Rare Earth Process Gets Trial
Transcript of Rare Earth Process Gets Trial
Meter Chemicals With this Controlled
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H e r e ' s t h e p u m p for p rec i s e m e t e r i n g of chemica ls in con t ro l led v o l u m e . H a n d l e s p r ac t i ca l ly a n y l iquid , f rom heavy v iscous l iqu ids to l igh t solvents, sol ids in suspension, abrasive s lurr ies , liquefied gases, and o the r " h a r d - t o - h a n d l e " materials .
Ava i lab le w i th f rac t ional or int e g r a l h o r s e p o w e r g e a r - h e a d m o t o r s . Capac i t i e s from 3 mill il i te rs t o 2700 gallons per hou r , aga in s t pressures t o 50,000 psi . Flexib ly a d a p t a b l e to manual , s e m i - a u t o m a t i c o r a u t o m a t i c con t ro l of c a p a c i t y . Simplicity is t h e k e y n o t e .
W r i t e for specifications and d a t a o n y o u r app l i ca t ion . Milton R o y C o m p a n y , Manufacturing Engineers, 1300 E a s t M e r m a i d L a n e , Ph i l ade lph ia 18, P a .
P R O D U C T I O N
Rare Earth Process Gets Trial Liquid ion exchange basis of rare earth separation method being developed by Horizons, Inc.
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A . RARE EARTH SEPARATION process expected to combine the high capacity of solvent extraction with the high efficiency of ion exchange is about to get bench scale trials at Horizons, Inc. in Cleveland. Devised by Ronald C. Vickery, who heads Horizons' chemistry department, it's essentially a liquid ion exchange process using 2-diethylhexyl-phosphoric acid in a petroleum ether carrier. Chief advantages expected: unusually sharp separations and adaptability to continuous operation.
Such a method had been on Vickery's mind for some time, when he ran across a solvent extraction process developed by Colorado School of Mines for uranium refining. It used dodecylphos-phoric acid in a kerosene carrier. The mechanism looked like ion exchange, and Vickery hastened to try it on rare earth separations.
An early move was the switch from D D P A , with its one exchangeable hydrogen, to D H P A which has two exchangeable hydrogens. Another change substituted petroleum ether for the kerosene carrier, which gave intractable emulsions w h e n used with rare earths.
• The Process Today. As the process now stands, D H P A (0.1 Molar) in petroleum ether contacts a water solution of mixed rare earth chlorides. The rare earths move very quickly into the petroleum ether, from which they are extracted with ammonium citrate. By regulating the p H of the extractant and its weight ratio to the petroleum ether layer, Vickery finds he can get preferential extraction of individual rare earths. These are then precipitated as oxalates and fired to oxides.
L a b separations to date, says Vickery, have averaged 97% recovery (as oxides) of individual rare earths at 99 .5% purity. Mixed chlorides of gadolinium, europium, and samarium, for instance, can be separated much more readily this way than by sodium amalgam reduction, a standard method, he says. Samarium and europium ox
ides come out close to 99.9r> pure; the gadolinium contains about 0.2% samarium. From a 50-50 mixture of yttrium and erbium chlorides, another difficult separation, the method recovers about 99 # of the yttrium, 9 8 ^ of the erbium. Purity is better than 99'.'* for each.
• The N e x t S tage . Vickery's next move is a bench-scale arrangement of 200 cc. columns set up in series. Feed will most likely be a mixture of chlorides of heavy- and light-group lantha-nons previously separated from mona-zite and xenotime. Initial contact will move these chlorides from water solution into the DHPA-petroleum ether layer, which will then move through the columns in series, countercurrently to the ammonium citrate extractant.
In each column, ammonium citrate of the proper pH and amount will preferentially extract one rare earth. Extracted rare earths will come off the bottom of each column for precipitation and firing. Barren DHPA-petroleum ether, from the last extractant column, will pass through an acid column to get back into the hydrogen cycle, then return to the initial contacting column.
Vickery plans to set this system up to run continuously for about 14 days. He believes it will separate roughly 900 grams a day of mixed rare earth chlorides. It's too soon, he says, to discuss the engineering aspects of running the method on a very large scale. But if it works out as expected, commercial production would not require a very large system. One disadvantage is the use of petroleum ether, requiring a closed system; none of the less flammable carriers tried so far seem to work as well. At this stage, however, Vickery believes that both the economics and products of the process will be very competitive. This opinion includes working the process into existing mon-azite-treating plants which, he believes, could be done with little difficultv. m
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Plate Gold Chemically Dip coating process plates gold by ionic displacement
C H E M I C A L GOLD-PLATING passes another milestone this week. Baker & Co., Newark, N. J., refiner of precious metals, has come up with a water soluble gold/amino complex which is said to reduce plating costs by 25% through use of less gold than in electroplating.
An important industrial use is foreseen on copper in electric and electronic applications, the company says. Copper foil patterns on printed circuits are sometimes gold plated for solderability. Other possibilities: trophies, costume jewelry, metallized plastics.
No electricity is needed for chemical plating. Objects to be coated are immersed in a heated bath . Gold displaces metal ions from the surface and is reduced to metal on the spot. Deposed ions are inactivated by chelation and carried out into the body of the solution. When a 24 karat film has been deposited over the whole surface, the process stops itself, Baker claims.
On most metals (iron, steels except stainless, die casting alloys, soft solder), an average of 1 mg. of gold pe r square inch deposits in a few minutes. The higher the temperature, the more rapid is deposition. Final coating thickness ranges up to a quarter of a micron on most of these metals, although "flash" coatings can be applied by pulling the sample from the bath before plating action stops by itself.
• Nitration of glycerol, glycol, and allied products by a new Swedish process is safer and cheaper than present methods, according to Nitroglycerin Aktie-bolaget of Sweden. An injector transfers nitrated products as a nonexplosive spent acid emulsion to a separate area. There the ester is removed b y a centrifugal separator running without direct supervision.
• Antibiotic treatment of western white pine trees has saved thousands of them from blister rust, according to a U. S. Forest Service forester. A four-year test of Acti-dione, an Upjohn fungicidal antibiotic, has shown that t reatment gives control of the fungus in some 80% of the trees.
D O M E S T I C ores mined a n d processed domestically for American industry! T h a t ' s the story of HEAVY MINERALS C O . ' S new Chattanooga plant now approaching peak production.
The plant, one of the most modern of its kind in the world, processes its own plentiful supplies of rare earth-bearing raw materials. HEAVY MINERALS C O . now has available in quantity any mixed rare earth compound or pure rare earth compound for industrial use.
Purified rare earths impar t unique qualities to metals, glass, ceramics a n d illuminating materials. New, exciting applications are being developed for the nuclear and chemical industr ies .
Heavy Minerals ' integrated domestic rare earths operation is supported by a team of research specialists ready to share its experience with you.
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PRODUCTION
• An ion generating tube which contains not more than 50 millicuries of tritium may be put under a general license by the Atomic Energy Commission. The AEC has proposed an amendment to its by-product material (radioisotope) regulation to permit possession and use without a specific license from the commission. The tube that is being considered is designed for use in air conditioning equipment.
• Laminagage, a tool used to check platings and coatings on metals, will now be manufactured, under license, by Gulton Industries, Inc. General Motors Corp. holds the patent rights. The instrument measures the thickness of enamel or ceramic coatings and metal platings. It will also detect pinholes and flaws in production line items.
• Improved cotton bleaching process has been developed by Solvay Process Division of Allied Chemical & Dye. The new process adds a prebleacbing step with specially prepared hypochlorite solution after caustic purification and before hydrogen peroxide exposure. Resulting advantages, according to Allied: higher brightness, brightness retention, absorbency, and dye-abibty, with reduced ash and metals content—all at reduced bleaching cost.
• A water washing system for semiconductors has been adapted from tube techniques by Miles V. Sullivan of Bell Telephone Laboratories. The system uses distilled water to remove water soluble materials from the semiconductors after etching. Wash effectiveness is monitored by electrical conductivity of the wash water. Bell claims the system has given improved breakdown voltage, sharpness of voltage-current characteristics, saturation current, and emitter reverse impedance.
> Niobium and iron can be recovered along with titanium from low grade Arkansas materials by a process developed by Bureau of Mines at Rolla, Mo. The ore is concentrated, sintered, and chlorinated at less than 500° C. Fractional distillation yields the titanium, niobium, and iron. The process has been tried on brookite and rutile (two titanium minerals) and on two types of alumina plant wastes containing titanium minerals.
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