Synthesis and thermal stability of a novel phosphorus-nitrogen containing intumescent flame retardant

A novel phosphorus-nitrogen containing intumescent flame retardant （P-N IFR） was prepared via the reaction of dichlor-opentate with N-methylaniline. The structure of the product was confirmed by ^1H NMR, ^31p NMR, MS and IR. TGA analysis showed it has effective thermal stability.

Intumescent Flame-retardant Modification of Polypropylene/Carbon Fiber Composites

To improve the flame resistance of polypropylene(PP)/carbon fiber(CF)composite materials,triazine char-forming agent(TCA)was compounded with ammonium polyphosphate(APP)or modified APP(CS-APP)in a 2:1 ratio to prepare intumescent flame retardant(IFR)and the modified intumescent flame retardant(CS-IFR)in this paper.Flame retardancy and thermal degradation behaviors of the composites modified by IFR and CS-IFR were characterized by Fourier Transform Infrared(FTIR),contact angle measurement,oxygen index(OI),vertical burning tests(UL-94),thermogravimetric analyer(TGA),and thermogravimetric analyzer coupled with Fourier transform infrared(TG-FTIR).It was found that 25.0 phr of IFR and 24.0 phr of CS-IFR could improve the LOI value of PP/CF composites to 28.3%and 28.9%,respectively.At the same time,a UL-94 V-0 rating was achieved.The experimental results show that the IFR and CS-IFR prepared could effectively improve the flame retardancy and thermostability of PP/CF composites,and they would greatly expand the application range of PP/CF composite materials.

Synthesis and Application of Novel Triazine-Based Charring-Foaming Agents in Intumescent Flame Retardant Polypropylene

Three novel triazine-based charring-foaming agents (M2-CFA, M4-CFA, and M6-CFA) were synthesized successfully with only water as the solvent and were characterized by FT-IR and thermal gravimetric analysis (TGA). These three charring-foaming agents and the byproduct 944-by were employed to study the effectiveness of the novel intumescent flame retardant dopant on the fire retardancy of polypropylene(PP) investigated through UL-94 and limiting oxygen index (LOI) tests. TGA results showed that the M4-CFA presented good char formation ability (char residue: 26.8% at 700 °C). It was found that the sample with a 2/1 mass ratio of APP to M4-CFA exhibited the best flame retardancy among all the PP composites: 35.5% LOI and a V-0 rating of UL-94. Additionally, the microstructure and morphology of char residues were further studied by XRD, Raman spectroscopy and SEM. © 2017, Tianjin University and Springer-Verlag Berlin Heidelberg.

Regulating the Localization of Intumescent Flame Retardant for Improving the Flame Retardancy of Ethylene-vinyl Acetate Copolymer Using Polyamide 6 as a Charring Agent

Polyamide 6 (PA6) was employed as a charring agent of intumescent flame retardant (IFR) to improve the flame retardancy of ethylene-vinyl acetate copolymer (EVA). Different processing procedures were used to regulate the localization of IFR in the EVA matrix. Localizations in which IFR was dispersed in the PA6phase or in the EVA phase were prepared. The effect of the localization of IFR on the flame retardancy of EVA was investigated. The limited oxygen index (LOI), vertical burning (UL 94) and cone calorimeter test (CCT)showed that the localization of IFR in the EVA matrix exhibited a remarkable influence on the flame retardancy.Compared with EVA/IFR, a weak improvement in the flame retardancy was observed in the EVA/PA6/IFR blend withthe localization of IFR in the PA6 phase. When IFR was regulated from the PA6 phase to the EVA matrix,a remarkable increase in the flame retardancy was exhibited. The LOI was increased from 27.8%to 32.7%, and the UL 94 vertical rating was increased from V-2 to V-0. Moreover, an approximately 41.36%decrease in the peak heat release rate was exhibited. A continuous and compact intumescent charring layer that formed in the blends with the localization of IFR in the EVA matrix should be responsible for its excellent flame retardancy.

A NEW SYNERGIST FOR INTUMESCENT FLAME RETARDANT POLYPROPYLENE

The synergistic effects of silicotungstic acid (SiW12) as a catalyst in the phosphorus-nitrogen compounds AM-based intumescent flame-retardant (IFR) polypropylene (PP) were studied using the limiting oxygen index (LOI), the UL-94 test, thermogravimetric analysis (TGA), real time Fourier transform infrared (FTIR), laser Raman spectroscopy (LRS). The LOI data show that SiW12 added to PP/IFR systems has a synergistic FR effect with an IFR additive named AM. The TGA data show that SiW12 apparently increases the thermal stability of the PP/IFR systems at high temperature (T > 500degreesC). The FTIR results provide the positive evidence that IFR can improve the thermal stability of PP and SiW12 can induce a higher rate of formation of phosphoric acid and its derivatives. The LRS measurements provide useful information on the carbonaceous microstructures. In short, a suitable amount of SiW12 (1.5 wt%) exerts synergistic effects with the IFR by increasing the LOI value and the thermal stability at high temperature and promoting the formation of charred structures on the burning PP surface.

Synergistic effect of MXene on the flame retardancy and thermal degradation of intumescent flame retardant biodegradable poly(lactic acid)composites

The effect of Ti3C2 MXene nanosheets on the intumescent flame retardant(IFR)poly(lactic acid)(PLA)composites was investigated among a series of PLA/IFR/MXene,which were prepared by melt blending 0-2.0 wt%MXene,10.0 wt%-12.0 wt%IFR and PLA together.The results of limiting oxygen index(LOI)and vertical burning(UL-94)discover that the combination of 0.5 wt%MXene and 11.5 wt%IFR synergistically improves the fire safety of PLA to reach UL-94 V-0 rating with LOI value of 33.0%.The PLA/IFR/MXene composites perform an obvious reduction in peak of heat release rate(HRR)in cone calorimeter tests(CCTs).Furthermore,the carbon residues after CCTs were characterized by scanning electron microscope(SEM),laser Raman spectroscopy(LRS),X-ray diffraction(XRD)and X-ray photoelectron spectroscopy(XPS).It is demonstrated that both the titanium composition of the MXene structure and the characteristics of the two-dimensional material enhance the PLA/IFR/MXene composite materials’ability to produce a dense barrier layer to resist burnout during thermal degradation.

AN S-AND P-CONTAINING FLAME RETARDANT FOR POLYPROPYLENE

A novel charring agent,bis(1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane) phenylphosphine sulfide (BCPPS),has been synthesized,and it is combined with ammonium polyphosphate (APP) and melamine phosphate (MP) to impart flame retardance and dripping resistance for polypropylene (PP).The fire performance of the treated PP is investigated by limiting oxygen index (LOI),vertical burning test (UL-94) and cone calorimeter,and the thermal stability and thermal oxidative stability of the composite...

Anti-Bacterial and Flame Retardant for Cotton Fabric by One-Bath Finishing

A research on the process of cotton fabric flame-re-tarding,anti-bacterial finishing and one-bath finish-ing of anti-bacterial and flame-retarding is discussed.The flame retardant agent was phosphorous-contained,and the bacteriostatic finishing agent named SFR-1 wassynthesized.The flame retardancy of the fabric finishedcan meet the DOC FF3-71 Children Sleepwear Stan-dard.Its bacterial inhibiting capacity can meet and ex-ceed the requirements of similar products

聚苯胺-碳化硅复合材料在膨胀型防火涂料中的应用

膨胀型防火涂料在阻隔基材迅速升温方面具有明显效果。试验合成了聚苯胺-碳化硅(PANI-SiC)复合材料,通过SEM、FTIR、XRD等手段分析了复合材料的形貌、组成和结构,考察了单组分膨胀型防火涂料乳液的种类及复合材料含量对涂层防火耐火性能的影响。结果表明:醋酸乙烯-乙烯(VAE)乳液相比于苯丙乳液和丙烯酸乳液可以更好地提升涂层的膨胀倍率和耐火性能。随着PANI-SiC含量的增加,涂层的膨胀倍率增加,背面温度降低,10%含量复合材料的防火涂层表现出优异的耐火性能。

利用OVMT和CMS提高IFR/H-PP复合材料的阻燃和力学性能

以打包盒PP废塑料(H-PP)为原料、膨胀型阻燃剂(IFR)为阻燃剂、有机蛭石(OVMT)和碳微球(CMS)为阻燃协效剂,制备阻燃H-PP复合材料,对复合材料的极限氧指数(LOI)、UL 94阻燃等级和力学性能进行测试,并且,采用TG、锥形量热仪和SEM进行分析。结果表明,OVMT和IFR在H-PP中具有协同阻燃效果,当H-PP中OVMT含量为4%、IFR含量为24%时,复合材料的LOI值为29.8%,阻燃级别达到UL 94 V-0级,OVMT提高了IFR/H-PP的力学性能;CMS和IFR在H-PP中具有协同阻燃效果,CMS能提高IFR/H-PP的力学性能;在IFR/H-PP中同时加入OVMT和CMS,复合材料的阻燃和力学性能均得到提高,2-OVMT/2-CMS/24-IFR/H-PP的LOI为32.4%,阻燃级别达到UL 942.0 mm V-0级,其拉伸强度、弯曲模量、弯曲强度和缺口冲击强度分别为22.5、1132.1、26.2 MPa和3.8 kJ/m^(2),与28-IFR/H-PP相比,分别提高了11.9%、0.3%、8.3%和31.0%。

SYNERGISTIC EFFECTS OF LAYERED DOUBLE HYDROXIDE WITH PHOSPHORUS-NITROGEN INTUMESCENT FLAME RETARDANT IN PP/EPDM/IFR/LDH NANOCOMPOSITES

Synergistic effects of layered double hydroxide （LDH） with intumescent flame retardanct （IFR） of phosphorusnitrogen （NP） compound in the polypropylene/ethylene-propylene-diene/IFR/LDH （PP/EPDM/IFR/LDH） nanocomposites and related properties were studied by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, scanning electron microscopy （SEM）, limiting oxygen index （LOI）, UL-94 test, cone calorimeter test （CCT） and thermo-gravimetric analysis （TGA）. The XRD and TEM results show that the intercalated and/or exfoliated nanocomposites can be obtained by direct melt-intercalation of PP/EPDM into modified LDH and that LDH can promote the IFR additive NP to disperse more homogeneously in the polymer matrix. The SEM results provide positive evidence that more compact charred layers can be obtained from the PP/EPDM/NP/LDH sample than those from the PP/EPDM/LDH and PP/EPDM/NP samples during burning. The LOI and UL-94 rating tests show that the synergetic effects of LDH with NP can effectively increase the flame retardant properties of the PP/EPDM/NP/LDH samples. The data from the CCT and TGA tests indicate that the PP/EPDM/NP/LDH samples apparently decrease the HRR and MLR values and thus enhance the flame retardant properties and have better thermal stability than the PP/EPDM/LDH and PP/EPDM/NP samples.

Study on fire retardant mechanism of nano-LDHs in intumescent system

This paper investigated the fire-retardant mechanism of the nano-LDHs in the intumescent system by the temperature programmed oxidation (TPO). Researches were also conducted to explore the function of the nano-LDHs in the composite fire-retardant agents in air and nitrogen atmosphere, respectively. The results indicated that the nano-LDHs species were responsible for the catalytic oxidation of the rich-carbon compound in oxygen atmosphere. In addition, the nano-LDHs species and their calcinated products at high temperature could increase the carbonaceous residue-shield of the carbon-rich materials, improve the quality and the graphitization degree of the formed char-layer, and accelerate the intumescence and expansion of the melting carbon-rich materials to a certain degree under the oxygen-free condition, leading to the carbonization and expansion of the intumescent layer.

单组分磷-氮膨胀阻燃剂的合成及成炭性能

以六氯环三磷腈、对羟基苯甲醛及9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)等为原料,合成出新型单组分磷-氮膨胀阻燃剂六(4-(9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物)-羟甲基苯氧基)环三磷腈(Ⅴ),其结构经红外光谱(IR)、质谱(MS)和核磁共振(1H-NMR)表征。热失重分析表明,化合物(Ⅴ)具有较高热稳定性和良好成炭性,起始分解温度为195℃,800℃时炭残量达50.3%。扫描电镜观测发现,500℃时,化合物(Ⅴ)产生连续、致密、光滑、均匀的膨胀炭层。变温红外光谱研究表明,当温度从200℃加热至700℃时,化合物(Ⅴ)官能团强度逐渐由强变弱,并在1631 cm-1处产生新的芳香环炭层结构吸收峰。

新型单组分磷-氮膨胀型阻燃剂的合成及其阻燃性能

以氯化螺环磷酸酯(1)和对甲苯胺(2)为原料,经亲核取代反应合成了"三源"一体的新型单分子磷-氮膨胀型阻燃剂——季戊四醇螺环磷酰对甲苯胺(3),其结构经1H NMR和IR表征。考察了溶剂、原料配比、反应温度、反应时间和缚酸剂对3产率的影响。合成3的最佳反应条件为:乙腈为溶剂,三乙胺为缚酸剂,1 10mmol,n(1)∶n(2)=1∶3,于80℃反应4 h,产率79.3%。阻燃性能研究结果表明,3的初始分解温度为220℃,500℃成炭率达43.3%。

膨胀型阻燃剂磷酸-季戊四醇-三聚氰酰胺聚合物的合成及其在聚丙烯中的应用

研究了磷酸 -季戊四醇 -三聚氰酰胺聚合物的合成条件及膨胀效果 ,测定了阻燃聚丙烯的氧指数、水平燃烧性能 ,实验结果说明膨胀型阻燃剂的膨胀效果与组分有关 ,聚丙烯的阻燃效果随阻燃剂的膨胀效果增强 ,磷含量增大而显著改善。

新型阻燃剂CN-329的合成及阻燃性能

该文由三氯氧磷、季戊四醇、三聚氰胺和水合成一种新型阻燃剂CN - 32 9,并研究影响反应的因素 ,得出最佳工艺条件 ,用红外光谱、元素分析测定产品的化学结构。进行阻燃剂CN - 32 9在聚乙烯泡沫塑料的应用试验 ,阻燃聚乙烯泡沫塑料的氧指数 (OI)值为 2 7,显示CN - 32 9是一种较好的新型阻燃剂。采用差示扫描量热 (DSC)进行CN - 32 9的热分析 ,探讨了膨胀阻燃机理。该文对CN - 32 9的差示扫描量热 (DSC)

N-(5,5-二甲基-1,3,2-二氧杂己内磷酰基)取代苯甲醛腙的合成及其阻燃性能

采用 5 ,5 二甲基 2 氯 2 氧 1,3,2 二氧磷杂己内磷酸酯和水合肼及取代苯甲醛反应 ,合成了N (5 ,5 二甲基 1,3,2 二氧杂己内磷酰基 )取代苯甲醛腙系列化合物 (3a～ 3h)。通过元素分析、IR、1HNMR和MS对其结构进行了表征。对部分化合物的热重和差热分析表明 ,化合物的最大失重速率温区在 2 2 0～4 0 0℃ ,这与大部分高分子材料的热氧降解温区重叠 ,具有很好的阻燃配伍性能。化合物 3a～ 3h在醇酸清漆和环氧树脂 (E 4 4 )中的初步阻燃试验表明 ,有很好的阻燃性能。

复合阻燃剂对PE-LD阻燃和力学性能影响的研究

通过氧指数测试、热重分析和力学性能测试研究了超细硼酸锌对由聚磷酸铵与季戊四醇组成的膨胀型阻燃剂(IFR)阻燃的低密度聚乙烯阻燃性能和力学性能的影响。结果表明：超细硼酸锌与膨胀型阻燃剂以4．2：25．8质量比组成的复合阻燃剂的协同阻燃效果最好,含量达到30%(以PE-LD计)时,氧指数从24．5%(IFR阻燃的PE-LD)提高至26．2%,力学性能亦有一定程度的改善,拉伸强度从7．39 MPa升高到8．51 MPa,断裂伸长率从57%提高到68．1%。热重分析表明当温度高于540℃后,复合阻燃剂阻燃的PE-LD明显比IFR阻燃的PE-LD失重变慢,高温残重率增加。从扫描电镜和能谱分析可知,阻燃试样550℃的灼烧样品成炭较致密,在炭层中除了含碳外,还含有较大量的磷元素和少量的氮元素,可能与其凝聚相阻燃机理相关。

磷-氮大分子膨胀型阻燃剂及其阻燃聚丙烯的研究进展

磷-氮大分子膨胀型阻燃剂(MIFR)有效克服了传统多组分膨胀型阻燃剂易迁移、易吸湿、与基体相容性差等缺点,是目前最具发展前景的无卤阻燃剂之一。文中综述了近年来国内外关于多组分和单组分磷-氮MIFR及其阻燃聚丙烯(PP)的最新研究进展,分析了磷-氮MIFR亟需解决的问题,并指出了"三源一体"和多功能化是磷-氮MIFR的发展趋势。