新型膨胀阻燃剂及其在涂料中的应用

采用干法合成了季戊四醇磷酸酯三聚氰胺盐,并采用红外光谱（IR）、热重分析（TGA）对阻燃剂进行了表征,结果表明合成P-N膨胀阻燃剂具有双螺环磷酸酯结构,其热分解温度为200℃左右,扫描电镜（SEM）观察发现,燃烧后的阻燃剂发泡均匀,炭层结构稳定,炭层气泡孔径为100~200μm。将该阻燃剂用于超薄型钢结构防火涂料中,具有膨胀效果好,炭层粘结能力强,耐火时间长等优点。     

星状单分子磷氮膨胀型阻燃剂在防火涂料中的应用研究

将星状单分子磷氮膨胀型阻燃剂六(4-DOPO羟甲基苯氧基)环三磷腈(DOPOMPC)应用于防火涂料中,研究其与传统膨胀阻燃剂(AMP)的协同阻燃效果。结果显示:DOPOMPC阻燃剂使AMP膨胀阻燃体系的炭层膨胀倍数明显增加,耐燃时间延长;平均热释放速率(av-HRR)和热释放速率峰值(pk-HRR)较AMP阻燃体系降低了23.18%和25.36%,峰值推迟出现了75 s,总释放热(THR)下降了11.73%,一氧化碳释放率平均值(av-COY)增大了95.6%,平均比消光面积(avSEA)增加了39.44%;火势增长指数(FGI)和放热指数(THRI6 min)分别下降了39.5%和10.35%,发烟指数(TSPI6 min)和毒性气体生成速率指数(Tox PI6 min)分别增长了6.3%和28.6%。结果表明涂料很好地保护了基材,使其不易被点燃,炭层厚度的增加阻止了热量向基材传递,延长了点燃时间,火灾的危险性大幅降低,DOPOMPC阻燃剂与AMP膨胀阻燃体系之间存在显著协同阻燃作用;但DOPOMPC增大了涂料的烟气和毒性气体的生成量。     

阻燃剂在膨胀型防火涂料中的应用

根据阻燃剂的分类,阐述了各类阻燃剂的阻燃机理。评述了国内外几种阻燃性好的阻燃剂的应用。提出了膨胀型防火涂料中阻燃体系及阻燃剂的选用原则。     

水性防火涂料配方研究

介绍了水性防火涂料的机理,叙述了硅丙乳液膨胀型防火涂料研制过程中的材料选择及阻燃剂体系的配方优化,对该涂料的理化性能和防火性能进行了测定。实验结果表明:以硅丙乳液为成膜物质配制成的水性防火涂料理化性能优良,防火性能达到国家饰面型防火涂料一级标准。     

防火涂料

防火性好、燃烧时不释放有毒气体的带夹层的光纤绳,硅丙乳液膨胀型防火涂料,硅丙乳液膨胀型防火涂料的研制,用废聚苯乙烯泡沫研制木材用膨胀型阻燃涂料,     

硅丙乳液膨胀型防火涂料

叙述了硅丙乳液膨胀型防火涂料研制过程中的材料选择、工艺设计及配方优化,对该涂料的理化性能、技术指标等进行了全面讨论。     

硅丙乳液膨胀型防火涂料的研制

叙述了硅丙乳液膨胀型防火涂料研制过程中的材料选择、工艺设计及配方优化。对该涂料的理化性能、技术指标等进行了全面讨论。该防火涂料的特点是：不但防火性能好、不污染环境、适用范围广，而且装饰效果好，具有普通涂料的装饰水平。     

LL阻燃剂的加入对防火涂料性能的影响

在防火涂料中加入了LL阻燃剂后,通过采用小室燃烧试验法、产烟试验、热分析仪、电子显微镜等实验检测和分析结果为依据,指出使用LL复合阻燃剂是进一步提高防火涂料性能的途径之一.提出LL阻燃剂的加量在15%时,防火涂料既有很好的防火性能,又有优良的理化性能.     

超薄膨胀型硅丙乳液防火涂料的研究

以自合成硅丙乳液为基料,以聚磷酸铵、三聚氰胺和季戊四醇为阻燃剂体系,配制出膨胀型硅丙乳液防火涂料。实验比较了膨胀型硅丙乳液防火涂料与丙烯酸酯乳液防火涂料的耐火性,探索了涂层厚度对防火性能的影响,选择出具有优异防火性能的阻燃体系各组分的配合比例。     

无皂硅丙乳液的合成及其在建筑涂料中的应用

以甲基丙烯酸甲酯(MMA)、甲基丙烯酸(MAA)、乙烯基三甲氧基硅烷(YDH-171)、四甲基四乙烯基环硅氧烷(DV4)、烯丙基羟乙基醚(AOE)为原料,K2S2O8-Na2SO3为氧化还原引发体系,实施自乳化、开环同步进行的自由基无皂乳液聚合,合成了无皂硅丙乳液。通过L9(3)4正交实验优化的单体配比是:当体系p H值为4.5~5、K2S2O8与Na2SO3的质量比为2∶1且用量为单体总质量的0.5%时,MAA、AOE、YDH、DV4、MMA的质量比为8∶9∶4∶20∶59,此时聚合反应的凝胶率0.18%。红外光谱证实,DV4已开环且所有单体均已参与共聚反应;热重分析表明,无皂硅丙乳液的热稳定性好,最大热分解温度为449℃;粒度和透射电镜分析表明,乳胶粒平均粒径为158 nm,粒径分布窄(PDI=0.031,Zeta=-53.9 m V),具有单分散性;常规性能检测表明,乳液的各项指标均达到国标要求。将硅丙乳液与金红石型钛白粉及各种助剂混合,配成建筑内墙涂料,其涂层的主要性能指标达到或超过国家标准。     

磷酸盐阻燃液的制备及阻燃棉布的应用

室内常用装饰材料大多是由棉、木材等易燃物质制成,易引发火灾、造成人员伤亡和财产损失。因此,对室内常用装饰材料的燃烧性能进行研究是非常必要的。磷酸盐阻燃剂作为一种添加型阻燃剂,采用喷涂或浸渍等方式使棉布、木材等室内常用装饰材料获得较好的阻燃性能。本文采用磷酸氢二铵和磷酸二氢铵作为原料,分别按9:1、8:2、7:3、6:4、5:5、4:6、3:7、2:8、1:9共9种不同的质量比例混合配制磷酸盐阻燃液,并应用于棉布进行浸泡阻燃处理,然后对样品进行阻燃性能表征。实验结果表明,2:8比例的阻燃处理棉布点燃时间和达到峰值时间最长,阻燃效果最佳,目前的研究对于后续改进磷酸盐阻燃液的阻燃性能并分析影响其性能的因素具有重要意义。     

含磷/硅阻燃剂的研究进展

介绍了磷系阻燃剂、硅系阻燃剂与磷/硅阻燃剂的阻燃机理,综述了含磷/硅阻燃剂的研究现状与应用前景,展望了今后的发展趋势。     

一种新型含磷阻燃剂的合成

以邻苯基苯酚和三氯化磷为起始原料,路易斯酸为催化剂,合成了新型阻燃剂[(6 氧 6H 二苯并 (c,e)(1,2) 氧磷杂己环 6 酮) 甲基] 丁二酸(DDP),测定了DDP在丙酮 水混合体系中的溶解度。结果表明,质量百分数0.6的丙酮 水溶液是DDP重结晶较为合适的溶剂,为产品的纯化提供了基础数据。     

Synthesis of flame retardant polyester‐urethanes and their applications in nanoclay composites and coatings

This paper describes the synthesis of phosphorus‐containing polyester‐urethanes and their applications in nanoclay composites and coatings. Polyester was prepared by the reaction of bis(bisphenol‐A) monophenyl phosphonate, maleic anhydride and phthalic anhydride. The polyester was reacted with various diols such as ethylene glycol, diethylene glycol and propylene glycol to obtain polyester polyols. Synthesized polyester polyols were characterized by chemical analysis and instrumental analysis and was used further to react with different isocyanates to develop polyester‐urethanes. The synthesized polyester‐urethanes were blended with organo‐modified montmorillonite nanoclay (1 wt%, 3 wt% and 5 wt%) and were cast in a mold and coated on mild steel panels. The thermal stability of neat polyester‐urethane and the nanoclay composites was determined by thermogravimetric analysis. The flame retardant properties of cast films and their composites were determined by the limiting oxygen index and UL‐94 test methods. The physical and mechanical properties of coatings such as pot life, drying properties, scratch hardness, pencil hardness, impact resistance, adhesion and flexibility were investigated. The chemical resistance properties of the coatings were also determined in different reagents. The data reveal that the polyester‐urethane nanoclay composites with 3 wt% clay hold promise for use in effective flame retardant coatings. © 2013 Society of Chemical Industry     

茶皂素基膨胀型阻燃剂的制备及其在涂料中的应用

采用多羟基、多羧基的活性天然产物茶皂素为原料,与聚磷酸铵和季戊四醇在一定条件下反应,制备一种聚磷酸酯类茶皂素基三位一体新型环保膨胀型阻燃剂。采用傅里叶红外分析技术对阻燃剂进行了结构表征,采用综合热分析仪对阻燃剂的热降解性能进行了研究。结果表明,茶皂素与聚磷酸铵、季戊四醇发生反应,生成聚磷酸酯类茶皂素基膨胀型阻燃剂,且该阻燃剂具有良好的热稳定性,降解热释放较小,高温残留率高,最终的质量残留率高达30.77%。将制备阻燃剂用于阻燃涂料中,并采用氧指数测试仪和锥形量热仪研究了阻燃涂料的阻燃性能和热解性能。研究表明,茶皂素基三位一体膨胀型阻燃剂能显著提高涂料的阻燃性能,阻燃涂料的氧指数值高达34.2%,耐火时间为11.1 min,且锥形量热实验中,该阻燃涂料试样的平均热释放速率（m-HRR）为36.18 kW/m2,总热释放量（THR）为5.25 kJ/m2,平均有效燃烧热（m-EHC）为5.11 kJ/kg,与含复合型阻燃剂的阻燃涂料试样相比,阻燃性能得到极大提高。该制备阻燃剂不含卤素,集三源一体,具有阻燃性能优越,相容性能良好,高效环保等优点。     

磷系阻燃PET合成工艺探讨

采用共聚的方法,将阻燃元素磷引入到PET中,进行阻燃改性,生产环保型阻燃PET。介绍了该阻燃剂的阻燃机理。对研发过程中的合成工艺参数如酯化反应配料比,温度和压力,缩聚反应工艺参数进行了探讨。利用红外光谱对磷系阻燃PET的结构进行了表征。     

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.     

Preparation of a novel synergistic flame retardant and its application in silicone rubber composites

Dehydration condensation product (DHCP) was prepared by addition and dehydration condensation reactions of 9,10-dihydro-9-oxa-10-phenanthrene-10-oxide (DOPO), vinyl trimethoxysilane, and (3-aminopropyl) triethoxysilane. DHCP-PA with high phosphorus content was prepared by reaction between DHCP and phytic acid (PA). It was then compounded with oxidized multi-walled carbon nanotubes (OMWCNTs) to prepare silicone rubber (SR) flame retardant composites. The results showed that the SR with a small amount of DHCP-PA owned good flame retardant effect. The heat release rate (HRR) was decreased from 436 kW/m² for pure SR to 288 kW/m² for the SR with 5 phr DHCP-PA, and the decreasing degree was 33.9%. After mixing 5 phr DHCP-PA with 1 phr OMWCNTs, the HRR of SR composite was decreased from 436 to 251 kW/m², the smoke production rate was decreased from 0.161 to 0.087 m²/s, the limited oxygen index value was increased from 20.4% to 28.4%, and the flame retardant grade can reach UL94 V-0. In addition, the synergistic flame retardant mechanism was researched and analyzed.     

基于环三磷腈/磷酸酯反应型磷-氮阻燃剂的合成、热降解及应用

以六氯环三磷腈(HCCP)、对羟基苯甲醛及亚磷酸二乙酯等为原料,成功合成了一种反应型磷-氮膨胀阻燃剂六(4-磷酸二乙酯羟甲基苯氧基)环三磷腈(HPHPCP),HPHPCP结构经傅里叶红外光谱(FTIR)、核磁共振(NMR)证实。热失重(TG/DTG)表明HPHPCP具有较高的热稳定性及良好的成炭性,氮气氛下的起始分解温度为162.7℃,800℃时残炭量大于40%(质量分数);利用HPHPCP的羟基结构,应用于硬质聚氨酯泡沫塑料中,可以显著提高聚氨酯硬泡的阻燃性能,添加30%的HPHPCP就可以使聚氨酯氧指数达到27%。     

软膜型煤炭阻燃抑尘剂的微波合成及其应用

以环氧树脂E-51、丙烯酸丁酯(BA)、甲基丙烯酸(MAA)、苯乙烯(St)、植酸等为原料,K2S2O8和Na HSO3为引发剂,烷基酚醚磺基琥珀酸酯钠(MS-1)和辛基酚聚氧乙烯醚(OP-10)为乳化剂,在微波辅助下,合成了一种高分子阻燃抑尘剂乳液。采用FTIR、SEM、TGA等对产品进行了结构表征和应用性能测试。结果表明,在m(BA)∶m(St)=2∶1,引发剂用量为0.6%(以单体的总质量为基准,下同),乳化剂用量为6%,m(MS-1)∶m(OP-10)=2∶3,E-51用量为6%,植酸用量为2%,微波功率100 W,微波辐射时间90 min条件下,所合成的乳液稳定,粒径分布均匀,成膜柔软。喷洒阻燃抑尘剂的煤样相较于喷洒水的煤样的失水率、风蚀损失率、振荡损失率、CO质量浓度分别减小了47.7%、96.6%、96.0%、67.5%。