引用本文:
刘畅, 褚劲松, 邵传强, 杨兴钰. 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[J]. 应用化学,
2007, 24(7): 818-822.
Citation: LIU Chang, ZHU Jing-Song, SHAO Chuan-Qiang, YANG Xing-Yu. Synthesis and Flame Retardance of 2,4,8,10-Tetraoxa-3,9-Diphosphaspiro[5,5]-Undecane-3,9-Dioxa-3,9-Disubstitution Benzoylhydrazone Derivatives[J]. Chinese Journal of Applied Chemistry, 2007, 24(7): 818-822.
Citation: LIU Chang, ZHU Jing-Song, SHAO Chuan-Qiang, YANG Xing-Yu. Synthesis and Flame Retardance of 2,4,8,10-Tetraoxa-3,9-Diphosphaspiro[5,5]-Undecane-3,9-Dioxa-3,9-Disubstitution Benzoylhydrazone Derivatives[J]. Chinese Journal of Applied Chemistry, 2007, 24(7): 818-822.
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
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,LOI达到28.7%左右,有较好的阻燃性能。
English
Synthesis and Flame Retardance of 2,4,8,10-Tetraoxa-3,9-Diphosphaspiro[5,5]-Undecane-3,9-Dioxa-3,9-Disubstitution Benzoylhydrazone Derivatives
Abstract:
Spirocyclic pentaerythritol di (phosphate monochloride)(SPDPC) containing acid source and carbon source was prepared from phosphorus oxychloride and pentaerythritol.A new series of 2,4,8,10-tetraoxa-3,9-diphosphorus spirocyclic[5,5]undecane-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 E-44.These synthesized compounds have a good flame retardance.
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Key words:
- pentaerythritol
- / benzaldehyde
- / substitution benzoylhydrazone
- / synthesize
- / flame retardance
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