CN114717681B - High-temperature-resistant flame-retardant polyamide-imide filament and green preparation and in-situ enhancement method thereof - Google Patents

High-temperature-resistant flame-retardant polyamide-imide filament and green preparation and in-situ enhancement method thereof Download PDF

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CN114717681B
CN114717681B CN202210585126.4A CN202210585126A CN114717681B CN 114717681 B CN114717681 B CN 114717681B CN 202210585126 A CN202210585126 A CN 202210585126A CN 114717681 B CN114717681 B CN 114717681B
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temperature
imide
polyamide
filament
pai
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CN114717681A (en
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李玉瑶
华乐珍
季泽楷
崔旺
吴峥
刘雍
范杰
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Nantong Bolian Material Technology Co ltd
Tianjin Polytechnic University
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Nantong Bolian Material Technology Co ltd
Tianjin Polytechnic University
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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
    • 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

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  • 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 flame-retardant polyamide-imide filament and a green preparation and in-situ reinforcement method thereof. The PAI proportion in the filament is more than or equal to 90%, the diameter is 0.1-2 mm, and the limiting oxygen index is 40-50%; the filaments are prepared in a green way in coagulating bath water by a wet spinning technology, another component polymer is introduced as an elastomer in the spinning process, and the elastomer is melted by in-situ heating, so that in-situ enhancement of mechanical stretching performance of the filaments 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 property, 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 retardance protection and the like.

Description

High-temperature-resistant flame-retardant polyamide-imide filament and green preparation and in-situ enhancement method thereof
Technical Field
The invention belongs to the field of new materials, and relates to a high-temperature-resistant flame-retardant polyamide imide (PAI) base filament, in particular to a green preparation and in-situ reinforcement method of the filament, which is characterized in that water is used as a coagulating bath, a wet spinning technology is adopted to prepare the PAI filament, another component polymer is introduced based on a 'rigid/flexible polymer network complementation' principle, in-situ reinforcement of fibers is realized through in-situ heating, and the application prospect of the fiber in the fields of high-temperature filtration, battery diaphragms, flame-retardant protection and the like is expanded.
Background
Polyimide (PI) is a special engineering material, and downstream products such as fibers, filaments, fabrics and the like prepared by taking the Polyimide (PI) as a raw material have excellent heat resistance (-269 ℃ to 400 ℃), flame retardance and self-extinguishing capability, and are widely applied to various fields such as insulating materials of transformers and capacitors, insulating materials of aerospace, antistatic shielding materials used in high-temperature environments and the like. However, PI has inherent defects of difficult and infusible properties, resulting in great difficulty in post-processing, and thus, various products have high cost, which limits its wide application in civil fields.
As a polymer of the same family as PI, PAI has a glass transition temperature (250 to 300 ℃ C.) comparable to that of PAI, and more importantly, it has a good solubility, so that it can be post-processed by a solution spinning method. The invention realizes the green preparation of PA1 filaments by using a wet spinning technology, and provides a novel textile raw material. The technology closely related to the present invention is mainly obtained by searching for the keywords "polyamideimide & filament", "polyamideimide & wet", "polyamideimide & fiber". Among the disclosed technologies, french Rona-Brookfield fiber company in 1990 discloses polyamide-imide filaments and wet preparation technology thereof in CN 1041406A polyamide-imide filaments and methods for producing and processing the same, but the patent focuses on the evaluation of the mechanical properties of the filaments, the flame retardant property of the filaments is not involved, the method involved in the patent adopts binary or ternary coagulation bath spinning, the development requirement of green environment-friendly production is not met, the filaments obtained in the technology need water washing, and the invention adopts water as the coagulation bath, thus being green and environment-friendly, and having no need of water washing and low cost. The PAI fiber in the patent CN103757721A, a polyamide-imide fiber wet one-step spinning process, is prepared by two coagulating baths, and the coagulating baths contain toxic and harmful chemical reagents. The above technology is essentially different from the material and the preparation method of the patent.
Disclosure of Invention
The invention aims to provide a novel high-temperature-resistant flame-retardant filament, which supplements high-performance materials for the fields of high-temperature filtration, battery diaphragms and flame-retardant protection, and discloses a green preparation and mechanical property in-situ enhancement method based on a wet spinning technology.
The present invention provides a high temperature resistant, flame retardant polyamideimide-based filament comprised of PAI and another polymer having a low melting point (.ltoreq.240 ℃).
As a preferable technical scheme:
the high-temperature-resistant flame-retardant PAI-based filament is characterized in that the main component of the material is PAI, the weight ratio is more than or equal to 90%, the polymer is in a powder form and a liquid form, the molecular weight is 5000-800000, and the types are block type or homo-polymerization type.
The high-temperature-resistant flame-retardant PAI-based filament is smooth in surface, cylindrical in section and 0.1-2 mm in diameter.
The PAI can be used as a rigid polymer network due to the fact that the PAI has a benzene ring, the other components are used as a flexible polymer network, the melting temperature of the PAI is lower than the glass transition temperature (250 ℃) of the PAI, and the PAI can be polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate and the like.
The high-temperature-resistant flame-retardant PAI-based filament is long-term use at 220 ℃, has the characteristics of self-extinguishment from fire, no fuming and no melting drop, and has a limiting oxygen index of 40-50%.
The high-temperature-resistant flame-retardant PAI-based filament has the mechanical tensile strength of 20-200 MPa and the elongation at break of 5-30%.
The invention also provides a green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament, which is used for preparing a mixed solution of PAI and another component polymer, forming hybrid nascent fibers after synchronous spinning by using water as a coagulating bath by utilizing a wet spinning technology, and realizing the improvement of the mechanical properties of the fibers by in-situ heating at a receiving roller.
As a preferable technical scheme:
the green preparation method of the high-temperature-resistant flame-retardant PAI-based filament comprises the step of preparing the other polymer component from polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polymethyl methacrylate and the like, wherein the solvent can be one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone and tetrahydrofuran.
The green preparation method of the high-temperature-resistant flame-retardant PAI-based filament is characterized in that 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 flame-retardant PAI-based filament comprises the steps of enabling the concentration of the spinning solution to be 20-40 wt% and enabling the spinning speed to be 5-20 m/min.
According to the in-situ reinforcing method for the high-temperature-resistant flame-retardant PAI-based filaments, the controllable temperature receiving roller is utilized for in-situ heating, the heating temperature is adjustable within the range of 150-240 ℃, the heating time is 1-10 h, and the mechanical properties of the filaments before and after heating can be reinforced by 1-3 times.
Advantageous effects
The high-temperature-resistant flame-retardant polyamide-imide-based filament has the advantages of raw materials and technology, and the raw materials are low in cost and easy to dissolve, so that the high-molecular processing and forming are easy, and the flame-retardant and high-temperature-resistant effects are realized; the processing technology is green coagulation bath wet spinning, meets the development requirement of ecological environment protection, and has mature industrialized equipment in the prior art, so the material provided by the invention has important significance for developing textiles for green industry.
The in-situ reinforcing method of the high-temperature-resistant flame-retardant polyamide-imide filament provided by the invention has the advantages of simple operation and strong expansibility, and can provide a technical reference for mechanical reinforcement of filaments or fiber materials
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Example 1
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI (polyamide) and 91% by weight, wherein the polymer is in a powdery form, has a molecular weight of 10000 and is of a homo-polymerization type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.2mm; the PAI can be used as a rigid polymer network due to the benzene ring, polyurethane is introduced as a flexible polymer network, and the melting temperature 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 43%; the mechanical tensile strength is 50MPa, and the elongation at break is 10%.
Example 2
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI with the weight proportion of 93 percent, and the polymer is in a liquid state, has the molecular weight of 50000 and is in a block type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.4mm; the PAI can be used as a rigid polymer network due to the benzene ring, nylon is introduced as a flexible polymer network, and the melting temperature 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 44%; the mechanical tensile strength is 100MPa, and the elongation at break is 12%.
Example 3
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main component of PAI with the weight ratio of 92%, and the polymer is in a powdery form, has the molecular weight of 60000 and is in a block type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.4mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 45%; the mechanical tensile strength is 80MPa, and the elongation at break is 8%.
Example 4
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI with the weight proportion of 94%, and the polymer is in a liquid state, has the molecular weight of 70000 and is of a homo-polymerization type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.8mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl formal is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 45%; the mechanical tensile strength is 150MPa, and the elongation at break is 13%.
Example 5
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises PAI as a main component and 95% by weight of the fiber, wherein the polymer is in a powdery form, has a molecular weight of 80000 and is of a homo-type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.4mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl butyral is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 43%; the mechanical tensile strength is 130MPa, and the elongation at break is 18%.
Example 6
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI with the weight proportion of 94%, and the polymer is in a liquid state, has the molecular weight of 90000 and is in a block type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.8mm; the PAI can be used as a rigid polymer network due to the benzene ring, polymethyl methacrylate is introduced as a flexible polymer network, and the melting temperature 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 46%; the mechanical tensile strength is 105MPa, and the elongation at break is 21%.
Example 7
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI in a weight ratio of 96%, and the polymer is in a powdery form, has a molecular weight of 500000 and is of a homo-type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 1mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl butyral is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 44%; the mechanical tensile strength is 87MPa, and the elongation at break is 15%.
Example 8
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI with the weight proportion of 94%, and the polymer is in a liquid state, has the molecular weight of 600000 and is in a block type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 1.2mm; the PAI can be used as a rigid polymer network due to the benzene ring, polyurethane is introduced as a flexible polymer network, and the melting temperature 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 45%; the mechanical tensile strength is 113MPa, and the elongation at break is 18%.
Example 9
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI in a weight ratio of 93%, and the polymer is in a powdery form, has a molecular weight of 700000 and is of a homo-type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 1.4mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 43%; the mechanical tensile strength is 84MPa, and the elongation at break is 15%.
Example 10
In the embodiment, the high-temperature-resistant flame-retardant PAI-based filament comprises the main components of PAI in a weight ratio of 95%, and the polymer is in a liquid state, has a molecular weight of 800000 and is of a homo-type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 1.8mm; the PAI can be used as a rigid polymer network due to the benzene ring, and polyvinyl alcohol is introduced 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 ℃, has the characteristics of self-extinguishing after leaving fire, no fuming and no melting drop, and has a limiting oxygen index of 46%; the mechanical tensile strength is 111MPa, and the elongation at break is 19%.
Example 11
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer as the other component is nylon, the solvent is N, N-dimethylformamide, the concentration of the spinning solution is 20wt%, and the coagulating bath is deionized water; the spinning speed is 5m/min, the temperature of the spinning is 200 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 2h, and the mechanical properties of filaments before and after heating can be enhanced by 1.2 times.
Example 12
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer as the other component is polyvinyl alcohol, the solvent is N-methyl pyrrolidone, the concentration of the spinning solution is 30wt%, and the coagulating bath is mineral water; the spinning speed is 8m/min, the temperature of the spinning is 180 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 3h, and the mechanical properties of filaments before and after heating can be enhanced by 2 times.
Example 13
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament is characterized in that the polymer of the other component is polyvinyl butyral, the solvent is tetrahydrofuran, the concentration of the spinning solution is 31wt%, and the coagulating bath is distilled water; the spinning speed is 7m/min, the temperature of the spinning is 190 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 2h, and the mechanical properties of filaments before and after heating can be enhanced by 1.5 times.
Example 14
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer serving as the other component is polyurethane, the solvent is N, N-dimethylformamide, the concentration of the spinning solution is 25wt%, and the coagulating bath is deionized water; the spinning speed is 12m/min, the temperature of the spinning is 210 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 3h, and the mechanical properties of filaments before and after heating can be enhanced by 2 times.
Example 15
In the embodiment, the one-step green preparation and in-situ reinforcement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer serving as the other component is polyvinyl alcohol, the solvent is N, N-dimethylacetamide, the concentration of the spinning solution is 32 weight percent, and the coagulating bath is distilled water; the spinning speed is 14m/min, the temperature of the spinning is 180 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 2h, and the mechanical properties of filaments before and after heating can be enhanced by 1.8 times.
Example 16
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer serving as the other component is polyurethane, the solvent is N, N-dimethylformamide, the concentration of the spinning solution is 34 weight percent, and the coagulating bath is deionized water; the spinning speed is 17m/min, the temperature of the spinning is 190 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 5h, and the mechanical properties of filaments before and after heating can be enhanced by 2.8 times.
Example 17
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament is characterized in that the polymer of the other component is polymethyl methacrylate, the solvent is tetrahydrofuran, the concentration of the spinning solution is 34 weight percent, and the coagulating bath is tap water; the spinning speed is 15m/min, the temperature of the spinning is 180 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 4 hours, and the mechanical properties of filaments before and after heating can be enhanced by 1.5 times.
Example 18
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament is characterized in that the polymer serving as the other component is polyvinyl formal, the solvent is N-methylpyrrolidone, the concentration of the spinning solution is 23wt%, and the coagulating bath is tap water; the spinning speed is 9m/min, the temperature of the spinning is 220 ℃ by utilizing a temperature-controllable receiving roller for in-situ heating, the heating time is 3h, and the mechanical properties of filaments before and after heating can be enhanced by 3 times.
Example 19
In the embodiment, the one-step green preparation and in-situ enhancement method of the high-temperature-resistant flame-retardant PAI-based filament is characterized in that the polymer as the other component is polyvinyl formal, the solvent is N-methyl pyrrolidone, the concentration of the spinning solution is 25wt%, and the coagulating bath is mineral water; the spinning speed is 13m/min, the temperature of the spinning is 210 ℃ by utilizing the temperature-controllable receiving roller for in-situ heating, the heating time is 2h, and the mechanical properties of filaments before and after heating can be enhanced by 2 times.
Example 20
In the embodiment, the one-step green preparation and in-situ reinforcement method of the high-temperature-resistant flame-retardant PAI-based filament comprises the steps that the polymer as the other component is polyurethane, the solvent is N, N-dimethylformamide, the concentration of spinning solution is 28wt%, and the coagulating bath is mineral water; the spinning speed is 13m/min, the temperature of the spinning is 170 ℃ and the heating time is 5 hours by utilizing the temperature-controllable receiving roller to heat in situ, and the mechanical properties of filaments before and after heating can be enhanced by 2 times.

Claims (6)

1. The high-temperature-resistant flame-retardant polyamide-imide filament is characterized by comprising polyamide-imide and another component polymer, wherein the weight proportion of the polyamide-imide is more than or equal to 90%, the polyamide-imide is in a powder form and a liquid form, the molecular weight of the polyamide-imide is 5000-800000, and the type of the polyamide-imide is a block type or a homopolymerization type; the surface of the filament is smooth, the section is cylindrical, and the diameter is 0.1-2 mm;
The polyamide imide is used as a rigid high molecular network due to the benzene ring, another component polymer is used as a flexible high molecular network, the melting temperature of the other component polymer is lower than the glass transition temperature of the polyamide imide, and the other component polymer is polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral or polymethyl methacrylate;
The high-temperature-resistant flame-retardant polyamide-imide-based filament is used at the temperature lower than 220 ℃ and has the characteristics of self-extinguishing after leaving fire, no fuming or melting drop, and the limiting oxygen index is 43-50%;
Firstly, preparing a spinning solution of polyamide imide, another component polymer and a solvent, and then extruding the spinning solution into a coagulating bath by using a wet spinning technology and taking water as the coagulating bath to obtain hybridized nascent fibers; the hybridized nascent fiber is heated in situ by a temperature-controllable receiving roller, the heating temperature is adjustable within the range of 150-240 ℃, the heating time is 1-10 h, and the mechanical properties of filaments before and after heating are enhanced by 1-3 times.
2. The high temperature resistant, flame retardant polyamideimide-based filament according to claim 1, wherein the mechanical tensile strength of the high temperature resistant, flame retardant polyamideimide-based filament is 20-200 MPa and the elongation at break is 5-30%.
3. The method for preparing the high-temperature-resistant and flame-retardant polyamide-imide filament yarn as claimed in claim 1, wherein a spinning solution of polyamide-imide, another polymer and a solvent is prepared, and then the spinning solution is extruded into a coagulating bath by using a wet spinning technology by using water as the coagulating bath to obtain the hybrid nascent fiber; the hybridized nascent fiber is heated in situ by a temperature-controllable receiving roller, the heating temperature is adjustable within the range of 150-240 ℃, the heating time is 1-10 h, and the mechanical properties of filaments before and after heating are enhanced by 1-3 times.
4. The method for preparing the high-temperature-resistant flame-retardant polyamide-imide filaments according to claim 3, wherein the polymer of the other component is one or more of polyurethane, nylon, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral and polymethyl methacrylate, and the solvent is one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone and tetrahydrofuran.
5. A process for preparing a high temperature resistant, flame retardant polyamideimide-based filament according to claim 3 wherein the coagulation bath is deionized water, distilled water, mineral water or tap water.
6. A process for preparing a high temperature resistant, flame retardant polyamideimide-based filament according to claim 3, wherein the concentration of the spinning solution is 20 to 40wt%, and the spinning speed is 5 to 20m/min.
CN202210585126.4A 2022-05-27 2022-05-27 High-temperature-resistant flame-retardant polyamide-imide filament and green preparation and in-situ enhancement method thereof Active CN114717681B (en)

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CN101619502A (en) * 2009-07-29 2010-01-06 东华大学 Method for preparing polyamide-imide fiber
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

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FR1603108A (en) * 1968-06-04 1971-03-22
CN103757721B (en) * 2014-01-20 2016-09-07 江苏巨贤合成材料有限公司 A kind of polyamide-imide fiber wet method one step spinning technique
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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CN101619502A (en) * 2009-07-29 2010-01-06 东华大学 Method for preparing polyamide-imide fiber
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

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