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【答案】应助回帖
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朱岩0308: 金币+35, 翻译EPI+1, ★★★★★最佳答案 2015-05-29 16:58:42
Synthesis of Asymmetric Cyclotriphosphazene-Benzoxazine Monomer
Abstract
六氯环三磷腈化合物是一类耐热阻燃性能优良的杂环化合物，每个磷上面连接两个氯原子，其含磷量相对较高，这也使得它相应的衍生物具有优异的阻燃性和热稳定性。而苯并噁嗪树脂是在传统的树脂基础上发展起来的一种新型类酚醛树脂。它不但继承了传统树脂的耐热、阻燃等优点，自身还具有传统酚醛树脂所不具有的性能，如：体积零收缩、固化不需催化剂、便于加工成型及灵活的分子结构设计等，具有良好应用前景。本文通过向磷腈环上引入部分噁嗪结构，意欲提高原有六氯环三磷腈的阻燃和耐热性。Hexachloro cyclotriphosphazene (HCC) are heterocyclic compounds with excellent heat-resistant and flame-retardant properties. In HCC each phosphorus is connected with two chlorine; its phosphorus content is relatively high, which provides its derivatives with excellent flame retardant properties and thermal stability. Benzoxazine resin is a new phenol formaldehyde resin (phenolic resin) evolved from the traditional resin. It not only has the heat-resistant, fire-retardant and other features, it also has its unique properties that traditional phenolic resins do not have, such as: no shrinkage, can be cured without a catalyst, ease to be processed to desired shapes and the flexibility in the design of molecular structures. It therefore has an excellent prospects in applications. In this paper, we introduced a portion of benzoxazine structure to the phosphazene ring in order to improve the flame retardant and heat resistance properties of the original HCC. 本实验先以六氯环三磷腈和2,2’-联苯酚为原料合成T1，后用对氨基苯酚和水杨醛合成含有C=N结构的中间体，随后利用NaBH4将C=N双键还原，然后在1,4-二氧六环溶液中加入多聚甲醛回流，使其生成含有酚羟基的苯并噁嗪单体C3。最后在1,4-二氧六环体系中将T1与C3发生亲核取代反应。分别利用通过FI-IR、1H NMR和31P NMR对所合成化合物结构进行了表征。
Staring from HCC and 2,2'-Biphenol as the raw materials, we first synthesized the intermediate T1, then, from p-aminophenol and salicylaldehyde, we initially synthesized a C=N containing Schiff’s base intermediate, followed reduction using NaBH4 to reduced the C=N double bond, then treated with containing in 1,4-dioxane under reflux to generate phenolic hydroxyl-containing benzoxazine monomer C3. Finally, the substitution reaction of T1 and C3 were reacted in1,4-dioxane . The structures of the synthesized compounds were characterized by FI-IR, NMR 1H and NMR 31P, respectively..
Keywords: hexachloro cyclotriphosphazene, benzoxazine, synthesis, heat resistant, flame retardant |
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