CN101545152A - Ageing-resistant high-strength nylon filament suitable for outdoor use, and preparation method thereof - Google Patents
Ageing-resistant high-strength nylon filament suitable for outdoor use, and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nylon filament, in particular to a nylon filament prepared through compound modification and having high strength, resistance to ultraviolet radiation ageing and suitability for long-term outdoor use. The ageing-resistant high-strength nylon filament suitable for outdoor use is prepared by melting, blending and spinning nylon resin added with additives by weight percentage as follows: 0.01 to 0.5 percent of heat stabilizer, 0.01 to 0.5 percent of anti-ultraviolet additive and 0.01 to 0.5 percent of lubricant, wherein the weight percentage takes 100 kilograms of nylon resin as 100 percent. The nylon resin adopts nylon 6 or nylon 66, and has relative viscosity between 2.7 and 3.6. The preparation method is based on the mechanism of nylon degradation, adds the compound additives to the nylon resin, and blocks off the prior way of degrading nylon material, thereby improving the comprehensive performance of the nylon filament and prolonging the life span of nylon-filament products in outdoor environment.
Description
Technical field
The present invention relates to a kind of Tynex, refer in particular to the high strength that makes by composite modified, ultraviolet-resistant aging, the Tynex of suitable long-term outdoor use.
Technical background
Nylon is owing to its excellent comprehensive performance, and as higher intensity, endurance, self-lubricating, wear-resisting, resistance to chemical attack have purposes very widely.As nylon fiber, roughly can be divided into following big classification at present:
The first kind is an industrial filament, and main purposes is the framework material as rubber, as tyre cord, tire bead cloth, and conveyer belt, rubber tube etc.These class long filament great majority are multifilament.This class purposes requires long filament that high intensity is arranged, good DIMENSIONAL STABILITY, and high heat resistance requires long filament to expose to the open air in 180 ℃ air 4 hours, and strength retention is greater than 90%.But because on all purposes, nylon all is in the inside of rubber, so color and luster, the ultraviolet resistance degraded of Tynex do not claimed.
Second class is the purposes of textile clothing, just usually said civilian silk, and these class long filament great majority also are multifilament, pure nylon can satisfy the needs of these type of all physical properties of purposes fully.
The 3rd class also is a main application of the present invention, various ropes, fishing net, industry or military ribbon, tarpaulin, lamp house cloth.The long filament that this class purposes is used is when goods are new product, and its intensity is satisfied the demand fully.Owing to can not occur in the situation that environment uses more than 100 ℃ substantially, so this type of nylon products is not generally made requirement to heat resistance.But, under high temperature or strong UV environment, all can degrade because the weatherability of pure nylon is general.And this type of purposes substantially all out of doors, and along with the prolongation of service time, the intensity of goods can reduce gradually, until using.
Chinese invention patent application (application number: 200510031902.2) disclose a kind of high strength ultra tough nylon alloy of ageing resistance by ultraviolet light, in nylon resin, be that the polymer of main flexibilizer, band oxygen functional group is secondary flexibilizer, adds compound ultraviolet light auxiliary agent and antioxidant simultaneously, improve the combination property of nylon resin by the polymer that adds an amount of band high reaction activity functional group.Its component and content (parts by weight) are as follows: 70～90 parts of nylon resins, 10～30 parts of main flexibilizer, 0.2～3 part of secondary flexibilizer, 0.1～1 part of compound ultraviolet light auxiliary agent, 0.1～0.5 part in antioxidant.Alloy material has the excellent in resistance low-temperature impact, ultraviolet resistance is aging and good mechanical strength.
Summary of the invention
In order to solve above-mentioned technological deficiency, an object of the present invention is to provide a kind of high fracture strength that both had, have the Tynex of good weather resistance again, to satisfy under continuous high-intensity ultraviolet environment, to the requirement in service life of nylon fiber goods.Second purpose of the present invention provides the preparation method of above-mentioned Tynex.
In order to realize first above-mentioned purpose, the present invention has adopted following technical scheme:
A kind of ageing-resistant high-strength nylon filament of suitable outdoor use, this Tynex adds the auxiliary agent melt blending of following components by weight percent by nylon resin, makes by spinning technique again:
Heat stabilizer: 0.01～0.5wt%;
Uvioresistant auxiliary agent: 0.01～0.5wt%;
Lubricant: 0.01～0.5wt%;
Above-mentioned percentage by weight is 100% with the 100kg nylon resin; Nylon resin is selected nylon 6 or nylon 66 for use, and its relative viscosity is 2.7～3.6.
Above-mentioned heat stabilizer is used to improve the heat resistanceheat resistant oxygen degradation property of product; The uvioresistant auxiliary agent is used to improve the ultraviolet light degradation property of product; Lubricant is used for increasing when melt extruding lubricated, prevents to extrude the living hot heat that produces of molecule outside and internal friction and causes degraded, the spinning property of raising product.
As preferably, above-mentioned heat stabilizer is selected from one or both and the two or more compounds in arylamine class, Hinered phenols, halogen copper salt kind, phosphorous acid lipid, the benzimidazole type thermal stabilizing agent.
As preferred again, above-mentioned heat stabilizer is selected from 2-mercaptobenzidazole, cuprous iodide, three (2, the 4-di-tert-butyl-phenyl) phosphite ester, 4,4-butylidene-two (6-tert-butyl group metacresol, N, N '-hexa-methylene-two [(3,5-di-t-butyl-4-hydroxy benzenes propionamide], one or both and two or more compounds in four (3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) season the eleventh of the twelve Earthly Branches tetrol ester.
As preferably, above-mentioned uvioresistant auxiliary agent is selected from one or both and the two or more compounds in hindered amines, benzotriazole, hindered piperidine class, the benzophenone uvioresistant auxiliary agent.
Be selected from (2-(the 2-hydroxyl-3-tert-butyl group-5-aminomethyl phenyl)-5-chlorinated benzotriazole as preferred again, above-mentioned uvioresistant auxiliary agent, two (2,2,6,6-tetramethyl-4-piperidyl) sebacate, Octabenzone, poly-{ [6-[(1,1,3, the 3-tetramethyl butyl) amino]]-1,3,5-triazine-2,4-two [(2,2,6,6 ,-tetramethyl-4-piperidyl) imino group]-1, oneself two supports [(2 of 6-, 2,6,6-tetramethyl-4-piperidyl) imino group], 2-(2-hydroxyl-3,5-di-tert-butyl-phenyl) benzotriazole, succinic acid and (4-hydroxyl-2,2,6, the polymer of 6-tetramethyl-1-piperidines alcohol, Octabenzone, N, N '-two (2,2,6,6-tetramethyl-4-piperidyl) one or both in 1,3 benzenedicarboxamide and two or more compounds.
As preferably, above-mentioned lubricant is selected from a kind of in erucyl amide, stearic amide, the metallic soap of stearic acid.
As preferably, above-mentioned Tynex is that Denier range is the multifilament of 210～3360 DENIER.
In order to realize first above-mentioned purpose, the present invention has adopted following technical scheme:
A kind of method of ageing-resistant high-strength nylon filament of suitable outdoor use, this method comprise the steps: to adopt above-mentioned prescription to mix in the load weighted said components input bipyramid spiral agitator; Add screw extruder then, the temperature of screw extruder is set to 290～298 ℃, 295～305 ℃, 295～305 ℃, 295～305 ℃, 290～295 ℃, 290～295 ℃, head pressure is set at 10～15Mpa, 290～300 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 15～17RPM, the tow of ejection is at 15～20 ℃, quenching is shaped in the air of relative humidity 75%～85%, then at 190～200 ℃ of following two-stages drawing and settings of totally 4.5～5.5 times that pass through, again by behind the compressed air network device, coiling and molding.
The present invention adds composite assistant from the mechanism of nylon degraded in nylon resin, all known degradation pathway of blocking-up nylon material are improved the combination property of Tynex, prolongs its goods service life under the environment out of doors.
The specific embodiment
Embodiment 1
Nylon 6 resin 100kg, relative viscosity 3.45, composite type heat stabilizing agent 0.33wt% (2-mercaptobenzidazole 0.3wt%+ cuprous iodide 0.03wt%, with 100kg nylon resin weight is radix), (2-(the 2-hydroxyl-3-tert-butyl group-5-aminomethyl phenyl)-5-chlorinated benzotriazole 0.2wt%+ two (2 for compound uvioresistant auxiliary agent 0.4wt%, 2,6,6-tetramethyl-4-piperidyl) sebacate 0.2wt%, with 100kg nylon resin weight is radix), lubricant ethylene bis stearic acid amide 0.3wt% (is radix with 100kg nylon resin weight).To mix 1 hour in the load weighted said components input bipyramid spiral agitator.Add screw extruder then, the temperature of screw extruder is set to 298 ℃, 305 ℃, 305 ℃, 305 ℃, 295 ℃, 295 ℃, head pressure is set at 12Mpa, 295 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 16.28RPM, the tow of ejection is at 18 ℃, quenching is shaped in the air of relative humidity 80%, then at 195 ℃ of following two-stages drawing and settings of totally 4.9 times that pass through, after being 0.6Mpa compressed air network device by bleed pressure, the finished product long filament was with 2610m/ minute speed coiling and molding.The specification of finished product long filament is 840D/140f.The finished product long filament is tested according to GB/T14344-93, the results are shown in Table 1:
(table 1)
The ultraviolet-resistant aging performance test of embodiment finished product long filament, because synthetic fiber also do not have relevant examination criteria at present, so, GB/T16422.1 and GB/T16422.3 plastics laboratory light source exposure test method are adopted in the wood invention, to the finished product long filament with to carry out ultraviolet accelerated ageing in the same old way, according to GB/T14344-93 the sample after aging is tested then.To adopt pure nylon 6 in the same old way, processing method is identical with embodiment.Degradation adopts UV-B type fluorescent ultra-violet lamp, and the form that exposes to the open air of sample is: to sample irradiation 4 hours, condensation exposed to the open air 4 hours under 50 ± 3 ℃ of conditions of black normal temperature then, these two steps of circulation repetition under black 60 ± 3 ℃ of conditions of normal temperature.Test result after 500 hours and accelerated ageing in 1000 hours sees Table 2:
Table (2)
Because there are general character in the thermal-oxidative degradation and the ultraviolet degradation of nylon material on mechanism of degradation, and influence each other, so adopt the condition that exposes 4 hours in 180 ℃ the air to the open air to embodiment 1 finished product with to carry out the heat resistance test in the same old way simultaneously, characterize the ultraviolet-resistant aging performance of sample from the side.After the hot oxygen accelerated ageing, the sample test method is according to GB/T14344-93, and test result sees Table 3:
Table (3)
Embodiment 2
Nylon 6 resin 100kg, relative viscosity 3.35, composite type heat stabilizing agent 0.3wt% (three (2, the 4-di-tert-butyl-phenyl) phosphite ester 0.1wt%+4,4-butylidene-two (6-tert-butyl group metacresol) 0.2wt%, with 100kg nylon resin weight is radix), (Octabenzone 0.2wt%+ gathers { [6-[(1,1,3 to compound uvioresistant auxiliary agent 0.4wt%, the 3-tetramethyl butyl) amino]]-1,3,5-triazine-2,4-two [(2,2,6,6 ,-tetramethyl-4-piperidyl) imino group]-1,6-oneself two the support [(2,2,6,6-tetramethyl-4-piperidyl) imino group] 0.2wt%, with 100kg nylon resin weight is radix), lubricant ethylene bis stearic acid amide 0.3wt% (is radix with 100kg nylon resin weight).To mix 1 hour in the load weighted said components input bipyramid spiral agitator.Add screw extruder then, the temperature of screw extruder is set to 290 ℃, 295 ℃, 295 ℃, 295 ℃, 290 ℃, 290 ℃, head pressure is set at 12Mpa, 290 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 16.28RPM, the tow of ejection is at 18 ℃, quenching is shaped in the air of relative humidity 80%, then at 195 ℃ of following two-stages drawing and settings of totally 4.9 times that pass through, after being 0.6Mpa compressed air network device by bleed pressure, the finished product long filament was with 2610m/ minute speed coiling and molding.The specification of finished product long filament is 840D/140f.The finished product long filament is tested according to GB/T14344-93, the results are shown in Table 4:
Table (4)
GB/T16422.1 and GB/T16422.3 plastics laboratory light source exposure test method are adopted in the ultraviolet-resistant aging performance test of finished product long filament, and the finished product long filament is carried out ultraviolet accelerated ageing, according to GB/T14344-93 the sample after aging are tested then.Degradation adopts UV-B type fluorescent ultra-violet lamp, and the form that exposes to the open air of sample is: to sample irradiation 4 hours, condensation exposed to the open air 4 hours under 50 ± 3 ℃ of conditions of black normal temperature then, these two steps of circulation repetition under black 60 ± 3 ℃ of conditions of normal temperature.Test result after 500 hours and accelerated ageing in 1000 hours sees Table 5:
Table (5)
Adopt the condition that exposes 4 hours in 180 ℃ the air to the open air that embodiment 2 finished products are carried out the heat resistance test.After the hot oxygen accelerated ageing, the sample test method is according to GB/T14344-93, and test result sees Table 6:
Table (6)
Embodiment 3
Nylon 6 resin 100kg, relative viscosity 3.35, composite type heat stabilizing agent 0.45wt% (three (2, the 4-di-tert-butyl-phenyl) phosphite ester 0.15wt%+N, N '-hexa-methylene-two [(3,5-di-t-butyl-4-hydroxy benzenes propionamide] 0.3wt%, with 100kg nylon resin weight is radix), compound uvioresistant auxiliary agent 0.5wt% (2-(2-hydroxyl-3,5-di-tert-butyl-phenyl) benzotriazole 0.25wt%+ succinic acid and (4-hydroxyl-2,2,6, the polymer of 6-tetramethyl-1-piperidines alcohol) 0.25wt% is a radix with 100kg nylon resin weight), magnesium stearate lubricant 0.3wt% (is radix with 100kg nylon resin weight).To mix 1 hour in the load weighted said components input bipyramid spiral agitator.Add screw extruder then, the temperature of screw extruder is set to 290 ℃, 295 ℃, 295 ℃, 295 ℃, 290 ℃, 290 ℃, head pressure is set at 12Mpa, 290 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 16.28RPM, the tow of ejection is at 18 ℃, quenching is shaped in the air of relative humidity 80%, then at 195 ℃ of following two-stages drawing and settings of totally 4.9 times that pass through, after being 0.6Mpa compressed air network device by bleed pressure, the finished product long filament was with 2610m/ minute speed coiling and molding.The specification of finished product long filament is 840D/140f.The finished product long filament is tested according to GB/T14344-93, the results are shown in Table 7:
Table (7)
GB/T16422.1 and GB/T16422.3 plastics laboratory light source exposure test method are adopted in the ultraviolet-resistant aging performance test of finished product long filament, and the finished product long filament is carried out ultraviolet accelerated ageing, according to GB/T14344-93 the sample after aging are tested then.Degradation adopts UV-B type fluorescent ultra-violet lamp, and the form that exposes to the open air of sample is: to sample irradiation 4 hours, condensation exposed to the open air 4 hours under 50 ± 3 ℃ of conditions of black normal temperature then, these two steps of circulation repetition under black 60 ± 3 ℃ of conditions of normal temperature.Test result after 500 hours and accelerated ageing in 1000 hours sees Table 8:
Table (8)
Adopt the condition that exposes 4 hours in 180 ℃ the air to the open air that embodiment 3 finished products are carried out the heat resistance test.After the hot oxygen accelerated ageing, the sample test method is according to GB/T14344-93, and test result sees Table 9:
Table (9)
Embodiment 4
Nylon 6 resin 100kg, relative viscosity 3.35, composite type heat stabilizing agent 0.45wt% (three (2,4 di-tert-butyl-phenyls) (3-(3 for phosphite ester 0.15wt%+ four, the 5-di-tert-butyl-hydroxy phenyl) season the eleventh of the twelve Earthly Branches tetrol ester 0.3wt% propionic acid), with 100kg nylon resin weight is radix), compound uvioresistant auxiliary agent 0.5wt%2-hydroxyl-4-oxy-octyl benzophenone 0.25wt%+N, N '-two (2,2,6,6-tetramethyl-4-piperidyl) 1,3 benzenedicarboxamide 0.25wt are radix with 100kg nylon resin weight), magnesium stearate lubricant 0.3wt% (is radix with 100kg nylon resin weight).To mix 1 hour in the load weighted said components input bipyramid spiral agitator.Add screw extruder then, the temperature of screw extruder is set to 290 ℃, 295 ℃, 295 ℃, 295 ℃, 290 ℃, 290 ℃, head pressure is set at 12Mpa, 290 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 16.28RPM, the tow of ejection is at 18 ℃, quenching is shaped in the air of relative humidity 80%, then at 195 ℃ of following two-stages drawing and settings of totally 4.9 times that pass through, after being 0.6Mpa compressed air network device by bleed pressure, the finished product long filament was with 2610m/ minute speed coiling and molding.The specification of finished product long filament is 840D/140f.The finished product long filament is tested according to GB/T14344-93, the results are shown in Table 10:
Table (10)
GB/T16422.1 and GB/T16422.3 plastics laboratory light source exposure test method are adopted in the ultraviolet-resistant aging performance test of finished product long filament, and the finished product long filament is carried out ultraviolet accelerated ageing, according to GB/T14344-93 the sample after aging are tested then.Degradation adopts UV-B type fluorescent ultra-violet lamp, and the form that exposes to the open air of sample is: to sample irradiation 4 hours, condensation exposed to the open air 4 hours under 50 ± 3 ℃ of conditions of black normal temperature then, these two steps of circulation repetition under black 60 ± 3 ℃ of conditions of normal temperature.Test result after 500 hours and accelerated ageing in 1000 hours sees Table 11:
Table (11)
Adopt the condition that exposes 4 hours in 180 ℃ the air to the open air that embodiment 4 finished products are carried out the heat resistance test.After the hot oxygen accelerated ageing, the sample test method is according to GB/T14344-93, and test result sees Table 12:
Table (12)
Claims (10)
1. the ageing-resistant high-strength nylon filament of a suitable outdoor use is characterized in that this Tynex adds the auxiliary agent melt blending of following components by weight percent by nylon resin, makes by spinning technique again:
Heat stabilizer: 0.01～0.5wt%;
Uvioresistant auxiliary agent: 0.01～0.5wt%;
Lubricant: 0.01～0.5wt%;
Above-mentioned percentage by weight is 100% with the 100kg nylon resin; Nylon resin is selected nylon 6 or nylon 66 for use, and its relative viscosity is 2.7～3.6.
2. the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1 is characterized in that: heat stabilizer is selected from a kind of in arylamine class, Hinered phenols, halogen copper salt kind, phosphorous acid lipid, the benzimidazole type thermal stabilizing agent.
3. the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1, it is characterized in that: heat stabilizer is a composite thermal stabilizer, is selected from two or more the compound in arylamine class, Hinered phenols, halogen copper salt kind, phosphorous acid lipid, the benzimidazole type thermal stabilizing agent.
4. the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1, it is characterized in that: heat stabilizer is selected from 2-mercaptobenzidazole, cuprous iodide, three (2, the 4-di-tert-butyl-phenyl) phosphite ester, 4,4-butylidene-two (6-tert-butyl group metacresol, N, N '-hexa-methylene-two [(3,5-di-t-butyl-4-hydroxy benzenes propionamide], one or both and two or more compounds in four (3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) season the eleventh of the twelve Earthly Branches tetrol ester.
5. according to the ageing-resistant high-strength nylon filament of any described a kind of suitable outdoor use of claim of claim 1～4, it is characterized in that: the uvioresistant auxiliary agent is selected from a kind of in hindered amines, benzotriazole, hindered piperidine class, the benzophenone uvioresistant auxiliary agent.
6. according to the ageing-resistant high-strength nylon filament of any described a kind of suitable outdoor use of claim of claim 1～4, it is characterized in that: the uvioresistant auxiliary agent is compound uvioresistant auxiliary agent, is selected from two or more the compound in hindered amines, benzotriazole, hindered piperidine class, the benzophenone uvioresistant auxiliary agent.
7. according to the ageing-resistant high-strength nylon filament of any described a kind of suitable outdoor use of claim of claim 1～4, it is characterized in that: the uvioresistant auxiliary agent is selected from (2-(the 2-hydroxyl-3-tert-butyl group-5-aminomethyl phenyl)-5-chlorinated benzotriazole, two (2,2,6,6-tetramethyl-4-piperidyl) sebacate, Octabenzone, poly-{ [6-[(1,1,3, the 3-tetramethyl butyl) amino]]-1,3,5-triazine-2,4-two [(2,2,6,6 ,-tetramethyl-4-piperidyl) imino group]-1, oneself two supports [(2 of 6-, 2,6,6-tetramethyl-4-piperidyl) imino group], 2-(2-hydroxyl-3,5-di-tert-butyl-phenyl) benzotriazole, succinic acid and (4-hydroxyl-2,2,6, the polymer of 6-tetramethyl-1-piperidines alcohol, Octabenzone, N, N '-two (2,2,6,6-tetramethyl-4-piperidyl) one or both in 1,3 benzenedicarboxamide and two or more compounds.
8. the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1 is characterized in that: lubricant is selected from a kind of in erucyl amide, stearic amide, the metallic soap of stearic acid.
9. the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1, it is characterized in that: described Tynex is that Denier range is the multifilament of 210～3360 DENIER.
10. the method for the ageing-resistant high-strength nylon filament of a kind of suitable outdoor use according to claim 1 is characterized in that this method comprises the steps: to mix in the load weighted said components input bipyramid spiral agitator; Add screw extruder then, the temperature of screw extruder is set to 290～298 ℃, 295～305 ℃, 295～305 ℃, 295～305 ℃, 290～295 ℃, 290～295 ℃, head pressure is set at 10～15Mpa, 290～300 ℃ of condition of spinning manifold temperature, spinning pump rotating speed 15～17RPM, the tow of ejection is at 15～20 ℃, quenching is shaped in the air of relative humidity 75%～85%, then at 190～200 ℃ of following two-stages drawing and settings of totally 4.5～5.5 times that pass through, again by behind the compressed air network device, coiling and molding.
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