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United States Patent Office Patented Nov 2,959,567 United States Patent Office Patented Nov. 8, 1960 2 include, among other compounds, a variety of alumi num trialkyls such as aluminum trimethyl, aluminum tri 2,959,567 ethyl, aluminum tripropyl, aluminum triisobutyl and POLYETHYLENE STABILIZED WITH TETRA higher aluminum trialkyls as well as dialkyl aluminum 5 halides, dialkyl aluminum hydrides and dialkyl alumi AS9, SUBSTITUTED ETHYLENE D num alkoxides. Salts of metals selected from the group Charles R. Pfeifer, Midland, Mich., assignor to The Dow consisting of titanium, zirconium, vanadium, uranium, Chemical Company, Midland, Mich., a corporation of thorium and chromium are preferably employed as the Delaware group IV-B, V-B and VI-B metallic compounds in the 10 catalyst, although salts of the remaining metals in these No Drawing. Filed Jan. 26, 1956, Ser. No. 561,685 sub-groups may also be employed. Compounds of these 4 Claims. (C. 260-45.9) metals including their halogenides, oxyhalogenides, com plex halogenides, freshly precipitated oxides and hydrox ides and such organic compounds as alcoholates, acetates, This invention relates to improved, non-corrosive com 5 benzoates, acetyl acetonates and the like may be used in positions comprised of select corrosion-inhibiting agents the catalyst. and polymerized olefinic and other ethylenically unsat A particularly active catalyst mixture for the Zeigler urated materials which have been prepared with certain process may be obtained by mixing a titanium or zir catalytic metal compounds. In particular it relates to conium compound, such as a tetrachloride, oxychloride compositions of this nature which are not promotive of 20 or acetyl acetonate with an aluminum trialkyl or a dialkyl oxidative corrosion of metals and other materials of con aluminum compound. Generally, the molar quantities struction, particularly ferrous metals and alloys that do of the aluminum alkyl employed to constitute the cat not have special corrosion-resisting properties and that alyst admixture are two to three times the valence of are susceptible to oxidative corrosion and formation of the group IV-B, V-B and VI-B metal compound for each oxide films on their surfaces, especially at elevated tem 25 mole of the latter compound which is present, although peratures. The invention also relates to a method for many other ratios may also be employed satisfactorily. preparing such compositions. Amounts of the catalyst admixture varying from 0.01 to Various olefins and other ethylenically unsaturated ma a few percent by weight, depending on the degree of terials, particularly ethylene, may be efficiently polymer purity of the materials being polymerized, the desired ized, even as relatively impure materials, to high mo 30 rate of polymerization and the intended molecular weight, lecular weight polymeric compounds at comparatively may suitably be employed. low pressures and temperatures, according to a process After polymerization according to the Ziegler process, first proposed by Karl Ziegler and his associates in Ger however, polyethylene and similar polymerized products many. In this process, mixtures of strong reducing contain residues from the admixed metallic catalyst em agents such as aluminum alkyls with compounds of group 35 ployed. The residues are not sufficiently removed by the IV-B, V-B and VI-B metals of the periodic system in conventionally utilized aftertreatment of polymeric ma cluding thorium and uranium and employed as catalysts terials prepared according to the Zeigler process. Such for the polymerization. Polyethylenes, for example, after treatment usually involves filtration, preferably in having average apparent molecular weights (as indicated the presence of air (which tends to lighten the color of by measurement of such characteristics as their melt vis 40 the product), to separate the polymerization product cosities and the like) in excess of 40,000 and as large from the reaction mass. This maybe followed by se as 100,000 to 3,000,000 can be manufactured by poly quential trituration with hexane, isopropanol, water, ace merizing ethylene gas with such catalyst at temperatures tone and pentane prior to drying. When higher cat beneath about 100° C. and under pressures less than alyst concentrations are employed in the Ziegler process, about 100 atmospheres. It is frequently preferable when 45 some of the metallic compounds may be removed from employing such catalyst according to the Ziegler process the polymeric product by extracting it with methanolic to operate at temperatures of about 50 C. and under hydrochloric acid, then washing it in methanol or acetone. pressures between about 1 and 10 atmospheres. The Butanol washings after the filtration in air have also reaction may suitably be conducted in the presence of been proposed to decompose and remove the catalyst an organic liquid medium such as hexane, benzene, sat 50 urated petroleum hydrocarbon fractions and the like. residue. The polyethylenes prepared by the Ziegler process It has been observed that the presence of certain cat have superior and highly desirable properties. For ex alyst residues in polymeric materials prepared accord ample, they may be made containing less than 3 and ing to the Ziegler process tends to impart decidedly un even less than 0.03 methyl groups per each 100 methyl 55 desirable characteristics to the polymers. For example, ene groups in the polymer molecule. The polymer such polymers, particularly when the catalyst residue. molecules are practically completely linear and are crys contains halogens, especially chlorine, which may cause talline almost to their melting points, which usually are the presence of hydrogen halides or like corrodents in in the neighborhood of about 125-135 C. Their densi the polymer, tend not only to be extremely corrosive to ties are commonly in the range of about 0.94-0.96 gram 60 most of the materials of construction commonly utilized per cubic centimeter and higher. They are insoluble in in apparatus for extruding, shaping or molding the poly most solvents at ordinary temperatures. Shaped articles mer, but are also accessorial to the relatively higher formed with such polyethylenes have tear strengths be temperature oxidation of such materials. This is greatly tween about 1400 and 2800 pounds per square inch. pronounced in the frequent cases when the construction Unstretched films prepared from them have tensile 65 materials employed in such apparatus are particularly strengths in excess of about 2800 pounds per square inch sensitive or susceptible to being oxidized at relatively and may be oriented by stretching to polyethylene film higher temperatures and to form relatively heavy, blue structures having tensile strengths as high as about 42,500 colored films, on their surface. Such an effect may be pounds per square inch. delineated as a "blueing' of the surface of the construc The strong reducing agents which advantageously are 70 tion material. Many of the frequently employed ferrous. employed in the catalyst mixtures of the Ziegler process metals and alloys are susceptible to such corrosive at 2,959,567 3 4. tack, especially at elevated temperatures of about 180" idative corrosion of the apparatus is also advantageously C. and higher. obtained during fabrications at elevated temperatures. While, as disclosed in the copending applications hav The compositions do not necessitate employing fabricat ing Serial Nos. 553,690,553,721, 553,722, 553,729, and ing apparatus which is made from relatively more expen 553,746, all of which were filed on December 19, 1955, 5 sive materials of construction which have special corro and in each of which the present applicant is an inventor, sion-resisting characteristics and eliminate the expensive various substances may be employed to diminish the damage and waste which occurs when conventional ap corrosive propensities of halogen-containing polymeric paratus is oxidatively corroded. In addition, better qual materials, particularly polyethylene, prepared according ity products may be obtained when the fabricating ap to the Ziegler process, by countereffecting the presence of 0. paratus is kept free from the physical damage caused by or acting as receptors for hydrogen halides and the like oxidative corrosion. which may be present or formed in the polymer, many In a series of illustrative examples, N,N',N',N'-tetrakis of these substances are not effective to prevent the sur (2-hydroxypropyl-) ethylene diamine was incorporated face "blueing' or oxidative corrosion which is frequent along with various corrosion-inhibiting compounds which ly experienced when molding, such polymeric materials, 5 have a receptor function for and are capable of counter especially at the relatively high temperatures which are effecting hydrogen halide and like corrodents in a rela benefically employed for fabricating Ziegler type poly tively high molecular weight polyethylene which was pre meric materials, particularly polyethylene. Fabricating pared with an admixed aluminum alkyl-titanium tetra temperatures in excess of about 180–200° C. and fre chloride catalyst according to the herein described quently as high as 300 to 350° C. have been found ad 20 Ziegler process. The polyethylene had a catalyst residue vantageous for fabricating such polymers as polyethylene which contained between 0.02 and 0.08 percent by weight prepared according to the Ziegler process in order to ob of chlorine, based on the weight of the polyethylene. tain optimum physical properties in the fabricated poly For purposes of
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