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3,3-双叠氮甲基氧丁环及其均聚物的合成与性能 总被引:15,自引:5,他引:10
以1,1,1-三溴甲基-1-羟甲基甲烷为原料,无水乙醇为溶剂,在NaOH的作用下经关环反应合成了3,3-二溴甲基氧丁环(BBMO)。BBMO经叠氮基取代反应制备出3,3-二叠氮甲基氧丁环(BAMO)。BAMO单体经阳离子开环聚合即可制备出固态含能黏合剂PBAMO。用核磁、红外、DSC和GPC表征了聚合物的结构,测试了PBAMO的理化性质。结果表明,PBAMO具有感度较低.熔融温度适中,熔融黏度较低等特点,可以作为含能热塑性弹性体的硬段成分。 相似文献
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3-叠氮甲基-3-乙基氧杂环丁烷及其均聚物的合成与性能 总被引:7,自引:2,他引:5
为开发新型含能黏合剂,以三羟甲基丙烷、碳酸二乙酯、对甲苯磺酰氯、叠氮化钠为原料,合成出一种新型叠氮类氧杂环单体3-叠氮甲基-3-乙基氧杂环丁烷(AMEO)。用核磁、红外、元素分析和DSC表征了AMEO的结构与性能。以1,4-丁二醇为起始剂,三氟化硼乙醚络合物为催化剂,二氯甲烷为溶剂,AMMO为单体,借助于阳离子开环聚合,合成出聚3-叠氮甲基-3-乙基氧杂环丁烷(PAMEO)。用红外光谱、核磁共振、元素分析、羟值、数均分子质量表征和测定了聚合物的结构和性能。 相似文献
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3-硝酸酯甲基-3-甲基氧杂环丁烷的合成及表征 总被引:7,自引:4,他引:3
为发展硝酸酯聚醚黏结剂,以3-羟甲基-3-甲基氧杂环丁烷(HMMO)为底物,N2O5为硝化剂,制备了一种含能单体3-硝酸酯甲基-3甲基氧杂环丁烷(NIMMO)。讨论了N2O5与HMMO的摩尔比及反应温度对选择性硝化的影响。确定了最佳反应条件:N2O5与HMMO的摩尔比为(1.0~1.1):1.0,温度为-15~-10℃,滴加完毕后待温度下降时立即中和终止反应。通过红外、核磁及元素分析对产品进行结构表征,表明是目标化合物,差热分析表明NIMMO的热稳定性较好。 相似文献
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3-叠氮甲基-3-甲基氧杂环丁烷与四氢呋喃共聚醚的合成与表征 总被引:2,自引:0,他引:2
以1,4-丁二醇(BDO)为引发剂,三氟化硼·乙醚(BF3·Et2O)为催化剂,使3-叠氮甲基-3-甲基氧杂环丁烷(AMMO)与四氢呋喃进行本体法阳离子开环聚合,得到3-叠氮甲基-3-甲基氧杂环丁烷与四氢呋喃的共聚醚(PAT).通过红外光谱、核磁共振氢谱、碳谱和凝胶渗透色谱对共聚醚进行表征.结果表明,合成的共聚醚中两种不同结构单元的摩尔比与投料比基本吻合,共聚醚的相对分子质量可控、分布较窄.差热扫描量热法测得PAT的玻璃化转变温度为-59.2℃,分解峰温为264.1℃,表明其具有良好的低温性能和热稳定性. 相似文献
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用聚乙二醇(PEG)作标准样建立了凝胶渗透色谱(GPC)试验法,测定了3-叠氮甲基-3-甲基氧丁环均聚物(PAMMO)的相对分子质量及其分布。研究了柱温和样品浓度对测试结果的影响,测试了不同批次样品的相对分子质量,比较了GPC试验法与凝胶渗透色谱-十八角度激光散射仪联用(GPC-MALLS)法、蒸汽压渗透(VPO)法和羟端基滴定法所得结果。结果表明,GPC试验法的重复性良好,数均分子量(Mn)、重均分子量(Mw)和分子量分布指数(PD)的相对标准偏差(RSD)均小于5%,显示传统GPC试验法可用于测定PAMMO的相对分子质量及其分布,对PAMMO合成工艺的改进和后处理方法的选择具有参考价值。 相似文献
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3,3′‐Bisazidomethyl oxetane‐3‐azidomethyl‐3′‐methyl oxetane (BAMO‐AMMO) tri‐block copolymer was successfully synthesized by azidation of a polymeric substrate containing bromo leaving groups, and an alternative block energetic thermoplastic elastomer (ETPE) was prepared by chain extension reaction. The tri‐block copolymer was characterized by Fourier transform infrared (FTIR), 1H NMR, and 13C NMR spectroscopy, X‐ray diffraction (XRD), and thermogravimetric analysis (TGA). It was found that the composition of the copolymer is nearly 1 : 1; crystallinity of the copolymer (71.81 %) is less than that of PBAMO (78.30 %). This is due to a partly mixture between soft and hard segments. Kinetic result shows that a crosslinking network is formed after the decomposition of azide group. Tensile strength of alternative block ETPE is 150 % of traditionally synthesized BAMO‐AMMO ETPE. 相似文献
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The thermal decomposition process and combustion wave structure of azide polymer were studied to determine the parameters which control the burning rate. The azide polymer studied was 3-azidomethyl-3-methyl oxetane (AMMO) which contains energetic –N3 groups. From the experiments, it was found that the thermal decomposition process of AMMO consists of a two-stage weight loss process: the first-stage corresponds to an exothermic reaction which is caused by the scission of N-N2 bond, and the second-stage corresponds to the decomposition of the remaining fragments. The burning rate of AMMO is approximately 50% of the burning rate of GAP propellant and is as high as that of conventional double base propellant. The heat feedback from gas phase to the burning surface increase with increasing pressure. The burning surface temperature and the heat of reaction at the surface decrease with increasing pressure. 相似文献
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Vladimir A. Petrov Nina V. Kuznetsova Timur I. Muhametshin Aydar T. Gubaydullin 《Propellants, Explosives, Pyrotechnics》2014,39(4):545-549
Polyurethane copolymers of 3,3‐bis (azidomethyl) oxetane (BAMO) and 3‐azidomethyl‐3‐methyloxetane (AMMO) with molecular structures of types B(AB)n, A(AB)n, (BB)n and ABn with different ratios of oligomeric units were investigated, where A is the non‐crystallizable “soft” block of oligoAMMO and B is the “hard” block of oligoBAMO and the included urethane diol fragments. The amorphous‐crystalline structures of copolymers BAMO and AMMO were elucidated by wide angle X‐ray diffraction measurements. The influences of the molecular structure and the ratio of oligomeric units on the structural parameters were identified. The degree of crystallinity is in a range from 8 to 22 % and sizes of the crystallites were determined. The defectivenesses of first and second kind in the structure were evaluated, which show high values of the first kind defectiveness (approx. 20 %), which describes the displacement of theoretical lattice sites and the existence of unequal sizes of the lattice sites, and minor values for the second kind defectiveness (approx. 3 %), which describes the lattice site disorder in large distances. Small‐angle X‐ray diffraction measurements were used to investigate the domain structures of copolymers BAMO and AMMO. The distribution and sizes of the crystallites in the structures of the copolymers were calculated. 相似文献
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Energetic thermoplastic elastomers containing energetic groups, such as azido, nitrato, nitro, and so forth, are emerging as attractive binder systems for advanced solid rocket propellants. Poly[3,3‐bis(Azidomethyl) oxetane (BAMO)‐co‐3‐azidomethyl‐3‐methyl oxetane (AMMO)] comprising hard crystalline BAMO segment and the soft/amorphous AMMO segment in various molar ratios (80 : 20, 50 : 50 and 20 : 80) were synthesized during the present work. The homo polymers namely Poly‐BAMO and Poly‐AMMO were also synthesized. All the polymers and copolymers were characterized by spectral and thermal methods. They were found to be thermally stable. The most promising 80 : 20 copolymer softened at 56°C with Tg of −36°C. Rheological studies were also carried out to determine their suitability as a binder in explosive and propellant formulations. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 相似文献
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E. A. Murphy T. Ntozakhe C. J. Murphy J. J. Fay L. H. Sperling G. E. Manser 《应用聚合物科学杂志》1989,37(1):267-281
The homopolymers, poly(3,3-bisethoxymethyl oxetane) (polyBEMO), poly(3,3-bisazidomethyl oxetane) (polyBAMO), and triblock copolymers based on these homopolymers and a statistical copolymer center block composed of BAMO and 3-azidomethyl-3-methyl oxetane AMMO were synthesized and characterized by differential scanning calorimetry, modulus-temperature, optical microscopy, membrane osmometry, and solution and melt viscosity. The values of K and a for the Mark-Houwink equation were found to be 7.29 × 10?3 mL/g and 0.80, respectively, for polyBEMO at 25°C using number-average molecular weights. Glass transition temperatures were in the range ?25 to ?40°C and melting temperatures were between 65 and 90°C for all polymers. The melting temperature was found to increase as expected with molecular weight. Melt viscosities of triblock copolymers with polyBAMO end blocks were at least an order of magnitude lower than those with polyBEMO end blocks and clear optically, suggesting that the polyBAMO-based triblock copolymers formed one phase in the melt, while the polyBEMO-based triblock materials (milk white) phase separated. The addition of filler raised the melt viscosity to a level between that predicted by the Guth-Smallwood and the Mooney equations. 相似文献
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在无溶剂、无催化剂、微波辐射条件下,取代吲哚-3-甲醛与3-甲基-1-苯基-5-吡哇啉酮通过固相Knoevenagel缩合反应合成了一系列4-(取代吲哚基-3-次甲基)-3-甲基-1-苯基-5-吡唑啉酮,产物结构经IR,1H NMR确证.最佳反应条件为:n(吲哚-3-甲醛):n(3-甲基-1-苯基-5-吡哇啉酮)=1.... 相似文献
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顾艳霞 《化学工业与工程技术》2008,29(4):20-23
以3-乙基-3-羟甲基环氧丁烷为单体,BF1·O(C2H5)2为引发剂,二氯甲烷为溶剂,在-50~30℃的不同温度下通过阳离子自缩合开环聚合,合成超支化聚3-乙基-3-羟甲基环氧丁烷,产物相对分子质量在5000左右。^13C NMR测定结果表明,聚3-乙基-3-羟甲基环氧丁烷的支化度随聚合温度的升高而增大,聚合温度在20℃以上时聚合物支化度随反应温度的变化趋势变小,趋向不变。 相似文献
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A comparison of triazole cross‐linked polymers based on poly‐AMMO and GAP: Mechanical properties and curing kinetics 下载免费PDF全文
Triazole cross‐linked polymers based on poly(3‐azidomethyl‐3‐methyl oxetane) (poly‐AMMO) and glycidyl azide polymer (GAP) were prepared using bis‐propargyl‐1,4‐cyclohexyl‐dicarboxylate (BPHA) as curing agent, respectively. Swelling tests demonstrated that cross‐linking densities of the resulted polymers both increased with the increase of BPHA. Triazole cross‐linked polymers based on poly‐AMMO showed superior tensile strength and elongation at break than those of GAP at comparable stoichiometry. The curing kinetics was also investigated by FTIR, and GAP exhibited faster reaction rate when reacted with BPHA than that of poly‐AMMO. In addition, with the increase of cross‐linking density, the glass transition temperature (Tg) of as‐prepared polymers significantly increased, and poly‐AMMO‐based polymers showed stronger Tg‐raising effect than GAP‐based polymers. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43341. 相似文献
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Poly(3,3‐bisazidomethyl oxetane/3‐azidomethyl‐3‐methyl oxetane) energetic thermoplastic elastomers (P(BAMO/AMMO) ETPEs) is one of the most valuable ETPEs in the field of energetic binders. P(BAMO/AMMO) ETPEs were prepared using different diisocyanates (TDI, HMDI, IPDI, and HDI) to investigate the influence of the diisocyanate on the performance of P(BAMO/AMMO) ETPEs. Mechanical properties and heats of formation were investigated. FT‐IR spectroscopy results showed that TDI‐based ETPE has the highest degree of hydrogen bonding with a value of 69.00 %. Mechanical test results showed that the TDI‐based ETPE has better mechanical property with maximum stress at 5.24 MPa and breaking elongation at 390 %. The order for degree of hydrogen bonding and mechanical property of different diisocyanate‐based ETPEs was TDI>HMDI>IPDI>HDI. The heats of formation were calculated by the group additivity method and by the heat of combustion method. The values of heats of formation for TDI‐based ETPE were 3.44 kJ g−1 and 3.75 kJ g−1 according to the two methods. Additionally, TDI‐based ETPE has a lager heat of formation than the other ETPEs. 相似文献