CN106757467B - Ultra-high molecular weight polyethylene fiber and preparation method thereof - Google Patents

Ultra-high molecular weight polyethylene fiber and preparation method thereof Download PDF

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CN106757467B
CN106757467B CN201611036204.6A CN201611036204A CN106757467B CN 106757467 B CN106757467 B CN 106757467B CN 201611036204 A CN201611036204 A CN 201611036204A CN 106757467 B CN106757467 B CN 106757467B
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molecular weight
weight polyethylene
ultra
high molecular
antistatic agent
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CN106757467A (en
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许海霞
辛春荣
吴喜龙
张振雷
李自学
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SURREY HI-TECH Inc
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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
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • 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
    • D01D10/02Heat treatment
    • 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
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/16Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/08Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/08Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
    • D06M13/085Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons cycloaliphatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/262Sulfated compounds thiosulfates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • D06M13/463Compounds containing quaternary nitrogen atoms derived from monoamines

Abstract

The invention discloses a preparation method of ultra-high molecular weight polyethylene fibers, which comprises the following steps: (1) preparing ultra-high molecular weight polyethylene gel precursor by a gel spinning method; (2) carrying out balanced standing treatment on the gel protofilaments; (3) sequentially carrying out pre-drafting, extraction and drying and hot-drafting not less than three levels on the gel protofilament subjected to the balanced standing treatment, and enabling the ultra-high molecular weight polyethylene gel protofilament to pass through a coating roller with an antistatic agent aqueous solution while carrying out the hot-drafting; (4) and drying to obtain the ultra-high molecular weight polyethylene fiber. The ultrahigh molecular weight polyethylene fiber prepared by the method of the invention improves high strength and high modulus, solves the problem that the post-processing is influenced by electrification of the fiber, and has lower static electricity.

Description

Ultra-high molecular weight polyethylene fiber and preparation method thereof
Technical Field
The invention belongs to the technical field of fiber preparation, and particularly relates to an ultrahigh molecular weight polyethylene fiber and a preparation method thereof.
Background
The ultra-high molecular weight polyethylene fiber (UHMWPE for short), also called high-strength high-modulus polyethylene fiber, is a high-performance fiber prepared by sequentially spinning, extracting, drying and super-drawing polyethylene with relative molecular weight of more than 100 ten thousand. The fiber reinforced composite material prepared from the ultra-high molecular weight polyethylene fiber has the advantages of light weight, impact resistance, high dielectric property and the like, and is widely applied to the fields of aerospace, sea defense, weaponry, daily industry and the like.
In the prior art, the gel spinning technique is generally used for preparing the ultra-high molecular weight polyethylene fiber. The technology generally uses polyethylene with relative molecular weight of more than 100 ten thousand as raw material, firstly, the raw material is mixed with proper solvent, suspension obtained by mixing and swelling is used as spinning dope, then the spinning dope is sheared, evenly mixed and unwound by a screw extruder, then the spinning dope is extruded by a spinning pack for stretching-condensation forming, thereby obtaining gelation pre-oriented yarn, and finally the gelation pre-oriented yarn is extracted, dried and ultra-drawn to obtain the ultra-high molecular weight polyethylene fiber.
In the production process of the ultra-high molecular weight polyethylene fiber, due to the high friction links such as solvent extraction, drying, hot stretching and high-speed winding, the tows and finished fibers are easy to generate static electricity. In the hot stretching stage, if the static electricity generated by the tows is large and the cohesion of the tows is poor, the tows are mutually entangled during winding, so that the number of broken ends is increased. If the static electricity of the finished fiber is large, a bundle of threads is fluffy and scattered, and thread guide frame hanging and the like are easy to happen when the finished fiber is applied to the downstream for unwinding production, so that the end breakage rate is increased, and the production and the processing are influenced. In order to solve the problem, patent CN103276465A discloses an ultra-high molecular weight polyethylene fiber and a preparation method thereof, which relates to an antistatic oil agent, which is a mixture of a polyoxyethylene ether type antistatic agent and an anionic type antistatic agent, so that the fiber has low static while maintaining high strength and high modulus.
Disclosure of Invention
The invention also aims at the problems in the prior art, and provides the low-static ultrahigh molecular weight polyethylene fiber and the preparation method thereof by using the antistatic agent different from the type, so that the high strength and the high modulus are improved, and the problem that the post-processing of the fiber is influenced by electrification is solved.
The invention also aims to eliminate the static electricity generated in the fiber production process, and the fiber is simultaneously passed through an application roller with antistatic bath solution in the hot drawing process of the fiber, and then is dried and rolled in a hot box. The adopted antistatic bath lotion is a mixed liquid of antistatic liquid and water, the mass concentration of the antistatic liquid is 0.2-0.8%, the liquid feeding speed is 3-15 m/min, the antistatic agent is an efficient cationic antistatic agent (different from an anionic antistatic agent common in the industry), the pH value is 7-9, the effective components are 55-60%, and the antistatic agent is easily soluble in water and most organic solvents such as acetone, butanol, benzene, chloroform, DMF and the like. The action mechanism of the antistatic agent is as follows: the conductive channel is formed on the surface of the material quickly, so that the charge is transferred quickly, a hydrophobic oil film can be formed, the friction coefficient of the fiber is reduced, the static electricity is reduced, and the positive electricity is generated.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the present invention provides a method for preparing ultra-high molecular weight polyethylene fiber, comprising the steps of:
(1) preparing ultra-high molecular weight polyethylene gel precursor by a gel spinning method;
(2) carrying out balanced standing treatment on the ultra-high molecular weight polyethylene gel precursor in the step (1);
(3) then, sequentially carrying out pre-drafting, extraction and drying and not less than three-level hot drafting on the ultra-high molecular weight polyethylene gel precursor yarn subjected to the balanced standing treatment in the step (2), and enabling the ultra-high molecular weight polyethylene gel precursor yarn to pass through a coating roller with an antistatic agent aqueous solution while carrying out the hot drafting;
(4) drying to obtain ultra-high molecular weight polyethylene fiber;
the mass concentration of the antistatic agent aqueous solution is 0.2-0.8%, the antistatic agent is a quaternary ammonium salt cation high-efficiency antistatic agent obtained by reacting an alkylating agent with fatty amine, and the kinematic viscosity of the antistatic agent at 40 ℃ is 15-20 mPa.s.
Further, the alkylating agent is any one of alkyl halide or dialkyl sulfate; the aliphatic amine is any one of a lower tertiary amine or a higher polyamine.
Further, the halogenated alkyl is methyl chloride or benzyl chloride, etc., and the dialkyl sulfate is dimethyl sulfate.
Further, the quaternary ammonium salt cation high-efficiency antistatic agent is selected from one or more of alkyl trimethyl ammonium salt, dialkyl dimethyl ammonium salt and alkyl dimethyl benzyl ammonium salt.
Further, the quaternary ammonium salt cation high-efficiency antistatic agent comprises dodecyl dimethyl ethyl ammonium bromide, dodecyl dimethyl hydroxyethyl ammonium chloride and didodecyl dimethyl ammonium chloride.
Preferably, the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 30-40% of dodecyl dimethyl ethyl ammonium bromide, 20-30% of dodecyl dimethyl hydroxyethyl ammonium chloride and 30-40% of didodecyl dimethyl ammonium chloride by mass percentage; more preferably, the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 35% of dodecyl dimethyl ethyl ammonium bromide, 28% of dodecyl dimethyl hydroxyethyl ammonium chloride and 37% of didodecyl dimethyl ammonium chloride.
Further, the pH value of the antistatic agent is 7-9; preferably, the pH value of the antistatic agent is 7.5-8.5.
Further, the water in the antistatic oil solution is soft water with the hardness of less than 0.1-0.15 mmol/L alkaline earth ion concentration; preferably, the water in the antistatic oil solution is soft water with the hardness of less than 0.12-0.13 mmol/L alkaline earth ion concentration.
Further, the liquid feeding speed of the coating roller is 3-15 m/min, and the liquid carrying amount is 1-5%; preferably, the liquid feeding speed of the coating roller is 8-12 m/min, and the liquid carrying amount is 3-4%.
Further, the hot drawing comprises a first-stage hot drawing, a second-stage hot drawing and a third-stage hot drawing, and the antistatic oil solution is coated behind a first drawing roller of the second-stage hot drawing and in front of a hot air box of the second-stage hot drawing.
Further, the total drafting multiple applied to the ultra-high molecular weight polyethylene gel precursor in the processes of pre-drafting, extracting, drying and carrying out hot drafting not less than three levels is 40-50; preferably, the total stretching multiple is 45-47.
Further, the drying temperature in the step (3) is 50-60 ℃; preferably, the drying temperature is 52-58 ℃; more preferably, the drying temperature is 55-56 ℃.
Further, the drying temperature in the step (4) is 60-80 ℃; preferably, the drying temperature is 65-78 ℃; more preferably, the drying temperature is 70-72 ℃.
In a second aspect of the present invention, there is provided an ultra-high molecular weight polyethylene fiber prepared by the above method.
Further, the electrostatic voltage of the ultra-high molecular weight polyethylene fibers is <0.05 kV.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the method adopts cationic active amines as antistatic agents, has simple formula, can be mutually dissolved with water, and can quickly transfer charges by quickly forming a conductive channel on the surface of a material; the cationic active amine antistatic agent can form a hydrophobic oil film on the surface of the fiber, can effectively reduce the friction coefficient of the fiber, and also protects the surface of the fiber from generating broken filaments due to friction; the adopted antistatic agent has strong effect, good cohesive force and less dosage; the cationic active amine antistatic agent used in the invention has small viscosity and low liquid feeding speed, the fiber is not easy to stick and wind a stick in the production process, and the fiber does not influence the fineness while eliminating static electricity; in addition, the hot drafting is not less than three-level positive drafting, and the upper liquid coating roller is positioned before the last level hot drafting (namely heat setting), so that the drying of the antistatic liquid can be ensured, and the chapping of the surface of the fiber due to the front several levels of positive drafting can be avoided; the ultra-high molecular weight polyethylene fiber prepared by the method has the electrostatic voltage of less than 0.05kV, has good antistatic effect, is relatively soft, and has good social popularization and application values.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
The invention provides a preparation method of ultra-high molecular weight polyethylene fibers, which comprises the following steps:
(1) preparing ultra-high molecular weight polyethylene gel precursor by a gel spinning method;
the process is thatAs is well known to those skilled in the art, this includes in particular: feeding the ultra-high molecular weight polyethylene spinning solution into a double-screw extruder for blending extrusion to obtain a first spinning solution, then feeding the first spinning solution into a spinning manifold, and performing drafting and rapid cooling solidification to obtain ultra-high molecular weight polyethylene gel precursor; wherein the weight average molecular weight of the ultra-high molecular weight polyethylene adopted by the invention is preferably 3-5 multiplied by 106More preferably, the invention adopts a first ultrahigh molecular weight polyethylene and a second ultrahigh molecular weight polyethylene in a weight ratio of 3-8: 1, wherein the weight average molecular weight of the first ultrahigh molecular weight polyethylene is 4-5 x 106The weight average molecular weight of the second ultra-high molecular weight polyethylene is 3-4 multiplied by 106(ii) a In addition, the ultra-high molecular weight polyethylene powder used in the invention is preferably distributed in a Gaussian curve, and the particle size is preferably 60-200 meshes;
(2) carrying out balanced standing treatment on the ultra-high molecular weight polyethylene gel precursor in the step (1);
the ultra-high molecular weight polyethylene gel precursor can shrink to a certain extent when standing still, so that the original internal stress is effectively reduced; the balanced standing treatment is a technical means well known by a person skilled in the art, the standing temperature is preferably 25-45 ℃, more preferably 20-55 ℃, and the standing time is 4-6 hours;
(3) then, sequentially carrying out pre-drafting, extraction and drying and not less than three-level hot drafting on the ultra-high molecular weight polyethylene gel precursor yarn subjected to the balanced standing treatment in the step (2), and enabling the ultra-high molecular weight polyethylene gel precursor yarn to pass through a coating roller with an antistatic agent aqueous solution while carrying out the hot drafting;
after standing, pre-drafting high molecular weight polyethylene gel precursor, wherein the pre-drafting, extracting, drying and hot-drafting are carried out for not less than three levels, and the total drafting multiple applied to the ultra-high molecular weight polyethylene gel precursor in the process is 40-50; preferably, the total stretching multiple is 45-47; the drying temperature is 50-60 ℃; preferably, the drying temperature is 52-58 ℃; more preferably, the drying temperature is 55-56 ℃; further, the liquid feeding speed of the coating roller is 3-15 m/min, and the liquid carrying amount is 1-5%; the liquid feeding speed of the coating roller is 8-12 m/min, and the liquid carrying amount is 3-4%; the hot drawing comprises a first-stage hot drawing, a second-stage hot drawing and a third-stage hot drawing, and the antistatic oil solution is coated behind a first drawing roller of the second-stage hot drawing and in front of a hot air box of the second-stage hot drawing;
(4) drying to obtain ultra-high molecular weight polyethylene fiber; wherein the drying temperature is 60-80 ℃; preferably, the drying temperature is 65-78 ℃; more preferably, the drying temperature is 70-72 ℃.
Wherein the mass concentration of the antistatic agent aqueous solution is 0.2-0.8%, preferably 0.3-0.6%, and more preferably 0.4-0.5%; the kinematic viscosity of the antistatic agent at 40 ℃ is 15-20 mPa.s, preferably 16-18 mPa.s; the pH value of the antistatic agent is 7-9; preferably, the pH value of the antistatic agent is 7.5-8.5; preferably 7.8-8.2, so that the aqueous solution of the antistatic agent is alkaline.
In the invention, the antistatic agent is a quaternary ammonium salt cation high-efficiency antistatic agent obtained by reacting fatty acid with organic amine. From the technical effect, the cationic active amine as the antistatic agent has simple formula, can be mutually dissolved with water, and can quickly transfer charges by quickly forming a conductive channel on the surface of a material; a hydrophobic oil film can be formed on the surface of the fiber, so that the friction coefficient of the fiber can be effectively reduced, and broken filaments generated on the surface of the fiber due to friction are also protected; the adopted antistatic agent has strong effect, good cohesive force and less dosage; meanwhile, the antistatic agent has low viscosity and low liquid feeding speed, the fiber is not easy to stick and wind a stick in the production process, and the fiber does not influence the fineness while eliminating static electricity; the electrostatic voltage of the ultra-high molecular weight polyethylene fiber prepared by the quaternary ammonium salt cation high-efficiency antistatic agent is less than 0.05kV, preferably 0.002-0.008 kV, and the antistatic effect is good. The ultra-high molecular weight polyethylene fiber may have a fineness of 50D, 75D, 100D, 125D, 150D, 200D, 300D, 400D, 600D, 800D, 1200D, 1600D, and the like. The static voltage of the ultra-high molecular weight polyethylene fiber prepared by the invention is far lower than that of the prior patent CN103276465A, so that the ultra-high molecular weight polyethylene fiber has lower static electricity and good strand aggregation, and is beneficial to application.
Wherein, the alkylating reagent is any one of alkyl halide or dialkyl sulfate; the fatty amine is any one of lower tertiary amine or higher polyamine; preferably, the alkyl halide is methyl chloride or benzyl chloride, or the like. The dialkyl sulfate is dimethyl sulfate.
In order to further improve the mechanical property or antistatic property of the ultrahigh molecular weight polyethylene fiber, the quaternary ammonium salt cation high-efficiency antistatic agent is selected from one or more of alkyl trimethyl ammonium salt, dialkyl dimethyl ammonium salt and alkyl dimethyl benzyl ammonium salt; preferably, the quaternary ammonium salt cation high-efficiency antistatic agent comprises dodecyl dimethyl ethyl ammonium bromide, dodecyl dimethyl hydroxyethyl ammonium chloride and didodecyl dimethyl ammonium chloride.
More preferably, the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 30-40% of dodecyl dimethyl ethyl ammonium bromide, 20-30% of dodecyl dimethyl hydroxyethyl ammonium chloride and 30-40% of didodecyl dimethyl ammonium chloride by mass percentage; more preferably, the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 35% of dodecyl dimethyl ethyl ammonium bromide, 28% of dodecyl dimethyl hydroxyethyl ammonium chloride and 37% of didodecyl dimethyl ammonium chloride.
Compared with the antistatic liquid in the patent in the same benefit of Beijing, the antistatic liquid adopted by the invention has the advantages that: a. the antistatic effect is strong, the cohesion of the fiber bundles is good, and particularly, an oil film formed on the surface can greatly reduce the friction coefficient and has a larger effect on fine denier fibers; b. the dosage is small, and the cost is low; c. the formula is simple and the use is convenient; d. the oil solution is not sticky and is dried quickly, the stability of the production process is not influenced basically, and the fineness of the product is not influenced; e. the paint is soluble in water and is environment-friendly; f. has wide application range and can be mixed with other cationic and nonionic surfactants.
When the antistatic oil solution is prepared, softened water is preferably used to form a clear solution, so that the application is facilitated, namely the water in the antistatic oil solution is preferably soft water with the hardness of 0.1-0.15 mmol/L alkaline earth ion concentration; preferably, the water in the antistatic oil solution is soft water with the hardness of less than 0.12-0.13 mmol/L alkaline earth ion concentration.
In order to further understand the present invention, the following will specifically describe the ultra-high molecular weight polyethylene fiber and the preparation method thereof provided by the present invention with reference to the examples.
In the following examples, the weight average molecular weight of the first ultra-high molecular weight polyethylene powder was 4.8 × 106The weight average molecular weight of the second ultra-high molecular weight polyethylene powder was 3.2X 106The granularity of the powder is 80-100 meshes.
The mass concentration of the antistatic agent aqueous solution is 0.2-0.8%, the antistatic agent is a quaternary ammonium salt cation high-efficiency antistatic agent obtained by reacting an alkylating agent with fatty amine, the kinematic viscosity of the antistatic agent at 40 ℃ is 15-20 mPa.s, and the antistatic agent is mixed with soft water to obtain the antistatic oil solution.
EXAMPLE 1 preparation of ultra high molecular weight polyethylene fibers
a. Preparing ultra-high molecular weight polyethylene 150D gel precursor by a gel spinning method;
b. and after balancing treatment, pre-drafting, extracting and drying the gel protofilament in sequence, and then performing hot drafting not less than three levels to obtain the 150D fiber.
c. The obtained fiber passes through a coating roller with antistatic bath liquid, then passes through a hot box, and is dried and heat-set at the same time, so as to obtain a 150D product of the ultra-high molecular weight polyethylene low-static fiber.
The bath solution is a mixed solution of antistatic liquid and water, the antistatic liquid is a quaternary ammonium salt cation high-efficiency antistatic agent prepared from 30% of dodecyl dimethyl ethyl ammonium bromide, 30% of dodecyl dimethyl hydroxyethyl ammonium chloride and 40% of didodecyl dimethyl ammonium chloride, the concentration of the liquid feeding is 0.3%, the roll surface of the coating roll is made of a chromium plating material, the surface roughness is 0.5, and the liquid feeding speed of the coating roll is 10 m/min.
EXAMPLE 2 preparation of ultra high molecular weight polyethylene fibers
The process of a and b was the same as in example 1 to obtain 200D fiber.
c. The procedure is as in example 1, but the feed concentration is 0.5%, and the feed speed of the coating roll is 6 m/min; a 200D product of ultra high molecular weight polyethylene low static fiber. .
EXAMPLE 3 preparation of ultra high molecular weight polyethylene fibers
a and b were processed as in example 1 to provide 1600D fibers.
c. The process is the same as example 1, but the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 35% of dodecyl dimethyl ethyl ammonium bromide, 28% of dodecyl dimethyl hydroxyethyl ammonium chloride and 37% of didodecyl dimethyl ammonium chloride, the concentration of the solution feeding is 0.5%, the solution feeding speed of a coating roller is 6m/min, and a 1600D product of the ultra-high molecular weight polyethylene low-static fiber is prepared.
Comparative example 1 preparation of ultra high molecular weight polyethylene fiber
a. Preparing ultra-high molecular weight polyethylene 200D gel precursor by a gel spinning method;
b. and after balancing treatment, pre-drafting, extracting and drying the gel protofilament in sequence, and then performing hot drafting not less than three levels to obtain the 200D fiber.
c. The obtained fiber passes through a coating roller with antistatic bath liquid, then passes through a hot box, and is dried and heat-set at the same time, so that the ultra-high molecular weight polyethylene low-static fiber is obtained.
The bath liquid is a mixture of antistatic liquid and water, the antistatic liquid is PP-L969 from Goulstontech flores, USA, and the concentration of the supernatant liquid is 0.5%. The surface of the coating roller is made of chromium plating material, the surface roughness is 0.5, and the liquid feeding speed of the coating roller is 12 m/min.
Comparative example 2 preparation of ultra high molecular weight polyethylene fiber
Different from example 2, the antistatic oil agent in the antistatic oil agent aqueous solution was used as follows: the mixture of the polyoxyethylene ether type antistatic agent and the anionic antistatic agent has the pH value of 7 at the temperature of 20 ℃ and the viscosity of 85 mPa.s at the temperature of 20 ℃ to prepare a 200D product of the ultra-high molecular weight polyethylene fiber.
Comparative example 3 preparation of ultra high molecular weight polyethylene fiber
The technical scheme of patent CN103276465A example 3 is adopted to prepare a 200D product of the ultra-high molecular weight polyethylene fiber.
Comparative example 4 preparation of ultra high molecular weight polyethylene fiber
Different from example 3, the antistatic oil agent in the antistatic oil agent aqueous solution was used as follows: the mixture of the polyoxyethylene ether type antistatic agent and the anionic antistatic agent has the pH value of 7 at the temperature of 20 ℃ and the viscosity of 85 mPa.s at the temperature of 20 ℃ to prepare a 1600D product of the ultra-high molecular weight polyethylene fiber.
Comparative example 5 preparation of ultra high molecular weight polyethylene fiber
A1600D product of the ultra-high molecular weight polyethylene fiber is prepared by adopting the technical scheme of patent CN103276465A example 4.
And (3) performance testing:
the products obtained in examples 1 to 3 and comparative examples 1 to 5 were subjected to performance tests such as electrostatic voltage tests, respectively. The test results are shown in table 1 below:
TABLE 1 Main Performance indices of ultra-high molecular weight polyethylene fibers
Figure BDA0001159732180000081
From the test results in table 1, it can be seen that, compared with the prior art or the technical scheme of patent CN103276465A, the ultrahigh molecular weight polyethylene fiber prepared by the method of the present invention has lower electrostatic voltage, higher modulus and strength, is more beneficial to popularization and application, and has the advantages of simple preparation method, convenient operation, and good social and economic benefits.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.

Claims (6)

1. A preparation method of ultra-high molecular weight polyethylene fiber is characterized by comprising the following steps:
(1) preparing ultra-high molecular weight polyethylene gel precursor by a gel spinning method;
(2) carrying out balanced standing treatment on the ultra-high molecular weight polyethylene gel precursor in the step (1);
(3) then, sequentially carrying out pre-drafting, extraction and drying and not less than three-level hot drafting on the ultra-high molecular weight polyethylene gel precursor yarn subjected to the balanced standing treatment in the step (2), and enabling the ultra-high molecular weight polyethylene gel precursor yarn to pass through a coating roller with an antistatic agent aqueous solution while carrying out the hot drafting; wherein the liquid feeding speed of the coating roller is 3-15 m/min, and the liquid carrying amount is 1-5%;
(4) drying to obtain the ultra-high molecular weight polyethylene fiber, wherein the electrostatic voltage of the ultra-high molecular weight polyethylene fiber is less than 0.05 kV; the mass concentration of the antistatic agent aqueous solution is 0.2-0.8%, the antistatic agent is a quaternary ammonium salt cation high-efficiency antistatic agent obtained by reacting an alkylating agent with fatty amine, and the kinematic viscosity of the antistatic agent at 40 ℃ is 15-20 mPa.s;
the quaternary ammonium salt cation high-efficiency antistatic agent is prepared from 30-40% of dodecyl dimethyl ethyl ammonium bromide, 20-30% of dodecyl dimethyl hydroxyethyl ammonium chloride and 30-40% of didodecyl dimethyl ammonium chloride in percentage by mass.
2. The method of claim 1, wherein the water in the antistatic oil solution is soft water having a hardness of less than 0.1 to 0.15 mmol/l alkaline earth ion concentration.
3. The method of claim 1, wherein the hot drawing comprises a first stage hot drawing, a second stage hot drawing and a third stage hot drawing, and the antistatic oil solution is applied after the first drawing roller of the second stage hot drawing and before the hot air box of the second stage hot drawing.
4. The method for preparing ultra-high molecular weight polyethylene fiber according to claim 1, wherein the total draft ratio applied to the ultra-high molecular weight polyethylene jelly precursor fiber during the pre-drafting, the extracting, the drying and the hot-drafting not less than three stages is 40 to 50.
5. The method for preparing ultra-high molecular weight polyethylene fiber according to claim 1, wherein the drying temperature in the step (3) is 50 to 60 ℃ and the drying temperature in the step (4) is 60 to 80 ℃.
6. An ultra high molecular weight polyethylene fiber prepared by the method of any one of claims 1 to 5.
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