US3719732A - Method for producing aluminum alloy shaped particles and active raney catalysts therefrom - Google Patents

Method for producing aluminum alloy shaped particles and active raney catalysts therefrom Download PDF

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Publication number
US3719732A
US3719732A US00099014A US3719732DA US3719732A US 3719732 A US3719732 A US 3719732A US 00099014 A US00099014 A US 00099014A US 3719732D A US3719732D A US 3719732DA US 3719732 A US3719732 A US 3719732A
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Prior art keywords
particles
aluminum
percent
alloy
shaped
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US00099014A
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English (en)
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R Diffenbach
T Cheavens
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WR Grace and Co Conn
WR Grace and Co
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WR Grace and Co
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/08—Other methods of shaping glass by foaming
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J25/00—Catalysts of the Raney type
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F2009/0804—Dispersion in or on liquid, other than with sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F2009/0804—Dispersion in or on liquid, other than with sieves
    • B22F2009/0808—Mechanical dispersion of melt, e.g. by sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • These particles can range from 1-99 percent aluminum, although for subsequent use as active metal catalysts, the concentration ranges from 50 to 90 percent aluminum and 10 to 50 percent of nickel, cobalt, copper or iron.
  • These shaped particles are produced by a melt drop technique whereby individual drops of alloy are dropped into a water bath or onto a cold flat plate.
  • a steady stream is segmentally cut by a vibrating Wire or screen to produce drops prior to contacting the water bath or plate.
  • This invention relates to the formation of shaped aluminum alloy particles. These particles are then leached to produce fixed bed Raney nickel, cobalt, copper or iron catalysts of high activity.
  • This technique comprises semisolidiied aluminum dropping through an orifice to form a teardrop particle which solidies on its short drop.
  • These techniques do not disclose methods for shaping aluminum alloys in a high surface area condition and alloys which can subsequently be leached to form highly active Raney nickel, cobalt, iron or copper catalysts.
  • This melt drop technique is a new way to form Raney catalysts, and results in catalysts of unexpectedly high activity. It is further a very convenient and comparatively inexpensive method for shaping these highly ductile alloys. Further, it produces a convenient fixed bed catalyst in contrast to the commonly used powdered catalysts which require the addition of a ltering step for removal from a product stream.
  • the present process produces aluminum alloys in shapes which, when leached to produce a Raney nickel catalyst, yield a catalyst of unexpectedly increased activity while also having the advantage that catalyst filtration steps are not required. This is a considarent erable contribution to the process industries which carry out continuous hydrogenation reactions.
  • Raney nickel, cobalt, copper and iron catalysts of comparatively low nickel, cobalt, copper or iron contents.
  • This invention comprises a process for producing shaped aluminum particles having preferred alloy concentration ranges of from to 90 percent aluminum and l0 to 50 percent of either nickel, cobalt, copper or iron or mixtures of these components. These particles are produced from a melt by allowing discrete liquid or semiliquid particles to fall onto a cooled surface or into a cooled liquid. Subsequent to particle shaping, the aluminum can be leached to yield the shaped Raney nickel, cobalt, copper or iron catalyst particles.
  • FIG. 1 is an elevational assembly view illustrating the apparatus for producing at least partially hollowed particles.
  • FIG. 2 is an elevational assembly View illustrating the apparatus using a vibrating screen and a grooved rotating drum.
  • FIG. 3 is an elevational assembly view illustrating the apparatus using a vibrating screen and a cooled plate having raised ribs.
  • FIGS. 4 and 5 illustrate some of the shapes of the resulting particles.
  • this invention comprises methods of forming aluminum-nickel, aluminum-cobalt, aluminum-copper and aluminum-iron alloys, or mixtures, into shaped particles of comparatively high surface area.
  • This property of high surface area is of concern, since the preferred end use for these shaped particles is in the formation of highly active metal catalysts of the Raney type.
  • a Raney nickel, cobalt, copper or iron catalyst is one in which the nickel, cobalt, copper or iron has been put in a high surface area, highly active condition via the technique of alkali leaching the aluminum content out of the alloy.
  • the end Raney catalyst has essentially the same shape as the form of the shaped aluminum alloy. This technique allows for the shaping of the catalystic material in the unactivated form, and then activating for subsequent use while maintaining the predesigned shape.
  • these soft, ductile alloys can be shaped into high surface area active catalyst particles at a low cost for equipment and alloy. This is a significant advance in the art, permitting hydrogenation reactions to be more easily carried out by the use of fixed bed catalytic reactors.
  • this invention is directed to a means for producing a fixed bed Raney catalyst material.
  • the shape, size and other features of the catalyst particles would have to be such that they would not become entrained in the product stream, would further have to be crush resistant, while having a high surface area and being highly active.
  • the basic technique most useful for alloy shaping is melt forming, that is, putting the alloy into a shape while in a melt condition with subsequent cooling to ambient temperatures.
  • the shapes of preferred importance are those of FIGS. 4 and 5, although essentially any shape can be utilized.
  • the aim of any shape, however, is to attain a high surface area while maintaining crush resistance and still minimizing pressure drop on the fixed bed reactors.
  • the shapes of this invention are produced by dropping molten alloy into or onto a cooled medium. When dropped onto a cold medium such as a plate, the drop will spread to the form of a disc. If a shaped cold surface is used, the drop will form a shape complementary to the cold surface to which it was contacted.
  • the drop When dropped into a cold medium, which can be Water or some surface, the drop deforms to form a novel shape depending on the liquid, the energy of the falling drop, and its melt condition.
  • the preferred particle shape from this technique is an essentially hollow, partially spherical particle. Particles of any of these types have proven to subsequently yield very active Raney catalysts.
  • FIG. 1 illustrates the embodiment of dropping molten Ni-Al particles into a liquid.
  • 1 here is a containing vessel of a material which can withstand temperatures of 650 C. to 1000 C.
  • 2 is the base plate of vessel 1, and 3 the holes in the base plate to allow flow of the alloy melt.
  • 4 is the liquid alloy, and 5 the molten metal level.
  • molten drops 6 are formed which fall into vessel 7 ⁇ which contains cooling liquid 8.
  • the molten drops strike the liquid surface 10, they are slightly deformed, and in some instances they trap liquid therein which is then usually vaporized out of the hot particles, which vaporizing appears to hollow out the particle. The cooled, shaped particles then fall to the bottom of the vessel.
  • the alloy should be maintained in the range of 10 C. to 100 C. above its melting point.
  • the holes 3 should range in size from %,2 inch to l1A; inch, and the molten metal head 5 should be about 2 inches to v24 inches. These parameters insure a ilow of metal through the base plate 3 to form drops or a stream which can be subsequently cut.
  • the height of the vessel-1 above level 10 of vessel 8 is also of importance. This should range from 3-24 inches so that the drops 6 will not be solidified prior to striking liquid level 10.
  • the level 5 can be greater than 24 inches if smaller holes 3 are used, or if the temperature is maintained at near the alloy solidiiication range. Further, if a superheated metal is used, the distance of base plate 3 from surface 10i can be greater without any likelihood of particle solidiiication. Other variations are also possible, but these are considered to be within the present concept.
  • the liquid is 8 in vessel 7 is preferably water, but can also be an organic solvent, or a mixture of organic solvents and Water.
  • the function of this liquid is to aid in forming the particle to a shape.
  • the liquid aids in forming the particle by ⁇ flattening the molten drop as it strikes the surface, and by the liquid being partially encapsulated by the cooling drop, so that as it cools it vaporizes this encapsulated liquid and causes the formation of at least partially hollow particles.
  • This dual function of cooling and shaping is an essential feature of this invention.
  • the temperature of the cooling liquid, and the condition of the surface and subsurface can vary widely within the bounds of this process.
  • this may range in temperature from 1 C. to 99 C.
  • this solution may be mixed under mild to vigorous agitation, turbulently or symmetrically, to further shape and produce uniquely characteristic particles. These are some modifications which can be used to vary the shapes and characteristics of the particles.
  • FIG. 2 sets out an apparatus and technique similar to that of FIG. l.
  • the differences are essentially that the molten alloys flows from the baseplate holes 3 in continuous streams, these streams being continuously cut by the vibrating wire grid ,13.
  • This grid 13 has a series of wires 14 which may be in the form of a screening grid, but preferably are solely in one direction.
  • This grid is then vibrated at frequencies of from 2. c.p.s. (cycles per second) to c.p.s., depending on the number of wires in the grid.
  • the amplitude of each vibration is such that each stream is cut twice by a Wire 14 of the grid during each complete vibration cycle. lIt is preferred that the molten stream be cut from 24 to 100 times per second.
  • container 17 After being cut by the grid, the drops fall on cooled drum 15, and are collected in container 17. 'Ihe particles which fall onto drum 15 are given a hat shape by grooves 16 in drum 15. On rotation of drum 15, the particles will fall into container 17. Further, container 17 can have an incorporated hopper or other device for further handling of the formed particles.
  • FIG. 3 illustrates an essentially hat cooling plate 18 onto which the molten droplets fall.
  • 19 are the inlets and outlets for the plate or drum cooling fluids.
  • This embodiment provides a means whereby the slope of the plate causes the particles to fall into the collection container.
  • Raised ribs 20 serve to shape the drops which strike the plate 18.
  • the particles may be formed from drops falling from apertures 3 in base plate 2, or by use of the vibrating grid molten stream slicing technique.
  • the energy of the falling particle will determine the degree of spread when the drop hits the plate. Therefore, in a preferred technique, the vessel 1 is maintained at a height of from 6 inches to 12 inches above the forming and cooling plate or drum.
  • the surface of the plate or drum may be dimpled, grooved, or otherwise shaped so as to produce a particle of a shape of other than a flat disc.
  • FIG. 4 illustrates a particle formed from a grooved plate or drum. This shape is preferred over a hat disc in iixed bed catalyst use, since there is a decreased tendency to pack tightly, with a resulting loss of effective surface area and increase in pressure drop.
  • the particles of FIG. 5 are those produced by the technique of FIG. l of dropping the alloy into a cooled water tank.
  • any of the known techniques can vbe used. This consists essentially of leaching from to 50 percent of the aluminum content from the particle with sodium hydroxide. The amount of aluminum leached is determined from the volume of hydrogen evolved. 1 mole of aluminum will evolve 1.5 moles of hydrogen gas on leaching.
  • the catalyst can be immediately used or stored in various media.
  • the shaped particles comprise an aluminum content of about 50 to 90 percent by weight and a nickel content of about 10 to 50y percent by weight, with the shaped active catalyst particles comprising an aluminum content of about 33 to 91 percent by weight and a nickel content of about 9 to 67 percent by weight.
  • Alloys of from l to 99 percent aluminum can be shaped using the instant technique, 'but due to the friability after leaching of those particles greater than 90 percent aluminum, these are not as useful. Further, the catalyst particle should contain at least 10 percent of the nickel cobalt, copper or iron component.
  • a molten Ni-Al alloy (20 percent Ni, 80 percent Al) at about 800 C. is poured into a graphite crucible tube which has a series of twelve 1/16 inch holes in a base plate area.
  • the crucible is maintained at about 800 C., and a head of molten alloy at 10 inches. At this head of molten metal discrete drops form and fall into the water containing vessel.
  • the height of the baseplate to the Water surface is 12 inches.
  • a kilogram of particles are produced, the shape being essentially that of FIG. 5.
  • Example II The procedure of Example I is repeated, but using a Co-Al alloy of 30 percent cobalt and 70 percent aluminum content. The temperature of the molten metal is maintained at 950 C., with the height of the baseplate above the water being 12 inches. Particles of essentially the same shape as FIG. 5 are formed.
  • EXAMPLE III In this example, a series of NiAl alloy particles are formed using the apparatus of FIG. l, but with a vibrat ing screen included to cut the molten alloy streams.
  • the alloy series of the table are each heated to about 800 C. and poured into a graphite crucible so as to maintain a molten metal head of about 20 inches.
  • a Tyler 3 mesh screen that is a screen having M1 inch openings, is used as the vibrating grid.
  • the screen vibration rate is 4 c.p.s. This vibrating grid is placed about 3 inches below the grid.
  • particles nches below the grid On impact with the water, particles shaped essentially as shown in FIG. 5 are formed, these particles having a diameter of from about 1A to 1/2 inch.
  • Example II Ille procedure of Example I is repeated, but using an Fe-Al alloy of percent by weight aluminum and 20 percent by weight iron. The temperature of the molten metal is maintained at 950 C. with the height of the baseplate above the water being l0 inches. Particles of essentially the same shape as FIG. 5 are formed.
  • a method for producing shaped active catalyst particles comprising:
  • melt consisting essentially of an alloy selected from the group consisting of aluminum-nickel, aluminum-cobalt, aluminum-iron yand aluminumcopper, said melt being maintained in the range of 10 C. to 100 C. above the melting point of said alloy;
  • said alloy further contains from about 1 to 15 percent of a promotional material selected from the group consisting of chromium and molybdenum.
  • shaped particles are shaped aluminum-cobalt alloy particles containing about 50 to 90 percent aluminum and 10 to 50 percent cobalt.
  • said shaped particles are shaped aluminum-copper alloy particles containing about 50 to 90 percent aluminum and 10 to 50 percent copper.
  • said shaped particles are shaped aluminum-iron alloy particles containing about 50 t0 90 percent aluminum and 10 to 50 percent iron.
  • said shaped particles comprise an aluminum content of about 50 to 90 percent by weight and a nickel content of about 10 to 50 percent by weight, with said shaped active catalyst particles comprising an aluminum content of about 33 to 91 percent by weight and a nickel content of about 9 to 67 percent by weight.
  • a method for producing shaped active catalyst particles comprising:
  • melt consisting essentially of an alloy se-r lected from the group consisting of aluminum-nickel, aluminum-cobalt, aluminum-iron and aluminumcopper, said melt -being maintained in the range of 10 C. to 100 C. above the melting point of said alloy;
  • said cooled metal surface is a cooled plate having raised ribs.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
US00099014A 1970-12-17 1970-12-17 Method for producing aluminum alloy shaped particles and active raney catalysts therefrom Expired - Lifetime US3719732A (en)

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BE (1) BE776828A (enExample)
CA (1) CA1023119A (enExample)
DE (1) DE2162111A1 (enExample)
FR (1) FR2118707A5 (enExample)
IT (1) IT944039B (enExample)
NL (1) NL7117247A (enExample)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4127158A (en) * 1973-10-15 1978-11-28 Toyo Kohan Co., Ltd. Process for preparing hollow metallic bodies
US4450885A (en) * 1977-11-12 1984-05-29 Mizusawa Kagaku Kogyo Kabushiki Kaisha Process for preparation of granules of low-melting-point metals
US4580967A (en) * 1984-09-12 1986-04-08 Sociedad Anonima de Racionalization y Mechanization (Sadrym) Machine for obtaining spherical bodies from jellifiable liquids
US5154220A (en) * 1990-12-06 1992-10-13 Crawford Tommy N Method and apparatus for making metal shot
EP0773063A1 (en) * 1995-11-08 1997-05-14 Towa Chemical Industry Co., Ltd. Raney catalyst, process for producing it and process for producing a sugar-alcohol using the same
RU2180264C2 (ru) * 1996-08-01 2002-03-10 Уреа Касале С.А. Способ контролируемого диспергирования струй жидкости и устройство для его осуществления
US20050120827A1 (en) * 1999-04-12 2005-06-09 Fetcenko Michael A. Method of making a catalyst
US20080161185A1 (en) * 2006-12-25 2008-07-03 Khabibullin Farkhat K Catalyst for Hydration of Vegetable Oils, Fats and Fatty Acids
EP2845671A1 (en) * 2013-09-05 2015-03-11 Uvån Holding AB Granulation of molten material
US10618112B2 (en) 2013-09-05 2020-04-14 Uvan Holding Ab Granulation of molten material

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4175954A (en) * 1978-07-24 1979-11-27 The United States Of America As Represented By The United States Department Of Energy Self-disintegrating Raney metal alloys
FR2972729A1 (fr) * 2011-03-14 2012-09-21 Univ Joseph Fourier Procede et dispositif pour la formation de billes de verre metallique

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4127158A (en) * 1973-10-15 1978-11-28 Toyo Kohan Co., Ltd. Process for preparing hollow metallic bodies
US4450885A (en) * 1977-11-12 1984-05-29 Mizusawa Kagaku Kogyo Kabushiki Kaisha Process for preparation of granules of low-melting-point metals
US4580967A (en) * 1984-09-12 1986-04-08 Sociedad Anonima de Racionalization y Mechanization (Sadrym) Machine for obtaining spherical bodies from jellifiable liquids
US5154220A (en) * 1990-12-06 1992-10-13 Crawford Tommy N Method and apparatus for making metal shot
US6995107B2 (en) 1995-11-08 2006-02-07 Towa Chemical Industry Co., Ltd. Raney catalyst, process for producing it and process for producing a sugar-alcohol using the same
EP0773063A1 (en) * 1995-11-08 1997-05-14 Towa Chemical Industry Co., Ltd. Raney catalyst, process for producing it and process for producing a sugar-alcohol using the same
EP0951938A1 (en) * 1995-11-08 1999-10-27 Towa Chemical Industry Co., Ltd. Process for producing a Raney catalyst
KR100310189B1 (ko) * 1995-11-08 2002-01-15 아사이 요시히사 라니촉매,이의제조방법및이를사용한당(糖)알콜의제조방법
US20050153837A1 (en) * 1995-11-08 2005-07-14 Towa Chemical Industry Co., Ltd. Raney catalyst, process for producing it and process for producing a sugar-alcohol using the same
RU2180264C2 (ru) * 1996-08-01 2002-03-10 Уреа Касале С.А. Способ контролируемого диспергирования струй жидкости и устройство для его осуществления
US20050120827A1 (en) * 1999-04-12 2005-06-09 Fetcenko Michael A. Method of making a catalyst
US7045484B2 (en) * 1999-04-12 2006-05-16 Ovonic Battery Company, Inc. Method of making a catalyst
US20060205590A1 (en) * 1999-04-12 2006-09-14 Fetcenko Michael A Method of making a catalyst
US7462577B2 (en) * 1999-04-12 2008-12-09 Ovonic Battery Company, Inc. Method of making a catalyst
US20080161185A1 (en) * 2006-12-25 2008-07-03 Khabibullin Farkhat K Catalyst for Hydration of Vegetable Oils, Fats and Fatty Acids
EP2845671A1 (en) * 2013-09-05 2015-03-11 Uvån Holding AB Granulation of molten material
US10618112B2 (en) 2013-09-05 2020-04-14 Uvan Holding Ab Granulation of molten material

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Publication number Publication date
BE776828A (fr) 1972-04-17
FR2118707A5 (enExample) 1972-07-28
NL7117247A (enExample) 1972-06-20
IT944039B (it) 1973-04-20
CA1023119A (en) 1977-12-27
DE2162111A1 (de) 1972-07-06

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