PROCESS DEVELOPMENT QUARTERLY REPORT. PART I--LABORATORY WORK

Technical Report · Wed Jul 01 04:00:00 EDT 1959

OSTI ID:4227167

Shepardson, J U; Nelson, J.A. eds.

4 4 3 4 8 3 5 7 g program of refinery streams has again shown that aqueous entrainment in the TBP-hexane extract is responsible for the major fraction of the impurities in refinery NOK liquors. In particular it was demonstrated that sodium, magnesium, vanadium, iron, and molybdenum contamination of the final product could be effectively reduced by reducing this aqueous entrainment. Distribution data for extraction of uranium into 30% TBP-hexane in the presence of sulfate has been gathered over a wide range of concentrations. The rate of reduction of fluid beddenivated UO/sub 3/ was found to increase with an increase in surface area and with increase in reduction temperature in the range 528 to 647 deg C. The nature of the hydrofluorination reaction depends upon the type of particles used as starting material. In very thin beds one type of fluid-bed-denitration product has an increasing hydrofluorination rate with temperature in the range 380--620 deg C, while in thicker beds thermal damage is observed. A second type of UO/sub 3/, consisting of spongelike aggregates of smaller particles, showed thermal damage in thin beds (445 deg C rate > 640 deg C rate). Two distinct types of UO/sub 3/ have been prodced in the fluidbed- denitrator. Both types are characterized by low surface area, and both reduce to a brown oxide of relatively high surface area. The product of pilot plant runs prior to run 61 can be characterized as being made up of a shell surrunding a concentric, layer-type structure. The product of later runs have an interior made up of spongy matter without the concentric rings. Although both types of material are thermally damaged at high temperature, the latter material was the more susceptible. The rate of hydrofluorination of flameprocessed UO/sub 2/ is apparently controlled by two consecutive mechanisms a) adsorption of HF on the available rent activaF and f 10 kcal/mole. The observed rate for the final 50% of hydrofluorination is proportional to the first power of the HF mole fraction in HF-Argon mixtures. Activated charcoal appeared to be the best method of adding carbon to small bombs. Neither hydrogen nor metal yield was adversely affected in the production of metal containing 400-500 ppm carbon. A careful quantitative s indicates that a) the hydrogen in U metal is primarily dein the bomb at firing and b) at constant hydrogen content, the degree of contaimination is proportional to the maximum pressure occurring during the reaction. Good of metal made in 4-kg bombs and that from 3300-lb dingots was obtained when the small scale bombs were fired with center temperatures approximating those of the large dingot. Bomb changes held at temperatures of 300 deg C or higher show a decrease in the hydrogen in as-reduced metal with increased time at temperatures before firing. Soaking at 250 deg C was ineffective in reducing hydrogen. The magnitude of this effect seems to depend on the water soluble content of the greensalt. Four-kg bombs containing added water (equivalent to 280 to 1120 ppm hydrogen) produced metal with hydrogen content providing all bombs were fired at similar center temperture. Examination of plane sections taken at various distances from the quenched end of Jominy-type spccimens by inverse pole figure and growth indices'' reveal similar structures in uranium, which prior to beta quenehing had been: a) gamma-extruded, alpha-rolled dingot; b) alpha-forged., alpha-rolled dingot; c) or alpha-rolled ingot. The rate controlllng role of nitrous acid concentration in the

• Research Organization: Mallinckrodt Chemical Works, St. Louis
• NSA Number: NSA-13-018768
• OSTI ID: 4227167
• Report Number(s): MCW-1430
• Country of Publication: Country unknown/Code not available
• Language: English

Related Subjects

ACTIVATED CARBON-- CONTAMINATION-- EXPLOSIONS-- HYDROGEN-- NUCLEAR EXPLOSIONS-- NUCLEAR REACTIONS-- PRESSURE-- PRODUCTION-- QUANTITATIVE ANALYSIS-- REDUCTION-- SOLUBILITY-- TEMPERATURE-- URANIUM-- URANIUM TETRAFLUORIDE-- WATER-- WEIGHT
ADSORPTION-- ARGON-- CONTROL-- DIFFUSION-- ENERGY-- FILMS-- HEAT TREATMENTS-- HYDROFLUORIC ACID-- MIXING-- SURFACES-- URANIUM DIOXIDE-- URANIUM TETRAFLUORIDE-- WATER
ALLOTROPY-- CONFIGURATION-- EXTRUSION-- FORGING-- HEAT TREATMENTS-- QUENCHING-- ROLLING-- URANIUM
ARSENIC-- CHEMICAL REACTIONS-- COBALT-- COMPLEXES-- COPPER-- EDTA-- IMPURITIES-- IRON-- MOLYBDENUM-- ORGANOMETALLICS-- SODIUM COMPOUNDS-- TUNGSTEN-
TECHNOLOGY