CN103710779B - Method for improving alkali resistance of polyimide fiber - Google Patents
Method for improving alkali resistance of polyimide fiber Download PDFInfo
- Publication number
- CN103710779B CN103710779B CN201310548886.9A CN201310548886A CN103710779B CN 103710779 B CN103710779 B CN 103710779B CN 201310548886 A CN201310548886 A CN 201310548886A CN 103710779 B CN103710779 B CN 103710779B
- Authority
- CN
- China
- Prior art keywords
- fiber
- polyimide fiber
- fibers
- alkali
- acquisition
- 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.)
- Active
Links
Landscapes
- Artificial Filaments (AREA)
Abstract
The invention provides a method for improving the alkali resistance of a polyimide fiber. The polyimide fiber is prepared mainly as follows: adding one or two of two monomers of 2-(4-amino phenyl)-5-amino benzimidazole or 2-(4-amino benzene)-6-amino-4(3 H)-quinazolinone for copolymerization with other aromatic diamine and aromatic dianhydride for synthesis so that the alkali resistance of the polyimide fiber can be improved. The environment-resistant performances (especially the alkali-resistant performance) of the polyimide fiber prepared by adding the two monomers of 2-(4-amino phenyl)-5-amino benzimidazole or 2-(4-amino benzene)-6-amino-4(3 H)-quinazolinone in acidic environment influences, alkaline environment influences, organic solvent environment influences, uv (ultraviolet) irradiation influences and other aspects are greatly improved. The alkali resistance of the polyimide fiber is improved through the method, the tolerance of the polyimide fiber under the complex environments can be improved, and the polyimide fiber has the characteristics of high preparation efficiency, low energy consumption and the like and can be used for large-scale industrial production.
Description
Technical field
A kind of method for improving polyimide fiber alkali resistance, mainly using addition 2- (4- aminophenyls) -5- amino
Any one in -4 (3H)-quinazolinone both monomers of benzimidazole or 2- (4- amido benzene) -6- amidos or two kinds
Polyimide fiber is prepared with other aromatic diamines and aromatic dianhydride copolymerization, to improve the alkaline-resisting of polyimide fiber
Performance, by adding -4 (3H)-quinoline azoles of 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -6- amidos
Polyimide fiber prepared by quinoline ketone both monomers, affects in sour environment, alkaline environment affects, organic solvent environment shadow
The environmental resistance of the aspects such as sound, ultra-vioket radiation impact is substantially improved, especially alkaline resistance properties.Polyamides is improved with this kind of method sub-
The alkaline resistance properties of amine fiber, can increase toleration of the polyimide fiber under complex environment.The present invention belongs to polyimides
Technical field of fiber preparation.
Background technology
As the representative of high-performance fiber, polyimides (PI) fiber not only have high-strength and high-modulus the characteristics of, also have concurrently resistance to
The multiple characteristic such as high/low temperature, radiation hardness, fire-retardant, shows good combination property, especially in practical application complicated and changeable
Under environment, competitive advantage is obvious.
(1) thermal stability
In general, full aromatic polyimide fiber starts the temperature decomposed at 500 DEG C or so.By p-phenylenediamine and biphenyl
Polyimide fiber prepared by dianhydride, the temperature for starting to decompose can reach 600 DEG C, be thermally-stabilised in high molecular polymer so far
One of property highest kind.Industrialized P84 fibers, environment life-time service that can be at 260 DEG C.
(2) radiation-resistant property
The radiation-resistant property of polyimide fiber is excellent, and experiment shows, after 80-100 DEG C of ultraviolet light 24h, gathers
Imide fiber can keep 90% intensity, and the intensity of Kevlar fibers only keeps 20%.Through 1 × 1010The fast electronics of rad
After irradiation, polyimide fiber still can keep 90% strength character, table of the other types of fiber in radiation resistance
Existing aspect is then incomparable, therefore in the application aspect of aerospace field, polyimide material is one of first-selected material, together
When be also radioactive substance and high-temperature medium filtering material.
(3) low temperature resistant energy
Polyimide fiber in -269 DEG C of liquid helium still will not embrittlement, possess fabulous resistance to low temperature, therefore can answer
In the investigation test of low temperature environment.
(4) good dielectric properties
The dielectric constant of common aromatic polyimide fibre material is typically 3.4 or so, and the polyamides of fluorine-containing system
Imine fiber its dielectric constant can drop to 2.5 or so, and dielectric loss is 10-3The order of magnitude, 100~300KV/mm of dielectric strength, body
Product resistivity is 1017Ω·cm.Remain to keep in these performances broad range from low temperature to high temperature and from low to high compared with
High level.
(5) other performance
Polyimide fiber has good biocompatibility, is self-extinguishing, limited oxygen index be 38-50% it
Between, with relatively low smoke rate.Thermal coefficient of expansion is little, is 10-5~10-7/ DEG C the order of magnitude, is in same order of magnitude water with metal
It is flat.In addition, it is comparatively stable to organic solvent, with relatively low water absorption rate.
With reference to above advantage, polyimide fiber can be made into non-woven fabrics, be applied to high temperature, radioactivity, organic gas and
The aspects such as the drainage screen of liquid, fire insulation blanket, are that temperature highest filtering material is used under special environment.The P84 of commercialization at present
Fiber has been made into filter bag, non-woven fabrics etc., in terms of being widely applied to industrial dust removal by filtration, and has good
Using effect.But the P84 fibers of commercialization and most of polyimide fiber alkali resistance environmental effect performance are weaker.
The present invention is using addition -4 (3H)-quinoline azoles of 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -6- amidos
Any one or two kinds in quinoline ketone both monomers are prepared with other aromatic diamines and aromatic dianhydride copolymerization
Polyimide fiber, -4 (3H)-quinoline azoles of 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -6- amidos
The addition of any one or two kinds in quinoline ketone both monomers, can improve intermolecular interaction, especially improve
Intermolecular Hyarogen-bonding, the reinforcement of intermolecular force improve the resistance to environmental effect performance of polyimide fiber, especially
Which is alkali resistance environmental effect performance.
The content of the invention
It is an object of the invention to solve the deficiencies in the prior art, and provide a kind of raising polyimide fiber alkaline resistance properties
Method, its production process is simple, low production cost, from initial polyamic acid (PAA) solution to last polyamides
Imine fiber, pilot process are continuously finished, and without being interrupted, production efficiency efficiently, can be directly used for industrial mass production.
The present invention is a kind of method for improving polyimide fiber alkaline resistance properties, mainly using addition 2- (4- aminobenzenes
Base) it is any one in -4 (3H)-quinazolinone both monomers of -5- aminobenzimidazoles or 2- (4- amido benzene) -6- amidos
Kind or two kinds with other aromatic diamines and aromatic dianhydride copolymerization preparation polyimide fibers, this fiber compared to
On market commonly use P84 series polyimide fibers, sour environment affect, alkaline environment affect, organic solvent environment affect,
The environmental resistance of the aspects such as ultra-vioket radiation impact is substantially improved, especially alkaline resistance properties.
For achieving the above object, technical scheme is as follows:
A kind of method for improving polyimide fiber alkaline resistance properties, it is characterised in that addition 2- (4- aminophenyls) -5- ammonia
Any one in -4 (3H)-quinazolinone both monomers of base benzimidazole or 2- (4- amido benzene) -6- amidos or two
Plant the polyimide fiber prepared with other aromatic diamines and aromatic dianhydride copolymerization.
A kind of method for improving polyimide fiber alkaline resistance properties, it is characterised in that 2- (4- aminophenyls) -5- aminobenzenes
And the molar content in diamidogen of imidazoles or 2- (4- amido benzene) -4 (3H)-quinazolinone of -6- amidos is 0.1%-
Between 99.9%.
A kind of method for improving polyimide fiber alkaline resistance properties, it is characterised in that addition 2- (4- aminophenyls) -5- ammonia
Any one in -4 (3H)-quinazolinone both monomers of base benzimidazole or 2- (4- amido benzene) -6- amidos or two
Kind with polyamic acid (PAA) solution that other aromatic diamines and aromatic dianhydride copolymerization solid content are 3%-40%, mistake
After filter evacuation bubble removing, using any one spinning work in dry-spinning process, wet spinning technology or dry-jet wet spinning process
Skill carries out spinning and obtains alkali-resistant polyimide fiber.
A kind of method for improving polyimide fiber alkaline resistance properties, it is characterised in that compared to the P84 systems commonly used on market
Row polyimide fiber, using addition 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -6- amidos -4
(3H) any one or two kinds in-quinazolinone both monomers and other aromatic diamines and aromatic dianhydride combined polymerization
Into prepare alkali-resistant polyimide fiber sour environment affect, alkaline environment affect, organic solvent environment affect, it is ultraviolet
The environmental resistance of the aspects such as irradiation impact is substantially improved, especially alkaline resistance properties.
Compared with prior art, the present invention has following advantage:
By adding 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -4 (3H)-quinoline of -6- amidos
Any one or two kinds in oxazoline ketone both monomers are prepared with other aromatic diamines and aromatic dianhydride copolymerization
Polyimide fiber, 2- (4- aminophenyls) -5- aminobenzimidazoles or 2- (4- amido benzene) -4 (3H)-quinoline of -6- amidos
The addition of any one or two kinds of monomers in oxazoline ketone both monomers, can improve intermolecular interaction, especially
It is to improve intermolecular Hyarogen-bonding, the reinforcement of intermolecular force improves the resistance to environmental effect of polyimide fiber
Performance, compared with P84 polyimide fibers common on market, the alkali resistance environment shadow of polyimide fiber prepared by the present invention
Ring performance to be greatly improved.
Description of the drawings
Fig. 1:2- (4- aminophenyls) -5- aminobenzimidazoles (BIA), -4 (3H)-quinoline azoles of 2- (4- amido benzene) -6- amidos
Quinoline ketone (AAQ) monomer chemistries structural formula;
Fig. 2:Equal phthalate anhydride/4,4 '-diaminodiphenyl ether/2- (4- aminophenyls) -5- aminobenzimidazole systems
Alkali-resistant polyimide fiber and P84 fibers etch the contrast of different time alkaline resistance properties at normal temperatures in 5wt%NaOH solution;
Fig. 3:Equal phthalate anhydride/4,4 '-diaminodiphenyl ether/2- (4- aminophenyls) -5- aminobenzimidazole systems
Alkali-resistant polyimide fiber and P84 fibers etch 10 hours in 5wt%NaOH solution at normal temperatures after surface SEM photograph,
a:P84 fibers, b:Alkali-resistant polyimide fiber;
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment the invention will be further described, but the invention is not restricted to following examples.
Embodiment 1
A:Using pyromellitic acid anhydride and 4,4 '-diaminodiphenyl ether and 2- (4- aminophenyls) -5- amino benzos
Polyamic acid (PAA) solution of the imidazoles synthesis solid content for 10wt%, 2- (4- aminophenyls) -5- aminobenzimidazoles are in diamidogen
In molar content be 5%, filter evacuation bubble removing after, spinning is carried out using wet spinning technology and alkali resistance polyamides is obtained
Imine fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention is as shown in Figure 2.After alkali-resistant polyimide fiber is etched 10 hours in 5wt%NaOH solution with P84 fibers
Surface SEM photograph it is as shown in Figure 3.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
Embodiment 2
A:Using pyromellitic acid anhydride and 4,4 '-diaminodiphenyl ether and 2- (4- amido benzene) -6- amidos -4 (3H) -
Polyamic acid (PAA) solution of the quinazolinone synthesis solid content for 15wt%, -4 (3H)-quinoline azoles of 2- (4- amido benzene) -6- amidos
Molar content of the quinoline ketone in diamidogen is 10%, after filtering evacuation bubble removing, carries out spinning using wet spinning technology and obtains
Obtain alkali-resistant polyimide fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
Embodiment 3
A:Using 3,3 ', 4,4 '-two methyl phenyl ethers anisole tetracarboxylic dianhydrides (ODPA) and 4,4 '-diaminodiphenyl ether and 2- (4- ammonia
Base phenyl) -5- aminobenzimidazoles and -4 (3H)-quinazolinone of 2- (4- amido benzene) -6- amidos synthesis solid content be 20wt%
Polyamic acid (PAA) solution, 2- (4- aminophenyls) -5- aminobenzimidazoles and 2- (4- amido benzene) -6- amidos -4 (3H) -
Molar content of the quinazolinone in diamidogen is respectively 8%, after filtering evacuation bubble removing, is spun using dry-spinning process
Silk simultaneously obtains alkali-resistant polyimide fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
Embodiment 4
A:Using 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride (BTDA)/4,4 '-diaminodiphenyl ether and 2- (4- amidos
Benzene) -4 (3H)-quinazolinone of -6- amidos synthesis solid content for 25wt% polyamic acid (PAA) solution, 2- (4- amido benzene) -
Molar content of -4 (the 3H)-quinazolinone of 6- amidos in diamidogen is 20%, after filtering evacuation bubble removing, using dry spinning
Technique carries out spinning and obtains alkali-resistant polyimide fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
Embodiment 5
A:Using 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA)/p-phenylenediamine (pPDA) and 2- (4- aminobenzenes
Base) -5- aminobenzimidazoles synthesis solid content for 30wt% polyamic acid (PAA) solution, 2- (4- aminophenyls) -5- amino
Molar content of the benzimidazole in diamidogen is 50%, after filtering evacuation bubble removing, is carried out using dry-jet wet-spinning spinning technique
Spinning simultaneously obtains alkali-resistant polyimide fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
Embodiment 6
A:Using pyromellitic acid anhydride, 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride and diaminodiphenyl ether and 2- (4-
Amido benzene) -4 (3H)-quinazolinone of -6- amidos synthesis solid content for 35wt% polyamic acid (PAA) solution, 2- (4- amidos
Benzene) molar content of -4 (the 3H)-quinazolinone of -6- amidos in diamidogen be 80%, after filtering evacuation bubble removing, using dry spray
Wet spinning spinning technique carries out spinning and obtains alkali-resistant polyimide fiber;
B:The alkali-resistant polyimide fiber of acquisition adds the NaOH of the 5wt% under room temperature molten with the P84 fibers of commercialization
After 10h being soaked in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fracture of the fiber of acquisition
Strength retention.
C:The alkali-resistant polyimide fiber of acquisition adds the H of the 20wt% under room temperature with the P84 fibers of commercialization2SO4It is molten
After soaking 120 hours in liquid, both fibers cleaned, be dried and tested with the mechanical property of fiber, the fiber of acquisition
Rupture strength retention.
D:The alkali-resistant polyimide fiber of acquisition is divided to two groups with the P84 fibers of commercialization, is separately added under room temperature
The HNO of 10wt%3The HNO of 5wt% at solution and 95 DEG C3After soaking 120 hours in solution, this two groups of fibers are carried out cleaning,
It is dried and tests the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
E:The alkali-resistant polyimide fiber of acquisition divides three groups with the P84 fibers of commercialization, the N being separately added under room temperature,
After soaking 840 hours in N- dimethyl acetylamide (DMAc), acetone, three kinds of organic solvents of toluene, this three groups of fibers are carried out clearly
Wash, be dried and test the mechanical property of fiber, the rupture strength retention of the fiber of acquisition.
F:The alkali-resistant polyimide fiber of acquisition and the P84 fibers of commercialization, are exposed to intensity for 16mw/cm2Purple
Radiation resistance experiment is carried out under outer illumination, irradiation time is 160 hours.The mechanical property of test fiber, the fiber of acquisition
Rupture strength retention.
In above-described embodiment 1-6,2- (4- aminophenyls) -5- aminobenzimidazoles (BIA), 2- (4- amido benzene) -6- amine
- 4 (3H)-quinazolinone (AAQ) monomer chemistries structural formula such as Fig. 1 of base;Equal phthalate anhydride/4,4 '-diaminodiphenyl ether/2-
5wt%NaOH is molten at normal temperatures with P84 fibers for (4- aminophenyls) -5- aminobenzimidazole system alkali-resistant polyimide fibers
Fig. 2 is shown in the contrast that different time alkaline resistance properties is etched in liquid;Equal phthalate anhydride/4,4 '-diaminodiphenyl ether/2- (4- amino
Phenyl) -5- aminobenzimidazole system alkali-resistant polyimide fibers and P84 fibers carved in 5wt%NaOH solution at normal temperatures
Surface SEM photograph after losing 10 hours is shown in Fig. 3.
In above-described embodiment 1-6, the environmental resistance such as table of various system alkali-resistant polyimide fibers and P84 fibers
Shown in 1.
The environmental resistance contrast of various system alkali-resistant polyimide fibers and P84 fibers in 1 embodiment 1-6 of table
(rupture strength retention)
Claims (1)
1. it is a kind of improve polyimide fiber alkaline resistance properties method, it is characterised in that adopt 3,3 ', 4,4 '-two methyl phenyl ethers anisole tetracids
Dianhydride (ODPA) and 4,4 '-diaminodiphenyl ether and 2- (4- aminophenyls) -5- aminobenzimidazoles and 2- (4- aminobenzenes) -
Polyamic acid (PAA) solution of -4 (3H)-quinazolinone of 6- amino synthesis solid content for 20wt%, 2- (4- aminophenyls) -5-
The molar content of aminobenzimidazole and -4 (3H)-quinazolinone of 2- (4- aminobenzenes) -6- amino in diamidogen is respectively 8%,
After filtering evacuation bubble removing, prepared using dry-spinning process, obtain alkali-resistant polyimide fiber.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310548886.9A CN103710779B (en) | 2013-11-01 | 2013-11-01 | Method for improving alkali resistance of polyimide fiber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310548886.9A CN103710779B (en) | 2013-11-01 | 2013-11-01 | Method for improving alkali resistance of polyimide fiber |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103710779A CN103710779A (en) | 2014-04-09 |
CN103710779B true CN103710779B (en) | 2017-04-12 |
Family
ID=50404114
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310548886.9A Active CN103710779B (en) | 2013-11-01 | 2013-11-01 | Method for improving alkali resistance of polyimide fiber |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103710779B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018155598A1 (en) * | 2017-02-23 | 2018-08-30 | 旭化成株式会社 | Composition, composite film and membrane electrode assembly |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101200822A (en) * | 2007-11-30 | 2008-06-18 | 四川大学 | Polyimide fibre containing benzimidazole structure and preparation method thereof |
CN101914819A (en) * | 2010-07-30 | 2010-12-15 | 北京化工大学 | Polyimide fiber containing quinazoline structure and preparation method thereof |
CN101921483A (en) * | 2010-09-07 | 2010-12-22 | 东华大学 | Polybenzimidazole imide membrane and preparation method thereof |
CN102191581A (en) * | 2011-03-28 | 2011-09-21 | 中国科学院长春应用化学研究所 | Polyimide fiber and preparation method thereof |
CN102345177A (en) * | 2011-08-04 | 2012-02-08 | 北京化工大学 | High-strength high modulus polyimide fiber and preparation method thereof |
CN102558860A (en) * | 2011-12-22 | 2012-07-11 | 桂林电器科学研究院 | Dimensionally-stable polyimide film and preparation method thereof |
JP2012207147A (en) * | 2011-03-30 | 2012-10-25 | Ube Industries Ltd | Method for producing polyimide film, polyimide film, and polyimide metal laminate using the same |
-
2013
- 2013-11-01 CN CN201310548886.9A patent/CN103710779B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101200822A (en) * | 2007-11-30 | 2008-06-18 | 四川大学 | Polyimide fibre containing benzimidazole structure and preparation method thereof |
CN101914819A (en) * | 2010-07-30 | 2010-12-15 | 北京化工大学 | Polyimide fiber containing quinazoline structure and preparation method thereof |
CN101921483A (en) * | 2010-09-07 | 2010-12-22 | 东华大学 | Polybenzimidazole imide membrane and preparation method thereof |
CN102191581A (en) * | 2011-03-28 | 2011-09-21 | 中国科学院长春应用化学研究所 | Polyimide fiber and preparation method thereof |
JP2012207147A (en) * | 2011-03-30 | 2012-10-25 | Ube Industries Ltd | Method for producing polyimide film, polyimide film, and polyimide metal laminate using the same |
CN102345177A (en) * | 2011-08-04 | 2012-02-08 | 北京化工大学 | High-strength high modulus polyimide fiber and preparation method thereof |
CN102558860A (en) * | 2011-12-22 | 2012-07-11 | 桂林电器科学研究院 | Dimensionally-stable polyimide film and preparation method thereof |
Non-Patent Citations (4)
Title |
---|
《Structure and Properties of Novel PMDA/ODA/PABZ Polyimide Fibers》;Guanqun Gao,Liang Dong,Xiangyang Liu,Guangdou Ye,Yi Gu;《Polymer Engineering and Science》;20081231;第912-917页 * |
《聚酰亚胺纤维的制备与应用研究进展》;陈英韬;《高分子通报》;20131031(第10期);第71-79页 * |
张国慧.《轶纶®聚酰亚胺短纤维耐化学性研究》.《高科技纤维与应用》.2012,第37卷(第4期),第25-34及40页. * |
杨军杰.《轶纶®聚酰亚胺短纤维的性能及其应用》.《高科技纤维与应用》.2012,第37卷(第3期),第57-60页. * |
Also Published As
Publication number | Publication date |
---|---|
CN103710779A (en) | 2014-04-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110105570B (en) | Polyimide material with high heat resistance and low thermal expansion coefficient and preparation method thereof | |
CN102766270B (en) | Polyimide nano-fiber membrane with crosslinked structure and preparation thereof | |
CN102218871B (en) | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof | |
CN103696033B (en) | A kind of preparation method of polyimide fiber | |
CN113403707A (en) | Polyimide aerogel fiber and preparation method thereof | |
CN106012107B (en) | A kind of preparation method of carbon aerogels fiber | |
CN102560707B (en) | Polyimide fiber with kidney-shaped section and preparation method thereof | |
CN105040276A (en) | Polyimide fibrous membrane with crosslinking morphology and preparation method thereof | |
CN108085872A (en) | A kind of high-temperature resistant sound absorption tunica fibrosa and preparation method | |
CN105019141A (en) | Polyimide nanofiber flocculus, preparation method and application thereof | |
CN111394892A (en) | Polyimide nanofiber membrane coaxially coated with nano zirconium dioxide inorganic layer and preparation method thereof | |
CN108003375A (en) | Preparation method of polyimide diaphragm of high air penetrability and products thereof | |
CN108755144B (en) | Preparation method of crosslinked polyimide fiber membrane | |
Yan et al. | A high-performance aromatic co-polyimide fiber: structure and property relationship during gradient thermal annealing | |
CN102817112B (en) | Preparation method of activated carbon fibers | |
CN102383217B (en) | Polyimide fiber and preparation method thereof | |
CN103710779B (en) | Method for improving alkali resistance of polyimide fiber | |
CN104178837A (en) | Porous polyimide fiber and preparation method thereof | |
CN109293978B (en) | High-porosity polyimide aerogel and normal-pressure drying preparation method thereof | |
CN109853135B (en) | Polybenzimidazole coated polyimide nanofiber core-shell structure nanofiber membrane and preparation method thereof | |
CN113818097B (en) | Polyimide fiber and method for preparing polyimide fiber | |
KR20110072006A (en) | Nano web and method for manufacturing the same | |
Yuan et al. | High performance electrospun polynaphthalimide nanofibrous membranes with excellent resistance to chemically harsh conditions | |
KR102266753B1 (en) | Polyimide based carbon fiber with excellent flexibility and manufacturing method thereof | |
CN103046427A (en) | Method for preparing aromatic polyamide fiber paper base material by electrospinning technology |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
DD01 | Delivery of document by public notice |
Addressee: Chen Jinmei Document name: Notification of Acceptance of Request for Reexamination |
|
GR01 | Patent grant | ||
GR01 | Patent grant |