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http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C08F110-00
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filingDate 1961-10-02-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1963-08-28-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-935229-A
titleOfInvention Process of reduction of transition metal halides
abstract <PICT:0935229/III/1> <PICT:0935229/III/2> <PICT:0935229/III/3> Transition metal halides are reduced in an anhydrous liquid medium under non-oxidizing atmospheres in the presence of at least 30 times the stoichiometric quantity of a metal reducing agent having a smallest dimension of 0,3 mm. The temperature range is -5 DEG to 200 DEG C., and renewal of the metal surface is effected by circulation of the liquid medium or by mechanical agitation, small quantities of polar compounds may be added if desired. <PICT:0935229/III/4> The reactants may be contained in a cylindrical drum which may be rocked or rotated about its axis. Specified reducing agents are aluminium, beryllium, magnesium, zinc, iron, copper and mixtures or alloys of these metals; liquid media specified are hexane, heptane, oxtane, cyclohexane, decalin, liquid paraffin, benzene, toluene, xylene, ethyl benzene, polyalkylbenzene, cumene, tetralin, naphthalene, diphenyl, diphenylmethane, bromobenzene, chlorobenzene, ethyl chloride and bromide, tertiary butyl chloride, benzyl chloride, tetrachloroethane, hexachlorobenzene, chlorinated paraffins, chlorinated naphthalenes and polyphenyls. In examples titanium tetrachloride was reduced using aluminium metal with (1) heptane, (2) cyclohexane, (3) cyclohexane and zinc chloride, (4) petrol and dimethyl silane, (5) ethyl benzene, 130 DEG C., (6) ethyl benzene, 40 DEG C., (7) toluene, (8) octane, (9) toluene and heptane, (10) cyclohexane, ethylbenzene, dimethyl silane, benzyl chloride and zinc chloride, (12) hexane, toluene, mercuric chloride and ethyl bromide, (13) hexane, toluene, stannic chloride, and ethyl chloride, (14) liquid paraffin, toluene, and dimethyl silicane, (16) decahydronaphthalene, tetrahydronaphthalene and beryllium chloride, (20) cyclohexane, toluene and boron trichloride, (23) decahydronaphthalene, and tricresyl phosphates, (24) toluene and isobutyl alcohol, (11) VCl4, MoCl5, VOCl3, VObr3, ZrCl4, MoBr4, MoF6, MoF4 and CrO2Cl2, all may be reduced using ethylbenzene, phenylmethyl silicane and aluminium metal, (15) alumin-beryllium alloys, (17) magnesium, (18) zinc, (19) aluminium and copper are used with various liquid media to reduce titanium tetrachloride.ALSO:Ethylenic compound are polymerized in the presence of organometallic compounds and a reduced transition metal halide (see Group III). Ethylenic compounds are, ethylene, propylene, ethylene/propylene mixture, ethylene/a -butene mixture; organometallic compounds are monochlorodiethyl aluminium and triethyl aluminium.
priorityDate 1960-10-03-04:00^^<http://www.w3.org/2001/XMLSchema#date>
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