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Preparation method of novel hyperbranched triazine char forming agent

A technology of hyperbranched triazine and carbon-forming agent, applied in the field of polymer materials, can solve the problems of difficulty in solvent distillation and recovery, discontinuous reaction process, poor thermal stability of products, etc., and achieve shortened reaction time, continuous reaction process, and thermal stability. good effect

Active Publication Date: 2013-10-02
合肥安聚达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a continuous reaction process in view of the shortcomings of the prior art that the reaction process is discontinuous, the reaction time is long, the amount of organic solvent is large, the solvent distillation recovery is difficult, the thermal stability of the product is poor, and the amount of carbon is low. , the reaction time is shorter, the synthesis process is simplified, no or a small amount of ethanol solvent is used to replace some environmentally unfriendly organic solvents as the reaction system, the triazine hyperbranched macromolecular char-forming agent with good thermal stability and high char-forming rate Preparation

Method used

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  • Preparation method of novel hyperbranched triazine char forming agent
  • Preparation method of novel hyperbranched triazine char forming agent
  • Preparation method of novel hyperbranched triazine char forming agent

Examples

Experimental program
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Effect test

Embodiment 1

[0032]Dissolve 0.52mol of piperazine in 150mL of water and add to a 500mL three-necked flask equipped with a reflux condenser, constant pressure dropping funnel, and stirrer, then dissolve 0.25mol of cyanuric chloride in 80mL of ethanol and water (vol. ratio of 4:1) into the mixed solvent, dropwise added to the system, and reacted at 0°C for 4 hours, then raised the temperature to 50°C, dissolved 0.78mol of NaOH in 80mL of water, and slowly added dropwise to the system, And react at this temperature for 6 hours, finally heat up to 95°C, react for 9 hours, stop stirring, suction filter while hot, wash with water 3 times, and vacuum dry at 80°C for 8 hours to obtain 60.13g of triazine hyperbranched charcoal agent , the productive rate is 97.4%, and the chlorine element content is 1.17%. Under a nitrogen atmosphere, the weight loss at 468°C is 1%, and the carbon content at 600°C is 42%.

[0033] figure 1 It is the infrared spectrogram of the product in Example 1. As can be seen...

Embodiment 2

[0036] Dissolve 0.5mol of ethylenediamine in 50mL of water into a 500mL three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel, and a stirrer, then dissolve 0.25mol of cyanuric chloride in 25mL of ethanol, and gradually Add dropwise to the system, and react at 10°C for 1 hour, then raise the temperature to 70°C, add 0.4mol of Na 2 CO 3 Dissolve in 40mL of water, slowly drop into the system, and react at this temperature for 3 hours, finally raise the temperature to 150°C, react for 6 hours, stop stirring, suction filter while hot, wash with water 3 times, and dry at 100°C for 2 hours , 46.5 g of triazine hyperbranched charcoal agent was obtained, the yield was 95.9%, and the content of chlorine element was 0.95%. The elemental analysis results of the product in Example 2 show that in the triazine hyperbranched charcoal agent, the theoretical percentages of C, N, and H are respectively 43.30%, 50.52%, and 6.19%, while the measured values ​​are...

Embodiment 3

[0038] Dissolve 0.15mol of N-aminoethylpiperazine in a mixture of 300mL of water and ethanol (4:1 by volume) and add it to a 1000mL three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel, and a stirrer. Then, dissolve 0.05mol of cyanuric chloride in 100mL of water, add dropwise to the system, and react at 5°C for 3 hours, then raise the temperature to 30°C, dissolve 0.18mol of KOH in 180mL of water, slowly add dropwise into the system, and react at this temperature for 8 hours, and finally raise the temperature to 90°C, react for 10 hours, stop stirring, suction filter while hot, wash with water 3 times, and vacuum dry at 50°C for 10 hours to obtain a triazine-based hyperbranched charcoal Agent is 15.56g, and productive rate is 93.45%, and chlorine element content is 1.56%. The elemental analysis results of the product in Example 3 show that the theoretical percentages of C, N, and H in the triazine hyperbranched charcoal agent are respectivel...

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Abstract

The invention discloses a preparation method of a novel hyperbranched triazine char forming agent, which comprises the following steps: adding a dissolved diamine solution at 0-10 DEG C, gradually and dropwisely adding a dispersed cyanuric chloride solution, and reacting for 1-4 hours; heating to 30-70 DEG C, adding an acid-binding agent, and reacting for 3-8 hours; heating to 90-150 DEG C, and reacting for 6-10 hours; and stopping stirring, carrying out vacuum filtration, washing with water, and drying to obtain the triazine hyperbranched char forming agent. Compared with the prior art, the invention has the advantages of continuous reaction process, short reaction time, cheap raw materials, low solvent consumption, no addition of any blocking agent in the reaction process, simplified synthesis technique, high heat stability and high char forming ratio.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a preparation method of an intumescent flame-retardant char-forming agent, in particular to a preparation method of a novel hyperbranched triazine char-forming agent. Background technique [0002] Intumescent flame retardants are one of the types of green flame retardants widely used in recent years. It also overcomes the disadvantage of causing suffocation of personnel, and also overcomes the adverse effects of inorganic flame retardants on material mechanics and processing properties due to large additions. Intumescent flame retardant (IFR) meets the requirements of today's protection of the ecological environment due to its unique flame retardant mechanism, halogen-free, low smoke, low toxicity, and the generated carbon layer can effectively prevent polymer droplets. Generally speaking, IFR includes 3 parts, namely carbon source (usually polyol, such as pentaerythrito...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 温攀月时虎
Owner 合肥安聚达新材料科技有限公司
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