共聚型磷系阻燃聚酯聚合反应动力学及其性能

为探究共聚型磷系阻燃聚酯的反应规律及其影响因素,以2-羧乙基苯基次磷酸(CEPPA)为阻燃剂制备不同磷含量的阻燃共聚酯,建立了聚酯反应动力学模型并分析其影响因素。借助红外光谱仪、差示扫描量热仪、热失重测试仪、极限氧指数仪、锥形量热仪对聚酯的结构及性能进行测试与分析。结果表明:随着CEPPA质量分数的增加,缩聚反应活化能逐渐增大,最高增加至106.83 kJ/mol;聚合物的玻璃化转变温度、熔点均呈下降趋势;阻燃剂中磷元素以共价键形式共聚到PET分子链中,抑制了分子链的结晶;当磷含量为1%时,阻燃共聚酯的极限氧指数达到31%,引燃时间明显延长,最大热释放速率降低了24%,阻燃效果显著。     

磷硅改性阻燃抑熔滴聚酯纤维的制备及其性能

针对聚酯(PET)纤维易燃且燃烧时伴随着大量熔滴与烟气的问题,将二乙基次膦酸盐阻燃剂、大分子型有机硅与PET载体共混制备磷硅阻燃母粒。将磷硅阻燃母粒按照一定质量分数添加到常规PET切片中混合,经熔融纺丝制得阻燃抑熔滴PET纤维。借助扫描电子显微镜、复丝强度仪、差示扫描量热仪、热重分析仪、氧指数测试仪、拉曼光谱仪对阻燃PET的力学性能、热性能与阻燃性能等进行表征和分析。结果表明：二乙基次膦酸盐阻燃剂使PET表面脱水成炭,大分子型有机硅提升了炭层的石墨化程度,形成有序稳定的炭层,增强了阻燃PET纤维阻燃性能并抑制熔滴形成,且燃烧形成的烟气量下降;添加质量分数为3%的二乙基次膦酸盐阻燃剂与0.77%大分子型有机硅纺制的阻燃PET纤维,其极限氧指数达到31%以上,垂直燃烧测试等级达到V-0级;通过磷硅元素间的阻燃协效作用改善了阻燃PET纤维的可纺性,同时使其具有良好的阻燃与抑熔滴性能。     

碳点对阻燃聚对苯二甲酸乙二醇酯性能的影响

为探究零维碳纳米材料碳点(CDs)对阻燃聚对苯二甲酸乙二醇酯(FRPET)热力学性能、阻燃性能、力学性能及荧光性能的影响,将对PET具有良好阻燃效果的共聚型阻燃剂2-羧乙基苯基次膦酸(CEPPA)与碳点同时采用原位聚合的方式添加到PET基体中,研究碳点添加量对FRPET各项性能的影响规律。通过极限氧指数(LOI值)、垂直燃烧(UL94)、锥形量热(CONE)等测试分析不同碳点添加量对FRPET的性能影响。结果表明:在碳点添加量为1.50%时,FRPET的LOI值最高可达34%,垂直燃烧级别为V-0级,较只添加CEPPA的FRPET引燃时间变长、热释放速率峰值与平均热释放速率及总热释放量均降低;加入CDs后FRPET的力学性能也有很大改善,且赋予了荧光性能,有益于拓宽FRPET的应用领域。     

DDPSi-FR阻燃整理对羊毛织物染色性能的影响

采用硅磷杂化单体DDPSi-FR对羊毛织物进行轧烘焙阻燃整理,讨论了阻燃整理效果及其对羊毛织物的润湿性能、染色性能、力学性能及防紫外线性能的影响。结果表明:DDPSi-FR阻燃整理能提高羊毛纤维的疏水性,静态接触角增加≤3.02%;引起LANASOL系列染料染色羊毛织物的色度参数波动,特别是使K/S值下降≤13.85%;显著提高未染色以及LANASOL系列染料特别是蓝3G染料染色羊毛织物的紫外线防护性能;提高未染色或染色羊毛织物顶破强力,认为由DDPSi-FR与羊毛分子链间的交联作用所致。     

阻燃PET纤维的染色性能探讨

本文采用分散红3B 和分散蓝RRL 染料对新研制的阻燃PET 纤维进行了高温高压染色。阻燃PET 纤维的上染率随阻燃剂含量的增加先上升然后下降,最大上染率为4%(重量百分数)。对分散红3B 和分散蓝RRL 的最高上染率的染色条件分别为分散红温度120℃,时间60分钟;分散蓝温度130℃,时间60分钟。     

阻燃Lyocell与羊毛混纺经编坐垫织物开发

以Lyocell纤维为原料,通过添加20%阻燃剂CEPPA制备阻燃Lyocell纤维,利用半精纺系统纺制26 tex阻燃Lyocell纤维与羊毛混纺纱(55∶45),并采用该纱线在德国RD6-DPLM经编机上开发经编坐垫织物。介绍纤维制备、混纺纱制备及织物编织工艺,并测试分析阻燃Lyocell纤维与羊毛混纺织物的压缩性能、阻燃性、透气性、弯曲性、抗皱性、抗起毛起球性。结果表明,开发的织物压缩性能良好,抗起毛起球等级达到4级,纵横向断裂强力分别为613.12 N和442.73 N,缓弹性折皱回复角为143.9°,透气性达到223L/(m~2·s),织物各项性能均良好,且具有一定的阻燃效果。     

红磷阻燃增强PET/蒙脱土复合材料的研究

以PET/蒙脱土为基材树脂,通过添加玻纤、红磷阻燃剂、增韧剂等,制备出可在低模温下成型的PET/蒙脱土玻纤增强无卤阻燃工程塑料。研究了红磷阻燃剂、增韧剂对工程塑料性能的影响,结果表明,采用红磷阻燃体系,当添加量为16%时,能达到UL94-V0;在相同含量阻燃剂的情况下,随着增韧剂PTW含量的增加,复合材料的抗冲击性能逐步得到提高,复合材料的拉伸强度先随着增韧剂含量的增加而增加;当增韧剂含量达到2.5%之后,拉伸强度略有降低;复合材料具有良好的成型加工性等综合性能。     

PET的含硼阻燃剂和磷腈阻燃剂协同阻燃整理北大核心

苯氧基环三磷腈衍生物spb-100(PNCP)是一种商品化的磷腈阻燃剂,应用于聚对苯二甲酸乙二醇酯(PET)阻燃整理时融滴现象严重。为提高PNCP应用于PET的阻燃效果,合成了两种含硼阻燃剂硼酸乙烯苯酯(ATPB)和含硼超支化聚合物(HBb),并分别与PNCP共混应用于PET阻燃。利用极限氧指数仪(LOI)、垂直燃烧仪(UL-94)、热失重分析测试仪(TGA)、扫描电镜仪(SEM)和激光共聚焦显微拉曼仪(Raman)等对织物的阻燃性能、热稳定性能、成炭性能等进行测试。结果表明,ATPB、HBb均能与PNCP产生协同阻燃效应,不仅进一步提高了PET材料的LOI值,还能提高PET基复合材料的抗融滴性能。当PNCP、HBb添加量分别为10%和5%时,协同效果最好,其PET基复合材料的LOI值达到31.8,UL-94等级通过V-0级,热分解速率较纯PET下降29.9%。利用热裂解-气质联用、扫描电镜、拉曼光谱等分析了PNCP/含硼阻燃剂体系对PET的协同阻燃机理,发现该阻燃体系能够在PET燃烧时的气相和凝聚相中同时起阻燃作用。     

PET的含硼阻燃剂和磷腈阻燃剂协同阻燃整理

苯氧基环三磷腈衍生物spb-100(PNCP)是一种商品化的磷腈阻燃剂,应用于聚对苯二甲酸乙二醇酯(PET)阻燃整理时融滴现象严重。为提高PNCP应用于PET的阻燃效果,合成了两种含硼阻燃剂硼酸乙烯苯酯(ATPB)和含硼超支化聚合物(HBb),并分别与PNCP共混应用于PET阻燃。利用极限氧指数仪(LOI)、垂直燃烧仪(UL-94)、热失重分析测试仪(TGA)、扫描电镜仪(SEM)和激光共聚焦显微拉曼仪(Raman)等对织物的阻燃性能、热稳定性能、成炭性能等进行测试。结果表明,ATPB、HBb均能与PNCP产生协同阻燃效应,不仅进一步提高了PET材料的LOI值,还能提高PET基复合材料的抗融滴性能。当PNCP、HBb添加量分别为10%和5%时,协同效果最好,其PET基复合材料的LOI值达到31.8,UL-94等级通过V-0级,热分解速率较纯PET下降29.9%。利用热裂解-气质联用、扫描电镜、拉曼光谱等分析了PNCP/含硼阻燃剂体系对PET的协同阻燃机理,发现该阻燃体系能够在PET燃烧时的气相和凝聚相中同时起阻燃作用。     

环三磷腈和三嗪衍生物协同阻燃对聚酯性能的影响

为提高聚对苯二甲酸乙二醇酯（PET） 的阻燃性能,合成了阻燃剂（4?烯丙氧羰基苯氧基） 环三磷腈（HACP）和三（4?烯丙氧羰基苯氧基）?1,3,5?三嗪（TATZ）,并与PET通过熔融共混制备了PET/HACP/TATZ复合材料。采用极限氧指数仪、垂直燃烧仪、微型量热仪、热失重分析测试仪、差示扫描量热仪和拉伸试验机等测试仪器对复合材料的阻燃性能、热稳定性能、力学性能和成炭性能进行测试与分析。结果表明：HACP和TATZ的协同阻燃性不仅提高了PET材料的阻燃效率,而且降低了对基材PET力学性能的负面影响,复合材料的极限氧指数值达到32.4%,垂直燃烧性能达到V-0 级,热释放速率较纯PET下降了30.9%。     

阻燃聚酯的研制及其结构和性能

首先用磷系阻燃剂2-羧乙基苯基次膦酸(CEPPA)与乙二醇(EG)合成2-羧乙基苯基次膦酸乙二酯(CEPPA-EG),再加入到对苯二甲酸乙二醇酯的缩聚体系中合成含磷阻燃聚酯。借助IR、SEM、DSC、TGA、LOI等测试方法对其结构以及热性能、成炭情况、燃烧性能进行研究。结果表明,阻燃剂以共聚的方式结合到聚酯大分子链上,并且随着阻燃剂添加量的增多,阻燃聚酯的Tg、Tm下降,而Tc则呈上升趋势,同时阻燃聚酯高温处理后成炭情况良好,炭粒均匀,相对未添加阻燃剂的纯聚酯,极限氧指数(LOI)有很大程度提高,阻燃效果得到较好的改善。     

磷杂菲基共聚协效阻燃聚酰胺6纤维的制备及其性能

为提高聚酰胺6(PA6)纤维的阻燃性能,以10-(2,5-二羧基苯氧基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(DOPODP)为共聚阻燃剂,复配二硫化钼(MoS₂)或硫化锌(ZnS),制备DOPODP共聚协效阻燃PA6,经熔融纺丝制备阻燃PA6纤维,并对其结构、性能及阻燃机制进行研究。结果表明:DOPODP经共聚法成功引入PA6,DOPODP可提高PA6的阻燃性能,但其熔融温度、结晶温度等下降;引入协效阻燃剂后,阻燃PA6垂直燃烧(UL94)级别为V-0级,极限氧指数(LOI值)达30%以上;DOPODP对PA6主要表现为气相阻燃作用,DOPODP分解产生含磷自由基可捕获活性自由基,协效阻燃剂可促进PA6成炭;相比PA6纤维,阻燃PA6纤维力学性能下降,而织物的LOI值提高。     

Preparation of microencapsulated carbon microspheres coated by magnesium hydroxide/polyethylene terephthalate flame–retardant functional fibers and its flame retardant properties

In order to improve the compatibility between the flame retardants of carbon microspheres coated by magnesium hydroxide (MH@CMSs) and the PET matrix and improve the spinnability of the masterbatch, MH@CMSs have been microencapsulated by PET to obtain microencapsulated carbon microspheres coated by magnesium hydroxide flame retardants – MMH@CMSs.Morphologies and structures of MMH@CMSs have been studied by scanning electron microscope (SEM), transmission electron microscopy (TEM), and FTIR, which showed that an organic shell layer of PET as capsule wall was coated on the surface of MH@CMSs. A series of MMH@CMSs/PET fibers with different MMH@CMSs contents were successfully prepared through the melt-spinning method. The morphology and structure of MMH@CMSs/PET fibers were characterized by SEM and FTIR. The flame retardancy of MMH@CMSs/PET fibers was determined via limiting oxygen index (LOI) test and cone calorimeter. Results showed that the MMH@CMSs/PET fibers possessed optimum flame retardancy when the MMH@CMSs content is 0.6 wt.%, at which the LOI reached a maximum of 25.8, and the pk-HRR, total heat release, and total smoke release were reduced by 27.4, 20, and 13.6%, compared with pure PET fibers, respectively. Moreover, the flame-retardant mechanism was studied by thermogravimetric analysis, thermogravimetric analysis-infrared spectrometry, and the SEM of the residue char, which disclosed that MMH@CMSs enhanced the thermal stability of PET fibers, and promoted PET fibers to form a dense and continuous protective char layer that effectively blocked heat transfer and combustible gas release.     

PBT/PET共混纤维的结构和性能

研究了ＰＢＴ／ＰＥＴ共混纤维结构和拉伸、染色性能的关系．实验结果表明．随着ＰＳＴ／ＰＥＴ共混比的增加,初生纤维的结晶度、取向度及纤维的断裂强度、上染率均增加．而断裂伸长下降,纤维经拉伸定形后．结构和住能有较大的变化．     

涤纶窗帘布阻燃涂层整理工艺探讨

采用涂层法对涤纶窗帘布进行阻燃整理,探讨了非卤素环保型阻燃剂TEX-8或TEX-4(有机膦高聚物)与水性聚丙烯酸酯涂层胶的配伍性、比例以及阻燃涂层胶涂覆量对织物阻燃性能、断裂强力、手感的影响.研究表明:阻燃剂TEX-8与涂层胶混合后的稳定性较好,阻燃性能比TEX-4稍好,当m(阻燃剂TEX-8)∶m(涂层胶)=1∶1、涂覆量30 g/m2时,阻燃性能可达国家B1级标准,且对断裂强力和手感无明显影响.     

Enhancing the flame retardant of polyethylene terephthalate (PET) fiber via incorporation of multi-walled carbon nanotubes based phosphorylated chitosan

Phosphorylated chitosan (PCS) were first deposited on the multi-walled carbon nanotubes (MWNTs) surface via chemical modification to obtain functionalized MWNTs-based PCS (PCS-MWNTs). Then, a series of PET fibers with MWNTs or PCS-MWNTs were prepared via melt spinning. The microstructure and molecular structure of PCS-MWNTs were characterized by field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy. The morphological structures, mechanical, thermal, and flame-retardant properties of the PET fibers containing MWNTs or PCS-MWNTs were analyzed by FESEM, therogravimetry, differential scanning calorimetry, cone and electronic tension meter method. The results showed that MWNTs were coated with PCS. Compared to PET fiber, when the content of PCS-MWNTs was 0.9 wt.%, the PCS-MWNTs/PET fibers exhibited an efficient flame-retardant capacity, with the lower heat release rate and total release rate values of 81.03 kW/m² and 39.05 MJ/m², respectively, decreasing by 130.06 kW/m² and 11.87 MJ/m². The thermal stability of PCS-MWNTs/PET fibers strengthened, and the char residue increased from 7.21 to 13.52%. Compared to MWNTs/PET fiber, the crystallization property and tensile strength of PCS-MWNTs/PET fiber improved, because of the good dispersion and strong interface binding force with the PET fiber. Overall, the PCS layer endowed the MWNTs with good dispersion and flame-retardant characteristics.     

Structures and flammability properties of polyethylene terephthalate(PET) fibers containing encapsulated carbon materials

In this paper, carbon nanotubes (CNTs) and carbon microspheres (CMSs) have been microencapsulated to obtain microencapsulated carbon nanotubes (MCNTs) and microencapsulated carbon microspheres (MCMSs). Moreover, a series of PET fibers with CNTs/CMSs or MCNTs/MCMSs were prepared by melt spinning. Morphologic structures, mechanical, thermal, and flame retardant properties of MCNTs/MCMSs /PET fibers have been studied by TEM, SEM, electronic tension meter, DSC, TG, limiting oxygen index (LOI), and vertical flammability instruments. The results show that the tensile strength of MCNTs/MCMSs/PET fibers are increased because of better dispersion and compatibility of MCNTs/MCMSs in PET and enhanced orientation degrees of fibers, compared with CNTs/CMSs/PET fibers. Moreover, the highest values of mechanical properties are observed with 0.4 wt% content. Meanwhile, the MCNTs/MCMSs/PET fibers have good thermal stabilities and their fabrics have higher LOI value of 25.3%, reaching B1 class of China standard GB 17591-2006. Overall, this method endowed the MCNTs/MCMSs/PET fibers with the good mechanical and flame-retardant properties.     

聚磷腈改性沸石咪唑酯骨架材料的制备及其在聚酯阻燃中的应用

为提高聚对苯二甲酸乙二醇酯(PET)的阻燃性能,以六水合硝酸锌和2-甲基咪唑制备沸石咪唑酯骨架材料(ZIF-8),之后用六氯环三磷腈和4,4 -二羟基二苯砜对ZIF-8进行表面修饰合成一种ZIF-8聚环三磷睛-共磺酰基双酰/(PZS)亚微米颗粒,并与PET通过熔融共混制备PET阻燃复合材料。借助热重分析仪、极限氧指数仪、垂直燃烧仪、万能材料试验机以及扫描电镜等对复合材料的热稳定性、阻燃抗熔滴性、力学性能以及阻燃机制进行分析。结果表明:添加6%的ZIF-8/PZS亚微米颗粒使PET的极限氧指数(LOI值)提高到29.2%,并通过UL-94 V-0等级,而复合材料的力学性能没有受到严重影响;ZIF-8/PZS可以在气相和凝聚相中同时发挥效用,从而赋予PET复合材料优异的阻燃性能。