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    112.
    发明专利
    未知

    公开(公告)号：DE1203467B

    公开(公告)日：1965-10-21

    申请号：DEB0070344

    申请日：1963-01-16

    Applicant: BASF AG

    Inventor： GEHM DR ROBERT ,  STEINBRUNN DR GUSTAV ,  JENTZSCH DR WOLFGANG ,  WILHELM DR HANS ,  BAYERLEIN DR FRIEDRICH ,  SCHICKH DR OTTO VON

    IPC: C08G69/20

    Abstract: In a process for the anionic polymerization of lactams having 5 to 14 ring members, the polymerization activator used is a compound of the general formula where n is 1 or 2, R1 and R2 are each monovalen hydrocarbon radicals having one to seven carbon atoms or R1 and R2 joined together form a divalent radical, R3 is hydrogen or a hydrocarbon radical having one to eight carbon atoms and R, when n is 1 is an alkyl amine, arylamino or aralkylamino radical having one to fourteen carbon atoms, and, when n is 2 is a divalent radical having the formula -NH-R3-NH- where R4 is a divalent hydrocarbon radical having two to fifteen carbon atoms. Specified lactams are pyrrolidone, piperidone, e -caprolactam, capryllactam, oenanthiclactam, capriclactam, laurolactam, e -ethyl-e -caprolactam, #x-ethyl-#x-oenantholactam and methylenebis-caprolactam. Fillers, e.g. glass fibres, asbestos, graphite, gypsum, chalk, molybdenum sulphide, wood flour and fibres may be incorporated into the polymerization mixture. In Examples (1) to (6), e -caprolactam is polymerized in the presence of sodium caprolactam and: (1) benzimidazole-1-carboxylic anilide; (2) imidazole-1-carboxylic acid N : N1-diphenyl amide; (3) benzimidazole-1-carboxylic acid (N1-methyl) anilide; (4) 2-methylimidazoline-N(1)-carboxylic acid N : N1-diphenyl amide; (5) N : N - hexamethylene - bis - (carbamyldimethyl formamidine) and (6) (a) hexamethylene - bis - (N1 - carbamyl - 2 - methylimidazoli (b) hexamethylene-bis-(N-carbamyltriphenyl formamidine). In Example (7) pyrrolidone is polymerized in the presence of sodium methylate and imidazole-1-carboxylic diphenylamide.

    115.
    发明专利
    未知

    公开(公告)号：DE1177340B

    公开(公告)日：1964-09-03

    申请号：DEB0068906

    申请日：1962-09-19

    Applicant: BASF AG

    Inventor： BAYERLEIN DR FRIEDRICH ,  WILHELM DR HANS

    IPC: C08G69/18 ,  C08J9/00

    Abstract: Expanded polyamides are produced by heating a mixture of (A) one or more lactams having seven to fourteen ring members, (B) one or more alkaline catalysts, (C) one or more activators and (D) agents which under the prevailing conditions of polymerization volatilize or decompose with the evolution of gas thereby causing the polymerization product to expand, in the absence of substances containing or forming hydroxyl groups to temperatures above the melting point of the lactam and not more than 200 DEG C. and polymerizing the melt with expansion in the presence of 0.05 to 5% by weight of calcined gypsum with reference to the total weight of the polyamide forming materials. Lactams which are suitable are those of omega-aminocarboxylic acids such as caprolactam, oenantholactam, capryllactam, caprilactam and laurolactam. C-substituted lactams, e.g. 4-isopropylcaprolactam and lactams having chain-branching or cross-linking effects, e.g. alkylene-bis lactams may also be used. Suitable alkaline catalysts are metals such as sodium, potassium and calcium or compounds of these metals such as potassamide, sodium alcoholates and sodium hydroxide, organometallic compounds and especially alkali lactamates. Specified activators are acyl-lactams, monoisocyanates, polyisocyanates, acid derivatives such as carboxylic acid halides, esters or anhydrides, but particularly substituted ureas, thioureas, guanidines and urethanes. Examples of these are hexamethylene-1,6-biscarbamidocapryllactam or phenylcarbamidocaprolactam. Suitable expanding agents are aliphatic and cycloaliphatic hydrocarbons such as hexane, octane and cyclohexane, aromatic hydrocarbons such as benzene and toluene and straight-chain and cyclic ethers such as dibutyl ether and dioxane. Liquids having low boiling points, e.g. pentane may be used under pressure. Solid compounds, such as azoisobutyronitrile, benzene sulphonic acid hydrazide and arylsulphazides may also be used. Dyes, fillers and stabilizers may also be incorporated in the mixture.

    118.
    发明专利
    未知

    公开(公告)号：DE1162509B

    公开(公告)日：1964-02-06

    申请号：DEB0064621

    申请日：1961-11-02

    Applicant: BASF AG

    Inventor： HAHN DR ERWIN ,  LANGE DR GUENTER ,  LINKE DR WOLFGANG ,  LOUIS DR GERD ,  WILHELM DR HANS ,  GULBINS DR KLAUS

    IPC: C08F2/44 ,  C08F8/30

    Abstract: Coloured hair lacquers or hair setting compositions containing a coloured macromolecular substance, are formed by chemically combining a dye with the macromolecular substance or by copolymerizing the dye with a colourless monomer. The dye may be combined with the polymer through the reactive groups by means of a condensation reaction. Suitable polymers are the copolymers of acrylamide or methacrylamide with acrylic acid esters, methacrylic acid esters, vinyl esters, vinyl lactams and if desired small amounts of unsaturated carboxylic acids. Dyes suitable for this purpose are those of the azo or anthraquinone series containing N-methylol groups as reactive groups. Dyes which can be used for copolymerization are those of the azo or anthraquinone series containing in the molecule a polymerizable olefinically unsaturated group outside the chromophoric system. Suitable monomers for copolymerizing with these dyes are acrylamide, methacrylamide, a low molecular weight acrylic esters or methacrylic ester, vinylacetate, vinyl-propionate and/or a vinyl-lactam. Specification 877,402 is referred to.ALSO:Coloured hair or hair setting compositions containing a coloured macromolecular substance are formed by chemically combining a dye with the macromolecular substance or by copolymerizing the dye with a colourless monomer. The dye may be combined with the polymer through the reactive groups by means of a condensation reactive. suitable dyes are those of the azo or anthraquinone series containing N-methylol groups e.g. the coupling product of diazotized N-(p-aminophenyl)-glyoxal-diureine and 1-(p-sulfophenyl)-3-methyl pyrazoline-(5) which has been reacted with formaldehyde, the coupling product of diazotized N-(p-amino phenyl)-glyoxal-diureine and N-acetyl aminonaphthol-(1-3, 6, disulfonic acid which has been reacted with formaldehyde; the coupling product of diazotized N-p-amino phenyl urea and 4-tertiary-butyl phenol which has been reacted with formaldehyde; and 4-azophenyl acetoacetic acid anilide. Suitable dyes for copolymerization are anilide. Suitable dyes for copolymerization are those of the azo or anthraquinone series containing in the molecule a polymerizable olefinically unsaturated group outside the chromophoric system e.g. the coupling products of 1-amino-3-acryloyl aminobenzene with 1-[N-(2-hydroxyethyl)-N-(2-cyanoethyl)-amino]-3-methylbenzene, of 1-amino-4-acryloyl aminobenzene with 1-hydroxynaphthalene-4-sulfonic acid, or 2, 4-dichloroaniline with N-ethyl-N-b -vinyl oxyethylaniline, of p-aminostyrene with 1-hydroxynaphthalene-4-sulfonic acid and 1-amino 2-acetyl-4-acryloyl-aminoanthraquinone. Specification 877,402 is referred to.

    119.
    发明专利
    未知

    公开(公告)号：DE1162069B

    公开(公告)日：1964-01-30

    申请号：DEB0065327

    申请日：1961-12-23

    Applicant: BASF AG

    Inventor： DAUMILLER DR GUENTHER ,  WILHELM DR HANS ,  WEGNER DR EBERHARD ,  GEHM DR ROBERT

    IPC: C08F8/30 ,  C08G18/62 ,  C08J9/02

    Abstract: An expanded plastic is produced by reacting at least one polyisocyanate and water, with a copolymer derived from (a) at least one olefinically unsaturated polymerizable monomer containing at least one tertiary nitrogen atom and at least one group which will react with isocyanate, the proportion of this monomer being at least 0.25% by weight of the copolymer and (b) at least one other olefinically unsaturated polymerizable monomer. Copolymer formation may be carried out in bulk, solution, emulsion or suspension, between 0 and 300 DEG C., using as catalysts: peroxides, e.g. benzoyl and cyclohexanone peroxides, hydroperoxides, e.g. tert.-butyl hydroperoxide, azo compounds, e.g. azodiisobutyronitrile or redox systems. The copolymer should have a K value of 15-50, and an OH number of less than 125 for soft foams and 125-300 for rigid foams. The foaming reaction is carried out at 0-100 DEG C. 1-1.5 moles of isocyanate per mole of isocyanate reactive groups and 1 mole of water per mole of unreacted isocyanate group are required. Stabilizers and plasticizers may be added, e.g. silicones, tin octoate, dibutyltin diethyl hexoate or metal chelates. Isocyanate reactive groups specified are hydroxyl, carboxyl, carbonamide, thiocarbonyl, thioamide, sulphhydryl, primary and secondary amino and active hydrogen attached to carbon. Compounds of type (a) specified are heterocycles with at least one tertiary nitrogen atom in the ring system; e.g. hydroxy and hydroxyalkyl, vinyl and allyl derivatives of a pyridine, quinoline, isoquinoline, acridine, pyrimidine, indazole, imidazole, pyrazole, triazole, benzoxazole and oxazole such as 5-hydroxymethyl-2-vinyl-pyridine, hydroxymethylvinyl-benzoxazole, N-vinyl-2-methylol-imidazole and N-vinyl-2-hydroxyethyl-imidazole and compounds of the formula: where X=NH or O; R1=H, alkyl, hydroxyalkyl or halogen; R2= -CH2-, -C2H4- or -C4H8- optionally branched or hydroxylated and R3 and R4 may be alkyl, aryl or aralkyl optionally branched or hydroxylated, at least one of R2, R3 or R4 containing a hydroxyl group, preferably b to the nitrogen atom, e.g. di-(b -hydroxyethyl)-aminomethylene methacylamide and substituted amides and esters of maleic, fumaric, and itaconic acids. Compounds of type (b) may or may not contain tertiary nitrogen atoms or isocyanate reactive groups. Specified compounds include: acrylic esters, methacrylic esters, maleic esters, fumaric esters, itaconic esters, vinyl esters, vinyl halides, vinylidine halides, vinyl aromatic hydrocarbons, halostyrenes, N-substituted amides, acrylonitrile, N-vinyl lactams, N-vinyl pyridine, vinyl ethers, dienes and allyl compounds. The esters may be wholly or partly saponified. Several polyisocyanates are specified. In examples copolymer formation is carried out under N2 in the presence of tertiary dodecyl mercaptan and azodiisobutyronitrile and in Examples (1-3 and 5) using CH2Cl2 as solvent. Monomers of type (a) are N-vinyl-2 methylol-imidazole (1, 2 and 4-8), diethanolaminomethylene methacrylate (3) and N-vinyl-2-hydroxyethyl-imidazole (9). Monomers of type (b) are n-butyl acrylate (2 and 6-9), isobutyl acrylate (1 and 3-5), butane-1, 4-diol monoacrylate (4, 5 and 8), propylene glycol monoacrylate (6) and ethylene glycol monoacrylate (7). Butane-1, 4-diol is used in Example (5). Foaming is by adding tolylene diisocyanate, silicone oil, water and the sodium salt of a sulphonated sperm oil/ethylene oxide adduct.

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