Basf Aktiengesellschaft

Eduard Heil

Adolf Echte

Juergen Hambrecht

Hermann Fischer

Herbert Naarmann

Johann Swoboda

Rudi W Reffert

Peter Siebel

Hermann Dreher

Albert Nikles

Hermann Gausepohl

Gunter Pipper

Claus Cordes

Rainer Theysohn

Franz Schmidt

Hugo Strehler

Paul Matthies

Klaus Hinselmann

Hermann Brandt

Richard Thoma

Ludwig Beer

Helmut Doerfel

Friedrich Urbanek

Siegfried Riegger

Gerd Schwoebel

Rosemarie Berger

Friedrich Mertes

Polyphenylene ethers are prepared from monohydric phenols, which possess alkyl substituents in the two ortho-positions and, if desired, in the meta-position, but not in the para-position, by an oxidative coupling reaction with oxygen at from 15.degree. to 50.degree. C. and under from 1 to 10 bar in the presence of a catalyst complex, of a solvent and, if required, of an activator, by a method in which the conversion of the phenols is carried out in two more reaction zones, in which some or all of the solvent, the catalyst complex and the phenols and, where relevant, the activator is initially taken and is circulated by means of a conveying unit, and about 60-100% of the stoichiometric amount of oxygen required for the oxidative coupling is introduced into the first reaction zone and from 0 to about 40% of the said stoichiometric amount is introduced into the second reaction zone.

Preparation of polyphenylene ethers, and an apparatus for this purpose

The catalyst is removed in the preparation of high molecular weight polyphenylene ethers from monohydric phenols, which are alkyl-substituted at the two ortho-positions but not at the para-position and may or may not be alkyl-substituted at the meta-position, by an oxidative coupling reaction with oxygen at from 15.degree. to 50.degree. C. in the presence of a catalyst complex obtained from a copper salt and an organic amine, in the presence of from 1 to 20 parts by weight of a solvent per part by weight of the monomeric phenol, and in the presence or absence of an activator, and removal of the metal component of the catalyst from the polyphenylene ether solution with a complex-forming or chelate-forming compound in aqueous solution, in the presence or absence of reducing and stabilizing substances and assistants for accelerating the interphase reactions and for phase separation, by a method in which the continuous removal of the copper catalyst is carried out in one or more mixer-settler stages at a phase volume ratio of the organic phase to the aqueous phase of from 1:0.1 to 1:1.0, preferably from 1:0.4 to 1:0.6.

Continuous removal of the catalyst from polyphenylene ethers

Nylons are prepared by a continuous process in which, in a precondensation zone, an aqueous solution of a salt of a dicarboxylic acid of 6 to 18 carbon atoms and a diamine of 6 to 18 carbon atoms is heated to 250.degree.-300.degree. C. under superatmospheric pressure, with simultaneous vaporization of water and formation of a prepolymer, the prepolymer and the vapor are separated, and the former is fed into a polycondensation zone and condensed under superatmospheric pressure of from 1 to 10 bar and at from 250.degree. to 300.degree. C., wherein the aqueous salt solution is condensed under superatomspheric pressure of from 1 to 10 bar in the first third of the tubular precondensation zone provided with baffles, until the degree of conversion is not less than 93%, and the prepolymer and the vapor phase are brought into intimate contact with one another in the remaining two thirds of the precondensation zone.

Continuous preparation of nylon from aqueous salt solution in

Molding materials containing high molecular weight polyphenylene ethers are produced by a process in which a solution of a polyphenylene ether in an organic solvent, together with another polymer, is freed of solvent by multi-stage evaporation. The solvent is preferably an aromatic compound from the class comprising the hydrocarbons, halohydrocarbons, ethers or esters, the ratio of the other polymer to the polyphenylene ether is advantageously from 99:1 to 20:80 parts by weight, the other polymer is, in particular, a homopolymer or copolymer of styrene or of a homolog thereof, which may be modified with rubber, and the multi-stage evaporation process preferably comprises not less than two and not more than four working up stages. The evaporation is carried out in general at from 120.degree. to 280.degree. C. and under a pressure of from 1 to 3,000 mbar, advantageously in the presence of assistants which reduce the partial pressure, eg. water and/or methanol.

Production of molding materials containing polyphenylene ethers

An improved process for the continuous manufacture of polyamides by continuously conveying the aqueous solution of a salt of essentially equivalent amounts of a diamine, or of a mixture of several diamines, and of a dicarboxylic acid, or of a mixture of several dicarboxylic acids, or of mixtures of such salts with lactams and/or aminocarboxylic acids, through several reaction zones under polyamide-forming conditions, wherein the mixture of starting materials is heated, in a first reaction zone, to from 200.degree. to 300.degree. C, preferably from 220.degree. to 280.degree. C, at pressures which are above the corresponding saturation vapor pressure of water and prevent the formation of a vapor phase, the pressure action on the polycondensation mixture is released in a second reaction zone and condensation of the mixture, to form high molecular weight polyamides, is then completed in further reaction stages. According to the invention,

Continuous manufacture of polyamides

A process for the continuous manufacture of linear, high molecular weight, polybutylene terephthalates, in which dimethyl terephthalate is trans-esterified with 1,4-butanediol, if desired in the presence of up to 40 mole% of other starting materials which form linear polyesters, in the molar ratio of from 1:1.2 to 1:1.5, in a plurality of successive stages at temperatures rising from 160.degree. to 230.degree. C, the mixture thus obtained is passed, at from 230.degree. to 270.degree. C and from 2 mm Hg to 20 mm Hg, upward through a bundle of stationary heated tubes, and immediately thereafter through a hold tank, with the proviso that the volume of the hold tank is at least 1/4 and at most 2.5 times the volume of the tube bundle and the mean residence time in the tube bundle and hold tank together is from 10 to 60 minutes, and the precondensate thus obtained is polycondensed at from 240.degree. to 260.degree. C and from 0.1 to 2 mm Hg. with continuous formation of thin films. The polybutylene terephthalates manufactured by the above process may be used for the manufacture of products such as fibers, films, sheeting and injection moldings.

Continuous manufacture of polybutylene terephthalates

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Limburgerhof, Germany

Eduard Heil