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    Production of open chain oligomers of 1,3-dienes
    22.
    发明专利
    Production of open chain oligomers of 1,3-dienes 未知

    公开(公告)号：GB1043143A

    公开(公告)日：1966-09-21

    申请号：GB2964563

    申请日：1963-07-26

    Applicant: BASF AG

    Inventor： SEIBT HUBERTUS ,  KUTEPOW NIKOLAUS VON

    IPC: B01J31/16 ,  B01J31/18 ,  B01J31/24 ,  C07C2/40

    Abstract: Open chain dimers of 1,3-diolefins are obtained by dimerizing the diene in the presence of a catalyst containing zero valent nickel and a compound of trivalent phosphorus, arsenic or antimony and in the presence of at least an equimolar amount with reference to nickel of a non-aromatic organic hydroxyl compound, i.e. one wherein the hydroxyl is attached to an aliphatic or cycloaliphatic carbon atom. The catalysts are conventional and may also contain carbon monoxide, an olefin, an acetylene or an a ,b -olefinically unsaturated aldehyde or nitrile and may be formed in situ from a nickel compound, reducing agent and electron donor. Amounts of 0.001-1% by weight calculated as nickel based on diene are used. The hydroxyl compound may contain 1-15 carbons and is preferably saturated and may also contain alkoxy groups, e.g. methanol, ethanol, propanols, butanols, 2-ethylhexanol-1,crotyl alcohol,cyclohexyl carbinol, cyclohexanol, cyclo-octanol, benzyl alcohol, b -phenylethyl alcohol, lauryl alcohol, cinnamyl alcohol or methyl or butyl glycol. The alcohol is preferably used as solvent also being used in molar amounts of 2-5 times nickel; alternatively a hydrocarbon solvent is added. A phenolic or amine polymerization inhibitor may be added. Reaction is effected at 0-250 DEG C. and up to 20 atmospheres gauge. Catalysts containing phosphites yield from butadiene mainly octatriene-1,3,6, those containing phosphines octatriene-1,3,7, and those containing phosphorous acid triamides octatriene-2,4,6.ALSO:3 - (But - 2 - enyl) - 4,5 - diacid anhydridecyclohexene-1 is obtained by a Diels-Alder condensation of octatriene-1,3,6 with maleic anhydride. The di-n-butyl ester of the acid is produced on reacting the anhydride with n-butanol in the presence of hydrochloric acid. The ester is used as a plasticizer.

    Self extinguishing molding material based on propylene polymers
    23.
    发明专利
    Self extinguishing molding material based on propylene polymers 未知

    公开(公告)号：GB1037392A

    公开(公告)日：1966-07-27

    申请号：GB2119163

    申请日：1963-05-28

    Applicant: BASF AG

    Inventor： MAHLING DIETER ,  MUELLER-TAMM HEINZ ,  SEIBT HUBERTUS ,  ZUERN LUDWIG ,  SCHARF EMIL

    IPC: C08K5/02 ,  D06M15/227

    Abstract: A self-extinguishing composition comprises a propylene polymer, antimony trioxide and an organic bromine compound containing 45 to 93% of aliphatically combined bromine and having a boiling point above 200 DEG C. The propylene polymer may be a homopolymer or a copolymer with ethylene, butene, vinyl-acetate or -propionate, styrene or an ester of acrylic or of methacrylic acid; and the bromine compound may be a tetrabromocyclooctane, hexabromocyclododecane, phenyl - hexabromodecane, 1,2 - dibromo - 4 - (a ,b - dibromoethyl)-cyclohexane, N,N1,N11 - tri - (a ,b - dibromopropionyl) - trimethylene triamine, methylene-bis-(1,2 - dibromo - 1 - methylpropionamide), or a bromobutene-diol such as 2,3-dibromobutene-2-diol-1,4. Optional ingredients are other flameretardant agents, stabilizers, lubricants, dyes, fillers, antistatic agents and polymers, such as octabromodiphenyl, halogenated diphenyl containing Br and Cl, tribromotrichlorodiphenyl ether, dilauryl, thiodipropionate, bisphenols, aromatic sulphides, organic phosphites, benzophenone derivatives, thiazole derivatives, epoxides, stearates, salicylates, carbon black, pentaerythritol, alkali salts of tartaric acid or ethylene diamine tetracetic acid, polyisobutylene, polyethylene, polystyrene, copolymers of ethylene with vinyl acetate or ethyl acrylate, chlorinated polyisobutylene, and chlorinated paraffins and/or polynuclear aromatic compounds. The bromine compounds may be added in the form of pastes or solutions in acetone or chloroform. The compositions find application as sheets, boards, tubes, fibres, hollow articles, mouldings and coatings.

    28.
    发明专利
    未知

    公开(公告)号：FR1295072A

    公开(公告)日：1962-06-01

    申请号：FR867204

    申请日：1961-07-06

    Applicant: BASF AG

    Inventor： KUTEPOW NIKOLAUS VON ,  SEIBT HUBERTUS ,  MEIER FRITZ

    IPC: B01J31/18 ,  B01J31/20 ,  C07C2/46 ,  C07F15/04

    Abstract: The invention comprises a compound of the general formula: in which R is an alkyl or aromatic radical, Z is an a , b -unsaturated aldehyde or an a ,b -unsaturated nitrile, x is 2 or 3 and y is O or 1, the sum of x and y being les than or equal to 3. Such compounds and similar phosphite-containing nickel complexes with less than four ligands may be obtained by reacting an organic nickel complex containing O-valent nickel and which is free from carbon monoxide groups with a triester of phosphorous acid in an inert solvent or diluent with substantial exclusion of oxygen. Suitable nickel complexes for use in the process are nickel (O)-bis-acrylonitrile, nickel(O)-bis-cinnamonitrile, nickel(O)-bis-fumaronitrile, and nickel(O)-bis-acrolein. The group R in the phosphite may be the radical of a C1-C12 alkano or of a phenol or naphthol which may be substituted by alkyl or aryl radicals, alkoxy groups or halogen atoms, e.g. chlorine. The reaction is suitably carried out at from 20 DEG to 120 DEG C. at normal pressure but higher or lower pressures may be used. Suitable solvents are hydrocarbons, ethers, and nitriles of lower fatty acids e.g. acetonitrile or propionitrile. Examples are given for the production of the following complexes: tris-(tri-m-tolyl-phosphite)-nickel, and complexes obtained from nickel(O)-bis-acrylonitrile and tri-(a -naphthyl)-phosphite, tri-(2,4-dimethylphenyl)-phosphite, and tri-(p-tertiary-butylphenyl)-phosphite respectively. The products are useful as catalysts for the dimerisation of butidiene to form cyclooctadiene-1,5 (see Division C5).ALSO:Cyclooctadiene-(1,5) is obtained by dimerization of butadiene at an elevated temperature of at least 50 DEG C. in the presence of a catalyst consisting of a nickel complex with less than four ligands which has been obtained by reaction of an organic nickel complex compound free from carbon monoxide groups and containing O-valent nickel with a triester of phosphorous acid in an inert solvent or diluent with substantial exclusion of oxygen (see Division C2). Particularly suitable catalysts are the complexes obtained from a triester of phosphorous acid and nickel (O) complexes with a ,b -unsaturated aldehydes or a ,b -unsaturated nitriles, e.g. acrolein, g -bromocrotonaldehyde, acrylonitrile, cinnamonitrile, and fumaronitrile. The triester of phosphorous acid may be derived from a C1-C12 alkanol or from a phenol or naphthol which may be substituted by an alkyl, aryl or alkoxy group or by a halogen atom, e.g. chlorine. The dimerization of the butadiene is preferably carried out in the presence of a solvent or diluent, e.g. a hyrocarbon, a liquid carboxylic acid amide, a cyclic ether, a nitrile or a ketone and a polymerization inhibitor, e.g. hydroquinone may be present. Suitable dimerization temperatures are from 50 DEG to 250 DEG C. and it is preferred to operate at an elevated pressure, e.g. 3 to 20 atmospheres. Higher pressures may also be used by forcing in an inert gas such as nitrogen, rare gases, saturated or mono-olefinic gaseous hydrocarbons or carbon dioxide. The process may also be carried out at normal pressure, e.g. by blowing butadiene in gaseous form into a solution of the catalyst in a suitable solvent. The butadiene may be used pure or in admixture with other hydrocarbons, e.g. those obtained in the cracking of higher hydrocarbons. The process may be carried out batchwise, continuously, or semi-continuously. Small amounts of 4-vinyl-cyclohexene-(1) may be obtained as by-product. Examples are given in which the following complexes are used as catalysts: tris-(tri m-tolyl phosphite nickel, nickel (O)-bis-(p-tertiarybutylphenyl)-phosphite, tris-(tri-phenyl phosphite) nickel and the complexes obtained from nickel (O)-bis-acrylonitrile and tri-2,4-dimethylphenyl phosphite tri-(a -naphthyl) phosphite and tri-4-isooctyl phenyl phosphite respectively.

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