MIXTURE COMPRISING BIS(SILYLORGANYL)POLYSULFANE AND SILYLORGANYL THIOCYANATE, ITS PRODUCTION AND PRODUCTION OF VULCANIZABLE PLASTIC-RUBBER MIXTURE

    公开(公告)号:JPH11116583A

    公开(公告)日:1999-04-27

    申请号:JP21260798

    申请日:1998-07-28

    Applicant: DEGUSSA

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject mixture useful for the production or the like of a vulcanizable plastic-rubber mixture by reacting a silylorganylpolysulfane or the like with a metallic cyanide compound and then reacting the resultant compound with a halogenalkylalkoxysilane. SOLUTION: A silylorganylpolysulfane (mixture) represented by formula I R to R are each a 1-8C alkyl and/or a 1-8C alkoxy group in which at least one thereof is the alkoxy group; R is a 1-8C bivalent alkylidene or a group represented by formula II [(y) is 1-4]; (n) is 2-20} is reacted with a nucleophilic compound represented by the formula M CN [M is an alkali metallic cation, a (substituted)ammonium ion, a half alkaline earth metallic ion or zinc ion] and the resultant compound is then reacted with a compound represented by formula III at a high temperature under a high pressure to afford a mixture of a bis(silylorganyl)polysulfane represented by formula IV [X is Sn when (x) is 2 and X is SCN when (x) is 1] with a silylorganyl thiocyanate useful as a phase transfer assistant or the like for incorporating an acidic substance in a rubber matrix for the production or the like of a vulcanizable mixture.

    PRODUCTION OF HIGH-PURITY ORGANOSILICON DISULFANE

    公开(公告)号:JPH11116585A

    公开(公告)日:1999-04-27

    申请号:JP22315598

    申请日:1998-08-06

    Applicant: DEGUSSA

    Abstract: PROBLEM TO BE SOLVED: To produce the subject new high-purity compound useful for the production or the like of tires by reacting elementary sulfur with an anhydrous sulfide and a specific organosilicon compound in a specific proportion in a polar organic solvent and further adding and reacting an anhydrous sulfide therewith. SOLUTION: Elementary sulfur and a part of all of an anhydrous sulfide represented by the formula MeS [Me is an alkali (alkaline earth) metal, zinc or ammonium] are dissolved or suspended in a polar organic solvent at (1:0.2) to (1:0.9) molar ratio and an organosilicon compound represented by formula I [Z is a group represented by formula II (R1 is a 1-5C alkyl, a 5-8C cycloalkyl, benzyl or phenyl; R is a 1-5C alkoxy, a 5-8C cycloalkoxy, phenoxy or benzyloxy); Alk is a 1-10C bivalent saturated hydrocarbon or a group represented by formula III; Hal is Cl or Br] and the resultant solution or suspension is then reacted with the compound represented by the formula I so as to provide (1.2:1) to (2:1) molar ratio of the compound represented by the formula I to S. A compound represented by the formula; Me2 S in an amount so that the sulfide and the total amount of the elementary sulfur are nearly equimolar is added thereto. The resultant product is subsequently isolated to provide a high-purity organosilicon disulfane represented by formula IV.

    3.
    发明专利
    未知

    公开(公告)号:DE59806324D1

    公开(公告)日:2003-01-02

    申请号:DE59806324

    申请日:1998-06-30

    Applicant: DEGUSSA

    Abstract: Two-stage preparation of highly pure organosilicon disulfans of formula Z-Alk-S2-Alk-Z (I) comprises (1) dissolving or suspending sulfur (S) and an anhydrous sulfide of formula Me2S (II) in 1:(0.2-0.9) molar ratio and treating the solution or suspension with an organosilicon compound of formula Z-Alk-Hal (III), with a molar ratio of (III) to sulfur of (1.2-2):1; and (2) adding more (II) after reaction, in an amount approximately equimolar to the total amounts of (II) and S used for reaction, and isolating (I); in which Z = -Si(R )2R , -Si(R )(R )2 or -Si(R )3; R = 1-5C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group optionally substituted by methyl (Me), ethyl (Et) or chlorine (Cl); R = 1-5C alkoxy, 5-8C cycloalkoxy, phenoxy or benzyloxy; Alk = a 1-10C divalent, saturated linear or branched hydrocarbon group or -CH2-Phe-CH2-; Phe = phenylene; Me = ammonium, an alkali metal or one equivalent of an alkaline earth metal or zinc; Hal = Cl or bromine (Br).

    4.
    发明专利
    未知

    公开(公告)号:ES2187857T3

    公开(公告)日:2003-06-16

    申请号:ES98112029

    申请日:1998-06-30

    Applicant: DEGUSSA

    Abstract: Two-stage preparation of highly pure organosilicon disulfans of formula Z-Alk-S2-Alk-Z (I) comprises (1) dissolving or suspending sulfur (S) and an anhydrous sulfide of formula Me2S (II) in 1:(0.2-0.9) molar ratio and treating the solution or suspension with an organosilicon compound of formula Z-Alk-Hal (III), with a molar ratio of (III) to sulfur of (1.2-2):1; and (2) adding more (II) after reaction, in an amount approximately equimolar to the total amounts of (II) and S used for reaction, and isolating (I); in which Z = -Si(R )2R , -Si(R )(R )2 or -Si(R )3; R = 1-5C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group optionally substituted by methyl (Me), ethyl (Et) or chlorine (Cl); R = 1-5C alkoxy, 5-8C cycloalkoxy, phenoxy or benzyloxy; Alk = a 1-10C divalent, saturated linear or branched hydrocarbon group or -CH2-Phe-CH2-; Phe = phenylene; Me = ammonium, an alkali metal or one equivalent of an alkaline earth metal or zinc; Hal = Cl or bromine (Br).

    6.
    发明专利
    未知

    公开(公告)号:DD135494A5

    公开(公告)日:1979-05-09

    申请号:DD20280977

    申请日:1977-12-20

    Applicant: DEGUSSA

    Abstract: There are prepared compounds of the formula [Rn1(R2O)3-n-Si-Alk-S-]xZ(I) where Z is 3BOND PO, 3BOND PS, 3BOND P, =PR, -P(R)2, -P(OR)2, =P(OR), -PO(OR)2, -PS(OR)2, =PO(OR) or =PS(OR) where R is an alkyl group of 1 to 5 carbon atoms, phenyl or o-, m- or p-nitrophenyl; Alk is an alkylene group with 2 to 4 carbon atoms; R1 is an alkyl group having 1 to 5 carbon atoms, benzyl or phenyl; R2 is an alkyl group having 1 to 5 carbon atoms, a cycloalkyl group having 5 to 8 carbon atoms, phenyl, benzyl or 2-methoxyethyl, each R1 and R2 can have the same or different meanings; n is 0, 1 or 2; and, x is 1, 2 or 3, being the residual valence of Z. The compounds are useful as reinforcing agents in vulcanizable rubber mixtures which contain a silicate filler and optionally carbon black.

    7.
    发明专利
    未知

    公开(公告)号:PT895996E

    公开(公告)日:2003-03-31

    申请号:PT98112029

    申请日:1998-06-30

    Applicant: DEGUSSA

    Abstract: Two-stage preparation of highly pure organosilicon disulfans of formula Z-Alk-S2-Alk-Z (I) comprises (1) dissolving or suspending sulfur (S) and an anhydrous sulfide of formula Me2S (II) in 1:(0.2-0.9) molar ratio and treating the solution or suspension with an organosilicon compound of formula Z-Alk-Hal (III), with a molar ratio of (III) to sulfur of (1.2-2):1; and (2) adding more (II) after reaction, in an amount approximately equimolar to the total amounts of (II) and S used for reaction, and isolating (I); in which Z = -Si(R )2R , -Si(R )(R )2 or -Si(R )3; R = 1-5C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group optionally substituted by methyl (Me), ethyl (Et) or chlorine (Cl); R = 1-5C alkoxy, 5-8C cycloalkoxy, phenoxy or benzyloxy; Alk = a 1-10C divalent, saturated linear or branched hydrocarbon group or -CH2-Phe-CH2-; Phe = phenylene; Me = ammonium, an alkali metal or one equivalent of an alkaline earth metal or zinc; Hal = Cl or bromine (Br).

    8.
    发明专利
    未知

    公开(公告)号:DE19732725A1

    公开(公告)日:1999-02-04

    申请号:DE19732725

    申请日:1997-07-30

    Applicant: DEGUSSA

    Abstract: Mixtures of bis(organosilyl)sulphanes (IA) and organosilyl thiocyanates (IB) of formula: (R R R SiR )xX (I) (Where: X = Sn; n = 2-20, especially 2-8 if x = 2; and X = SCN if x = 1 (thiocyanato-silane); (a) R , R , R = 1-8 carbon (C) alkyl and/or alkoxy or (b) at least one of R , R , R = alkoxy, the rest = H or monovalent aryl, especially phenyl, tolyl or benzyl; R = divalent 1-8, especially 2-4 C alkylidene or -(CH2)y-Phe-(CH2)y-; Phe = phenylene; y = 1-4.) Also claimed is a method of producing the mixtures.

    9.
    发明专利
    未知

    公开(公告)号:PT894803E

    公开(公告)日:2003-06-30

    申请号:PT98112124

    申请日:1998-07-01

    Applicant: DEGUSSA

    Abstract: Mixtures of bis(organosilyl)sulphanes (IA) and organosilyl thiocyanates (IB) of formula: (R R R SiR )xX (I) (Where: X = Sn; n = 2-20, especially 2-8 if x = 2; and X = SCN if x = 1 (thiocyanato-silane); (a) R , R , R = 1-8 carbon (C) alkyl and/or alkoxy or (b) at least one of R , R , R = alkoxy, the rest = H or monovalent aryl, especially phenyl, tolyl or benzyl; R = divalent 1-8, especially 2-4 C alkylidene or -(CH2)y-Phe-(CH2)y-; Phe = phenylene; y = 1-4.) Also claimed is a method of producing the mixtures.

    10.
    发明专利
    未知

    公开(公告)号:DK0894803T3

    公开(公告)日:2003-04-22

    申请号:DK98112124

    申请日:1998-07-01

    Applicant: DEGUSSA

    Abstract: Mixtures of bis(organosilyl)sulphanes (IA) and organosilyl thiocyanates (IB) of formula: (R R R SiR )xX (I) (Where: X = Sn; n = 2-20, especially 2-8 if x = 2; and X = SCN if x = 1 (thiocyanato-silane); (a) R , R , R = 1-8 carbon (C) alkyl and/or alkoxy or (b) at least one of R , R , R = alkoxy, the rest = H or monovalent aryl, especially phenyl, tolyl or benzyl; R = divalent 1-8, especially 2-4 C alkylidene or -(CH2)y-Phe-(CH2)y-; Phe = phenylene; y = 1-4.) Also claimed is a method of producing the mixtures.

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