Allylic Rearrangements. L. Reactions of α- and γ-Trifluoromethylallyl Alcohols with Thionyl Chloride and Thermal Decomposition of the Chlorosulfinate Intermediates1

1961 ◽  
Vol 83 (15) ◽  
pp. 3251-3258 ◽  
Author(s):  
J. A. Pegolotti ◽  
W. G. Young
Keyword(s):  
Thermal Decomposition ◽  
Thionyl Chloride

The Polymerization of Methacrylonitrile. Polymethacrylonitrile

1945 ◽  
Vol 18 (2) ◽  
pp. 267-279 ◽  
Author(s):  
Werner Kern ◽  
Helmut Fernow
Keyword(s):  
Thermal Decomposition ◽  
Hydrogen Chloride ◽  
Thionyl Chloride ◽  
Hydroxy Acid ◽  
Raw Materials ◽  
Phosphorus Pentoxide ◽  
Slight Excess ◽  
Starting Point ◽  
Pure Compounds ◽  
Ready Availability

Abstract As the starting point for the preparation of methaerylonitrile, acetonecyanohydrin (α-hydroxybutyronitrile) was chosen because of its ready availability. β-Hydroxybutyronitrile should likewise be well suited for the purpose, but, because of the difficulties involved in its preparation, it was not utilized in the work. The removal of water can be accomplished in various ways. (1) Phosphorus pentoxide does not give such smooth results as it does with ethyleneeyanohydrin, but the reaction can be carried out successfully by centrifuging and the addition of quinoline. Under the same conditions acetaldehydeeyanohydrine (lactonitrile) yields no acrylonitrile. (2) The thermal decomposition of acylated hydroxy-acid derivatives can be applied to acetonecyanohydrin, but this method of preparation is difficult to carry out on a laboratory scale. (3) Removal of water can be carried out very smoothly with thionyl chloride. In addition to methacrylonitrile, α-chloroisobutyronitrile is formed, and from the latter more methacrylonitrile can be obtained by scission of hydrogen chloride. In this procedure, it is highly important to use pure raw materials, especially thionyl chloride, for with pure compounds the yields are higher. It is likewise advantageous to use a slight excess of thionyl chloride.

REARRANGEMENT STUDIES WITH C14: XIV. THE REACTION OF 2-p-ANISYLETHANOL-1-C14 WITH THIONYL CHLORIDE

1963 ◽  
Vol 41 (3) ◽  
pp. 620-624 ◽  
Author(s):  
C. C. Lee ◽  
Donna Newman ◽  
D. P. Thornhill
Keyword(s):  
Thermal Decomposition ◽  
Thionyl Chloride ◽  
Ion Pair ◽  
Excess Thionyl Chloride

Reaction between 2-p-anisylethanol-1-C14 and thionyl chloride was carried out with pyridine, n-hexane, toluene, dioxane, or excess thionyl chloride as solvent. The 2-p-anisylethyl chloride obtained showed rearrangement of the C14 label from the C-1 to C-2 positions ranging from about 0.5% for the reaction in pyridine to about 46% for the reaction in excess thionyl chloride. The results can be explained on the basis of varying degrees of involvement of the ethylene-p-methoxyphenonium chlorosulphite ion pair, thus supporting the suggestion that thermal decomposition of alkyl chlorosulphites to give chlorides may be considerably ionic in character.

Applications of Photoelectron Microscopy

1976 ◽  
Vol 34 ◽  
pp. 506-507
Author(s):  
William J. Baxter
Keyword(s):  
Electron Microscopy ◽  
Thermal Decomposition ◽  
Chemical Composition ◽  
Ultraviolet Radiation ◽  
Thin Layer ◽  
Edge Effects ◽  
Electron Optics ◽  
Surface Layers ◽  
Crystalline Orientation ◽  
Fluorescent Screen

In this form of electron microscopy, photoelectrons emitted from a metal by ultraviolet radiation are accelerated and imaged onto a fluorescent screen by conventional electron optics. image contrast is determined by spatial variations in the intensity of the photoemission. The dominant source of contrast is due to changes in the photoelectric work function, between surfaces of different crystalline orientation, or different chemical composition. Topographical variations produce a relatively weak contrast due to shadowing and edge effects.Since the photoelectrons originate from the surface layers (e.g. ∼5-10 nm for metals), photoelectron microscopy is surface sensitive. Thus to see the microstructure of a metal the thin layer (∼3 nm) of surface oxide must be removed, either by ion bombardment or by thermal decomposition in the vacuum of the microscope.

Preparation and characterisation of vanadium pentoxide supported rhodium catalyst

1988 ◽  
Vol 46 ◽  
pp. 946-947
Author(s):  
A. Legrouri
Keyword(s):  
Aqueous Solution ◽  
Thermal Decomposition ◽  
Physicochemical Properties ◽  
Surface Area ◽  
Vanadium Pentoxide ◽  
High Purity ◽  
Gas Adsorption ◽  
Rhodium Catalyst ◽  
Optical Methods ◽  
Reducible Oxides

The industrial importance of metal catalysts supported on reducible oxides has stimulated considerable interest during the last few years. This presentation reports on the study of the physicochemical properties of metallic rhodium supported on vanadium pentoxide (Rh/V2O5). Electron optical methods, in conjunction with other techniques, were used to characterise the catalyst before its use in the hydrogenolysis of butane; a reaction for which Rh metal is known to be among the most active catalysts.V2O5 powder was prepared by thermal decomposition of high purity ammonium metavanadate in air at 400 °C for 2 hours. Previous studies of the microstructure of this compound, by HREM, SEM and gas adsorption, showed it to be non— porous with a very low surface area of 6m2/g3. The metal loading of the catalyst used was lwt%Rh on V2Q5. It was prepared by wet impregnating the support with an aqueous solution of RhCI3.3H2O.

Observations of the Thermal Decomposition of Brucite

1968 ◽  
Vol 26 ◽  
pp. 446-447
Author(s):  
P. L. Burnett ◽  
W. R. Mitchell ◽  
C. L. Houck
Keyword(s):  
Thermal Decomposition ◽  
Magnesium Oxide ◽  
Basal Plane ◽  
Magnesium Ions ◽  
A Value ◽  
Reaction Proceeds

Natural Brucite (Mg(OH)2) decomposes on heating to form magnesium oxide (MgO) having its cubic ﹛110﹜ and ﹛111﹜ planes respectively parallel to the prism and basal planes of the hexagonal brucite lattice. Although the crystal-lographic relation between the parent brucite crystal and the resulting mag-nesium oxide crystallites is well known, the exact mechanism by which the reaction proceeds is still a matter of controversy. Goodman described the decomposition as an initial shrinkage in the brucite basal plane allowing magnesium ions to shift their original sites to the required magnesium oxide positions followed by a collapse of the planes along the original <0001> direction of the brucite crystal. He noted that the (110) diffraction spots of brucite immediately shifted to the positions required for the (220) reflections of magnesium oxide. Gordon observed separate diffraction spots for the (110) brucite and (220) magnesium oxide planes. The positions of the (110) and (100) brucite never changed but only diminished in intensity while the (220) planes of magnesium shifted from a value larger than the listed ASTM d spacing to the predicted value as the decomposition progressed.

A magnetic super lattice

1987 ◽  
Vol 45 ◽  
pp. 360-361 ◽  
Author(s):  
M.D. Bentzon ◽  
J. v. Wonterghem ◽  
A. Thölén
Keyword(s):  
Thermal Decomposition ◽  
Oleic Acid ◽  
Magnetic Fluid ◽  
Magnetic Particles ◽  
Carbon Film ◽  
Thick Layer ◽  
Amorphous Iron ◽  
Super Lattice ◽  
Carrier Liquid ◽  
Median Diameter

We report on the oxidation of a magnetic fluid. The oxidation results in magnetic super lattice crystals. The “atoms” are hematite (α-Fe2O3) particles with a diameter ø = 6.9 nm and they are covered with a 1-2 nm thick layer of surfactant molecules.Magnetic fluids are homogeneous suspensions of small magnetic particles in a carrier liquid. To prevent agglomeration, the particles are coated with surfactant molecules. The magnetic fluid studied in this work was produced by thermal decomposition of Fe(CO)5 in Declin (carrier liquid) in the presence of oleic acid (surfactant). The magnetic particles consist of an amorphous iron-carbon alloy. For TEM investigation a droplet of the fluid was added to benzine and a carbon film on a copper net was immersed. When exposed to air the sample starts burning. The oxidation and electron irradiation transform the magnetic particles into hematite (α-Fe2O3) particles with a median diameter ø = 6.9 nm.

Supersonic jet spectrometry of chemical species resulting from thermal decomposition of polystyrene and polycarbonate

1992 ◽  
Vol 64 (19) ◽  
pp. 931A-940A ◽  
Author(s):  
Totaro Imasaka ◽  
Masami Hozumi ◽  
Nobuhiko Ishibashi
Keyword(s):  
Thermal Decomposition ◽  
Supersonic Jet ◽  
Chemical Species
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