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High-heat-stability charring agent and preparation method thereof

A high thermal stability, carbon-forming agent technology, applied in the field of char-forming agents, can solve the problems of harsh reaction conditions, complicated purification process, and low thermal stability of products, and achieve low cost, high yield, and simple and easy preparation method Effect

Active Publication Date: 2014-11-05
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, most of the synthesis of hyperbranched triazine derivatives reported in journals is carried out in nitrogen atmosphere, the reaction conditions are harsh, and the purification process is complicated, and the thermal stability of the obtained products is not high.

Method used

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  • High-heat-stability charring agent and preparation method thereof
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  • High-heat-stability charring agent and preparation method thereof

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preparation example Construction

[0048]The present invention also provides a preparation method of a high thermal stability char-forming agent, comprising the following steps:

[0049] (a), mix the cyanuric chloride, the acid-binding agent and the organic solvent accounting for 60-75% of the total volume together, drop the mixed solution formed by ethylenediamine and the remaining organic solvent, and keep the temperature of the reaction system at the same time 0-20℃;

[0050] (b) After adding the ethylenediamine dropwise, add the nitrogen-containing compound and react for 2-4 hours, raise the temperature of the reaction system to 40-70°C for 3-8 hours;

[0051] (c), then raising the temperature of the reaction system to 80-100° C. for 3-8 hours to obtain a reaction mixture;

[0052] (d) Suction-filtering the reaction mixture to obtain a solid, washing the solid with water until it is neutral, and then drying it.

[0053] The preparation method of the high thermal stability char forming agent provided by th...

Embodiment 1

[0062] Add 55.92g of cyanuric chloride, 104.93g of anhydrous sodium carbonate and 450ml of dioxane in the three-necked flask, and after stirring evenly, add dropwise 150ml of dioxane solution of 22.72g of ethylenediamine in the reaction system at 0°C, After dripping, add 5.67g urea to react for 3h; raise the temperature of the reaction system to 50°C for 3h, then raise the temperature to 100°C for 3h; filter the reaction mixture, and wash the solid mixture in 100°C water until neutral. Then dry the product washed to neutral in an oven at 100°C to obtain the final product, the reaction formula is as follows figure 2 As shown, the yield is 99.9%, and the temperature at which the product decomposes 1% is 302°C. From figure 2 The structural formula and figure 1 It can be seen from the comparison of the structural formula (char-forming agent of the prior art) that the char-forming agent prepared by the present invention has significantly increased branch points and molecular ch...

Embodiment 2

[0064] Add 55.92g of cyanuric chloride, 119.11g of anhydrous sodium sulfite, and 364ml of acetonitrile into the three-necked flask, and after stirring evenly, add 24.14g of ethylenediamine in 242ml of acetonitrile solution dropwise to the reaction system at 7°C. After the dropwise addition, add 4.26g Urea was reacted for 2 hours; after the temperature of the reaction system was raised to 60°C for 4 hours, the temperature was raised to 80°C for 8 hours; The final product was dried in an oven at 120°C to obtain the final product with a yield of 99.8%, and the temperature at which the product decomposed 1% was 295°C. The structural formula of the char-forming agent prepared in this embodiment is consistent with the structural formula of the product in Example 1.

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Abstract

The invention relates to the field of charring agents, and particularly relates to a high-heat-stability charring agent and a preparation method thereof. The high-heat-stability charring agent is prepared from the following raw materials: cyanuric chloride, an acid-binding agent, a nitrogen-containing compound, ethylenediamine and an organic solvent, wherein the nitrogen-containing compound is one of urea, aqua ammonia and ammonium carbonate; the molar ratio of the cyanuric chloride to the acid-binding agent is 1: (3.0-3.5), the molar ratio of the cyanuric chloride to the ethylenediamine is 1: (1-2), the molar ratio of the nitrogen-containing compound to the ethylenediamine is 1: (4-19), and the molar volume ratio of the cyanuric chloride to the organic solvent is 0.4-0.6 mol / L. The high stability of the high-heat-stability charring agent provided by the invention is significantly increased, molecular chains of an obtained charring agent are uneasily entangled, and the charring agent is high in productivity. The preparation method is simple and practicable, low in cost, high in yield, and less in produced wastes, and the obtained high-heat-stability charring agent has extremely good high heat stability, thereby facilitating the wide application of the high-heat-stability charring agent.

Description

technical field [0001] The invention relates to the field of char-forming agents, in particular to a high-thermal-stable char-forming agent and a preparation method thereof. Background technique [0002] In recent years, triazine and its derivatives have attracted much attention as new char-forming agents in intumescent flame retardants. They contain stable triazine rings and are rich in nitrogen atoms, are halogen-free, low-toxic, and have high thermal stability. Excellent flame retardant properties, little impact on the mechanical properties of materials, etc., are currently a hot spot in the research of charring agents, including linear triazine derivative charring agents, dendritic triazine derivative charring agents and hyperbranched triazine derivative charring agents. Charcoal. [0003] Hyperbranched polymer is a special polymer with highly branched structure formed by the polymerization reaction of multifunctional monomers newly developed in the past 20 years. Comp...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 钱立军许梦兰
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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