A kind of high nitrogen content hyperbranched triazine-based char-forming agent and its preparation method and flame retardant composite material

A hyperbranched triazine and char-forming agent technology, which is applied in the field of polymer flame-retardant materials, can solve the problems of long reaction time, low nitrogen content, and poor thermal stability of char-forming agents in the synthesis of triazine-based char-forming agents, achieving Low cost, little damage to mechanical properties, enhanced flame retardant effect

Active Publication Date: 2021-10-29
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Chinese patent with application number 201310219592.1 "Preparation method of hyperbranched triazine charcoal agent" (authorized announcement number is CN103333336 B), the Chinese patent with application number 201610410728.0 "A kind of triazine macromolecule halogen-free flame retardant synthetic Charcoal compound and preparation method thereof " (authorized announcement number is CN106009037B), although the disclosed method of the above-mentioned patent has obtained some effects, but the reaction time of synthesizing triazine series charcoal agent is long, nitrogen content is low, and the charcoal agent obtained is hot poor stability

Method used

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  • A kind of high nitrogen content hyperbranched triazine-based char-forming agent and its preparation method and flame retardant composite material
  • A kind of high nitrogen content hyperbranched triazine-based char-forming agent and its preparation method and flame retardant composite material
  • A kind of high nitrogen content hyperbranched triazine-based char-forming agent and its preparation method and flame retardant composite material

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Embodiment 1

[0021] Embodiment 1: a kind of high nitrogen content hyperbranched triazine series char-forming agent, wherein: the structural general formula of described char-forming agent is as follows:

[0022]

[0023] in,

[0024] The reaction principle of the present invention is with reference to following reaction equation:

[0025]

Embodiment 2

[0026] Embodiment 2: the preparation of a kind of hyperbranched triazine char-forming agent with high nitrogen content comprises the following steps: take 36.5g cyanuric chloride and put it into a 500mL four-necked flask, add 200mL acetone thereinto, place the device in In an ice-water bath, control the temperature of the solution at -10 to 10°C. In this example, it is 0°C, and use an electric stirring paddle to stir; put 20mL of diethanolamine solution into a constant pressure funnel, and add it dropwise to the trimer at a rate of 2 drops / second. In the acetone solution of cyanogen chloride, react continuously in a fume hood for 3 hours; place the device in an oil bath, control the temperature between 40 and 60°C. This embodiment is 50°C, and install a condensation reflux device; measure 7.5mL of di Mix ethylenetriamine and 100mL of 1.0mol / L sodium carbonate aqueous solution, add the mixture dropwise to the flask, control the speed at 1 drop / second, and continue to react in th...

Embodiment 3

[0034] Example 3: The prepared triazine intumescent flame retardant char-forming agent and ammonium polyphosphate APP are compounded into an intumescent flame retardant IFR in a ratio of 1:1, such as image 3 Shown are photos before and after the IFR expansion test. The intumescent flame retardant compounded by high nitrogen content hyperbranched triazine char-forming agent and ammonium polyphosphate in a ratio of 1:1 was pressed into a disc (diameter 1.2cm, thickness 2mm, The total mass is 0.3g) put it on the aluminum foil paper, mark it, put it into a box-type resistance furnace at 400°C, and take it out after 5 minutes.

[0035] Intumescent flame retardant IFR was blended with PP to prepare flame-retardant composite materials. The material ratio of flame-retardant composite materials is shown in Table 1, and the oxygen index test results are shown in Table 2. After the IFR is ground evenly, it is melt-blended with PP to obtain a flame-retardant composite material. When th...

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Abstract

The invention provides a high nitrogen content hyperbranched triazine char-forming agent and its preparation method and flame-retardant composite material, adopting a three-stage heating method, adding cyanuric chloride and Acetone, then slowly add diethanolamine, stir for 2~4h; raise the temperature to 40~60°C, add diethylenetriamine and sodium carbonate aqueous solution dropwise, stir for 4~8h; raise the temperature to 90~110°C, add dropwise diethylenetriamine and Sodium carbonate aqueous solution, stirred for 5~9h, cooled, suction filtered, washed, dried and pulverized to obtain charcoal agent. The char forming agent of the present invention has the advantages of non-toxicity, low cost, high thermal stability, difficulty in hydrolysis, and little damage to the mechanical properties of the flame-retardant matrix, etc., and can be used for polypropylene (PP), nylon-66 (PA-66), polypropylene Flame-retardant char-forming agent for ethylene (PE) and other materials, easy to mass-produce. The structural formula of the carbon forming agent is shown in the following formula:.

Description

technical field [0001] The patent of the invention belongs to the technical field of polymer flame-retardant materials, and relates to an intumescent flame-retardant char-forming agent and its preparation method and a flame-retardant composite material, in particular to a hyperbranched triazine-based char-forming agent with high nitrogen content and its Preparation. Background technique [0002] Intumescent flame retardant (IFR) has the advantages of no halogen, low smoke, low toxicity, and no corrosive gas generation. It has three basic elements, namely acid source, gas source and carbon source. Carbon sources are also called charring agents, which are the basis for forming the foam carbonization layer. Some polyols with high carbon content are often used as charring agents for mixing IFR, such as pentaerythritol, starch, phenolic resin, etc., but these charring agents are also There are defects such as insufficient thermal stability and easy migration. [0003] Therefore...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/12C08K5/3492C08K3/32
CPCC08K3/32C08K5/3492C08K2003/323C08L23/12
Inventor 于守武石鹏翔肖淑娟赵泽文霍晓文王悦
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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