CN108251916A - It is a kind of suitable for polyether-ether-ketone composite material of spinning technique and preparation method thereof - Google Patents
It is a kind of suitable for polyether-ether-ketone composite material of spinning technique and preparation method thereof Download PDFInfo
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- CN108251916A CN108251916A CN201711269932.6A CN201711269932A CN108251916A CN 108251916 A CN108251916 A CN 108251916A CN 201711269932 A CN201711269932 A CN 201711269932A CN 108251916 A CN108251916 A CN 108251916A
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- 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
- D01D1/00—Treatment of filament-forming or like material
-
- 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
- D01D5/08—Melt spinning methods
-
- 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
- D01D5/12—Stretch-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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Reinforced Plastic Materials (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a kind of polyether-ether-ketone composite materials suitable for spinning technique, it is characterized in that, including polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly P phenylene terephathalamide, the polyphenylene sulfide, polyimides, polyether-ether-ketone, polyether sulfone, thermotropic poly P phenylene terephathalamide mass ratio be 1 ﹕, 23 ﹕, 68 72 ﹕, 20 25 ﹕ 16.Polyether-ether-ketone composite material prepared by the present invention, drafting multiple is more than 2.1;Fracture strength is more than 3.4cN/dtex;Not less than 22%, toughness is improved significantly elongation at break simultaneously;Scanned Electronic Speculum test display, composite material are whole that molecule Fusion Strain is presented without apparent melting interface;145 DEG C of glass transition temperature, 172 DEG C of crystallization temperature, melt index improves more than 22%;As spinning material good fluidity, spinning is easy, and rejection rate is low.
Description
Technical field
The present invention relates to high-performance composite materials technical field, especially a kind of polyether-ether-ketones suitable for spinning technique to answer
Condensation material.
Background technology
Three development experience of macromolecular structure material general-purpose plastics, engineering plastics and high-performance special engineering plastics hairs
The exhibition stage.One of branch of the polyetheretherketonematerials materials as high-performance special engineering plastics, is widely used in every field.
By its excellent heat resistance, stability, chemical resistance, radioresistance etc., be widely used in Aeronautics and Astronautics, military project,
The multiple fields such as nuclear energy, electronics, machinery, medical treatment.
In spinning process, the variation of geometric shape and physical aspect will occur for fibre-forming polymer, such as the dissolving of polymer
Or melt, the flowing and deformation of spin fluid, in the gelling, crystallization, diauxic shift and elongational flow in strand solidification process
Macromolecular orientation and diffusion, heat transfer and mass transfer in the process etc..Therefore it is required that the material of spinning has the characteristics that:Flowing
Property is preferable, and molten system viscosity is relatively low;Better heat stability avoids aoxidizing, discoloration;Elimination " interior friction " has been had in system
Auxiliary agent, improve host molecule chain scope of activities;Toughness is preferable.
The molecular backbone of high-performance polyether-ether-ketone resin is made of phenyl ring and ehter bond, and this structure causes material to have in itself
There is higher heat resistance, but more highlighted with the raising shortcoming of heat resistance, melt viscosity height, poor fluidity, melting temperature
Degree is high, difficulty of processing is big etc., and in these performances of polyetheretherketonematerials materials the defects of leads to its development in terms of spinning processing
Limited, spinning difficulty is larger, high rejection rate;Simultaneously as polyether-ether-ketone price is relatively high, single use polyether-ether-ketone carries out
Spinning, cost is higher, and economy is bad.Therefore in the environment of spinning technique rapid development, there is an urgent need for polyether-ether-ketone is changed
Property processing, make that it is suitable for spinning techniques.
Invention content
The technical problems to be solved by the invention be to provide a kind of polyether-ether-ketone composite material suitable for spinning technique and
Preparation method, solve in the prior art polyether-ether-ketone as spinning material melt viscosity height, poor fluidity, melting temperature height,
The shortcomings that difficulty of processing is big, spinning difficulty is larger, high rejection rate.
The technical solution adopted by the present invention to solve the technical problems is:A kind of polyether-ether-ketone suitable for spinning technique is answered
Condensation material, which is characterized in that including polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic polyparaphenylene to benzene
Diamides, the polyphenylene sulfide, polyimides, polyether-ether-ketone, polyether sulfone, thermotropic poly P phenylene terephathalamide matter
Amount is than being 1 ﹕ 2-3 ﹕ 68-72 ﹕ 20-25 ﹕ 1-6.
Preferably, the polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic polyparaphenylene terephthalate
The grain size of amine is is respectively 90-100 μm, 110-120 μm, 100-110 μm, 60-70 μm, 50-60 μm.
A kind of preparation method of polyether-ether-ketone composite material suitable for spinning technique, includes the following steps:
(1) it is dry:The raw material for providing a kind of above-mentioned polyether-ether-ketone composite material suitable for spinning technique carries out respectively
Vacuum drying, specific drying condition are:Polyether-ether-ketone:150-180 DEG C, it is dried in vacuo 150-180min;Polyether sulfone:130-180
DEG C, it is dried in vacuo 140-160min;Polyphenylene sulfide:120-160 DEG C, it is dried in vacuo 150-160min;Polyimides:170-180
DEG C, it is dried in vacuo 160-180min;Thermotropic poly P phenylene terephathalamide:115-125 DEG C, it is dried in vacuo 220-
240min;
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly-
Continuous column is squeezed out to obtain to phenylene terephthalate amine melt blending at a temperature of 375-405 DEG C;
(3) the continuous column obtained by step (2) is subjected to drawing-off and forms fiber, then in 85-99 DEG C of bath temperature
Middle cooling and shaping is up to fiber polyether-ether-ketone composite material.
Preferably, the melt blending of the step (2) selects extruder, injection molding machine or mixer.
Preferably, step (2) selects double screw extruder to carry out melt blending.
Preferably, the fiber polyether-ether-ketone composite material obtained by step (3) is subjected to coiling, the coiling rate is 20-
100m/min。
Preferably, a diameter of 2-8mm of the continuous column of step (2).
The beneficial effects of the invention are as follows:The present invention is using polyether-ether-ketone as base material, by adding in polyether sulfone, polyphenylene sulfide, gathering
Acid imide, thermotropic poly P phenylene terephathalamide carry out pre-treatment, then pass through melt blending system by specific drying process
Standby polyether-ether-ketone composite material, drafting multiple is more than 2.1;Fracture strength is more than 3.4cN/dtex;Elongation at break simultaneously
Not less than 22%, toughness is improved significantly;Scanned Electronic Speculum test display, composite material are whole without apparent melting interface
Molecule Fusion Strain is presented;145 DEG C of glass transition temperature, 172 DEG C of crystallization temperature, melt index improves more than 22%;With
Make spinning material good fluidity, spinning is easy, and rejection rate is low.
The present invention a kind of polyether-ether-ketone composite material suitable for spinning technique preparation method, due to each step ginseng
Several interactions and drying temperature, the time, melt blending extrusion temperature, water-bath temperature determine so that preparation is answered
Condensation material, good fluidity, thermal stability are good, high melt index, can be used as spinning material;Economic benefit is improved, is reduced poly-
The consumption of ether ether ketone unit cost.
Specific embodiment
With reference to embodiment, the present invention is further described.
The technical solution adopted by the present invention to solve the technical problems is:A kind of polyether-ether-ketone suitable for spinning technique is answered
Condensation material, which is characterized in that including polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic polyparaphenylene to benzene
Diamides, the polyphenylene sulfide, polyimides, polyether-ether-ketone, polyether sulfone, thermotropic poly P phenylene terephathalamide matter
Amount is than being 1 ﹕ 2-3 ﹕ 68-72 ﹕ 20-25 ﹕ 1-6.Thermotropic poly P phenylene terephathalamide, also known as LCP industrialize liquid crystal and gather
Object is closed, one kind has the new polymers of outstanding performance.Selected raw material is commercial product, the present invention using polyether-ether-ketone powder as
Motif material is modified, remaining, which adds materials, belongs to beneficial to modification, and the most important effect of polyether sulfone is the melting of reduction system
Viscosity reduces " wire drawing " difficulty, while increases system mobility;The main function of polyphenylene sulfide is reduction system " interior friction ",
Solve the problems, such as that the occupy-place of polyether-ether-ketone space is excessive;Polyimides improves the tolerable temperature of system, improves mechanical property;It is thermotropic
Poly- is " toughening " to methylene terephthalate amine main function, and system " rigidity " is reduced, and toughness improves.
The polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly P phenylene terephathalamide grain
Diameter is is respectively 90-100 μm, 110-120 μm, 100-110 μm, 60-70 μm, 50-60 μm.
A kind of preparation method of polyether-ether-ketone composite material suitable for spinning technique, includes the following steps:
(1) it is dry:The raw material for providing a kind of above-mentioned polyether-ether-ketone composite material suitable for spinning technique carries out respectively
Vacuum drying, specific drying condition are:Polyether-ether-ketone:150-180 DEG C, it is dried in vacuo 150-180min;Polyether sulfone:130-180
DEG C, it is dried in vacuo 140-160min;Polyphenylene sulfide:120-160 DEG C, it is dried in vacuo 150-160min;Polyimides:170-180
DEG C, it is dried in vacuo 160-180min;Thermotropic poly P phenylene terephathalamide:115-125 DEG C, it is dried in vacuo 220-
240min.It due to feedstock property difference, such as dries simultaneously, and drying time is long, temperature is excessively high, is likely to result in surface of material
Dusting or denaturation if drying temperature and time are inadequate, cause water content in material higher, can go out during continuous drafting
Situations such as existing fracture of wire, bubble, hydraulic performance decline, cause product qualification rate relatively low;The drying condition that the present invention selects so that mixture
Drafting multiple is stablized in drafting process, and product qualification rate is high.
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly-
Phenylene terephthalate amine melt blending at a temperature of 375-405 DEG C is squeezed out a diameter of 2-8mm continuous column;
(3) the continuous column obtained by step (2) is subjected to drawing-off and forms fiber, then in 85-99 DEG C of bath temperature
Middle cooling and shaping is up to fiber polyether-ether-ketone composite material.
The melt blending of the step (2) selects extruder, injection molding machine or mixer.Step (2) selects twin-screw extrusion
Machine carries out melt blending.Fiber polyether-ether-ketone composite material obtained by step (3) is subjected to coiling, the coiling rate is 20-
100m/min.Drawing-off, coiling technique are a continuous processes, and continuous column, melt blending squeezes at a temperature of 375-405 DEG C
Go out, cooling and shaping at being then 85-99 DEG C in bath temperature in drafting process, then coiling at room temperature;Temperature is by 400 DEG C or so
Room temperature and a material are gradually lowered to by the gradual cured process of molten state, macromolecule product is in the process of cooling and solidifying
In be divided into three phases:Mainly " viscoelastic is utilized in glassy state, viscoelastic state, molten state, drawing-off, coiling in process of the present invention
The proper property of state " is processed substance in system so that the product draw ratio increase monfil diameter after coiling is steady
Fixed, product qualification rate is high.If cooling temperature is too low, fused materials directly cure, and viscoelastic state elapsed time is shorter, and drawing-off is compared
Small, the diameter of monfil is with regard to larger.If cooling temperature is excessively high, monfil can not be changed into glassy state by viscoelastic state in time.
The diameter of fiber will generate larger difference, and product fibre diameter is caused to differ greatly, and influence final properties of product.
Embodiment 1:
(1) it is dry:Raw material is dried in vacuo respectively, specific drying condition is:Polyether-ether-ketone:150 DEG C, vacuum drying
180min;Polyether sulfone:130 DEG C, it is dried in vacuo 160min;Polyphenylene sulfide:120 DEG C, it is dried in vacuo 160min;Polyimides:170
DEG C, it is dried in vacuo 180min;Thermotropic poly P phenylene terephathalamide:115 DEG C, it is dried in vacuo 240min;
(2) melt blending:It is using extruder that dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyamides is sub-
Amine, thermotropic the poly P phenylene terephathalamide melt blending at a temperature of 375 DEG C squeeze out a diameter of 2-8mm continuous column
Object;
(3) continuous column is subjected to drawing-off and forms fiber, then cooling and shaping is to obtain the final product fine in 85 DEG C of bath temperature
Tie up polyether-ether-ketone composite material;
(4) the fiber polyether-ether-ketone composite material obtained by detects its performance after carrying out room temperature coiling, and the coiling rate is
20m/min。
Embodiment 2:
(1) it is dry:Raw material is dried in vacuo respectively, specific drying condition is:
Polyether-ether-ketone:180 DEG C, it is dried in vacuo 150min;Polyether sulfone:180 DEG C, it is dried in vacuo 140min;Polyphenylene sulfide:
160 DEG C, it is dried in vacuo 150min;Polyimides:180 DEG C, it is dried in vacuo 160min;Thermotropic polyparaphenylene terephthalate
Amine:125 DEG C, it is dried in vacuo 220min;
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly-
Phenylene terephthalate amine is selected at a temperature of 405 DEG C injection molding machine melt blending squeeze out a diameter of 2-8mm continuous column
Object;
(3) the continuous column of gained is subjected to drawing-off and forms fiber, then the cooling and shaping in 99 DEG C of bath temperature
Up to fiber polyether-ether-ketone composite material.
(4) the fiber polyether-ether-ketone composite material of gained is carried out to the rate coiling of 100m/min, then detects its performance.
Embodiment 3:
(1) it is dry:Raw material is dried in vacuo respectively, specific drying condition is:
Polyether-ether-ketone:160 DEG C, it is dried in vacuo 180min;Polyether sulfone:130 DEG C, it is dried in vacuo 150min;Polyphenylene sulfide:
140 DEG C, it is dried in vacuo 150min;Polyimides:170 DEG C, it is dried in vacuo 180min;Thermotropic polyparaphenylene terephthalate
Amine:125 DEG C, it is dried in vacuo 240min;
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly-
To phenylene terephthalate amine at a temperature of 385 DEG C using double screw extruder melt blending squeeze out a diameter of 2-8mm company
Continuous column;
(3) the continuous column of gained is subjected to drawing-off and forms fiber, then the cooling and shaping in 95 DEG C of bath temperature
Up to fiber polyether-ether-ketone composite material.
(4) the fiber polyether-ether-ketone composite material obtained by carries out the rate coiling of 55m/min, then detects its performance.
Embodiment 4:
(1) it is dry:Raw material is dried in vacuo respectively, specific drying condition is:
Polyether-ether-ketone:160 DEG C, it is dried in vacuo 180min;Polyether sulfone:130 DEG C, it is dried in vacuo 150min;Polyphenylene sulfide:
150 DEG C, it is dried in vacuo 150min;Polyimides:170 DEG C, it is dried in vacuo 180min;Thermotropic polyparaphenylene terephthalate
Amine:125 DEG C, it is dried in vacuo 240min;
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly-
Mixer melt blending is selected to squeeze out to obtain continuous column at a temperature of 385 DEG C phenylene terephthalate amine;
(3) by continuous column carry out drawing-off and form fiber, then cooling and shaping in 95 DEG C of bath temperature to obtain the final product
Fiber polyether-ether-ketone composite material.
(4) the fiber polyether-ether-ketone composite material obtained by carries out the rate coiling of 55m/min, then detects its performance.
Following table is the quality proportioning of embodiment 1-4:
The quality proportioning of 1 embodiment 1-4 of table
Above-mentioned raw materials polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly P phenylene terephathalamide
Grain size for be respectively 100 μm, 120 μm, 105 μm, 60 μm, 50 μm.
The main performance index of 2 coiling of table polyether-ether-ketone composite material after molding
Main performance index of the upper table for embodiment 1-4 and control group coiling polyether-ether-ketone composite material after molding,
Middle control group is unmodified polyether-ether-ketone resin, it can be seen that polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, heat
Composite material drafting multiple after cause property poly P phenylene terephathalamide blending and modifying is up to 4.1 times;Fracture strength is reachable
3.9cN/dtex, while elongation at break maximum is up to 29.1%, elongation at break maximum lift more than 55%, i.e. composite wood
The toughness of material is remarkably enhanced;And scanned Electronic Speculum test display, intermingling material are whole to present without apparent melting interface
Molecule Fusion Strain;145 DEG C of glass transition temperature, 172 DEG C of crystallization temperature, 335-338 DEG C of melting temperature, heat decomposition temperature
561-579 DEG C, thermal stability is good, and melt index greatly improves.
Claims (7)
1. a kind of polyether-ether-ketone composite material suitable for spinning technique, which is characterized in that including polyether-ether-ketone, polyether sulfone, gather
Diphenyl sulfide, polyimides, thermotropic poly P phenylene terephathalamide, the polyphenylene sulfide, polyimides, polyether-ether-ketone,
Polyether sulfone, thermotropic poly P phenylene terephathalamide mass ratio be 1 ﹕ 2-3 ﹕ 68-72 ﹕ 20-25 ﹕ 1-6.
2. a kind of polyether-ether-ketone composite material suitable for spinning technique according to claim 1, which is characterized in that described
Polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly P phenylene terephathalamide grain size for be respectively 90-
100μm、110-120μm、100-110μm、60-70μm、50-60μm。
3. the preparation method of a kind of polyether-ether-ketone composite material suitable for spinning technique, which is characterized in that include the following steps:
(1) it is dry:A kind of raw material of polyether-ether-ketone composite material suitable for spinning technique described in claims 1 or 2 is provided
It is dried in vacuo respectively, specific drying condition is:
Polyether-ether-ketone:150-180 DEG C, it is dried in vacuo 150-180min;
Polyether sulfone:130-180 DEG C, it is dried in vacuo 140-160min;
Polyphenylene sulfide:120-160 DEG C, it is dried in vacuo 150-160min;
Polyimides:170-180 DEG C, it is dried in vacuo 160-180min;
Thermotropic poly P phenylene terephathalamide:115-125 DEG C, it is dried in vacuo 220-240min;
(2) melt blending:By dried raw material polyether-ether-ketone, polyether sulfone, polyphenylene sulfide, polyimides, thermotropic poly- to Asia
Phenyl terephthalate amine melt blending at a temperature of 375-405 DEG C squeezes out to obtain continuous column;
(3) the continuous column obtained by step (2) is subjected to drawing-off and forms fiber, it is then cold in 85-99 DEG C of bath temperature
But it shapes up to fiber polyether-ether-ketone composite material.
4. a kind of preparation method of polyether-ether-ketone composite material suitable for spinning technique according to claim 3, special
Sign is that the melt blending of the step (2) selects extruder, injection molding machine or mixer.
5. a kind of preparation method of polyether-ether-ketone composite material suitable for spinning technique according to claim 4, special
Sign is that step (2) selects double screw extruder to carry out melt blending.
6. a kind of preparation method of polyether-ether-ketone composite material suitable for spinning technique according to claim 3, special
Sign is, the fiber polyether-ether-ketone composite material obtained by step (3) is carried out coiling, the coiling rate is 20-100m/min.
7. according to a kind of preparation side of polyether-ether-ketone composite material suitable for spinning technique of claim 1-6 any one of them
Method, which is characterized in that a diameter of 2-8mm of the continuous column of step (2).
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CN110184744A (en) * | 2019-05-09 | 2019-08-30 | 吉林大学 | A kind of crystal type poly(aryl ether ketone) nano fibrous membrane, preparation method and applications |
CN110184744B (en) * | 2019-05-09 | 2022-01-21 | 吉林大学 | Crystalline polyaryletherketone nanofiber membrane, and preparation method and application thereof |
CN115679478A (en) * | 2022-11-08 | 2023-02-03 | 东华大学 | High-strength low-shrinkage polyether-ether-ketone monofilament and preparation method thereof |
CN115679478B (en) * | 2022-11-08 | 2024-03-01 | 东华大学 | High-strength low-shrinkage polyether-ether-ketone monofilament and preparation method thereof |
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