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United States Patent Patented July 10, 1956

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United States Patent Patented July 10, 1956 2,754,256 United States Patent Patented July 10, 1956 2 is convenient, economical and adaptable to commercial 2,754,256 production. A still further object of the invention is to provide a PROCESS FOR PG TITANIUM superior method for removing a major portion of the TETRACHLORIDE impurities from crude titanium tetrachloride in a manner Edge] P. Stambaugll, Metuchen, N. J., assignor to Na such that no polymerization occurs and the residue formed tional Lead Company, New York, N. Y., a corporation may be readily removed from the still. of New Jersey These and other objects will become more apparent from the following more complete description of the No Drawing. Application April 24, 1953, 10 instant invention. Serial No. 351,028 In its broadest aspects the present invention relates to 9 Claims. (Cl. 202—57) a process for producing substantially pure liquid titanium tetrachloride by admixing crude titanium tetrachloride and a liquid chlorinated hydrocarbon of the methane The present invention relates in general to the prepara 15 series containing at least 5 carbon atoms and at least one tion of the tetrahalides of metals of the fourth group of chlorine atom per molecule and heating the mixture from elements and more especially to the puri?cation of tita 65° C. to boiling point of said mixture and separating the nium tetrachloride and similar stable normally liquid dis puri?ed titanium tetrachloride therefrom. tillable tetrahalides. As used herein, the term “Chlorinated hydrocarbons of In general the tetrahalides of metals of the fourth group 20 the methane series” includes all saturated hydrocarbons of elements are prepared by chlorinating a metal-bearing having at least 5 carbon atoms per molecule and chlorin material and recovering the metal from the tetrachloride ated para?ins including polyvinyl chlorides. Only the vapor in the form of a relatively impure liquid conden chlorinated hydrocarbons of the methane series which sate. By way of example, liquid titanium tetrachloride are liquid at room temperature are contemplated by the is commonly prepared by treating a titaniferous material 25 instant invention. The purifying agent must contain at such as titaniferous iron ore, or ilmenite with chlorine least 5 carbon atoms and at least 1 chlorine atom per gas, in a static bed or lino-solids operation, to form tita molecule. Those compounds which are most satisfactory nium tetrachloride vapor which is subsequently condensed for puri?cation and which are liquid usually contain from to form a crude titanium tetrachloride condensate. Since about 5% to about 60% chlorine by weight. These liquid there are a number of elements in the raw material, in chlorinated hydrocarbons are saturated and therefore con addition to titanium, which react with chlorine to form tain no double or triple bonds. These saturated com volatile chlorides and which carry over with the titanium pounds therefore do not polymerize in the titanium tetra tetrachloride vapors, the titanium tetrachloride conden chloride and therefore are desirable as a purifying agent. sate, sometimes hereinafter referred to as crude titanium The treatment of crude titanium tetrachloride, by which tetrachloride, is invariably impure. Moreover, it has is meant a liquid titanium tetrachloride containing such been found that these volatile chlorides are not readily impurities as vanadium, silica, alumina, niobium, tungsten eliminated by distillation since the respective chlorides and the like, with chlorinated hydrocarbons may be car— such as, for example, the chlorides of silicon, aluminum, ried out, according to the present invention, in any con~ niobium, tungsten and vanadium, tend to distill over with venient manner which will insure the required intimacy the titanium tetrachloride values and to be found in the of contact between the crude titanium tetrachloride and condensate. One such impurity which, because of the the purifying agent. The puri?cation treatment may be proximity of its boiling point to that of titanium tetra carried out in a puri?cation unit comprising, for example, chloride, cannot be separated therefrom by fractional a still having a fractionating column, a re?ux return and distillation is vanadium chloride. Vanadium chloride is a condenser, by heating the crude titanium tetrachloride present in substantially all crude titanium tetrachloride with a chlorinated hydrocarbon in the still at a tempera condensate and comprises a major portion of the impuri ture from 65° C. to boiling point of the mixture and there ties in the condensate and hence is chie?y responsible for after separating the treated titanium tetrachloride by dis the yellowish color of crude titanium tetrachloride. By tilling and condensing the puri?ed titanium tetrachloride. way of example, a typical crude titanium tetrachloride The puri?cation treatment may also be carried out in a may comprise from 0.25 to 0.35% vanadium based on 50 vessel by heating the mixture at a temperature between the weight of the titanium tetrachloride, the other impuri 65° C. and the boiling point of the mixture and ?ltering ties being present in relatively small amounts such as, for the heat-treated mixture to obtain the puri?ed titanium example, from 0.04 to 0.2% silica, from 0.02 to 0.025% tetrachloride as the ?ltrate. In using liquid chlorinated . alumina, from 0.01 to 0.02% niobium, and from 0.05 to hydrocarbons as puri?cation agents it has been found that 0.08% tungsten. 55 puri?ed titanium tetrachloride may be recovered from the While it has been proposed heretofore to purify crude mixture by either the distillation or ?ltration method titanium tetrachloride and other similar tetrahalides by described above. treatment with such materials as hydrogen sulphide, silica The chemical reaction which takes place between the. gel, carbon, salts of the heavy metals, soya bean oil, art purifying agent and the titanium tetrachloride is not com gum, etc., such methods have been characterized by the 60 pletely understood. The purifying agents contemplated formation of residues which have been either insoluble by the instant invention, that is, the liquid chlorinated or removable from the still bottoms only with the greatest hydrocarbons are apparently soluble in the titanium tetra difficulty. As a consequence the adaptation to commer chloride and only a very small residue or reaction product cial production of prior methods for purifying crude is formed. This residue, however, apparently is ?nely titanium tetrachloride have been attended by much di?i 65 divided and remains suspended in the titanium tetrachlo culty and high cost. ride during the heat treatment. An object of the present invention is, therefore, to The type of residue which forms in the instant inven provide a superior method for producing substantially tion is entirely different from that obtained when employ ing organic compounds which polymerize and form bulky I pure liquid tetrahalides of the fourth group of elements. A further object of the invention isto provide a superior 70 and sticky still bottoms which are dit?cult to handle. When the chlorinated hydrocarbons are employed, how , method for purifying crude titanium tetrachloride which ever, only very small amount of suspended residues are 2,754,256 '2 -. ‘3 formed inthe ,still- , ,Thiscresidue. was held .il1...,SJ-l§Pen5_i9.n obtained which can be concentrated and ?ltered fromtime and did not form a stickyor bulky still bottom. The to time and therefore stillibottom difficulties are elimi residue when dried had a volume of less than 1% of the nated. The total amount of residue formed in the vessel total volume of the titanium tetrachloride used. is 'ii'siially'less than about 1% ‘of the total ‘volume of titanium tetrachloride used. Example 2 ‘The amount of chlorinated hydrocarbon used as a puri To 100 parts of the same crude titanium tetrachloride _ fying'ag'e'nt‘ is. dependent upon the amount of impurities at substantially ‘room temperature was added ‘051 'part ofv "and particularly the vamount of vanadium present in the chlorinated para?in containing 50% chlorine by weight ‘crude titanium tetrachloride and upon the time and tem whereupon the mixture was re?uxed at a temperature of perature of the treatment employed. It has been found 10 about 136°C. for a period of 15 minutes. The ‘treated vthatfro'rn'about 0.01% to about 1% should be employed mixture was then distilled and yielded a substantially pure to remove substantially all ofthe vanadium from the titaniumitetrachloride.H The vanadium content of the crude titanium tetrachloride. The amount of agent will pure titanium tetrachloride was 0.0003% V. ‘vary vaccording to the vanadium content present in the crude material. In 'most cases this amount will'vary Example 3 i'fr'o‘rh approximately 0.04 to 0.5% Vin the crude titanium The same procedure was used to purify crude titanium tetrachloride. The smaller amounts of purifying agent 'tetrachloride except that a polyvinyl chloride was used ‘may be'ernploye'd for purifying the crude titanium tetra and substantially identical results were obtained. chloride which contains the 'smaller'amounts of vana Example 4 dium. The smaller amounts, that is, below about 0.1% 20 ‘may be employed when the treatment is made at substan To 100 parts of‘the vsame crude titanium tetrachloride tially boiling temperatures. When operating at tempera were added 0.3 part of chlorinated para?n containing "tui‘es below boiling, it‘ is necessary to increase the amount 42% chlorine whereupon the mixture was heated to 120° of'purifying agent employed until the larger amounts are C. and held at that temperature for a period of' l‘hour. ‘used at the lower treatment temperatures. With respect The. solution'rwas then ?ltered and a substantially pure 'to "the time of treatment'it is necessary to lengthen the titanium tetrachloride ‘which contained 0.0003% V was 1time as lower temperature treatments are employed.
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