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    Production of chloralkyl esters of acrylic acid and substitution products thereof
    21.
    发明专利
    Production of chloralkyl esters of acrylic acid and substitution products thereof 未知

    公开(公告)号：GB886649A

    公开(公告)日：1962-01-10

    申请号：GB728559

    申请日：1959-03-03

    Applicant: BASF AG

    Inventor： BARON HUBERTUS ,  FRIEDERICH HERBERT

    IPC: C07C67/26 ,  C08F20/22 ,  C08F20/28

    Abstract: The invention comprises acrylic acid-1-chlor-3-ethoxypropyl ester-(2), and acrylic acid-1-chlorpropylester-(2). Chloralkyl esters of acrylic acid which may be substituted in the alpha-position by halogen or in alpha or beta-position by a methyl radical are made by reacting an acrylic acid chloride which may be substituted in the alpha-position by halogen or in alpha or beta-position by a methyl radical with an epoxide, preferably in the presence of an acid-reacting catalyst such as Friedel-Crafts catalysts. Suitable epoxides are epichlorhydrin, alkylene oxides of 2 to 3 carbon atoms, styrene oxide, alkyl or aryl glycidol ethers, and glycidol esters. In general, the reaction is effected in the temperature range between 20 DEG C. and 150 DEG C. Solvents such as chlorinated hydrocarbons or benzene may be used if desired. It is preferred to discontinue reaction at 50% to 70% conversion to avoid polymerization. The products may be purified by distillation under reduced pressure and stabilized with phenothiazine or hydroquinone.

    Copolymers and their production
    24.
    发明专利
    Copolymers and their production 未知

    公开(公告)号：GB857261A

    公开(公告)日：1960-12-29

    申请号：GB3379059

    申请日：1959-10-06

    Applicant: BASF AG

    Inventor： WILLERSINN HERBERT ,  KLAUS GERHARD DIETRICH ,  FUST JUERGEN ,  FRIEDERICH HERBERT ,  SIEBEL HANS PETER

    IPC: C08F36/04 ,  C08F36/16

    Abstract: Copolymers are produced by the polymerization of a mixture comprising (A) 5 to 75 parts of 5, 6-bismethylene-1, 2, 3, 4, 7, 7-hexachlorbicyclo-(2, 2, 1)-heptene-2 of formula: (B) 10-80 parts of styrene and/or styrene derivatives and (C) 0-70 parts of an unsaturated polyester of an alpha-olefinic dicarboxylic acid and a polyhydric alcohol, the total of A, B and C amounts to 100 parts. Specified styrene derivatives are alpha-methyl styrene, alpha-chlorstyrene alpha-bromostyrene, methyl styrene, dimethyl styrene, chlorostyrene, dichlorostyrene and dibromostyrene. Specified dicarboxylic acids are maleic, fumaric, itaconic, citraconic, aconitic, chlormaleic acids and anhydrides; these may be partially replaced by succinic, glutaric, adipic, pimelic, sebasic, suberic, alpha-methyl glutaric, oxadibutyric, sulphone-dibutyric, phthalic, endomethylene or hexachloroendo-methylene, tetrahydrophthalic acid, tetrachloro-phthalic, tetrabromophthalic and phenylene-butyric acid or anhydrides. Propylene glycol is the specified alcohol. Specified polymerization catalysts are benzoyl, lauroyl, ditertiary butyl, cyclohexanone, or methyl ethyl ketone, peroxides, perlauric acid, cumne hydroperoxide, tertiary butyl hydroperoxide azodi-isobutyro-dinitrile, hydrogen peroxide or potassium persulphate together with light. Redox systems using the above catalysts together with reducing agents, e.g. benzoin, sodium formaldehyde sulphoxylate, and sugar may be used. The polymerization may take place under bulk, solution or emulsion conditions. Stabilizers such as p-tertiary-butylcatechol, and hydroquinone, as well as cobalt octoate, cobalt naphthenate, dibutyl phthalate and polyvinylpyrrolidone may also be present.ALSO:5, 6-bismethylene-1, 2, 3, 4, 7, 7-hexachlorbicycle-(2, 2, 1)-heptene-(2) of the formula: is prepared by reacting 1, 4-dichlorbutene-2 with hexachlorcyclopentadiene by a Diels-Alder reaction to form 5, 6-bichlormethyl-1, 2, 3, 4, 7, 7-hexachlorbicyclo -(2, 2, 1)- heptane-2 and then splitting off hydrogen chloride using a sodium methylate.

    Improvements in the production of hydrochlorides of basic carbamic acid esters
    26.
    发明专利
    Improvements in the production of hydrochlorides of basic carbamic acid esters 未知

    公开(公告)号：GB848737A

    公开(公告)日：1960-09-21

    申请号：GB1945358

    申请日：1958-06-18

    Applicant: BASF AG

    Inventor： FRIEDERICH HERBERT ,  BINDIG JOHANNA

    IPC: C07D279/30

    Abstract: Carbamic acid ester hydrochlorides of the formula: where R3 is a straight- or branched-chain alkylene group of 2 or more carbon atoms, and R1 and R2 are the same or different aliphatic radicals, or where two of the three R groups form a heterocyclic system with the N atom, R4 and R5 are the same or different aromatic rings or heterocyclic rings with aromatic character which may be joined to each other, in addition to through the nitrogens, either directly or through carbon or hetero atoms, are prepared by reacting with the hydrochloride of a chloroformic acid ester of an animoalcohol of formula: The reaction may be effected in the presence of an halohydrocarbon solvent, a Friedel-Crafts catalyst of the metallic halide type, hydrogen chloride, carbon monoxide and/or carbon dioxide. The aromatic rings R4 and R5 may be substituted, e.g. by one or more alkyl, alkoxy, hydroxyalkyl or halogen groups. Specified amines are phenthiazine and its 2-chloro-, 3-chloro-, 2-methoxy-, 3-methoxy-, 2-acetyl-and 3-acetyl derivatives, 2, 4-dichloro- and 2, 4-diethoxy1, 3-diazaphenthiazine, 1-azaphenthiazine, phenoxazine, acridane, acridone, 2,21-iminodibenzyl, dihydrophenazine, diphenylamine, phenyl-naphthylamine, dinaphthylamine and phenyl-2-pyridylamine. Specified aminoalcohols are dimethyl-, diethyl-, dipropyl-, dibutyl-, and methylethylaminoethanol, dimethyl- and diethyl-aminopropanol-1, 3, 1-dimethylamino-2-hydroxypropane, N-(b -hydroxyethyl)-pyrolidine, N-ethyl-3-hydroxypyrrolidine, N, N1-di-(b -hydroxyethyl)-piperazine and N,N1-(g -hydroxypropyl-b -hydroxyethyl)-piperazine; when several hydroxy groups are present, those which are to be free in the product can be protected in known manner. The hydrochlorides of the chloroformic acid esters of the aminoalcohols may be prepared by dissolving the aminoalcohol in a solvent, reacting with, e.g. hydrogen halides, trichloracetic acid or sulphonic acids, converting the salt into the chloroformic acid ester hydrochloride with phosgene in the cold, and removing the excess of phosgene and the solvent. Specifications 708,896, 808,050 and 817,558 are referred to.

    Expandable plastic compositions for the production of foam plastics
    29.
    发明专利
    Expandable plastic compositions for the production of foam plastics 未知

    公开(公告)号：GB1015709A

    公开(公告)日：1966-01-05

    申请号：GB3905862

    申请日：1962-10-16

    Applicant: BASF AG

    Inventor： STAHNECKER ERHARD ,  MUELLER-TAMM HEINZ ,  FRIEDERICH HERBERT

    IPC: C08F8/04 ,  C08J9/14

    Abstract: Expandable plastic compositions for the production of foam plastics comprise a vinyl cyclohexane polymer, the molecular weight of which is more than 10,000, preferably 50,000 to 1,000,000, which has been obtained by hydrogenation (and preferably perhydrogenation) of a styrene polymer, or copolymer containing at least 50% by weight of styrene in polymerized form, and which contains at least 20% by weight of cyclohexyl radicals, and 2 to 20%, preferably 5 to 10%, by weight, with reference to the vinyl cyclohexane polymer, of an organic compound whose boiling point is lower than the softening point of the polymer and which does not dissolve the polymer, as an expanding agent. The foam plastic is obtained by heating the expandable plastic composition above its softening point. Suitable vinylcyclohexane polymers are those which have been obtained by hydrogenation of polystyrene, and copolymers of styrene containing at least 50% by weight of styrene, and up to 50% by weight of a -methyl styrene or nuclear-substituted methylstyrene, in polymerized form. The styrene polymers may also contain up to 5% by weight of other monomers, e.g. acrylonitrile, esters of acrylic and methacrylic acid with alcohols having one to eight carbon atoms or vinyl carbazole, in polymerized form. In perhydrogenated styrene polymers and copolymers, all the phenyl radicals have been converted into cyclohexyl radicals. Hydrogenation of the styrene polymers may be carried out in liquid phase with hydrogen in the presence of catalysts. The polymers may be hydrogenated in molten condition or dissolved in inert organic solvents, e.g. a mixture of cyclohexane and tetrahydrofuran. Hydrogen pressures of more than 170 atmospheres may be used. Suitable catalysts are nickel, cobalt or the metals of the platinum group, in finely powdered or colloidally dispersed distribution, and they may be supported on porous substances, e.g. carbon, aluminium oxide, pumice or di-atomaceous earth. Suitable expanding agents are volatile hydrocarbons, e.g. propane, butane, pentane, hexane, cyclopentane or cyclohexane; volatile halo-hydrocarbons, e.g. methylene chloride or dichlorodifluoro methane; or volatile or alkyl ethers, e.g. dimethyl ether. Homogeneous mixtures of the vinylcyclohexane polymers and expanding agents may be obtained by various means, e.g. mechanical mixing, adding expanding agent to a solution of the plastic and removing the solvent, suspending the polymer in finely divided form in water, and treated with expanding agent under pressure while stirring or by pouring solutions of the polymer and expanding agent into water containing a suspension agent while stirring, and removing the solvent while continuing the stirring. Foamed mouldings from the finely divided plastic compositions containing expanding agent may be prepared in one operation, by expanding and sintering the particles by heating them in moulds, e.g. with superheated steam, infra-red radiation or in a high frequency field, which are not gas-tight when closed. Extrusion techniques may also be employed to prepare foamed shapes continuously. The foams have high thermal stability under load, good mechanical strength and a low bulk density. They absorb practically no water owing to their closed cell structure.

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