关于五氧化二磷在乙烯制备中应用的讨论

实验室乙烯的制备常采用乙醇和浓硫酸共热的方法,由于浓硫酸具有强脱水性和强氧化性,反应中会产生大量的积碳及CO2和SO2气体,严重影响着乙烯的性质和合成实验。人们不断探索各种改进方法,其中以五氧化二磷为脱水剂和无水乙醇作用制备乙烯的方法报道最多,影响也最广。笔者对该改进实验进行了研究,结果发现用五氧化二磷和无水乙醇作用制备乙烯的方法,在实验中难以得到乙烯,在理论上也缺乏足够的依据,本文就此提出自己的一点粗浅看法,与作者、读者讨论。     

SO4^2—TiO2—Hβ—Al2O3催化剂的制备及催化性能研究

以Ｈβ沸石为，通过ＴｉＯ２改性及硫酸铵处理制备了ＳＯ４＾２－－ＴｉＯ２－Ｈβ－Ａｌ２Ｏ３催化剂，并由ＸＲＤ、ＸＰＳ、ＮＨ３－ＴＰＤ、ＦＴＩＲ及化学吸附等手段考察了不同焙烧温度对该催化剂表面性质、酸性及催化性能的影响。结果表明；适宜的焙烧温度使ＳＯ４＾２－－ＴｉＯ２－Ｈβ－Ａｌ２Ｏ３的酸量大幅度增加，强酸比例增大，并产生部分增强酸中心，高强度的酸性中心中，以Ｌ酸中心为主；５５０℃焙烧的样品能使沸石表     

磷酸浸渍黏土砖中五氧化二磷含量测定方法的改进

研究了磷钼酸铵容量法测定磷酸浸渍黏土砖中五氧化二磷含量的方法,对国家标准分析方法进行了改进,讨论了不同实验条件对实验结果的影响,并进行了精密度和准确度实验。结果准确、重现性好,证明方法可靠。     

混合溶剂中TS-1催化丙烯环氧化反应的研究

对甲醇、异丙醇混合溶剂中的TS－1催化丙烯环氧化过程进行了实验研究。通过单因素实验和正交实际，系统考察了溶剂组成（甲醇质量／异丙醇质量），反应温度，H2O2浓度和TS－1催化剂浓度四个因素对反应的影响，得到了反应的最佳工艺条件。在此条件下反应30min,H2O2转化率为94．1％，环氧丙烷选择性为95．3％，环氧丙烷收率为89．7％。     

对五氧化二磷催化乙醇脱水反应的研究

研究了不同反应条件下用P2O5催化乙醇脱水反应的情况,并用GC和GC-MS方法检测反应产物。为苏教版《有机化学基础》教材中“认识乙醇的脱水反应”提供教学参考。     

电感耦合等离子体发射光谱法测定磷石膏中的水溶性五氧化二磷

建立电感耦合等离子发射光谱法(ICP–OES)测定磷石膏中水溶性五氧化二磷含量的方法。用超声波快速提取磷石膏中的磷,在178.284 nm波长下,用CID固体检测器测定样品溶液的光谱强度。五氧化二磷的质量浓度在0.007~200 mg/L范围内与光谱强度线性关系良好,线性相关系数r=0.999 96,检出限为0.006 9 mg/L。样品加标回收率在98%~102%之间,测定结果的相对标准偏差为0.95%~1.11%(n=6),该方法的测定结果与国标法基本一致。该法简便、快速,适合磷石膏中水溶性五氧化二磷的测定。     

五氧化二磷使乙醇脱水的实证探索与反思

通过实验探究和文献分析,说明五氧化二磷具有强脱水性,它与乙醇反应生成磷酸氢乙酯和磷酸二乙酯,不是乙醇脱水的催化剂,分析了造成人们错误认识的原因。     

负载型水相催化剂的制备及其在丙烯氢甲酰化中的应用

以ＳｉＯ２为载体,制备了负载型水相铑膦催化剂。在反应温度为１００－１１０℃,合成气ＣＯ：Ｈ２＝１：１,反应压力２．０ＭＰａ,「Ｒｈ」＝７．５×１０＾５,Ｐ／Ｒｈ＝２５的条件下,进行丙烯氢甲酰化反应。结果表明,时空收率可达１９４－２２８ｇ丁醛,正异比高达约１４．２,反应结束后催化剂与体系易分离,铑在有机相中的浓度仅为１×１０＾－９－４×１０＾－９,基本消除了铑的流失,克服了均相反应中催化剂铑的回收和     

完全交替结构乙烯-丙烯共聚物的制备与表征

对顺-1,4含量为100%的高顺式聚异戊二烯(HCPI)进行加氢反应,得到了序列结构高度规整的乙烯-丙烯交替共聚物(alt-EP).所用的HCPI有适当的分子量(Mn=41×104)和极窄的分子量分布(Mw/Mn=1.02).HCPI的加氢反应以环烷酸镍和三异丁基铝为催化剂,在60℃和4.0MPa氢压的条件下反应3h,加氢产物的加氢度为100%.GPC测试结果显示所得乙烯-丙烯交替共聚物保持了窄分布的特点,表明HCPI加氢后未发生交联和降解反应;NMR,FTIR和广角X射线衍射测试结果表明此乙烯-丙烯交替共聚物具有高度规整的序列结构,为完全交替结构的乙烯-丙烯共聚物.并通过TGA和DSC对乙烯-丙烯交替共聚物的热性能进行了表征.     

Sol-Gel Preparation of Fast Proton-Conducting P2O5-SiO2 Glasses

We have investigated the proton conductivities of the sol-gel-derived P₂O₅-SiO₂ glass at –50 to 120°C. The obtained glass is porous, where the surface area, pore volume and pore diameter are 740 m²/g, 0.5 cm³/g and <5 nm, respectively. The freezing temperature of water molecules adsorbed in the pores was –20°C, which is much lower than that of free liquid water due to the quantum size effect of the water confined in the pores. The electrical conductivities followed the Arrhenius equation in the temperatures between –20 and 120°C. Below –20°C, the adsorbed-water molecules were frozen, resulting in a rapid decrease of the proton conductivity. Considering the high conductivity, chemical and thermal stability, this oxide glass membranes have potential for the fuel cell membrane.     

P2O5/SiO2 as an Efficient Reagent for the Preparation of Z -Aldoximes Under Solvent-Free Conditions

Abstract

A facile and efficient method for the preparation of Z-aldoximes is improved by means of P₂O₅/SiO₂ reagent in solvent-free media. Advantages of this method are the use of inexpensive and selective reagent, with high yields in simple operation, and short reaction time under solvent-free conditions.     

Phase equilibria in the P2O5-rich part of the system Y2O3−Na2O−P2O5

In the ternary system Y₂O₃?Na₂O?P₂O₅, the partial system Y(PO₃)₃?NaPO₃?P₂O₅ was examined by means of differential thermal analysis and X-ray powder diffraction; its phase diagram is given.     

Phosphorus pentoxide supported on silica gel and alumina (P2O5/SiO2, P2O5/Al2O3) as useful catalysts in organic synthesis

Phosphorus pentoxide supported on silica gel or alumina (P₂O₅/SiO₂, P₂O₅/Al₂O₃) has been used in many organic transformations as versatile solid catalysts. These catalysts have received considerable attention as an inexpensive, eco-friendly, highly reactive, easy to handle and non-toxic acid catalyst for various organic transformations, affording the corresponding products in excellent yields and high selectivity. In this review, some applications of these catalysts in organic reactions are discussed.     

The system Y2O3−CaO−P2O5

The ternary system Y₂O₃?CaO?P₂O₅ has been examined by DTA, X-ray diffraction, IR and microscopic methods. Its phase diagram has been provided within the composition range YPO₄?Ca₃(PO₄)₂?P₂O₅. The occurrence of four mixed phosphates: Ca₃Y(PO₄)₃, CaYP₃O₁₀, CaY(PO₃)₅, Ca₂Y(PO₃)₇ has been discovered in the system. Basic X-ray data have been determined for these newly discovered compounds and several methods of their synthesis developed.     

The system Y2O3−MgO−P2O5

The previously unknown ternary system Y₂O₃?MgO?P₂O₅ has been examined by thermal, X-ray and microscopic methods. Its phase diagram has been determined over the composition range: YPO₄?Mg₃(PO₄)₂?Mg(PO₃)₂?Y(PO₃)₃. In the system, the existence of two mixed phosphates: MgYP₃O₁₀ and MgY(PO₃)₅ has been found, and they occur, according to their composition, at the sections YPO₄?Mg(PO₃)₂ and Y(PO₃)₃?Mg(PO₃)₂, respectively.     

Au／Fe2O3／Al2O3催化剂上丙烯选择催化还原NO

以浸渍法制备的Fe2O3/γ-Al2O3为载体,采用均相沉积沉淀方法制备了Au/Fe2O3/Al2O3催化剂.该催化剂在丙烯选择催化还原NO反应中显示出很好的低温催化活性,300℃时NO被选择还原为N2的转化率可达43%,而在Au/Al2O3催化剂上,NO的转化率仅为21%.水蒸气的加入对催化剂活性的影响较小.X射线衍射结果表明,Au和Fe2O3高度分散在Al2O3载体上.吸附氢气的程序升温还原结果表明,Au与Fe2O3之间存在着强相互作用,Au的存在促进了Fe2O3的还原,Au和Fe2O3之间的协同作用可能是Au/Fe2O3/Al2O3催化剂在丙烯选择还原NO反应中具有较高低温催化活性的原因之一.     

Investigations of potassium-cerium phosphates rich in P2O5

In the ternary system Ce₂O₃-K₂O-P₂O₅, the partial system Ce(PO₃)₃-KPO₃-P₂O₅ was examined by means of differential thermal analysis and powder X-ray diffraction. The phase compositions of the products obtained on various thermal treatments were investigated. The phase diagram of the system Ce(PO₃)₃-KPO₃-P₂O₅ is suggested.

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Zusammenfassung Mittels DTA und Röntgendiffraktion wurde im ternären System Ce₂O₃-K₂O-P₂O₅ das Teilsystem Ce(PO₃)₃-KPO₃-P₂O₅ untersucht. Die Phasenzusammensetzungen der durch verschiedene Erhitzungsvorgänge erhaltenen Produkte wurden untersucht und ein Phasendiagramm für das System Ce(PO₃)₃-KPO₃-P₂O₅ erstellt.

     

工业废气中五氧化二磷的测定

环境空气中五氧化二磷样品的采集方法主要有过氯乙烯滤膜富集法和水溶液吸收法。前者存在过滤乙稀滤膜不易获得且价格昂贵，滤膜样品需前处理，操作较为繁琐等缺点；五氧化二磷定量方法通常采用抗坏血酸或氯化亚锡作还原剂测定，氯化亚锡作还原剂方法存在显色受温度影响大，试剂空白高的缺点。本文以活性炭生产行业为例，用蒸馏水做吸收液，在抗坏血酸还原体系中，测定工业废气中五氧化二磷，并对吸收条件、样品稳定性、