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    Production of polyamide moldings
    41.
    发明专利
    Production of polyamide moldings 未知

    公开(公告)号：GB1116068A

    公开(公告)日：1968-06-06

    申请号：GB4272265

    申请日：1965-10-08

    Applicant: BASF AG

    Inventor： DACHS KARL ,  WILHELM HANS

    IPC: B29C39/00 ,  B29C41/00 ,  B29C41/04 ,  C08G69/18 ,  C08J9/04

    Abstract: A polyamide is produced by subjecting a lactam to activated anionic polymerization in a mould in the presence of an epoxide. Suitable epoxides are e.g. butylene-1:2-oxide, butadiene monoxide, cyclooctene oxide and phenyldeca-triene-1:4:8-monoxide, and they may contain neutral-reacting groups, e.g. -CN, -CO.O-, phenoxy, ether, thio-ether and amino groups and dibutylamino- or butylthio-groups. Particularly suitable are compounds having 2-6 epoxy groups, e.g. wherein R is a C2- 14 hydrocarbon group, wherein R is a hydrocarbon group and R1 is an aliphati C1- 6 hydrocarbon group, wherein R is a hydrocarbon group and wherein R is a hydrocarbon group. They are used in amounts of 0.05-30 wt. per cent of the lactam. Polyepoxide precondensates still containing epoxy groups are also suitable. Suitable lactams are caprolactam, enantholactam, capryllactam, capric lactam, laurolactam and C-substituted derivatives of these, e.g. 3-methylcaprolactam and 4-isopropylcaprolactam. Suitable anionic catalysts are alkali and alkaline earth metals, hydrides and hydroxides of these, sodium or potassium alcoholates, and Grignard compounds, and also alkali or alkaline earth metal derivatives of lactams. Amounts of 0.01-5% of the weight of lactam may be used of these. Suitable activators are organic acid halides, anhydrides, esters, and nitriles and also isocyanates and carbodiimides and urea derivatives, e.g. pyrrolidone-N-(carboxylic acid)-hexamethylene diamide-1:6 and triphenylmethane-4:41:411 - triscarbamidocaprolactam, and N-substituted carbamic esters and bisisoalkyl-urethanes. These may amount to 0.05-10 wt. per cent of the lactam. Conventional additives may be present, and expanding agents, e.g. cyclohexane, gasoline or gas-forming compounds, if it is desired to prepare a foam. In the example e -caprolactam is polymerized in the presence of Na-e -caprolactam, pentaery-thritol triglycidyl ether, CaSO4. 1/2 H2O and a petroleum ether/gasoline mixture. The mould is preferably heated to 80-200 DEG C. before addition of the lactam melt.

    Manufacture of expanded polyamides
    44.
    发明专利
    Manufacture of expanded polyamides 未知

    公开(公告)号：GB918059A

    公开(公告)日：1963-02-13

    申请号：GB3437761

    申请日：1961-09-26

    Applicant: BASF AG

    Inventor： BRUEGGEMANN HORST ,  DACHS KARL ,  SCHWARTZ ERICH ,  WILHELM HANS

    IPC: C08G69/18 ,  C08J9/04

    Abstract: Expanded polyamides are produced by polymerizing a lactam with at least 7 ring members, at temperatures above its melting point and below the melting point of the resultant polyamide, with the aid of an alkaline catalyst in the absence of substances containing or forming hydroxyl groups and in the presence of expanding agents which, under the polymerization conditions, volatilize or decompose with the evolution of gas. A polymerization activator may also be present in the reaction mixture. Specified are lactams caprolactam, oenanthic lactam, caprylic lactam, lauric lactam and 4-isopropylcaprolactam and mixtures polymerization catalysts alkali and alkaline earth metals and alkaline-reacting compounds of these metals, e.g. alkali-lactam compounds, potassium hydroxide, potassium carbonate, sodium methylate, sodium amide and calcium oxide and polymerization activators carboxylic acid halides such as benzoyl chloride, esters and anhydrides, isocyanuric and isothiocyanuric acid esters, cyanamides, carbodi-imides and especially substituted ureas, thioureas, guanidines and urethanes. Additives such as kieselguhr and animal charcoal promote the formation of homogeneous, fine cells. In most of the examples the polymerization activator used is bis-(caprylic lactam-N-carboxylic acid)-hexamethylene diamide.ALSO:Expanded polyamides are produced by polymerizing a lactam with at least 7 ring members, at temperatures above its melting point and below the melting point of the resultant polyamide, with the aid of an alkaline catalyst in the absence of substances containing or forming hydroxyl groups and in the presence of expanding agents which, under the polymerization conditions, volatilise or decompose with the evolution of gas. A polymerization activator may also be present in the reaction mixture. Specified are lactams caprolactam, oenanthic lactam, caprylic lactam; lauric lactam and 4- isopropylcaprolactam and mixtures polymerisation catalysts alkali and alkaline earth metals and alkaline-reacting compounds of these metals, e.g. alkalilactam compounds, potassium hydroxide, potassium carbonate, sodium methylate, sodium amide and calcium oxide and polymerization activators carboxylic acid halides such as benzoyl chloride, esters and anhydrides, isocyanuric and isothiocyanuric acid esters, cyanamides, carbodi-imides and especially substituted ureas, thioureas, guanidines and urethanes. Additives such as kieselguhr and animal charcoal promote the formation of homogeneous fine cells. In most of the examples, the polymerisation activator used is bis- (caprylic lcotam - N - carboxylic acid)-hexamethylene diamide. Specified expanding agents are pentane, hexane, heptane, octane, cyclohexane, benzene, toluene, dibutyl ether, dioxene, azoisobutyronitrile, benzene sulphonic acid hydrazide and aryl sulphazides and mixtures. The polymerization/expansion may be in a mould, or partial polymerization may be allowed to proceed in an extruder followed by extrusion of the viscous expandable melt through a die into a heated medium to complete the polymerization and effect the expansion.

    Process for cementing materials or articles
    45.
    发明专利
    Process for cementing materials or articles 未知

    公开(公告)号：GB900152A

    公开(公告)日：1962-07-04

    申请号：GB3325460

    申请日：1960-09-28

    Applicant: BASF AG

    Inventor： BRUEGGEMANN HORST ,  DACHS KARL ,  SCHWARTZ ERICH ,  WILHELM HANS

    IPC: B32B27/00 ,  C08G69/18

    Abstract: Polyamides used as cements are formed in situ by the alkaline polymerization of single or mixed lactams at temperatures up to 280 DEG C. The preferred lactams are caproic, caprylic, oenanthic, or lauric, the first two being used singly or mixed together in various proportions and the two latter being used in mixtures as minor constituents. Known alkali carriers and activators are included in the compositions and lists of these are given. Cross-linking agents, e.g. methylene-bis-caprolactam, may also be included. Polymerization, with or without heating, may be controlled by applying the lactam melts in two parts, containing the alkali carrier and the activator respectively, or by applying the activator separately in solution. Specifications 900,150 and 900,151 are referred to.

    A process for the alkaline polymerisation of lactams
    46.
    发明专利
    A process for the alkaline polymerisation of lactams 未知

    公开(公告)号：GB900150A

    公开(公告)日：1962-07-04

    申请号：GB2422060

    申请日：1960-07-12

    Applicant: BASF AG

    Inventor： DACHS KARL ,  BRUEGGEMANN HORST ,  BOECK EDMUND

    IPC: C08G69/20

    Abstract: A process for the polymerization of lactams having from 4 to 12 ring carbon atoms in the presence of an alkaline polymerization initiator and a polymerization activator comprises using as the activator a substituted urea, thiourea or guanidine, which is capable of being dissolved undecomposed in the lactams at the polymerization temperature, having the general formula where R1, R2 and R3 are hydrogen atoms or monovalent hydrocarbon radicals having from 1 to 20 carbon atoms, or R1 and R2 together represent a divalent aryl radical of the general formula -CH-(CH2)n-CO- where n is an integer from 3 to 11, and in which said radicals R1, R2 and R3 may be substituted by fluorine or ether groups, X is oxygen, sulphur or the radical > N-R5 where R5 is a hydrogen atom or a monovalent hydrocarbon radical having from 1 to 20 carbon atoms, and R4 is a monovalent hydrocarbon radical with from 1 to 20 carbon atoms or one of the radicals and wherein Y represents a divalent and Z a trivalent hydrocarbon radical with from 1 to 20 carbon atoms which may be substituted by fluorine or ether groups and X, R1, R2 and R3 have the same meanings as given above. A large number of activators is specified. Specified lactams are pyrrolidone, piperidone, S -caprolactam, oenanthic lactam, caprylic lactam and lauric lactam. Specified initiators are the alkali and alkaline earth metals and alkaline reacting compounds thereof. The examples describe the polymerization of caprylic lactam, S -caprolactam, lauric lactam and a -pyrrolidone in the presence of as activators 1,6-bis(N1-butylureids)hexane, 1,3-bis(N1-butylureids)benzene, 1,6-bis(caprolactam-N-carbamido)hexane, 1,6-bis(caprylic lactam-N-carbamido)-hexane, 1,6-bis(pyrrolidone-N-carbamido)-hexane, pyrrolidone N-carbonic acid anilide, 1,5-bis(caprolactam-N-carbamido)-naphthalene, N-phenyl-N1-butyl urea, N-phenyl-N1-stearyl urea, N-phenyl-N1-a -naphthyl urea, N-phenyl-N1-butyl thiourea, N-phenyl-N1-a -naphthyl thiourea, N-p-fluorphenyl-N1-phenyl urea, N-p-ethoxyphenyl-N1-phenyl urea, N-p-fluorphenyl-N1-p-methoxyphenyl urea, N,N1,N11-tricyclohexyl guanidine, morpholine-N-thiocarbonic acid anilide, 1,3-bis(N1-phenylthioureido)-4-methylbenzene, 1,3-bis-(N1-phenylureido)-4-methylbenzene, 1,3-bis-(N1,N11 - dicyclohexylguanido) - 4 - methylbenzene, 4,41-bis-(N1-phenylureido)-dicyclohexylmethane, 4,41-bis-(N1-phenylthioureido)-dicyclohexylmethane, 4,41-bis-(N1-phenylureido)-diphenyl ether, 4,41-bis-(N1-phenylureido)-diphenyl sulphone, 1,10-bis-(N1-phenylureido)-2-n-nonyldecane, 1,11-bis-(N1-phenylthioureido)-2-n-octylundecane, 4,41,411-tris-(N1-phenylureido) -tricyclohexylmethane, 4,41,411-tris-(N1-phenylthioureido) - 3,31 - dimethoxy - triphenylmethane, 3,31,311-tris-(N1-p-fluorphenylureido) -tri-n-propylamine, 3,31,311-tris-(N1-p-methoxyphenylureido) -tri-n-propylamine, pyrrolidone-N-carbonic acid anilide, pyrrolidone-N-carbonic acid p-fluoranilide, pyrrolidone-N-carbonic acid p-ethoxyanilide, caprylic lactam-N-carbonic acid stearylamine, 1,3-bis-(pyrrolidone-N-carbamido)-4-methylbenzene, 1,3-bis-(lauroylic lactam-N-carbamido)-4-methylbenzene, 1,5-bis-(pyrrolidone-N-carbamido)-naphthalene, 1,10-bis-(caprylic lactam-N-carbamido)-2-n-nonyl-decane, caprylic lactam-N-carbonic acid-N1,N11-dicyclohexylamidine, 4,41,411-tris-(caprylic lactam-N-carbamido)-triphenyl methane, 4,41,411-tris-(caprolactam-N-carbamido)-triphenyl methane, 6,61,611-tris-(caprylic lactam-N-carbamido)-tri-n-hexylamine and 2,4,41-tris-(caprylic lactam-N-carbamido)-biphenyl.

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