A PEEK monofilament preparation system and preparation method thereof

By combining technical means such as multi-stage vacuum drum dryer, screw extruder and hot roll tensile setting device, the problem that the existing technology cannot prepare small diameter PEEK monofilaments, and high-performance PEEK monofilaments are achieved. The performance reaches a break strength of 36CN and an elongation of 41.1%.

CN116623304BActive Publication Date: 2024-12-20JIANGSU XINREN ENVIRONMENTAL PROTECTION TECH CO LTD
View PDF 0 Cites 0 Cited by

Patent Information

Application Number
CN202310577348.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-22
Publication Date
2024-12-20
Estimated Expiration
2043-05-22

AI Technical Summary

Technical Problem

The prior art cannot produce PEEK monofilaments with fiber diameters less than 35 μm, due to the high melting temperature of PEEK, large melt viscosity and poor fluidity.

Method used

Using a combination system of multi-stage vacuum drum dryer, screw extruder, spinning assembly, cooling device, multi-stage hot roll stretching and shaping device and wire splitter, through precrystallization, hot melt extrusion, wire drawing, multi-stage The steps of hot roll stretching and wire winding are controlled, and the heating temperature zone and roller temperature of the screw extruder are controlled, and the multi-stage vacuum drum dryer and hot air circulation device are used to dry and heat to ensure the filter net of the spinning assembly. and spinneret structure, the tension is controlled to prepare small diameter PEEK monofilaments.

Benefits of technology

PEEK monofilament with a fiber diameter of less than 35μm was successfully prepared, with excellent performance, a breaking strength of up to 36CN, an elongation of breaking of up to 41.1%, and a shrinkage of up to 8.2% at 200℃.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN116623304B_ABST
    Figure CN116623304B_ABST
Patent Text Reader

Abstract

The invention discloses a PEEK monofilament preparation system, comprising a multi-stage vacuum drum dryer, a dry slice silo, a screw extruder, a metering pump, a spinning assembly, a cooling device, an oiling device, a bundling device, a multi-stage hot roller stretching and shaping device, a multifilament winding machine and a wire separator arranged in sequence along the PEEK monofilament preparation direction; the feeding section length of the screw extruder accounts for 30-50% of the total length of the screw, the compression section length accounts for 25-35% of the total length of the screw, and the metering section length accounts for 25-35% of the total length of the screw; the screw extruder is divided into six heating temperature zones in sequence along the extrusion direction; the multi-stage hot roller stretching and shaping device includes a primary stretching hot roller, a secondary stretching hot roller stretching, and a tertiary shaping hot roller. The invention has the advantage of being able to produce PEEK monofilaments with a fiber diameter less than 35 μm.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of special fiber preparation, and in particular to a PEEK monofilament preparation system and a preparation method thereof. Background Art

[0002] Polyetheretherketone (PEEK) is a linear wholly aromatic polymer with a regular structure and high crystallinity. PEEK monofilaments obtained by melt extrusion are widely used in aerospace, automotive industry, electronics, medical, automotive and other fields due to their excellent properties such as high strength, high toughness, high temperature resistance, corrosion resistance and high flame retardancy. Since PEEK has a high melting point and high melt viscosity and poor fluidity after melting, the currently commonly used monofilament preparation method cannot produce PEEK monofilaments with a fiber diameter of less than 35μm. Contents of the invention

[0003] The first object of the present invention is to provide a preparation system capable of producing PEEK monofilaments with a fiber diameter less than 35 μm.

[0004] To achieve the above-mentioned purpose, the present invention adopts the following technical scheme: a PEEK monofilament preparation system, comprising a multi-stage vacuum drum dryer, a dry slice silo, a screw extruder, a metering pump, a spinning assembly, a cooling device, an oiling device, a bundling device, a multi-stage hot roller stretching and shaping device, a multifilament winding machine and a wire separator arranged in sequence along the PEEK monofilament preparation direction; the screw extruder is divided into a feeding section, a compression section and a metering section in sequence along the extrusion direction, the length of the feeding section accounts for 30-50% of the total length of the screw, the length of the compression section accounts for 25-35% of the total length of the screw, and the length of the metering section accounts for 25-35% of the total length of the screw; and the screw extruder is arranged in sequence along the extrusion direction. The multi-stage hot roller stretching and shaping device comprises a first-stage stretching hot roller with a roller temperature of 150-200°C and a roller speed of 300-500m / min for fiber stretching, a second-stage stretching hot roller with a roller temperature of 180-240°C and a roller speed of 600-1000m / min for fiber shaping, and a third-stage shaping hot roller with a roller temperature of 180-240°C and a roller speed of 600-1000m / min for fiber shaping.

[0005] Furthermore, the aforementioned PEEK monofilament preparation system, wherein: the structure of the spinning assembly includes: a shell, a feed port is arranged at the top of the shell, a discharge port is arranged at the bottom of the shell, and an upper filter mesh group, a distribution plate, a lower filter mesh group and a spinneret are arranged in sequence from top to bottom inside the shell, and the spinneret is located at the discharge port of the shell, the upper filter mesh group is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 to 600 meshes; the lower filter mesh group is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 to 800 meshes.

[0006] Furthermore, the aforementioned PEEK monofilament preparation system, wherein: the cooling device includes a slow cooling device and a side blowing device arranged in sequence along the PEEK monofilament preparation direction, the slow cooling device is used to slowly cool the nascent monofilaments ejected from the spinning assembly to 280-330°C, and the side blowing device is used to cool the nascent monofilaments slowly cooled to 280-330°C by the slow cooling device to room temperature.

[0007] Furthermore, in the aforementioned PEEK monofilament preparation system, a tension controller is provided on the wire dividing machine, and the wire dividing machine controls the tension range of the PEEK monofilament within 5 to 20 CN through the tension controller.

[0008] Furthermore, the aforementioned PEEK monofilament preparation system, wherein: in the multi-stage vacuum drum dryer, the pre-crystallization temperature of the multi-stage vacuum drum dryer for the PEEK resin raw material is 100-140°C, the pre-crystallization time is 2-4 hours, the vacuum pumping speed is 10-20 liters / second, the drum drying temperature is 150-180°C, and the drying time is 3-6 hours.

[0009] Furthermore, in the aforementioned PEEK monofilament preparation system, a hot air circulation device is provided in the dry slice silo, and the hot air circulation device is used to maintain the temperature of the PEEK resin raw material in the silo at 140-170°C.

[0010] Furthermore, in the aforementioned PEEK monofilament preparation system, the length of the feed section of the screw extruder accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw.

[0011] The second object of the present invention is to provide a method for preparing PEEK monofilaments with a fiber diameter of less than 35 μm.

[0012] To achieve the above object, the present invention adopts the following technical solution: a method for preparing a PEEK monofilament, comprising the following steps:

[0013] (1) Crystallization, drying and purification: Add the PEEK resin raw material to a multi-stage vacuum drum dryer, and use the multi-stage vacuum drum dryer to pre-crystallize and dry the PEEK resin raw material; wherein the pre-crystallization temperature is 100-140°C, the pre-crystallization time is 2-4 hours, the vacuum pumping speed is 10-20 liters / second, the drum drying temperature is 150-180°C, and the drying time is 3-6 hours;

[0014] (2) Raw material heating: The crystallized, dried and purified PEEK resin raw material is put into the dry chip silo. The dry chip silo uses hot air circulation to keep the temperature of the PEEK resin raw material in the silo at 140-170°C;

[0015] (3) Hot melt extrusion: The PEEK resin raw material in the dry slice silo is input into a screw extruder for melt extrusion to obtain a PEEK melt; wherein the screw extruder is divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 30-50% of the total length of the screw, the length of the compression section accounts for 25-35% of the total length of the screw, and the length of the metering section accounts for 25-35% of the total length of the screw; wherein the screw extruder is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 330-380°C, 350-400°C, 380-420°C, 390-440°C, 385-430°C, 385-430°C;

[0016] (4) Wire drawing: PEEK melt is first metered by a metering pump and then fed into a spinning assembly. The spinning assembly ejects the PEEK melt to form a number of primary monofilaments. Each primary monofilament is first slowly cooled to 280-330°C by a slow cooling device, then cooled to room temperature by a side blowing device, then oiled by an oiling device, and then bundled by a bundling device to form primary multifilaments.

[0017] (5) Multi-stage hot roller stretching, shaping and winding: The spun multifilament is first stretched by a primary stretching hot roller and a secondary stretching hot roller, and then shaped by a tertiary shaping hot roller before being sent to a multifilament winding machine for winding; wherein the roller temperature of the primary stretching hot roller is 150-200°C, the roller speed is 300-500 m / min, and the residence time of the spun multifilament on the primary stretching hot roller is 0.5-0.8 seconds; the roller temperature of the secondary stretching hot roller is 180-240°C, the roller speed is 600-1000 m / min, and the residence time of the spun multifilament on the secondary stretching hot roller is 0.3-0.5 seconds; the stretching ratio of the secondary stretching hot roller to the primary stretching hot roller is 1.2-3.3; the roller temperature of the tertiary shaping hot roller is 180-240°C, the roller speed is 600-1000 m / min, and the residence time of the spun multifilament on the tertiary shaping hot roller is 0.3-0.5 seconds;

[0018] (6) Filament winding: The multifilament wound in the multifilament winding machine is divided into several single filaments by a fiber dividing machine and rewound to make PEEK single filaments.

[0019] Furthermore, the aforementioned method for preparing PEEK monofilaments, wherein: the structure of the spinning assembly includes: a shell, a feed port is provided at the top of the shell, a discharge port is provided at the bottom of the shell, and an upper filter mesh group, a distribution plate, a lower filter mesh group and a spinneret are arranged in sequence from top to bottom inside the shell, and the spinneret is located at the discharge port of the shell, the upper filter mesh group is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 to 600 meshes; the lower filter mesh group is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 to 800 meshes.

[0020] Furthermore, in the aforementioned method for preparing PEEK monofilament, in step (1), the PEEK resin raw material is dried until the water content reaches below 50 ppm.

[0021] Furthermore, in the aforementioned method for preparing a PEEK monofilament, in step (6), the wire splitting machine controls the tension range of the PEEK monofilament within 5 to 20 CN through a tension controller.

[0022] Furthermore, in the aforementioned method for preparing PEEK monofilament, the length of the feed section of the screw extruder accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw.

[0023] Through the implementation of the above technical scheme, the beneficial effects of the present invention are: PEEK monofilaments with a fiber diameter of less than 35 μm can be produced, and the produced PEEK monofilaments have excellent performance, with a breaking strength of up to 36 CN, a breaking elongation of up to 41.1%, and a shrinkage rate of up to 8.2% at 200°C. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a schematic diagram of the structural principle of a PEEK monofilament preparation system described in the present invention.

[0025] Figure 2 Schematic diagram of the structure of the spinning assembly.

[0026] Figure 3 This is a schematic diagram of the diameter of a PEEK monofilament obtained by a PEEK monofilament preparation method described in the third specific embodiment of the present invention under an image measuring instrument. DETAILED DESCRIPTION

[0027] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments.

[0028] like Figure 1 , Figure 2 As shown, the PEEK monofilament preparation system comprises a multi-stage vacuum drum dryer 1, a dry slice silo 2, a screw extruder 3, a metering pump 4, a spinning assembly 5, a cooling device, an oiling device 8, a bundling device 9, a multi-stage hot roller stretching and shaping device 10, a multifilament winding machine 11 and a wire dividing machine 12 arranged in sequence along the PEEK monofilament preparation direction; in this embodiment, the cooling device comprises a slow cooling device 6 and a side blowing device 7 arranged in sequence along the PEEK monofilament preparation direction, the slow cooling device 6 is used to slowly cool the nascent monofilament ejected from the spinning assembly to 280-330°C, and the side blowing device 7 is used to cool the nascent monofilament slowly cooled to 280-330°C by the slow cooling device to room temperature; the screw extruder 3 is divided into a feeding section, a compression section and a metering section in sequence along the extrusion direction, the length of the feeding section accounts for 30-50% of the total length of the screw, the length of the compression section accounts for 25-35% of the total length of the screw, and the length of the metering section accounts for 10% of the total length of the screw. In this embodiment, the length of the feeding section of the screw extruder accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw; and the screw extruder 3 is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 330-380°C, 350-400°C, 380-420°C, 390-440°C, 385-430°C, 3 85~430℃; the multi-stage hot roller stretching and shaping device 10 includes a primary stretching hot roller 13 with a roller temperature of 150~200℃ and a roller speed of 300~500m / min for fiber stretching, a secondary stretching hot roller stretching 14 with a roller temperature of 180~240℃ and a roller speed of 600~1000m / min, and a third-stage shaping hot roller 15 with a roller temperature of 180~240℃ and a roller speed of 600~1000m / min for fiber shaping;

[0029] In this embodiment, the structure of the spinning assembly 5 includes: a shell 51, a feed port is arranged at the top of the shell 51, a discharge port is arranged at the bottom of the shell 51, and an upper filter mesh group 52, a distribution plate 53, a lower filter mesh group 54 and a spinneret 55 are arranged in sequence from top to bottom inside the shell 51, and the spinneret 55 is located at the discharge port of the shell 51. The upper filter mesh group 52 is composed of a plurality of stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 to 600 meshes; the lower filter mesh group 54 is composed of a plurality of stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 to 800 meshes;

[0030] In this embodiment, a tension controller is provided on the wire separator 12, and the wire separator 12 controls the tension range of the PEEK monofilament within 5 to 20 CN through the tension controller; in this embodiment, in the multi-stage vacuum drum dryer 1, the multi-stage vacuum drum dryer 1 has a pre-crystallization temperature of 100 to 140° C. for the PEEK resin raw material, a pre-crystallization time of 2 to 4 hours, a vacuum pumping speed of 10 to 20 liters / second, a drum drying temperature of 150 to 180° C., and a drying time of 3 to 6 hours; a hot air circulation device 16 is provided in the dry slice silo 2, and the hot air circulation device 16 is used to maintain the temperature of the PEEK resin raw material in the silo at 140 to 170° C.; Specific embodiment 1

[0031] A method for preparing a PEEK monofilament comprises the following steps:

[0032] (1) Crystallization, drying and purification: 50 kg of PEEK resin raw material is added to a multi-stage vacuum drum dryer, and the PEEK resin raw material is pre-crystallized and dried and purified by the multi-stage vacuum drum dryer; wherein the pre-crystallization temperature is 100°C, the pre-crystallization time is 2 hours, the vacuum pumping speed is 10 liters / second, the drum drying temperature is 150°C, and the drying time is 3 hours, wherein the PEEK resin raw material is dried to a water content of less than 50 ppm;

[0033] (2) Raw material heating: The crystallized, dried and purified PEEK resin raw material is put into the dry chip silo. The dry chip silo uses hot air circulation to keep the temperature of the PEEK resin raw material in the silo at 140°C;

[0034] (3) Hot melt extrusion: The PEEK resin raw material in the dry slice silo is input into a screw extruder for melt extrusion to obtain a PEEK melt; wherein the screw extruder is divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw; wherein the screw extruder is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 330°C, 350°C, 380°C, 390°C, 385°C, 385°C;

[0035] (4) Wire drawing: PEEK melt is first metered by a metering pump and then fed into a spinning assembly. The spinning assembly ejects the PEEK melt to form a plurality of primary monofilaments. Each primary monofilament is first slowly cooled to 280°C by a slow cooling device, then cooled to room temperature by a side blowing device, then oiled by an oiling device, and then bundled by a bundling device to form primary multifilaments; wherein: the structure of the spinning assembly 5 includes: a shell 51, a feed port is provided at the top of the shell 51, and a feed port is provided at the bottom of the shell 51; A discharge port is provided, and an upper filter mesh group 52, a distribution plate 53, a lower filter mesh group 54 and a spinneret 55 are arranged in order from top to bottom inside the housing 51. The spinneret 55 is located at the discharge port of the housing 51. The upper filter mesh group 52 is composed of a plurality of stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 meshes; the lower filter mesh group 54 is composed of a plurality of stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 meshes;

[0036] (5) Multi-stage hot roller stretching, shaping and winding: The spun multifilament is first stretched by a primary stretching hot roller and a secondary stretching hot roller, and then shaped by a tertiary shaping hot roller before being sent to a multifilament winding machine for winding; wherein the temperature of the primary stretching hot roller is 150°C, the roller speed is 500 m / min, and the residence time of the spun multifilament on the primary stretching hot roller is 0.5 second; the temperature of the secondary stretching hot roller is 180°C, the roller speed is 600 m / min, and the residence time of the spun multifilament on the secondary stretching hot roller is 0.3 second; the stretching ratio of the secondary stretching hot roller to the primary stretching hot roller is 1.2; the temperature of the tertiary shaping hot roller is 180°C, the roller speed is 600 m / min, and the residence time of the spun multifilament on the tertiary shaping hot roller is 0.3-0.5 second;

[0037] (6) Filament winding: The multifilament wound in the multifilament winding machine is divided into several single filaments by a fiber dividing machine and rewound to make PEEK single filaments with a fiber diameter of 34.3 μm. The fiber dividing machine controls the tension range of the PEEK single filaments in the range of 5 to 20 CN through a tension controller. Specific embodiment 2

[0038] A method for preparing a PEEK monofilament comprises the following steps:

[0039] (1) Crystallization, drying and purification: 50 kg of PEEK resin raw material is added to a multi-stage vacuum drum dryer, and the PEEK resin raw material is pre-crystallized and dried and purified by the multi-stage vacuum drum dryer; wherein the pre-crystallization temperature is 140°C, the pre-crystallization time is 4 hours, the vacuum pumping speed is 20 liters / second, the drum drying temperature is 180°C, and the drying time is 6 hours, wherein the PEEK resin raw material is dried to a water content of less than 50 ppm;

[0040] (2) Raw material heating: The crystallized, dried and purified PEEK resin raw material is put into the dry chip silo. The dry chip silo uses hot air circulation to keep the temperature of the PEEK resin raw material in the silo at 170°C;

[0041] (3) Hot melt extrusion: The PEEK resin raw material in the dry slice silo is input into a screw extruder for melt extrusion to obtain a PEEK melt; wherein the screw extruder is divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw; wherein the screw extruder is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 380°C, 400°C, 420°C, 440°C, 430°C, 430°C;

[0042] (4) Wire drawing: PEEK melt is first metered by a metering pump and then fed into a spinning assembly. The spinning assembly ejects the PEEK melt to form a plurality of primary monofilaments. Each primary monofilament is first slowly cooled to 330°C by a slow cooling device, then cooled to room temperature by a side blowing device, then oiled by an oiling device, and then bundled by a bundling device to form primary multifilaments; wherein: the structure of the spinning assembly 5 includes: a shell 51, a feed port is provided at the top of the shell 51, and a feed port is provided at the bottom of the shell 51; A discharge port is provided, and an upper filter mesh group 52, a distribution plate 53, a lower filter mesh group 54 and a spinneret 55 are arranged in order from top to bottom inside the housing 51. The spinneret 55 is located at the discharge port of the housing 51. The upper filter mesh group 52 is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 600 meshes; the lower filter mesh group 54 is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 800 meshes;

[0043] (5) Multi-stage hot roller stretching, shaping and winding: The spun multifilament is first stretched by a primary stretching hot roller and a secondary stretching hot roller, and then shaped by a tertiary shaping hot roller before being sent to a multifilament winding machine for winding; wherein the temperature of the primary stretching hot roller is 200°C, the roller speed is 400 m / min, and the residence time of the spun multifilament on the primary stretching hot roller is 0.8 seconds; the temperature of the secondary stretching hot roller is 240°C, the roller speed is 720 m / min, and the residence time of the spun multifilament on the secondary stretching hot roller is 0.5 seconds; the stretching ratio of the secondary stretching hot roller to the primary stretching hot roller is 1.8; the temperature of the tertiary shaping hot roller is 240°C, the roller speed is 720 m / min, and the residence time of the spun multifilament on the tertiary shaping hot roller is 0.5 seconds;

[0044] (6) Filament winding: The multifilament wound in the multifilament winding machine is divided into several single filaments by a fiber dividing machine and rewound to make PEEK single filaments with a fiber diameter of 33.8 μm. The fiber dividing machine controls the tension of the PEEK single filament in the range of 5 to 20 CN through a tension controller. Specific embodiment three

[0045] A method for preparing a PEEK monofilament comprises the following steps:

[0046] (1) Crystallization, drying and purification: 50 kg of PEEK resin raw material is added to a multi-stage vacuum drum dryer, and the PEEK resin raw material is pre-crystallized and dried and purified by the multi-stage vacuum drum dryer; wherein the pre-crystallization temperature is 120° C., the pre-crystallization time is 3 hours, the vacuum pumping speed is 15 liters / second, the drum drying temperature is 170° C., and the drying time is 5 hours, wherein the PEEK resin raw material is dried to a water content of less than 50 ppm;

[0047] (2) Raw material heating: The crystallized, dried and purified PEEK resin raw material is put into the dry chip silo. The dry chip silo uses hot air circulation to keep the temperature of the PEEK resin raw material in the silo at 150°C;

[0048] (3) Hot melt extrusion: The PEEK resin raw material in the dry slice silo is input into a screw extruder for melt extrusion to obtain a PEEK melt; wherein the screw extruder is divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw; wherein the screw extruder is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 350°C, 380°C, 400°C, 420°C, 410°C, 410°C;

[0049] (4) Wire drawing: PEEK melt is first metered by a metering pump and then fed into a spinning assembly. The spinning assembly ejects the PEEK melt to form a plurality of primary monofilaments. Each primary monofilament is first slowly cooled to 300°C by a slow cooling device, then cooled to room temperature by a side blowing device, then oiled by an oiling device, and then bundled by a bundling device to form primary multifilaments; wherein: the structure of the spinning assembly 5 includes: a shell 51, a feed port is provided at the top of the shell 51, and a feed port is provided at the bottom of the shell 51. A discharge port is provided, and an upper filter mesh group 52, a distribution plate 53, a lower filter mesh group 54 and a spinneret 55 are arranged in order from top to bottom inside the housing 51. The spinneret 55 is located at the discharge port of the housing 51. The upper filter mesh group 52 is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 450 meshes; the lower filter mesh group 54 is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 600 meshes;

[0050] (5) Multi-stage hot roller stretching, shaping and winding: The spun multifilament is first stretched by a primary stretching hot roller and a secondary stretching hot roller, and then shaped by a tertiary shaping hot roller before being sent to a multifilament winding machine for winding; wherein the roller temperature of the primary stretching hot roller is 180°C, the roller speed is 400 m / min, and the residence time of the spun multifilament on the primary stretching hot roller is 0.6 seconds; the roller temperature of the secondary stretching hot roller is 210°C, the roller speed is 800 m / min, and the residence time of the spun multifilament on the secondary stretching hot roller is 0.4 seconds; the stretching ratio of the secondary stretching hot roller to the primary stretching hot roller is 2; the roller temperature of the tertiary shaping hot roller is 210°C, the roller speed is 800 m / min, and the residence time of the spun multifilament on the tertiary shaping hot roller is 0.4 seconds;

[0051] (6) Filament winding: The multifilament wound in the multifilament winding machine is re-divided into several single filaments by a fiber dividing machine and rewound to make a PEEK single filament with a fiber diameter of 32.9 μm (the single filament diameter is as follows Figure 3 As shown in the figure, the wire dividing machine controls the tension range of the PEEK monofilament within 5 to 20CN through a tension controller.

[0052] The invention has the advantages that: PEEK monofilaments with a fiber diameter less than 35 μm can be produced, and the produced PEEK monofilaments have excellent performance, with a breaking strength of up to 36 CN, a breaking elongation of up to 41.1%, and a shrinkage rate of up to 8.2% at 200°C.

[0053] The above description is only a preferred embodiment of the present invention and does not constitute any other form of limitation to the present invention. Any modification or equivalent change made based on the technical essence of the present invention still falls within the scope of protection required by the present invention.

Claims

1. A PEEK monofilament preparation system, characterized in that: The invention comprises a multi-stage vacuum drum dryer, a dry slice silo, a screw extruder, a metering pump, a spinning assembly, a cooling device, an oiling device, a bundling device, a multi-stage hot roller stretching and shaping device, a multi-filament winding machine and a wire dividing machine which are sequentially arranged along the preparation direction of PEEK monofilaments; the screw extruder is sequentially divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 30-50% of the total length of the screw, the length of the compression section accounts for 25-35% of the total length of the screw, and the length of the metering section accounts for 25-35% of the total length of the screw; and the screw extruder is sequentially divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 330-380°C, 350-400°C, 380-420°C, 390-440°C, 385-430°C, 385-430°C; the multi-stage hot roller stretching and shaping device comprises The invention comprises a primary stretching hot roller with a roller temperature of 150-200°C and a roller speed of 300-500 m / min for fiber stretching, a secondary stretching hot roller with a roller temperature of 180-240°C and a roller speed of 600-1000 m / min, and a tertiary shaping hot roller with a roller temperature of 180-240°C and a roller speed of 600-1000 m / min for fiber shaping; the cooling device comprises a slow cooling device and a side blowing device arranged in sequence along the preparation direction of PEEK monofilaments, the slow cooling device is used to slowly cool the nascent monofilaments ejected from the spinning assembly to 280-330°C, and the side blowing device is used to cool the nascent monofilaments slowly cooled to 280-330°C by the slow cooling device to room temperature; a tension controller is arranged on the filament separator, and the filament separator controls the tension range of the PEEK monofilaments within 5-20CN through the tension controller.

2. A PEEK monofilament preparation system according to claim 1, characterized in that: The structure of the spinning assembly includes: a shell, a feed port is arranged at the top of the shell, a discharge port is arranged at the bottom of the shell, and an upper filter mesh group, a distribution plate, a lower filter mesh group and a spinneret are arranged in sequence from top to bottom inside the shell, and the spinneret is located at the discharge port of the shell. The upper filter mesh group is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 to 600 meshes; the lower filter mesh group is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 to 800 meshes.

3. A PEEK monofilament preparation system according to claim 1, characterized in that: In the multi-stage vacuum drum dryer, the pre-crystallization temperature of the PEEK resin raw material is 100-140°C, the pre-crystallization time is 2-4 hours, the vacuum pumping speed is 10-20 liters / second, the drum drying temperature is 150-180°C, and the drying time is 3-6 hours.

4. A PEEK monofilament preparation system according to claim 1, characterized in that: A hot air circulation device is provided in the dry slice silo, and the hot air circulation device is used to maintain the temperature of the PEEK resin raw material in the silo at 140-170°C.

5. A PEEK monofilament preparation system according to claim 1, characterized in that: The length of the feed section of the screw extruder accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw.

6. A method for preparing a PEEK monofilament, characterized in that: A PEEK monofilament preparation system as claimed in any one of claims 1 to 5 is used, comprising the following steps: (1) Crystallization, drying and purification: Add the PEEK resin raw material to a multi-stage vacuum drum dryer, and use the multi-stage vacuum drum dryer to pre-crystallize and dry the PEEK resin raw material; wherein the pre-crystallization temperature is 100-140°C, the pre-crystallization time is 2-4 hours, the vacuum pumping speed is 10-20 liters / second, the drum drying temperature is 150-180°C, and the drying time is 3-6 hours; (2) Raw material heating: The crystallized, dried and purified PEEK resin raw material is put into the dry chip silo. The dry chip silo uses hot air circulation to keep the temperature of the PEEK resin raw material in the silo at 140-170°C; (3) Hot melt extrusion: The PEEK resin raw material in the dry slice silo is input into a screw extruder for melt extrusion to obtain a PEEK melt; wherein the screw extruder is divided into a feeding section, a compression section and a metering section along the extrusion direction, the length of the feeding section accounts for 30-50% of the total length of the screw, the length of the compression section accounts for 25-35% of the total length of the screw, and the length of the metering section accounts for 25-35% of the total length of the screw; wherein the screw extruder is divided into six heating temperature zones along the extrusion direction, and the temperature ranges of the six heating temperature zones are: 330-380°C, 350-400°C, 380-420°C, 390-440°C, 385-430°C, 385-430°C; (4) Wire drawing: PEEK melt is first metered by a metering pump and then fed into a spinning assembly. The spinning assembly ejects the PEEK melt to form a number of primary monofilaments. Each primary monofilament is first slowly cooled to 280-330°C by a slow cooling device, then cooled to room temperature by a side blowing device, then oiled by an oiling device, and then bundled by a bundling device to form primary multifilaments. (5) Multi-stage hot roller stretching, shaping and winding: The spun multifilament is first stretched by a primary stretching hot roller and a secondary stretching hot roller, and then shaped by a tertiary shaping hot roller before being sent to a multifilament winding machine for winding; wherein the roller temperature of the primary stretching hot roller is 150-200°C, the roller speed is 300-500 m / min, and the residence time of the spun multifilament on the primary stretching hot roller is 0.5-0.8 seconds; the roller temperature of the secondary stretching hot roller is 180-240°C, the roller speed is 600-1000 m / min, and the residence time of the spun multifilament on the secondary stretching hot roller is 0.3-0.5 seconds; the stretching ratio of the secondary stretching hot roller to the primary stretching hot roller is 1.2-3.3; the roller temperature of the tertiary shaping hot roller is 180-240°C, the roller speed is 600-1000 m / min, and the residence time of the spun multifilament on the tertiary shaping hot roller is 0.3-0.5 seconds; (6) Filament winding: The multifilament wound in the multifilament winding machine is divided into several single filaments by a fiber dividing machine and rewound to make PEEK single filaments; wherein, the fiber dividing machine controls the tension range of the PEEK single filament in the range of 5 to 20 CN through a tension controller.

7. A method for preparing a PEEK monofilament according to claim 6, characterized in that: The structure of the spinning assembly includes: a shell, a feed port is arranged at the top of the shell, a discharge port is arranged at the bottom of the shell, and an upper filter mesh group, a distribution plate, a lower filter mesh group and a spinneret are arranged in sequence from top to bottom inside the shell, and the spinneret is located at the discharge port of the shell. The upper filter mesh group is composed of multiple stacked upper filter meshes, and the mesh number of the upper filter mesh is 300 to 600 meshes; the lower filter mesh group is composed of multiple stacked lower filter meshes, and the mesh number of the lower filter mesh is 400 to 800 meshes.

8. The method for preparing a PEEK monofilament according to claim 6, characterized in that: In step (1), the PEEK resin raw material is dried until the water content is less than 50 ppm.

9. The method for preparing a PEEK monofilament according to claim 6, characterized in that: The length of the feed section of the screw extruder accounts for 40% of the total length of the screw, the length of the compression section accounts for 30% of the total length of the screw, and the length of the metering section accounts for 30% of the total length of the screw.