Basf Aktiengesellschaft

Rudi W Reffert

Adolf Echte

Juergen Hambrecht

Johann Swoboda

Johann Zizlsperger

Hans Wild

Gunter Thielen

Eduard Heil

Hermann Dreher

Peter Fink

Herbert Naarmann

Volker Muench

Rudolf H Jung

Hans H Schuster

Klaus Hinselmann

Peter Siebel

Albert Nikles

Ernst Tetzlaff

Guenter Jeckel

Peter Minges

Rosemarie Berger

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

High molecular weight polyphenylene ethers are prepared from a monohydric phenol by an oxidative coupling reaction with oxygen in the presence of a catalyst complex obtained from a copper salt and an organic amine, and in the presence of a solvent, by a process in which the metal component of the catalyst is removed after the polymerization by adding one or more organic ammonium salts of the general formula ##STR1## where A.sup..crclbar. is an anion or polyanion of an organic carboxylic, sulfonic or phosphonic acid, R.sup.1 is hydrogen, R.sup.2 and R.sup.3 are each hydrogen, alkyl of 1 to 18 carbon atoms or aryl and R.sup.4 is alkyl of 1 to 18 carbon atoms or aryl.

Removal of the catalyst from polyphenylene ethers

(Co)polymers which are composed of one or more monomers from the group comprising

Treatment of (Co)polymers to remove residual monomers

A process for the preparation of high molecular weight polyphenylene ethers from alkyl-substituted monohydric phenols by an oxidative coupling reaction with oxygen in the presence of a catalyst complex of a copper salt and an organic amine, subsequent stopping of the reaction and removal of the metal component of the catalyst by addition of chelating and/or salt-forming agents, wherein the polymer solution is treated with a compound having the general structure: ##STR1## where R.sup.2 and R.sup.3 can be identical or different and each is OH, NH.sub.2, NHR.sup.5, where R.sup.5 is alkyl or cycloalkyl, or SH, and where R.sup.1 and R.sup.4 are identical or different, being hydrogen, alkyl, cycloalkyl, aryl, carbonyl, carboxyl, carboxyalkyl or nitrile, and can be linked to form a ring, advantageously in an amount of from 0.1 to 100 mmoles and advantageously in from 1 to 20% strength aqueous solutions.

Stabilization of polyphenylene ether solutions

High molecular weight polyphenylene ethers are prepared from monohydric phenols by an oxidative coupling reaction with oxygen in the presence of a catalyst complex obtained from a copper salt and an organic amine by a method wherein the metal component of the catalyst is separated off, after the polymerization, by the addition of a polymeric polycarboxylic acid which is essentially composed of unsaturated monofunctional or difunctional carboxylic acids and/or their anhydrides. Advantageously, the polymeric polycarboxylic acids used are homopolymers or copolymers of (a) from 50 to 100% by weight of one or more unsaturated monofunctional acids of 3 to 10 carbon atoms and/or one or more difunctional acids or their anhydrides of 4 to 6 carbon atoms and from 0 to 50% by weight of one or more monomers which do not possess an acid function and can be copolymerized with (a).

In the preparation of a high molecular weight polyphenylene ether from a monohydric phenol by an oxidative coupling reaction with oxygen in the presence of a catalyst complex obtained from a metal salt and an organic amine and in the presence of a solvent, and isolation of the metal ion component of the catalyst from the polyphenylene ether solution by means of a complex-forming or chelate-forming compound, the catalyst is removed by a method wherein complex formation and isolation of the metal ion component of the catalyst are carried out in an aqueous medium in the presence of from 0.1 to 5,000 mg of an anionic or non-ionic surfactant.

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

A process for removing vaporizable constituents from high-viscosity solutions or melts of thermoplastics by continuous evaporation along a heated devolatilization zone and separation of the vapor phase from the liquid phase in a downstream separating vessel. The plastic solution or melt is first heated stepwise in increments, in the devolatilization zone, while the product is in the form of thin layers from about 0.5 to 4 mm, so as to maintain a temperature difference of less than 50.degree. C. between the heat transfer medium and the plastic solution or melt until the devolatilization temperature is reached, the distribution of the solution or melt to form thin layers of product taking place while the temperature conditions still correspond to those of the feed of solution or melt, after which the vaporizable constituents are evaporated so as to form a two-phase system of vapor and melt, and the heat of evaporation absorbed is substantially returned to the product during the evaporation along the devolatilization zone. The process permits the removal of vaporizable constituents under mild conditions.

Process and apparatus for removing vaporizable constituents from viscous

A process and an apparatus for heating or cooling very viscous solutions or melts of thermoplastics in the form of thin layers. The plastic solution or melt is spread under the temperature conditions of the feed solution or melt, and the thin layers are heated stepwise so that the temperature difference between the heat transfer medium and the solution or melt is at all times less than 50.degree. C. and preferably less than 20.degree. C. Viscous solutions or melts of thermoplastics can be heated or cooled rapidly and uniformly under gentle and controlled conditions, to prepare the solutions or melts for further treatment in conventional equipment.

Process and apparatus for controlled and gentle heating or  cooling of

A process for admixing additives to plastics and simultaneously removing volatile constituents in a horizontal devolatilizing extruder. Taken in sequence in the direction of flow, the additives are first introduced into the devolatilizing extruder from above, and the plastic melt, solution or dispersion is then introduced from below, while the bulk of the volatile constituents are withdrawn from the devolatilizing extruder at an orifice located vertically above the point at which the plastic is fed in. The process permits the removal of volatile constituents with simultaneous admixture of additives during aftertreatment of plastics, in a single step and at very high throughputs.

Process for the admixture of additives into plastics with simultaneous

A continuous process for the polymerisation of olefinically unsaturated monomers in bulk or in solution in which at least a portion of the low-viscosity materials to be fed to the polymerization zone is thoroughly mixed with a portion of the high-viscosity contents of the polymerization zone in a mixing zone disposed upstream of the polymerization zone, which mixture is then continuously fed to the polymerization zone. The resulting polymers have a uniform composition and a narrow molecular weight distribution. They may be converted to shaped articles by thermoplastic methods.

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Beindersheim, Germany

Rudi W Reffert