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    12.
    发明专利
    未知

    公开(公告)号：DE1158249B

    公开(公告)日：1963-11-28

    申请号：DEF0033593

    申请日：1961-04-05

    Applicant: HOECHST AG

    Inventor： STEMMER DR HANS DIETER ,  SCHMIDT DIPL-CHEM ERICH ,  WINTER DR JAKOB ,  KUEHLKAMP DR ALFRED

    IPC: C08F8/30 ,  C08F255/00 ,  C08G18/62 ,  C08J5/06 ,  D06M15/227 ,  D06N7/06

    Abstract: Copolymers of ethene and propene and/or butene-1 are modified to render them capable of reacting with isocyanates either by heating them in an inert organic solvent, e.g. benzene, chlorobenzene or gasoline, with an organic peroxy compound, e.g. ditertiary butyl peroxide, dicumyl peroxide, dibenzoyl peroxide, tertiary butyl perbenzoate, cumyl hydroperoxide or tertiary butyl hydroperoxide, and acrylamide, methacrylamide or N-methylol acrylamide for 1-72 hours at a temperature above 50 DEG C. to produce a graft copolymer, or by heating them with an organic peroxy compound, preferably in the presence of an aldehyde, e.g. formaldehyde, in an inert organic solvent for 1-72 hours at a temperature above 50 DEG C.ALSO:Textile materials, e.g. fibres, cords and fabrics made from natural or regenerated cellulose, silk, wool, polyamides or polyesters, are treated with a di- or poly-isocyanate and with a copolymer of ethene and propene and or butene-1 which is modified to render it capable of reacting with an isocyanate, and are then vulcanized into a mixture containing an amorphous copolymer of ethene and propene and/or butene-1 as rubber constituent. Suitable modified copolymers are those prepared by heating a copolymer of ethene and propene and/or butene-1 in an inert organic solvent, e.g. benzene, chlorobenzene or gasoline, with an organic peroxy compound, e.g. a dialkyl peroxide such as ditertiary butyl peroxide and dicumyl peroxide, diacyl peroxide such as dibenzoyl peroxide, per acid ester such as tertiary butyl perbenzoate or hydroperoxide such as cumyl hydroperoxide or tertiary butyl hydroperoxide, and a compound containing in addition to a reactive double bond, other functional groups, e.g. OH-, NH=, NH2- or -NH-CH2OH groups or a further reactive carbon-carbon double bond, e.g. acrylamide, methacrylamide and N-methylol acrylamide, for 1-72 hours at temperatures above 50 DEG C. Alternatively modified copolymers prepared by heating copolymers of ethene and propene and/or butene-1 with an organic peroxy compound preferably in the presence of an aldehyde in an inert organic solvent for 1-72 hours at a temperature above 50 DEG C may be used. The textile materials may be dipped into a solution containing 0.5-10% by weight of the modified copolymer and 0.1-20% by weight of a di-or poly-isocyanate, e.g. methane-tri-(phenyl-isocyanate-4), 2, 4-toluylene diisocyanate, hexamethylene diisocyanate or naphthalene diisocyanate, in an organic solvent, e.g. aliphatic, cycloaliphatic and aromatic hydrocarbons and halogenated hydrocarbons, and then dried in dry air or under reduced pressure or the textile material may be dipped first into a solution containing 0.1-20% by weight of the di- or poly-isocyanate and then into a solution containing 0,5-10% by weight of the modified copolymer prior to drying. The treated textile materials may then be incorporated into mixtures containing amorphous copolymers of ethene and propene and/or butene-1 containing vulcanization agents, e.g. dicumyl peroxide, tertiary butyl cumyl peroxide, ditertiary butyl peroxide, 2, 5-dimethyl-2, 5-bis(tertiary butyl peroxy hexane, sulphur and/or unsaturated monomers such as maleic anhydride and divinyl adipate, rubber fillers, e.g. carbon black and silica, and plasticizers, e.g. paraffinic and naphthenic oils.

    15.
    发明专利
    未知

    公开(公告)号：DE1123110B

    公开(公告)日：1962-02-01

    申请号：DEF0032114

    申请日：1960-09-14

    Applicant: HOECHST AG

    Inventor： ZIMMERMANN DR JOHANN WOLFGANG ,  KUEHLKAMP DR ALFRED

    IPC: C08F2/22 ,  C08F2/32

    Abstract: Water-soluble bead polymers are produced by polymerization of one or more vinyl, acryl and/or methacryl monomers, (A) that are completely soluble in water alone or with one or more water-soluble monomers, (B) not polymerizable alone with free radical agents or with one or more sparingly water-soluble monomers, (C) the monomers are polymerized in the presence of a water-soluble free radical forming polymerization catalyst in an emulsion of which the aq. solution, e.g. 20-80%, of the monomer is the outer phase and an organic solvent which is immiscible or soluble in water at 50 DEG C. to an extent of not more than 15% is the inner phase, the ratio of the aqueous to organic phases being 1 : 0.5-10, the concentration of emulsifier being 0.01-5%, the polymerization temperature being from 20 DEG C. to the boiling point of the organic solvent or its azeotrope with water and the sparingly soluble monomers being present in a sufficiently small proportion to ensure that the polymer is soluble in water at up to at least 50 DEG C. Monomers (A) may be all ethylenically unsaturated water-soluble compounds which undergo radical initiated polymerization, e.g. methacrylamide, acrylamide; acrylic and methacrylic acids or ethene sulphonic acid or their alkali metal, e.g. Na, salts; an N-substituted acryl- or methacrylamide such as N-methacrylamide, or a sulphonated styrene. Monomers (B) may be maleic acid diamide or crotonic acid. Monomers (C) may be a vinyl ester of a saturated aliphatic monocarboxylic acid with C1- 4, e.g. vinyl acetate; an acrylic or methacrylic acid ester of a saturated aliphatic monohydric alcohol with C1- 4; acrylo- or methacrylonitrile. The catalyst may be 0.001-2% alkali, e.g. K, persulphates; alkyl hydroperoxides and/or H2O2 alone or as redox systems with e.g. alkali, e.g. Na, metabisulphites; Na formaldehyde-sulphoxylate; Na salt of ethylene diamine tetracetic acid. Irradiation may be used to activate the polymerization. The organic solvent may dissolve not more than 20 parts of monomer or 10 parts polymer/100 parts solvent and may be chlorinated hydrocarbons of b.p. below 100 DEG C. such as those with C1- 2, e.g. CCl4, C2H4Cl2, C2HCl3; aliphatic and cycloaliphatic hydrocarbons, e.g. gasoline fractions of b.p. below 100 DEG C. such as petroleum ether b.p. 80-90 DEG C.; hexane or cyclohexane; aromatic hydrocarbons, e.g. benzene, toluene or xylene; and/or esters, e.g. of saturated aliphatic monocarboxylic acids containing C1- 3 with aliphatic saturated monohydric alcohols with C1- 5. The emulsion may be formed by emulsifying the organic solvent with emulsifier, e.g. ethylene oxide condensates of phenol; nonyl phenols such as those with 13-23 mols. C2H4O; long chain monocarboxylic acids and fatty alcohols; fatty acid, e.g. lauric or oleic, esters of cyclic mono-anhydro-sorbitol; lauryl sulphate or sulphosuccinic acid ester. The emulsion may be formed in a stirrer vessel under an inert atmosphere, e.g. N2, and the monomer may be dissolved in the formed or pre-formed emulsion and the catalyst may be added to the emulsion or simultaneously with the emulsification, e.g. introducing the organic phase together with the aq. monomer containing the catalyst. A portion, e.g. one-fifth, of the emulsion may be heated while stirring and the remainder added after polymerization is complete. Polymerization may be continuous. The beads, e.g. 1/2 -1.5 mm., may be filtered and washed, e.g. using the organic solvent and e.g. hexane, and then dried, e.g. at 40-60 DEG C., in a vacuum, fluidized bed or roller drier.

    16.
    发明专利
    未知

    公开(公告)号：DE1084477B

    公开(公告)日：1960-06-30

    申请号：DEF0027294

    申请日：1958-12-18

    Applicant: HOECHST AG

    Inventor： STARCK DR WERNER ,  KAHRS DR KARL-HEINZ ,  KUEHLKAMP DR ALFRED ,  EHMANN DR WERNER

    IPC: C08F8/12

    Abstract: In a process for the manufacture of solid polyvinyl alcohol, a polyvinyl ester of a carboxylic acid having 1 to 10 carbon atoms is hydrolysed within the temperature range 10 DEG to 120 DEG C. with 0,01 to 10% by weight of the reaction mixture of a strong acid as catalyst and 0,5 to 15% by weight of the reaction mixture of water, the balance being a mixture of 1 to 50% by weight of said ester and 99 to 50% by weight of a water-miscible and acid-miscible solvent for the polyvinyl ester but non-solvent for the polyvinyl alcohol and, under the reaction conditions does not form an ester with the carboxylic acid radical of the polyvinyl ester, whereby polyvinyl alcohol is precipitated in powdery form and recovered from the reaction mixture. The polyvinyl ester may be polyvinyl acetate, propionate or formate. The solvent may be acetone, methyl ethyl ketone, diethyl ketone, t-butanol, methyl acetate or tetrahydrofuran and mixtures thereof with aromatic hydrocarbons. The acid may be hydrochloric, sulphuric, phosphoric, perchloric or a sulphonic acid. The hydrolysis may be interrupted to give partially hydrolysed products, or such products may be obtained by selection of appropriate reactants and conditions. Specification 818,294 is referred to.

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