US2875033A - Method of separating titanium crystals - Google Patents

Description

United States Patent 2,875,033 METHOD OF SEPARATING TITANIUM CRYSTALS Lester D. Grady, Palmerton, Pa., assignor to The New Jersey Zinc Company, New York, N. Y., a corporation of New Jersey N0 Drawing. Application June 11, 1957 Serial No. 664,898

8 Claims. c1. 75-5 This invention relates to the production of titanium metal, and more particularly to the recovery of the highest purity fraction of a mass of electrodeposited titanium metal.

In the electrolytic production of titanium metal, the metal is obtained as a massive deposit on the electrolytic cell cathode. Inasmuch as the electrolysis is predicated upon electrolytic decomposition of a titanium compound carried in a fused halide salt bath, the titanium deposit on the cathode contains a considerable amount of occluded salt from the bath. And when the cathode deposit is harvested by bodily withdrawing the cathode r and its deposit from the fused salt bath, a further considerable quantity of salt adheres to the surface of the deposit. Accordingly, the recovery. of the titanium metal component of this cathode deposit requires separation of the entrained salt from the metal, and this is usually achieved by leaching the salt away from the metal after the massive cathode deposit has been crushed to expose the entrained salt.

The lattice work of titanium metal in the cathode deposit is composed of a dendritic mass of titanium crystals having a large range of particle sizes. The finer crystals, to the extent that their surfaces are exposed, have a larger ratio of surface area to volume than do the coarser crystals, and consequently there is more opportunity for surface oxidation per unit of volume in the case of the fine crystals than in the coarse crystals. In

' attemptingto recover titanium metal of the highest purity from the electrolytic deposits it is natural to attempt separation of the fine, impure, high-oxygen containing particles of titanium from the higher purity, coarse material. In addition coalesced granules coarser than 8 mesh need to be broken down into their component. individual crystals so that any entrained impure fines may be removed in later sizing operations. While this may appear to be a simple operation, many methods and different types of apparatus have been triedwith little success. The difiiculty is that titanium metal of high purity is soft, and milling methods that function by impact simply compress the soft metal granules without shattering them into their individual components. Prolonged ball milling, for example, willproduceflakes of metal in which very fine, highly impure, titanium particles are embedded. These embedded particles cannot be removed from the purer larger particles by subsequent screening or elutriation operations.

In my copending application Ser. No. 628,709, filed December 17, 1956, now U. S. Patent No. 2,821,468, there is described a method of selectively separating relatively pure and relatively impure crystals of electrolytically deposited titanium metal from a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts.

This selective separation is accomplished without the distortion and welding together of the particles of titanium characteristic of the aforementioned milling procedure.

2,875,533 Patented Feb. 24, 1959 ice The method of my copending application comprises first crushing the cathode deposit to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one-quarter inch screen openings, leaching the crushed mass with an aqueous medium to dissolve the electrolyte salts away from the titanium metal, and disintegrating the residual mass of titanium metal predominantly into its own component crystals with a scissor-like action between cutting blades spaced apart a distance at least as great as the maximum particle size of the individual titanium crystals of the cathode deposit. The blades move at sutficiently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, and a chemically inert atmosphere is maintained surrounding the mass of titanium metal While it is being disintegrated. The resulting disintegrated mass is classified by screening, elutriation, centrifuging, or the like, to separate a relatively pure fraction composed of the relatively coarse titanium crystals from a relatively impure fraction composed of the relatively fine titanium crystals.

As explained in my aforementioned copending application, the scissor-like shearing action of the cutting blades disintegrates the mass of titanium metal for the most part into its component crystals, and subsequent classification of this disintegrated mass of titanium crystals to elfect separation of a fraction composed of relatively coarse titanium crystals from a fraction composed of relatively fine titanium crystals also effects a corresponding separation of the titanium crystals into a fraction composed of relatively pure titanium and a fraction composed of relatively impure titanium. The efficiency of this separation of the titanium crystals into fractions composed of relatively pure and relatively impure titanium is remarkably high. However, I have now found that this separation can be made even more efficient and precise if the thusalisintegrated mass of titanium crystals is subjected to a special scrubbing operation in an aqueous medium following the aforementioned disintegration operation and prior to the final classification operation. The special scrubbing action is eifected by vigorous agitation of the aqueous medium in which the titanium crystals are suspended. This vigorous agitation of the aqueous medium causes the aqueous medium and the metal crystals suspended therein to impinge against each other and to substantially completely dislodge all metal crystals that may be clinging together either as a result of cohesion or mechanical entrainment. With each individual crystal thus scrubbed clean and separated from all other crystals of whatever size, the resulting disintegrated scrubbed mass of crystals can be far more accurately classified into fractions composed of crystals of a definite particle size range. As a result, the fraction composed of relatively large sized crystals of titanium is substantially completely free of any residual crystals of a relatively smaller size, and therefore the purity of the fraction composed of the relatively large crystals of titanium is greatly enhanced.

Accordingly, my invention comprises an important improvement in the process of the aforementioned copending application. In the practice of the present invention the harvested cathode deposit composed of metallic titanium and entrained electrolyte salts is first broken up by any conventional crushing operation. A jaw crusher is wholly satisfactory for this purpose, but regardless of the apparatus used in this operation the cathode deposit should not be crushed fine enough to cause such comitate extraction of the entrained salt, the major amount of disintegration of the titanium metal into its own component crystals being effected by the scissor-like shearing impact action to which the salt-free mass is subjected, together with the subsequent vigorous scrubbing action pursuant to the invention. For example, a relatively low metal-content cathode deposit composed of about 35% by weight of metallic titanium and the balance entrained salt should not be crushed finer than-that required for it to pass through approximately one-quarter inch screen openings. On the other hand, a relatively high metal-content cathode deposit containing about 60% metallic titanium should not be crushed finer than that required for it to pass-through approximately one inch screen openings.

The electrolyte salts are extracted by any suitable aqua-- ousmedium. For example, plain water may be used, although the use of water acidified with. about 0.5% by weight of hydrogen chloride is particularly advantageous.-

Such a dilute hydrochloric acid solution tends-to minify' hydration of the salts to relatively insoluble residues with resulting oxygen-contamination of the leached metal. It must be understood, however, that any other effective leaching medium may be used in practicing my invention, the only requirement of the leaching operation being that it produces a mass of titanium metal substantially free of entrained salts. I

The resulting salt-free mass of titanium 'metal is then disintegrated pursuant to my invention so as to obtain the original crystals of the titanium cathode deposit largely freed of one another. This disintegration is effected by subjecting the crushed and leached mass to a scissor-like action between-cutting blades spaced apart a-distance at least as great as the maximum particle size of the individual titanium crystals in the leached mass. When the spacing between theblades is significantly less than the maximum-crystal particle size, the larger crystals, which are relatively pure, are broken up into" smaller par ticles within the range of the lower-purity naturally occurring crystals.

A variety of machines presently available on the market are suitable'for disintegrating the crushed and leached titanium cathode deposit pursuant to the invention. For example, the rotary cutters and knife cutters used to distintegrate plastic chips, leather and rubber scraps, asbestos,- cork, paper board, and the like, are particularly suitable. These rotary cutters comprise a cylindricalenclosure provided with stationary or bed knives and an inner rotary member carrying cooperating knives. The relative motion of these knives, whose spacing maybe readily adjusted, provides a scissor-like cutting'action by shearing impact which is wholly different from the coinpressive and distorting action of roller crushers, ball mills, tumbling mills, disk grinders, and the like. In a specific, rotary cutter having an outer cylindrical stator of 7 /2 inches in diameter, a rotor velocity of 1200 R. P. M. was found to be particularly satisfactory. This velocity is not critical, however; the only requirement of the rotor velocity is that it should be sufficient to effect separation of the titanium crystals by scissor-like shearing impact.

' The turbulence imparted to the mass of titanium metal by its disintegration in such a rotary cutter tends to heat the metal particles and thus accelerate their oxidation if they are exposed to an oxidizing environment.

Accordingly, I have found it advisable to maintain a' chemically inert protective atmosphere about .the titanium While it is being disintegrated. While a protective atmosphere is afforded solely by a gas such as argon, the cooling efiect of water either with or without the argon is presently preferred. Thus, I have found that if the particles are simply moistened with water while being subjected to the shearing impact, the temperature of the particles is held low, but the further use of an argon atmosphere within the rotary cutteraugments the-protection from oxidation afforded by the water coating on the particles. On the other hand, I have found that the use of a sufficient amount of water to completely submerge the metal particles in the rotary cutter will provide both the cooling and protection which is desirable.

Still further protection of the metal against oxidation during distintegration is assured by providing the rotary cutter with charging and discharging locks which facilitate the maintenance of a non-oxidizing atmosphere within vention. The scrubbing of the particles of titanium is accomplished by vigorous agitation of the disintegrated mass of particles in an aqueous medium. The agitation of the aqueous medium must be sufiiciently vigorous to cause the aqueous medium and the titanium particles suspended therein-to impinge against one another with sufiicient force'todislodge any crystals in contact withother crystals and thereby to substantially. completely separate the disintegrated mass into its individual crystal components. Moreover, it is possibleeither to sub ect the'entire disintegrated mass obtained from the disintegration operation to the subsequent scrubbing operation, or to carry out a preliminary classification operation to effect separation of the disintegrated mass into a first fraction composed predominantly of relatively coarse titanium particles and a second fraction composed of relatively fine titanium particles. only the said first fraction composed predominantly of relatively coarse titanium particles is subjected to the subsequent intensive scrubbing operation.

'Asthe intensive scrubbing operation is' carried out by vigorous "agitation of the titanium particles suspended in an aqueous medium, the amount of the aqueous medium (such as water) present must be sufficient to permit the titanium to be carried in suspension therein-but must not be so much as to reduce toan uneconomical extent the frequency with which the particles of titanium suspended in the aqueous medium will impinge against one another. In this connection I presently prefer to use 3 to 10 volumes of water disintegrated titanium particles. Moreover, to achieve the necessary vigorous agitation of the aqueous medium sufficient to effect substantially complete separation of the disintegrated mass into its individual component crystals, I have found it advantageous to employ a high speed propeller-type stirrer operating at a speed of about 1600 to 1800 R. P. M., operation is carried out being advantageously provided with conventional baffles that contribute to the efiiciency of agitation in the manner known to the'art. However,

the actual. velocity of the stirrer is not critical provided the agitation of the aqueous medium is sufficiently vigorous to insure thorough scrubbing of the titanium particles and 'I have successfully used stirrers screen sizing operation. When the titanium cathode deposit has been disintegrated and scrubbed pursuant to the present invention, the final product is a mass of nonoxidized individual crystals consisting of those of which the cathode deposit was composed. .Of these crystals, those having a particle size of through 8 and on 65 mesh (Tyler standard) appear to have a significantly higher degree of purity than the smaller size crystals not only with respect to their oxygen content but also with respect to the presence of nitrogen, hydrogen and the various metallic elements with which titanium is generally contaminated.

Within'this range, the crystalshavin'g a particle s'iz'e'rang'e In the latter case,

for each volume of the the vessel in which the scrubbing,

d of through 14 and on 35 mesh have the highest purity. And for each of these ranges, the degree of ductility, measured as Brinell hardness number, is commensurate with the degree of purity.

The practice of my invention and the improved results obtained thereby are illustrated by the following specific examples:

EXAMPLE I A quantity of electrodeposited titanium and solidified electrolyte salts entrained therewith was crushed, and the crushed particles of titanium and entrained salt were leached to dissolve the major portion of the said electrolyte salts. The titanium particles were then mixed with a quantity of water and passed through a rotary disintegrator in accordance with the method described in my copending application Serial No. 628,709. A portion of the disintegrated mass was then screened to separate the mass into a fraction composed of relatively coarse crystals and a fraction composed of relatively fine crystals of metallic titanium in accordance with the aforesaid method. The fraction containing the relatively large crystals was dried and melted under a vacuum to form a titanium metal ingot which was found to have a Brinell hardness number of 121.

Another portion of the disintegrated titanium particles not classified as to size was introduced into a cylindrical scrubber vessel, the material charged to the scrubber vessel comprising about 317 parts by weight of titanium and 1083 parts by weight of water. The scrubber vessel was 6" in diameter and was equipped with four vertical bafiles extending inwardly from the inner surface of the vessel a distance of about 4 of an inch. A scrubber agitator having a diameter of 3" and having four propeller blades pitched at an angle of 45 to the vertical shaft of the agitator was centrally positioned in the scrubber vessel. The agitator was operated for minutes at a speed of 1750 R. P. M., whereupon the scrubbed sample was removed from the scrubber vessel and wet screened to separate a fraction composed of relatively coarse titanium crystals from a fraction composed of relatively fine titanium crystals in accordance with the method of my invention. The fraction containing the relatively coarse titanium crystals was dried and then was consolidated by melting under a vacuum to form a titanium metal ingot having a Brinell hardness number of 109.

EXAMPLE II Six different cathode deposits were each given the disintegration and the disintegration plus scrubbing treatment described in Example 1. Two different scrubber agitator speeds were employed. The average Brinell hardness numbers of the titanium metal product obtained following each type of treatment of the six cathode deposits are given in the following table:

Table Scrubber Tyler Brinell Operation agitator, Screen Hard- R. P. M. Size ness Disintegrated but not Scruhbed 8+65 124 Disintegrated and Serubbed 8+65 118 Do 8+65 114 disintegrating the residual mass of titanium metal pre dominantly into its component crystals with a scissorlike action between cutting blades spaced apart a distance at least as great as the maximum particle size of the individual titanium crystals and moving at sutficiently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, maintaining a chemically inert atmosphere surrounding the mass of titanium metal while it is being disintegrated, subjecting the disintegrated mass while suspended in an aqueous medium to vigorous mechanical agitation of sufiicient force to cause the, suspended particles to impinge against one another with such force as to dislodge any titanium metal crystals in adhering contact with other such crystals and to substantially completely separate the mass into its individual crystal components, and classifying the resulting scrubbed disintegrated mass to separate a. relatively pure fraction composed of relatively coarse titanium crystals from a relatively impure fraction composed of relatively fine titanium crystals.

2. The method of selectively separating relatively pure and relatively impure crystals of electrolytically deposited titanium metal from a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts whichcomiprises crushing the cathode deposit to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one-quarter inch screen openings, leaching the crushed mass with an aqueous medium to dissolve the electrolyte salts away from the titanium metal, disintegrating the residual mass of titanium metal predominantly into its component crystals with a scissor-like action between cutting blades spaced apart a' distance at least as great as the maximum particle 'size of the individual titanium crystals and moving at sufiiciently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, maintaining a chemically inert atmosphere surrounding the mass of titanium metal while it is being disintegrated, subjecting the disintegrated mass while suspended in an aqueous medium to vigorous mechanical agitation of sufiicient force to cause the suspended particles to impinge against one another with such force as to dislodge any titanium metal crystals in adhering contact with other such crystals and to substantially completely separatethe mass into its in: dividual crystal components, and classifying the resulting scrubbed disintegrated mass to separate a relatively pure fraction composed of titanium crystals having a size range of through 8 and on 65 mesh screen from a relatively impure fraction composed of the remaining titanium crystals finer than said range.

3. The method of selectively separating relatively pure and relatively impure crystals of electrolytically deposited titanium metal from a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts which comprises crushing the cathode deposit to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one-quarter inch screen openings, leaching the crushed mass with an aqueous medium to dissolve the electrolyte salts away from the titanium metal, disintegrating the residual mass of titanium metal predominantly into its component crystals with a scissor-like action between cutting blades spaced apart a distance at least as great as the maximum particle size of the individual titanium crystals and moving at sufliciently high speed so that'the mass of titanium metal is distintegrated substantially exclusively by shearing impact, maintaining the titanium metal suspended in a body of water while it is being disintegrated, subjecting the disintegrated mass while suspended in an aqueous medium to vigorous mechanical agitation of the aqueous medium of sufiicient force to cause the suspended particles to impinge against one another with such force as to dislodge any titanium metal crystals in adhering contactwith other such crystals agar-mas and tosubstantially completelyseparate the inassiinto its individual crystal coinponents,the volume of the aqueous medium being between 3 to lO timesthe apparent volume of the disintegrated mass of metal and classifyingthe resulting scrubbed disintegrated'mass toseparate a relatively pure fraction composed of relatively coarse titanium crystals from a relatively impurefractioncomposed of relatively fine titanium crystals.

'4. The method of *selectivelyseparating relatively pure and relatively impure crystals of electrolytically deposited titanium metal froma massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts which comprises crushing the cathode deposit to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one-quarter inch screen openings, leaching the crushed mass with an aqueous medium to dissolve the electrolyte salts away from the titanium metaL-disintegrating the residual-mass of titanium metal predominantly into its component crystals with a scissorlike action between cutting blades spaced apart a distanceat least'asrgreat as the maximum particle size of the individual titanium crystals and moving at sufficiently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, maintaining a chemically inert atmosphere surrounding the mass of titanium metal while it is being disintegrated, classifying the resulting disintegrated mass to separate a fraction composed predominantly of relatively coarse titanium crystals'from a fraction composed of relatively fine titanium crystals, subjecting the fraction composed predominantly of relativ'elycoarse titanium crystals while suspended in an aqueous medium to vigorous mechanical agitation of sufiicient force to causethesuspended particles to impinge against one another with such force-as to dislodge any relatively small titanium metal crystals present in said fraction from adhering contact with the relatively large titanium metal crystals predominantly present in said'fraction, whereby said'fraction is substantially completely separated into its individual crystal components, and classifying the resulting scrubbed fraction of said disintegrated mass to separate'a relatively pure fraction composed of relatively coarse titanium crystals from a relatively impure fraction composed of rela' tively fine titanium crystals.

'5. The method of selectivelyseparating relatively pure and relatively impurecrystais'of electrolytically deposited titanium metal from a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering-and entrained electrolyte-saltswhich comprises crushing the cathode deposit to forms. mass. of coarse aggro gates not substantially smaller than that whichwill pass through approximately one-quarter inch screen openings, leaching the crushed mass with an aqueous medium to dissolve the electrolyte salts awayfrom the titanium metal, disintegrating the;rcsidual mass of titanium metal predominantly intoits component crystals with a scissor-like action betweencutting bladesspacedapart a distance at least as great as the maximum particle size of the individual titanium crystals and moving at suiiiciently high speed so'that the mass oftitanium metal is disintegrated substantially exclusively by shearing impact, maintaining a chemically inert atmosphere surrounding the mass oi ti tanium metal While it is being disintegrated, classifying the resulting disintegrated mass to separate a first fraction composed predominantly of titanium particles having'a size range of through 8 and on 65 mesh screen from a second traction composed of therremaining titanium particles finer than said range, subjectingsaid first fraction While suspended in an aqueous medium to vigorous me chanical agitation ofsufficient force to cause the suspended particles to impin e against one another with such forceias to dislodge-any relatively small titanium metal crystals present in'said firstfract'ionfrom all contact'witii the :relatively large :t'ita'niurn m'e'tal crystals "predominantly presentin said frac'tion, whereby said first fraction is substantially completely separated into its individual crystal components, and classifying the resulting scrubbed first fraction of said disintegrated mass to separate-a relatively'purethird fraction composedof titanium crystals having a size range of through 8 and on 65 mesh :screen from a relatively impure fourth fraction composed o'fthc remaining titanium crystals finer than said range.

-.6. The method :of. selectively separating relatively pure and relatively impure crystals of electrolytically deposited titaniunmmetal .from amassivecathode deposit composed-essentially ofia mixture oftitaniurn crystals with adhering and entrained electrolyte salts which comprises crushing the cathode deposit to form a mass of coarse aggregatesnotsubstantially smaller than that whichwill passfthrough, approximately onequarter inch screen openings, leaching-the crushed. mass with an aqueous medium to dissolve the electrolytersalts away from thetitanium metal, disintegrating ltheiresidual mass of titanium metal predominantly into its-component crystals with a scissorlike'action betweenvcutting blades spacedapart a distance atsleast as great asthe maximum particle size of the individual titanium crystals and moving at sufficiently high speed so that the mass of titanium metal is disintegrated substantially exclusively bysshearing impact, maintaining the titanium metalsuspended. in a body of water while it is being disintegrated, classifying the resulting disintegrated mass to, separate a fraction composed predominantlyofrelatively coarsetitanium crystals from a fraction composed of relativelyfine titanium crystals, subjecting the fraction composed predominantly of relatively coarse titanium crystals while suspended in an aqueous medium to vigorous mechanical agitation of sufiicient force to cause the suspended particles .to impinge against one another with such force -asto dislodge any relatively. small titanium metalcrystals present-in said fraction from adhering contact with the relatively large titanium metal crystals predominantly present. in said fraction, the volume of the aqueous medium being between 3 to 10 times the apparentvolume of said fraction of the disintegrated mass ,of-ruetal, wherebytsaid fraction is'su'bstantially completely separated .into its individualcrystal components, and classifying. the resultingscru'bbed fraction of said disintegrated mass to separate a relatively pure fraction composed of relatively coarse titanium crystals from alrelatively impure fraction composed of relatively fine titanium crystals.

7.. ln theimethod of selectively separating relatively pureand relatively. impure crystals of electrolytically idepositedvtitanium metal 'frorn' a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts in which the-cathode deposit is firstcrushed to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one quarter inch screen openings, in which the crushed mass is leached With'an aqueous medium to dissolve the electrolyte salts away'from the titanium metal, in which the residual mass of titanium metal is disintegrated into its own component crystals with a scissor-like action between cutting blades spaced apart a distance at least as great'as the maximum particle size of the individual titanium crystalsand moving at sufiiciently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, a chemically inert atmosphere being maintained surrounding the mass of titanium metal while it is being disintegrated, and in which the resulting disintegrated mass of titanium crystals is classified to separate a relatively pure fraction composed of relatively coarse titanium crystals from a relatively impure fraction com posed of therelatively fine titanium crystals, theimprovement which comprises subjecting the disintegrated mass tovigorousmechanical' agitation while suspended in an aqueous medium prior to classification thereof, the agitation-being "of sufiicient force to cause the suspended particles to impinge against one another with such force as to dislodge any titanium metal crystals in adhering contact with other such crystals in the mass suspended in the aqueous medium whereby the disintegrated mass is substantially completely separated into its individual crystal components.

8. In the method of selectively separating relatively pure and relatively impure crystals of electrolytically deposited titanium metal from a massive cathode deposit composed essentially of a mixture of titanium crystals with adhering and entrained electrolyte salts in which the cathode deposit is crushed to form a mass of coarse aggregates not substantially smaller than that which will pass through approximately one quarter inch screen openings, in which the crushed mass is leached with an aqueous medium to dissolve the electrolyte salts away from the titanium metal, in which the residual mass of titanium metal is disintegrated into its own component crystals with a scissor-like action between cutting blades spaced apart a distance at least as great as the maximum particle size of the individual titanium crystals and moving at sufficiently high speed so that the mass of titanium metal is disintegrated substantially exclusively by shearing impact, a chemically inert atmosphere being maintained surrounding the mass of titanium metal while it is being disintegrated, and in which the resulting disintegrated mass of titanium crystals is classified to separate a relatively pure fraction composed of titanium crystals having a size range of through 8 and on mesh screen from a relatively impure fraction composed of the remaining titanium crystals finer than said range, the improvement which comprises subjecting the disintegrated mass while suspended in an aqueous medium to vigorous mechanical agitation prior to classification thereof, the agitation being References Cited in the file of this patent UNITED STATES PATENTS 1,999,825 Saklatwalla et al Apr. 30, 1935

Claims (1)

1. THE METHOD OF SELECTIVELY SEPARTING RELATIVELY PURE AND RELATIVELY IMPURE CRYSTALS OF ELECTROLYTICALLY DEPOSITED TITANIUM METAL FROM A MASSIVE CATHODE DEPOSIT COMPOSED ESSENTIALLY OF A MIXTURE OF TITANIUM CRYSTALS WITH ADHERING AND ENTRAINED ELECTROLYTE SALTS WHICH COMPRISES CRUSHING THE CATHODE DEPOSIT TO FORM A MASS OF COARSE AGGREGATES NOT SUBSTANTIALLY SMALLER THAN THAT WHICH WILL PASS THROUGH APPROXIMATELY ONE-QUARTER INCH SCREEN OPENINGS, LEACHING THE CRUSHED MASS WITH AN AQUEOUS MEDIUM TO DISSOLVE THE ELECTROLYTE SALTS AWAY FROM THE TITANIUM METAL, DISINTEGRATING THE RESIDUAL MASS OF TITANIUM METAL PREDOMINANTLY INTO ITS COMPONENT CRYSTALS WITH A SCISSORLIKE ACTION BETWEEN CUTTING BLADES SPACED APART A DISTANCE AT LEAST AS GREAT AS THE MAXIMUM PARTICLE SIZE OF THE INDIVIDUAL TITANIUM CYRSTALS AND MOVING AT SUFFICIENTLY HIGH SPEED SO THAT THE MASS OF TITANIUM METAL IS DISINTEGRATED SUBSTANTIALLY EXCLUSIVELY BY SHEARING IMPACT, MAINTAINING A CHEMICALLY INERT ATMOSPHERE SURROUNDING THE MASS OF TITANIUM METAL WHILE IT IS BEING SISINTEGRATED, SUBJECTING THE DISINTEGRATED MASS WHILE SUSPENDED IN AN AQUEOUS MEDIUM TO VIGOROUS MECHANICAL AGITATION OF SUFFICIENT FORCE TO CAUSE THE SUSPENDED PARTICLES TO IMPINGE AGAINST ONE ANOTHER WITH SUCH FORCE AS TO DISLODGE ANY TITANIUM METAL CRYSTALS IN ADHERING CONTACT WITH OTHER SUCH CRYSTALS AND TO SUBSTANTIALLY COMPLETELY SEPARATE THE MASS INTO ITS INDIVIDUAL CRYSTAL COMPONENTS, AND CLASSIFYING THE RESULTING SRUBBED DISINTEGRATED MASS TO SEPARATE A RELATIVELY PURE FRACTION COMPOSED OF RELATIVELY COARSE TITANIUM CRYSTALS FROM A RELATIVELY IMPURE FRACTION COMPOSED OF RELATIVELY FINE TITANIUM CRYSTALS.