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    Method of halogenating thermoplastic polyolefins
    1.
    发明授权
    Method of halogenating thermoplastic polyolefins 失效
    卤化热塑性聚烯烃的方法

    公开(公告)号：US3909486A

    公开(公告)日：1975-09-30

    申请号：US37452173

    申请日：1973-06-28

    Applicant: GEN ELECTRIC

    Inventor： LEVER RAY CLARENCE ,  WILKUS EDWARD VINCENT

    IPC: C08F8/00 ,  C08F8/20 ,  C08F8/22 ,  C08F45/04

    CPC classification number: C08F8/22 ,  C08F10/00

    Abstract: A method of halogenating thermoplastic polyolefin materials, comprising mixing a thermoplastic polyolefin in particulate form with particulate filler type material in an atmosphere comprising vaporous halogen and in progressive sequence, melting the surface portions of the particles of thermoplastic polyolefin, reacting the halogen with the molten surface portions of the polyolefin particles while combining filler with said molten surface portions, and removing the resulting halogen reacted melt which has been combined with filler from the underlying thermoplastic polyolefin material of the particles. The mixing and melting, halogenating, and the combining and removing of the combined components, are each continued until the desired extent of halogenation of the polyolefin is achieved, and can be carried to the substantial complete diminution of the particles of polyolefin material whereby the polyolefin material is substantially uniformly halogenated throughout its mass.

    Abstract translation: 一种卤化热塑性聚烯烃材料的方法，包括将颗粒形式的热塑性聚烯烃与颗粒状填料型材料混合在包含气态卤素的气氛中并按顺序排列，熔化热塑性聚烯烃颗粒的表面部分，使卤素与熔融表面反应 同时将填料与所述熔融表面部分组合，并且除去已经与颗粒的下面的热塑性聚烯烃材料与填料组合的所得卤素反应的熔体。 混合和熔融，卤化和组合和除去组合的组分各自一直持续到达到所需聚烯烃的卤化程度，并且可以承受聚烯烃材料颗粒的实质性完全减少，由此聚烯烃 材料在其整个质量中基本均匀卤化。

    4.
    发明专利
    未知

    公开(公告)号：DE1231241B

    公开(公告)日：1966-12-29

    申请号：DEG0040353

    申请日：1964-04-15

    Applicant: GEN ELECTRIC

    Inventor： WILKUS EDWARD VINCENT ,  BERGER ABE

    IPC: C07F7/02 ,  C07F17/00 ,  C07F17/02

    Abstract: Lubricating compositions comprise bis (silylmetallocene) compounds of the formula [(R1)3Si-R-Y-Z-Y1]2A, where R is a divalent hydrocarbon or halohydrocarbon radical having at least 2 carbon atoms, A is R or methylene, R1 is a monovalent hydrocarbon, halohydrocarbon, cyanoalkyl, fluoralkyl or halogen radical, Y and Y1 are carbonyl, carbinol, carbamino, carbazido or methylene, Z is a divalent metallocene radical -[Q4C5]M[C5Q4]-, where M is a transition metal, Q is hydrogen, aryl, hydroxyaryl, cycloaliphatic, nitroaliphatic, aliphatic acyl, arylacyl, carboxyaryl, aldehydic, sulpho, carboxyaryl, nitroaryl, haloaryl or haloaliphatic.ALSO:The invention comprises bis-(silylmetallocene) compounds of the formula [(R1)3Si-R-Y-Z-Y1]2A where R is a divalent hydrocarbon or halohydrocarbon radical having at least 2 carbon atoms, A is R or methylene, R1 is a monovalent hydrocarbon, halohydrocarbon, cyanoalkyl, fluoralkyl or halogen radical, Y and Y1 are carbonyl, carbinol, carbamino, carbazido or methylene, Z is a divalent metallocene radical -[Q4C5]M[C5Q4]-where M is a transition metal, Q is hydrogen, aryl, hydroxyaryl, cycloaliphatic, nitroaliphatic, aliphatic acyl, arylacyl, carboxyaryl, aldehydic, sulpho, carboxyaryl, nitroaryl, haloaryl or haloaliphatic. Specified metals are titanium, vanadium, chromium, manganese, iron, cobalt, nickel, zirconium, columbium, molybdenum, technitium, ruthenium, rhodium, palladium, hafnium, tantalum, tungsten, rhenium, osmium, indium and platinum. The compounds may be prepared by (1) reacting a dibasic acid anhydride XCOACOX, wherein X is halogen with two moles of the silylorganometallocene at - 25 DEG to 100 DEG C.; or (2) acylating a metallocene [Q5C5]M[C5Q5] with XCO.A.COX and acylating the product with two moles of a silylcarboxylic acid halide (R1)3Si-R1-COX; the carbonyl groups may be converted to other Y and Y1 groups by conventional methods. Suitable dibasic acid halides are o-, p- and m-phthaloylchloride, malonyl chloride, adipylchloride, succinylchloride, glutarylchloride, sebacoyl chloride; oxalylchloride yields bis-(silylmetallocene) compounds free of A radicals. Compounds containing a hydrolysable group may be hydrolysed to polysiloxane polymers and copolymers containing metallocene units. The examples describe the preparation of (1) 11,11 - bis(betatrimethylsilylpropionyl) terephthaloylferrocene; (2) 11,11 - bis(p - trimethyl-silylbenzoyl) adipylferrocene; (3) 11,11-bis-(gamma - trimethylsilylpropyl)p - xylylene-ferrocene; and (4) 11,11-bis(p-trimethylsilyl-benzoyl) terephthaloylferrocene. The compounds may be used as heat stabilizer for polysiloxanes-in (1) 11,11-bis(beta-trimethylsilyl-propionyl) terephthaloylferrocene is mixed with a polydimethylsiloxane gum, silica and benzoyl peroxide are added, and the composition cured. Other uses are U.V. absorbers, antioxidants, anti-knock materials, complexing agents, lubricants, coating materials and elastomers.

    7.
    发明专利
    未知

    公开(公告)号：DE1237113B

    公开(公告)日：1967-03-23

    申请号：DEG0040354

    申请日：1964-04-15

    Applicant: GEN ELECTRIC

    Inventor： WILKUS EDWARD VINCENT ,  BERGER ABE

    IPC: C07F7/02 ,  C07F9/00 ,  C07F11/00 ,  C07F13/00 ,  C07F17/00 ,  C08G77/22 ,  C08G77/48

    Abstract: Compounds of Formula (I) wherein Q11 is H, an electron donating radical (as defined) or an electron withdrawing radical (as defined), M is vanadium, chromium, molybdenum, tungsten or manganese, n is 1-5, m is 0-4, m + n = 5, x is 2 or 3 depending on the valency of M, R is H, halogen, alkoxy, hydrocarbon, halohydrocarbon or cyanoalkyl, R1 is -CH-, -(divalent hydrocarbon radical)-CHOH-or -R11-Y-, where R11 is a divalent hydrocarbon radical of at least two carbon atoms, Y is a divalent methylene, carbonyl, carbinol, carbamino or carbazido radical, and A is R or -O 1/2 , may be used as lubricants.ALSO:The invention comprises compounds of Formula (1) wherein Q11 is H, an electron donating radical (as defined) or an electron withdrawing radical (as defined), M is vanadium, chromium, molybdenum, tungsten or manganese, n is 1-5, m is 0-4, m + n = 5, x is 2 or 3 depending on the valency of M, R is H, halogen, alkoxy, hydrocarbon, halohydrocarbon or cyanoalkyl, R1 is -CH2-, -(divalent hydrocarbon radical)CHOH -or-R11-Y-, where R11 is a divalent hydrocarbon radical of at least two carbon atoms, Y is a divalent methylene, carbonyl, carbinol, carbamino or carbazido radical, and A is R or -O 1/2 -. The compounds wherein Y is carbonyl may be prepared by reacting a compound of Formula (2) (R)3-Si-R11-CO-X with a carbonyl of Formula (3) H5- mQ11mM (CO)x in the presence of a Friedel-Crafts catalyst; the carbonyl group Y in the product may be converted to the other Y groups by conventional reactions. Compounds wherein R1 is methylene may be prepared by (a) reacting the methylene lithiate of a compound of Formula (3) (see Division C2) with a halosilane; or (b) reacting the quaternized product of an aldehyde, secondary amine and a compound of Formula (3) with a substituted silyl metallic. Compounds wherein R1 is -CH2CH(OH)-may be prepared by reacting a metal carbonyl of Formula (3) substituted by a formaldehydic radical with, for example, a Grignard reagent of a halomethyl trimethyl silane. Disiloxanes, i.e. compounds wherein A is O 1/2 may be prepared by the hydrolysis of the corresponding monomer having a hydrolysable group bonded to the silicon atom. The compounds of the invention may be used as heat stabilizers for siloxane polymers. In Example 7 a polydimethyl siloxane is mixed with (CH3)3Si(CH2)3CO -[C5H4Mn(CO)3] fumed silica and benzoyl peroxide, and cured.ALSO:Metallocene carbonyl complexes of formula H5- mQ111C5M(CO)x wherein M is vanadium, chromium, molybdenum, tungsten or manganese, Q11 is H or an electron-donating or electron-withdrawing radical (as defined), m is 1-5, and x is 3 in the case of manganese and 2 in the case of the other metals, are subjected to the following reaction sequences: (a) acetylation, conversion of the acetyl radical to a -COOH radical by hypohalite reduction, reduction of the carboxylate by LiAlH4 to the carbinol, methoxylation of the carbinol, and metalation of the methoxy compound by butyl lithium to the methylene lithiate-no examples are given; (b) condensation with a mixture, or reaction product, of an aldehyde and a secondary amine, in the presence of phosphoric acid or PCl3, and quaternization of the product with an alkyl halide-in Example 2, cyclopentadiene manganese tricarbonyl is condensed with bis-(dimethylamino)-methane to yield dimethylaminomethyl cyclopentadienyl manganese tricarbonyl, which is then quaternized with CH3I.

    10.
    发明专利
    未知

    公开(公告)号：DE2332583A1

    公开(公告)日：1974-02-28

    申请号：DE2332583

    申请日：1973-06-27

    Applicant: GEN ELECTRIC

    Inventor： LEVER RAY CLARENCE ,  WILKUS EDWARD VINCENT

    IPC: C08L71/00 ,  B29B7/00 ,  B29B7/90 ,  B29B9/02 ,  B29B9/12 ,  B29C47/02 ,  C08G18/00 ,  C08J3/20 ,  C08K9/10 ,  C08L1/00 ,  C08L7/00 ,  C08L21/00 ,  C08L23/00 ,  C08L27/00 ,  C08L67/00 ,  C08L75/00 ,  C08L77/00 ,  C08L101/00 ,  H01B3/00 ,  B29B1/04

    Abstract: A method of compounding thermoplastic polymeric material and fillers, including additives and agents, and unique compounded products. The compounding method comprises mixing the thermoplastic polymeric material in particulate form with particulate filler, and in progressive sequence melting the surface portion of the thermoplastic particles, blending the filler with said molten surface portion of the thermoplastic particles and removing the resultant blended melt and filler from the surface of the thermoplastic particles. The mixing and melting, and the blending and removing, are continued until the filler is substantially assimilated into the polymeric material and the thermoplastic particles become substantially diminished by melting and blending, or the method can be carried further if desired. The compounded product thus prepared is characterized by a distinctive stratified consistency.

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