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    Production of oligomers of 1,3-diones
    32.
    发明专利
    Production of oligomers of 1,3-diones 未知

    公开(公告)号：GB923470A

    公开(公告)日：1963-04-10

    申请号：GB3295061

    申请日：1961-09-14

    Applicant: BASF AG

    Inventor： MUELLER HERBERT

    IPC: B01J31/22 ,  B01J31/26 ,  C07C2/46 ,  C07C2/52

    Abstract: A catalyst for the oligomerization of 1, 3-dienes to form cyclic olefins is made by mixing in any sequence, (a) a divalent nickel compound, (b) a metal having a reducing action on the divalent nickel compound, and (c) an organic compound of an element of Group V(a) of the Periodic System which has an atomic weight of at least 30. The component (a) may be nickel chloride, sulphide, cyanide, bromide, iodide, carbonate, formate, acetate, oxalate, oxide, benzoate, hydroxide, sulphate, nitrate, acetylacetonate, acetylacetonate dialcoholate, acetylacetonate diphenolate, acetoacetic esters, benzoylacetonate, or nickel dimethyl glyoxime. Suitable metals are lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium or cerium. The (c) catalyst component is preferably selected from the following groups, organic phosphines, phosphine oxides, arsines, stibines, phosphorous acid esters, thiophosphorous acid esters, or phosphorous acid tri-amides substituted by organic radicals. A long list of suitable (c) components are specified. Exemplified (c) components are triphenyl phosphine, triphenyl phosphite, triphenyl phosphine oxide, triphenyl stibine, tri- (o-tolyl) phosphine, and triphenyl arsine. Prior to, during, or after the preparation of the catalyst, a small amount, e.g. 1 to 10% by weight of the mixture, of a hydrocarbon containing ethylenic or acetylenic unsaturation, may be added to the catalyst. Specified dienes are butadiene, 2-methyl butadiene-(1, 3), 2, 3-dimethylbutadiene-(1, 3), 2-ethylbutadiene-(1, 3), pentadiene-(1, 3), hexadiene-(1, 3), hexadiene-(2, 4), cyclohexadiene-(1, 3) and cyclooctadiene-(1, 3). A halide of an element of Group II(b) or III(a) may also be included with the catalyst components. Specified halides are boron trichloride, aluminium chloride or bromide, gallium bromide, indium chloride, thallium chloride, zinc chloride, and cadmium chloride. The Periodic Table used is published in "The Handbook of Chemistry and Physics" 39th Edition, 1957/58 , on pages 400-401. Cyclic olefins prepared from butadiene are cyclooctadiene, cyclododecatriene and vinylcyclohexene.

    33.
    发明专利
    未知

    公开(公告)号：FR1321808A

    公开(公告)日：1963-03-22

    申请号：FR896466

    申请日：1962-05-04

    Applicant: BASF AG

    Inventor： MUELLER HERBERT

    IPC: C08F36/04

    34.
    发明专利
    未知

    公开(公告)号：FR1301247A

    公开(公告)日：1962-08-10

    申请号：FR873793

    申请日：1961-09-21

    Applicant: BASF AG

    Inventor： MUELLER HERBERT

    IPC: B01J31/22 ,  B01J31/26 ,  C07C2/46 ,  C07C2/52

    Abstract: A catalyst for the oligomerization of 1, 3-dienes to form cyclic olefins is made by mixing in any sequence, (a) a divalent nickel compound, (b) a metal having a reducing action on the divalent nickel compound, and (c) an organic compound of an element of Group V(a) of the Periodic System which has an atomic weight of at least 30. The component (a) may be nickel chloride, sulphide, cyanide, bromide, iodide, carbonate, formate, acetate, oxalate, oxide, benzoate, hydroxide, sulphate, nitrate, acetylacetonate, acetylacetonate dialcoholate, acetylacetonate diphenolate, acetoacetic esters, benzoylacetonate, or nickel dimethyl glyoxime. Suitable metals are lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium or cerium. The (c) catalyst component is preferably selected from the following groups, organic phosphines, phosphine oxides, arsines, stibines, phosphorous acid esters, thiophosphorous acid esters, or phosphorous acid tri-amides substituted by organic radicals. A long list of suitable (c) components are specified. Exemplified (c) components are triphenyl phosphine, triphenyl phosphite, triphenyl phosphine oxide, triphenyl stibine, tri- (o-tolyl) phosphine, and triphenyl arsine. Prior to, during, or after the preparation of the catalyst, a small amount, e.g. 1 to 10% by weight of the mixture, of a hydrocarbon containing ethylenic or acetylenic unsaturation, may be added to the catalyst. Specified dienes are butadiene, 2-methyl butadiene-(1, 3), 2, 3-dimethylbutadiene-(1, 3), 2-ethylbutadiene-(1, 3), pentadiene-(1, 3), hexadiene-(1, 3), hexadiene-(2, 4), cyclohexadiene-(1, 3) and cyclooctadiene-(1, 3). A halide of an element of Group II(b) or III(a) may also be included with the catalyst components. Specified halides are boron trichloride, aluminium chloride or bromide, gallium bromide, indium chloride, thallium chloride, zinc chloride, and cadmium chloride. The Periodic Table used is published in "The Handbook of Chemistry and Physics" 39th Edition, 1957/58 , on pages 400-401. Cyclic olefins prepared from butadiene are cyclooctadiene, cyclododecatriene and vinylcyclohexene.

    Production of benzene and its trisubstituted and hexasubstituted derivatives
    36.
    发明专利
    Production of benzene and its trisubstituted and hexasubstituted derivatives 未知

    公开(公告)号：GB890542A

    公开(公告)日：1962-03-07

    申请号：GB3563460

    申请日：1960-10-18

    Applicant: BASF AG

    Inventor： MUELLER HERBERT ,  FRIEDERICH HERBERT

    IPC: C07C2/48

    Abstract: The trimerization of acetylenes to benzenes is effected in the presence as catalyst of:- (i) an iron (III) halide or a titanium or nickel compound (ii) a metal of Group Ia, IIa, IIb, IIIa or the lanthanide series and (iii) a halide of an element of Group IIb, IIIa, IVa or Va, aluminium or an aluminium halide being essentially present; the Periodic Table references are to one in which the transition elements are in sub-Groups B and Group VIII and the remaining elements in sub-Groups A. In the catalyst system the compound (i) may be a lower alkyl titanate, e.g. titanium tetra-methylate, -ethylate or -propylate, a titanium halide, e.g. the tri- or tetra-chloride or -bromide, a titanium ester halide, e.g. diethoxy titanium dichloride or dibutoxy titanium dibromide, organo-titanium halides, e.g. bis-cyclopentadienyl titanium dichloride or dimethyl titanium dibromide, ferric chloride or bromide, or nickel salts or chelate complexes, e.g. nickelous chloride, bromide, iodide, carbonate, formate, acetate, oxalate, benzoate, oleate, sulphate or nitrate nickel acetylacetonate, nickel acetoacetic acid ester, nickel benzoyl acetonate, nickel monoacetyl-acetonate ethylate, nickel dimethylglyoxime, nickelous oxide, hydroxide or sulphide or nickelic hydroxide. Nickel compounds are preferably anhydrous, those containing water of crystallization may be used with an excess of metal (ii). The metal (ii) may be lithium, sodium, potassium, berryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc or cerium and preferably has a large surface area. The halide (iii) may be a chloride or bromide of boron, aluminium, gallium, indium, thallium, silicon, tin, zinc, phosphorus, antimony or bismuth. Where compound (i) is a halide and metal (ii) is aluminium, aluminium halide as halide (iii) may be formed in situ. A compound forming a complex with the halide (iii) may be used, e.g. an ether, thioether, sulphoxide nitrone, tertiary base, or alkali or alkaline earth halide, hydroxide, hydride or cyanide, typical examples being anisol, phenetol, diethyl ether, diphenyl ether, diphenylene oxide, diphenyl sulphide, thiobutyric acid, quinoline, triethylamine, sodium chloride, magnesium chloride, calcium chloride, lithium hydride, calcium hydride, and potassium cyanide. The mol. ratio of (i) to redox equivalent of (ii) to mol. of (iii) may be from 1:300:100 to 1:10:10 or the titanium compound may be in excess and the mol. ratio of the sum of (i) and (iii) to complex forming compound may be 1:0,2-3. The total amount of catalyst may be as low as 0,3% by weight of the acetylene. Two or all of the components of the catalyst are preferably ground in a ball mill at up to 150 DEG C. for 1-10 hours in the solvent to be used which is present in an amount of 0,2 to 0,5 that of the acetylene and may be, e.g. benzene, toluene, xylene, pentane, ethylbenzene, cumene, chlorobenzene, heptane, cyclohexane, iso-octane or tetrahydrofurane. Specification 802,510 is referred to.ALSO:The production of benzene or tri- or hexasubstituted benzenes by the trimerisation of acetylene or a mono- or di-substituted acetylene is effected in the presence as catalyst of (i) an iron (III) halide or a titanium or nickel compound; (ii) a metal of group Ia, IIa, IIba or the lanthanide series; and (iii) a halide of an element of group IIb, IIIa, IVa or Va; aluminium or an aluminium halide being essentially present; the Periodic Table references are to one in which the transition elements are in sub-groups B and group VIII and the remaining elements in sub-groups A. The starting material may be acetylene propine, butine-1, pentine-1, hexine-1, octine-1, dodecine-1, octadecine-9, octadecine-1, vinyl acetylene, phenyl acetylene, cyclohexyl acetylene, benzyl acetylene, butine-2, hexine-3, methyl ethyl acetylene or tolane. In the catalyst system the compound (i) may be a lower alkyl titanate, e.g. titanium tetra-methylate, -ethylate or -propylate, a titanium halide, e.g. the tri- or tetra-chloride or -bromide, a titanium ester halide, e.g. diethoxy titanium dichloride or dibutoxy titanium dibromide, organo-titanium halides, e.g. bis-cyclopentadienyl titanium dichloride or dimethyl titanium dibromide, ferric chloride or bromide, or nickel salts or chelate complexes, e.g. nickelous chloride, bromide, iodide, carbonate, formate, acetate, oxalate, benzoate, oleate, sulphate or nitrate nickel acetylacetonate, nickel acetoacetic acid ester, nickel benzoyl acetonate nickel monoacetylacetonate ethylate, nickel dimethylglyoxime, nickelous oxide, hydroxide or sulphide or nickelic hydroxide. Nickel compounds are preferably anhydrous, those containing water of crystallisation may beused with an excess of metal (ii). The metal (ii) may be lithium sodium, potassium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc or cerium and preferably has a large surface area. The halide (iii) may be a chloride or bromide of boron, aluminium, gallium, indium, thallium, silicon, tin, zinc, phosphorus, antimony or bismuth. Where compound (i) is a halide and metal (ii) is aluminium, aluminium halide as halide (iii) may be formed in situ. A compound forming a complex with the halide (iii) may be used, e.g. an ether, thioether, sulphoxide nitrone, tertiary base, or alkali or alkaline earth halide, hydroxide, hydride or cyanide, typical examples being anisol, phenetol, diethyl ether, diphenyl ether, diphenylene oxide, diphenyl sulphide, thiobutyric acid, quinoline, triethylamine, sodium chloride, magnesium chloride, calcium chloride, lithium hydride, calcium hydride, and potassium cyanide. The mol ratio of (i) to redox equivalent of (ii) to mol of (iii) may be from 1 : 300 : 100 to 1 : 10 : 10 or the titanium compound may be in excess and the mol ratio of the sum of (i) and (ii) to complex forming compound may be 1 : 0.2-3. The total amount of catalyst may be as low as 0.3% by weight of the acetylene. Two or all of the components of the catalyst are preferably ground in a ball mill at up to 150 DEG C. for 1-10 hours in the solvent to be used which is present in an amount of 0.2 to 0.5 that of the acetylene and may be, e.g. benzene, toluene, xylene, pentane, ethylbenzene, cumene, chlorobenzene, heptane, cyclohexane, iso-octane, or tetrahydrofurane. The reaction temperature may be -5 DEG C. to 150 DEG C. and the pressure preferably atmospheric or up to 10 atmospheres gauge if low-boiling reactants are used.

    40.
    发明专利
    未知

    公开(公告)号：DE4219129A1

    公开(公告)日：1993-12-16

    申请号：DE4219129

    申请日：1992-06-11

    Applicant: BASF AG

    Inventor： PFLEGER KLAUS DR ,  ARNOLD GERHARD ,  SCHILLER SIEGFRIED ,  MUELLER HERBERT

    IPC: C08F2/00 ,  C08F2/34 ,  C08F2/38 ,  C08F210/02 ,  C08F220/12 ,  H01B3/44

    Abstract: A process for the preparation of copolymers of ethylene with acrylic esters (acrylates) by copolymerisation of 100 parts by weight of ethylene with from 0.1 to 25.0 parts by weight of acrylic esters in a continuous, tubular polymerisation system at pressures of from 500 to 4,000 bar and temperatures of from 100 to 400 DEG C in the presence of polymerisation initiators which decompose to form free radicals, where the temperature regime for the reaction mixture comprising ethylene, acrylic esters, polymerisation initiators and optionally regulators after entry into the reaction zone is designed in such a way that the quotient dT/dt (increase in temperature per time unit) is kept constant at a value between 1.5 and 2.5 DEG C per second.

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