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    Production of oligomers of butadiene (1,3)
    31.
    发明专利
    Production of oligomers of butadiene (1,3) 未知

    公开(公告)号：GB1009017A

    公开(公告)日：1965-11-03

    申请号：GB3142462

    申请日：1962-08-16

    Applicant: BASF AG

    Inventor： WITTENBERG DIETMAR ,  LAUTENSCHLAGER HANS ,  KUTEPOW NIKOLAUS VON ,  MEIER FRITZ ,  SEIBT HUBERTUS

    IPC: C07C2/46 ,  C07C2/52 ,  C07F9/02 ,  C07F9/145 ,  C07F9/6574

    Abstract: Cyclic olefins are obtained by the polymerization of butadiene in the presence of a catalyst prepared from (a) a compound of iron, cobalt or nickel; (b) a hydride or organo-compound of an element of Group Ia, IIa, IIb or IIIa (i.e. non-transitional elements of Group III) and (c) a phosphite having an aryl radical with a substituent ortho to the phosphite group or a condensed 6-membered ring ortho and meta to the phosphite group. The constituent (a) is preferably an inorganic or organic salt or a chelate compound of nickel or cobalt. The ortho substituent in the aryl phosphite, which may be derived from benzene, naphthalene or diphenyl, may be an alkyl, alkoxy, halogen or aryloxy or together with the aryl group may form a fused, six-membered, carbocyclic ring. The other two phosphite substituents may be the same or different. The mol ratio of (a) : (b) : (c) may be 1 : 0.5-20: 1-4, the amount by weight of (a) being 0.001-0.1 times that of butadiene. A hydrocarbon or ether solvent, including reaction products, may be present and the temperature may be 0-250 DEG C. with sufficient pressure to maintain liquid phase. Octadiene-1,5 is the principal product. Specification 917,103 is referred to.

    Improvements in the production of arylaluminium compounds
    33.
    发明专利
    Improvements in the production of arylaluminium compounds 未知

    公开(公告)号：GB918720A

    公开(公告)日：1963-02-20

    申请号：GB3262361

    申请日：1961-09-12

    Applicant: BASF AG

    Inventor： LAUTENSCHLAGER HANS ,  WITTENBERG DIETMAR

    IPC: C07F5/06

    Abstract: Arylaluminium compounds may be produced by reacting aryl halides and activated aluminium. Suitable aryl halides include iodobenzene, bromobenzene, chlorobenzene, 1-chloronaphthalene, 2-chloronaphthalene, halo-toluenes and halo-xylenes. Compounds with several halo-phenyl radicals or with more than one halogen attached to the phenyl nucleus may be used. The aluminium should be comminuted e.g. aluminium dust, powder or grit, and may be activated by mechanical and/or chemical means. A halide of an element of Group Ia, IIa or IIIa may be present, or may be added to the reaction product. A reducing metal e.g., lithium, sodium, potassium, magnesium, calcium, barium, zinc, titanium or magnesium may also be present, and if desired the aluminium may be used as an alloy. Inert solvents such as aliphatic or aromatic hydrocarbons may be used, but it is preferred to use as solvent the aryl halide employed in the reaction. The immediate product of the reaction is a sesquichloride, which by reaction with a p Group Ia, IIa or IIIa halide may be separated into its components, (thus phenyl-aluminium sesquichloride reacts with sodium chloride to give sodium phenyl aluminium trichloride and sodium diphenyl aluminium dichloride) or which by reaction with a reducing metal gives a triaryl aluminium compound.

    Production of liquid oligomers of 1,3-dienes
    39.
    发明专利
    Production of liquid oligomers of 1,3-dienes 未知

    公开(公告)号：GB1002721A

    公开(公告)日：1965-08-25

    申请号：GB2137562

    申请日：1962-06-04

    Applicant: BASF AG

    Inventor： WITTENBERG DIETMAR

    IPC: C07C2/40

    Abstract: Liquid, mainly acyclic, oligomers of 1,3-diolefins are obtained from the dienes in the presence of a catalyst obtained from a cobalt compound and a reducing agent the ratio of cobalt in mols. to reducing agent in equivalents being below 1. Optionally the catalyst is prepared in the presence of an olefinic or acetylenic compound as activator and a polymerization inhibitor and/or a base may be added. The diolefin may be butadiene, isoprene, 2,3-dimethyl butadiene, 2-ethylbutadiene, pentadiene-1,3, hexadiene-2,4 or a dimer of butadiene obtained by the process, e.g. 3-methyltheptatriene-1,4,6 or octatriene-1,3,6. The cobalt compound may be an organic or inorganic salt or a chelate compound and is used in amounts of 0.1-10% by weight of the diene. Suitable reducing agents are metals of Group Ia, IIa, IIb, IIIa or IIIb, or a hydride or organo-derivative or complex thereof of a metal of Group Ia, IIa, IIb, IIIa or IVa (non-transition metals being in the B sub-groups). A compound containing up to 4 olefinic or up to 3 acetylenic groups may also be added in a molar proportion to cobalt of 1 : 1 or greater, such compound being a hydrocarbon or containing inert groups, e.g. ether, hydroxy, carboxylic ester, nitrile, carboxylicamide, amine, imine, epoxy, aldehyde, lactone or sulphide groups. If used in excess the activator can be used as solvent or a hydrocarbon or ether solvent may be used in an amount up to 100 times that of the cobalt compound. The catalyst is formed by mixing the ingredients at - 50 DEG to 150 DEG C. and ageing if desired; undissolved material may be filtered off. If the reducing agent is a polymerization catalyst an inhibitor must be added, e.g. water, an alcohol, phenol, aldehyde, ketone or primary or secondary amine in an amount sufficient to react with excess reducing agent. Also if a halide is present an inhibitor containing a lone electron pair is added, e.g. an ether, thioether, amine, phosphine, organic phosphite, phosphate or phosphine oxide, sulphoxide, sulphone, nitrile, carboxylate, carboxylic acid or amide or anhydride thereof, nitro compound or arylhydrazine. In a preferred embodiment a base is added, e.g. oxide, hydroxide, alkoxide, amide, carbonate, bicarbonate, acetate or phenolate of an alkali or alkaline earth metal or a strong organic base such as guanidine or tetralkyl ammonium hydroxide, in an amount of 0.001 to 0.2 that of the diene; this increases the production of conjugated triene dimers. The base is added in solution in water or an alcohol or on a carrier such as alumina or silica gel. Oligomerization is effected at 0-250 DEG C. for up to 30 hours at a pressure up to 30 atm. to maintain the liquid phase. All the diene may be added at the beginning which favours the production of dimers or gradually or in increments when higher oligomers are formed.ALSO:Liquid, mainly acyclic, oligomers of 1,3-diolefins are obtained from the dienes in the presence of a catalyst obtained from a cobalt compound and a reducing agent the ratio of cobalt in mols to reducing agent in equivalents being below 1. Optionally the catalyst is prepared in the presence of an olefinic or acetylenic compound as activator and a polymerization inhibitor and/or a base may be added. The cobalt compound may be an organic or inorganic salt of a chelate compound and is used in amounts of 0,1-10% by weight of the diene. Suitable reducing agents are metals of Group Ia, IIa, IIb, IIIa or IIIb, or a hydride or organo-derivative or complex thereof of a metal of Group Ia, IIa, IIb, IIIa or IVa (non-transition metals being in the B sub group). A compound containing up to 4 olefinic or up to 3 acetylenic groups may also be added in a molar proportion to cobalt of 1 : 1 or greater, such compound being a hydrocarbon or containing inert groups, e.g. ether, hydroxy, carboxylic ester, nitrile, carboxylic amide, amine, imine, epoxy, aldehyde, lactone or sulphide groups. If used in excess the activator can be used as solvent or a hydrocarbon or ether solvent may be used in an amount up to 100 times that of the cobalt compound. The catalyst is formed by mixing the ingredients at -50 DEG C. to 150 DEG C. and ageing if desired; undissolved material may be filtered off. If the reducing agent is a polymerization catalyst an inhibitor must be added, e.g. water, an alcohol, phenol, aldehyde, ketone or primary or secondary amine in an amount sufficient to react with excess reducing agent. Also if a halide is present an inhibitor containing a lone electron pair is added, e.g. an ether, thioether, amine, phosphine, organc phosphite, phosphate or phosphine oxide, sulphoxide, sulphone, nitrile, carboxylate, carboxylic acid or amide or anhydride thereof, nitro compound or arylhydrazine. In a preferred embodiment a base is added, e.g. oxide, hydroxide, alkoxide, amide, carbonate, bicarbonate, acetate or phenolate of an alkali or alkaline earth metal or a strong organic base such as guanidine or tetralkyl ammonium hydroxide, in an amount of 0,001-0,2 that of the diene; this increases the production of conjugated triene dimers. The base is added in solution in water or an alcohol or on a carrier such as alumina or silica gel.

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