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Halogen-free flame-retardant high-temperature nylon

A high-temperature, nylon technology, applied in the field of halogen-free flame-retardant semi-aromatic high-temperature nylon, can solve the problems of insufficient chemical resistance, reduced processing fluidity of high-temperature nylon, strong plasticity, etc.

Active Publication Date: 2014-10-29
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The DOPO derivative has good flame retardant effect, good thermal stability and chemical stability, and can overcome the lack of chemical resistance or strong plasticity of existing DiDOPO flame retardants without reducing the processing fluidity of high-temperature nylon. shortcoming

Method used

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  • Halogen-free flame-retardant high-temperature nylon
  • Halogen-free flame-retardant high-temperature nylon
  • Halogen-free flame-retardant high-temperature nylon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Embodiment 1 has the preparation of formula (2) structural compound A

[0086] DOPO (86.40 g, 0.40 mol), acetophenone (24.05 g, 0.20 mol) and 10 ml of xylene were added to a three-necked flask equipped with a thermometer, a water separator, a magnetic stir bar and a constant pressure funnel. Under nitrogen protection, the mixture was heated to 154°C, and phosphorus oxychloride was added dropwise. POCl 3 (30.25g) was slowly added dropwise to the reaction solution within 25 hours, and the distillate was collected in the water trap, keeping the reaction temperature at 154-160°C. After dropping phosphorus oxychloride, keep warm for half an hour. After cooling, add 120g of isopropanol, stir under reflux, most of the crude product dissolves after softening, and the system becomes turbid. Stirring was stopped, cooled, and a large amount of product precipitated after standing for a period of time. Suction filtration, the solid product was first washed with a small amount of...

Embodiment 2

[0088] Embodiment 2 has the preparation of formula (3) structure compound

[0089] Add DOPO (86.40 g, 0.40 mol) and naphthalene ethyl ketone (34.04 g, 0.20 mol) into a three-necked flask equipped with a thermometer, a magnetic stir bar and a constant pressure funnel. Under nitrogen protection, the mixture was heated to 170°C, and phosphorus oxychloride was added dropwise. POCl 3 (15.96g) was slowly added dropwise in the reaction solution within 20 hours, keeping the reaction temperature at 170-180 degrees. After dropping phosphorus oxychloride, keep warm for half an hour. 31 P NMR spectrum showed no starting material. Cool, add 50ml of 90% ethanol to dissolve, then drop about 60ml of 2.5% Na 2 CO 3 Solution The pH of the reaction solution was adjusted to 6-7, and the white solid product was obtained by suction filtration after reflux for half an hour. Yield 70.6%.

[0090] The resulting product is characterized by H spectrum and P spectrum on a magnetic resonance instru...

Embodiment 3

[0093] Compound A, PPA, and antioxidant 1010 obtained in Example 1 were mixed in an internal mixer with a rotation speed of 50 rpm according to a weight ratio of 9:51:0.12, and the temperature was set at 300 ° C. After 5 minutes, they were taken out and cooled. dry. Then fill it into a mold, preheat it in a flat vulcanizing machine at 280°C for 10 minutes, hold the pressure at 10MPa for 4 minutes, and then cold press it. Cut samples and test after cooling down. The flame retardancy level of 0.8mm sample is UL94V-0.

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Abstract

The invention relates to a halogen-free flame-retardant high-temperature nylon, which is characterized by comprising polyamide and DOPO derivatives. The halogen-free flame-retardant high-temperature nylon reaches the UL94V-0 grade in 0.8 mm burning tests, has excellent thermal stability, chemical stability, and mechanical performance, can be used as the main material to prepare surface mount devices (SMD), and meets the operating requirements of a high-temperature infrared reflow oven welding technology during the process of a surface mount technology (SMT).

Description

technical field [0001] The invention relates to a halogen-free flame-retardant semi-aromatic high-temperature nylon. Background technique [0002] The miniaturization and multi-functionalization of electronic appliances has prompted the manufacturing industry to accelerate the adoption of surface mount technology (SMT) to achieve high density of electronic components. Since the SMT process requires the use of high-temperature infrared reflow furnaces to solder surface mount components (SMD), SMD materials are required to have outstanding thermal stability, chemical stability and mechanical properties, and semi-aromatic high-temperature nylon is therefore extremely popular in SMD. big application. However, due to the flammability of general semi-aromatic high-temperature nylon, it is necessary to add flame retardants in actual use to meet fire safety requirements. Traditionally, brominated flame retardants are usually used in semi-aromatic high-temperature nylon to achieve ...

Claims

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Application Information

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IPC IPC(8): C08L77/00C08K5/5313C08K7/14
CPCC08K5/5313C08K7/14C08L77/06C08L2201/02C08L2201/08C08L2201/22C08L2205/025C08L2205/03C08L27/18
Inventor 姚强周浩曹微虹张伟伟刘正西徐子平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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