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    Improvements in or relating to propylene polymerization with hf-bf
    81.
    发明专利
    Improvements in or relating to propylene polymerization with hf-bf 未知

    公开(公告)号：GB700616A

    公开(公告)日：1953-12-09

    申请号：GB1664150

    申请日：1950-07-04

    Applicant: STANDARD OIL CO

    Inventor： EVERING BERNARD L ,  PETERS EDWIN F

    IPC: C07C2/20

    Abstract: C12 - C15 polymers of propylene are produced by contacting with an HF - BF3 catalyst under pressure sufficient to maintain the propylene and the HF in liquid phase and employing a sufficiently large amount of an inert diluent in which HF is soluble ao that the HF is completely dissolved in the diluent-propylene mixture during polymerization. The diluent, e.g. propane, may be passed through a column of HF and the resulting solution intimately mixed with the propylene and the BF3 component, and polymerization effected under a pressure of 300 to 600 lbs./sq. in. at a temperature of 40 DEG to 140 DEG F. The conversion to detergent polymers is from 40 to 100 per cent. In the apparatus shown, propylene is introduced through line 10 to mixer 12 where it is admixed with BF3, from line 15, and HF (preferably in solution in propane) introduced through line 16. Propane is passed through line 20 and at least a portion passes in liquid phase through the HF in vessel 19 and thence to line 16. The mixture from 12 is passed into the reaction chamber 14 provided with cooling coils 16a. The effluent then proceeds to the settler 25 where any complex may separate out. The product stream is withdrawn into heat exchanger 31 where it is heated to about 250 DEG F. before being led into depropanizer tower 32. This may be operated at a pressure of about 260 psig. with a top temperature of 180 DEG F. and a bottom temperature of 480 DEG F. The polymer passes by line 78 through heat exchanger 31 and thence through one or more bauxite treaters 79 to gasoline fractionating tower 81 which may operate at about 20 psig. with a bottom temperature of 500 DEG F. The overhead fraction, consisting of gasoline-boiling range polymers, is condensed in cooler 83, collected in receiver 84 and withdrawn through line 87. Polymer fractions of higher boiling point are passed to fractionating tower 89 which may operate at 350 mm. Hg pressure with a top temperature of 365 DEG F. and a bottom temperature of 550 DEG F. C18 and heavier polymers are withdrawn through line 91 and the overhead is condensed in cooler 92 and collected in receiver 93. A part of this condensate is returned by pump 94 and line 95 for reflux in tower 89 and the net C12 - C15 polymers are withdrawn through line 96. In the example about 2 volumes of propane are used per 3 volumes of propylene. The catalyst may contain 80-50 mol. per cent. HF, and may be in amounts of 3 to 4 mol. per cent. based on propylene charged to give a total weight per cent. of HF in the total hydrocarbon charge of about 0.5. BF3 and other gas must not accumulate in the reaction system and lines 28 and 29 are provided for their withdrawal. From the depropanizing zone 32, the overhead is separated into a propane fraction, a gas fraction, a BF3 and an HF fraction and the propane and catalyst components may be recycled. Alternatively to dissolving the HF in propane, homogeneity may be maintained by other means, e.g. reacting HF with a portion of the propylene to form propylene fluoride which liberates HF in the mixer or reaction zones.

    82.
    发明专利
    未知

    公开(公告)号：DE1214001B

    公开(公告)日：1966-04-07

    申请号：DEST010946

    申请日：1956-03-08

    Applicant: STANDARD OIL CO

    Inventor： PETERS EDWIN F ,  EVERING BERNARD L

    IPC: B01J23/22 ,  B01J23/26 ,  B01J23/28 ,  B01J23/88 ,  C08F2/00 ,  C08F10/00

    Abstract: Polymerization catalysts comprise an oxide of a Group 5A metal and/or a supported oxide of a Group 6A metal, in conjunction with a co-catalyst AIR3, wherein R is selected from hydrogen and hydrocarbon radicals. The oxides may be used in admixture with each other or with the oxides of copper, tin, zinc, nickel, cobalt, titanium and zirconium, e.g. the mixtures obtained by calcining Group 5A or 6A metal salts of metavanadic or molybdic acids. The oxides may be pre-reduced before use. In examples, the aluminium compounds used are the trimethyl, triethyl and triphenyl compounds, but many others are specified. The supports listed, which may also be used for Group 5A metal oxides, are activated carbon, alumina, activated and tabular alumina, magnesia, titania, zirconia, silica, aluminosilicates, clays, fused silicates, silicon carbide, diatomaceous earths, metals (such as iron or steel) preferably treated to produce a film of the corresponding oxide (e.g. anodized aluminium), kaolin, iron oxide, carbon block, and fluorides of alkali metals, alkaline earth metals, aluminium, gallium and indium. The catalyst may be in the form of a film of oxide on the inner surface of the reactor, e.g. V2O5 coated on a calcined aluminium surface. Example 13 also illustrates the use of unsupported 6A metal oxide catalyst. Relative proportions for catalyst, co-catalyst and support are given.ALSO:C2 to C4 mono-olefines are polymerized at low pressure and temperature using a catalyst comprising an oxide of a Group 5A metal and/or a supported oxide of a Group 6A metal, in conjunction with a cocatalyst of formula AlR3 wherein R is selected from hydrogen and hydrocarbon radicals. Ethylene, which may contain oxygen as impurity, propylene and 1-butene are specified olefines and these may be copolymerized with t-butyl-ethylene, butadiene, isoprene, styrene, aryl alkyl styrenes, tetrafluoroethylene and trifluoromonochloroethylene. Oxides disclosed are V2O5, Cb2O5, Ta2O5, Vo2, V2O3, VO, CbO2, CbO, TaO2, MoO3, Cr3O3, WO3 and mixtures with each other or with oxides of copper, tin, zinc, nickel, cobalt, titanium and zirconium, e.g. the mixtures obtained by calcining Group 5A or 6A metal salts of metavanadic or molybdic acids. The oxides may be calcined or pre-reduced before use. In examples the aluminium compounds used are the trimethyl, triethyl and triphenyl compounds, but many others are specified. The supports listed, which may also be used for Group 5A metal oxides, are activated carbon, alumina, activated alumina, tabular alumina, magnesia, titania, zirconia, silica, aluminosilicates, clays, fused silicates, silicon carbide, diatomaceous earths, metals (such as iron or steel) preferably treated to produce a film of the corresponding oxide (e.g. anodized aluminium), kaolin, iron oxide, carbon black and fluorides of alkali metals, alkaline earth metals, aluminium, gallium and indium. The catalyst may be in the form of a film of oxide on the inner surface of the reactor, e.g. V2O5 coated on a calcined aluminium surface. Example 13 also illustrates the use of unsupported 6A metal oxide catalysts. Relative proportions of catalyst, cocatalyst and support are given and preferred space velocities are stated. The polymerization may be carried out in the gas phase, the catalyst being treated from time to time to remove polymer and to be reactivated, but preferably in an inert liquid hydrocarbon medium of which many aliphatic, aromatic and olefinic examples are given. The catalyst may be in a fixed bed and olefine may be led continuously into and out of contact with the catalyst. In order to avoid reaction of contaminants in the olefinic feed with the aluminium compound the liquid medium should be purified, e.g. by treatment with p-toluene-sulphonic acid, sulphuric acid, Friedel-Crafts catalysts, maleic anhydride, calcium, calcium hydride, sodium or other alkali metals, alkali metal hydrides, lithium aluminium hydride, hydrogen, hydrogenation catalysts or filtration through grains of copper or Group 8 metal. High density, crystalline polymers may be obtained. The products may be mixed with anti-oxidants, stabilizers, fillers, extenders, plasticizers, pigments, insecticides, fungicides, lower molecular weight polyethylene, hydrocarbon oils, lubricating oils, xylene, paraffin, petrolatum and ester waxes, and high molecular weight polybutylenes, and may be used in the manufacture of carboys, plastic pipe, gas barriers, packaging and coating materials and binders. The polymers may be milled, halogenated, halogenated followed by dehalogenation, sulphohalogenated, sulphonated and irradiated with X-rays or radioactive materials to effect cross-linking, and may be converted into sponges or latices. Specification 713,081 is referred to.

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