二季戊四醇磷酸酯三聚氰胺盐的合成及阻燃性能测试

以磷酸、季戊四醇、三聚氰胺为原料,通过酸醇直接酯化和烘焙中和两步反应合成膨胀型阻燃剂二季戊四醇磷酸酯三聚氰胺盐,并对烘焙中和反应条件及其在聚乙烯中的阻燃性能进行了研究.确定最佳合成条件:n (二季戊四醇磷酸酯):n (三聚氰胺)=1:1;反应温度130-140℃;反应时间3-4h.将此阻燃剂添加到聚乙烯中,样品重量35...     

二季戊四醇的定量分析

采用两种不同的方法即重量法和杂质减除法对自行研制的二季戊四醇(简称二季或双季,DPE)进行了定值.重量法测得二季戊四醇的含量为98.97%,SD为0.078%;杂质减除法测得二季戊四醇的含量为98.79%,SD为0.092%;并进行了不等精度数据分析;结果表明这两种方法测得的结果是一致的.     

高效液相色谱法测定季戊四醇和二季戊四醇

建立了分离测定季戊四醇和二季戊四醇的反相高效液相色谱法。在C18烷基键合相分离柱上,以乙腈∶水[5∶95(V/V)]为流动相,流速为1.0ml·min-1。紫外检测波长为196nm,方法的相对标准偏差季戊四醇和二季戊四醇分别为2.4%和4.5%。加标回收率分别为96.36%和95.78%。方法用于二季戊四醇生产工艺条件的选择和反应液浓度的控制分析。     

单丁基磷酸酯的合成与表征

本文报道用三氯氧磷酯化、水解方法制备单丁基磷酸酯，用红外、核磁共振，质谱等方法对其结构进行了分析与表征。     

蔗渣木聚糖磷酸酯的合成与表征

以蔗渣木聚糖为主要原料,正磷酸盐(NaH2PO4与Na2 HPO4)为酯化剂,尿素为催化剂,在湿法工艺下合成了蔗渣木聚糖磷酸酯.考察了酯化温度、酯化时间、蔗渣木聚糖与酯化剂和催化剂配比、pH等因素对取代度的影响,采用正交试验设计对合成条件进行优化,运用统计分析方法探讨了各因素影响的主次顺序和显著性,得到较佳的合成条件为...     

三苯基锡壳聚糖磷酸酯的合成、表征及其杀钉螺活性

用磷酸二氢钠和尿素在稀醋酸介质中对壳聚糖(CTS)进行磷酸化改性,得到壳聚糖磷酸酯(P-CTS),然后在85%的甲醇中与三苯基氯化锡发生亲核取代反应,合成出三苯基锡壳聚糖磷酸酯(P-CTS.SnPh3),通过红外光谱、核磁共振、热分析和粉末X-射线衍射等手段表征了这些化合物.用所得产品进行杀钉螺活性试验,结果显示,当其浓度在0.5mg/L以上时,浸杀3d后,钉螺的死亡率达100%.     

环戊甲基苯并咪唑衍生物的合成、表征及抑菌活性

环戊甲基苯并咪唑衍生物的合成、表征及抑菌活性;环戊甲基苯并咪唑衍生物;合成;微波辐射;抑菌活性     

S-四嗪类高氮含能化合物的合成及表征

传统的有机含能化合物生成焓普遍较低,一般为负值或接近于零,所释放的能量主要来源于生成CO2和H2O的放热过程。四嗪类化合物是近年来国外研究较多的一类高氮化合物,其化学潜能主要来源于其正生成焓;同时分子结构中的高氮、低碳、氢含量不仅使其成气量大、燃烧产物少烟或无烟,而     

新型双生磷酸酯表面活性剂的合成与表征

以三氯氧磷、二元醇和正十二醇为原料,通过酯化和水解反应合成了两种新型的双生磷酸酯表面活性剂——丁撑双十二烷基二磷酸酯和己撑双十二烷基二磷酸酯,其结构经^1HNMR,IR,MS和元素分析表征。     

新型不饱和聚磷酸酯的合成、表征及性能

通过溶液聚合制备了一种新型不饱和聚磷酸酯(Polymer Ⅰ), 经季铵化得到了侧基含季铵基的不饱和聚磷酸酯(PolymerⅡ). 对聚合物的结构和热性能进行了表征. 研究了PolymerⅡ与聚丁二酸丁二醇酯(PBS)的共混片基(Polymer Ⅱ的质量分数分别为5%, 10%和20%)在pH=7.4的磷酸缓冲溶液中的溶胀和降解性能. 结果表明, 以纯三甲胺为季铵化试剂, 在V(氯仿): V(异丙醇): V(DMF)=3: 5: 5的混合溶剂中, 于60℃反应24 h可得到季铵化率高达48%的PolymerⅡ. 在PBS中PolymerⅡ的含量越多, 达到溶胀平衡时, 共混片基的溶胀率越高, 越容易降解. 磷酸酯的引入使聚合物的熔点(T_m)和热稳定性(T_d)降低.     

微波辐射下润滑油类双季戊四醇六酯的合成

世界能源危机的出现,使合成润滑油的研究得到迅速发展。合成润滑油与矿物油相比,以其挥发性低、节省能耗、低温性能好、热氧化安定性好、使用寿命长等优点广泛用于军事、航空、机械等领域。随着高科技密集现代航空器的发展和环保要求的不断提高,国际上对润滑油的性能要求日益苛刻。合成酯类润滑油因其独特的高低温性能、粘温性能、润滑性能、无毒、可生物降解性能被广泛用作航空燃气涡轮发动机润滑油、仪表油、压缩机润滑剂的基础油,被称为环境友好的基础油。     

Effects of nanoparticles on the flame retardancy of the ammonium sulphamate‐dipentaerythritol flame‐retardant system in polyamide 6

This paper extends the work of Lewin et al., which showed that high levels of flame retardancy could be conferred on polyamide 6 (PA6) in the presence of small concentrations of ammonium sulphamate (AS) and dipentaerythritol (DP). PA6 samples were compounded with similarly low concentrations (2.5%w/w AS and 1%w/w DP) with or without nanoclays and fumed silica present at 1 and 2%w/w levels. Compounded samples were characterized by X‐ray diffraction, thermal analysis (differential thermal analysis/thermogravimetric analysis) and Fourier transform infrared. Flammability properties were measured by UL‐94, limiting oxygen index (LOI) and cone calorimetry test methods. All PA6 blended samples with or without nanoparticles were found to be V‐2 rated which differed from the results reported by Lewin et al. for similar samples where V‐0 ratings were obtained for clay‐free samples. LOI increases promoted by the inclusion of AS and DP alone were slightly reduced following the addition of all nanoparticles with the functionalized clays showing the largest effect. Introduction of silica, however, had the smallest effect in reducing LOI. Cone calorimetric results showed that while the presence of AS and DP raise peak heat release rate values with respect to PA6, addition of nanoparticles reduced values to below that for pure PA6. These reductions are dependent on nanoparticle concentration although differences between them, within experimental error, are very similar. While smoke generation is little affected by addition of AS and DP, the presence of nanoparticles promotes a slight increase. Results were interpreted in terms of previously published mechanisms for PA6‐AS‐DP thermal degradation and nanoparticle‐polymer interactions. Copyright © 2012 John Wiley & Sons, Ltd.     

双季戊四醇六丙烯酸酯的合成和表征

以双季戊四醇和丙烯酸为原料直接酯化合成了双季戊四醇六丙烯酸酯,考察了原料配比、溶剂用量、催化剂、阻聚剂用量、温度、脱色剂、反应时间等因素对反应的影响,得到了最佳反应条件,当双季戊四醇∶丙烯酸∶甲苯=1∶7.2∶3.77(物质的量之比),催化剂选用对甲苯磺酸,加入量为双季戊四醇质量的4%,采用复合阻聚剂,加入量为丙烯酸质量的4%,反应时间8 h,脱色剂TSJ-1用量为双季戊四醇用量的3%,产率较高可达75.0%,副反应少,产品色度较浅可达30号色.     

硫杂蒽酮的合成和表征

为了寻求合成硫杂蒽酮的高效新方法,以2,2′-二硫代二苯甲酸和苯酚为原料,硫酸为溶剂和催化剂,考察了沸石分子筛、Al2O3和P2O5、温度、原料的物质的量之比、反应时间对反应收率的影响,确定了最佳反应条件,推测了可能的反应过程;进而以2,2′-二硫代二苯甲酸和相应的苯衍生物为原料,在H2SO4-P2O5体系中于最佳反应条件下制备了13个硫杂蒽酮类化合物,并利用柱色谱分离以及红外光谱与核磁共振谱对产物进行表征.结果表明,在反应体系中引入P2O5有利于促进反应的完成;最佳反应条件为:温度70℃、2,2′-二硫代二苯甲酸/苯衍生物物质的量之比1∶6、反应时间6h.邻苯二酚与二硫代水杨酸的反应产物——化合物11(a)和11(b)为同分异构体.     

双Schiff碱过渡金属配合物的合成及对环己烯催化氧化性能的研究

Schiff碱及其配合物在治疗肿瘤、抗菌、仿生载氧等方面具有优异的性能,在催化领域中也表现出多种性质。本文合成了三种结构简单的Schiff碱配体以及它们的过渡金属配合物,并研究了其对环己烯的催化环氧化性能。配体的结构如下。     

Synthesis, application and flame retardancy mechanism of a novel flame retardant containing silicon and caged bicyclic phosphate for polyamide 6

A novel flame retardant containing silicon and caged bicyclic phosphate groups, tri(2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane-1-oxo-4-hydroxymethyl) phenylsilane (TPPSi) was successfully synthesized. The chemical structure of TPPSi was characterized by FTIR, ¹H NMR and ³¹P NMR. The application of TPPSi (25 wt%) as a flame retardant in polyamide 6 (PA6) not only gains satisfied flame retardancy and smoke suppression, but also retains the high toughness and inherent appearance of pure PA6. The influence of TPPSi on the decomposition pathway of PA6 was discussed based on TG-FTIR and FTIR analysis. The interaction between TPPSi and PA6 at high temperature alters the decomposition pathway of PA6 resulting in the formation of the residue containing phosphorus and silicon. The heat and smoke release behaviors at different external heat fluxes were measured by cone calorimeter, and the fire residue was analyzed by SEM-EDX. The condensed phase action resulting from the barrier effect of residue is proposed to be the major flame retardancy mechanism of TPPSi in PA6, with the fuel reduction action as the minor.     

Synthesis, characterization, thermal properties and flame retardancy of a novel nonflammable phosphazene-based epoxy resin

Hexakis(4-hydroxyphenoxy)-cyclotriphosphazene (PN-OH) was synthesized through nucleophilic substitution of the chloride atoms of hexachlorocyclotriphosphazene and reduction of the aldehyde groups, and its chemical structure was characterized by elemental analysis, ¹H and ³¹P NMR, and Fourier transform infrared (FTIR) spectroscopy. A new phosphazene-based epoxy resin (PN-EP) was successfully synthesized through the reaction between diglycidyl ether of bisphenol-A (DGEBA) and PN-OH, and its chemical structure was confirmed by FTIR and gel permeation chromatography. Four PN-EP thermosets were obtained by curing with 4,4′-diaminodiphenylmethane (DDM), dicyandiamide (DICY), novolak and pyromellitic dianhydride (PMDA). The reactivity of PN-EP with the four curing agents presents an increase in the order of DDM, PMDA, novolak and DICY. An investigation on their thermal properties shows that the PN-EP thermosets achieve higher glass-transition and decomposition temperatures in comparison with the corresponding DGEBA ones while their char yields increase significantly. The PN-EP thermosets also exhibit excellent flame retardancy. The thermosets with novolak, DICY and PMDA achieve the LOI values above 30 and flammability rating of UL94 V-0, whereas the one with DDM reaches the V-1 rating. The nonflammable halogen-free epoxy resin synthesized in this study has potential applications in electric and electronic fields in consideration of the environment and human health.     

Thermal stability and flame retardancy of novel phloroglucinol based organo phosphorus compound

A series of organo phosphorus flame retardants (FR) based on cyclic phosphates were synthesized in an attempt to find an efficient FR for polycarbonate (PC) and acrylonitrile-butadiene-styrene copolymer (ABS). The success of synthesis was confirmed by FT-IR and ¹H and ³¹P NMR. Their thermal stability and flame-retarding efficiency as a single component additive were investigated and compared with those of aromatic based phosphate, resorcinol bis(diphenyl phosphate) (RDP). Thermogravimetric analysis (TGA) results reveal that cyclic phosphates synthesized in this study show more than one-step degradation and act in the condensed phase mechanism rather than in the vapor phase mechanism. Flame-retarding efficiency was evaluated by UL-94 test method. V-0 rating was achieved at 3-5 wt% of FR loading for PC, which is better than the FR performance of RDP. The high P-OH generation tendency is responsible for the better FR performances of these compounds. The degradation path is also discussed.