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Polyhydroxy-substituted aromatic Schiff base synergistic halogen-free and flame-retardant nylon 6 composition and preparation method thereof

A flame-retardant nylon and polyhydroxyl technology, which is applied in the field of polymer material modification, can solve the problems of nylon 6 mechanical properties degradation, low flame-retardant efficiency, and tensile strength decline, and achieve the effect of blocking heat and oxygen transfer and blocking Good, good effect of cross-linked carbon layer

Active Publication Date: 2019-07-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With ammonium polyphosphate as the main component, together with melamine cyanurate, carbon nanotubes (CNTs) and other synergists, it has a certain flame retardant effect on nylon 6. Chinese invention patent CN10786446 discloses an GWIT825℃ halogen-free flame retardant nylon material and its preparation method, the patent uses 30wt.% ammonium polyphosphate as the main flame retardant, 4wt.% zinc borate and melamine cyanurate as synergistic flame retardants, Adding 0.2wt.% anti-dripping agent polytetrafluoroethylene, the total addition of flame retardants is 34.2wt.% can make nylon 6 pass the UL94V-0 flame retardant grade test, but it has low flame retardant efficiency and affects the performance of PA6 Major and other issues
Yang Dian et al. (Research on the synergistic effect of adding CNTs, APP and ABS on the improvement of the flame retardancy of nylon 6[J]. Journal of Materials Research, 2016,30(3):199-208.) Using 1wt% carbon nanotubes and 20wt. % ammonium polyphosphate flame retardant modified nylon 6, so that it passed the UL94V-0 flame retardant grade, but the mechanical properties of the obtained nylon 6 deteriorated seriously. Compared with pure nylon 6, the tensile strength decreased by 51.8%, and the notched impact strength decreased 73.6%

Method used

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  • Polyhydroxy-substituted aromatic Schiff base synergistic halogen-free and flame-retardant nylon 6 composition and preparation method thereof
  • Polyhydroxy-substituted aromatic Schiff base synergistic halogen-free and flame-retardant nylon 6 composition and preparation method thereof
  • Polyhydroxy-substituted aromatic Schiff base synergistic halogen-free and flame-retardant nylon 6 composition and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 0.16mol 4,4'-diaminodiphenyl ether and 0.32mol 2,4-dihydroxybenzaldehyde into a 1000mL three-necked flask equipped with a magnet, a thermometer, and a nitrogen inlet tube, and then add 6.40mol of methanol solvent , magnetically stirred, and reacted at 60°C for 8h; the reaction liquid was cooled and filtered, washed with ethanol, and the filter cake was dried in a vacuum oven at 70°C for 11h to obtain an orange-yellow solid product, which was 4,4'-bis(2,4 -dihydroxyphenylimino) diphenyl ether, the yield is 92%; the infrared spectrum of the product is as attached figure 1 , 3100~3600cm on the spectrum -1 There is a broad characteristic absorption peak corresponding to the phenolic hydroxyl group, 1620cm -1 Corresponding to the characteristic peak of stretching vibration of imine bond (C=N), 1505cm -1 corresponding to the stretching vibration peak of the benzene ring (Ar), 1255cm -1 corresponding to the stretching vibration peak of the phenyl ether bond (Ar-O-Ar...

Embodiment 2

[0037] (1) Add 0.16mol 4,4'-diaminodiphenyl ether and 0.40mol 2,4-dihydroxybenzaldehyde to a 1000mL three-necked flask equipped with a magnet, a thermometer, and a nitrogen inlet tube, then add 6.80mol 1, 4-dioxane solvent, magnetic stirring, react at 85°C for 6h; the reaction liquid is cooled and filtered, washed with ethanol, and the filter cake is dried in a vacuum oven at 85°C for 6h to obtain an orange-yellow solid product, which is 4,4 '-bis(2,4-dihydroxyphenylimino)diphenyl ether, the yield is 96%; the infrared spectrum, hydrogen nuclear magnetic resonance spectrum and molecular structural formula of the product are consistent with those of the product in step (1) of Example 1;

[0038] (2) 685g of nylon 6, 80g of 4,4'-bis(2,4-dihydroxyphenylimino)diphenyl ether produced in step (1), 150g of high degree of polymerization ammonium polyphosphate, 80g of POE-g- MAH compatibilizer, 3g antioxidant B225 and 2g stearic acid join in the high-speed mixer, after stirring and mixi...

Embodiment 3

[0040] (1) Add 0.16mol 4,4'-diaminodiphenyl ether and 0.48mol 2,4-dihydroxybenzaldehyde to a 1000mL three-necked flask equipped with a magnet, a thermometer, and a nitrogen inlet tube, and then add 9.60mol toluene Solvent, magnetically stirred, reacted at 95°C for 4h; the reaction liquid was cooled and filtered, washed with methanol, and the filter cake was dried in a vacuum oven at 50°C for 12h to obtain an orange-yellow solid product, which was 4,4'-bis(2, 4-dihydroxyphenylimino) diphenyl ether, the yield is 94%; the infrared spectrum, hydrogen nuclear magnetic resonance spectrum and molecular structure of the product are consistent with those of the product in step (1) of Example 1;

[0041] (2) 716g of nylon 6, 80g of 4,4'-bis(2,4-dihydroxyphenylimino)diphenyl ether produced in step (1), 120g of high degree of polymerization ammonium polyphosphate, 80g of POE-g- MAH compatibilizer, 2g antioxidant 1010 and 2g stearic acid join in the high-speed mixer, after stirring and mix...

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Abstract

The invention discloses a polyhydroxy-substituted aromatic Schiff base synergistic halogen-free and flame-retardant nylon 6 composition and a preparation method thereof. The raw material formula of the nylon 6 composition comprises, by mass, 68.5-75.8% of nylon 6, 5.0-8.0% of a polyhydroxy-substituted aromatic Schiff base, 12.0-15.0% of ammonium polyphosphate with a high polymerization degree, 3.0-8.0% of a polyolefin grafted maleic anhydride compatibilizer, 0.1-0.3% of an antioxidant and 0.1-0.2% of a lubricant. The flame-retardant nylon 6 is formed by compounding the polyhydroxy-substitutedaromatic Schiff base with the ammonium polyphosphate with the high polymerization degree; and when the total amount of the two components is 20.0 wt%, the nylon 6 can pass UL94V-0@3.2 mm flame-retardant level, is resistant to dripping, and can well keep the rigidity of pure nylon 6 and have good mechanical performances on the premise of achieving the V-0 flame-retardant level.

Description

technical field [0001] The invention relates to the halogen-free flame-retardant modification of nylon 6, in particular to a polyhydroxyl-substituted aromatic Schiff base synergistic halogen-free flame-retardant nylon 6 composition and a preparation method thereof, belonging to the technical field of polymer material modification. Background technique [0002] Nylon 6 (PA6) is an engineering plastic with unique mechanical properties, thermal properties, processing properties, etc. It is widely used in the fields of electrical and electronic, automobile and machinery industries. However, unmodified nylon 6 is flammable, and it releases a large amount of heat during the combustion process while showing serious melting and dripping, which is a great fire hazard. Therefore, the flame retardant modification of nylon 6, especially halogen-free crucial. Aluminum phosphinate has an outstanding flame retardant effect on PA6, but the price is very expensive, and the flame retardant c...

Claims

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Application Information

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IPC IPC(8): C08L77/02C08L51/06C08K3/32C08K5/29C08K5/134C08K5/526C08K5/09C08K13/02
CPCC08K2003/323C08L77/02C08L2201/02C08L51/06C08K3/32C08K5/29C08K5/1345C08K5/526C08K5/09C08K13/02
Inventor 赵建青韦兰刘述梅黄皓浩
Owner SOUTH CHINA UNIV OF TECH
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