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2,4,8,10-四氧杂-3,9-二磷杂螺环[5.5]十一烷-3,9-二氧-3,9-二取代苯甲醛腙的合成及其阻燃性能 被引量:6

Synthesis and Flame Retardance of 2,4,8,10-Tetraoxa-3,9-Diphosphaspiro[5,5]-Undecane-3,9-Dioxa-3,9-Disubstitution Benzoylhydrazone Derivatives
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摘要 以季戊四醇、三氯氧磷为原料合成了富含酸源(磷)、碳源的氯化螺环磷酸酯(SPDPC),再将其与水合肼、取代苯甲醛反应,合成了系列化合物2,4,8,10-四氧杂-3,9-二磷杂螺环[5.5]十一烷-3,9-二氧-3,9-二取代苯甲醛腙,利用元素分析、FTIR、1H NMR和MS测试技术对其结构进行了表征。目标化合物分子结构对称性高、分子量较大、含较多芳构型碳和磷杂环碳,热重(TG)和差热(DSC)分析结果表明,具有较高的热稳定性。将这些化合物添加于环氧树脂(E-44)中进行水平燃烧实验,当添加质量分数为10%时,样条燃烧长度在10-20 mm之间,均具有很好的自熄效果;同时,LO I达到28.7%左右,有较好的阻燃性能。 Spirocyclic pentaerythritol di (phosphate monochloride ) (SPDPC) containing acid source and carbon source was prepared from phosphorus oxyehloride and pentaerythritol. A new series of 2,4,8,10-tetraoxa-3,9-diphosphorus spiroeyelie [ 5.5 ] undeeane-3,9-dioxa-3,9-disubstituted benzoylhydrazone derivatives was synthesized from SPDPC, hydrazine hydrate (85%) and substitution benzaldehyde. Their structures were confirmed by elemental analysis, FTIR, ^1H NMR and MS. TG and DSC results show that the target compounds have certain thermal stability due to their higher symmetry structure, heavier molecular mass, more arylgeometry carbon and phosphorus heterocycle carbon. All the compounds are self-extinguish, when the addition amount of the compound was 10% in epoxy resin (E-44) , the combustion length was about 10 20 mm in the level combustion test. The LOI was improved to 28.7% when 10% the target compound was added to epoxy E44. These synthesized compounds have a good flame retardanee.
出处 《应用化学》 CAS CSCD 北大核心 2007年第7期818-822,共5页 Chinese Journal of Applied Chemistry
基金 武汉市重点攻关科技项目(20021002052)资助
关键词 季戊四醇 苯甲醛 取代苯甲醛腙 合成 阻燃性 pentaerythritol, benzaldehyde, substitutionbenzoylhydrazone, synthesize, flame retardance
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