铜对Mn/Al_2O_3氨还原SO_2到单质硫催化性能的影响

ＳＯ2 是危害最为严重的大气污染物之一 ,也是造成酸雨的元凶。将ＳＯ2 选择性还原为单质硫 ,既能消除ＳＯ2 对环境的污染 ,又能回收单质硫 ,具有特别重要的意义。根据所用的还原剂的不同 ,催化还原ＳＯ2 到单质硫可分为Ｈ2 、炭、烃类 (主要是ＣＨ4 )、ＣＯ和ＮＨ3还原法[1] 。氨还原法是基于氨的催化分解生成Ｎ2 和Ｈ2 混合气 ,其中的Ｈ2 再还原ＳＯ2 到硫和Ｈ2 Ｓ ,然后进行高温Ｃｌａｕｓ反应生成单质硫。Ｐａｉｋ[2 ] 等以第四周期过渡金属硫化物载于Ａｌ2 Ｏ3 作为催化剂 ,研究了Ｈ2 还原ＳＯ2 为单质硫的反应 ,认为过渡金属硫化物是…     

含杂环卡宾碳的铁羰基簇合物的结构化学研究Ⅱ.—Fe3（CO）8（：CNH（S）C（…

Ｆｅ３（ＣＯ）１２和取代２，４－二硫代乙内酰脲反应，得到新的取代物Ｆｅ３（ＣＯ）８＾－（：ＣＮＨＣ（Ｓ）Ｃ（ＣＨ３）２ＮＨ（μ３－Ｓ２），并进行了ＩＲ，＾１ＨＮＭＲ，ＭＳ表征，测定了它的分析和晶体结构，讨论了杂环卡宾碎片：ＣＮＨＣ（Ｓ）Ｃ（ＣＨ３）２ＮＨ的取代位置，它是通过卡宾碳原子与Ｆｅ配位。     

含杂环卡宾碳的铁羰基簇合物的结构化学研究Ⅱ．—Fe_3(CO)_8[:CNHC(S)C(CH_3)_2NH]的合成和晶体结构

Ｆｅ３（ＣＯ）＿（１２）和取代２，４＿二硫代乙内酰脲反应，得到新的取代物Ｆｅ３（ＣＯ）＿８－［：ＣＮＨＣ（Ｓ）Ｃ（ＣＨ＿３）＿２ＮＨ］（μ＿３－Ｓ）＿２，并进行了ＩＲ、１￣ＨＮＭＲ、ＭＳ表征，测定了它的分子和晶体结构，讨论了杂环卡宾碎片：ＣＮＨＣ（Ｓ）Ｃ（ＣＨ＿３）＿２ＮＨ的取代位置，它是通过卡宾碳原子与Ｆｅ配位。     

MgSO4-NaOH-H2O四元交互体系160℃水热相作用

在ＭｇＯ-ＭｇＳＯ4-Ｈ2Ｏ体系中存在多种硫氧镁化合物[1-4],其中5Ｍｇ(ＯＨ)2·ＭｇＳＯ4·2Ｈ2Ｏ晶须(简称ＭＯＳ)被开发用作塑料、树脂和橡胶等复合材料添加剂,提高基底材料的抗冲击力、抗弯曲力和耐磨性,也可以用作填料和过滤材料和阻燃剂[5-8]。由于ＭＯＳ价廉、安全,同时具有多种功能,具有广阔的应用前景。本文对ＭｇＳＯ4-ＮａＯＨ-Ｈ2Ｏ四元交互体系160℃水热条件下相作用进行研究,得到同一组成形貌不同的晶须,同时还存在另外两种硫氧镁化合物。1　实验用分析纯ＭｇＳＯ4·7Ｈ2Ｏ(西安化学试剂厂)分别配制质量百分比浓度为6%、1…     

2001年全国高中学生化学竞赛（决赛）理论试题答案

第 1题1- 1　Ａ :ＮＨ4 ＨＣＯ3[或 (ＮＨ4 ) 2 ＣＯ3]　Ｂ :ＫＣｌ　Ｃ :Ｋ2 ＳＯ4 　Ｄ :ＮＨ4 Ｃｌ　Ｅ :Ｆｅ2 Ｏ3　Ｆ :ＣＯ21- 2　反应 (1) :(ｍ +ｎ)ＦｅＳＯ4 + 2 (ｍ +ｎ)ＮＨ4 ＨＣＯ3=Ｆｅｍ +ｎ(ＯＨ) 2ｎ(ＣＯ3) ｍ↓ + (ｎ +ｍ) (ＮＨ4 ) 2 ＳＯ4 + (2ｎ +ｍ)ＣＯ2 ↑ +ｍＨ2 ＯＮＨ4 ＨＣＯ3 写成 (ＮＨ4 ) 2 ＣＯ3,Ｆｅｍ +ｎ(ＯＨ) 2ｎ(ＣＯ3) ｍ 写成 (1)Ｆｅ2 (ＯＨ) 4-2ｍ(ＣＯ3) ｍ,(2 )Ｆｅ2 (ＯＨ) 2 ＣＯ3,(3)Ｆｅ(ＯＨ) 2 和ＦｅＣＯ3 且配平的 ,也给分。反应 (2 ) :2Ｆｅｍ +ｎ(ＯＨ) 2ｎ(ＣＯ3) ｍ+ ｍ +ｎ2 Ｏ2…     

含2,4—二硫代乙丙酰脲分子片卡宾铁羰基簇合物的合成和结构

Ｆｅ３（ＣＯ）１２与５个２，４－二硫代乙内酰脲ＳＣＮＨＣ（Ｒ１）（Ｒ２）Ｃ（Ｓ）ＮＨ应制得通式为Ｆｅ３（ＣＯ）８（μ３－Ｓ）２（Ｌ）含卡宾配体的５个新铁羰基簇合物（１～５）对其进行了元素分析，ＩＲ、ＨＮＭＲ和ＭＳ表征，并用Ｘ射线衍射法测定了簇合物３的晶体和分子结构，表明２，４－二硫代乙内酰脲分子片配位基：ＣＮＨＣ（ＣＨ３）２Ｃ（Ｓ）ＮＨ的卡宾碳具有ｓｐ＾２成键特征，其Ｃ－Ｆｅ键长０．１８９８ｎｍ，     

变温红外确定硫氰化铵固-固相变机理(英文)

硫氰化铵分子晶体在固 固转变时 ,能可逆地吸收大量的热。作者利用变温红外光谱确定了其固 固相变机理。结果表明 ,随着温度升高 ,固 固转变时分子晶体内相邻的氢键断裂 ,晶型由低对称转变为高对称并引入振动和转动无序 ,吸收大量热。     

NaF-SnCl_2光度法测定磷的方法中,钼磷黄还原为钼磷蓝的反应式应如何表述?

答 :关于钼磷杂多酸还原为钼磷蓝的反应式一般表示为 :(ＮＨ4 ) 3 Ｈ4 [ＰＭｏ2 Ｏ7) 6]+2ＳｎＣｌ2 +4ＨＣｌ　　　　　　 (ＮＨ4 ) 3 Ｈ4 [Ｐ(Ｍｏ2 Ｏ5)·5 (Ｍｏ2 Ｏ7) ]+2ＳｎＣｌ4 +2Ｈ2 Ｏ但有报道认为在有ＮａＦ存在下 ,反应中不可能有ＳｎＣｌ4 或ＳｎＣｌ2 - 6的形式的化合状态 ,因为ＳｎＦ2 - 6的积累稳定常数的对数值ｌｇβ6等于 2 5 ,远高于ＳｎＣｌ2 - 6的积累稳定常数的对数值 (ｌｇβ6=14)。此外 ,一般认为磷钼蓝分子中只有 2个Ｍｏ(Ⅵ )被还原为Ｍｏ(Ⅴ )。但用光度滴定法研究钼磷蓝的结果表明在 12个Ｍｏ(Ⅵ )中有 4个Ｍ…     

锌-硫氰酸铵还原体系用于氢化偶氮苯的合成

氢化偶氮苯是重要的精细有机化工原料及中间体,染料工业用于制备联苯胺染料,医药工业用于生产解热镇痛药保泰松等[1]。传统的制备方法是在强碱性介质中用锌粉还原硝基苯,反应时间长,产率低[2]。用硫化铵快速还原偶氮苯生成氢化偶氮苯[3],则硫化铵用量大,刺激性气味对操作者及环境造成极大危害。我们采用ＮＨ4ＣＮＳ的饱和溶液与锌粉组成还原体系,在25℃时还原偶氮苯,反应条件温和,锌粉用量少,时间短,产率高,操作简单。反应方程式如下:ＰｈＮ=ＮｐＨ(橙红色)Ｚｎ-ＮＨ4ＣＮＳ25℃,ＥｔＯＨＰｈＮＨＮＨＰｈ(白色)1　实验部分在50ｍｌ圆底…     

Mechanism of the Deaquation of Aquopentaaminocobalt(III) Bromide

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｓｏｌｉｄ ｐｈａｓｅｄｅａｑｕａｔｉｏｎ ａｎａｔｉｏｎｒｅａｃｔｉｏｎ[Ｍ(ＮＨ3 ) 5(Ｈ2 Ｏ) ]Ｘ3 → [Ｍ(ＮＨ3 ) 5Ｘ]Ｘ2 +Ｈ2 Ｏ(Ｍ =Ｃｏ3 + ,Ｃｒ3 + ｏｒＲｕ3 + ａｎｄＸ =Ｃｌ- ,Ｂｒ- ｏｒＮＣＳ- )ｈａｓｂｅｅｎｗｉｄｅｌｙｓｔｕｄｉｅｄｓｉｎｃｅｔｈｅｎｉｎｅｔｅｅｎｓｉｘｔｉｅｓ .Ｔｈｅｔｈｅｒｍａｌａｎｄｋｉｎｅｔｉｃｐａｒａｍｅｔｅｒｓｈａｖｅｂｅｅｎｃａｌｃｕｌａｔｅｄａｎｄｔｈｅｄｉｆｆｅｒｅｎｔｍｅｃｈａｎｉｓｍｈａｓｂｅｅｎｐｒｏｐｏｓｅｄａｎｄｄ…     

紫外拉曼光谱研究焙烧气氛对氧化锆相变的影响

 以紫外拉曼光谱技术研究了在不同焙烧气氛中氧化锆样品的表面晶相结构及其转变过程．结果表明，在有氧气氛中焙烧的氧化锆样品易转变为单斜相，而在惰性气氛中焙烧可以有效地稳定样品体相和表面的四方相结构．在缺氧气氛中焙烧的样品暴露于空气中后，表面极易转变为单斜相，而其体相仍为四方相结构，这表明四方相氧化锆在样品表面是极不稳定的．     

Three-phase separation in nonionic surfactant/hydrophobically modified polymer aqueous mixtures

Three-phase separation for Triton X-114 or Triton X-100 solutions with addition of hydrophobically modified hydroxyethyl cellulose was investigated experimentally. When the surfactant concentration was high enough, the solution slightly above the cloud point could separate into three macroscopic phases: a cloudy phase in between a clear phase and a bluish, translucent phase. The rate of phase separation was very low with the formation of the clear and cloudy phases followed by the emergence of the bluish phase. The volume fraction of the cloudy phase increases linearly with the global polymer concentration, whereas the volume fraction of the bluish phase increases linearly with the global surfactant concentration. Composition analyses found that most of the polymer stayed in the cloudy phase, as opposed to most of the surfactant in the bluish phase. The interesting phase behavior can be explained by an initial associative phase separation followed by a segregative phase separation in the cloudy phase.     

Ion-pair mediated transport of angiotensin, neurotensin, and their metabolites in liquid phase microextraction under acidic conditions

This paper discusses the behaviour of angiotensin 1 and neurotensin together with their metabolites in a three-phase liquid phase microextraction under acidic conditions. Variations in donor phase, organic phase, and acceptor phase are studied with extraction recovery as response variable. It is proved that for all peptides the transport across the organic phase is mediated by heptane-1-sulphonic acid. n-Octanol gave overall best results as organic phase. A donor phase volume of 1.0 mL was chosen as a compromise between optimal recovery and robustness of the LPME device. The optimal pH of the donor phase (using acceptor phase of pH 2) was found to be different for the peptides, which opens opportunities for selective sample preparation. Decreasing the acceptor phase pH to 1.0 resulted in increased extraction recoveries. On using 1.0 mL of donor phase containing 50 mM heptane-1-sulphonic acid pH 3, n-octanol as organic phase immobilized in the pores of the fibre, and 20 microL of acceptor phase containing 0.1 mol/L HCl, extraction recoveries up to 82% (enrichment factor = 41) were achieved. To our knowledge this is the first report on liquid phase microextraction of angiotensins and neurotensins.     

基于虚拟相位平面的相位展开方法

在基于相位分析的三维测量系统中,为了准确地得到物体的高度,相位展开扮演着很重要的角色。传统的相位展开方法常常需要额外的投影图,而傅里叶变换轮廓术只需要采集一幅或两幅变形条纹图就可以实现对物体轮廓的测量,其方法速度快,易于实现。针对傅里叶变换轮廓术方法计算得到的截断相位分布,本文提出了一种利用截断相位与参考平面相位差值2π的整数倍数获得截断相位的正确级次,辅助相位展开的方法。当被测物体较复杂,或者相位截断次数较多时,该方法在已有参考平面相位的基础上虚拟新的相位平面,依次比较截断相位和虚拟相位,进行多次分级相位展开,结合多个展开相位结果,最终得到正确的展开相位。该方法展开速度快,展开错误不会蔓延传递。仿真和实物实验结果证明了该方法的可行性,说明该方法可用于傅里叶变换轮廓术中进行截断相位的快速展开。     

薄膜梯度扩散技术结合相研究进展

薄膜梯度扩散(DGT)技术是一种新型原位被动采样技术,已被广泛应用于水体、土壤、沉积物中目标物的采集与测量。结合相是DGT技术的重要组成部分,决定了与目标物的结合能力、结合速度、结合容量以及目标物的形态选择性等。DGT结合相分为固态结合相和液态结合相。本文重点综述了树脂、氧化物、无机盐、活性炭、改性硅胶、分子印迹、共聚物、复合、液态等结合相在DGT技术中的应用,展望了DGT结合相的发展前景。     

LYOTROPIC LIQUID CRYSTALS IN BINARY SYSTEMS N-ALKYL GLYCOSIDES/WATER*

The formation of lyotropic mesophases (liquid crystals) in four binary systems n-alkyl glycosides/water was examined in dependence on surfactant concentration, temperature and the chain lengths (alkyl = heptyl, octyl, nonyl, decyl). The binary phase diagrams were established and the enthalpies of phase transitions were measured. The following phase transitions were detected by texture observation and calorimetry: hexagonal phase H, lamellar phase L, cubic phase Q, gel phase G and crystalline phase C. The positions of the corresponding regions of these phases in the phase diagram were determined. Sequence of phases and the localization of the phase regions were depended on the chain length of the alkyl group. So in the binary system n-decyl-β-D-glucoside/water the H-phase was not observed.     

辛基三甲基溴化铵与辛基硫酸钠混合水溶液的相行为

对辛基三甲基溴化铵(OTAB)与辛基硫酸钠(SOS)正、负离子混合表面活性剂水溶液的相行为进行了研究.在高浓度的溶液中,混合表面活性剂形成液晶相,随着混合摩尔比OTAB/SOS接近于1,液晶结构由六角相转层状相,同时夹杂少量沉淀物;在中等浓度时,任意混合摩尔比例下皆为均相透明溶液;在低浓度下,在很宽的OTAB/SOS混合摩尔比的范围,出现双水相,其中的表面活性剂稀薄相,为不同大小的胶团与囊泡组成的稀溶液,另一表面活性剂富集相中则为数密度很大的囊泡聚集体,富集相对油溶性染料的增溶作用比非富集相高得多.     

Effect of molecular weight on the polymorphic transformation of isotactic poly(1-butene)

The effect of molecular weight on the polymorphic transformation of isotactic poly(1-butene)(iPB) under room temperature had been investigated by fourier transform infrared spectroscopy(FT-IR). The phase transformation time, phase transformation rate and phase transformation time difference between phase I and phase II at a given transformation degree were used to analysis the phase transformation kinetics of iPB aging at room temperature. The results show that the reduction of phase II can occur quickly at room temperature and seem less dependent on the molecular weight. However, the molecular weight has great effect on the formation of phase I. When the phase transformation degree for phase I reach 90%, a distinct transformation time difference can be observed. In order to clearly explain the difference in the reduction of phase II and the growth of phase I, a phase transformation model from the chain conformation level for iPB with different molecular weight have been drawn. DSC analysis was used to support the proposed model.     

Phase transfer catalytic system with the third liquid phase

Phase transfer catalysis, a technique to bring the reactants in two immiscible phases together by adding a phase transfer agent, has been employed in the production of fine chemicals and pharmaceuticals in the last few decades. The third liquid phase (catalytic phase) may be formed when phase transfer catalysts (PTC), cannot be dissolved in either organic or aqueous phase. The third phase catalytic systems have the following three advantages, that is, (1) high activity (2) repeated use and (3) separation between the organic phase and the aqueous phase. It is expected that simple new processes can be constructed by applying these three advantages.     

Emulsification liquid phase microextraction followed by on-line phase separation coupled to high performance liquid chromatography

An emulsification liquid phase microextraction followed by on-line phase separation coupled to high performance liquid chromatography (HPLC) is introduced based on a novel idea for the separation of dispersed organic phase from aqueous phase. In this method, the dispersed organic extraction phase was filtered using an in-line filter and it was separated from the water sample. The new approach is simple and, in addition to improving some limitations of the conventional emulsification liquid phase microextraction, eliminates the need for centrifugation in the phase separation step.