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    Production of 1,3-diene polymers in aqueous emulsion
    61.
    发明专利
    Production of 1,3-diene polymers in aqueous emulsion 未知

    公开(公告)号：GB1149793A

    公开(公告)日：1969-04-23

    申请号：GB3859166

    申请日：1966-08-30

    Applicant: BASF AG

    Inventor： NAARMANN HERBERT ,  KASTNING ERNST-GUENTHER

    IPC: C08F36/04

    Abstract: 1,149,793. Catalysts for diene polymerization. BADISCHE ANILIN- & SODA-FABRIK A.G. 30 Aug., 1966 [31 Aug., 1965], No. 38591/66. Heading C3P. Conjugated dienes are polymerized in aqueous emulsion using as catalyst a cation exchanger having combined therewith a transition metal as ions. Cocatalysts such as organic halogen compounds and ethylenically unsaturated cycloaliphatic compounds may be added to the emulsion. The process is also applicable to the production of copolymers e.g. with styrene.

    Production of 1,3-diene polymers
    63.
    发明专利
    Production of 1,3-diene polymers 未知

    公开(公告)号：GB1144884A

    公开(公告)日：1969-03-12

    申请号：GB2813366

    申请日：1966-06-23

    Applicant: BASF AG

    Inventor： NAARMAAN HERBERT ,  EILINGSFIELD HEINZ ,  KASTNING ERNST-GUENTHER

    IPC: C08F36/04 ,  C08F36/06

    Abstract: 1,144,884. Polymerizing dienes. BADISCHE ANILIN- & SODA-FABRIK A.G. 23 June, 1966 [24 June, 1965], No. 28133/66. Heading C3P. Polymers of dienes are made by polymerizing 1,3-dienes containing 4-6 carbon atoms in the presence of a catalyst which comprises a transition metal chelate complex of a thio-α, γ-dicarbonyl compound. A co-catalyst such as a cycloalkene, an organic halogen compound, or transition metal chelate complexes of α,γ-dicarbonyl compounds which contain no sulphur, or a salt of a metal of Groups I to III of the Mendeleev Periodic Table may also be present. Suitable complexes are copper (II) thioacetoacetic ethyl ester, cobalt (III) monothioacetylacetonate, manganese (III) mono-thiobenzoylacetone, cerium (IV) dithiobenzoyl-methane, and thallium (I) monothioacetyl acetonate. The Specification contains extensive lists of co-catalysts. The polymerization may be effected in bulk, solution, suspension, or emulsion, particularly aqueous emulsion using conventional recipes. Stabilizers such as trinonylphenyl phosphite, may be added before or during polymerization. Specified dienes are butadiene, isoprene, 2,3-dimethylbutadiene, 2- phenylbutadiene, and chloroprene. Minor amounts of other ethylenic compounds may be copolymerized with the diene e.g. esters of acrylic and methacrylic acid, esters of fumaric and maleic acids, acrylic acid, methacrylic acid, acrylo or methacrylonitrile, styrene, vinylethers and vinyl esters. The polymers are preferably recovered from the aqueous emulsions by adding, prior to precipitation of the polymer, a strong complex - forming substance which binds the metal ions of the catalyst into watersoluble stable complex compounds. The polymers are suitable for motor tyres.

    Production of elastomeric 1,3-diene polymers having improved strength and elongation
    64.
    发明专利
    Production of elastomeric 1,3-diene polymers having improved strength and elongation 未知

    公开(公告)号：GB1127135A

    公开(公告)日：1968-09-11

    申请号：GB5091165

    申请日：1965-12-01

    Applicant: BASF AG

    Inventor： NAARMANN HERBERT ,  KASTNING ERNST-GUENTHER

    IPC: C08F36/04 ,  C08F279/02

    Abstract: 1,127,135. Diene graft polymers. BADISCHE ANILIN- & SODA-FABRIK A.G. 1 Dec., 1965 [2 Dec., 1964], No. 50911/65. Heading C3G. 1,3-Dienes are polymerized in aqueous emulsion using a polymerization catalyst and in the presence of a diene polymer which has a crystallinity of more than 30% and a molecular weight of 15,000 to 1,500,000. The reaction is carried out at - 10‹ to 100‹ C. at a pressure of 1 to 20 atmospheres absolute. The catalysts may be inorganic or organic peroxides, redox systems or metal chelate complexes such as those described in Specification 1,065,406 and may be supplied to the polymerization vessel as an emulsion in a portion of the aqueous reaction medium. The partly crystalline diene polymers are generally derived from linear or branched aliphatic 1,3-dienes having 4 to 6 carbon atoms and are exemplified by 1,4-trans polyisoprene, 1,4-trans-butadiene and a polyisoprene having a 1,2-vinyl fraction of less than 10%; they are preferably supplied to the graft reaction in solution in hydrocarbons or emulsified, and may be supplied either continuously or intermittently during the polymerization. Suitable 1,3-dienes having 4-10 carbon atoms are butadiene, isoprene, 2,3-dimethylbutadiene, 2-phenylbutadiene, and 2-chlorobutadiene. In Examples 1 and 3, the 1,3-dienes are partially polymerized before the partially crystalline diene polymer is added. Monoethylenically unsaturated compounds, such as (a) α,#- ethylenically unsaturated aliphatic monocarboxylic acids having 3 or 4 carbon atoms and their esters particularly with alkanols having 1-8 carbon atoms, (b) esters of fumaric acid and maleic acid particularly with alkanols having 1-4 carbon atoms, (c) acrylic and/or methacrylic compounds such as their amides, nitriles and N-methylol derivatives thereof, (d) vinylaromatic compounds having one benzene nucleus, (e) vinyl ethers particularly of alkanols having 1-4 carbon atoms, and (f) vinyl ketones having 4 or 5 carbon atoms, may be copolymerized with the 1,3-dienes provided that these 1,3-dienes comprise at least 50% by weight of the total monomers.

    Production of tin containing polymerisation products
    65.
    发明专利
    Production of tin containing polymerisation products 未知

    公开(公告)号：GB1118135A

    公开(公告)日：1968-06-26

    申请号：GB4672465

    申请日：1965-11-04

    Applicant: BASF AG

    Inventor： NAARMANN HERBERT ,  KASTNING ERNST-GUENTHER

    IPC: C08C19/26 ,  C08F279/02

    Abstract: The reaction products of alkyl or aryl tin halides or hydrides and polymers of butadiene or isoprene with a degree of polymerization of at least four are polymerized in the presence of 0.001 to 3% of a polymerization initiator. The tin hydrides may be triisobutyl or tri-n-butyl hydride, diisobutyltin dihydride, diethyltin-dihydride or diphenyltin dihydride while the reaction product may have a tin content of 1 to 20%. Comonomers may be present and the copolymers preferably contain 5 to 25% of the reaction product. The polymerization may take place in solution, in aqueous suspension with an emulsifier, and continuously or as a batch process, to 70% conversion. In Examples (1) the reaction product of 82% cis-1-4-polybutadiene and diisobutyltin dihydride is polymerized with 3 times the amount of styrene, using butyllithium as catalyst, (2) 50 parts of the reaction product of polybutadiene of 60% 1-2-vinyl and triethyltin hydride are mixed with 100 parts polybutadiene of 94% cis-1-4 content, 500 parts styrene and 0.5 parts di-t-butyl peroxide and polymerized to a graft polymer, (3) a polyisoprene-13.8% tin reaction product containing 9% 1,2-vinyl is polymerized with a mixture of acrylonitrile and styrene using t-butyl peroxide, (4) a polybutadiene-5.3% tin reaction product is polymerized with styrene using t-butyl perbenzoate and (5) 80% 1-4-trans polybutadiene-3.9% tin reaction product is polymerized with butadiene and styrene using a mixture of sodium and naphthalene.

    Production of 1,3-diene polymers in aqueous media
    67.
    发明专利
    Production of 1,3-diene polymers in aqueous media 未知

    公开(公告)号：GB1092854A

    公开(公告)日：1967-11-29

    申请号：GB1052265

    申请日：1965-03-12

    Applicant: BASF AG

    Inventor： NAARMANN HERBERT ,  KASTNING ERNST-GUENTHER

    IPC: C08F2/08 ,  C08F36/04

    Abstract: 1,3-Dienes are polymerized in aqueous emulsion using 0.001 to 3% of a catalyst mixture of (a) a chelate complex of a metal with a 1,3-dicarbonyl compound, and (b) a cycloalkene having 5 to 12 ring carbon atoms, the metal being monovalent and/or divalent copper, silver or mercury, monovalent and/or trivalent thallium, trivalent chromium, manganese and cobalt, tetravalent cerium and titanium and/or divalent nickel, platinum and palladium, the ratio of cycloalkene to chelate compound being between 0.3 to 1 and 40 to 1. Specified catalysts are copper (II) or cobalt (III) aceto-acetate, manganese (III) benzoylacetone, copper (II) malonodialdehyde, cerium (IV) dibenzoylmethane, chromium (III)-3-methyl-butane-(1)-ol-(3) acetoacetate and thallium (1) acetylacetonate. Specified cycloalkenes are cyclopentadiene, cyclohexadiene, cycloheptadiene, cyclooctatetraene, cyclooctadiene-(1,5), cyclooctadiene -(1,4), cyclooctadiene-(1,3), the cyclodecatrienes and cycloheptatriene. The diene may be butadiene, isoprene, 2,3-dimethylbutadiene-1,3 or 2-phenylbutadiene while comonomers, e.g. acrylic, methacrylic, trimaric or maleic esters, styrene or substituted styrenes, vinyl ethers and esters may also be present. The polymerization may take place in the presence of added stabilizer, e.g. trinonylphenyl phosphite; it may take place continuously, preferably to conversions of 55 to 60%.

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