CN114717681A - High-temperature-resistant and flame-retardant polyamideimide-based filament and green preparation and in-situ reinforcement method thereof - Google Patents
High-temperature-resistant and flame-retardant polyamideimide-based filament and green preparation and in-situ reinforcement method thereof Download PDFInfo
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- CN114717681A CN114717681A CN202210585126.4A CN202210585126A CN114717681A CN 114717681 A CN114717681 A CN 114717681A CN 202210585126 A CN202210585126 A CN 202210585126A CN 114717681 A CN114717681 A CN 114717681A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000002787 reinforcement Effects 0.000 title claims abstract description 18
- 229920002312 polyamide-imide Polymers 0.000 title abstract description 87
- 239000004962 Polyamide-imide Substances 0.000 title abstract description 85
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 229920000642 polymer Polymers 0.000 claims abstract description 47
- 238000009987 spinning Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000015271 coagulation Effects 0.000 claims abstract description 16
- 238000005345 coagulation Methods 0.000 claims abstract description 16
- 229920005570 flexible polymer Polymers 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 238000002166 wet spinning Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 50
- 239000000835 fiber Substances 0.000 claims description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 230000009477 glass transition Effects 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 229920002635 polyurethane Polymers 0.000 claims description 9
- 239000004814 polyurethane Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- 239000004677 Nylon Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229920001778 nylon Polymers 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000007774 longterm Effects 0.000 claims 1
- 239000002657 fibrous material Substances 0.000 abstract description 12
- 238000001914 filtration Methods 0.000 abstract description 3
- 229920001971 elastomer Polymers 0.000 abstract 2
- 239000000806 elastomer Substances 0.000 abstract 2
- 239000000779 smoke Substances 0.000 description 11
- 239000004642 Polyimide Substances 0.000 description 7
- 229920001721 polyimide Polymers 0.000 description 7
- 230000001112 coagulating effect Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229920001519 homopolymer Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000003014 reinforcing effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of fiber materials, and discloses a high-temperature-resistant and flame-retardant polyamideimide-based filament and a green preparation and in-situ reinforcement method thereof. The PAI content in the filament is more than or equal to 90%, the diameter of the filament is 0.1-2 mm, and the limiting oxygen index of the filament is 40-50%; the filament is prepared in a green color in coagulation bath water by a wet spinning technology, another component of polymer is introduced as an elastomer in the spinning process, and the elastomer is heated in situ to be molten, so that the in-situ enhancement of the mechanical tensile property of the filament is realized based on the principle of 'rigid/flexible polymer network complementation'. The filament has the advantages of high temperature resistance, flame retardance, excellent mechanical properties, simple and convenient preparation method, easy operation and low cost, and has wide application prospect in the fields of high-temperature filtration, battery diaphragm, flame retardant protection and the like.
Description
Technical Field
The invention belongs to the field of new materials, relates to a high-temperature-resistant and flame-retardant polyamide-imide (PAI) based filament, and particularly relates to a green preparation and in-situ reinforcement method of the filament, in particular to a PAI filament prepared in a green way by using water as a coagulating bath and adopting a wet spinning technology, and introducing another component of polymer based on a rigid/flexible polymer network complementation principle, so that in-situ reinforcement of fiber is realized by in-situ heating, and the application prospect of the PAI filament in the fields of high-temperature filtration, battery diaphragm, flame-retardant protection and the like is expanded.
Background
Polyimide (PI) is a special engineering material, downstream products such as fibers, filaments and fabrics prepared by taking the PI as a raw material have excellent heat resistance (269 ℃ to 400 ℃), flame retardance and self-extinguishing capability, and the PI is widely applied to various fields such as transformer capacitor insulating materials, aerospace insulating materials and antistatic shielding materials used in high-temperature environments. However, PI has inherent defects of being insoluble and infusible, which causes great difficulty in subsequent processing, so that various products have high cost, and the wide application of PI in the civil field is limited.
PAI, a polymer of the same family as PI, has a glass transition temperature (250 to 300 ℃) equivalent to that of PAI, and more importantly, has good solubility, and therefore can be post-processed by a solution spinning method. The invention realizes the green preparation of the PA1 filament by using a wet spinning technology, and provides a novel textile raw material. The technologies closely related to the present invention are mainly obtained by searching for the keywords "polyamideimide & filament", "polyamideimide & wet method", "polyamideimide & fiber". In the disclosed technology, French Rona-Brown fiber company has disclosed polyamideimide filament and its wet preparation technology in "CN 1041406A polyamideimide filament and its method for production and processing" in 1990, but the patent focuses on the evaluation of filament mechanical properties, and does not relate to its flame retardant property, and the method related to the patent adopts spinning of binary or ternary coagulation bath, does not meet the development requirement of green and environment-friendly production, and the filament obtained in the technology needs to be washed with water, but the invention adopts water as coagulation bath, and is green and environment-friendly, does not need to be washed with water, and has low cost. In patent CN103757721A one-step wet spinning process of polyamide-imide fiber, PAI fiber is prepared through two coagulating baths containing toxic and harmful chemical reagents. The above technology is essentially different from the materials and preparation method of the patent.
Disclosure of Invention
The invention aims to provide a novel high-temperature-resistant and flame-retardant filament, which supplements high-performance materials for the fields of high-temperature filtration, battery diaphragm and flame-retardant protection, and discloses a green preparation and mechanical property in-situ enhancement method based on a wet spinning technology.
The invention provides a high-temperature-resistant flame-retardant polyamide-imide-based filament, which consists of PAI and another polymer with a low melting point (less than or equal to 240 ℃).
As a preferred technical scheme:
the PAI-based filament with high temperature resistance and flame retardance mainly comprises PAI, wherein the PAI accounts for more than or equal to 90 wt%, the polymer is in a powdery or liquid state, the molecular weight of the polymer is 5000-800000, and the polymer is in a block type or homopolymerization type.
The high-temperature-resistant and flame-retardant PAI-based filament has a smooth surface, a cylindrical section and a diameter of 0.1-2 mm.
A high temperature resistant, flame retardant PAI-based filament as described above, said PAI being capable of acting as a rigid polymer network due to the presence of benzene rings, the remainder of the incorporated components acting as a flexible polymer network, having a melting temperature below the glass transition temperature (250 ℃) of the PAI, and being capable of being polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate, and the like.
The PAI-based filament yarn with high temperature resistance and flame retardance can be used for a long time at 220 ℃, has the characteristics of self-extinguishing after leaving fire, no smoke generation and no molten drop, and has the limiting oxygen index of 40-50%.
The high-temperature-resistant and flame-retardant PAI-based filament has the advantages that the mechanical tensile strength of the material is 20-200 MPa, and the elongation at break is 5-30%.
The invention also provides a green preparation and in-situ reinforcement method of the high-temperature-resistant and flame-retardant PAI-based filament, which comprises the steps of preparing a mixed solution of PAI and another component of polymer, forming hybrid nascent fiber by using a wet spinning technology and taking water as a coagulating bath through synchronous spinning, and realizing the improvement of the mechanical property of the fiber through in-situ heating at a receiving roller.
As a preferred technical scheme:
in the green preparation method of the PAI-based filament with high temperature resistance and flame retardance, the other component polymer can be polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate and the like, and the solvent can be one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone and tetrahydrofuran.
In the green preparation method of the PAI-based filament with high temperature resistance and flame retardance, the coagulating bath is water, and can be deionized water, distilled water, mineral water, tap water and the like.
The in-situ reinforcing method of the high-temperature-resistant and flame-retardant PAI-based filament has the advantages that the concentration of the spinning solution is 20-40 wt%, and the spinning speed is 5-20 m/min.
According to the in-situ reinforcing method for the high-temperature-resistant and flame-retardant PAI-based filament, the temperature-controllable receiving roller is used for in-situ heating, the heating temperature is adjustable within the range of 150-240 ℃, the heating time is 1-10 hours, and the mechanical properties of the filament before and after heating can be enhanced by 1-3 times.
Advantageous effects
The high-temperature-resistant and flame-retardant polyamide-imide-based filament disclosed by the invention has the advantages of raw materials and technology, is low in raw material cost and easy to dissolve, so that the high-temperature-resistant and flame-retardant polyamide-imide-based filament is easy to process and form high polymers and resists flame and high temperature; the processing technology is green coagulating bath wet spinning, meets the development requirement of ecological environmental protection, and has mature industrialization equipment in the prior art, so the material provided by the invention has important significance for developing green industrial textiles.
The in-situ reinforcing method of the high-temperature-resistant and flame-retardant polyamideimide-based filament provided by the invention has the advantages of simple and convenient operation and strong expansibility, and can provide technical reference for mechanical reinforcement of the filament or fiber material
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber is PAI, 91% by weight, the polymer is in the form of powder with a molecular weight of 10000 and is of the homopolymer type; the filament has smooth surface, cylindrical section and 0.2mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and polyurethane is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 43 percent; the mechanical tensile strength is 50MPa, and the elongation at break is 10%.
Example 2
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber is PAI in a weight proportion of 93%, the polymer is in the form of a liquid with a molecular weight of 50000 and is of the segmented type; the filament has smooth surface, cylindrical section and 0.4mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and nylon is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃) of the PAI. In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 44%; the mechanical tensile strength is 100MPa, and the elongation at break is 12%.
Example 3
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber is PAI, in 92% by weight, the polymer is in powder form, has a molecular weight of 60000, and is of the block type; the filament has smooth surface, cylindrical section and 0.4mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 45%; the mechanical tensile strength is 80MPa, and the elongation at break is 8%.
Example 4
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber is PAI, the weight proportion is 94%, the polymer form is liquid, its molecular weight is 70000, the kind is homopolymerization type; the filament has smooth surface, cylindrical section and 0.8mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl formal is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 45%; the mechanical tensile strength is 150MPa, and the elongation at break is 13%.
Example 5
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber is PAI in 95% by weight, the polymer is in the form of powder with a molecular weight of 80000 and is of the homopolymer type; the filament has smooth surface, cylindrical section and 0.4mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and the polyvinyl butyral is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 43 percent; the mechanical tensile strength is 130MPa, and the elongation at break is 18%.
Example 6
In this example, a high temperature resistant, flame retardant PAI-based filament, the fiber comprises PAI as the major component in a proportion of 94% by weight, and the polymer is in the form of a liquid having a molecular weight of 90000 and is of the block type; the filament has smooth surface, cylindrical section and 0.8mm diameter; the PAI can be used as a rigid polymer network due to the benzene ring, and polymethyl methacrylate is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 46%; the mechanical tensile strength is 105MPa, and the elongation at break is 21%.
Example 7
In this example, a PAI-based filament with high temperature resistance and flame retardancy, the main component of the fiber is PAI with a weight proportion of 96%, the polymer is in the form of powder with a molecular weight of 500000 and is of a homopolymer type; the filament has smooth surface, cylindrical section and diameter of 1 mm; the PAI can be used as a rigid polymer network due to the benzene ring, and the polyvinyl butyral is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 44%; the mechanical tensile strength is 87MPa, and the elongation at break is 15%.
Example 8
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber was PAI in a 94% by weight ratio, the polymer was in liquid form, had a molecular weight of 600000 and was of the block type; the filament has smooth surface, cylindrical section and diameter of 1.2 mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyurethane is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 45%; the mechanical tensile strength is 113MPa, and the elongation at break is 18 percent.
Example 9
In this example, a high temperature resistant, flame retardant PAI-based filament, the major component of the fiber was PAI in a weight ratio of 93%, the polymer was in the form of powder with a molecular weight of 700000 and was of the homopolymer type; the filament has smooth surface, cylindrical section and diameter of 1.4 mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after leaving fire, no smoke and no molten drop, and the limited oxygen index is 43 percent; the mechanical tensile strength is 84MPa, and the elongation at break is 15%.
Example 10
In this example, a PAI-based filament resistant to high temperature and flame, the main component of the fiber is PAI, 95% by weight, the polymer is in liquid form, its molecular weight is 800000, and the type is homopolymerization type; the filament has smooth surface, cylindrical section and diameter of 1.8 mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced to be used as a flexible polymer network, and the melting temperature of the PAI is lower than the glass transition temperature (250 ℃). In addition, the fiber material can be used for a long time at 220 ℃, and has the characteristics of self-extinguishing after fire, no smoke generation and no molten drop, and the limit oxygen index is 46%; the mechanical tensile strength is 111MPa, and the elongation at break is 19%.
Example 11
In this example, a one-step green process for preparing and in-situ reinforcing a high temperature resistant, flame retardant PAI-based filament, the other component polymer was nylon, the solvent was N, N-dimethylformamide, the spinning solution was 20 wt%, and the coagulation bath was deionized water; the spinning speed is 5m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 200 ℃, the heating time is 2 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 1.2 times.
Example 12
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyvinyl alcohol, the solvent was N-methylpyrrolidone, the spinning solution was 30 wt%, and the coagulation bath was mineral water; the spinning speed is 8m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 180 ℃, the heating time is 3 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 2 times.
Example 13
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyvinyl butyral, the solvent was tetrahydrofuran, the spinning solution had a concentration of 31 weight percent, and the coagulation bath was distilled water; the spinning speed is 7m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 190 ℃, the heating time is 2 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 1.5 times.
Example 14
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyurethane, the solvent was N, N-dimethylformamide, the spinning solution was 25 wt%, and the coagulation bath was deionized water; the spinning speed is 12m/min, the in-situ heating is carried out by utilizing a temperature-controllable receiving roller, the heating temperature is 210 ℃, the heating time is 3 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 2 times.
Example 15
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the additional component polymer was polyvinyl alcohol, the solvent was N, N-dimethylacetamide, the spinning solution was 32 wt%, and the coagulation bath was distilled water; the spinning speed is 14m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 180 ℃, the heating time is 2 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 1.8 times.
Example 16
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyurethane, the solvent was N, N-dimethylformamide, the spinning solution was 34 wt%, and the coagulation bath was deionized water; the spinning speed is 17m/min, the in-situ heating is carried out by utilizing a temperature-controllable receiving roller, the heating temperature is 190 ℃, the heating time is 5 hours, and the mechanical property of the filaments before and after the heating can be enhanced by 2.8 times.
Example 17
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polymethylmethacrylate, the solvent was tetrahydrofuran, the concentration of the spinning solution was 34 wt%, and the coagulation bath was tap water; the spinning speed is 15m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 180 ℃, the heating time is 4 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 1.5 times.
Example 18
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyvinyl formal, the solvent was N-methyl pyrrolidone, the spinning solution was 23 wt%, and the coagulation bath was tap water; the spinning speed is 9m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 220 ℃, the heating time is 3 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 3 times.
Example 19
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyvinyl formal, the solvent was N-methyl pyrrolidone, the spinning solution was 25 wt%, and the coagulation bath was mineral water; the spinning speed is 13m/min, the in-situ heating is carried out by utilizing a temperature-controllable receiving roller, the heating temperature is 210 ℃, the heating time is 2 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 2 times.
Example 20
In this example, a one-step green process for the preparation and in-situ reinforcement of high temperature resistant, flame retardant PAI-based filaments, the other component polymer was polyurethane, the solvent was N, N-dimethylformamide, the spinning solution was 28 wt%, and the coagulation bath was mineral water; the spinning speed is 13m/min, the in-situ heating is carried out by using a temperature-controllable receiving roller, the heating temperature is 170 ℃, the heating time is 5 hours, and the mechanical properties of the filaments before and after the heating can be enhanced by 2 times.
Claims (10)
1. The high-temperature-resistant and flame-retardant PAI-based filament is characterized in that the main component of the material is PAI, the weight proportion of the PAI is more than or equal to 90%, the polymer is in a powdery or liquid state, the molecular weight of the polymer is 5000-800000, and the polymer is in a block type or a homopolymerization type.
2. The high-temperature-resistant and flame-retardant PAI-based filament is characterized in that the surface of the filament is smooth, the cross section of the filament is cylindrical, and the diameter of the filament is 0.1-2 mm.
3. A high temperature resistant, flame retardant PAI-based filament as claimed in claim 1 wherein the PAI is a rigid polymer network due to its benzene ring and the remaining components are incorporated as a flexible polymer network having a melting temperature below the glass transition temperature (250 ℃) of PAI, which can be polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate, etc.
4. A high temperature resistant, flame retardant PAI based filament as in claim 1 wherein the material is capable of long term use below 220 ℃ and has self-extinguishing, non-fuming, non-dripping characteristics from fire, limiting oxygen index of 30-50%.
5. A high temperature resistant, flame retardant PAI based filament as claimed in claim 1 wherein the material has a mechanical tensile strength of 20 to 200MPa and an elongation at break of 5 to 30%.
6. A green manufacturing method of PAI-based filament with high temperature resistance and flame retardance as claimed in claim 1, wherein the PAI, the other component polymer and the solvent are mixed to prepare a mixed solution, and then the mixed solution is extruded into the coagulation bath by using water as the coagulation bath by using the wet spinning technology to obtain the hybrid nascent fiber.
7. A process for preparing high temperature resistant, flame retardant PAI based filaments in green form as claimed in claim 6, wherein the other component polymer is selected from polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate, etc., and the solvent is selected from one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, tetrahydrofuran.
8. A process for the green production of high temperature resistant, flame retardant PAI based filaments as claimed in claim 6 wherein the coagulation bath is water, such as deionized water, distilled water, mineral water, tap water, etc.
9. The in-situ reinforcement method for PAI-based filament with high temperature resistance and flame retardance as claimed in claim 1, wherein the concentration of the spinning solution is 20-40 wt% and the spinning speed is 5-20 m/min.
10. The in-situ reinforcement method of the PAI-based filament yarn with high temperature resistance and flame retardance as claimed in claim 1, wherein a temperature-controllable receiving roller is used for in-situ heating, the heating temperature is adjustable within the range of 150-240 ℃, the heating time is 1-10 hours, and the mechanical property of the filament yarn before and after heating can be enhanced by 1-3 times.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT296488B (en) * | 1968-06-04 | 1972-02-10 | Rhodiaceta | Process for the production of threads and fibers from polyamide-imides |
| CN101619502A (en) * | 2009-07-29 | 2010-01-06 | 东华大学 | Method for preparing polyamide-imide fiber |
| CN103757721A (en) * | 2014-01-20 | 2014-04-30 | 江苏巨贤合成材料有限公司 | Polyamide-imide fiber wet one-step spinning process |
| CN113073397A (en) * | 2021-03-16 | 2021-07-06 | 株洲时代新材料科技股份有限公司 | Aromatic fiber spinning solution, aromatic fiber and preparation method thereof |
| CN113832558A (en) * | 2021-09-24 | 2021-12-24 | 天津工业大学 | Polyamide-imide crimped nanofiber with electret effect and preparation method thereof |
-
2022
- 2022-05-27 CN CN202210585126.4A patent/CN114717681B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT296488B (en) * | 1968-06-04 | 1972-02-10 | Rhodiaceta | Process for the production of threads and fibers from polyamide-imides |
| CN101619502A (en) * | 2009-07-29 | 2010-01-06 | 东华大学 | Method for preparing polyamide-imide fiber |
| CN103757721A (en) * | 2014-01-20 | 2014-04-30 | 江苏巨贤合成材料有限公司 | Polyamide-imide fiber wet one-step spinning process |
| CN113073397A (en) * | 2021-03-16 | 2021-07-06 | 株洲时代新材料科技股份有限公司 | Aromatic fiber spinning solution, aromatic fiber and preparation method thereof |
| CN113832558A (en) * | 2021-09-24 | 2021-12-24 | 天津工业大学 | Polyamide-imide crimped nanofiber with electret effect and preparation method thereof |
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