資源描述:
《氮磷反應(yīng)型阻燃劑的合成及其阻燃聚氨酯的性能.pdf》由會(huì)員上傳分享,免費(fèi)在線閱讀,更多相關(guān)內(nèi)容在行業(yè)資料-天天文庫(kù)。
1、88第42卷,第6期工程塑料應(yīng)用Vb1.42.No.62014年6月ENGrNEERINGPLASTICSAPPLICATIONJun.2O14doi:lO.3969/j.issn.1001-3539.2014.06.020氮磷反應(yīng)型阻燃劑的合成及其阻燃聚氨酯的性能鄧前軍,張五一,陳東初,袁毅樺,丁森林(1.佛山科學(xué)技術(shù)學(xué)院理學(xué)院,廣東佛山528000;2.華南理工大學(xué)材料科學(xué)與工程學(xué)院,廣州510006)摘要:以多聚甲醛、二異丙醇胺和亞磷酸二乙酯為原料,通過(guò)兩步反應(yīng)合成了反應(yīng)型阻燃劑N,N-二f2一羥異丙基)氨甲基膦
2、酸二乙酯(HPAPE),采用單因素法得到了合成中間體5.甲基一3一(2.羥異丙基)一1,3一惡唑的最佳條件:反應(yīng)時(shí)間為4h,反應(yīng)溫度為60qC,多聚甲醛與二異丙醇胺的摩爾比為1.2:1.0,蒸餾壓力為18kPa:利用正交試驗(yàn)得到了合成阻燃劑HPAPE的最佳條件:溫度為50cIC,時(shí)間為5.0h,反應(yīng)物料MHPZ與亞磷酸二乙酯的摩爾比為1.0:1.1,催化劑強(qiáng)酸性陽(yáng)離子交換樹(shù)脂用量為反應(yīng)物料總質(zhì)量的0.3%。利用極限氧指數(shù)fLOI)、垂直燃燒法測(cè)試了HPAPE阻燃聚氨酯(PUR)的性能,采用熱重分析研究了HPAPE阻燃P
3、UR的熱分解過(guò)程及成炭性能,并用ProteusAnalysis軟件計(jì)算了其動(dòng)力學(xué)參數(shù)熱分解活化能。結(jié)果發(fā)現(xiàn),HPAPE質(zhì)量分?jǐn)?shù)為24%時(shí),HPAPE阻燃PUR的LOI為26.2%,阻燃級(jí)別可達(dá)UL94V一0級(jí),說(shuō)明阻燃劑HPAPE對(duì)PUR具有明顯的阻燃效果。在700qC時(shí),HPAPE阻燃PUR的質(zhì)量保持率比PUR高4.91%,動(dòng)力學(xué)參數(shù)熱分解活化能比PUR提高了32.40kJ/(mo1.K1,表明阻燃劑HPAPE對(duì)PuR的熱降解具有加速成炭的功效。關(guān)鍵詞:反應(yīng)型阻燃劑;N,N-二(2.羥異丙基)氨甲基膦酸二乙酯;聚氨酯
4、;熱降解中圖分類(lèi)號(hào):TQ328.3文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):1001.3539(2014)06.0088.05SynthesisofReactiveFlameRetardantContainingNitrogenandPhosphorusandItsFlameRetardancytoPolyurethaneDengQianjun,ZhangWuyi,ChenDongchu,YuanYihua,DingSenlin(1.ScienceSchool,F(xiàn)oshanUniversity,F(xiàn)oshan528000,China;2.
5、SchoolofMaterialsScienceandEngineering,SouthChinaUniversityofTechnology,Guangzhou510006,China)Abstract:AreactiveflameretardantN,N-bis(2一hydroxyisopropy1)一aminomethylphosphonicaciddiethylester(HPAPE)wassynthesizedviaparaformaldehyde,diisopropanolamine,diethylphos
6、phitebytwostepreaction.Thebestreactionconditionsof5-methy一3一(2一hydroxyisopropy1)一1,3-oxazole(MHPZ)wereobtainedbythesinglefactorexperiment:thereactiontimeis4h,thereactiontemperatureis60℃,themoleratioofparaformaldehydeanddiisopropanolamineis1.2:1.0.thedistillation
7、pressureis18kPa.ThebestreactionconditionsofHPAPEwerefoundbytheorthogonalexperiment:thetemperatureis50℃.thetimeis5.0h,themoleratioofMHPZanddimethylphosphiteis1.0:1.1,themassfractionofcatalyststrongacidcationexchangeresininthereactantis0.3%.Theflameretardancyandth
8、etherma1degradationbehaviorofHPAPEflameretardantpolyurethane(PUR)werestudiedbythelimitingoxygenindex(LOI),UL94verticalflametestandthethermogravimetricanalysis.Theresu