皮芯复合阻燃疏水纤维的制备工艺

采用有机膦系G-77阻燃剂对聚对苯二甲酸乙二醇酯(PET)进行共混改性用作芯层料,赋予纤维阻燃性能,采用聚偏氟乙烯(PVDF)和共聚阻燃母粒对自制阻燃母粒进行改性用作皮层料,赋予纤维一定的阻燃性和疏水性;将改性后皮芯料通过皮芯复合纺丝制得多功能阻燃疏水纤维;探讨了芯层料和皮层料阻燃加入量对其阻燃性能的影响,研究了皮芯复合阻燃疏水纤维的制备工艺及其原丝的力学性能。结果表明:当芯层料中的G-77阻燃剂与PET的质量比为7.25/100时,其极限氧指数(LOI)为27.8%;当皮层料中的PVDF的质量分数为6%,自制阻燃母粒与共聚阻燃母粒质量比为7.0/3.0时,其与水的接触角为83.4°,LOI为26.3%;当皮芯复合比为20.0/40.5,卷绕速度为1 200 m/min,拉伸倍数为3.75时,皮芯复合阻燃疏水纤维的可纺性较好,原丝的线密度为2.15 dtex,断裂强度为4.52 cN/dtex。     

六苯氧基环磷腈阻燃聚乙烯醇纤维结构与性能研究

将六苯氧基环磷腈(HPCTP)无卤阻燃剂与聚乙烯醇(PVA)进行共混纺丝制备阻燃PVA纤维,研究了纤维的阻燃性能及阻燃机理;并将阻燃性较好的纤维进行缩甲醛化处理,观察HPCTP在醛化过程中的稳定性。结果表明:随着HPCTP含量的增加,阻燃PVA纤维的阻燃性能有所增加,当HPCTP质量分数为30%时,阻燃PVA纤维的热稳定性得到大幅提高,其在600℃下的质量保持率为18. 77%,极限氧指数(LOI)达到31%,阻燃PVA纤维经缩甲醛化后LOI达26. 5%,仍然能达到阻燃要求;对阻燃PVA纤维的阻燃机理研究发现,当HPCTP质量分数小于30%时,其在纤维中仅有气相阻燃作用,而当HPCTP质量分数为30%时,其在凝聚相和气相中均起到阻燃作用;随着HPCTP含量的增加,阻燃PVA纤维的力学性能降低,当添加HPCTP质量分数为30%时,阻燃PVA纤维的断裂强度为2. 8 c N/dtex,仍能满足纤维的使用要求。     

磷硅无卤阻燃聚乙烯醇缩甲醛纤维的制备与表征

采用无卤阻燃剂二硫代焦磷酸酯和二氧化硅与聚乙烯醇(PVA)进行共混纺丝,制备了无卤阻燃聚乙烯醇缩甲醛(PVFM)纤维,研究了阻燃剂配比、阻燃剂含量对纤维结构与性能的影响,并对阻燃纤维的力学性能、阻燃性能、热性能以及残炭的化学结构、表面形貌进行了测试表征。结果表明:当二硫代焦磷酸酯和二氧化硅质量比为5∶5时,纤维综合性能较好;随着复配阻燃剂含量的增加,PVFM纤维的极限氧指数(LOI)逐步提高,高温下的最大分解速率温度和残炭量均增加,但其断裂强度有所下降;当复配阻燃剂质量分数为20%时,阻燃PVFM纤维的LOI为29.4%,断裂强度为5.78 cN/dtex,最大热分解温度和残炭率比纯PVFM纤维均有较大幅度的增加,燃烧可形成连续致密的炭层。     

二硫代焦磷酸酯微胶囊阻燃PVA纤维的制备及性能

采用原位聚合的方法制备了以新戊二醇二硫代焦磷酸酯(DDPS)为核、三聚氰胺甲醛树脂(MF)为壳的阻燃微胶囊(MDDPS),分别将DDPS和MDDPS无卤阻燃剂与聚乙烯醇(PVA)共混纺丝,制备了无卤阻燃PVA纤维;表征了MDDPS的结构及形貌,研究了纯PVA纤维、DDPS/PVA纤维、MDDPS/PVA纤维的力学性能、阻燃性能、热稳定性、燃烧前后的形貌。结果表明:微胶囊MDDPS的平均粒径增大至7.82μm,仍能满足共混纺丝要求;DDPS及MDDPS的加入,PVA纤维力学性能下降;MDDPS/PVA纤维阻燃性能较好,极限氧指数达31.3%,燃烧时膨胀较为明显,且600℃时残炭率达到19.1%,炭层较为致密,有气泡产生,释放不燃性气体阻止了燃烧。     

增韧改性ADP-12阻燃ABS树脂的性能研究

使用二乙基次膦酸铝(ADP-12)并用协效阻燃剂三聚氰胺氰尿酸盐(MCA)制备无卤阻燃丙烯腈-丁二烯-苯乙烯(ABS)复合材料,使用不同增韧剂对阻燃ABS进行增韧改性,对其阻燃性能及力学性能进行了研究。结果表明,填加增韧剂聚醚型聚氨酯(TPU)制备的阻燃ABS合金综合阻燃性能最优,氧指数达到33.6%,垂直燃烧显示出V-1级别;SBS对阻燃ABS增韧效果最好,制备的阻燃苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS)/ABS合金力学性能最优,冲击强度、断裂伸长率均比未填加增韧剂的阻燃ABS有所提高;通过偏光显微镜发现,阻燃剂在TPU/ABS合金中阻燃剂分散较好,但仍有团聚现象存在。     

无卤阻燃改性超高分子量聚乙烯纤维的制备及性能

通过氮磷系阻燃剂复配方式,以三聚氰胺氰尿酸盐(MCA)为主阻燃剂,二乙基次膦酸铝(ADP)为协效阻燃剂,六方氮化硼(h-BN)为杂化改性剂,白油为溶剂,制备了无卤阻燃超高分子量聚乙烯(PE-UHMW)纤维。首先对阻燃剂粉体进行干燥、表面处理,然后与白油共混,经过超声波液相分散、研磨机高速研磨,得到无卤阻燃浆料。将此阻燃浆料分散到PE-UHMW纺丝原液中,经双螺杆挤出机挤出得到冻胶丝,冻胶丝经过溶剂萃取、干燥、热牵伸,最终得到阻燃PE-UHMW纤维,对纤维的阻燃性能和力学性能进行表征。结果表明,通过研磨机的反复研磨,可将粉体粒径降低到百纳米级别,更易于在PE-UHMW溶胀液中分散,且极大地提升了阻燃纤维的可纺性;杂化改性剂提升了复配阻燃剂的阻燃性和材料的阻燃等级,当h-BN质量分数为4%时,阻燃剂质量分数可以到20%,PE-UHMW纤维的极限氧指数值达到27.5%,材料阻燃等级达到V-0级;通过一系列改性手段,可使PE-UHMW纤维在添加大量的阻燃粉体后,仍能保持良好的可纺性,且改性对纤维力学性能影响较小,拓宽了PE-UHMW纤维的应用领域,提升其使用价值。     

改性钠基膨润土协同卤锑阻燃LDPE的研究

采用钠基膨润土(Na-MMT)、卤锑复配阻燃剂和低密度聚乙烯(LDPE)树脂制备了阻燃复合材料,研究了改性Na-MMT协同卤锑复配阻燃剂对LDPE阻燃材料的燃烧性能、力学性能及热性能的影响。结果表明:改性Na-MMT替代部分卤锑复配阻燃剂时,其垂直燃烧等级均达到UL94 V-0级,极限氧指数均在32.0%以上。当改性Na-MMT质量分数为8%时,阻燃材料的极限氧指数达到33.8%;当改性Na-MMT质量分数为16%时,阻燃材料的力学性能最优。     

PVA/SA/MF阻燃复合纤维的制备和性能研究

以聚乙烯醇(PVA)、海藻酸钠(SA)和三聚氰胺-甲醛树脂(MF)混合液为纺丝原液,采用湿法纺丝工艺制备PVA/SA/MF复合纤维。研究了PVA与SA及MF的共混比例对复合纤维阻燃性能和力学性能的影响。结果表明:PVA/SA/MF复合纤维的表面均匀光滑,其内部为网状结构;随着MF含量的增加,复合纤维阻燃性能增强,但其断裂强度呈现先增加后降低的趋势;当PVA∶SA∶MF质量比为10∶1∶4时,复合纤维的阻燃性能和力学性能均较好,其极限氧指数(LOI)为29. 8%,断裂强度为3. 19 c N/dtex;当PVA∶SA∶MF质量比为10∶1∶6时,复合纤维的阻燃性能、热性能及耐阻燃耐久性最好,其LOI为32. 0%,600℃时的质量保持率为24%左右,水洗50次后的LOI为25. 9%。     

高耐磨阻燃改性聚丙烯电缆保护管的制备及性能研究

为提高改性聚丙烯电缆保护管的耐磨阻燃性能,采用自制的高耐磨及阻燃材料制备高耐磨阻燃改性聚丙烯电缆保护管。研究通过添加高耐磨材料及阻燃材料对改性聚丙烯电缆保护管的导热耐磨性能、阻燃性能及力学性能的影响。实验结果表明:采用自制纳米球形Al2O3接枝棕榈纤维耐磨剂和自制笼型聚倍半硅氧烷接枝二乙烯三胺五甲叉膦酸铵阻燃剂能显著的提高材料的阻燃性能和耐磨性能,同时在一定程度上提高材料的弯曲模量和环刚度;PP/阻燃剂/耐磨剂配比为100/25/15时,高耐磨阻燃改性聚丙烯电缆保护管极限氧指数为37%,质量磨损为43.8 mg,弯曲模量为63.3 MPa,环刚度Ф100为30.3 kN/m2,综合性能最为均衡。     

结构阻燃型腰果酚基硬质聚氨酯泡沫的制备及性能研究

以三聚氰胺改性腰果酚基阻燃多元醇和异氰酸酯为主要原料,采用环戊烷为发泡剂,添加无卤阻燃膨胀型阻燃剂石墨(EG)、匀泡剂等制备无卤阻燃生物基硬质聚氨酯泡沫塑料。探讨结构阻燃型聚醚多元醇、阻燃剂的添加对生物基硬质聚氨酯泡沫的热性能、燃烧性能和力学性能的影响。结果表明,随着阻燃剂的增加,导热系数和固化时间增加;添加相同阻燃剂的泡沫样品其阻燃性能随着添加量的增加而增加,EG在提高氧指数方面优于聚磷酸铵(APP)和乙基膦酸二乙酯(DEEP),固体阻燃剂APP和EG在增加力学性能、热稳定性方面较液体阻燃剂DEEP效果好。     

Preparation of flame‐retardant leather pretreated with pyrovatex CP

Resistance to burning is one of the most useful properties that can be imparted to leather. Pyrovatex CP is rich in phosphorus and nitrogen and has been successfully used as a flame‐retardant agent in the presence of etherified methylolated melamine (EMM). The effects of a finishing formulation containing Pyrovatex CP and EMM on the flame retardancy and other properties of modified leather have been studied under different conditions. The synergistic effect of the N/P ratio has been thoroughly investigated through the estimation of the nitrogen and phosphorus contents, and their impact on the flame retardancy, tensile strength, and elongation at break of the treated leather has been studied. An investigation of the different factors has led to the following conclusions: (1) the P and N percentages increase with increasing curing temperature and time, (2) increases in the Pyrovatex CP and EMM concentrations are accompanied by an enhancement of the P and N percentages, and (3) all samples exhibit loss in their tensile properties but within an acceptable range (20%). © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

Flame‐retardant properties of soybean fabric modified with N‐methylol diakyl phosphonopropionamide

Soybean is a competitive production material for fibers as it is abundant and cost effective. However, an inherent deficiency of soybean fiber is its poor flame‐retardant performance. In this study, the effect of N‐methylol diakyl phosphonopropionamide (Pyrovatex CP) on the flame retardancy of soybean was investigated by the Limiting Oxygen Index (L.O.I.) and the vertical flammability test. Little benefit with regard to flame retardancy was found when soybean was treated with Pyrovatex CP in the absence of additives. However, the incorporation of Lyofix MLF in the finishing treatment (3% w/v) increased the L.O.I. values of soybean fiber and enhanced char formation as indicated by Thermogravimetric Analysis (TGA). Improved fastness to washing was observed at higher application levels of Lyofix MLF (6% w/v). X‐ray Photoelectron Spectroscopy (XPS) indicated that surface phosphorus (% atomic) was reduced following washing for all fabrics examined. In addition, the substantivity of Lyofix MLF to soybean surface was exhibited. The flame‐retardant treatment presented in this article is cost effective and results in wash‐durable flame‐retardant fabrics. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Flame retardancy finish with an organophosphorus retardant on silk fabrics

The paper mainly deals with flame retardancy of silk fabrics treated with a commercial organophosphorus flame retardant [N‐hydroxymethyl (3‐dimethyl phosphono) propionamide (HDPP), also known as Pyrovatex CP], using the pad‐dry‐cure‐wash method. The structures and properties of the treated and control sample are discussed. The Limiting Oxygen Index (LOI) value of the modified sample is above 30%. After 50 laundry cycles, it still has some flame retardancy left. HDPP and a cross‐linking agent (HMM) were bound to silk fabrics which is confirmed by FT‐IR spectra and amino analysis. The reaction degree of the flame retardant with silk is also high; almost all the tyrosine units have reacted, which can be confirmed by amino acid analysis. The reaction between flame retardant and silk only occurs in the amorphous region of silk fibre, which is confirmed by X‐ray diffraction analysis and amino acid analysis. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis show that the flame retardant causes silk fabrics to decompose below its ignition temperature (600°C) and formed carbonaceous residue or char when exposed to fire. The char behaves as a thermal barrier to fire, so silk fabrics show good flame retardancy. The treatment has a little effect on the whiteness of the silk fabrics and the tensile strength of treated silk fabrics slightly decreased; both effects are negligible. Copyright © 2006 John Wiley & Sons, Ltd.     

The application of a novel flame retardant on viscose fiber

The paper is mainly about a novel organophosphorus flame‐retardant N‐1‐chloroisopropyl alcohol‐3‐dimethylphosphonopropionamide. Dimethyl phosphate, acrylamide and epichlorohydrin were used as raw materials. The mechanisms of synthesis and molecule structure of the flame retardant were discussed. The fiber was treated using the pad‐dry‐cure‐wash method. The limiting oxygen index value of the modified sample was 31%, higher than that of the sample treated with MDPA (Pyrovatex CP). After 50 laundry cycles, it still had some flame retardancy left. Thermogravimetry (TG) and Differentiate TG analyses confirmed that the flame retardant caused fiber to decompose below its ignition temperature and formed carbonaceous residue or char when exposed to fire. The treatment had an obvious effect on the denier of the fiber; the tensile strength of fiber slightly decreased, but that effect could be negligible. Copyright © 2008 John Wiley & Sons, Ltd.     

硅氮系阻燃黏胶纤维的结构与性能研究

分析了硅氮系阻燃黏胶纤维的结构与性能,探讨其阻燃机制。通过扫描电子显微镜、X射线衍射、力学性能以及极限氧指数等测试,分析了硅氮系阻燃剂含量对纤维阻燃性能、热性能和力学性能等的影响。结果表明:当阻燃剂质量分数为20%时,纤维的干态断裂强度为2.1 cN/dtex,极限氧指数为28%,在满足纺织服用需求的同时,达到国家阻燃标准,兼具安全环保与良好的阻燃性能。     

无卤阻燃聚乙烯醇缩甲醛纤维的制备与表征

以新戊二醇和三氯硫磷为原料,一步法合成了无卤膨胀型阻燃剂二硫代焦磷酸双新戊二醇酯(BGDTP);采用傅里叶变换红外光谱(FTIR)、核磁共振氢谱(~1H-NMR)对BGDTP的结构进行了表征。将BGDTP添加到聚乙烯醇(PVA)中进行共混纺丝,制备了阻燃聚乙烯醇缩甲醛(PVFM)纤维,并对其力学性能、阻燃性能和热性能进行了表征。结果表明:一步法合成BGDTP的收率为82%;随着纤维中BGDTP添加量的增加,PVFM纤维的极限氧指数(LOI)、高温下的最大分解速率温度和残炭量均增大,但其断裂强度略有下降;当w(BGDTP)为20%时,阻燃PVFM纤维的LOI为30.8%,断裂强度为5.42 cN/dtex,最大热分解温度和残炭率比纯PVFM纤维均有较大幅度增加,燃烧形成连续致密的膨胀炭层。     

Synthesis and application of a sulfur‐containing phosphoric amide flame retardant for nylon fabric

A sulfur‐containing flame retardant (SFR) was synthesized from polyphosphoric acid, epoxy chloropropane, and thiourea. Using a water‐soluble isocyanate‐terminated (WIT) cross‐linker, the flame retardant was applied as a flame‐retardant finishing on nylon fabric. WIT is a compound that not only cross‐links SFR and nylon cellulose but also contains no formaldehyde. Comparisons of the main performances of SFR with those of N‐methyloldimethylphosphonopropionamide (known as ‘Pyrovatex CP’) and a bicyclic phosphonite (known as ‘Antiblaze 19T’) indicate that the presence of sulfur in SFR plays a crucial role in decreasing the flammability of the nylon fabric. The limiting oxygen index value and damaged carbon length of the finished nylon fabric were 29.4% and 5.7 cm, respectively, when the concentrations of SFR and WIT were 200 and 40 g/L, respectively, and the baking temperature and time were 150 °C and 3 min, respectively. After 10 laundry cycles, the fabric still retains some flame retardancy. Copyright © 2016 John Wiley & Sons, Ltd.     

阻燃LDPE的研究

主要研究了添加卤素阻燃剂如氯化石蜡（CP）、双（六氯环在戊二烯）环辛烷（DCRP）和十溴联苯醚（DBDPO）的低密度聚乙烯（LDPE）燃烧性．用锥形量热仪和极限氧指数实验测试了其燃烧特性，讨论了卤素阻燃剂对LDPE力学性能的影响。结果表明．与纯LDPE相比．添加了卤素阻燃剂的LDPE的热释放速率峰值（QPHKR）、质量损失速率（QMLR）显著降低，但生烟速率（QSPR）增大；加入DCRP的LDPE的质量热释放速率（QHRR）、质量损失（QML）低于其他2种阻燃体系的，加入DBDPO的LDPEQHKR最高．添加CP的LDPEQSPR最低；并用卤素阻燃剂和Sb2O3后，LDPE的阻燃效果更为显著；DCRP对LDPE的拉伸强度影响最大，DBDPO对LDPE的断裂伸长率影响最小；DCRP，DBDPO．CP的加入提高了LDPE的弯曲强度。     

Valorization of kapok fiber by phosphorylation with a reactive phosphorus- and nitrogen-containing flame retardant for enhanced fire safety

Kapok fiber (KF) with a naturally hollow structure has found an increasing application in filling and composite materials, most of which have a demand of flame retardancy. To realize this high-value utilization, KF was phosphorylated by a reactive phosphorus- and nitrogen-containing flame retardant for enhanced fire safety. The flame retardant was first synthesized by the reaction of urea and diethylene triamine pentakis (methyl phosphonic acid) (a commercially available scale inhibitor) with low cost, and then, applied in the phosphorylation of KF in the presence of dicyandiamide. In thermogravimetric analysis, phosphorylated KF showed 38.1% residue weight in nitrogen and 10.2% residue weight in air at 700°C, whereas the residue weight of KF was 8.4% in nitrogen and 1.5% in air. In microcalorimetric analysis, the heat release capacity and total heat release of phosphorylated KF displayed a reduction of 81% and 55%, respectively. In vertical combustion test, phosphorylated KF was difficult to ignite and had no afterburning or smoldering. The tests indicated that phosphorylated KF had excellent charring properties, low heat release, and good flame retardancy. This work suggests a promising strategy of enhancing the flame retardancy of KF and increasing its applicability in filling and composite materials.