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
  • Description
  • 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,

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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