CN114481372B - Method for recovering solvent in fiber spinning process and fiber spinning system - Google Patents

Method for recovering solvent in fiber spinning process and fiber spinning system Download PDF

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Publication number
CN114481372B
CN114481372B CN202011148954.9A CN202011148954A CN114481372B CN 114481372 B CN114481372 B CN 114481372B CN 202011148954 A CN202011148954 A CN 202011148954A CN 114481372 B CN114481372 B CN 114481372B
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China
Prior art keywords
drying
temperature
solvent
air outlet
air
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CN114481372A (en
Inventor
孔凡敏
赵运生
于品华
张叶
徐莉
吴小莲
苏豪
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F13/00Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
    • D01F13/04Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of synthetic polymers
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06Washing or drying
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00Complete machines for producing artificial threads
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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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)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention relates to a method and a spinning system for recovering a solvent in a fiber spinning process, wherein the fiber spinning process comprises the steps of extruding and spinning a spinning solution, sequentially carrying out a cooling forming process, a drying process and a stretching process on a fiber precursor obtained by spinning, and recovering the solvent in the cooling forming process and the drying process. According to the invention, the solvents in the solvent are recovered in different modes through different working procedures, so that lower energy consumption and higher solvent recovery rate can be realized.

Description

Method for recovering solvent in fiber spinning process and fiber spinning system
Technical Field
The invention relates to the field of fiber spinning, in particular to a method for recycling solvent in a fiber spinning process and a fiber spinning system.
Background
Since the technology for producing ultra-high molecular weight polyethylene fibers by a gel spinning method was invented by P.Smith and P.J.Lemstra of the Dutch DSM company in 1979, two technological routes of dry spinning and wet spinning are formed successively through years of development, and large-scale industrialization is carried out worldwide.
CN109666976a proposes a method for improving the performance of polyethylene fiber products, which adopts a water bath quenching mode to improve the crystallization orientation degree of the fibers, thereby improving the performance of the fibers.
Disclosure of Invention
The invention aims to solve the problem of low solvent recovery rate in the prior art, and provides a novel method for recovering solvent in a fiber spinning process and a fiber spinning system.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for recovering a solvent in a fiber spinning process comprising extruding and spinning a spinning solution, sequentially performing a cooling molding process, a drying process and a drawing process on a fiber precursor obtained by spinning, and recovering the solvent in the cooling molding process and the drying process, wherein the solvent in the cooling molding process is recovered by a cyclone separation method, and the solvent in the drying process is recovered by a combination of cryogenic separation and adsorption desorption.
The second aspect of the invention provides a fiber spinning system, which comprises a melt extrusion unit, a spinning unit, a cooling forming unit, a drying unit, a stretching unit, a winding unit and a solvent recovery unit, wherein the melt extrusion unit is used for providing molten spinning raw materials for the spinning unit, the cooling forming unit and the drying unit are respectively used for cooling forming and drying solvent removal of fiber precursors spun by the spinning unit, the stretching unit is used for stretching the fiber precursors dried by the drying unit, and the solvent recovery unit is used for recovering the solvent; the solvent unit is characterized by comprising a cyclone separation device, a cryogenic separation device and an adsorption and desorption device, wherein the cyclone separation device is used for recovering the solvent in the cooling forming unit, and the cryogenic separation device and the adsorption and desorption device are used for recovering the solvent in the drying process.
According to the invention, the solvents in the solvent are recovered in different modes through different working procedures, so that lower energy consumption and higher solvent recovery rate can be realized. The invention can effectively improve the drying efficiency of materials and further improve the effect of fiber products by the cooperation with the drying hot box with the air knife with a specific structure. And the air outlet quantity and the air outlet direction of the air knife air outlet are adjustable, so that the air knife is more flexible to use and can adapt to various use requirements. By adopting the method of the invention, the recovery rate of the solvent can reach more than 95 percent.
Drawings
FIG. 1 is a schematic view of the structure of an embodiment of a knife according to the present invention;
FIG. 2 is a cross-sectional view of the inner and outer drums of FIG. 1;
FIG. 3 is a schematic view of the mobile flange of FIG. 1;
FIG. 4 is a schematic view of the mounting flange of FIG. 1;
fig. 5 is a schematic diagram of an embodiment of a fiber spinning system of the present invention.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, left, right" are used to refer generally to the orientation shown in the drawings. "inner and outer" means inner and outer relative to the contour of the respective parts themselves.
In the invention, the cooling forming process adopts a low-temperature quenching mode, so that the solvent volatility in the cooling forming process is low, the solvent is basically absent in a gas phase, the mixed gas exists in an aerosol form, and the separation of the coolant (particularly the gas for cooling) and the solvent can be realized only by a simple separation mode such as cyclone separation for the gas, thereby realizing the recycling of the coolant and the solvent. The temperature of the gas in the drying section is higher, a large amount of solvent volatilizes, and the separation of the drying gas and the solvent can be better realized by adopting a deep separation mode. Therefore, the invention adopts the mode of sectionally treating the return air with different temperature points, thereby realizing the reasonable distribution of the energy consumption in the system and achieving the recovery rate of the solvent more than 95 percent. Preferably, the deep separation mode adopts an integrated mode of cooling separation, cryogenic separation, compression, cooling separation and adsorption and desorption, wherein the cooling separation temperature is controlled to be less than 40 ℃, and the cryogenic separation temperature is controlled to be less than-5 ℃, so that the solvent recovery rate is more than 95%, the gas is recycled, and the solvent is recovered and recycled. In the present invention, therefore, the method of recovering the solvent in the fluid after cooling molding is a cyclone separation method, and the method of recovering the solvent in the dry gas is a method of combining cryogenic separation and adsorption/desorption.
Preferably, the temperature of the cyclone is <40 ℃, preferably 10-30 ℃.
In the present invention, the low-temperature quenching is performed by quenching the fiber filaments ejected through the spinneret orifices with a fluid having a temperature of not more than-10 ℃. The prior art method uses gas above 0 ℃ for cooling, both the dry method and the wet method. The inventor of the present invention has found through research that although the temperature of the gas above 0 ℃ is very low relative to the temperature of the spinning (fiber precursor) sprayed from the nozzle, the temperature difference is relatively large, and the mechanical properties and product stability of the fiber product can be further improved by using the fluid below-10 ℃. The reason for this is probably because the melt is in a uniform state before entering the spinneret plate for extrusion, and the internal folding chain structure is stable; after extrusion, the surface is cooled and rapidly solidified, so that the stable folding chain structure inside the precursor is ensured not to change, and after being further heated and drawn, the folding chain inside the precursor is gradually stretched into a stable lattice structure. Therefore, the quenching time of the precursor is shortened, the internal stable structure of the fiber can be protected to the greatest extent, and the spinnability of the fiber is improved.
In theory, fluids having a temperature below-10℃may be used in the present invention, but it is preferred that the temperature of the fluid used for cooling forming is-10 to-180℃preferably-10 to-50℃more preferably-20 to-30℃in view of the combined energy consumption and fiber product properties.
The curing of the gel silk is accelerated by adopting low-temperature wind, the lower the temperature is, the shorter the curing and forming time is, so that the gel silk is ensured not to be interfered by wind speed, the stable structure inside the gel silk is maintained, and meanwhile, the adhesion condition of the gel silk can be effectively avoided.
The fluid may be a gas or a liquid, and inert fluids that adversely affect the filament product may be used to achieve the objects of the present invention, as long as they do not react with the filament product. For example, one or more of liquid ammonia, liquid nitrogen, air, an aqueous glycol solution, an aqueous ethanol solution, and the like may be used.
The fluid for cooling molding is preferably a gas. For the dry spinning process, inert gas such as nitrogen is used, and air is not used.
The contact method is preferably blowing, and the blowing method is preferably circular blowing around the blown fiber strands. The circumferential blowing is to blow a quenching fluid around the fiber filaments, which is used for cooling the fiber filaments, to sufficiently cool the fiber filaments.
According to a preferred embodiment of the invention, the blowing time is 0.1 to 1 second, preferably 0.5 to 0.7 seconds, and the pressure is 0 to 100kPa, preferably 3 to 10kPa. The time of blowing refers to the period of time from when the filaments come into contact with the quench fluid to when they leave the quench fluid. The pressure herein refers to the pressure at which quench fluid exits, and is the gauge pressure.
In the invention, the blowing process is a continuous and stable process, the blowing effect is related to the stretching speed of the nozzle, and the faster the speed is, the shorter the time of blowing on the unit filament bundle is. When the die draw ratio is 8 times, the die extrusion rate is preferably 2 to 5m/min, more preferably 3 to 3.5m/min.
The low-temperature, ring-blow-drying and air-quenching molding mode provided by the invention can be suitable for the existing wet process and the dry process. Preferably suitable for dry processes. The cooperation of the above-described quench forming regime with the dry process is further described below.
Preferably, the combination of cryogenic separation and adsorption and desorption is that the cryogenic separation is performed first and then the adsorption and desorption is performed.
Preferably, the cryogenic separation temperature is < -5 ℃, preferably-20 to-10 ℃.
Preferably, the adsorption is performed by contacting the gas from the drying step with the adsorbent.
In the present invention, the volume space velocity of gas refers to the volume of gas that passes through a unit volume of adsorbent per unit time.
According to a preferred mode of the invention, the adsorbent is one or more of activated carbon, coconut carbon and molecular sieve, preferably cylindrical activated carbon with a diameter of 3-6 mm.
Preferably, the desorption conditions comprise desorption temperature of 5-25 ℃ and desorption pressure of 0.1-5MPa.
The method of the present invention is suitable for dry spinning process and wet spinning process, wherein the spinning solution is extruded and spun, and the spinning fiber precursor is dried and stretched in sequence.
The spinning solution generally contains polyethylene, a solvent and an auxiliary agent, preferably, the weight ratio of polyethylene to solvent is 1-30:100, preferably 4-20:100, and the weight ratio of auxiliary agent to polyethylene is 0.3-3:100, preferably 0.5-2:100.
The solvent is preferably one or more of decalin, tetrahydronaphthalene, toluene, xylene, white oil and paraffin oil.
In the present invention, for convenience of description, the fiber filaments before being drawn after spinning are referred to as fiber precursors or gel filaments, and the drawn product is referred to as a fiber product.
In the present invention, the fibers may be one or more of various plastic filament products such as polyethylene, acrylic, and the like.
The spin aid may be one or more of various substances that aid in the spinning process, such as antioxidants, plasticizers, modifiers and lubricants.
In the present invention, the stretching magnification of the stretching is 160 to 300, preferably 200 to 240. The stretching may be performed once or in multiple times, preferably in multiple times. When performed in multiple passes, the stretch ratio refers to the total stretch ratio.
Draw ratio refers to the length of the drawn fiber product/the length of the fiber precursor after cooling formation.
Preferably, the spray head stretching is 6-9 times, the pre-spinning pre-stretching multiplying power is 3-3.5 times, and the post-spinning stretching multiplying power is 7-8 times.
Preferably, the method of the present invention further comprises winding the drawn fiber product for convenience of product storage.
In the present invention, the cooling forming means comprises contacting the fiber strands with a fluid having a temperature of not more than-10 ℃. Preferably, the temperature of the fluid used for cooling the molding is-10 to-180 ℃, preferably-10 to-50 ℃, more preferably-20 to-30 ℃.
Preferably, the fluid is a gas, the contacting means is blowing, preferably the blowing means is circular blowing around the fiber precursor. Preferably, the blowing time is from 0.5 to 0.7 seconds and the pressure is from 0 to 100kPa, preferably from 3 to 10kPa.
Preferably, the fluid used for cooling the molding is one or more of liquid nitrogen, air, and inert gas.
Preferably, the drying means comprises contacting the cooled shaped fiber filaments with a drying gas having a velocity of not less than 20 m/s, preferably 30-40 m/s.
Preferably, the temperature of the drying gas is from 0 to 140 ℃, preferably from 40 to 80 ℃.
The invention provides a fiber spinning system, which comprises a melt extrusion unit, a spinning unit, a cooling forming unit, a drying unit, a stretching unit, a winding unit and a solvent recovery unit, wherein the melt extrusion unit is used for providing molten spinning raw materials for the spinning unit, the cooling forming unit and the drying unit are respectively used for cooling forming and drying for removing solvent from fiber precursors spun by the spinning unit, the stretching unit is used for stretching the fiber precursors dried by the drying unit, and the solvent recovery unit is used for recovering the solvent; the solvent unit is characterized by comprising a cyclone separation device, a cryogenic separation device and an adsorption and desorption device, wherein the cyclone separation device is used for recovering the solvent in the cooling forming unit, and the cryogenic separation device and the adsorption and desorption device are used for recovering the solvent in the drying process.
Preferably, the cryogenic separation device and the adsorption and desorption device are connected in sequence and are used for sequentially carrying out cryogenic separation and adsorption and desorption separation on the solvent in the drying process; preferably, the cryogenic separation plant comprises a cooler, a chiller and a gas-liquid separator connected in sequence.
Preferably, the adsorbent in the adsorption and desorption device is one or more of activated carbon, coconut shell carbon and molecular sieve, preferably cylindrical activated carbon with the diameter of 3-6 mm.
The air knife 60 comprises an inner cylinder 61 and an outer cylinder 62 coaxially sleeved, one end of the inner cylinder 61 is provided with an air inlet 611 for forming the air knife 60, a first air outlet 612 communicated with the air inlet 611 is formed in the wall of the inner cylinder 61, a second air outlet 621 (the second air outlet 621 is the air outlet of the air knife 60) is formed in the wall of the outer cylinder 62, a radial interval is formed between the inner cylinder 61 and the outer cylinder 62 for forming a communication channel 63 for communicating the first air outlet 612 and the second air outlet 621, and at least one of the inner cylinder 61 and the outer cylinder 62 is arranged to move along the radial direction of the air knife 60 for adjusting the air outlet quantity and the air outlet direction of the second air outlet 621.
In the above description, it will be understood that, in use, wind may enter the inner cylinder 61 through the air inlet 611, then enter the communication channel 63 through the first air outlet 612, and finally be discharged through the second air outlet 621. When the inner cylinder 61 is moved to gradually approach the second air outlet 621, the air output of the second air outlet 621 is gradually reduced; when the inner cylinder 61 is moved to be gradually far away from the second air outlet 621, the air output of the second air outlet 621 is gradually increased. When the wall of the inner cylinder 61 partially shields the second air outlet 621, the air outlet direction of the second air outlet 621 may be changed.
In addition, at least one of the inner tube 61 and the outer tube 62 is provided so as to be movable in the radial direction of the air knife 60, including the following three modes: the first is that the outer tube 62 is fixed, and the inner tube 61 is provided so as to be movable relative to the outer tube 62 in the radial direction of the air knife 60; the second is that the inner tube 61 is fixed, and the outer tube 62 is provided so as to be movable relative to the inner tube 61 in the radial direction of the air knife 60; the third is to provide the inner tube 61 and the outer tube 62 so as to be movable relative to each other in the radial direction of the air knife 60.
By adopting the technical scheme, the air knife 60 can enable the air output and the air output direction of the air outlet of the air knife to be adjustable, so that the air knife 60 is more flexible to use, can adapt to various use requirements, and can effectively improve the drying efficiency and effect on materials when being applied to a drying hot box.
In the present invention, the first air outlet 612 and the second air outlet 621 may have any appropriate shape and arrangement position as long as the above-described functions can be achieved. For example, the cross sections of the first air outlet 612 and the second air outlet 621 may be elliptical, square, etc., and the first air outlet 612 and the second air outlet 621 may be arranged at intervals along the axial direction and/or the circumferential direction of the air knife 60. Of course, the first air outlet 612 and the second air outlet 621 may be plural.
According to a preferred embodiment of the present invention, referring to fig. 1 and 2, the first air outlet 612 and the second air outlet 621 are respectively one, the first air outlet 612 is elongated extending along the axial direction of the inner cylinder 61, and the second air outlet 621 is elongated extending along the axial direction of the outer cylinder 62. In this case, the first air outlet 612 and the second air outlet 621 are offset from each other in the circumferential direction of the air knife 60, that is, the first air outlet 612 and the second air outlet 621 are preferably not aligned to prevent the air entering the inner tube 61 from being directly discharged from the second air outlet 621 after being discharged from the first air outlet 612.
Preferably, as shown in fig. 2, the first air outlet 612 and the second air outlet 621 are disposed opposite to each other in the circumferential direction of the air knife 60.
The cross section of the first air outlet 612 and the second air outlet 621 is preferably rectangular, and the opening angle of the first air outlet 612 and the second air outlet 621 in the circumferential direction of the air knife 60 is 0 to 90 °, preferably 25 to 40 °.
In the present invention, in order to prevent the wind entering the air knife 60 from being discharged from the inner tube 61 and/or other ports of the communication channel 63, one end of the inner tube 61 facing away from the air inlet 611 is provided in a closed shape, and both ends of the communication channel 63 are provided in a closed shape. Wherein the closure of the inner drum 61 can be closed by an end wall integral with the wall of the drum, or by means of a mounting assembly (to be described below) or other structure to be fitted with an air knife (for example a drying oven to be described below); the closure of the communication channel 63 may be closed by means of a mounting assembly or other structure where an air knife is to be mounted.
In the present invention, in order to integrate the inner tube 61 with the outer tube 62 and facilitate the overall assembly and disassembly of the air knife 60, the air knife 60 may further include an assembly for mounting the inner tube 61 and the outer tube 62. The mounting assembly can be any component that can integrate the inner barrel 61 with the outer barrel 62 while allowing movement of the inner barrel 61 and/or outer barrel 62.
In order to simplify the structure of the air knife 60 and reduce the manufacturing cost of the air knife 60, according to a preferred embodiment of the present invention, taking the outer cylinder 62 being stationary and the inner cylinder 61 moving relative to the outer cylinder 62 in the radial direction of the air knife 60 as shown in fig. 1, the mounting assembly may include two movable flanges 64 mounted at both ends of the inner cylinder 61 and two fixed flanges 65 mounted at both ends of the outer cylinder 62, respectively, the two movable flanges 64 being connected with the two fixed flanges 65 (i.e., the movable flanges 64 and the fixed flanges 65 at the same end of the air knife 60) and the two movable flanges 64 being provided to be capable of being lockably moved relative to the corresponding fixed flanges 65, respectively, in the radial direction of the air knife 60.
The movable flange 64 is sealingly mounted to the inner tube 61, and the fixed flange 65 is sealingly mounted to the outer tube 62. As shown in fig. 3 and 4, the movable flange 64 has a mounting hole for mounting the inner cylinder 61, and the fixed flange 65 has a mounting hole for mounting the outer cylinder 62, and since the diameter of the inner cylinder 61 is smaller than that of the outer cylinder 62, the aperture of the mounting hole of the movable flange 64 is smaller than that of the mounting hole of the fixed flange 65.
As shown in fig. 1, the movable flange 64 is located outside the fixed flange 65, and both ends of the inner cylinder 61 are respectively and sequentially penetrated through the mounting holes of the fixed flange 65 and the movable flange 64, and both ends of the outer cylinder 62 are respectively penetrated through the mounting holes of the fixed flange 65. In this case, both ends of the communication passage 63 may be closed by two movable flanges 64, respectively.
In the foregoing description, referring to fig. 1, the left end surface of the inner cylinder 61 may extend out of the left movable flange 64, or may be located in the movable flange 64 or be flush with the left end surface of the movable flange 64. The right end face of the inner cylinder 61 may extend out of the movable flange 64 on the right side or may be flush with the right end face of the movable flange 64, in both cases, the right end port of the inner cylinder 61 may be closed by an end wall integral with the cylinder wall thereof, or may be closed by other structures to which the air knife 60 is to be mounted; the right end face of the inner tube 61 may also be located in the right movable flange 64, in which case the right end port of the inner tube 61 may be closed by an end wall integral with its wall, or may be closed by the movable flange 64, that is, the mounting hole of the movable flange 64 for mounting the inner tube 61 is not a through hole, but a semi-closed hole having a right side wall.
Further, as shown in fig. 3 and 4, the movable flange 64 and the fixed flange 65 may be connected by a fastener, the movable flange 64 and the fixed flange 65 are respectively provided with a through hole through which the fastener passes, the through hole on the movable flange 64 is a round hole 641, and the through hole on the fixed flange 65 is a slotted hole 651.
In the foregoing description, the hole diameter of the circular hole 641 is adapted to the diameter of the fastener, the oblong hole 651 has a small hole diameter and a large hole diameter, the small hole diameter is adapted to the diameter of the fastener, and the large hole diameter is larger than the diameter of the fastener. The fastener achieves locking and connection of the movable flange 64 to the fixed flange 65 by locking the circular hole 641 in a position of the circular hole 651 in the extending direction of the circular hole 651. The extending direction of the oblong hole 651 is the moving direction of the inner tube 61. For example, as shown in fig. 4, the oblong hole 651 extends in the vertical direction, in which case the inner cylinder 61 and the movable flange 64 are movable up and down in the vertical direction with respect to the outer cylinder 62 and the fixed flange 65, and the first air outlet 612 and the second air outlet 621 are located in the vertical direction.
In order to strengthen the connection, as shown in fig. 3 and 4, a plurality of circular holes 641 may be provided on the movable flange 64, and a plurality of oblong holes 651 may be provided on the fixed flange 65 correspondingly, with the extending directions of the plurality of oblong holes 651 being uniform.
In use, the fasteners can be loosened, the inner barrel 61 and the movable flange 64 moved to the desired position, and then tightened to lock the movable flange 64 to the fixed flange 65.
In the present invention, the fastening member may be any member capable of connecting the movable flange 64 to the fixed flange 65. The fasteners are bolts, for example, in which case the circular holes 641 and oblong holes 651 may be threaded holes.
The second aspect of the present invention provides a drying heat box, the drying heat box 6 includes a box body and an air knife 60, a drying cavity for drying materials is provided in the box body, the air knife 60 is provided in the drying cavity, a second air outlet 621 of the air knife 60 is aligned to the materials, a feeding port, a discharging port, a drying gas inlet and a drying gas outlet which are communicated with the drying cavity are provided on the box body, an air inlet 611 of the air knife 60 is communicated with the drying gas inlet, and a second air outlet 621 of the air knife 60 is communicated with the drying gas outlet.
When the air knife 60 is used, the air output and the air output direction of the air knife 60 can be adjusted as required, the drying gas entering the drying cavity through the drying gas inlet enters the air knife 60 through the air inlet 611, and the air knife 60 intensively blows the drying gas to the materials in a certain air output and air output direction, so that the materials are quickly air-dried.
Wherein, referring to fig. 5, the inlet and the outlet are respectively located at opposite sides of the case (refer to the left and right sides of the drying oven 6 shown in fig. 5), and the drying gas inlet and the drying gas outlet are respectively located at opposite sides of the case (refer to the upper and lower sides of the drying oven 6 shown in fig. 5). A plurality of air knives 60 may be disposed in the drying chamber, and the air knives 60 extend along a direction perpendicular to the material in-out direction and are arranged at intervals along the material in-out direction (see the left-right direction shown in fig. 5). This can further improve the drying efficiency and effect.
In case that a plurality of air knives 60 are provided in the drying chamber, referring to fig. 5, a plurality of the drying gas inlets and drying gas outlets may be provided on the cabinet, respectively. It will be appreciated that the positions corresponding to the black arrows of the drying oven 6 shown in fig. 5 are the drying gas inlet and the drying gas outlet.
Further, as shown in fig. 5, the drying unit may further include a heating type roller drafting machine 5 and a non-heating type roller drafting machine 7 respectively provided before and after the drying oven 6. The heating type roller drafting machine 5 and the non-heating type roller drafting machine 7 are both preferably five-roller drafting machines. The roller type drafting machine of the drying unit mainly plays a role in drying, does not apply a large drafting force to draft, and has negligible drafting effect.
In the present invention, as shown in fig. 5, the melt extrusion unit may include a twin screw extruder 1, a booster pump 2, and a static mixer 3, the spinning unit may include a cooling fluid supply device and a spinning manifold 4, the drawing unit may include a drawing hot box 8 and a drawing machine 9, and the winding unit may include a winding machine 11.
The double-screw extruder 1 is used for carrying out melt extrusion on the spinning solution to form a stable melt; the booster pump 2 is used for applying a stable pressure output to the melt so as to ensure the stable output of the melt; the static mixer 3 is used for forming a stable and uniform melt; the cooling fluid supply device is used for supplying cooling fluid to the spinning box 4 and quenching and forming the fiber precursor ejected from the spinning holes (described below) in the spinning box 4; the spinning box 4 is used for converting the melt into gel elastic fluid and simultaneously carrying out dry air quenching to form solid gel filaments (i.e. fiber precursors); the drawing hot box 8 and the drawing machine 9 are used for drawing the dried fiber precursor, wherein the drawing hot box 8 is used for hot drawing so as to take solvent volatilization into account during drawing; the winder 11 winds the drawn fiber precursor.
In addition, the fiber spinning system may further comprise an oiling machine 10 for surface oiling the fiber filaments before the winder 11.
In the embodiment of the fiber spinning system shown in fig. 5, the black arrows represent the gas flow direction.
In the following examples, a fiber spinning system shown in fig. 1 was used, which includes a twin screw extruder, a spinning box, a hot five-roll drawing machine, a drying oven, a five-roll drawing machine one, a drawing oven, a five-roll drawing machine two, and a winding machine, which were connected in this order. The spinning box body is internally provided with an annular pipeline for circular blowing, the opening ratio is 35%, the opening size is 5mm, the inner diameter of the spinning box body is 1000 multiplied by 1200mm, the drying hot box comprises a box body and a plurality of air knives which are uniformly arranged along the axial direction (the in-out direction of materials) of the box body, a certain distance is reserved between every two adjacent air knives, the box body is internally provided with a drying cavity for drying materials, the air knives are arranged in the drying cavity, a second air outlet of each air knife is aligned with the materials, a feeding port, a discharging port, a drying gas inlet and a drying gas outlet which are communicated with the drying cavity are formed in the box body, a second air outlet is communicated with the drying gas outlet, the feeding port and the discharging port are respectively positioned on two opposite sides of the box body, each air knife comprises an inner barrel and an outer barrel which are coaxially sleeved, one end of each inner barrel is provided with an opening to form an air inlet of each air knife, the wall of each inner barrel is provided with a first air outlet which is communicated with the drying cavity, each second air outlet is axially communicated with a strip-shaped air outlet which is formed between the first air outlet and the second air outlet which is axially communicated with the second air outlet along the axial direction, and the air outlet which is communicated with the second air outlet; the opening angle of the first air outlet and the second air outlet in the circumferential direction of the air knife is 40 degrees, and the inner cylinder and the outer cylinder can move along the radial direction of the air knife to adjust the air outlet quantity and the air outlet direction of the second air outlet.
Firstly, mixing a solvent, polyethylene powder and a spinning auxiliary agent, enabling the ultra-high molecular weight polyethylene powder to be pre-swelled, then, entering a double-screw extruder for full dissolution and shearing, then, sending the pre-swelled ultra-high molecular weight polyethylene powder into a static mixer through a booster pump, sending the stabilized solution into a metering pump and a spinning box for extrusion, wherein the extrusion rate is 1-10 m/min, and the extruded gel strip is subjected to a heat-insulating oil jacket (200 ℃) to ensure the volatilization temperature of the solvent and the stabilization temperature of a spinneret plate. The gel strips passing through the heat preservation oil jacket are rapidly formed through ring blow-down air quenching, the ring blow-down pressure is 0-50kPa, the temperature is between-50 ℃ and-10 ℃, the quenched strips are rapidly solidified and formed to form a stable folded chain state, the quenched strips enter the hot five rollers through the godet rollers, the solvent on the surface of the fiber is volatilized through the heating of the hot five rollers at the temperature of 30-100 ℃, the strips are sent into a drying hot box to rapidly volatilize the solvent on the surface of the fiber through an air knife in the drying hot box, and the drying hot air sent out by the air knife is hot nitrogen. The internal temperature of the drafting heat box is controlled at 40-150 ℃, and then the drafting heat box is pre-drafted, drafting formed and wound, and the total drafting multiplying power is 160-300 times.
Example 1
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 425) to the solvent (decalin) is 8%, the mass percentage of the auxiliary agent (antioxidant: calcium stearate=7:3 weight, the same applies below) to the raw material is 0.8%, the swelling temperature is 98 ℃, the extrusion rate is 3m/min, the heat-insulating oil jacket is 200 ℃, the air with the ring quenching temperature of minus 10 ℃ is blown for 0.64s, the air pressure is 5kPa, the hot roller temperature is 40 ℃, the drying hot box temperature is 40 ℃ (the air knife air temperature is 40 ℃, the air speed is 30 m/s, the air pressure is 0.4 MPa), the drawing hot box temperature is 125 ℃, the pre-drawing multiplying power is 3 times, the multi-stage drawing hot box temperature is 140-145 ℃, and the total drawing multiplying power is 200 times. The performance test index for different batches of fiber products is shown in table 1 below. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is activated carbon. The recovery rate of the solvent is 97.17 percent.
TABLE 1
Example 2
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 425) to the solvent (decalin) is 8%, the mass percentage of the auxiliary agent to the raw material is 0.8%, the swelling temperature is 98 ℃, the extrusion speed is 3.25m/min, the heat-insulating oil jacket is 200 ℃, the air with the ring quenching temperature of minus 15 ℃ is blown for 0.54s, the wind pressure is 4kPa, the hot roller temperature is 40 ℃, the drying hot box temperature is 40 ℃ (the wind knife wind temperature is 40 ℃, the wind speed is 30 m/s and the wind pressure is 0.4 MPa), the drafting hot box temperature is 125 ℃, the pre-drafting multiplying power is 3 times, the multi-stage drafting hot box temperature is 140-145 ℃, and the total drafting multiplying power is 240 times. The fiber performance test index for the different batches is shown in Table 2 below. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is activated carbon. The recovery rate of the solvent was 97.22%.
TABLE 2
Example 3
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 487) to the solvent (decalin) is 8%, the mass percentage of the auxiliary agent to the raw material is 0.8%, the swelling temperature is 98 ℃, the extrusion speed is 3.25m/min, the heat-insulating oil jacket is 200 ℃, the ring-blowing quenching temperature is-20 ℃, the air is 0.7s, the wind pressure is 10kPa, the hot roller temperature is 50 ℃, the drying hot box temperature is 50 ℃ (the wind knife wind temperature is 50 ℃, the wind speed is 30 m/s, the wind pressure is 0.4 MPa), the drafting hot box temperature is 125 ℃, the pre-drafting multiplying power is 3 times, the multi-stage drafting hot box temperature is 140-145 ℃, and the total drafting multiplying power is 220 times. The fiber performance test index for the different batches is shown in Table 3 below. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is activated carbon. The recovery rate of the solvent is 97.19 percent.
TABLE 3 Table 3
Example 4
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 487) to the solvent (decalin) is 8%, the mass percentage of the auxiliary agent to the raw material is 0.8%, the swelling temperature is 98 ℃, the extrusion speed is 3m/min, the heat-insulating oil jacket is 200 ℃, the air with the ring quenching temperature of minus 25 ℃ is blown for 0.5s, the wind pressure is 0.4MPa, the hot roller temperature is 40 ℃, the drying hot box temperature is 40 ℃ (the wind knife wind temperature is 40 ℃, the wind speed is 30 m/s, the wind pressure is 0.4 MPa), the drafting hot box temperature is 125 ℃, the pre-drafting multiplying power is 3 times, the multi-stage drafting hot box temperature is 140-145 ℃, and the total drafting multiplying power is 220 times. The fiber performance test index for the different batches is shown in Table 4 below. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is activated carbon. The recovery rate of the solvent is 97.35%.
TABLE 4 Table 4
Example 5
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 487) to the solvent (tetrahydronaphthalene) is 6.5%, the mass percentage of the auxiliary agent to the raw material is 0.7%, the swelling temperature is 98 ℃, the extrusion speed is 3.25m/min, the heat-insulating oil jacket is 200 ℃, the ring-blowing quenching temperature is nitrogen at-20 ℃, the time is 0.6s, the wind pressure is 5kPa, the hot roller temperature is 40 ℃, the drying hot box temperature is 80 ℃ (the wind knife wind temperature is 80 ℃, the wind speed is 40 m/s, the wind pressure is 0.4 MPa), the drafting hot box temperature is 125 ℃, the pre-drafting multiplying power is 3 times, the multi-stage drafting hot box temperature is 140-145 ℃, and the total drafting multiplying power is 220 times. The fiber performance test index for the different batches is shown in Table 5 below. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is coconut shell activated carbon. The recovery rate of the solvent is 98.0%.
TABLE 5
Example 6
The mass/volume ratio of the raw material (polyethylene with the number average molecular weight of 487) to the solvent (toluene) is 6.5%, the mass percentage of the auxiliary agent to the raw material is 0.7%, the swelling temperature is 98 ℃, the extrusion speed is 3.25m/min, the heat-insulating oil jacket is 200 ℃, the ring-blowing quenching temperature is-10 ℃ of air, the time is 0.6s, the wind pressure is 5kPa, the hot roller temperature is 40 ℃, the drying hot box temperature is 60 ℃ (the wind knife wind temperature is 60 ℃, the wind speed is 50 m/s, the wind pressure is 0.4 MPa), the drafting hot box temperature is 125 ℃, the pre-drafting multiplying power is 3 times, the multi-stage drafting hot box temperature is 140-145 ℃, and the total drafting multiplying power is 300 times. The solvent is recovered by adopting the mode of staged recovery at different temperature points, a cyclone separator is adopted in a low-temperature zone, a cooling separation-cryogenic separation-cooling separation-adsorption desorption integrated mode is adopted in a high-temperature zone, the temperature of the cyclone separation and the cooling separation is less than 40 ℃, the temperature of the cryogenic separation is < -5 ℃, and the adsorbent is a molecular sieve. The recovery rate of the solvent is 98.5%. The fiber performance test index for the different batches is shown in Table 6 below.
TABLE 6
Comparative example 1
A fiber was produced in the same manner as in example 4, except that the circular blowing mode was changed to the side blowing mode described in CN106544741B, air was blown at a temperature of 10℃and the drying oven was not provided with an air knife structure, and the performance indexes of the fibers obtained in different batches were as shown in Table 7 below.
TABLE 7
Comparative example 2
Spinning was performed as in example 4, except that a conventional drying oven was used, i.e., no air knife structure was provided in the drying oven, and the fiber property detection index was as shown in Table 8 below. The solvent recovery was 84%.
TABLE 8
Comparative example 3
Spinning was performed in the same manner as in example 4, except that the solvent recovery unit employed two cyclones in series, i.e., the solvent of the drying unit was also separated and recovered by the cyclones. The solvent recovery was 55%.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (15)

1. A method for recovering solvent in a fiber spinning process comprising extruding and spinning a spinning solution, sequentially carrying out a cooling forming process, a drying process and a drawing process on a fiber precursor obtained by spinning, and recovering the solvent in the cooling forming process and the drying process, characterized in that the cooling forming process comprises contacting the fiber precursor with a gas having a temperature of-10 to-25 ℃, the contacting process is a blowing process in which the fiber precursor is subjected to a circular blowing process, the drying process comprises contacting the fiber precursor after the cooling forming with a drying gas having a velocity of not less than 20 m/s, the recovering solvent in the cooling forming process is a cyclone separation process, and the recovering solvent in the drying process is an integrated method of cooling separation-cryogenic separation-cooling separation-adsorption desorption, wherein the temperature of the cyclone separation is <40 ℃, the temperature of the cooling separation is <40 ℃, and the temperature of the cryogenic separation is < -5 ℃;
the drying process is carried out in a drying unit, the drying unit comprises a drying hot box, the drying hot box comprises a box body and an air knife (60), a drying cavity for drying materials is arranged in the box body, the air knife (60) is arranged in the drying cavity, the air knife (60) comprises an inner cylinder (61) and an outer cylinder (62) which are coaxially sleeved, one end of the inner cylinder (61) is in an opening shape to form an air inlet (611) of the air knife (60), a first air outlet (612) communicated with the air inlet (611) is formed in the wall of the inner cylinder (61), a second air outlet (621) is formed in the wall of the outer cylinder (62), a radial interval is arranged between the inner cylinder (61) and the outer cylinder (62) to form a communication channel (63) communicated with the first air outlet (612) and the second air outlet (621), at least one of the inner cylinder (61) and the outer cylinder (62) is arranged to be capable of moving along the radial direction of the air knife (60) to adjust the second air outlet (612) communicated with the air inlet (611), a drying air outlet (621) is arranged in the direction aligned with the air inlet (611) of the drying cavity, the second air outlet (621) is in communication with the dry gas outlet.
2. The method of claim 1, wherein the cyclone separation temperature is 10-30 ℃.
3. The method of any one of claims 1 or 2, wherein the cryogenic separation temperature is-20 to-10 ℃.
4. The method of claim 1, wherein the adsorption is by contacting the gas from the drying process with an adsorbent.
5. The method of claim 4, wherein the adsorbent is one or more of activated carbon, coconut carbon, molecular sieves.
6. The method of claim 5, wherein the adsorbent is cylindrical activated carbon having a diameter of 3-6 mm.
7. The process of claim 1, wherein the conditions of desorption comprise a temperature of 5-25 ℃ and a pressure of 0.1-5MPa.
8. The method of claim 1, wherein the spinning solution comprises polyethylene, solvent and auxiliary agent, the weight ratio of polyethylene to solvent is 1-30:100, and the weight ratio of auxiliary agent to polyethylene is 0.3-3:100.
9. The method of claim 1, wherein the spinning solution comprises polyethylene, solvent and auxiliary agent, the weight ratio of polyethylene to solvent is 4-20:100, and the weight ratio of auxiliary agent to polyethylene is 0.5-2:100.
10. The method of claim 8 or 9, wherein the solvent is one or more of decalin, tetrahydronaphthalene, toluene, xylene, white oil, and paraffinic oil.
11. The method of claim 1, wherein the blowing is for a period of 0.5 to 0.7 seconds and the pressure is 3 to 100kPa.
12. The method of claim 11, wherein the pressure is 3-10kPa.
13. The method of claim 1, wherein the drying comprises contacting the cooled shaped fiber filaments with a drying gas having a velocity of 30-40 m/s.
14. The method of claim 1, wherein the temperature of the drying gas is 0-140 ℃.
15. The method of claim 14, wherein the temperature of the drying gas is 40-80 ℃.
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