Electroinitiated polymerization of tetrahydrofuran (THF) was accomplished in 1MLiClO4‐THF organic electrolyte solutions by anodic electrolysis on platinum electrodes in a three‐compartment cell. THF was found to polymerize to form a viscose gel at 25°C. The rate of polymerization was followed by measuring the electrical resistance of the organic electrolyte solution as a function of time after the electroinitiation. The rate of polymerization was found to increase with the increase in the anodic charge passed. The average molecular weight of the polymer was determined to be 2×105 by viscometry. The polymer was found to be “living” in nature. Electrochemical evidence was presented to show that the initiation occurred as a result of the electro‐oxidation of THF rather than the ClO4− anion.
An alternative to a secondary battery as the power source for vehicle propulsion is a fuel cell, an example of which is the metal-air cell using metals such as aluminum, zinc, or iron. Aluminum is a particularly attractive candidate, having high energy and power densities, being environmentally acceptable and having a large, established industrial base for production and distribution.An aluminum-oxygen system is currently under development for a UUV test vehicle and recent work has focussed upon low corrosion aluminum alloys, and an electrolyte management system for processing the by-products of the energy-producing reactions.This paper summarizes the progress made in both areas. Anode materials capable of providing high utilization factors over current densities ranging from 5 to 150 mAJcm 2 have been identified, such materials being essential to realize mission life for the UUV. With respect to the electrolyte management system, a filter/precipitator unit has been successfully operated for over 250 hours in a large scale, half-cell system.
The anodic oxidation of A,iV-dimethylformamide has been studied in methanol and in acetic acid, with fluoroborates, nitrates, and acetates as the supporting electrolytes. The operation of two oxidation mechanisms has been demonstrated. In the one, the primary reaction is an electron transfer from the amide to give a cation radical. In the other, the initiating reaction is an electron transfer from nitrate ion to give a nitrate radical. With a nitrate salt as the supporting electrolyte, both mechanisms operate, and the conditions under which each occurs have been defined.There is evidence that, in acetic acid containing acetate ion, IV,IV-dimethylamides Oxidize at a lower potential than acetate ion.1•2 3and the first step in the oxidations to form IV-acetoxymethyl-IV-methylamides is an electron transfer from the amide substrate. Nevertheless, when these reactions are run at constant current for preparative purposes, the coulombic efficiencies arc low, and a significant portion of the charge passed is used in the Ivolbe oxidation of acetate ion to give ethane and carbon dioxide.lb
A comparative study of the involvement of surface oxides of platinum in the anodic oxidation of (a) formate, (b) hydrocarbons, and (c) hydrazine has been made. In case (a) the oxidation has also been studied in two rigorously dehydrated nonaqueous solvents, acetonitrile and propylene carbonate, to which were successively added initially traces and later larger quantities of water. Activation and inhibition effects arise and are related to the water content of the solutions. The oxide coverages were determined at various potentiostatically held potentials E by cathodic galvanostatic and differentiated galvanostatic transients for ascending and descending directions of change of E . Complications which may arise in the quantitative interpretation of results obtained from the repetitive potentiodynamic method are illustrated.
produced c/s-2-methylthiocyclopentanol (9.8 g, 74%), bp 52-54°( 0.3 mm); nmr 5 4.05 (m, 1 CHOH), 3.03 (d, 1,J = 2.5 Hz, OH), 2.95 (m, 1, C/íSCHg), 2.08 (s, 3, SCH3), and 1.74 (m, 6, (CHs)a).2-Methoxy-l-propanol and 1-methoxy-2-propanol were prepared by the acid-catalyzed ring opening of propylene oxide in methanol according to a known procedure,26 and the isomers were separated by preparative glpc.1-Methylthio-2-propanol was prepared by the procedure of Bordwell and Andersen:27 bp 67-69°(20 mm) [lit.27 bp 55-58°(10 mm)].2-Methylthio-l-propanol was prepared as follows: a mixture of 1-propenyl acetate (10 g, 0.1 mol), methanethiol (60 g), and benzoyl (26) S.
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