Process for the preparation of peek monofilaments

Abstract

The application discloses a preparation method of PEEK monofilament, which comprises the following steps: providing a liquid cooling device, wherein the liquid cooling device comprises a liquid storage tank containing cooling liquid and a cooling roller rotatably arranged on the liquid storage tank, the lower end of the cooling roller is in contact with the cooling liquid in the liquid storage tank, and the upper end of the cooling roller is exposed outside; mixing and melt spinning PEEK raw materials to obtain nascent filaments, and cooling the nascent filaments; controlling the rotation of the cooling roller, and making the nascent filaments adhere to the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments; and performing heat stretching on the nascent filaments to obtain the required PEEK monofilament after shaping. According to the preparation method of the PEEK monofilament, a layer of cooling liquid is attached to the surface of the nascent filaments, so that the temperature of the nascent filaments is rapidly reduced, the nascent filaments are rapidly cooled to form non-crystallized transparent nascent filaments, and the non-crystallized transparent nascent filaments are relatively soft, which is beneficial to subsequent high-multiple stretching.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of special fiber preparation, in particular to a preparation method of PEEK monofilament. BACKGROUND

[0002] PEEK material has natural properties of high rigidity, high toughness, flame retardant, corrosion resistance, hydrolysis resistance, ultraviolet resistance, etc., so the monofilament spun by PEEK also has similar excellent performance, and it is widely used in aerospace, electronics, automobiles, military, medical and other fields. However, there is no mature and complete set of PEEK monofilament spinning equipment and spinning process at home and abroad.

[0003] Because the processing temperature of PEEK raw material is about 400℃, the conventional wire drawing machine equipment cannot meet this requirement, and the PEEK raw material spinning process cannot use the traditional PET, PA, PPS process, so the extruder screw and barrel even the metering pump need special processing to meet the extrusion requirements. In addition, PEEK raw material is very expensive, and the development of spinning needs a lot of human and material resources, the application range is small, and the market lacks the grasp of the spinning conditions of PEEK raw material, so the development difficulty is very great. SUMMARY

[0004] Therefore, it is necessary to provide a preparation method of PEEK monofilament which can solve the above problems.

[0005] A preparation method of PEEK monofilament, comprising the following steps:

[0006] A liquid cooling device is provided, which comprises a liquid storage tank containing a cooling liquid and a cooling roller rotatably arranged on the liquid storage tank, the lower end of the cooling roller is in contact with the cooling liquid in the liquid storage tank, and the upper end of the cooling roller is exposed outside;

[0007] The PEEK raw material is mixed and melt spun to obtain a primary filament, and the primary filament is cooled to 240℃-260℃;

[0008] The temperature of the cooling liquid is set to 80℃-95℃, the cooling roller is controlled to rotate, the primary filament cooled to 240℃-260℃ is attached to the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the primary filament, so that the temperature of the primary filament is rapidly reduced to 80℃-150℃;

[0009] The primary filament with the temperature reduced to 80℃-150℃ is subjected to heat stretching, and the required PEEK monofilament is obtained after setting.

[0010] In one embodiment, the surface of the cooling roller is provided with a liquid absorption layer, and the primary filament is attached to the liquid absorption layer located at the upper end of the cooling roller.

[0011] In one embodiment, the speed of the cooling roller is 10 m / min to 60 m / min.

[0012] In one embodiment, the liquid absorbing layer is a cotton layer, and the cooling liquid is water.

[0013] In one embodiment, the operation of cooling the nascent filament to 240°C to 260°C is that the nascent filament is passed through a hot air surge channel with a length of 0.5 m to 4 m at a speed of 10 m / min to 60 m / min, so that the nascent filament is cooled to 240°C to 260°C, wherein the temperature of the hot air surge channel is 80°C to 120°C, and the temperature of the air in the hot air surge channel is 15°C to 60°C.

[0014] In one embodiment, the operation of preparing the nascent filament by mixing and melt spinning the PEEK raw material is that the PEEK raw material is dehumidified and dried, then fed to a single filament extruder hopper, and then passed through a screw for plasticizing and melting after passing through a single filament extruder discharge port, the temperature of the screw is set to 330°C to 360°C, 340°C to 375°C, 360°C to 390°C, 370°C to 400°C, 380°C to 400°C, and 380°C to 400°C from the discharge port area to the spinneret area in turn, and finally the nascent filament is extruded through a spinneret plate.

[0015] In one embodiment, the operation of heat stretching the nascent filament with a temperature reduced to 80°C to 150°C and then shaping to obtain the required PEEK single filament is that the nascent filament with a temperature reduced to 80°C to 150°C is pulled by the rotation of a first hot roller to pass through a first hot air box for primary stretching, then the nascent filament after primary stretching is pulled by the rotation of a second hot roller for secondary stretching, and finally the nascent filament after secondary stretching is shaped to obtain the required PEEK single filament.

[0016] In one embodiment, the temperature of the first hot roller is 100°C to 220°C, and the speed of the first hot roller is 15 m / min to 50 m / min.

[0017] The temperature of the first hot air box is 220°C to 250°C, and the length of the first hot air box is 3 m to 5 m.

[0018] The temperature of the second hot roller is 100°C to 220°C, and the speed of the second hot roller is 30 m / min to 120 m / min.

[0019] The temperature of the second hot air box is 220°C to 250°C, and the length of the second hot air box is 3 m to 5 m.

[0020] In one embodiment, the operation of shaping the primary filaments after the secondary stretching is performed by rotating the third hot roller and the fourth roller to draw the primary filaments after the secondary stretching through the third hot air box and the fourth hot air box in sequence to realize the shaping of the primary filaments after the secondary stretching.

[0021] In one embodiment, the temperature of the third hot roller is 100-220 DEG C, and the temperature of the fourth roller is 20-50 DEG C.

[0022] The speed of the third hot roller and the fourth roller is 40-115 m / min.

[0023] The temperature of the third hot air box and the fourth hot air box is 250-290 DEG C, and the length of the third hot air box and the fourth hot air box is 6-10 m.

[0024] The preparation method of the PEEK monofilament can realize the rapid cooling of the primary filaments to form the non-crystalline transparent primary filaments by controlling the rotation of the cooling roller, adhering the primary filaments cooled to 240-260 DEG C to the upper end of the cooling roller, and making the primary filaments adhere to a layer of cooling liquid with a temperature of 80-95 DEG C on the surface, so that the temperature of the primary filaments is rapidly reduced to 80-150 DEG C, thereby improving the high-temperature stability of the PEEK monofilament prepared finally, reducing the shrinkage of the PEEK monofilament at high temperature, and improving the tensile force of the PEEK monofilament.

[0025] Specifically, the traditional primary filaments are directly cooled by hot air, and the slow cooling of the hot air cooling causes the primary filaments to form crystals, which makes the hot air cooling harden and is not conducive to the subsequent high-stretching.

[0026] In the present application, the primary filaments are adhered to a layer of cooling liquid with a temperature of 80-95 DEG C on the surface by controlling the adhesion of the primary filaments to the upper end of the cooling roller, so that the primary filaments are rapidly cooled to form non-crystalline transparent primary filaments, and the non-crystalline transparent primary filaments are relatively soft and conducive to the subsequent high-stretching.

[0027] In addition, the traditional primary filaments are directly cooled by hot water, and the primary filaments have a large resistance when entering the water, and because the temperature of the primary filaments is high, the direct contact with the hot water causes the heat exchange to be too intense, which causes the primary filaments to vibrate and the appearance and diameter of the primary filaments to change dramatically, which is not conducive to the subsequent high-stretching.

[0028] In the present application, by controlling the adhesion of the nascent yarn to the upper end of the cooling roller, a layer of cooling liquid with a temperature of 80-95 DEG C is attached to the surface of the nascent yarn, on the one hand, there is no problem of water resistance of the nascent yarn, on the other hand, when the nascent yarn contacts the cooling liquid attached to the surface of the cooling roller, the degree of heat exchange is significantly reduced, avoiding the dramatic changes in morphology and diameter caused by the violent shaking of the nascent yarn, which is beneficial to the subsequent high-stretching. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description only show some embodiments of the present application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of these drawings.

[0030] Among them:

[0031] Figure 1 Flow chart of the preparation method of the PEEK monofilament of an embodiment.

[0032] Figure 2 Structure diagram of the liquid cooling device of an embodiment. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the specific embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0034] It should be noted that all directional indications (such as up, down, left, right, front, back, etc.) in the embodiments of the present application are only used to explain the relative position relationship, motion condition, etc. between the objects in a certain posture, and if the posture changes, the directional indications will also change accordingly.

[0035] In addition, the description of "first", "second" and the like in the present application is only for the purpose of description, and cannot be understood as indicating or implying the relative importance of the indicated technical features or implicitly indicating the number of the indicated technical features. Therefore, the features limited by "first", "second" can explicitly or implicitly include at least one of the features. In addition, the technical solutions of each embodiment can be combined with each other, but it must be based on the realization of those skilled in the art, when the combination of technical solutions appears contradictory or unachievable, it should be considered that the combination of technical solutions does not exist, and is not within the scope of protection required by the present application.

[0036] Combination Figure 1 This invention discloses a method for preparing PEEK monofilaments according to one embodiment, comprising the following steps:

[0037] S10, Provide liquid cooling device.

[0038] Combination Figure 2 The liquid cooling device of the present invention includes a storage tank 140 containing coolant 120 and a cooling roller 160 rotatably disposed on the storage tank 140. The lower end of the cooling roller 160 is in contact with the coolant 120 in the storage tank 140, and the upper end of the cooling roller 160 is exposed.

[0039] S20. PEEK raw materials are mixed and melt-spun to obtain nascent filament 200. Nascent filament 200 is cooled to 240℃~260℃.

[0040] Preferably, in this embodiment, the operation of mixing PEEK raw materials and then melt-spinning to obtain nascent filament is as follows: the PEEK raw materials are dehumidified and dried, then fed into the feeding hopper of a monofilament extruder, and then plasticized and melted by the screw after passing through the discharge port of the monofilament extruder. The temperature of the screw from the discharge port area to the spinneret area is set sequentially to 330℃~360℃, 340℃~375℃, 360℃~390℃, 370℃~400℃, 380℃~400℃, and 380℃~400℃. Finally, the nascent filament 200 is extruded through the spinneret.

[0041] It should be noted that the specific steps and process parameters for obtaining nascent filament by melt spinning after mixing PEEK raw materials can be determined according to the actual situation. This invention only provides a solution for reference and should not limit the inventive point of this application.

[0042] Preferably, in this embodiment, the operation of cooling the nascent filament 200 to 240°C to 260°C is as follows: the nascent filament is passed through a hot air surge channel with a length of 0.5m to 4m at a speed of 10m / min to 60m / min, thereby cooling the nascent filament to 240°C to 260°C. The temperature of the hot air surge channel is 80°C to 120°C, and the temperature of the air inside the hot air surge channel is 15°C to 60°C.

[0043] S30. Set the temperature of the coolant 120 to 80℃~95℃, control the rotation of the cooling roller 160, and bring the nascent filament 200, which has been cooled to 240℃~260℃, into contact with the upper end of the cooling roller 160, so that a layer of coolant 120 adheres to the surface of the nascent filament 200, thereby rapidly reducing the temperature of the nascent filament 200 to 80℃~150℃.

[0044] Preferred, combined Figure 2In the embodiment, the surface of the cooling roller 160 is provided with the liquid absorption layer 150, and the nascent yarn 200 is attached to the liquid absorption layer 150 at the upper end of the cooling roller 160.

[0045] The liquid absorption layer 150 can improve the cooling speed of the nascent yarn 200.

[0046] Preferably, in the embodiment, the speed of the cooling roller 160 is 10 m / min to 60 m / min.

[0047] Specifically, in the embodiment, the liquid absorption layer 150 is a cotton layer, and the cooling liquid 120 is water.

[0048] S40, heat stretching the nascent yarn 200 with the temperature reduced to 80℃ to 150℃, and obtaining the required PEEK monofilament after setting.

[0049] Specifically, the operation of heat stretching the nascent yarn 200 with the temperature reduced to 80℃ to 150℃ and obtaining the required PEEK monofilament after setting is as follows: the nascent yarn 200 with the temperature reduced to 80℃ to 150℃ is pulled through the first hot air box by the rotation of the first heat roller for primary stretching, then the nascent yarn 200 after the primary stretching is pulled for secondary stretching by the rotation of the second heat roller, and finally the nascent yarn 200 after the secondary stretching is set to obtain the required PEEK monofilament.

[0050] Preferably, in the embodiment, the temperature of the first heat roller is 100℃ to 220℃, and the speed of the first heat roller is 15 m / min to 50 m / min.

[0051] Preferably, in the embodiment, the temperature of the first hot air box is 220℃ to 250℃, and the length of the first hot air box is 3 m to 5 m.

[0052] Preferably, in the embodiment, the temperature of the second heat roller is 100℃ to 220℃, and the speed of the second heat roller is 30 m / min to 120 m / min.

[0053] Preferably, in the embodiment, the temperature of the second hot air box is 220℃ to 250℃, and the length of the second hot air box is 3 m to 5 m.

[0054] Considering that the temperature of hot water is not enough to reach the glass transition temperature (Tg: 150℃) of PEEK, it is not enough to make the PEEK molecular chain stretch and orient. Therefore, in the present application, the temperature of the nascent PEEK yarn is heated to 200℃ to 300℃ by the heat roller and the hot air box for stretching.

[0055] Specifically, in the present application, the first hot roller and the second hot roller are used to keep the overall temperature of the PEEK primary filament consistent, and the hot air of the first hot air box and the second hot air box needs a certain time to conduct heat, so the first hot roller and the second hot roller can be heated to a certain temperature in advance, which is convenient for complete stretching (i.e. high-stretching), thereby greatly improving the strength of the PEEK monofilament finally prepared.

[0056] Specifically, the operation of shaping the secondary-stretched primary filament 200 is that the third hot roller and the fourth roller rotate to pull the secondary-stretched primary filament 200 through the third hot air box and the fourth hot air box in turn, so as to shape the secondary-stretched primary filament 200.

[0057] Specifically, the temperature of the third hot roller is 100℃-220℃, and the temperature of the fourth roller is 20℃-50℃.

[0058] Specifically, the speed of the third hot roller and the fourth roller is 40m / min-115m / min.

[0059] Specifically, the temperature of the third hot air box and the fourth hot air box is 250℃-290℃, and the length of the third hot air box and the fourth hot air box is 6m-10m.

[0060] It should be pointed out that the specific stretching and shaping steps and process parameters can be determined according to actual conditions, and the present application only gives a reference solution, which should not limit the invention points of the present application.

[0061] The preparation method of the PEEK monofilament of the present application controls the rotation of the cooling roller 160 to make the primary filament 200 cooled to 240℃-260℃ adhere to the upper end of the cooling roller 160, so that a layer of cooling liquid with a temperature of 80℃-95℃ is attached to the surface of the primary filament 200, thereby rapidly reducing the temperature of the primary filament 200 to 80℃-150℃, so that the primary filament 200 is rapidly cooled to form a non-crystalline transparent primary filament, which is relatively soft and is beneficial to subsequent high-stretching, thereby improving the high-temperature stability of the PEEK monofilament finally prepared, reducing the shrinkage of the PEEK monofilament at high temperature, and improving the tensile strength of the PEEK monofilament.

[0062] Specifically, the traditional primary filament direct hot air surge cooling method is slow cooling, which will cause the primary filament to form crystals, resulting in hardening of the hot air surge cooling, which is not conducive to subsequent high-stretching.

[0063] In the application, the nascent filament 200 is attached to the upper end of the cooling roller 160, so that a layer of cooling liquid with a temperature of 80-95℃ is attached to the surface of the nascent filament 200, which can rapidly cool the nascent filament 200 to form a non-crystallized transparent nascent filament 200. The non-crystallized transparent nascent filament is relatively soft, which is beneficial to subsequent high-stretching.

[0064] In addition, in the traditional direct hot water cooling method of nascent filament, the nascent filament has a large resistance when entering the water. Since the nascent filament has a high temperature, the nascent filament directly contacts with the hot water, and the heat exchange is too intense, which can cause the nascent filament to shake, so that the appearance and diameter of the nascent filament change dramatically, which is not conducive to subsequent high-stretching.

[0065] In the application, the nascent filament 200 is attached to the upper end of the cooling roller 160, so that a layer of cooling liquid with a temperature of 80-95℃ is attached to the surface of the nascent filament 200. On the one hand, there is no problem of water resistance of the nascent filament 200, and on the other hand, when the nascent filament 200 contacts with the cooling liquid attached to the surface of the cooling roller 160, the heat exchange is significantly reduced, which avoids the dramatic changes in the appearance and diameter of the nascent filament 200 caused by the dramatic shaking of the nascent filament 200, and is beneficial to subsequent high-stretching.

[0066] The following is a specific embodiment.

[0067] In the specific embodiment, the PEEK raw material is PEEK 150G of Jilin Zhongyan High Polymer Material Co., Ltd. _550G ， The liquid cooling device is shown in FIG. 1, the cooling liquid is water, and the liquid absorbing layer is cotton. Figure 2

[0068] Embodiment 1

[0069] After the PEEK raw material is dehumidified and dried, it is conveyed to the hopper of the single filament extruder. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then, the material is plasticized and melted by the screw with a length-diameter ratio of 30:1 through the discharge port of the single filament extruder. The temperature of the screw is set to 355℃, 360℃, 365℃, 370℃, 375℃ and 375℃ from the discharge port area to the spinneret area, respectively. Finally, the nascent filament is extruded through the spinneret.

[0070] The nascent filament is passed through the hot air surge channel with a length of 2m at a speed of 20m / min, so that the nascent filament is cooled to 250℃. The temperature of the hot air surge channel is 100℃, and the temperature of the air in the hot air surge channel is 35℃.

[0071] ​The temperature of the cooling liquid is set to 90°C, and the cooling roller is controlled to rotate, so that the nascent yarn is attached to the liquid absorption layer at the upper end of the cooling roller, and a layer of cooling liquid is attached to the surface of the nascent yarn, so that the temperature of the nascent yarn is rapidly reduced to 80°C-150°C. The speed of the cooling roller is 20 m / min.

[0072] The nascent yarn with a temperature of 120°C-200°C is pulled through the first hot air box by the rotation of the first hot roller to perform primary stretching, and then the nascent yarn after primary stretching is pulled through the second hot air box by the rotation of the second hot roller to perform secondary stretching, and finally the nascent yarn after secondary stretching is pulled through the third hot air box and the fourth hot air box by the rotation of the third roller and the fourth roller in turn to realize the setting of the nascent yarn after secondary stretching. The temperature of the first hot roller is 200°C, the speed is 20 m / min, the temperature of the second hot roller is 200°C, the speed is 40 m / min, the temperature of the third hot roller is 200°C, the speed is 60 m / min, the temperature of the fourth roller is normal temperature 35°C, the speed is 55 m / min. The temperature of the first hot air box is 250°C, the length is 4 m, the temperature of the second hot air box is 260°C, the length is 4 m, the temperature of the third and fourth hot air boxes is 290°C, and the length is 8 m.

[0073] Example 2

[0074] After the PEEK raw material is dehumidified and dried, it is conveyed to the single yarn extruder hopper. The dehumidification and drying temperature is 150°C, and the dehumidification and drying time is 8H. Then it passes through the screw with a length-diameter ratio of 30:1 after the single yarn extruder discharge port for plasticizing and melting. The temperature of the screw from the discharge port area to the spinneret area is set to 355°C, 360°C, 365°C, 370°C, 375°C, 375°C in turn, and finally the nascent yarn is extruded through the spinneret plate.

[0075] The nascent yarn is passed through the hot air channel with a length of 2 m at a speed of 20 m / min, so that the nascent yarn is cooled to 240°C. The temperature of the hot air channel is 100°C, and the temperature of the air in the hot air channel is 35°C.

[0076] The temperature of the cooling liquid is set to 80°C, and the cooling roller is controlled to rotate, so that the nascent yarn is attached to the liquid absorption layer at the upper end of the cooling roller, and a layer of cooling liquid is attached to the surface of the nascent yarn, so that the temperature of the nascent yarn is rapidly reduced to 80°C-150°C. The speed of the cooling roller is 20 m / min.

[0077] The nascent filaments with the temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 200℃, the speed is 20m / min, the second hot roller temperature is 200℃, the speed is 40m / min, the third hot roller temperature is 200℃, the speed is 60m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 55m / min. The first hot air box temperature is 250℃, the length is 4m, the second hot air box temperature is 260℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0078] Example 3

[0079] The PEEK raw material is dehumidified and dried, and then conveyed to the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material passes through the screw with a length-diameter ratio of 30:1 for plasticizing and melting. The screw temperature from the discharge port to the spinneret port is set as 360℃, 365℃, 370℃, 375℃, 380℃, 375℃ in sequence. Finally, the nascent filaments are extruded through the spinneret plate.

[0080] The nascent filaments pass through the hot air surge passage with a length of 3m at a speed of 20m / min, so that the nascent filaments are cooled to 250℃. The hot air surge passage temperature is 100℃, and the air temperature in the hot air surge passage is 35℃.

[0081] The temperature of the cooling liquid is set to 90℃, and the cooling roller is controlled to rotate. The nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 20m / min.

[0082] The nascent filaments with the temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 200℃, the speed is 20m / min, the second hot roller temperature is 200℃, the speed is 40m / min, the third hot roller temperature is 200℃, the speed is 60m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 55m / min. The first hot air box temperature is 250℃, the length is 4m, the second hot air box temperature is 260℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0083] Example 4

[0084] The PEEK raw material is dehumidified and dried, and then conveyed to the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material passes through the screw with a length-diameter ratio of 30:1 for plasticizing and melting. The screw temperature from the discharge port to the spinneret port is set as 360℃, 365℃, 370℃, 375℃, 380℃, 375℃ in sequence. Finally, the nascent filaments are extruded through the spinneret plate.

[0085] The nascent filaments pass through the hot air surge passage with a length of 3m at a speed of 20m / min, so that the nascent filaments are cooled to 250℃. The hot air surge passage temperature is 100℃, and the air temperature in the hot air surge passage is 35℃.

[0086] The temperature of the cooling liquid is set to 90℃, and the cooling roller is controlled to rotate. The nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 20m / min.

[0087] The nascent filaments with the temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 150℃, the speed is 20m / min, the second hot roller temperature is 150℃, the speed is 40m / min, the third hot roller temperature is 150℃, the speed is 60m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 55m / min. The first hot air box temperature is 240℃, the length is 4m, the second hot air box temperature is 250℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0088] Example 5

[0089] The PEEK raw material is dehumidified and dried, and then conveyed to the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material passes through the single-filament extruder discharge port and is plasticized and melted by the screw with a length-diameter ratio of 30:1. The screw temperature from the discharge port area to the spinneret area is set as 365℃, 380℃, 390℃, 395℃, 390℃, and 385℃ in sequence. Finally, the nascent filaments are extruded through the spinneret plate.

[0090] The nascent filaments pass through the hot air surge passage with a length of 3m at a speed of 20m / min, so that the nascent filaments are cooled to 250℃. The hot air surge passage temperature is 100℃, and the air temperature in the hot air surge passage is 35℃.

[0091] The temperature of the cooling liquid is set to 90℃, and the cooling roller is controlled to rotate. The nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 20m / min.

[0092] The nascent filaments with temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 150℃, the speed is 20m / min, the second hot roller temperature is 150℃, the speed is 40m / min, the third hot roller temperature is 150℃, the speed is 50m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 45m / min. The first hot air box temperature is 250℃, the length is 4m, the second hot air box temperature is 260℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0093] Example 6

[0094] The PEEK raw material is dehumidified and dried, and then conveyed to the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material passes through the single-filament extruder discharge port and is plasticized and melted by the screw with a length-diameter ratio of 30:1. The screw temperature from the discharge port area to the spinneret area is set as 365℃, 380℃, 390℃, 395℃, 390℃, and 385℃ in sequence. Finally, the nascent filaments are extruded through the spinneret plate.

[0095] The nascent filaments pass through the hot air surge passage with a length of 3m at a speed of 15m / min, so that the nascent filaments are cooled to 260℃. The hot air surge passage temperature is 150℃, and the air temperature in the hot air surge passage is 35℃.

[0096] The temperature of the cooling liquid is set to 90℃, the cooling roller is controlled to rotate, and the nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 15m / min.

[0097] The nascent filaments with temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 150℃, the speed is 15m / min, the second hot roller temperature is 150℃, the speed is 30m / min, the third hot roller temperature is 150℃, the speed is 45m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 40m / min. The first hot air box temperature is 250℃, the length is 4m, the second hot air box temperature is 260℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0098] Example 7

[0099] The PEEK raw material is dehumidified and dried before being fed into the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material passes through the single-filament extruder discharge port and is plasticized and melted by the screw with a length-diameter ratio of 30:1. The screw temperature from the discharge port area to the spinneret area is set as 365℃, 380℃, 390℃, 395℃, 390℃, 385℃ in sequence. Finally, the nascent filaments are extruded through the spinneret.

[0100] The nascent filaments pass through the hot air surge passage with a length of 3m at a speed of 25m / min, so that the nascent filaments are cooled to 240℃. The hot air surge passage temperature is 150℃, and the air temperature in the hot air surge passage is 35℃.

[0101] The temperature of the cooling liquid is set to 90℃, and the cooling roller is controlled to rotate. The nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 25m / min.

[0102] The nascent filaments with temperature reduced to 120-200℃ are drawn by the first hot roller rotation to perform first stretching, then the first stretched nascent filaments are drawn by the second hot roller rotation to perform second stretching, and finally the second stretched nascent filaments are drawn by the third and fourth roller rotation to pass through the third and fourth hot air boxes in sequence to realize the setting of the second stretched nascent filaments. The first hot roller temperature is 150℃, the speed is 25m / min, the second hot roller temperature is 150℃, the speed is 50m / min, the third hot roller temperature is 150℃, the speed is 75m / min, the fourth roller temperature is normal temperature 35℃, and the speed is 70m / min. The first hot air box temperature is 250℃, the length is 4m, the second hot air box temperature is 260℃, the length is 4m, and the third and fourth hot setting air box temperature is 290℃, the length is 8m.

[0103] Example 8

[0104] The PEEK raw material is dehumidified and dried before being fed into the single-filament extruder hopper. The dehumidification and drying temperature is 150℃, and the dehumidification and drying time is 8H. Then the material is plasticized and melted by the screw with a length-diameter ratio of 30:1 after passing through the single-filament extruder discharge port. The screw temperature from the discharge port area to the spinneret area is set as 365℃, 380℃, 390℃, 395℃, 390℃, 385℃ in sequence. Finally, the nascent filaments are extruded through the spinneret.

[0105] The nascent filaments are passed through the hot air surge passage with a length of 3m at a speed of 20m / min, so that the nascent filaments are cooled to 260℃. The hot air surge passage temperature is 150℃, and the air temperature in the hot air surge passage is 45℃.

[0106] The temperature of the cooling liquid is set to 90℃, and the cooling roller is controlled to rotate. The nascent filaments are attached to the liquid absorption layer located at the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filaments, thereby rapidly reducing the temperature of the nascent filaments to 80-150℃. The speed of the cooling roller is 20m / min.

[0107] The nascent filaments with temperature reduced to 120-200°C are drawn by the rotation of the first hot roller to perform primary stretching through the first hot air box, then the nascent filaments after primary stretching are drawn by the rotation of the second hot roller to perform secondary stretching, and finally the nascent filaments after secondary stretching are drawn by the rotation of the third and fourth rollers to sequentially pass through the third and fourth hot air boxes to realize the setting of the nascent filaments after secondary stretching. The first hot roller has a temperature of 150°C and a speed of 20 m / min, the second hot roller has a temperature of 150°C and a speed of 40 m / min, the third hot roller has a temperature of 150°C and a speed of 60 m / min, and the fourth roller has a temperature of normal temperature 35°C and a speed of 55 m / min. The first hot air box has a temperature of 250°C and a length of 4 m, the second hot air box has a temperature of 260°C and a length of 4 m, and the third and fourth setting hot air boxes have a temperature of 290°C and a length of 8 m.

[0108] Comparative Example 1

[0109] The PEEK raw material is dehumidified and dried before being fed into the hopper of the single-filament extruder. The dehumidification and drying temperature is 150°C, and the dehumidification and drying time is 8H. Then the material passes through the screw with a length-diameter ratio of 30:1 for plasticizing and melting. The temperature of the screw from the hopper zone to the spinneret zone is set to 365°C, 380°C, 390°C, 395°C, 390°C, and 385°C in sequence. Finally, the nascent filaments are extruded through the spinneret.

[0110] The nascent filaments pass through the hot air channel with a length of 3 m at a speed of 20 m / min, so that the nascent filaments are cooled to 280°C. The temperature of the hot air channel is 100°C, and the temperature of the air in the hot air channel is 35°C.

[0111] The nascent filaments with temperature reduced to 150-250°C are drawn by the rotation of the first hot roller to perform primary stretching through the first hot air box, then the nascent filaments after primary stretching are drawn by the rotation of the second hot roller to perform secondary stretching, and finally the nascent filaments after secondary stretching are drawn by the rotation of the third and fourth rollers to sequentially pass through the third and fourth hot air boxes to realize the setting of the nascent filaments after secondary stretching. The first hot roller has a temperature of 150°C and a speed of 20 m / min, the second hot roller has a temperature of 150°C and a speed of 40 m / min, the third hot roller has a temperature of 150°C and a speed of 60 m / min, and the fourth roller has a temperature of normal temperature 35°C and a speed of 55 m / min. The first hot air box has a temperature of 250°C and a length of 4 m, the second hot air box has a temperature of 260°C and a length of 4 m, and the third and fourth setting hot air boxes have a temperature of 290°C and a length of 8 m.

[0112] Test Example

[0113] The PEEK monofilament prepared by example 8 and comparative example 1 was detected in diameter and tested in performance, and the test results were shown in table 1.

[0114] The test method was ISO 2062-2009, wherein the specific method was set with a gauge length of 250 mm and a tensile speed of 250 mm / min for tensile test. The tensile testing instrument was a universal material testing machine CREE-8007B of Metzler, and the dry heat shrinkage rate testing instrument was an aging oven PHH201 of Guangzhou Wusuo Environmental Instrument Co., Ltd.

[0115] Table 1

[0116]

[0117] As shown in table 1, the PEEK monofilament prepared by example 8 was obviously superior to the PEEK monofilament prepared by comparative example 1 in tensile strength, dry heat shrinkage rate, elongation at break and monofilament tension.

[0118] The above embodiments only express several embodiments of the present application, which are described in detail and specifically, but should not be understood as the limitation to the patent application scope. It should be pointed out that, for the ordinary skilled in the art, several modifications and improvements can be made without departing from the concept of the present application, which all belong to the protection scope of the present application. Therefore, the protection scope of the present application patent should be subject to the appended claims.

Claims

1. A method of making a PEEK monofilament, characterized in that, The method comprises the following steps: Providing a liquid cooling device, which comprises a liquid storage tank containing cooling liquid and a cooling roller rotatably arranged on the liquid storage tank, and a liquid absorption layer is arranged on the surface of the cooling roller; the lower end of the cooling roller is in contact with the cooling liquid in the liquid storage tank, and the upper end of the cooling roller is exposed to the outside; The PEEK raw material is mixed and melt-spun to obtain a nascent filament, and the nascent filament is passed through a hot air surge channel with a length of 0.5 m to 4 m at a speed of 10 m / min to 60 m / min, so that the nascent filament is cooled to 240 DEG C to 260 DEG C, wherein the temperature of the hot air surge channel is 80 DEG C to 120 DEG C, and the temperature of the air in the hot air surge channel is 15 DEG C to 60 DEG C; The temperature of the cooling liquid is set to 80 DEG C to 95 DEG C, the rotation of the cooling roller is controlled, the speed of the cooling roller is 10 m / min to 60 m / min, the nascent filament cooled to 240 DEG C to 260 DEG C is attached to the liquid absorption layer on the upper end of the cooling roller, so that a layer of cooling liquid is attached to the surface of the nascent filament, thereby rapidly reducing the temperature of the nascent filament to 80 DEG C to 150 DEG C; The nascent filament with the temperature reduced to 80 DEG C to 150 DEG C is subjected to heat stretching, and the desired PEEK monofilament is obtained after shaping.

2. The method of claim 1, wherein the PEEK monofilament is prepared by the steps of: The liquid absorption layer is a cotton layer, and the cooling liquid is water.

3. The method of claim 1, wherein the PEEK monofilament is prepared by the steps of: The operation of mixing and melt-spinning the PEEK raw material to obtain a nascent filament is as follows: the PEEK raw material is dehumidified and dried, then fed to the single-filament extruder hopper, then passed through the screw for plasticizing and melting after the single-filament extruder discharge port, the temperature of the screw from the discharge port area to the spinneret area is set to 330 DEG C to 360 DEG C, 340 DEG C to 375 DEG C, 360 DEG C to 390 DEG C, 370 DEG C to 400 DEG C, 380 DEG C to 400 DEG C, and 380 DEG C to 400 DEG C in sequence, and finally the nascent filament is extruded through the spinneret plate.

4. The method of claim 1, wherein the PEEK monofilament is prepared by the steps of: The operation of heat stretching the nascent filament with the temperature reduced to 80 DEG C to 150 DEG C and shaping to obtain the desired PEEK monofilament is as follows: the nascent filament with the temperature reduced to 80 DEG C to 150 DEG C is pulled by the rotation of the first heat roller to pass through the first hot air oven for primary stretching, then the nascent filament after primary stretching is pulled by the rotation of the second heat roller for secondary stretching, and finally the nascent filament after secondary stretching is shaped to obtain the desired PEEK monofilament.

5. The method of claim 4, wherein the PEEK monofilament is prepared by the steps of: The temperature of the first heat roller is 100 DEG C to 220 DEG C, and the speed of the first heat roller is 10 m / min to 60 m / min. The temperature of the first hot air oven is 220 DEG C to 260 DEG C, and the length of the first hot air oven is 3 m to 5 m. The temperature of the second heat roller is 100 DEG C to 220 DEG C, and the speed of the second heat roller is 30 m / min to 120 m / min.

6. The method of claim 4, wherein the PEEK monofilament is prepared by the steps of: The operation of shaping the nascent filament after secondary stretching is as follows: the nascent filament after secondary stretching is pulled by the rotation of the third heat roller and the fourth roller to pass through the third hot air oven and the fourth hot air oven in sequence, so as to shape the nascent filament after secondary stretching.

7. The method of claim 6, wherein the PEEK monofilament is prepared by the steps of: The temperature of the third hot roller is 100-220℃, and the temperature of the fourth roller is 20-50℃; The speed of the third hot roller and the fourth roller is 40-115m / min; The temperature of the third hot air box and the fourth hot air box is 250-300℃, and the length of the third hot air box and the fourth hot air box is 6-10m.

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