CN111254511B - Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof - Google Patents
Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof Download PDFInfo
- Publication number
- CN111254511B CN111254511B CN202010058457.3A CN202010058457A CN111254511B CN 111254511 B CN111254511 B CN 111254511B CN 202010058457 A CN202010058457 A CN 202010058457A CN 111254511 B CN111254511 B CN 111254511B
- Authority
- CN
- China
- Prior art keywords
- fiber
- ultra
- temperature
- molecular weight
- weight polyethylene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a low-temperature spun superfine ultra-high molecular weight polyethylene fiber and a preparation method thereof, the fiber is a fiber multifilament consisting of 2-2000 monofilaments, the linear density of the monofilaments in the fiber multifilament is 0.2-0.3dtex, and the mechanical strength of the fiber is 36 cN/dtex-42 cN/dtex. The raw materials are ultra-high molecular weight polyethylene resin, solvent and auxiliary agent which are mixed to prepare spinning solution, and the spinning solution is fed into a double-screw extruder to swell, mix and extrude after a special pretreatment process, and is extruded and molded through a spinneret plate, and is stretched through a critical ultra-high nozzle to form fine fiber. And (3) completely removing the solvent from the primary yarn, and then performing multistage hot stretching and rolling to form a final product. Compared with the prior art, the fiber multifilament prepared by the invention has uniform filament number, no broken filaments and broken filaments, the linear density of the monofilament is only 0.3-0.5 times of that of the conventional fiber, the hand feeling is soft and comfortable, the residual amount of the solvent is low, the spinning temperature in the preparation process is lower than that of the conventional spinning by nearly 150 ℃, and the energy consumption of the spinning is low.
Description
Technical Field
The invention belongs to the field of fiber materials, relates to an ultrahigh molecular weight polyethylene (UHMWPE) fiber and a preparation method thereof, and particularly relates to a low-temperature spun superfine denier UHMWPE fiber and a preparation method thereof.
Background
The UHMWPE fiber is the fiber material with the highest specific strength in the current industrialized fiber materials and is one of three high-performance fibers in the world. Owing to the ultrahigh molecular weight and narrow molecular weight distribution of UHMWPE, the UHMWPE fiber material has excellent mechanical property, wear resistance and chemical corrosion resistance, and has the characteristics of light weight, high heat conductivity coefficient and the like, so that the UHMWPE fiber material has wide application in the fields of national defense and military, aerospace, ocean engineering and civil protection.
The superfine denier fiber can be woven into high-grade textile fabric with soft hand feeling and comfortable wearing, and has high economic value. In the past, the application of UHMWPE fibers at home and abroad focuses on the fields of major engineering and high-end individual protection, and the application attention in the fields of soft protective articles, wearable clothes, home textiles and the like is less. The UHMWPE fiber prepared by the conventional wet spinning method comprehensively determines that the fiber product has higher solvent residue from factors such as production cost, efficiency and the like, the filament number is more than 2.5dtex, the texture is coarse and hard, the hand feeling is rough, and the application and development of the UHMWPE fiber in the soft individual protection and other clothing fields are limited; the fiber prepared by using the dry jelly spinning of volatile solvents such as decalin and xylene has the advantages of low solvent residue, lower extrusion temperature, large nozzle stretching ratio and the like, and although the ultra-fine denier and high-strength polyethylene fiber is easier to prepare, the problems of poor stability in the spinning process, easy generation of broken filaments, uneven fiber fineness and the like exist.
Chinese patent 201110090624.3 discloses a method for preparing ultra-high molecular weight polyethylene fine denier fiber by a jelly spinning method, which utilizes wet jelly spinning to obtain the ultra-high molecular weight polyethylene fine denier fiber through pre-drafting, extraction, drying and hot stretching. The invention optimizes the pre-drafting process of wet spinning, so that the gel yarn can shrink more uniformly, a higher pre-drafting multiple can be loaded subsequently, and the pre-drafting is carried out in multiple stages, the strength of the obtained product is more than 35cN/dtex, and the total denier of the fiber is preferably 30-400D, but specific monofilament titer related technologies are not mentioned.
Chinese patent CN201510107582.8 discloses a preparation method of polyethylene fine denier wet conductive fiber, which adopts fiber with molecular weight of 400-800 ten thousand to swell with ultra-high molecular weight polyethylene in decalin to form suspension, the suspension is dissolved and sheared by a double screw extruder, polyethylene macromolecular chains are fully unwound to form uniform spinning solution, then the spinning solution is spun by a spinneret plate, the decalin is removed from tows in a hot air circulation system, and the spinning solution is pre-stretched, subjected to one or more hot stretching steps, and subjected to one or more relaxation steps to obtain polyethylene fine denier wet conductive fiber with fineness of 22 dtex-1776 dtex. The fiber prepared by the above patents is mainly based on the high-strength and high-modulus characteristics of the fiber, or the production process is optimized, or the production method is improved, but the fine-denier and high-strength performance of the fiber is not involved, and particularly the breakthrough of the technology related to the linear density of the single filament of the fiber bundle is not mentioned, and the technology for preparing the fine-denier filament related to the concentration of the spinning solution is not involved. However, the linear density and strength of the monofilaments are the determining factors for determining the texture, hand feeling and the like of the material, so that fibers with the lowest linear density and the highest strength of the monofilaments are obtained so as to be widely applied and developed in the fields of soft individual protection and other clothes; the two are spearheads, and the existing fiber preparation method must sacrifice one property while improving the other property.
The invention aims to solve the problems of low finished product rate, low strength and the like of superfine denier fiber preparation aiming at the technical blank in the patent.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a low-temperature spun ultra-fine denier ultra-high molecular weight polyethylene fiber with high yield and high strength and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme: the low-temperature spun superfine ultra-high molecular weight polyethylene fiber is characterized in that the fiber is a fiber multifilament consisting of 2-2000 monofilaments, the linear density of the monofilaments in the fiber multifilament is 0.3-2.0dtex, and the mechanical strength of the fiber is 36 cN/dtex-42 cN/dtex.
The linear density of the fiber multifilament is 5dtex to 2000dtex, and the residual amount of the solvent in the fiber is 0.01 percent to 0.1 percent.
A preparation method for spinning ultra-fine denier ultra-high molecular weight polyethylene fiber at low temperature is characterized by comprising the following steps:
1) Mixing UHMWPE resin with solvent and adjuvant, feeding into an emulsifying machine, gradually heating for emulsification, allowing the first stage to reach 50-85 deg.C, the second stage to reach 85-115 deg.C, and the third stage to reach 115-130 deg.C, staying for no less than 0.5 hr, no less than 1 hr, no less than 2 hr, cooling to normal temperature, and feeding into a twin-screw extruder;
2) Swelling, mixing and extruding through a double-screw extruder, extruding and molding through a spinneret plate at 110-160 ℃, and stretching through a high-power spray nozzle to form fine fibers;
3) Removing the solvent in the gel fine fiber during the stretching process of the spray head, keeping the tension of the fiber to be not less than 50cN, solidifying the dried fiber at a constant temperature section of 60-110 ℃, and finally rolling and forming into the nascent fiber;
4) And performing multistage super-power hot stretching on the primary raw silk to obtain the finished product of superfine denier ultrahigh molecular weight polyethylene fiber.
The viscosity average molecular weight of the UHMWPE resin is 100 to 1000 ten thousand, the average grain diameter is 100 to 300 mu m, and the bulk density is 0.3 to 0.5g/cm 3 。
The mass ratio of the UHMWPE resin to the solvent is 1.
The mass ratio of the UHMWPE resin to the auxiliary agent is 1000-10. The mass ratio of the resin to the auxiliary agent is preferably 1000.
The solvent is one or more of paraffin oil, kerosene, vegetable oil, decahydronaphthalene, tetrahydronaphthalene, xylene, toluene, dichlorobenzene or petroleum ether;
the auxiliary agent is an antioxidant or a mixture of the antioxidant and an antioxidant auxiliary agent according to the mass ratio of 1000 to 1, wherein the antioxidant and the antioxidant auxiliary agent are one or more of a phenolic antioxidant and a hindered phenol antioxidant.
The diameter of the double-screw extruder in the step 3) is 15-135 cm, the length-diameter ratio is 30-72, and the screw temperature is 110-190 ℃.
The spinneret plate is one or more of a circular plate, a square plate and a special-shaped plate, the plate hole is one or more of a circular hole, a triangular hole, a square hole and a special-shaped hole, the aperture of the spinneret plate is 0.3-1 mm, and the length-diameter ratio is 5-30.
The method for removing the solvent in the step 3) comprises one or more of inert gas stripping, steam stripping, thermally induced phase separation and extraction; the inert gas is one or more of nitrogen, flue gas, carbon dioxide and steam.
The multistage hyperploid hot stretching in the step 4) is one-stage or more hot stretching, the first stage is the stretching of a spinning nozzle, the stretching ratio of the nozzle is 10-100 times, the total stretching ratio is 10-1000 times, and the stretching temperature is 60-160 ℃. Preferably, the total draft is 50 to 500 times and the drawing temperature is 100 to 155 ℃.
The total draft can be calculated as follows:
wherein DR General assembly Is the draw ratio, DR n Represents the multiple of the nth stage of hot drawing.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention finally prepares the superfine denier ultrahigh molecular weight polyethylene fiber multifilament through technological innovation, the filament titer is uniform, no broken filament is generated, the monofilament linear density is only 0.3-0.5 times of that of the conventional fiber, the hand feeling is soft and comfortable, the solvent residual quantity is low, the temperature of a spinning nozzle in the preparation process is lower than that of the conventional spinning by nearly 150 ℃ (the spinning temperature of the conventional spinning nozzle is generally 200-300 ℃), and the spinning energy consumption is low. The product can be used for wearable articles such as fishing lines, operation suture lines, protective gloves, cool fabrics and the like, and other application fields with higher requirements on fiber strength and flexibility.
And 2, in the gel spinning process of UHMWPE, the content (concentration) of solute in the spinning solution is increased, and the proportion of binding molecules in gel fibrils can be increased, so that the fiber can more easily reach a higher stretching ratio, and therefore, the fiber is thicker and has larger denier. Meanwhile, the higher concentration also increases the difficulty of disentanglement and orientation of the molecular chain in swelling and dissolution, which is not beneficial to the improvement of fiber strength. The strength of the fiber can be obviously improved by reducing the concentration, but the stretchability of the fiber is damaged, and broken ends of broken filaments are easily generated in the spinning process. In the process of the invention, the lower concentration of the spinning solution can effectively reduce the linear density of the spun primary yarn, and the ultra-fine denier ultra-high molecular weight polyethylene fiber can be prepared by effective high-power drawing of a spinneret. The invention firstly adopts gradual heating emulsification to uniformly swell UHMWPE resin in a solvent before a double-screw extruder, avoids subsequent melt fracture caused by overlarge solvent amount and nonuniform concentration in the melt, and then performs drawing forming at 110-170 ℃, and because the solvent amount is large, a special spinneret plate is matched for drawing at the temperature, the solvent can slowly volatilize, so that the fiber can not fracture or be nonuniform in the drawing process, and the reduction of the fluidity of the melt caused by overlow temperature can be avoided, thereby obtaining the high-strength low-denier fiber.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
Mixing UHMWPE resin with the viscosity-average relative molecular mass of 410 ten thousand and a solvent of decalin according to the mass ratio of 1 3 And the addition amount of the auxiliary agent is 3 per mill of that of the UHMWPE resin, spinning solution is prepared, the spinning solution is fed into an emulsifying machine, the temperature is gradually increased for emulsification, the temperature is 70 ℃,105 ℃,118 ℃, the temperature is respectively kept for 0.5h,1h and 2h in three time periods, then the temperature is reduced to the normal temperature, the spinning solution is fed into a double-screw extruder, and the screw mixing temperature is set to be 190 ℃. The diameter of a screw of the double-screw extruder is 30mm, the length-diameter ratio is 72, the dry spinning is carried out by swelling, mixing and extruding through the double-screw extruder, extruding and molding through a spinneret plate at 110-160 ℃, and stretching through a high-power nozzle to form fine fibers, wherein the number of holes selected by the spinneret plate is 100, the pore diameter is 0.7mm, the length-diameter ratio is 5, and the hole diameter of the spinneret plate is circular. And (3) simultaneously removing the solvent in the gel fine fibers in the process of stretching by using a spray head, and blowing and removing the solvent by using nitrogen at 135 ℃, wherein the stretch ratio (first stage) of the spray head of the fibers is 15 times, and the stretch ratios of the second stage, the third stage, the fourth stage and the fifth stage are respectively 4 times, 1.25 times, 1.20 times and 1.10 times.
The mechanical strength of the obtained fiber product is 36cN/dtex, the fiber linear density is 60dtex, the monofilament linear density is 0.14D/f, the fiber modulus is 1200cN/dtex, the solvent residue is 0.03%, and the yield is 90%.
Example 2
The viscosity phase relative to the molecular mass was 480 ten thousandThe UHMWPE resin and solvent tetrahydronaphthalene are mixed according to the mass ratio of 1 3 And the addition amount of the auxiliary agent is 5 per mill of the UHMWPE resin to prepare spinning solution, the spinning solution is fed into an emulsifying machine, the temperature is gradually increased for emulsification, the temperature is 70 ℃,105 ℃,118 ℃, the temperature is kept for 0.5h,1h and 2h in three time periods respectively, then the temperature is reduced to the normal temperature, the mixture is fed into a double-screw extruder, and the screw mixing temperature is set to be 170 ℃. The diameter of a screw of the double-screw extruder is 48mm, the length-diameter ratio is 60, the dry spinning is carried out by swelling, mixing and extruding through the double-screw extruder, extruding and molding through a spinneret plate at 110-160 ℃, and stretching through a high-power nozzle to form fine fibers, wherein the number of holes selected by the spinneret plate is 88, the pore diameter is 0.6mm, the length-diameter ratio is 10, and the hole diameter of the spinneret plate is square. And (3) simultaneously removing the solvent in the gel fine fibers in the process of stretching the spray head, and blowing and removing the solvent by using flue gas at 130 ℃, wherein the stretch ratio (the first stage) of the spray head of the fibers is 8 times, and the stretch ratios of the second stage, the third stage, the fourth stage and the fifth stage are respectively 3 times, 2.5 times, 1.35 times and 1.08 times.
The mechanical strength of the obtained fiber product is 37cN/dtex, the fiber linear density is 120dtex, the monofilament linear density is 0.28D/f, the fiber modulus is 1400cN/dtex, and the solvent residue is 0.02%; the yield was 88%.
Example 3
Mixing UHMWPE resin with viscosity relative molecular mass of 612 ten thousand and solvent xylene according to a mass ratio of 1 3 And the addition amount of the auxiliary agent is 2 per mill of that of the UHMWPE resin, spinning solution is prepared, the spinning solution is fed into an emulsifying machine, temperature is gradually increased for emulsification, the temperature is 70 ℃,105 ℃,118 ℃, the temperature is gradually increased for 0.5h,1h and 2h respectively in three time periods, then the temperature is reduced to normal temperature, the spinning solution is fed into a double-screw extruder, and the screw mixing temperature is set to be 160 ℃. The diameter of a screw of the double-screw extruder is 20mm, the length-diameter ratio is 64. The nozzle is simultaneously removed in the stretching processRemoving the solvent in the gel fine fiber, and blowing by using carbon dioxide at 140 ℃ to remove the solvent, wherein the nozzle drawing ratio (first stage) of the fiber is 20 times, and the second, third, fourth and fifth stage drawing ratios are respectively 3.8 times, 4 times, 1.35 times and 1.20 times.
The mechanical strength of the obtained fiber product is 38.2cN/dtex, the fiber linear density is 58dtex, the monofilament linear density is 0.30D/f, the fiber modulus is 1600cN/dtex, the solvent residue is 0.02 percent, and the yield is 92 percent.
Example 4
Mixing UHMWPE resin with a viscosity relative molecular mass of 767 ten thousand and a solvent decalin according to a mass ratio of 1 3 And the addition amount of the auxiliary agent is 2.5 per mill of that of the UHMWPE resin, spinning solution is prepared, the spinning solution is fed into an emulsifying machine, the temperature is gradually increased for emulsification, the temperature is 70 ℃,105 ℃,118 ℃, the temperature is respectively kept for 0.5h,1h and 2h in three time periods, then the temperature is reduced to the normal temperature, the spinning solution is fed into a double-screw extruder, and the screw mixing temperature is set to be 165 ℃. The diameter of a screw of the double-screw extruder is 30mm, the length-diameter ratio is 72, the dry spinning is carried out by swelling, mixing and extruding through the double-screw extruder, extruding and molding through a spinneret plate at 110-170 ℃, and stretching through a high-power nozzle to form fine fibers, wherein the number of holes selected by the spinneret plate is 40, the pore diameter is 0.45mm, the length-diameter ratio is 20, and the hole diameter of the spinneret plate is special-shaped. And (3) simultaneously removing the solvent in the gel fine fibers in the process of stretching by using a spray head, and blowing and removing the solvent by using nitrogen at 125 ℃, wherein the spray head stretching ratio (the first stage) of the fibers is 17 times, and the second, third, fourth and fifth stage stretching ratios are respectively 4 times, 3.6 times, 1.18 times and 1.05 times.
The obtained fiber product has the mechanical strength of 36.5cN/dtex, the fiber linear density of 38dtex, the monofilament linear density of 0.26D/f, the fiber modulus of 1450cN/dtex, the solvent residue of 0.01% and the yield of 95%.
Example 5
Mixing UHMWPE resin with molecular mass of 523 ten thousand and solvent decalin according to a mass ratio of 1. The diameter of a screw of the double-screw extruder is 20mm, the length-diameter ratio is 64. And (3) simultaneously removing the solvent in the gel fine fibers in the process of stretching by using a spray head, and blowing and removing the solvent by using nitrogen at 125 ℃, wherein the spray head stretching ratio (the first stage) of the fibers is 22 times, and the second, third, fourth and fifth stage stretching ratios are respectively 3 times, 4.5 times, 1.25 times and 1.12 times.
The obtained fiber product has the mechanical strength of 41.5cN/dtex, the fiber linear density of 15dtex, the monofilament linear density of 0.30D/f, the fiber modulus of 1780cN/dtex, the solvent residue of 0.01 percent and the yield of 86 percent.
Example 5
Mixing UHMWPE resin with a viscosity-homogeneous phase relative molecular mass of 350 ten thousand and a solvent decalin according to a mass ratio of 1:12.5, adding an auxiliary agent of 2.5 per thousand of the UHMWPE resin to prepare a spinning solution, feeding the spinning solution into an emulsifying machine, gradually heating and emulsifying, standing for 0.8h,1.1h and 2h in three time periods of 50 ℃,85 ℃,115 ℃ and then cooling to normal temperature, feeding the spinning solution into a double-screw extruder, and setting a screw mixing temperature to be 155 ℃. The diameter of a screw of the double-screw extruder is 20mm, the length-diameter ratio is 64. And (3) simultaneously removing the solvent in the gel fine fibers in the process of stretching by using a spray head, and blowing and removing the solvent by using nitrogen at 125 ℃, wherein the spray head stretching ratio (the first stage) of the fibers is 22 times, and the second, third, fourth and fifth stage stretching ratios are respectively 3 times, 4.5 times, 1.25 times and 1.12 times.
The obtained fiber product has the mechanical strength of 36.0cN/dtex, the fiber linear density of 19dtex, the monofilament linear density of 0.30D/f, the fiber modulus of 1665cN/dtex, the solvent residue of 0.01% and the yield of 78%.
Example 7
A preparation method for spinning ultra-fine denier ultra-high molecular weight polyethylene fiber at low temperature comprises the following steps:
1) Mixing UHMWPE resin with a solvent and an auxiliary agent, feeding into an emulsifying machine, gradually heating up for emulsification, respectively staying for 0.5h,1h and 2h at 70 ℃,105 ℃ and 118 ℃ in three time periods, then cooling to normal temperature, and feeding into a double-screw extruder; the viscosity average molecular weight of the UHMWPE resin is 100 ten thousand, the average grain diameter is 100 mu m, and the bulk density is 0.3g/cm 3 . The mass ratio of the UHMWPE resin to the solvent is 1. The solvent is paraffin oil; the auxiliary agent is an antioxidant.
2) The diameter of the double-screw extruder is 15cm, the length-diameter ratio is 30, the screw mixing temperature is 150 ℃, the double-screw extruder swells, is mixed and extruded, is extruded and molded through a spinneret plate at the temperature of 130 ℃, and is stretched through a high-power nozzle to form fine fibers; the spinneret plate is a circular plate, the plate hole is circular, the aperture of the spinneret plate is 0.3mm, and the length-diameter ratio is 5.
3) Removing the solvent in the gel fine fiber during the stretching process of the spray head, keeping the fiber to have 200cN tension and strength, solidifying the dried fiber at a constant temperature of 80 ℃, and finally rolling and forming into nascent fiber; the method for removing the solvent is a steam stripping method.
4) And performing multistage super-power hot stretching on the primary raw silk to obtain the finished product of superfine denier ultrahigh molecular weight polyethylene fiber. The multistage super-power hot stretching is one-stage hot stretching, the first stage is the stretching of a spinning nozzle, the stretching ratio of the nozzle is 10 times, the total stretching multiplying power is 10 times, and the stretching temperature is 60 ℃.
The low-temperature spun ultrafine ultra-high molecular weight polyethylene fiber is obtained, the fiber is a fiber multifilament consisting of 2 monofilaments, the linear density of the fiber multifilament is 2000detx, and the linear density of the monofilaments in the fiber multifilament is 0.2dtex. The mechanical strength of the fiber is 42cN/dtex, the residual quantity of solvent in the fiber is 0.1%, and the rate of finished products is 93%.
Example 8
A preparation method for spinning ultra-fine denier ultra-high molecular weight polyethylene fiber at low temperature comprises the following steps:
1) Mixing UHMWPE resin with a solvent and an auxiliary agent, feeding the mixture into an emulsifying machine, gradually heating for emulsification, standing for 0.5h,1h and 2h in three time periods of 70 ℃,105 ℃ and 118 ℃, then cooling to normal temperature, and feeding the mixture into a double-screw extruder; the viscosity average molecular weight of the UHMWPE resin is 1000 ten thousand, the average grain diameter is 300 mu m, and the bulk density is 0.5g/cm 3 . The mass ratio of the UHMWPE resin to the solvent is 1. The solvent is kerosene; the auxiliary agent is an antioxidant.
2) The diameter of the double-screw extruder is 135cm, the length-diameter ratio is 72, the screw temperature is 190 ℃, the double-screw extruder swells, mixes and extrudes, the mixture is extruded and molded through a spinneret plate at 170 ℃, and fine fibers are formed by stretching through a high-power nozzle; the spinneret plate is a square plate, the plate hole is square, the aperture of the spinneret plate is 1mm, and the length-diameter ratio is 30.
3) Removing the solvent in the gel fine fiber during the stretching process of the spray head, maintaining the tension and strength of the fiber at 60cN, solidifying the dried fiber at a constant temperature of 95 ℃, and finally rolling and forming to obtain a nascent fiber; the method for removing the solvent is a thermally induced phase separation method;
4) And performing multistage super-power hot stretching on the primary raw silk to obtain the finished product of superfine denier ultrahigh molecular weight polyethylene fiber. The multistage super-power hot stretching is more than one stage of hot stretching, the first stage of hot stretching is the stretching of a spinneret, the stretching ratio of the spinneret is 100 times, the total stretching ratio is 1000 times, and the stretching temperature is 160 ℃.
The low-temperature spun superfine ultra-high molecular weight polyethylene fiber is fiber multifilament consisting of 2000 monofilaments, the linear density of the fiber multifilament is 5dtex, and the linear density of the monofilaments in the fiber multifilament is 0.3dtex. The mechanical strength of the fiber is 39cN/dtex, the residual quantity of solvent in the fiber is 0.01%, and the yield is 85%.
Claims (10)
1. The low-temperature spun superfine ultra-high molecular weight polyethylene fiber is characterized in that the fiber is a fiber multifilament consisting of 2-2000 monofilaments, the linear density of the monofilaments in the fiber multifilament is 0.2-0.3dtex, and the mechanical strength of the fiber is 36 cN/dtex-42 cN/dtex;
the low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber is prepared by the following method:
1) Mixing UHMWPE resin with solvent and adjuvant, feeding into an emulsifying machine, gradually heating for emulsification, allowing the first stage to reach 50-85 deg.C, the second stage to reach 85-115 deg.C, and the third stage to reach 115-130 deg.C, staying for no less than 0.5 hr, no less than 1 hr, no less than 2 hr, cooling to normal temperature, and feeding into a twin-screw extruder;
2) Swelling, mixing and extruding through a double-screw extruder, extruding and molding through a spinneret plate at the temperature of 110-160 ℃, and stretching through a high-power spray nozzle to form fine fibers;
3) Removing the solvent in the gel fine fiber during the stretching process of the spray head, keeping the tension of the fiber to be not less than 50cN, solidifying the dried fiber at a constant temperature of 60-110 ℃, and finally rolling and forming into a nascent fiber;
4) And performing multistage super-power hot stretching on the primary raw silk to obtain the finished product of superfine denier ultrahigh molecular weight polyethylene fiber.
2. The low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber of claim 1, wherein the linear density of the fiber multifilament is 5dtex to 2000dtex, and the residual solvent content in the fiber is 0.01% to 0.1%.
3. A method of preparing low temperature spun ultra fine denier ultra high molecular weight polyethylene fiber as claimed in claim 1, comprising the steps of:
1) Mixing UHMWPE resin with solvent and adjuvant, feeding into an emulsifying machine, gradually heating for emulsification, allowing the first stage to reach 50-85 deg.C, the second stage to reach 85-115 deg.C, and the third stage to reach 115-130 deg.C, staying for no less than 0.5 hr, no less than 1 hr, no less than 2 hr, cooling to normal temperature, and feeding into a twin-screw extruder;
2) Swelling, mixing and extruding by a double-screw extruder, extruding and molding at 110-160 ℃ by a spinneret plate, and stretching by a high-power nozzle to form fine fibers;
3) Removing the solvent in the gel fine fiber during the stretching process of the spray head, keeping the tension of the fiber to be not less than 50cN, solidifying the dried fiber at a constant temperature of 60-110 ℃, and finally rolling and forming into a nascent fiber;
4) And performing multistage super-power hot stretching on the primary raw silk to obtain the finished product of superfine denier ultrahigh molecular weight polyethylene fiber.
4. The method for preparing the low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber according to claim 3, wherein the viscosity average molecular weight of the UHMWPE resin is 100 to 1000 ten thousand, the average particle diameter is 100 to 300 μm, and the bulk density is 0.3 to 0.5g/cm 3 。
5. The preparation method of the low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber according to claim 3, wherein the mass ratio of the UHMWPE resin to the solvent is 1;
the mass ratio of the UHMWPE resin to the auxiliary agent is 1000 to 1-10.
6. The method for preparing low-temperature spun ultra-fine denier ultra-high molecular weight polyethylene fiber according to claim 5, wherein the solvent is one or more of paraffin oil, kerosene, vegetable oil, decalin, tetrahydronaphthalene, xylene, toluene, dichlorobenzene or petroleum ether;
the auxiliary agent is an antioxidant or a mixture of the antioxidant and the antioxidant auxiliary agent according to the mass ratio of 1000 to 1, wherein the antioxidant and the antioxidant auxiliary agent are phenolic antioxidants.
7. The preparation method of the low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber according to claim 3, wherein the diameter of the twin-screw extruder in the step 3) is 15 to 135cm, the length-diameter ratio is 30 to 72, and the screw temperature is 110 to 190 ℃.
8. The preparation method of the low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber according to claim 3, wherein the spinneret plate is one or more of a circular plate, a square plate and a special-shaped plate, the hole of the spinneret plate is one or more of a circular hole, a triangular hole, a square hole and a special-shaped hole, the hole diameter of the spinneret plate is 0.3 to 1mm, and the length-diameter ratio is 5 to 1.
9. The method for preparing low-temperature spun ultra-fine ultra-high molecular weight polyethylene fiber according to claim 3, wherein the solvent removal method in step 3) is one or more of gas stripping, steam stripping, thermally induced phase separation and extraction; the gas is one or more of nitrogen, flue gas, carbon dioxide and steam.
10. The method for preparing the low-temperature spun ultra-fine denier ultra-high molecular weight polyethylene fiber according to claim 3, wherein the multistage hot drawing in the step 4) is one-stage or more hot drawing, the first stage is drawing of a spinneret, the drawing ratio of the spinneret is 10-100 times, the total drawing ratio is 10 to 1000 times, and the drawing temperature is 60 to 160 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010058457.3A CN111254511B (en) | 2020-01-19 | 2020-01-19 | Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010058457.3A CN111254511B (en) | 2020-01-19 | 2020-01-19 | Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111254511A CN111254511A (en) | 2020-06-09 |
| CN111254511B true CN111254511B (en) | 2022-11-08 |
Family
ID=70954230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010058457.3A Active CN111254511B (en) | 2020-01-19 | 2020-01-19 | Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111254511B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113279078B (en) * | 2021-05-24 | 2023-03-28 | 上海化工研究院有限公司 | Modified ultra-high molecular weight polyethylene fiber and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199798A (en) * | 2011-04-12 | 2011-09-28 | 常熟绣珀纤维有限公司 | Preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers |
| CN102505158A (en) * | 2011-10-25 | 2012-06-20 | 中国科学院宁波材料技术与工程研究所 | High-concentration preparation method for ultra-high molecular weight polyethylene fiber |
| CN104651974A (en) * | 2015-03-13 | 2015-05-27 | 浙江华峰氨纶股份有限公司 | Superfine denier polyurethane fiber and preparation method thereof |
| CN106032583A (en) * | 2015-03-12 | 2016-10-19 | 中国石油化工股份有限公司 | A preparing method of a polyethylene fine-denier moisture-conducting fiber |
| JP2017031545A (en) * | 2012-12-20 | 2017-02-09 | ディーエスエム アイピー アセッツ ビー．ブイ． | Polyolefin yarn and method for producing the same |
| CN110158160A (en) * | 2019-06-28 | 2019-08-23 | 上海化工研究院有限公司 | A kind of method of high concentration gel spinning preparation ultra high molecular weight polyethylene fiber |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015125064A1 (en) * | 2014-02-20 | 2015-08-27 | Reliance Industries Limited | High strength and high modulus ultra-high molecular weight polyethylene fibers |
-
2020
- 2020-01-19 CN CN202010058457.3A patent/CN111254511B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199798A (en) * | 2011-04-12 | 2011-09-28 | 常熟绣珀纤维有限公司 | Preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers |
| CN102505158A (en) * | 2011-10-25 | 2012-06-20 | 中国科学院宁波材料技术与工程研究所 | High-concentration preparation method for ultra-high molecular weight polyethylene fiber |
| JP2017031545A (en) * | 2012-12-20 | 2017-02-09 | ディーエスエム アイピー アセッツ ビー．ブイ． | Polyolefin yarn and method for producing the same |
| CN106032583A (en) * | 2015-03-12 | 2016-10-19 | 中国石油化工股份有限公司 | A preparing method of a polyethylene fine-denier moisture-conducting fiber |
| CN104651974A (en) * | 2015-03-13 | 2015-05-27 | 浙江华峰氨纶股份有限公司 | Superfine denier polyurethane fiber and preparation method thereof |
| CN110158160A (en) * | 2019-06-28 | 2019-08-23 | 上海化工研究院有限公司 | A kind of method of high concentration gel spinning preparation ultra high molecular weight polyethylene fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111254511A (en) | 2020-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101683089B1 (en) | Gelatinized pre-oriented filaments and preparation method thereof and ultra-high molecular weight polyethylene fibers and preparation method thereof | |
| KR101363813B1 (en) | Polyethylene fiber and method for production thereof | |
| CN101591813B (en) | Method for manufacturing super high molecular polyethylene fiber precursor | |
| CN104419996A (en) | Production method of ultrahigh molecular weight polyethylene fiber | |
| CN102181954B (en) | Method for producing polyester industrial yarns with high strength, high elongation and low shrinkage | |
| CN109306541B (en) | Preparation method of high-strength high-modulus polyethylene fiber | |
| CA2660766A1 (en) | Process for the preparation of uhmw multi-filament poly(alpha-olefin) yarns | |
| CN109440215A (en) | A kind of preparation method of high-performance polyethylene fibres | |
| CN102505158A (en) | High-concentration preparation method for ultra-high molecular weight polyethylene fiber | |
| CN103305954A (en) | Method for preparing ultra-high molecular weight polyethylene fiber | |
| CN104313709A (en) | Ultrahigh molecular weight polyethylene fiber and preparation method thereof | |
| CN111254511B (en) | Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof | |
| CN109487349A (en) | A kind of preparation method of ultra-high molecular weight polyethylene monofilaments | |
| WO2022083740A1 (en) | Fiber spinning method, and spun fibers and use thereof | |
| CN113388919A (en) | LDPE/PA6 sea-island fiber and preparation method thereof | |
| CN102644126A (en) | Preparation method for high-strength polyethylene fibers with net structures | |
| CN104846451B (en) | A kind of method directly preparing ultra high molecular weight polyethylene fiber | |
| CN112226851A (en) | Preparation method of polyacrylonitrile-based carbon fiber | |
| JPS6241341A (en) | High speed stretching of gel fiber | |
| CN101629326B (en) | Method for post-treating ultra-high molecular weight polyethylene fiber | |
| CN110820058B (en) | Preparation method of civil high-performance polyethylene fiber | |
| CN118272943A (en) | Preparation method of ultra-high molecular weight polyethylene fiber | |
| CN112941648B (en) | Method for manufacturing high-strength and high-modulus polyethylene fiber | |
| CN115074868B (en) | Preparation method of pre-oxidized fiber and pre-oxidized fiber | |
| CN117385487A (en) | Method for removing heat-resistant creep-resistant ultra-high molecular weight polyethylene oligomer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |