at least one in 2-(4-aminophenyl)-5-aminobenzimidazole (BIA).
The solvent adopted in step B is DMA (DMAc), DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO) or 1-METHYLPYRROLIDONE (NMP).
The coagulating bath that spinning technique described in step C adopts is water, methyl alcohol, ethanol, ethylene glycol, acetone, toluene, N, the mixed solution of one or more in N-dimethylacetylamide (DMAc), DMF (DMF), dimethyl sulfoxide (DMSO) (DMS0), 1-METHYLPYRROLIDONE (NMP).
The hot imidization technique adopted in step C is the hot imidization technique of gradient increased temperature, and temperature range is 280-500 DEG C.
The drafting multiple of the draft process adopted in step C is more than 2 times.
Compared with prior art comparatively, the present invention has following novelty and excellent results:
1, in the polyimide fiber that the present invention prepares, due to adding of hexafluorodianhydride (6FDA) copolymerization units, effectively reduce strand bulk density and intermolecular interaction, thus obtain the low dielectric polyimide fiber that dielectric constant is less than 3.0.
2, method provided by the invention can to realize the dielectric constant of polyimide fiber adjustable by changing the means such as copolymerization system composition, solid content, coagulating bath, hot imidization temperature and draw ratio.
3, the present invention adopts two-step process to prepare polyimide fiber, and synthetic method is relatively simple, and raw material sources are extensive, are conducive to realizing suitability for industrialized production.
Accompanying drawing illustrates:
Fig. 1: the dielectric constant of PI fiber and the graph of a relation of frequency in the embodiment of the present invention 1;
Fig. 2: the dielectric loss value of PI fiber and the graph of a relation of frequency in the embodiment of the present invention 1.
Detailed description of the invention:
The monomer structure formula of the employing that following examples are used is as follows:
Hexafluorodianhydride (6FDA) (6FDA)
3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA)
Pyromellitic acid anhydride (PMDA)
3,3 ', 4,4 '-Biphenyl Ether dianhydride (ODPA)
3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride (BTDA)
P-phenylenediamine (PPD) (p-PDA)
4,4 '-diaminodiphenyl ether (ODA)
2-(4-aminophenyl)-5-aminobenzimidazole (BIA)
Embodiment 1
The synthesis of polyamic acid solution: by the mol ratio of 6FDA: p-PDA=1: 1, diamines p-PDA is placed in there-necked flask, add the solvent N of metering, N-dimethylacetylamide (DMAc), under the condition of nitrogen, carry out stirring makes it fully dissolve, then 6FDA added in batches and stir, making the solid content of solution be 10%.Under the condition of nitrogen protection, stir 3h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 1.97dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 400 DEG C carries out hot imidization, and to its applying 2.5 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 0.55GPa, and initial modulus is 20.2GPa, and its dielectric constant is 2.55 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 2
The synthesis of polyamic acid solution: by the mol ratio of BPDA: 6FDA: p-PDA=7: 3: 10, diamines p-PDA is placed in there-necked flask, add the solvent N of metering, dinethylformamide (DMF), under the condition of nitrogen, carry out stirring makes it fully dissolve, then add after BPDA and 6FDA being mixed in batches and stir, making the solid content of solution be 15%.Under the condition of nitrogen protection, stir 3h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 2.38dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 450 DEG C carries out hot imidization, and to its applying 3 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 1.24GPa, and initial modulus is 33.6GPa, and its dielectric constant is 3.12 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 3
The synthesis of polyamic acid solution: by the mol ratio of BPDA: 6FDA: p-PDA=9: 1: 10, diamines p-POA is placed in there-necked flask, add the solvent N-methyl pyrilidone (NMP) of metering, under the condition of nitrogen, carry out stirring makes it fully dissolve, then add after BPDA and 6FDA being mixed in batches and stir, making the solid content of solution be 10%.Under the condition of nitrogen protection, stir 4h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 2.53dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 420 DEG C carries out hot imidization, and to its applying 4.0 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 1.53GPa, and initial modulus is 64.3GPa, and its dielectric constant is 3.30 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 4
The synthesis of polyamic acid solution: by the mol ratio of BPDA: 6FDA: p-PDA=3: 7: 10, diamines p-PDA is placed in there-necked flask, add the solvent dimethyl sulfoxide (DMSO) (DMSO) of metering, under the condition of nitrogen, carry out stirring makes it fully dissolve, then add after BPDA and 6FDA being mixed in batches and stir, making the solid content of solution be 20%.Under the condition of nitrogen protection, stir 5h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 1.646L/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 440 DEG C carries out hot imidization, and to its applying 3.5 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 0.77GPa, and initial modulus is 38.1GPa, and its dielectric constant is 2.76 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 5
The synthesis of polyamic acid solution: by the mol ratio of PMDA: 6FDA: p-PDA: BIA=3: 7: 7: 3, diamines p-PDA and BIA is placed in there-necked flask, add the solvent N of metering, its acetamide of N-diformazan (DMAc), under the condition of nitrogen, carry out stirring makes it fully dissolve, then add after PMDA and 6FDA being mixed in batches and stir, making the solid content of solution be 5%.Under the condition of nitrogen protection, stir 7h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 1.83dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 480 DEG C carries out hot imidization, and to its applying 4.5 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 1.45GPa, and initial modulus is 54.1GPa, and its dielectric constant is 2.90 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 6
The synthesis of polyamic acid solution: by the mol ratio of BPDA: 6FDA: p-PDA: BIA: ODA=9: 1: 6: 3: 1, by diamines p-PDA, BIA and ODA is placed in there-necked flask, add the solvent N of metering, dinethylformamide (DMF), under the condition of nitrogen, carry out stirring makes it fully dissolve, and adds in batches and stirs, make the solid content of solution be 15% after then being mixed by BPDA and 6FDA.Under the condition of nitrogen protection, stir 6h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 2.03dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 500 DEG C carries out hot imidization, and to its applying 5 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 2.46GPa, and initial modulus is 82.5GPa, and its dielectric constant is 3.17 under the frequency of 100Hz, and remains on reduced levels along with the change of frequency.
Embodiment 7
The synthesis of polyamic acid solution: by the mol ratio of PMDA: 6FDA: p-PDA: BIA: ODA=6: 4: 7: 2: 1, by diamines p-PDA, BIA and ODA is placed in there-necked flask, add the solvent N-methyl pyrilidone (NMP) of metering, under the condition of nitrogen, carry out stirring makes it fully dissolve, then add after PMDA and 6FDA being mixed in batches and stir, making the solid content of solution be 8%.Under the condition of nitrogen protection, stir 8h, obtain the polyamic acid spinning solution with certain viscosity, its inherent viscosity is 2.08dL/g.
The preparation of polyamic acid fiber: polyamic acid solution is filtered froth breaking, adopts wet spinning technology to carry out spinning.
The preparation of polyimide fiber: by polyamic acid fiber successively by 280 DEG C, the hot stove of 350 DEG C and 470 DEG C carries out hot imidization, and to its applying 4 times of drawing-offs.
The TENSILE STRENGTH of gained fiber is 1.73GPa, and initial modulus is 70.4GPa, and under the frequency of 100Hz, its dielectric constant is 2.85, and remains on reduced levels along with the change of frequency.
The above-mentioned explanation of the disclosed embodiments, enables professional and technical personnel in the field realize or just uses the present invention.To be apparent for those skilled in the art to the multiple amendment of embodiment, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to embodiment illustrated herein, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (8)

1. a low dielectric polyimide fiber, is characterized in that the dielectric constant range of described polyimide fiber is 2.55-3.3.
2. the preparation method of a kind of low dielectric polyimide fiber as claimed in claim 1, is characterized in that, comprise the following steps:
A: by hexafluorodianhydride (6FDA) (6FDA) and other dianhydrides, diamines, carries out proportioning by dianhydride and the total mol ratio 1: 1-1: 1.05 of diamines;
B: at N 2under protection, diamines is added in metering solvent and dissolve, then add dianhydride in batches, make the solid content of solution be 5-20wt%, fully obtain polyamic acid spinning solution after reaction;
C: polyamic acid spinning solution is carried out spinning according to wet method or dry-wet spinning technique, gained polyamic acid as-spun fibre obtains the polyimide fiber with low-dielectric energy through hot imidization and draft process.
3. preparation method as claimed in claim 2, it is characterized in that, other dianhydrides adopted in steps A are 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA), pyromellitic acid anhydride (PMDA), 3,3 ', 4,4 '-Biphenyl Ether dianhydride (ODPA) and 3,3 ', 4, at least one in 4 '-benzophenone tetracarboxylic dianhydride (BTDA).
4. preparation method as claimed in claim 2, it is characterized in that, other diamines adopted in steps A are p-phenylenediamine (PPD) (p-PDA), 4,4 ' diaminodiphenyl ether (ODA), at least one in 2-(4-aminophenyl)-5-aminobenzimidazole (BIA).
5. preparation method as claimed in claim 2, it is characterized in that, the solvent adopted in step B is N, N-dimethylacetylamide (DMAc), DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO) or N-methyl pyrrole be alkane ketone (NMP) slightly.
6. preparation method as claimed in claim 2, it is characterized in that, the coagulating bath that spinning technique described in step C adopts is water, methyl alcohol, ethanol, ethylene glycol, acetone, toluene, N, the mixed solution of one or more in N-dimethylacetylamide (DMAc), DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO), 1-METHYLPYRROLIDONE (NMP).
7. preparation method as claimed in claim 2, it is characterized in that, the hot imidization technique adopted in step C is the hot imidization technique of gradient increased temperature, and temperature range is 280-500 DEG C.
8. preparation method as claimed in claim 2, it is characterized in that, the drafting multiple of the draft process adopted in step C is more than 2 times.
CN201510432142.XA 2015-07-16 2015-07-16 Low dielectric polyimide fiber and preparation method thereof Pending CN105019047A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510432142.XA CN105019047A (en) 2015-07-16 2015-07-16 Low dielectric polyimide fiber and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510432142.XA CN105019047A (en) 2015-07-16 2015-07-16 Low dielectric polyimide fiber and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105019047A true CN105019047A (en) 2015-11-04

Family

ID=54409329

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510432142.XA Pending CN105019047A (en) 2015-07-16 2015-07-16 Low dielectric polyimide fiber and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105019047A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106009008A (en) * 2016-04-13 2016-10-12 安徽鑫柏格电子股份有限公司 Polyimide film with low dielectric constant and preparation method thereof
CN107573842A (en) * 2016-07-04 2018-01-12 大亚电线电缆股份有限公司 The polyimide insulative coating and enamel-covered wire of low dielectric
JP2020169323A (en) * 2017-02-23 2020-10-15 旭化成株式会社 Composition, composite membrane, and membrane electrode assembly
CN109880094B (en) * 2019-03-12 2021-08-24 黄山金石木塑料科技有限公司 Antistatic/conductive polyimide resin and preparation method and application thereof
CN115819764A (en) * 2022-11-28 2023-03-21 江苏先诺新材料科技有限公司 Polyimide fiber and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4370290A (en) * 1980-05-09 1983-01-25 Ube Industries, Ltd. Process for producing aromatic polyimide filaments
CN101338462A (en) * 2008-08-20 2009-01-07 中国科学院长春应用化学研究所 Method for preparing polyimide fiber
CN101914819A (en) * 2010-07-30 2010-12-15 北京化工大学 Polyimide fiber containing quinazoline structure and preparation method thereof
CN102041576A (en) * 2010-12-03 2011-05-04 中国科学院长春应用化学研究所 Polyimide fibers and preparation method thereof
CN102766919A (en) * 2012-08-14 2012-11-07 中国科学院长春应用化学研究所 Preparation method of polyimide fibers
CN102816327A (en) * 2012-08-28 2012-12-12 常州大学 Polyimides containing ditrifluoromethyl group and unsymmetrical structure and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4370290A (en) * 1980-05-09 1983-01-25 Ube Industries, Ltd. Process for producing aromatic polyimide filaments
CN101338462A (en) * 2008-08-20 2009-01-07 中国科学院长春应用化学研究所 Method for preparing polyimide fiber
CN101914819A (en) * 2010-07-30 2010-12-15 北京化工大学 Polyimide fiber containing quinazoline structure and preparation method thereof
CN102041576A (en) * 2010-12-03 2011-05-04 中国科学院长春应用化学研究所 Polyimide fibers and preparation method thereof
CN102766919A (en) * 2012-08-14 2012-11-07 中国科学院长春应用化学研究所 Preparation method of polyimide fibers
CN102816327A (en) * 2012-08-28 2012-12-12 常州大学 Polyimides containing ditrifluoromethyl group and unsymmetrical structure and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
西鹏 等: "《高技术纤维概论》", 31 March 2012, 中国纺织出版社 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106009008A (en) * 2016-04-13 2016-10-12 安徽鑫柏格电子股份有限公司 Polyimide film with low dielectric constant and preparation method thereof
CN107573842A (en) * 2016-07-04 2018-01-12 大亚电线电缆股份有限公司 The polyimide insulative coating and enamel-covered wire of low dielectric
CN107573842B (en) * 2016-07-04 2020-05-12 大亚电线电缆股份有限公司 Low-dielectric polyimide insulating paint and enameled wire
JP2020169323A (en) * 2017-02-23 2020-10-15 旭化成株式会社 Composition, composite membrane, and membrane electrode assembly
CN109880094B (en) * 2019-03-12 2021-08-24 黄山金石木塑料科技有限公司 Antistatic/conductive polyimide resin and preparation method and application thereof
CN115819764A (en) * 2022-11-28 2023-03-21 江苏先诺新材料科技有限公司 Polyimide fiber and preparation method thereof
CN115819764B (en) * 2022-11-28 2024-01-26 江苏先诺新材料科技有限公司 Polyimide fiber and preparation method thereof

Similar Documents

Publication Publication Date Title
CN102345177B (en) High-strength high modulus polyimide fiber and preparation method thereof
CN104928790A (en) Method for preparing polyimide fibers
JP5374817B2 (en) Polyimide film and method for producing the same
CN105019047A (en) Low dielectric polyimide fiber and preparation method thereof
Liu et al. Correlation between hydrogen‐bonding interaction and mechanical properties of polyimide fibers
CN102041577B (en) Polyimide fiber and preparation method thereof
Dong et al. Synthesis of organ-soluble copolyimides by one-step polymerization and fabrication of high performance fibers
CN110540752A (en) Filler orientation-reinforced high-thermal-conductivity polyimide composite film and preparation method thereof
CN108219133A (en) A kind of polyimide resin containing furan nucleus and preparation method thereof
US20180134848A1 (en) Polyimide resin and film using same
CN113604045A (en) Thermoplastic polyimide resin composite film with low dielectric property and preparation method thereof
US20130196562A1 (en) Copolymide nano-fiber non-woven fabric, process for producing the same and the use thereof
CN111019129A (en) Low-thermal expansion coefficient soluble polyimide resin powder and preparation method thereof
JP6202554B2 (en) Polyimide resin composition made of terminal-modified imide oligomer using 2-phenyl-4,4'-diaminodiphenyl ether and aromatic thermoplastic polyimide using oxydiphthalic acid, and varnish, and heat resistance and mechanical properties Excellent molded article of polyimide resin composition, prepreg, and fiber reinforced composite material thereof
CN111087812A (en) Colorless transparent polyimide film with stable dimension and preparation method thereof
CN101914819B (en) Polyimide fiber containing quinazoline structure and preparation method thereof
Wu et al. Preparation and characterization of low CTE thermoplastic copolyimide resins based on the structural design of block sequence
JP2017201027A (en) Polyimide resin composition prepared from terminal-modified imide oligomer using 2-phenyl-4,4'-diaminodiphenylether and aromatic thermoplastic polyimide using oxydiphthalic acid, varnish, polyimide resin composition molded article excellent in heat resistance and mechanical characteristic, prepreg, and fiber-reinforced composite material of the same
Wang et al. Influences of different imidization conditions on polyimide fiber properties and structure
CN112585198B (en) Polyimide film containing crystalline polyimide resin and thermally conductive filler, and method for producing same
CN109054018B (en) Polyamide acid solution and preparation method thereof
TW201815891A (en) Method for preparing adamantane-containing polyimide having properties such as low dielectric constant, high glass transition temperature (Tg) and good processability
CN114181392B (en) High-solid-content low-viscosity polyamic acid solution and preparation method and application thereof
CN111087813A (en) Dimensionally stable polyimide film and method for producing same
KR100552131B1 (en) Aromatic polyimide composite powders with low crystallinity and method for preparing them

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20151104

RJ01 Rejection of invention patent application after publication