CN107675288B - Polyimide ultrashort fiber and preparation method thereof - Google Patents
Polyimide ultrashort fiber and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
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Abstract
The invention discloses a polyimide ultrashort fiber and a preparation method thereof, relates to the field of fiber preparation, and can realize batch preparation of polyimide fiber products with nanometer fiber diameters and micron fiber lengths. The fiber length of the polyimide ultrashort fiber is 2-500 mu m, the fiber diameter is 0.1-50 mu m, and the specific surface area is 2-30 m2(ii) in terms of/g. By utilizing the physicochemical characteristics of the fibers at different heat treatment temperatures in the preparation process of the polyimide fibers, the dispersion and ultrashort of the fibers can be more easily realized by adopting a physical mechanical method under the state that the polyimide fibers are not completely imidized, then the complete imidization of the polyimide fibers can be realized by high-temperature treatment, and finally the ultrashort fibers of the polyimide can be obtained by adopting the mechanical crushing, grinding and screening methods again. The ultra-short polyimide fiber obtained by the preparation method has the characteristics of high and low temperature resistance, ultraviolet radiation resistance, good insulativity and the like, and can be used for preparing slurry coating liquid, strengthening resin, rubber and the like, pulp and the like.
Description
Technical Field
The invention relates to the technical field of fiber preparation, in particular to a polyimide ultrashort fiber and a preparation method thereof.
Background
Polyimide fibers are organic fibers with higher use temperature at present, and are superior to other high-performance fibers (such as aramid fibers and polyphenylene sulfide fibers) in the aspects of heat resistance, aging resistance, oxidation resistance, ultraviolet resistance, water absorption and the like, so the polyimide fibers are widely applied in the fields of environmental protection, aerospace, special and high-temperature heat insulation, civil textiles and the like. The ultrashort polyimide fiber not only has the excellent performance of the polyimide fiber, but also is made into slurry coating liquid, or used as filler for adding modification such as resin, rubber and the like, or used as special paper pulp material and the like, thereby greatly expanding the application field of the polyimide fiber.
At present, the preparation of the polyimide fiber into the ultra-short polyimide fiber with the diameter ranging from nanometer to micrometer and the length ranging from micrometer has great technical difficulty. Due to the mechanical and temperature-resistant properties of polyimide fibers, only chopped fibers having a length of 500 μm or more can be obtained by mechanical cutting. The polyimide pulp obtained by the papermaking pulping method or the precipitated polyimide fibrid obtained by the high-speed shearing precipitation dispersion method can realize the micron-sized fiber diameter, but the shortest fiber length is only 100 mu m; although polyimide fibers with diameters on the order of nanometers can be obtained by electrospinning, they are often in the form of non-woven fabrics, rather than chopped fibers. Particularly, the batch preparation of polyimide fiber products with nanometer fiber diameter and micron fiber length has not been reported.
Disclosure of Invention
The invention provides a preparation method of polyimide ultrashort fibers, which aims to prepare polyimide fiber products with nanometer fiber diameters and micron fiber lengths in batches.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the polyimide ultrashort fiber has the fiber length of 2-500 mu m, the fiber diameter of 0.1-50 mu m and the specific surface area of 2-30 m2/g。
The invention also provides a preparation method of the polyimide ultrashort fiber, which comprises the following steps:
step one, diamine and anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid non-woven fabric with the fiber diameter of nano-scale or micron-scale is obtained through an electrostatic spinning method or a solution spraying method; or, diamine and acid anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid continuous fiber with the fiber diameter of micron level is obtained by a dry method, a wet method or a dry-jet wet spinning method;
step two, performing high-temperature treatment on the product obtained in the step one, and controlling the treatment temperature and the treatment time to ensure that the product obtained in the step one is not completely imidized, wherein the treatment temperature is 160-220 ℃, and the treatment time is 5-20 min;
step three, mechanical crushing
Mechanically crushing the polyamide acid non-woven fabric subjected to high-temperature treatment to obtain uniform sheet-shaped distribution with the area of 0.5-2 cm2A/piece; mechanically crushing the polyamide acid continuous fiber subjected to high-temperature treatment to obtain short cut fibers, wherein the length of the short cut fibers is 3-6 mm;
step four, preparing slurry by using the product obtained in the step three, a solvent and a dispersing agent, wherein the concentration of the obtained slurry is 1-30%, and carrying out fluffing and fibrillation treatment after uniform stirring;
fifthly, concentrating and cleaning the slurry subjected to dispersion and defibering treatment, filtering out a solvent, and drying at 50-110 ℃ to obtain blocky or cake-shaped fiber flocculation aggregates;
step six, mechanically crushing the blocky or caky fiber floc aggregates to obtain granular or segmented fiber floc aggregates;
seventhly, performing high-temperature imidization treatment on the product obtained in the sixth step at the temperature of 260-450 ℃ to obtain granular or segmented polyimide fiber floc aggregates;
and step eight, performing hammer milling, ball milling or sand milling on the product obtained in the step seven, and screening by using different meshes to obtain the polyimide ultrashort fibers.
As a preferred embodiment, in step one, the polar solvent is selected from: one or more of Dimethylformamide (DMF), dimethylacetamide (DMAc), N-dimethylpyrrolidone (NMP), dimethylsulfoxide (DMso), and Tetrahydrofuran (THF).
As a preferred embodiment, in step one, the diamine is selected from: 4,4 '-diaminodiphenyl ether (ODA), p-phenylenediamine (PPD), 1, 4-bis (4-aminophenoxy) benzene (APB), 4' -bis (4-aminophenoxy) biphenyl (BAPB), 2 '-bis [4- (4-aminophenoxy) phenyl ] propane (BAPP), 3' -dimethyl-4, 4 '-diaminodiphenylmethane (DMMDA), 4' -diaminodiphenylmethane (MDA), 4 '-diaminodiphenylsulfone (DDS), 2' -bis (trifluoromethyl) -4,4 '-diaminobiphenyl (TFDB), 2' -bis [4- (4-aminophenoxy) phenyl ] Hexafluoropropane (HFBAPP).
In a preferred embodiment, in step one, the anhydride monomer is selected from: one or more of pyromellitic dianhydride (PMDA), biphenyl dianhydride (BPDA), benzophenone dianhydride (BTDA), diphenyl ether dianhydride (ODPA), triphenyldiether dianhydride (HQDPA), diphenyl sulfide dianhydride (TDPA), hexafluoro dianhydride (6FDA), Phthalic Anhydride (PA) and methyl tetrahydrophthalic anhydride (MTHPA).
In a preferred embodiment, in the first step, the molar ratio of the diamine to the anhydride monomer is: (0.95-1): 1.
In a preferred embodiment, the temperature in the second step is preferably 190 to 220 ℃.
In a preferred embodiment, in step four, the solvent is one or more selected from deionized water, ethanol, acetone and butanone.
In a preferred embodiment, in step four, the dispersant is one or more selected from polyethylene oxide (PEO), sodium hexametaphosphate and sodium polyacrylate.
In a preferred embodiment, in the seventh step, the temperature is preferably 320 to 360 ℃.
The invention has the beneficial effects that:
the invention utilizes the physical and chemical properties of the fibers at different heat treatment temperatures in the preparation process of the polyimide fibers, and the dispersion and ultrashort of the fibers are more easily realized by adopting a physical mechanical method under the state that the polyimide fibers are not completely imidized, then the complete imidization is realized by high-temperature treatment, and finally the ultrashort fibers of the polyimide are obtained by adopting the methods of mechanical crushing, grinding and screening again. The invention is suitable for batch production.
The ultra-short polyimide fiber obtained by the preparation method has the characteristics of high and low temperature resistance, ultraviolet irradiation resistance, good insulativity and the like, the fiber length is 2-500 mu m, the fiber diameter is 0.1-50 mu m, and the specific surface area is 2-30 m2The product can be used for preparing slurry coating liquid, strengthening resin and rubber, pulp and the like.
Detailed Description
According to the ultra-short polyimide fiber, a non-woven fabric which is not completely imidized and has a fiber diameter of a nanometer level or a micron level is obtained by adopting a conventional electrostatic spinning method or a conventional solution spraying method at present, or a continuous fiber which is not completely imidized and has a fiber diameter of a micron level is obtained by a dry method, a wet method or a dry-jet wet spinning method; then obtaining flocculent pulp through treatments of defibering, devillicating and the like, concentrating, cleaning, drying at low temperature, crushing, then carrying out high-temperature imidization treatment, finally carrying out hammer milling, ball milling or sand milling treatment on the fully imidized aggregate, and obtaining the fiber with the length of 2-500 mu m, the fiber diameter of 0.1-50 mu m and the specific surface area of 2-30 m through screening with different meshes2Ultra-short polyimide fiber in g.
The preparation method of the polyimide ultrashort fiber is realized by the following steps:
step one, diamine and anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid non-woven fabric with the fiber diameter of nano-scale or micron-scale is obtained through an electrostatic spinning method or a solution spraying method; or, diamine and acid anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid continuous fiber with the fiber diameter of micron level is obtained by a dry method, a wet method or a dry-jet wet spinning method; the molar ratio of diamine to anhydride monomer is: (0.95-1): 1.
Preferably, the polar solvent is selected from: one or more of Dimethylformamide (DMF), dimethylacetamide (DMAc), N-dimethylpyrrolidone (NMP), dimethylsulfoxide (DMso), and Tetrahydrofuran (THF).
Preferably, the diamine is selected from: 4,4 '-diaminodiphenyl ether (ODA), p-phenylenediamine (PPD), 1, 4-bis (4-aminophenoxy) benzene (APB), 4' -bis (4-aminophenoxy) biphenyl (BAPB), 2 '-bis [4- (4-aminophenoxy) phenyl ] propane (BAPP), 3' -dimethyl-4, 4 '-diaminodiphenylmethane (DMMDA), 4' -diaminodiphenylmethane (MDA), 4 '-diaminodiphenylsulfone (DDS), 2' -bis (trifluoromethyl) -4,4 '-diaminobiphenyl (TFDB), 2' -bis [4- (4-aminophenoxy) phenyl ] Hexafluoropropane (HFBAPP).
Preferably, the anhydride monomer is selected from: one or more of pyromellitic dianhydride (PMDA), biphenyl dianhydride (BPDA), benzophenone dianhydride (BTDA), diphenyl ether dianhydride (ODPA), triphenyldiether dianhydride (HQDPA), diphenyl sulfide dianhydride (TDPA), hexafluoro dianhydride (6FDA), Phthalic Anhydride (PA) and methyl tetrahydrophthalic anhydride (MTHPA).
And step two, in order to ensure that the material obtained in the step one is not completely imidized, performing high-temperature treatment on the product obtained in the step one, wherein the treatment temperature is 160-220 ℃, and the treatment time is 5-20 min.
Step three, mechanical crushing
Mechanically crushing the non-woven fabric subjected to high-temperature treatment to obtain uniform flaky distribution with the area of 0.5-2 cm2A/piece; and mechanically crushing the continuous fiber subjected to high-temperature treatment to obtain short cut fiber, wherein the length of the short cut fiber is 3-6 mm.
And step four, preparing slurry by using the product obtained in the step three, a solvent and a dispersing agent, wherein the concentration of the obtained slurry is 1-30%, and uniformly stirring the prepared slurry, and then defibering and brooming the slurry by using a defibering machine, a disc mill or a colloid mill.
Preferably, the solvent used is selected from one or more of deionized water, ethanol, acetone and butanone.
Preferably, the dispersant used is selected from one or more of polyethylene oxide (PEO), sodium hexametaphosphate, and sodium polyacrylate salt.
And step five, concentrating and cleaning the slurry subjected to dispersion and defibering treatment, filtering out a solvent, and drying at 50-110 ℃ to obtain blocky or cake-shaped fiber floc aggregates.
And step six, mechanically crushing the blocky or caky fiber floc aggregates to obtain granular or segmented fiber floc aggregates with different sizes.
And seventhly, performing high-temperature imidization treatment on the product obtained in the sixth step at the temperature of 260-450 ℃ to obtain granular or segmented polyimide fiber floc aggregates.
And step eight, performing hammer milling, ball milling or sand milling on the product obtained in the step seven, and screening by using different meshes to obtain the polyimide ultrashort fibers.
The present invention will be described in further detail with reference to examples.
Example 1
1mol of ODA, 0.8mol of PMDA, 0.18mol of HQDPA and 0.04mol of phthalic anhydride react in DMAc to generate polyamic acid solution; the solution is processed by electrostatic spinning method to obtain polyamic acid non-woven fabric, and then is processed for 10min at 200 ℃ to obtain non-woven fabric with fiber diameter of about 0.5 mu m and without complete imidization. The non-woven fabric is mechanically crushed into uniform flaky distribution, slurry is prepared, the concentration of the slurry is 1%, the solvent is deionized water and ethanol, and the dispersant is sodium polyacrylate. And uniformly stirring the prepared slurry, repeatedly treating the slurry by a fluffer, concentrating, cleaning, filtering a solvent, and drying at 90 ℃ to obtain the massive fiber flocculation aggregates. The agglomerate is mechanically crushed and imidized at 320 deg.c to form polyimide block fiber agglomerate. Then the polyimide agglomerate is processed by hammer milling, and is sieved by different meshes to obtain the ultra-short polyimide fiber with the fiber diameter of 0.45-0.55 mu m and the fiber length of 10-15 mu m, and the specific surface area is 19-21 m through testing2/g。
Example 2
1mol of ODA, 0.7mol of PMDA and 0.3mol of BPDA react in NMP to generate polyamic acid solution; the solution is processed by a wet spinning method to obtain polyamic acid fiber, and then the polyamic acid fiber is processed for 20min at 190 ℃ to obtain fiber with the diameter of about 15 mu m and without complete imidization. The fiber is chopped, the chopped strand length is 4mm, slurry is prepared, the concentration of the slurry is 15%, the solvent is deionized water and butanone, and the dispersant is PEO. And uniformly stirring the prepared slurry, repeatedly treating the slurry by using a disc mill, concentrating, cleaning, filtering out a solvent, and drying at 110 ℃ to obtain the cake-shaped fibrous floccule. The agglomerate is mechanically crushed and imidized at 360 deg.c to form granular polyimide fiber agglomerate. Then ball milling the polyimide aggregate, sieving with different mesh numbers to obtain the ultra-short polyimide fiber with the fiber length of 70-80 mu m and the fiber diameter of 14-16 mu m, and testing the specific surface area of 11-13 m2/g。
Example 3
1mol of PPD, 0.8mol of ODPA, 0.04mol of MTHPA and 0.18mol of TDPA react in a mixture of THF and DMso to generate polyamic acid solution; the solution is processed by an electrostatic spinning method to obtain polyamic acid non-woven fabric, and then the polyamic acid non-woven fabric is processed for 10min at 220 ℃ to obtain the non-woven fabric with the fiber diameter of about 1 mu m and without complete imidization. The non-woven fabric is mechanically crushed into uniform flaky distribution, slurry is prepared, the concentration of the slurry is 30%, the solvent is deionized water and ethanol, and the dispersant is sodium polyacrylate. And uniformly stirring the prepared slurry, repeatedly treating the slurry by a fluffer, concentrating, cleaning, filtering a solvent, and drying at 50 ℃ to obtain the massive fiber flocculation aggregates. The agglomerate is mechanically crushed and imidized at 450 deg.c to form polyimide block fiber agglomerate. Then the polyimide agglomerate is processed by hammer milling, and is sieved by different meshes to obtain the ultra-short polyimide fiber with the fiber diameter of 0.9-1.2 mu m and the fiber length of 45-50 mu m, and the specific surface area is 15-17 m through testing2/g。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of polyimide ultrashort fibers is characterized by comprising the following steps:
step one, diamine and anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid non-woven fabric with the fiber diameter of nano-scale or micron-scale is obtained through an electrostatic spinning method or a solution spraying method; or, diamine and acid anhydride monomers react in a polar solvent to generate polyamic acid, and the polyamic acid continuous fiber with the fiber diameter of micron level is obtained by a dry method, a wet method or a dry-jet wet spinning method;
step two, performing high-temperature treatment on the product obtained in the step one, and controlling the treatment temperature and the treatment time to ensure that the product obtained in the step one is not completely imidized, wherein the treatment temperature is 160-220 ℃, and the treatment time is 5-20 min;
step three, mechanical crushing
Mechanically crushing the polyamide acid non-woven fabric subjected to high-temperature treatment to obtain uniform sheet-shaped distribution with the area of 0.5-2 cm2A/piece; mechanically crushing the polyamide acid continuous fiber subjected to high-temperature treatment to obtain short cut fibers, wherein the length of the short cut fibers is 3-6 mm;
step four, preparing slurry by using the product obtained in the step three, a solvent and a dispersing agent, wherein the concentration of the obtained slurry is 1-30%, and carrying out fluffing and fibrillation treatment after uniform stirring;
fifthly, concentrating and cleaning the slurry subjected to dispersion and defibering treatment, filtering out a solvent, and drying at 50-110 ℃ to obtain blocky or cake-shaped fiber flocculation aggregates;
step six, mechanically crushing the blocky or caky fiber floc aggregates to obtain granular or segmented fiber floc aggregates;
seventhly, performing high-temperature imidization treatment on the product obtained in the sixth step at the temperature of 260-450 ℃ to obtain granular or segmented polyimide fiber floc aggregates;
step eight, performing hammer milling, ball milling or sand milling treatment on the product obtained in the step seven, and screening by using different meshes to obtain the polyimide ultrashort fibers;
the polyimide ultra-short fiber has the fiber length of 2-500 mu m, the fiber diameter of 0.1-50 mu m and the specific surface area of 2-30 m2/g。
2. The method as claimed in claim 1, wherein in step one, the polar solvent is selected from: one or more of dimethylformamide, dimethylacetamide, N-dimethylpyrrolidone, dimethyl sulfoxide and tetrahydrofuran.
3. The method as claimed in claim 1, wherein in step one, the diamine is selected from the group consisting of: 4,4' -diaminodiphenyl ether, p-phenylenediamine, 1, 4-bis (4-aminophenoxy) benzene, 4' -bis (4-aminophenoxy) biphenyl, 2' -bis [4- (4-aminophenoxy) phenyl ] propane, 3' -dimethyl-4, 4' -diaminodiphenylmethane, 4' -diaminodiphenylsulfone, 2' -bis trifluoromethyl-4, 4' -diaminobiphenyl, 2' -bis [4- (4-aminophenoxy) phenyl ] hexafluoropropane.
4. The method as claimed in claim 1, wherein in step one, the acid anhydride monomer is selected from: one or more of pyromellitic dianhydride, biphenyl dianhydride, benzophenone dianhydride, diphenyl ether dianhydride, triphenyl diether dianhydride, diphenyl sulfide dianhydride, hexafluoro dianhydride, phthalic anhydride and methyl tetrahydrophthalic anhydride.
5. The method for preparing ultrashort polyimide fiber as claimed in claim 1, wherein in the first step, the molar ratio of diamine to anhydride monomer is: (0.95-1): 1.
6. The method for preparing ultrashort polyimide fiber as claimed in claim 1, wherein the temperature in the second step is 190-220 ℃.
7. The method for preparing ultrashort polyimide fiber as claimed in claim 1, wherein in step four, the solvent is selected from one or more of deionized water, ethanol, acetone and butanone.
8. The method for preparing ultra-short polyimide fiber as claimed in claim 1, wherein in step four, the dispersant is selected from one or more of polyethylene oxide, sodium hexametaphosphate and sodium polyacrylate.
9. The method for preparing ultra-short polyimide fiber as claimed in claim 1, wherein in the seventh step, the temperature is 320-360 ℃.
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| CN109293978B (en) * | 2018-09-29 | 2021-06-04 | 长春高琦聚酰亚胺材料有限公司 | High-porosity polyimide aerogel and normal-pressure drying preparation method thereof |
| CN109608989A (en) * | 2018-12-17 | 2019-04-12 | 福州皇家地坪有限公司 | Superhard color inhibition epoxy flooring coating |
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| CN109734909B (en) * | 2019-01-16 | 2021-07-16 | 江苏先诺新材料科技有限公司 | Polyimide powder and preparation method thereof |
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| CN110106635B (en) * | 2019-05-21 | 2020-07-14 | 江西先材纳米纤维科技有限公司 | Ultrashort electro-spinning polyimide nanofiber and preparation method thereof |
| CN110528272B (en) * | 2019-09-16 | 2021-09-17 | 武汉纺织大学 | Polyimide fiber fibrillation treatment method |
| CN111501125B (en) * | 2020-04-29 | 2021-05-18 | 中国地质大学（北京） | High-whiteness polyimide superfine fiber and preparation method and application thereof |
| CN111961203B (en) * | 2020-08-11 | 2022-03-04 | 江苏奥神新材料股份有限公司 | Preparation method of modified polyimide pulp |
| CN112724402B (en) * | 2021-01-07 | 2022-03-11 | 安徽农业大学 | Extremely cold temperature resistant biomass functional polyamide and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009228190A (en) * | 2008-03-25 | 2009-10-08 | Kaneka Corp | Polyimide fiber, its utilization, and method for producing the fiber |
| CN104928790A (en) * | 2015-06-08 | 2015-09-23 | 北京化工大学 | Method for preparing polyimide fibers |
| CN105220262A (en) * | 2015-08-24 | 2016-01-06 | 江苏先诺新材料科技有限公司 | A kind of polyimides (PI) pulp and preparation method thereof |
| CN105504810A (en) * | 2016-01-07 | 2016-04-20 | 江苏先诺新材料科技有限公司 | Method for preparing high-intensity and high-modulus polyimide-fiber-reinforced polyimide sheet through continuous forming |
| CN107034542A (en) * | 2017-04-20 | 2017-08-11 | 北京化工大学 | A kind of method that three-step approach mixing imidization prepares polyimide fiber |
-
2017
- 2017-10-19 CN CN201710975625.3A patent/CN107675288B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009228190A (en) * | 2008-03-25 | 2009-10-08 | Kaneka Corp | Polyimide fiber, its utilization, and method for producing the fiber |
| CN104928790A (en) * | 2015-06-08 | 2015-09-23 | 北京化工大学 | Method for preparing polyimide fibers |
| CN105220262A (en) * | 2015-08-24 | 2016-01-06 | 江苏先诺新材料科技有限公司 | A kind of polyimides (PI) pulp and preparation method thereof |
| CN105504810A (en) * | 2016-01-07 | 2016-04-20 | 江苏先诺新材料科技有限公司 | Method for preparing high-intensity and high-modulus polyimide-fiber-reinforced polyimide sheet through continuous forming |
| CN107034542A (en) * | 2017-04-20 | 2017-08-11 | 北京化工大学 | A kind of method that three-step approach mixing imidization prepares polyimide fiber |
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