CN119082914A - A kind of high-strength nylon fiber and preparation method thereof - Google Patents
A kind of high-strength nylon fiber and preparation method thereof Download PDFInfo
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/32—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from aromatic diamines and aromatic dicarboxylic acids with both amino and carboxylic groups aromatically bound
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Abstract
The invention discloses a high-strength nylon fiber and a preparation method thereof, and relates to the technical field of chemical fibers, wherein the high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3-5 parts of a coupling agent, 10-20 parts of a reinforcing fiber, 1-2 parts of an antioxidant, 0.6-1 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl borazine, and the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl. The high-strength nylon fiber has high strength and excellent ultraviolet aging resistance and heat aging resistance.
Description
Technical Field
The invention relates to the technical field of chemical fibers, in particular to a high-strength nylon fiber and a preparation method thereof.
Background
Nylon is a commodity name of polyamide fiber, also called nylon, and is the first fiber for realizing industrialization in the world, and is suitable for fabric such as underwear, sportswear and the like due to the characteristics of good moisture absorption, softness, good elasticity and the like, and has good wearing comfort. However, the amide bond of the nylon fiber is easy to be hydrolyzed and cracked under the irradiation of light, particularly ultraviolet rays, so that the macromolecular chain segment is easy to be broken, the molecular weight is reduced, the oxidation aging phenomenon is generated, the strength of the fiber and the finished product is seriously reduced, the social development requirement is difficult to be met, and the high-strength nylon fiber is paid attention to.
Currently, there are many methods for controlling the flow of liquid. In the production process of the high-strength nylon fiber, in order to improve the strength, a plurality of functional master batches are added into the polymer, but the functional master batches are often uneven in dispersion, so that the fiber crystallization areas are distributed differently, and the fracture strength of the fiber is uneven and the durability is not high. In addition, the high-strength nylon fiber on the market has the defects of insufficient ultraviolet resistance, poor heat aging resistance, short service life and the like.
In order to solve the technical problems, the Chinese patent with the authority of bulletin No. CN109402764B discloses a high-strength low-elongation nylon 6 short fiber and a preparation method thereof, wherein the high-strength low-elongation nylon 6 short fiber is prepared by spinning a high-strength low-elongation nylon 6 melt, the high-strength low-elongation nylon 6 is prepared by sequentially carrying out surface chain growth reaction, ring-opening pre-polycondensation reaction, final polycondensation reaction and tackifying reaction on a mixture, the mixture mainly comprises caprolactam, reinforced powder with a catalyst coated on the surface and water, the linear density of the prepared high-strength low-elongation nylon 6 short fiber is 0.89-2.22 dtex, the breaking strength is more than or equal to 6.0cN/dtex, and the breaking elongation is less than or equal to 45%. According to the high-strength low-elongation nylon 6 short fiber and the preparation method thereof, the mechanical property of the nylon 6 short fiber is enhanced by the enhanced powder, and the dispersibility of the enhanced powder in the fiber is good due to the chain growth reaction of the surface of the enhanced powder, so that the finally prepared high-strength low-elongation nylon 6 short fiber has the advantages of good mechanical property, uniform strength distribution and high quality. However, the ultraviolet aging resistance and the heat aging resistance thereof are still to be further improved.
Therefore, the development of the high-strength nylon fiber with high strength and excellent ultraviolet aging resistance and heat aging resistance and the preparation method thereof meet the market demand, have wide market value and application prospect, and have very important significance in promoting the development of the nylon fiber field.
Disclosure of Invention
The invention mainly aims to provide high-strength nylon fiber with high strength and excellent ultraviolet aging resistance and heat aging resistance and a preparation method thereof.
The invention provides high-strength nylon fiber which is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3-5 parts of a coupling agent, 10-20 parts of reinforcing fiber, 1-2 parts of an antioxidant, 0.6-1 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl borazine, wherein the functional polyamide comprises structural units introduced by benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
Preferably, the preparation method of the functional polyamide comprises the following steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2' -bis (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 3-5 hours at the normal pressure of 120-130 ℃, heating to 230-250 ℃, carrying out polycondensation reaction for 15-22 hours at 300-500Pa, cooling to room temperature, regulating to normal pressure, precipitating in water, washing a crude product for 3-6 times by ethanol, and drying to constant weight in a vacuum drying oven at 85-95 ℃ to obtain the functional polyamide.
Preferably, the molar ratio of the benzomelamine, the 2, 3-quinoline dicarboxylic acid, the 2,2' -bis (trifluoromethyl) diaminobiphenyl, the catalyst and the high-boiling point solvent is 0.7:1:0.3 (0.8-1): 8-15.
Preferably, the catalyst is at least one of thiophosphonate, phosphorous acid and thiophosphamide, the high boiling point solvent is dimethyl sulfoxide, and the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570, the antioxidant is at least one of an antioxidant 1010 and an antioxidant 168, and the lubricant is at least one of pentaerythritol stearate and ethylene bis-stearamide.
Preferably, the reinforcing fiber is at least one of a carbon nanofiber and a boron nanofiber.
Preferably, the reinforcing fibers have an average diameter of 100 to 300nm and an aspect ratio of (20 to 30): 1.
The invention further provides a preparation method of the high-strength nylon fiber, which comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
Preferably, in the step S1, the melting temperature of the melt extrusion granulation is 235-285 ℃, and the extrusion pressure is 8-10 MPa.
Preferably, the process parameters of the melt spinning in the step S1 are that the spinning temperature is 230-270 ℃, the winding speed is 1000-1500 m/min, and the draft multiple is 2-4.
Preferably, the stretching ratio of the hot stretching in step S3 is 1 to 2.
Preferably, the radiation grafting in the step S3 is performed at room temperature, the absorption dose is 5-40 kGy, and the dose rate is 5-20 kGy/h.
Preferably, in step S3, the network pressure of the split charging type network device is 1-2kgf/cm 2.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) The preparation method of the high-strength nylon fiber disclosed by the invention has the advantages of simple process, convenience in operation control, high preparation efficiency and finished product qualification rate, low energy consumption, low equipment dependence, suitability for continuous large-scale production and higher popularization and application values. The comprehensive performance (strength, ultraviolet aging resistance and heat aging resistance) and the performance stability of the prepared product are good through reasonable selection of the preparation process parameters.
(2) The invention discloses high-strength nylon fiber which is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3-5 parts of a coupling agent, 10-20 parts of reinforcing fiber, 1-2 parts of an antioxidant, 0.6-1 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl borazine, wherein the functional polyamide comprises structural units introduced by benzene melamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl. Through the mutual matching and combined action of the raw materials, the prepared nylon fiber product has high strength and excellent ultraviolet aging resistance and heat aging resistance.
(3) According to the high-strength nylon fiber disclosed by the invention, through reasonable selection of the types and the dosage proportion of each raw material, the benzomelamine, quinoline, fluorine-containing biphenyl and boroxine structures are simultaneously introduced into the molecular structure of the fiber, and the structures enable the prepared fiber product to have higher strength and more excellent ultraviolet aging resistance and heat aging resistance under the multiple effects of an electronic effect, a steric effect, a conjugation effect and the like. The performance can be further improved by forming an interpenetrating network structure on the surface of the fiber through radiation grafting.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and other obvious variations will occur to those skilled in the art.
Example 1
The high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3 parts of a coupling agent, 10 parts of a reinforcing fiber, 1 part of an antioxidant, 0.6 part of a lubricant and 1 part of 2,4, 6-trivinyl boroxine, wherein the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
The preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2 '-di (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling-point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 3 hours at normal pressure, heating to 230 ℃, carrying out polycondensation reaction for 15 hours under 300Pa, cooling to room temperature, regulating to normal pressure, precipitating in water, washing a crude product with ethanol for 3 times, and drying to constant weight at 85 ℃ in a vacuum drying oven to obtain the functional polyamide, wherein the molar ratio of the benzomelamine to the 2, 3-quinoline dicarboxylic acid to the 2,2' -di (trifluoromethyl) diaminobiphenyl to the catalyst to the high-boiling-point solvent is 0.7:1:0.3:0.8:8, the catalyst is thiophosphonate, the high-boiling-point solvent is dimethyl sulfoxide, and the inert gas is nitrogen. The functional polyamide was measured by GPC test, M n=16183g/mol,MW/Mn =1.418, and the molar ratio of the structural units respectively introduced by benzomelamine, 2, 3-quinolinedicarboxylic acid, 2' -bis (trifluoromethyl) diaminobiphenyl in the functional polyamide was the same as the theoretical value, calculated by elemental analysis and weight change.
The coupling agent is silane coupling agent KH550, the antioxidant is antioxidant 1010, the lubricant is pentaerythritol stearate, the reinforcing fiber is carbon nanofiber, and the average diameter of the reinforcing fiber is 100nm and the length-diameter ratio is 20:1.
The preparation method of the high-strength nylon fiber comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
The melting temperature of the melt extrusion granulation in the step S1 is 235 ℃, the extrusion pressure is 8MPa, the process parameters of the melt spinning in the step S1 are that the spinning temperature is 230 ℃, the winding speed is 1000m/min, the drawing multiple is 3, the drawing ratio of the hot drawing in the step S3 is 2, the radiation grafting in the step S3 is carried out at room temperature, the absorption dose is 5kGy, and the dose rate is 5kGy/h.
The network pressure of the split charging type network device in the step S3 is 1kgf/cm 2.
Example 2
The high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3.5 parts of a coupling agent, 13 parts of a reinforcing fiber, 1.2 parts of an antioxidant, 0.7 part of a lubricant and 1.5 parts of 2,4, 6-trivinyl borazine, wherein the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
The preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2 '-di (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling-point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 3.5 hours at normal pressure, heating to 235 ℃, carrying out polycondensation reaction for 17 hours under 350Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing a crude product with ethanol for 4 times, and drying to constant weight at 87 ℃ in a vacuum drying oven to obtain the functional polyamide, wherein the molar ratio of the benzomelamine, the 2, 3-quinoline dicarboxylic acid, the 2,2' -di (trifluoromethyl) diaminobiphenyl to the catalyst to the high-boiling-point solvent is 0.7:1:0.3:0.85:10, the catalyst is phosphorous acid, the high-boiling-point solvent is dimethyl sulfoxide, and the inert gas is helium.
The coupling agent is silane coupling agent KH560, the antioxidant is antioxidant 168, the lubricant is ethylene bis stearamide, the reinforcing fiber is nano boron fiber, the average diameter of the reinforcing fiber is 150nm, and the length-diameter ratio of the reinforcing fiber is 23:1.
The preparation method of the high-strength nylon fiber comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
The melting temperature of the melt extrusion granulation in the step S1 is 255 ℃, the extrusion pressure is 8.5MPa, the process parameters of the melt spinning in the step S1 are that the spinning temperature is 245 ℃, the winding speed is 1200m/min, the drawing multiple is 3, the stretching ratio of the hot stretching in the step S3 is 2, the radiation grafting in the step S3 is carried out at room temperature, the absorption dose is 10kGy, the dose rate is 8kGy/h, and the network pressure of the split charging type network device in the step S3 is 1.2kgf/cm 2.
Example 3
The high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 4 parts of a coupling agent, 15 parts of a reinforcing fiber, 1.5 parts of an antioxidant, 0.8 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl boroxine, wherein the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
The preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2 '-bis (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling-point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 4 hours at normal pressure, heating to 240 ℃, carrying out polycondensation reaction for 19 hours at 400Pa, cooling to room temperature, regulating to normal pressure, precipitating in water, washing a crude product with ethanol for 5 times, and drying to constant weight at 90 ℃ in a vacuum drying oven to obtain the functional polyamide, wherein the molar ratio of the benzomelamine to the 2, 3-quinoline dicarboxylic acid to the 2,2' -bis (trifluoromethyl) diaminobiphenyl to the catalyst to the high-boiling-point solvent is 0.7:1:0.3:0.9:12, the catalyst is thiophosphamide, the high-boiling-point solvent is dimethyl sulfoxide, and the inert gas is neon.
The coupling agent is silane coupling agent KH570, the antioxidant is antioxidant 1010, the lubricant is pentaerythritol stearate, the reinforcing fiber is carbon nanofiber, the average diameter of the reinforcing fiber is 200nm, and the length-diameter ratio of the reinforcing fiber is 25:1.
The preparation method of the high-strength nylon fiber comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
The melting temperature of the melt extrusion granulation in the step S1 is 265 ℃, the extrusion pressure is 9MPa, the process parameters of the melt spinning in the step S1 are that the spinning temperature is 250 ℃, the winding speed is 1300m/min, the drawing multiple is 3, the stretching ratio of the hot stretching in the step S3 is 2, the radiation grafting in the step S3 is carried out at room temperature, the absorption dose is 25kGy, the dose rate is 10kGy/h, and the network pressure of the split charging type network device in the step S3 is 1.5kgf/cm 2.
Example 4
The high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 4.5 parts of a coupling agent, 18 parts of a reinforcing fiber, 1.8 parts of an antioxidant, 0.9 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl borazine, wherein the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
The preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2 '-di (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling-point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 4.5 hours at normal pressure, heating to 245 ℃, carrying out polycondensation reaction for 20 hours under 450Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing a crude product with ethanol for 6 times, drying to constant weight at 93 ℃ in a vacuum drying oven to obtain the functional polyamide, wherein the molar ratio of the benzomelamine to the 2, 3-quinoline dicarboxylic acid to the 2,2' -di (trifluoromethyl) diaminobiphenyl to the catalyst to the high-boiling-point solvent is 0.7:1:0.3:0.95:14, the catalyst is thiophosphonate, phosphorous acid and thiophosphoramide, the mass ratio of the catalyst to 1:1:3 is mixed, and the solvent is nitrogen gas with the inert gas.
The coupling agent is formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:2:3, the antioxidant is formed by mixing an antioxidant 1010 and an antioxidant 168 according to a mass ratio of 3:5, the lubricant is formed by mixing pentaerythritol stearate and ethylene bis stearamide according to a mass ratio of 1:1, the reinforcing fiber is formed by mixing carbon nanofiber and boron nanofiber according to a mass ratio of 1:4, the average diameter of the reinforcing fiber is 250nm, and the length-diameter ratio of the reinforcing fiber is 28:1.
The preparation method of the high-strength nylon fiber comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
The melting temperature of the melt extrusion granulation in the step S1 is 280 ℃, the extrusion pressure is 9.5MPa, the process parameters of the melt spinning in the step S1 are that the spinning temperature is 265 ℃, the winding speed is 1400m/min, the drawing multiple is 3, the stretching ratio of the hot stretching in the step S3 is 2, the radiation grafting in the step S3 is carried out at room temperature, the absorption dose is 35kGy, the dose rate is 15kGy/h, and the network pressure of the split charging type network device in the step S3 is 1.8kgf/cm 2.
Example 5
The high-strength nylon fiber is prepared from the following raw materials, by weight, 100 parts of functional polyamide, 5 parts of a coupling agent, 20 parts of a reinforcing fiber, 2 parts of an antioxidant, 1 part of a lubricant and 3 parts of 2,4, 6-trivinyl boroxine, wherein the functional polyamide comprises structural units introduced by the following monomers, namely benzomelamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
The preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2 '-bis (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling-point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 5 hours at normal pressure, heating to 250 ℃, carrying out polycondensation reaction for 22 hours under 500Pa, cooling to room temperature, regulating to normal pressure, precipitating in water, washing a crude product with ethanol for 6 times, and drying to constant weight under a vacuum drying oven at 95 ℃ to obtain the functional polyamide, wherein the molar ratio of the benzomelamine to the 2, 3-quinoline dicarboxylic acid to the 2,2' -bis (trifluoromethyl) diaminobiphenyl to the catalyst to the high-boiling-point solvent is 0.7:1:0.3:1:15, the catalyst is thiophosphonate, the high-boiling-point solvent is dimethyl sulfoxide, and the inert gas is helium.
The coupling agent is silane coupling agent KH560, the antioxidant is antioxidant 1010, the lubricant is pentaerythritol stearate, the reinforcing fiber is carbon nanofiber, and the average diameter of the reinforcing fiber is 300nm and the length-diameter ratio is 30:1.
The preparation method of the high-strength nylon fiber comprises the following steps:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
The melting temperature of the melt extrusion granulation in the step S1 is 285 ℃, the extrusion pressure is 10MPa, the technological parameters of the melt spinning in the step S1 are that the spinning temperature is 270 ℃, the winding speed is 1500m/min, the drawing multiple is 3, the stretching ratio of the hot stretching in the step S3 is 2, the radiation grafting in the step S3 is carried out at room temperature, the absorption dose is 40kGy, the dose rate is 20kGy/h, and the network pressure of the split charging type network device in the step S3 is 2kgf/cm 2.
Comparative example 1
A high-strength nylon fiber and a method for preparing the same, which are similar to example 1, except that 2,2' -bis (trifluoromethyl) diaminobiphenyl is replaced by equivalent benzomelamine.
Comparative example 2
A high strength nylon fiber and a method for preparing the same, which is similar to example 1, except that 2,2' -bis (trifluoromethyl) diaminobiphenyl is used in place of benzomelamine in an equivalent amount.
Comparative example 3
A high strength nylon fiber and method of making the same is similar to example 1 except that there is no radiation grafting step.
In order to further illustrate the beneficial technical effects of the high-strength nylon fibers according to the embodiments of the present invention, the high-strength nylon fibers according to examples 1 to 5 and comparative examples 1 to 2 were subjected to the performance test, and the test results are shown in table 1, and the test method is as follows:
(1) Dry breaking strength the dry breaking strength was tested with reference to GB/T14344-2022 method for testing tensile Property of chemical fiber filaments.
(2) Thermal aging resistance by placing the products in a thermal aging box to perform manual accelerated hot air aging under the condition of 85 ℃ for 96 hours, and measuring the thermal aging resistance by the retention rate of the dry breaking strength after aging, wherein the thermal aging resistance is better as the retention rate is larger.
(3) Anti-ultraviolet aging performance, namely, each product is placed in an artificial xenon lamp to be irradiated for 250 hours, the heat aging resistance is measured by the retention rate of the dry breaking strength after aging, and the higher the retention rate value is, the better the anti-ultraviolet aging performance is.
TABLE 1
| Test item | Dry break strength | Thermal aging resistance | Anti-ultraviolet aging property |
| Unit (B) | cN/dtex | % | % |
| Example 1 | 10.13 | 98.79 | 99.35 |
| Example 2 | 10.42 | 98.86 | 99.45 |
| Example 3 | 10.91 | 98.97 | 99.60 |
| Example 4 | 11.15 | 99.18 | 99.82 |
| Example 5 | 11.47 | 99.32 | 99.95 |
| Comparative example 1 | 9.20 | 96.46 | 99.03 |
| Comparative example 2 | 9.31 | 96.73 | 97.64 |
| Comparative example 3 | 9.03 | 95.47 | 98.79 |
As can be seen from table 1, the high-strength nylon fibers according to the examples of the present invention have more excellent breaking strength, uv aging resistance and thermal aging resistance, and the combined use of benzomelamine, 2' -bis (trifluoromethyl) diaminobiphenyl and radiation grafting is beneficial for improving the above properties.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The high-strength nylon fiber is characterized by being prepared from the following raw materials, by weight, 100 parts of functional polyamide, 3-5 parts of a coupling agent, 10-20 parts of reinforcing fiber, 1-2 parts of an antioxidant, 0.6-1 part of a lubricant and 1-3 parts of 2,4, 6-trivinyl borazine, wherein the functional polyamide comprises structural units introduced by benzene melamine, 2, 3-quinoline dicarboxylic acid and 2,2' -bis (trifluoromethyl) diaminobiphenyl.
2. The high-strength polyamide fiber according to claim 1, wherein the preparation method of the functional polyamide comprises the steps of adding benzomelamine, 2, 3-quinoline dicarboxylic acid, 2' -bis (trifluoromethyl) diaminobiphenyl and a catalyst into a high-boiling point solvent, uniformly mixing to obtain a mixed material, adding the mixed material into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 3-5 hours at the normal pressure of 120-130 ℃, heating to 230-250 ℃, performing polycondensation reaction for 15-22 hours at 300-500Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing a crude product with ethanol for 3-6 times, and drying to constant weight in a vacuum drying box at 85-95 ℃ to obtain the functional polyamide.
3. The high-strength nylon fiber according to claim 2, wherein the molar ratio of benzomelamine, 2, 3-quinolinedicarboxylic acid, 2' -bis (trifluoromethyl) diaminobiphenyl, catalyst, high boiling point solvent is 0.7:1:0.3 (0.8-1): 8-15.
4. The high-strength nylon fiber according to claim 2, wherein the catalyst is at least one of thiophosphonate, phosphorous acid and thiophosphamide, the high-boiling point solvent is dimethyl sulfoxide, and the inert gas is any one of nitrogen, helium, neon and argon.
5. The high-strength nylon fiber according to claim 1, wherein the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570, the antioxidant is at least one of an antioxidant 1010 and an antioxidant 168, and the lubricant is at least one of pentaerythritol stearate and ethylene bis-stearamide.
6. The high-strength nylon fiber according to claim 1, wherein the reinforcing fiber is at least one of a carbon nanofiber and a boron nanofiber.
7. The high-strength nylon fiber according to claim 1, wherein the reinforcing fiber has an average diameter of 100 to 300nm and an aspect ratio of (20 to 30): 1.
8. A method for producing the high-strength nylon fiber according to any one of claims 1 to 7, comprising the steps of:
Step S1, uniformly mixing the dried functional polyamide, a coupling agent, reinforcing fibers, an antioxidant and a lubricant to obtain a mixed material, adding the mixed material into a double-screw extruder for melt extrusion granulation, and then carrying out melt spinning by a melt spinning machine, wherein monofilaments are ejected from a spinneret plate;
S2, the monofilaments reach a bundling oiling point to be bundled and are oiled on the surface of the filament bundle, wherein the spinning oil contains 2,4, 6-trivinyl boroxine;
And S3, sequentially carrying out hot stretching on the oiled tows, carrying out radiation grafting by adopting 60 Co-gamma ray sources under the nitrogen atmosphere, and winding at a winding head after passing through a split-type network device to obtain the high-strength nylon fiber.
9. The preparation method of the high-strength nylon fiber according to claim 8, wherein the melting temperature of the melt extrusion granulation in the step S1 is 235-285 ℃, the extrusion pressure is 8-10 MPa, and the process parameters of the melt spinning in the step S1 are that the spinning temperature is 230-270 ℃, the winding speed is 1000-1500 m/min and the draft multiple is 2-4.
10. The preparation method of the high-strength nylon fiber according to claim 8, wherein the stretching ratio of the hot stretching in the step S3 is 1-2, the radiation grafting in the step S3 is performed at room temperature, the absorption dose is 5-40 kGy, the dose rate is 5-20 kGy/h, and the network pressure of the split charging type network device in the step S3 is 1-2kgf/cm 2.
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