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Preparation method for triazine hyperbranched macromolecular carbon forming agent

A technology based on macromolecules and triazines, which is applied in the field of preparation of triazine hyperbranched macromolecular char-forming agents to achieve the effects of short reaction time, broad application prospects and continuous reaction process

Inactive Publication Date: 2010-11-10
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there have been no public reports on the research on new char-forming agents with hyperbranched structures.

Method used

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  • Preparation method for triazine hyperbranched macromolecular carbon forming agent
  • Preparation method for triazine hyperbranched macromolecular carbon forming agent
  • Preparation method for triazine hyperbranched macromolecular carbon forming agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Dissolve 0.03 mol of 4,4-diaminodiphenyl ether and 0.1 mol of triethylamine in 25 ml of N,N-dimethylformamide (DMF), and stir at 0.5°C for 0.5 Hour. Dissolve 0.02 mol of cyanuric chloride in 50 ml of DMF, add dropwise to the system at this temperature, and continue to react at this temperature for 3 hours, raise the temperature to 90°C, react for 6 hours, and then add 0.1 mol of aniline, heated up to 100°C, reacted for another 2 hours, stopped stirring, precipitated in 1000 ml of water, washed twice with 50 ml of ether and 100 ml of acetone, filtered, and dried in vacuum at 70°C for 20 hours to obtain Hyperbranched polyamide triazine char forming agent, in nitrogen atmosphere, the weight loss is 3% at 300°C, and the carbon content is 72% at 600°C. figure 1 It is the H NMR spectrum of the product in Example 1. Three different types of tertiary amine hydrogen atoms can be observed in the figure, and their chemical shifts are respectively δ=10.15ppm, δ=9.15ppm,...

Embodiment 2

[0030]Embodiment 2: 0.04mol of 4,4-diaminodiphenylmethane and 0.3mol of N,N-diisopropylethylamine are dissolved in 40 milliliters of N,N-dimethylacetamide (DMAC), nitrogen The mixture was stirred at 5° C. for 0.5 hour in the atmosphere. Dissolve 0.06 mol of cyanuric chloride in 50 ml of DMF, add dropwise to the system at this temperature, and continue to react at this temperature for 4 hours, raise the temperature to 110°C, react for 7 hours, and then add 0.35 mol of 1-naphthylamine, heated to 120°C, reacted for another 2 hours, stopped stirring, precipitated in 800 ml of methanol, washed 3 times with 100 ml of water and 100 ml of acetone, filtered, and dried in vacuum at 100°C for 5 After 1 hour, a hyperbranched polyamide triazine char-forming agent was prepared. In a nitrogen atmosphere, the weight loss at 300° C. was 4%, and the carbon content at 600° C. was 67%.

Embodiment 3

[0031] Example 3: 0.07 mol of hexamethylenediamine and 0.5 mol of triethylamine were dissolved in 60 ml of tetrahydrofuran (THF), and stirred at 15° C. for 0.5 hour in a nitrogen atmosphere. Dissolve 0.07 mol of cyanuric chloride in 80 ml of THF, add dropwise to the system at this temperature, and continue to react at this temperature for 3 hours, raise the temperature to 85°C, react for 7 hours, and then add 0.3 mol of 1-naphthylamine, heated to 95°C, reacted for another 3 hours, stopped stirring, precipitated in 1500 ml of water, washed twice with 200 ml of methanol and 100 ml of toluene, filtered, and dried in vacuum at 50°C for 60 hours , to prepare a hyperbranched polyamide triazine char-forming agent, in a nitrogen atmosphere, the weight loss at 300°C is 6%, and the carbon content at 600°C is 65%.

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Abstract

The invention discloses a preparation method for a triazine hyperbranched macromolecular carbon forming agent. The method is characterized by comprising the following steps: 1), mixing diamino or hydroxyl compound with non-protonic organic solvent, and adding catalyst in the atmosphere of inert gases; 2), dropwise adding cyanuric chloride non-protonic organic solution, and continuing the reaction at the temperature after finishing dropwise adding the cyanuric chloride non-protonic organic solution; 3), adding blocking agent, and carrying out reaction again; and 4), precipitating, filtering, cleaning the organic solvent, separating, and drying to obtain the triazine hyperbranched macromolecular carbon forming agent. Compared with the prior art, the invention has the advantages that the 'one-pot' method is adopted, the reaction process is continuous, the reaction time is short, the product has favorable heat stability, the carbon forming rate is high, and the processability is good.

Description

technical field [0001] The invention relates to a preparation method of a char-forming agent, in particular to a preparation method of a triazine hyperbranched macromolecular char-forming agent. Background technique [0002] Intumescent flame retardant is one of the types of flame retardants widely used in recent years. It overcomes the fact that halogenated flame retardants are easy to emit irritating and corrosive gases and smoke when burning, pollute the environment, and endanger human health. Corrosion of equipment and other shortcomings, is a very promising green and environmentally friendly flame retardant. Intumescent flame retardants generally consist of three basic components: acid source, carbon source, and gas source. When burning, the "three sources" can be effectively matched to form a non-combustible carbon foam layer with a fluffy and closed structure, which weakens the heat conduction between the polymer and the heat source, and prevents the diffusion of oxy...

Claims

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Application Information

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IPC IPC(8): C08G83/00
Inventor 柯晨皓李娟方科益陶慷顾群范欣愉王玉忠
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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