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The invention discloses a dielectric hole-microhole composite material and synthesizing method in the inorganic porous material, adsorbing material and catalytic material technical domain, which comprises the following steps: adopting zeolite molecular sieve as raw material; reacting with sodium bisilicate solution under 30-60 deg.c for 10-300 min; disintegrating particle part of zeolite molecular sieve into piece with microhole structure; adding cetyl trimethyl ammonium bromide as molder; adjusting pH value of mother liquid to 10-12; aging 1-8h; adding in the high-pressure autoclave to do water heat synthesizing reaction at 80-130 deg.c for 24-72h; separating solid; washing; drying; sintering under 500-600 deg.c for 5-10h; obtaining the Si-Al porous material with dielectric hole and microhole composite structure.

本发明属于无机多孔材料、吸附材料和催化材料技术领域,涉及具有介孔-微孔复合材料及其合成方法。其特征是以沸石分子筛为原料,用偏硅酸钠的水溶液在30~60℃反应10~300分钟,使沸石分子筛的颗粒部分解离形成具有微孔结构的碎片,加入模板剂十六烷基三甲基溴化铵,然后调节母液pH值为10~12,老化1~8小时,然后加入高压釜于80~130℃进行水热合成反应。反应24~72小时后,分离出固体,水洗、干燥,然后于500~600℃焙烧5~10小时,得到具有介孔和微孔复合结构的硅铝多孔材料。本发明的效果和益处是所发明的合成方法可用于合成多种沸石结构和介孔结构的复合材料,所合成的材料经过质子交换可以具有较强的酸性,在吸附和催化领域具有广泛应用前景。

The results of catalytic activity show that both Ni-B and Ni-P sample have the same kinetic equation for hydrogenation of 1, 3-cyclopentadiene to cyclopentene and the same TOF. Therefore, it can be suggested that they have the similar active site. The catalytic activity of Ni-B sample is higher than that of Ni-P sample, and it is due to the more active sites of Ni-B sample having.

催化活性测试表明,Ni-B与Ni-P催化环戊二烯加氢反应对环戊二烯具有相同的动力学方程,而且两者具有相似的氢转换频率,表明两者的活性中心本质上是相似的,类金属不同导致的电子转移方向的不同仅仅影响反应的初活性,宏观活性的差别在于两者活性中心数量的不同。

This dissertation is mainly focused on the reactivity of methylenecyclopropanes and comprises six parts. 1 The reactions of methylenecyclopropanes with phenylsulfenyl chloride, phenylselenyl chloride and diphenyl diselenide; 2 The coupling reactions of the ring-opening products derivated from methylenecyclopropanes; 3 The palladium-catalyzed ring-enlargement of mono-aryl group substituted methylenecyclopropanes to cyclobutenes. 4 The gold-catalyzed domino ring-opening and ring-closing hydroamination of methylenecyclopropanes with sulfonamides; 5 The Lewis acid-catalyzed reactions of mono-aryl group substituted methylenecyclopropanes with diethyl ketomalonate in the presence of water; 6 The iodobenzene diacetate mediated novel 1,3-dipolar cycloaddition of methylenecyclopropanes, vinylidenecyclopropanes, and methylenecyclobutane with phthalhydrazine.

本论文主要研究了亚甲基环丙烷类化合物的一些化学反应性能,共由以下六部分组成:1、亚甲基环丙烷类化合物与苯硫氯、苯硒氯及二苯基二硒的反应;2、亚甲基环丙烷类化合物开环产物的偶联反应;3、单芳基取代的亚甲基环丙烷类化合物在钯催化剂作用下的扩环反应;4、金化合物催化磺酰胺对亚甲基环丙烷类化合物的串联开环关环氨氢化反应;5、路易斯酸催化亚甲基环丙烷类化合物与丙酮二羧酸二乙酯在有水存在下的反应;6、醋酸碘苯促进的亚甲基环丙烷类化合物、亚乙烯基环丙烷类化合物及亚甲基环丁烷类化合物与邻苯二甲酰肼的新型1,3-偶极环加成反应。

By use of titration analysis, the thesis investigated various factors such as isocyanate, PE molecular weight, reacting substance molecular ratio, reacting temperature and time etc. influencing upon prepolymerization step. It was found that 2, 4-tolulene diisocyanate and 4, 4'diphenylmethane diisocyanate is more rapidly reacted with PE600 than HDI. With PE molecular weight increasing, the reacting temperature or time should be raised or extended relevantly. Thus PE2000+2HDI pre-polymerization should be better carried out under some catalyst, for example, Triethylene diamine , Dibutyltin dilaurate and Tin octoate were used.

首先采用滴定分析方法对WRPU预聚反应的影响因素进行了研究:芳香族二异氰酸酯TDI、MDI比脂肪族二异氰酸酯HDI反应活性高,其中TDI在反应初始阶段的反应速率比MDI快,不过随着反应的进行,MDI比TDI反应速率加快,这主要是因为TDI分子中的两个-NCO反应活性差异大所致;二元醇分子量越大,反应速度越慢;聚醚二元醇比聚酯二元醇的反应速度快;当分子量超过2000的二元醇与HDI进行预聚反应时,需借助适当的催化剂来加快反应速度,从而使预聚反应能够顺利进行,分别选择DABCO、TOA和DBDTL三种催化剂进行催化反应,发现不同的催化剂,其催化效果相差较大。

The catalytic transformation pathway can change to decrease the yield of hydrogen and yield methyl-contained sulfides such as methyl mercaptan, dimethyl sulfide and dimethyl disulfide, but overlarge concentration of methanol would holdback the transformation of isobutyl mercaptan. The transformation of isobutyl mercaptan was favorable if the volume ratio of methanol and benzene was 0.2.The addition of methanol assume certain effect on the catalytic cracking of di-n-butyl sulfide in solvent benzene but without changing the cracking reaction mechanism of di-n-butyl sulfide.

甲醇也可以使异丁硫醇的催化转化路径发生改变降低硫化氢的产率,生成甲硫醇、甲硫醚及二甲基二硫化物等含甲基硫化物,但甲醇的浓度过高会抑制异丁硫醇的转化,在反应体系中当甲醇的体积占到溶剂苯体积的20%时对异丁硫醇的转化较为有利;甲醇的添加对丁硫醚在溶剂苯中的催化裂化有一定影响,但没有改变丁硫醚的裂解反应历程。

For the first time we synthesized nanoscale metal hydrides of lanthanum, neodymium, samarium, dysprosium, and ytterbium with high efficiency under mild condition by complexometric catalysis instead of traditional preparation at high temperature and high pressure. It is for the first time that we synthesized lanthanide organic compounds with catalysts or initiating agents at atmosphere and ambient temperature,and some of them are new compounds. Nanometric lanthanide metal powders are prepared by thermal decomposition of the compounds in vacuum. Differently from the traditional method, size of the products prepared by our method is less than 40nm, and the activity of the reaction is very high. They are pyrophoric at atmosphere. They can make some reactions without activity or low activity show extremely high activity .We investigated influent regulations of methods, conditions to scale and special surface.

我们首次成功地用络合催化等方法取代需在高温高压下进行的传统方法,在温和条件下高效率地合成出纳米尺寸镧、钕、钐、镝、镱的金属氢化物;首次在常压常温的条件下,通过催化、引发等方法合成镧系金属有机化合物,再将其真空热分解成功地制备了纳米尺寸的镧、钕、钐、镝、镱等金属粉末;与传统方法不同,这些方法得到的产品基本颗粒尺寸小于 40 nm,遇到空气燃烧,具有极高的化学反应活性,使原来活性很低甚至观察不到活性的反应大幅度提高反应速率和产率;考察了制备方法、制备条件等因素对晶粒尺寸、比表面积大小等的影响规律。

The types,structures of substrates and reaction mediums for the enzymatic synthetic polyphenol resin was surveyed and the manufacturing method,product structure and their performances of the polyphonel resin and aldehyde resin were compared.

概述了酶催化合成聚酚树脂用酶的种类、底物的结构、反应介质;比较了该树脂和传统酚醛树脂的生产、结构及性能特点;指出了其不仅具有良好的耐热性能,可作传统酚醛树脂的替代品,而且具有导电、发光等功能,在光电材料方面显示了极强的应用潜力,但降低HRP催化合成聚酚树脂的成本是其实现工业化亟待解决的问题。

Chiral SalanCrX complexesa saturated version of SalenCr(ⅢX are designed,and in conjunction with an ionic quaternary ammonium salt or organic strong base can efficiently catalyze the asymmetric,regio-and stereoselective alternating copolymerization of CO_2 with rac-PO at mild conditions to afford isotactic-enriched polycarbonates with~95%head-to-tail linkages and moderate enantioselectivity.

本论文在Salen构型配体的基础上,设计合成了一系列手性Salan型铬配合物,并将其与季铵盐/有机强碱组成亲电-亲核双组分催化体系,在室温下可以有效的催化CO_2和环氧丙烷的不对称交替共聚反应,实现了CO_2和环氧丙烷的不对称交替共聚反应的区域和立体化学控制,得到95%的头尾连接单元和中等光学纯度(对映体过量值ee%≈70%)的全同结构的聚碳酸酯。

At first, the rought C〓F〓 mixed gases are obtained by pyrolysis process of R22. A experimental pyrolysis device is designed and made by ourself. The optimum operating conditions are offered in the paper. Secondly, the much efforts is on the synthesis of R134. After through the discussion of basic thermodynamics and kinetics, selecting and preparating catalyst, it is possible that the synthesis of R134 by pyrolyzed gases hydrogenation. Base on the character of catalytic process, the kinetics equation about C〓F〓 catalytic hydrogenation is established. The rate constant of the reaction is obtained through experiment data regression. In order to achieve higher yield of R134, some optimum technological conditions is determined.

论文首先对R22裂解制成四氟乙烯混合原料气的裂解过程进行了讨论,自行设计和制作裂解反应装置,并确定裂解反应的最佳操作条件;然后,重点对R134的合成进行基础研究,分别从热力学和动力学的角度探讨以含四氟乙烯的R22裂解混合气为原料合成R134这一全新工艺的可能性,选择和制备加氢催化剂,根据催化过程特点建立四氟乙烯催化加氢反应的总包动力学方程,并在此基础上自行设计和制作中试合成装置,获得了以裂解混合气为原料合成R134的最佳工艺条件,为R134的工业化生产提供了必要的理论依据和实验基础。

In order to disclosure the reason why the electrocatalysis activeness and selectivity droped after being used several hundred hours continuously, the x-ray diffraction, scanning electron microscopy and energy dispersive spectroscope have been used to characterize the surface condition variations of Monel metal. The results indicated: Monel metal belongs to the Cu-Ni alloy around the electrolysis experiment.And after being used for 600hr, the surface layer element composition and geometry distribution of the alloy changed, namely in the alloy the Cu element /which superficial free enthalpy was smaller,"concentrated" to the alloy surface,and formed one kind of marble structure microcrystallite.Thus the electrode surface becamed rough a

为了揭示蒙乃尔合金阴极在连续使用数百个小时后电催化活性剂选择性下降的原因,采用X射线衍射仪、电子扫描电镜和电子能谱分析仪对电解实验所用的蒙乃尔阴极材料在电解实验前后的表面状态进行了表征,结果表明:所使用的蒙乃尔合金阴极材料在电解实验前后均属于Cu-Ni合金,使用600hr后,由于表面层元素组成和几何排布发生了变化,即合金中表面自由焓较小的Cu元素向合金表面&富集&,形成一种大理石结构的微晶,表面粗糙、不均一,这是造成其对硝基苯电还原的催化活性及选择性随着使用时间延长而逐渐下降的主要原因,同时也为此类电极的修饰改进提供了方向。

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