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用热分析方法得出,由芳香酸甲酯或乙酯与4,4’-二氨基二苯甲烷制备的铵盐的酰胺化,酰亚胺化反应,较芳香酸的铵盐更易进行,反应温度和表观活化能均比四酸铵盐时低。由铵盐生成的聚酰亚胺具有很好的热氧化稳定性。 相似文献
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裂解气相色谱-质谱法研究聚醚酰亚胺的热裂解行为 总被引:1,自引:0,他引:1
采用裂解气相色谱-质谱技术研究了聚醚酰亚胺(PEI)在550℃、650℃和750℃裂解温度下的热分解行为.随着裂解温度上升,裂解产物明显增加.在750℃时聚合物分子链断裂完全,共鉴别到25种碎片组分.PEI热分解的碎片中叔丁基苯酚、叔丁基甲基苯酚、苯酚、苯胺、氰苯、2-苯基-1H-异吲哚-1,3(2H)-二酮等5种裂解产物最重要,因此可以依据这几种化合物定性鉴别聚醚酰亚胺.依据热分解产物的数量以及结构推断降解机理为:裂解首先从醚键开始,其次是酰胺基团中的C-N键,然后再经过一系列消除反应、成环反应、重排反应等形成多种裂解碎片. 相似文献
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本文介绍了最近研制成功并用于材料热强度应变测量、耐热300℃、灵敏系数K>1.85和应变极限ε>8%,具有独特力学性能的耐高温高塑性(大)应变胶粘剂,以Ⅳ号胶为代表着重研究了这些溶液型共聚-共混聚酰胺酸在热酰亚胺化为最终产和过程中,各个阶段的特征及对性能的影响,结果发现,急剧酰亚胺化为最终产物过程中,各个阶段的物征及对性能的影响,结果发现,急剧酰亚胺化(155℃附近)之后,聚合物的Tg( >280℃)便已接近最大值,认为继续的酰亚胺化反应至安全(225℃附近)是在 玻璃态中进行的。文中确定了该胶粘剂呈现优良应变特性和粘结性的热-酰亚胺化温度是250-260℃。 相似文献
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采用裂解气相色谱一质谱法研究了在350~750℃之间聚苯硫醚(PPS)的裂解行为。350℃时裂解,仅检测到4种裂解产物。随裂解温度上升,裂解产物急剧增加。在750℃时,检测到25种裂解产物,主要特征裂解产物为硫化氢、苯、苯硫醇、1,4-苯二硫醇、二苯硫、二苯并噻吩、1,4-苯二硫醇基苯、噻茚等。聚苯硫醚裂解过程中,发生链剪切作用,由聚合物链断裂成苯硫醇单体、二聚体和三聚体等化合物。裂解过程还会发生重排,环化,次级反应等形成了各种裂解产物。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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