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双缩合螺吡喃的合成与光谱性能 总被引:1,自引:0,他引:1
利用过量Fischer碱与3,5-二溴水杨醛反应合成了4-(2-亚甲基-1,3,3-三甲基吲哚啉-2′-基)-6,8-二溴-1,3′,3′-三甲基-螺[3,4-二氢-2H-1-苯并吡喃-2,2′-吲哚啉],经元素分析、红外光谱、核磁共振氢谱和熔点确认了其化学结构.利用紫外-可见光谱和荧光光谱对目标化合物的吸收光谱和光致发光光谱进行了研究,探索了目标产物的光致变色 性能.结果表明,该化合物较相应单缩合螺吡喃多了1个吲哚单元且熔点提高了50℃,其紫外-可见吸收光谱中开环体在 555nm处有最大吸收波长,荧光光谱中在433nm处可观察到荧光. 相似文献
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1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷的合成 总被引:1,自引:0,他引:1
以硝基甲烷为原料合成了1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷,总收率为37.8%。采用1HNMR﹑IR和MS对目标产物及中间体的结构进行了表征。在三羟甲基硝基甲烷的合成中,结合反应机理确定了氢氧化钙的用量为:n(CH3NO2)n(Ca(OH)2)=1001;通过对催化剂浓硫酸﹑三氟化硼—乙醚络合物和对甲苯磺酸的比较,得出对甲苯磺酸为中间体2,2-二甲基-5-羟甲基-5-硝基-1,3-二氧杂环己烷合成的较优催化剂;分别采用2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硝酸酯和2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四对甲苯磺酸酯与NaN3反应,发现磺酸酯基易离去,叠氮化反应更易进行,收率较高;叠氮化反应的较优溶剂为DMSO。DSC分析表明,1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷的分解峰温为223.46℃。 相似文献
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用对硝基氯苯一步缩合法合成4,4’-二硝基二苯醚(DNDPE),研究了反应温度、原料配比(包括对硝基氯苯与碳酸钠、亚硝酸钠的摩尔比)、反应时间、溶剂量对DNDPE收率的影响,并用HPLC对目的产物进行分析。结果表明:DNDPE的较佳合成工艺条件为反应温度150℃,n(碳酸钠)∶n(对硝基氯苯)=0.7,n(亚硝酸钠)∶n(对硝基氯苯)=0.8,反应时间7h,n(DMF)∶n(对硝基氯苯)=5,溶剂回收循环利用可行。在该条件下,DNDPE收率可达77.3%。 相似文献
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一种制备(3AR,4S,7R,7AS)4,7-亚甲基-1H-异吲哚-1,3(2H)-二酮的工艺方法。以纳迪克酸酐为起始物料,经高温转型、氨水氨解、氢气还原得到标题化合物。其结构经1H-NMR、IR等表征。该工艺原料易得、操作简单、成本低廉,适用于工业化生产。 相似文献
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金属酞菁轴向配合物的合成及性质 总被引:3,自引:0,他引:3
综述了金属酞菁轴向配合物的合成方法 ,结构表征及其物理化学性质。金属酞菁轴向配合物的合成重点在于单体的合成。轴向配合物的合成通常有两种方法 :一种是通过金属酞菁的单体来直接合成 ,这种方法分别可以通过三条途径来达到 ,一是以苯腈为原料的途径 ,二是以苯酐为原料的途径 ,三是二亚氨基异吲哚啉路线 ,它们都是以单体为原料 ;第二种合成方法是通过金属酞菁聚合物在配体溶剂中的解离而得到的。金属酞菁轴向配合物的吸收光谱与简单的金属酞菁配合物相比 ,吸收峰明显红移 ,这就大大改进了它的光学性质 相似文献
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李洪娟 《中国新技术新产品》2014,(3):4-6
以环己烯与乙酸为原料,在大孔苯乙烯阳离子交换树脂D006的催化下,通过烯烃酯化反应合成乙酸环己酯。对合成条件进行优化,并考察了树脂催化剂的稳定性。得到较佳的工艺条件为:n(环己烯):n(乙酸)=1:3,反应温度90℃,树脂用量2%(相对于环己烯和乙酸总质量),反应时间5h,搅拌速率300r/min,环己烯转化率94.5%,乙酸环己酯收率83%。催化剂连续使用10次,乙酸环己酯选择性维持在94%左右。 相似文献
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用三羟甲基丙烷、亚磷酸三甲酯、甲基膦酸二甲酯(DMMP)为原料合成了环状膦酸酯阻燃剂,用正交法讨论了物料比、反应温度、反应时间、催化剂种类和用量对反应的影响,确定了反应的最佳条件:三乙胺为催化剂,用量为三羟甲基丙烷质量的3%,n(亚磷酸三甲酯):n(三羟甲基丙烷):n (甲基膦酸二甲酯)=1.09:1:1.06,第一步反应温度为80℃,反应时间5h,第二步反应温度185℃,反应时间16h,产品收率95,7%。产品经IR分析表征。 相似文献
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《International journal for numerical methods in engineering》2018,113(9):1488-1506
In this paper, we present a new method for inserting several triangulated surfaces into an existing tetrahedral mesh generated by the meccano method. The result is a conformal mesh where each inserted surface is approximated by a set of faces of the final tetrahedral mesh. First, the tetrahedral mesh is refined around the inserted surfaces to capture their geometric features. Second, each immersed surface is approximated by a set of faces from the tetrahedral mesh. Third, following a novel approach, the nodes of the approximated surfaces are mapped to the corresponding immersed surface. Fourth, we untangle and smooth the mesh by optimizing a regularized shape distortion measure for tetrahedral elements in which we move all the nodes of the mesh, restricting the movement of the edge and surface nodes along the corresponding entity they belong to. The refining process allows approximating the immersed surface for any initial meccano tetrahedral mesh. Moreover, the proposed projection method avoids computational expensive geometric projections. Finally, the applied simultaneous untangling and smoothing process delivers a high‐quality mesh and ensures that the immersed surfaces are interpolated. Several examples are presented to assess the properties of the proposed method. 相似文献
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Standards are the basis for production enterprises to organize production ex-factory inspection trade 《中国标准化(英文版)》2008,25(1):24-25
Standards are the basis for production enterprises to organize production, ex-factory inspection, trade (delivery) and technical exchanges, product certification, quality arbitration and supervision.…… 相似文献
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A flow calorimeter for enthalpy increment measurements on condensed gases is presented. A better knowledge of the properties of the liquefied natural gas is needed, and therefore a liquid loop has been designed for our flow calorimeter. The fluid loop in the calorimeter is designed in order to avoid the two-phase region, since two phases would give compositional disturbances in the measurements. The avoidance of the two-phase region is made possible by increasing the pressure of the test fluid after the measurement section, then heating the fluid at super-critical pressure past the critical point. Finally, the fluid is throttled to the low-pressure gas state at the inlet condition of the compressor that circulates the fluid. To perform the pressure increase, a new cryogenic pump has been designed. To evaluate the new equipment, measurements were taken on liquid ethane over the temperature range 146–256 K at pressure between 0.9 and 5.1 MPa. 相似文献
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On November 30, 2007, the China Association for Standardization (CAS) held a press conference at Beijing Diaoyutai State Guest House. Leaders from the China Household Electric Appliance Research Institute, the China Household Electric Appliance Association, and the China Consumers' Association attended and made speeches.…… 相似文献
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Zusammenfassung Bei der Gestaltung von Ernteprozessen — beispielsweise des Prozesses Mähdrusch, Körnertransport und -abnahme — als transportverbundene Fließarbeitsverfahren mit mindestens zwei verschiedenen Arbeitsmitteln gibt es einen großen Optimierungsspielraum. Solche Prozesse sind mehrstufige Bedienungsprozesse mit gemischter Anordnung der Bedienungseinrichtungen. Außerdem besitzen sie stark ausgeprägte räumliche Aspekte. Es wird vor allem gezeigt, welche Merkmale solcher Prozesse in Simulationsmodellen abgebildet sein müssen, welche Zielgrößen in Abhängigkeit von welchen Einflußgrößen unter Berücksichtigung welcher Prozeßbedingungen ermittelt werden sollten und wie der Bewertungsprozeß zur Ermittlung der gewünschten Informationen gestaltet werden muß. 相似文献
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C. Qihong W. Zhan‐Wen J. Yi J. Yehua L. Fei F. Hanguang 《Materialwissenschaft und Werkstofftechnik》2014,45(7):582-590
In the present study a high‐boron high speed steel (HSS) roll material was designed. Many expensive alloy elements have been substituted by cheap boron alloy, and high‐boron high speed steel roll has been manufactured by centrifugal casting method. The microstructures, mechanical properties and wear resistance of centrifugal casting high‐boron high speed steel roll have been investigated by optical microscopy (OM), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) analysis, hardness test, impact test and wear test. The results indicated that the solidification microstructures of high‐boron high speed steel roll consisted of M2(B,C), (W,Mo)2(B,C), M3(B,C), M23(B,C)6 type borocarbides and martensite, a small amount of retained austenite. Borocarbides were continuously distributed over the grain boundary. After quenching from 1050 °C, local broken network appeared in partial borocarbides, and fine secondary borocarbide precipitated from the matrix. After tempering from 525 °C, the amount of precipitated borocarbide increased significantly. After heat treatment, the hardness of high‐boron high speed steel roll excelled 60 HRC, and its impact toughness excelled 8.0 J/cm2. The single groove steel rolling amount of high‐boron high speed steel rolls increases by 500% than that of bainite cast iron roll, when the rolls are used in K1 mill housing of bar mill. 相似文献
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Dimiter Hadjistamov 《材料科学与工程:中英文B版...》2019,(2):56-65
The definition of the thixotropy is a decrease in viscosity with time in shear and a subsequent recovery of viscosity after the shear deformation is removed.We ... 相似文献
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《中国标准化(英文版)》2014,(4)
正Responding to ISO’s appeal for survey for the to-be-developed ISO Strategy Plan for 2016-2020,SAC hosted a special workshop over the needs and comments of various fi elds on June 8 in Beijing.The workshop was attended by ISO President-elect and Ansteel General Manager Zhang Xiaogang,SAC Vice-Administrator Yu Xinli,and 30 experts from 相似文献
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《中国标准化(英文版)》2014,(5)
正The review group of Asia Pacific Laboratory Accreditation Cooperation(APLAC)carried out a 4-day peer review of the proficiency testing provider(PTP)for China National Accreditation Service for Conformity Assessment(CNAS)from July 28 to 31,2014.CNAS passed the PTP review with excellent performance.Two senior peer reviewers of APLAC made a comprehensive,rigorous and detailed review of CNAS’s PTP accreditation activities,and made the on-spot inspection of the review groups in Shanghai and Shenzhen respectively. 相似文献