高分子消焰剂聚(N-丙烯酰基-甘氨酸钾)的合成及表征

用丙烯酰氯和甘氨酸在KOH浓溶液条件下反应合成了聚(N-丙烯酰基-甘氨酸钾)。通过四苯硼酸钠间接滴定法测定了聚合物中钾离子的含量,并测定了相对分子质量(Mr)、吸湿率等性能。结果表明,该聚合物同时含有消焰元素K和消焰基团NH,且该聚合物中钾离子质量分数较高,可达到23.19%,Mr适中,有抗迁移性,在抗吸湿性方面优于传统的小分子钾盐,可用作发射药的高分子消焰剂。     

5-(N-取代氨基)磺酰基-1-萘胺的合成

以5-氨基-1-荼磺酸为起始原料合成厂10个5-（N-取代氨基）磺酰基-1-萘胺化合物，其结构经质谱、红外光谱确证。     

N-丙烯酰基吗啉的制备及表征

以丙烯酸、氯化试剂和吗啉为原料,东乙胺作缚酸剂,丙酮为反应溶剂,制备N-丙烯酰基吗啉。优化反应条件:反应料比为n(丙烯酰氯):n(三乙胺):n(吗啉)=1:1:1.05,反应温度0～5℃,反应时间6h。N-丙烯酰基吗啉收率为80.5%(以丙烯酰氯计),气相色谱(GC)纯度大于99.0%。对最终产物进行了傅里叶红外光谱(FT-IR)及质谱(MS)表征。     

聚N-丙烯酰基甘氨酸水凝胶的合成及溶胀性能

以N-丙烯酰基甘氨酸（Acgly）为单体、过硫酸铵（APS）为引发剂、亚甲基双丙烯酰胺（MBA）为交联剂,通过溶液自由基聚合得到含有不同交联剂用量的水凝胶,并进行红外光谱表征．实验中对合成的水凝胶在不同pH条件下的平衡溶胀比和溶胀收缩可逆性进行测试．结果表明：随着交联剂质量分数从0.5％增大至7％,水凝胶外观由无色透明变为白色不透明,同时水凝胶由软变硬,弹性变小,硬度增加;在2．8〈pH〈3．8范围内水凝胶的平衡溶胀比随溶液的pH增大迅速增大,水凝胶表现出较好的pH敏感性;在pH=1．0和pH=6．8条件下的水凝胶具有很好的收缩溶胀可逆性．     

5-(N-桂皮酰基)氨基水杨酸的合成

目的：合成5-（N-桂皮酰基）氨基水杨酸。方法：以桂皮酸为原料,经酰氯化后与5-氨基水杨酸成酰胺修饰后合成目标物。结果与结论：合成得到了5-（N-桂皮酰基）氨基水杨酸,目标化合物通过IR、1HNMR和MS等确证,产率为61.8%。     

7-羟基-2-(N-丙基-N-丙酰基)氨基四氢萘满的合成

简单化合物2,7-二羟基萘经过羟基保护、金属钠还原、加成、酰化、去保护反应,得到了标题化合物.目标化合物经元素分析、核磁共振氢谱、质谱确证其化学结构.本方法原料易得、反应条件温和、操作简单.     

N-丙烯酰基邻苯二甲酰亚胺的合成研究

以丙烯酰氯和邻苯二甲酰亚胺钾盐为原料,丙酮为溶剂,合成N-丙烯酰基邻苯二甲酰亚胺。考察了反应原料配比、反应温度和反应时间对反应产率的影响。结果表明,优化反应条件为:n(丙烯酰氯)∶n(邻苯二甲酰亚胺钾盐)=4∶1,在28℃下反应8 h,N-丙烯酰基邻苯二甲酰亚胺的产率为54%。     

三（5-氨基四唑）三嗪的合成与表征研究

以5-氨基四唑和2,4,6-三氯-1,3,5-三嗪为起始原料,反应合成三（5-氨基四唑）三嗪。采用红外、核磁、元素分析、质谱等进行了表征。该化合物的含氮量高达77%。通过DSC研究分析,其分解温度高达296.6℃,具有对热稳定的性质。     

新试剂4-(α-呋喃丙烯酰基)-PMP的合成与表征

以α-呋喃甲醛为原料经呋喃丙烯酸及其酰氯,合成了新试剂1-苯基-3-甲基-4-(α-呋喃丙烯酰基)-吡唑啉-5-酮[4-(α-呋喃丙烯酰基)-PMP]。通过元素分析,红外光谱、紫外光谱和核磁共振氢谱、碳谱等对新试剂的分子结构进行了确定与表征,同时通过紫外吸收光谱对其互变异构现象进行了研究。     

N-马来酰基-氨基丙酸丁酯均聚和共聚反应的研究I单体N-马来酰基-氨基丙酸丁酯的合成

:以马来酸酐 (MA)、氨基丙酸 (Aln)、丁醇为原料用三步二釜法合成了N -马来酰基 -D ,L -氨基丙酸丁酯(BAM ) ,产率达 58%。并用PERKIN -ELMERFTIR - 1710红外光谱仪PE - 2 4 0 0有机元素分析仪对产品进行了检测。与传统方法相比 ,缩短了合成时间 ,节省了大量的溶剂 ,降低了成本 ,提高了产率。     

功能化聚六亚甲基盐酸胍的合成与表征

将带有胍基抗菌官能团的聚六亚甲基盐酸胍(PHGC)与甲基丙烯酸环氧丙酯(GMA)反应,制备了含碳碳双键官能团的功能化聚六亚甲基盐酸胍。利用紫外分光光度法测定了反应转化率,并考察了溶剂、反应物配比、反应时间及温度对反应转化率的影响规律。采用FT-IR、Raman、NMR和TG对功能化聚六亚甲基盐酸胍的组成、结构和热稳定性进行了表征。结果表明,在DMSO溶剂中,当GMA与PHGC摩尔比为1:1,在60℃下反应60 h后,反应转化率可达75%,且合成的功能化聚六亚甲基盐酸胍具有良好的热稳定性。功能化聚六亚甲基盐酸胍可用作大分子单体,与其他单体共聚制备具有抗菌性能的聚合物和微球。     

可生物降解聚苹果酸丁二醇酯弹性体的制备及表征

以苹果酸和1,4-丁二醇为单体通过熔融缩聚制备出来了一种新型的可生物降解弹性体材料——聚苹果酸丁二醇酯（PBM）,初步研究了材料的亲水性能和降解性能,并对材料的结构进行了初步表征。研究结果表明：PBM的聚集态结构为无定形态,透明柔软,玻璃化转变温度在0℃以下;通过调节合成单体的物质的量比,改变预聚物的后期固化时间,控制后期固化交联（反应）时间等手段,实现了降解性能可控,吸水率可调节的目标。     

Synthesis and characterization of poly(oxyethylene)–poly(caprolactone) multiblock copolymers

Novel poly(oxyethylene)/poly(caprolactone) POE/PCL copolymers were synthesized by step growth polymerization of poly(ε-caprolactone) diols and poly(ethylene glycol) diacids using dicyclohexylcarbodiimide as coupling agent. The reaction was performed at room temperature and yielded multiblock copolymers with predetermined POE and PCL block lengths. The resulting copolymers were characterized by various analytical techniques including SEC, IR, ¹H NMR, DSC and X-ray diffractometry. Data showed that the properties of these polymers can be modulated by adjusting the chain lengths of the macromonomers. In particular, one or two crystalline structures can exist within the copolymers of various crystallinities. © 1998 SCI.     

Preparation and characterization of double-layered microencapsulated red phosphorus and its flame retardance in poly(lactic acid)

A novel double-layered microencapsulated red phosphorus (DMRP) has been prepared through chemical precipitation of aluminum trihydrate (ATH) and in situ polymerization of melamine formaldehyde (MF) resin on the red phosphorus (RP) powder surface, and its structure was characterized by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The influence of DMRP on flame retardance and thermal stability of poly(lactic acid) (PLA) was thoroughly investigated by means of X-ray diffractometry (XRD), limiting oxygen index (LOI), vertical burning test, and thermogravimetric analysis (TGA). With an optimum mass ratio of RP/ATH/MF = 72.25%/12.75%/15%, it has been found that PLA with the addition of DMRP at 25 wt % loading level shows good flame retardance compared to plain RP as well as the conventional microencapsulated red phosphorus (CMRP), and can achieve UL94 V-0 rating along with an LOI increase from 20.5 to 29.3. The TGA and XRD studies indicate that the interaction occurs among all three components: RP, ATH, and MF resin. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Application of metallic phytates to poly(vinyl chloride) as efficient biobased phosphorous flame retardants

Simple, direct precipitation was used to synthesize green, renewable, biobased flame retardants. Copper phytate (Cu–Phyt), zinc phytate, aluminum phytate, and tin phytate (Sn–Phyt) were synthesized. Thermogravimetric analysis performed in N₂ revealed that the metallic phytate (M–Phyt, where M is Cu, Zn, Al, or Sn) salts showed good charring. The limiting oxygen index (LOI), cone calorimetry (CONE) test data, tensile strength, and impact toughness were measured for flexible poly(vinyl chloride) (PVC) containing 15 wt % M–Phyt salts. The PVC/Sn–Phyt LOI rose from 24.9 to 30.3%, and the PVC/Sn–Phyt mechanical properties were on par with those of the pure PVC. The CONE test results indicate that PVC/Cu–Phyt showed the lowest total smoke production (TSP) and peak heat‐release rate (pHRR) among the samples. The TSP and pHRR of PVC/Cu–Phyt were 15.77 m² and 181.77 kW/m², respectively, 62.63 and 44.48% lower than those of the neat PVC. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46601.     

聚氨基环磷腈的合成及其在PVA纤维中的应用

将六氯环三磷腈进行氨基取代,高温自聚得到不溶于水的聚氨基环磷腈(PHACTPA);PHACTPA通过粉末化后与聚乙烯醇(PVA)溶液共混纺丝得到阻燃PVA纤维。结果表明:PHACTPA在湿热条件下不稳定,但其干热稳定性好,在400℃高温氮气环境下稳定而不分解。PHACTPA在纤维中的质量分数小于22．5％时,对纤维的强度影响不大;含PHACTPA质量分数为15％的阻燃PVA纤维极限氧指数可达40％。     

Tin dioxide coated calcium carbonate as flame retardant for semirigid poly(vinyl chloride)

The flame retardant and smoke suppressant properties of semirigid PVC treated with calcium carbonate (CaCO₃), tin oxide (SnO₂), the mixture of CaCO₃/SnO₂ and SnO₂‐coated CaCO₃ have been studied through the limiting oxygen index, char yield, and smoke density rating (SDR) methods. The thermal degradation in air of the treated semirigid PVC was studied by thermogravimetry (TG) and differential thermal analysis (DTA) from ambient temperature to 1073 K. The morphologies of the additives and the char formation were studied through SEM. The mechanical property was also studied. The results showed that the semirigid PVC treated with SnO₂‐coated CaCO₃ has a higher limiting oxygen index and char yield, lower SDR and MSDR, a more compact structure of char formation than the semirigid PVC without flame retardant and the semirigid PVC with the equivalent CaCO₃, or SnO₂, or the mixture of CaCO₃/SnO₂, a similar tensile property and greatly improved impact strength compared with that of the semirigid PVC without flame retardant. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 731–738, 2006     

Synthesis and characterization of poly(pyridylurea) and poly(pyridylthiourea), potentially semiconducting polymers

Poly(pyridylureas) and poly(pyridylthioureas) were synthesized by reacting 2,6‐diaminopyridine with phosgene and thiophosgene, respectively, using THF and pyridine as solvent. The synthesized polymers were characterized by IR‐spectroscopy, elemental analysis, and X‐ray photoelectron spectroscopy. Thermal stability of the polymers was determined by thermal degradation between 35°C and 700°C. The 50% weight loss of polypyridylureas was above 400°C while for the polypyridylthioureas it was above 450°C. Undoped poly(pyridylureas) and poly(pyridylthioureas) behave as semiconductors, σ = 10^?9 (Ω cm)^?1. After doping with I₂ and SbF₅, the electrical conductivity increases several orders of magnitude, σ = 10^?7(Ω cm)^?1. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Synergistic flame retardant effect of poly(ether sulfones) and polysiloxane on polycarbonate

Flame retardance of bisphenol A polycarbonate (PC) was improved by the co‐addition of poly (ether sulfones) (PES) and polysiloxane/acrylate copolymer (PSiA) while retaining a high rigidity and toughness. A UL 94 V‐0 rating for 1.6‐mm thick samples of PC/PES/PSiA blend with 10.0 wt % PES and 0.5 wt % PSiA (PC/10PES/0.5PSiA) was obtained. Its average heat release rate (av‐HRR) in a cone calorimeter measurement was decreased by 19% on the basis of PC/PES blend with 10.0 wt % PES. Scanning electron microscopy (SEM) morphologies of impact‐fractured surfaces revealed that the incorporation of 0.5 wt % PSiA decreased the dimensions of PES dispersed phase and provoked the uniform distribution of PES in PC matrix. Thermogravimetric‐Fourier transform infrared spectroscopy analysis results revealed that PSiA dominantly promoted the degradation of PC and the degraded products were combined with PES to form a superior flame‐retarded carbon layer. A higher sulfur and silicon content on the residue surface after vertical burning tests detected by SEM/energy dispersive spectrometer signified their accumulation during combustion. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011