The B. F. Goodrich Company

Southern Research Institute

The B.f. Goodrich Corporation

Linwood P Tenney

Parley C Lane, Jr

George M Benedikt

Paul T Stricharczuk

Gerald V Wootton

Robert J Minchak

Timothy J Kettering

David J Smith

Dennis C Shen

Nancy Susan Marchant

John Victor Wessel

Kong Sung Yi

Robert W Layer

Robert W Hallman

James J Shipman

Kusay B Al-Jumah

Leman G Beall, Jr

Augusto C Ibay

A continuous process for the solution polymerization of appropriate polycycloolefins in a ROMP zone to obtain a processable ROMP homo- or copolymer in solution, and subsequent hydrogenation of the ROMP (co)polymer without removing the residual ROMP catalyst and co-catalyst, provides an optical product having a mol wt M.sub.w in the range from 50,000-300,000 and polydispersity M.sub.w /M.sub.n in the range from 1.3-5.0, more preferably from 1.3-3, the lower the polydispersity the more desirable the physical properties of the (co)polymer. The process comprises, (A) continuously polymerizing a substantially anhydrous solution of said monomer by ring opening metathesis polymerization in at least a first and a last reaction zone of a multi-zoned, single-stage, reaction vessel to form an unsaturated polymer cement essentially free of unreacted monomer; (B) hydrogenating said unsaturated polymer cement in the presence of an effective amount of a nickel-containing hydrogenation catalyst in an amount sufficient to produce a hydrogenated cement wherein more than 97% of double bonds in said unsaturated polymer are converted to single bonds; (C) removing more than 99% by weight of spent polymerization catalyst, used hydrogenation catalyst and filter aid present in said hydrogenated cement to produce an essentially solids-free hydrogenated cement; (D) devolatilizing said solids-free hydrogenated cement to produce a thickened hydrogenated polymer cement, and, (E) recovering a solid polymer which meets particle count specifications for optical grade polymer.

Continuous process for making melt-processable optical grade ring-opened

A continuous process for the solution polymerization of appropriate polycycloolefins in a ROMP zone to obtain a processable ROMP homo- or copolymer in solution, and subsequent hydrogenation of the ROMP (co)polymer without removing the residual ROMP catalyst and co-catalyst, provides an optical product having a mol wt M.sub.w in the range from 50,000-300,000 and polydispersity M.sub.w /M.sub.n in the range from 1.3-5.0, more preferably from 1.3-3, the lower the polydispersity the more desirable the physical properties of the (co)polymer. The process comprises, (A) continuously polymerizing a substantially anhydrous solution of said monomer by ring opening metathesis polymerization in at least a first and a last reaction zone of a multi-zoned, single-stage, reaction vessel to form an unsaturated polymer cement essentially free of unreacted monomer; (B) hydrogenating said unsaturated polymer cement in the presence of an effective amount of a nickel-containing hydrogenation catalyst in an amount sufficient to produce a hydrogenareal cement wherein more than 97% of double bonds in said unsaturated polymer are converted to single bonds; (C) removing more than 99% by weight of spent polymerization catalyst, used hydrogenation catalyst and filter aid present in said hydrogenated cement to produce an essentially solids-free hydrogenated cement; (D) devolatilizing said solids-free hydrogenated cement to produce a thickened hydrogeneated polymer cement, and, (E) recovering a solid polymer which meets particle count specifications for optical grade polymer.

A process for increasing the molecular weight of cycloolefin monomers is provided by this invention which can be incorporated into ring-opening polymerization methods. This method is particularly suited for bulk polymerization processes but can also be used for solution polymerization processes. By increasing the molecular weight of the cycloolefin monomers, polymers having higher glass transition temperatures are obtained.

Method for preparing cycloolefin copolymers with improved heat stability

Substantially optically clear molding compositions comprising polymerized cycloolefin monomers (e.g., norbornene-type polymers) which, subsequent to polymerization have been hydrogenated are provided. The polymers have a weight average molecular weight of from about 37-47.times.10.sup.3.

Process for making a polymer for an optical substrate by hydrogenating a

Polyester and cellulosic contaminants are removed from the surfaces of polyolefins by contacting the polyolefins with an aqueous composition of alkali metal hydroxide and/or alkaline earth metal hydroxide; and with an oxidizing agent.

Process for removing contaminants from polyolefins

Copolymers from a hydroxy acid and a polycarboxylic component, method of preparation thereof, and use thereof are provided.

Polymers from hydroxy acids and polycarboxylic acids

Copolymers for use in preparing prepregs, which in turn are used to prepare printed circuit wiring boards are provided, as well as processes for producing the prepregs and wiring boards. The copolymers comprise repeating units derived from cycloolefin monomers, e.g., norbornene-type monomers, e.g., dicyclopentadiene-type monomers. Some of the monomers are silane-substituted while others are non silane-substituted. The silane-substituted monomers provide copolymers which exhibit improved properties when employed as the copolymers in prepregs for printed circuit wiring boards. For example, improved adhesion is achieved between the noncellulosic substrate and the polymers of components used in the wiring boards. These properties include, but are not limited to improved dielectric properties, improved adhesion to glass cloth substrates, etc.

Prepreg comprising saturated or unsaturated silane substituted cyclic

Substrate for optical recording media and molding composition therefor

Copolymer for use in preparing prepregs, printed circuit wiring boards

This invention provides improved prepregs for producing laminates and improved laminates using such prepregs. Processes for producing the prepregs and the laminates are also provided. Processes for producing the prepreg include the steps of providing a dipping solution or suspension comprising a polynorbornene polymer, a polyolefin polymer derived from C.sub.2 -C.sub.4 monomers, and a solvent followed by impregnating a non-cellulosic cloth with the solution. The solvent is removed from the cloth to form the prepreg. Printed circuit boards are also provided by a process which includes the steps of providing such a prepreg and pretreating the surface of a conductive film with a solution of a silane compound, effective to increase the bond strength between the copper foil and the prepreg, followed by laminating the prepreg to the conductive film.

Low dielectric constant prepreg based on blends of polynorbornene and

Liquid dicyclopentadiene feedstocks are provided for bulk polymerization by the addition of reactive norbornene function containing cycloolefin monomers to solid, high purity dicyclopentadiene compositions. These liquid dicyclopentadiene feedstocks provide a high degree of conversion to polymer under bulk polymerization conditions.

Liquid dicyclopentadiene feedstock for bulk polymerization

Precipitation of a polymer from polymer cement containing about 15 to 80% solids is accomplished by mixing the cement with water and a nonsolvent near or above the boiling point of a ternary azeotrope whereby the polymer precipitates forming a slurry and the ternary azeotrope is withdrawn as a vapor, separating the polymer from the liquid phase and recycling the liquid phase to the mixing step, the polymer cement being a honey-like solution in a nonpolar solvent of a polymer prepared by ring opening polymerization in the nonpolar solvent of at least one cyclic olefin containing at least one norbornene group, the nonsolvent is selected from lower alcohols that form binary azeotropes with water, and the ternary azeotrope comprising the nonpolar solvent, the nonsolvent, and water. The process can be operated either in batchwise segments or continuously throughout.

Precipitation of polycycloolefins

Process for precipitating a polycycloolefin from polymer cement comprising mixing said cement with a sufficient amount of a lower alcohol and water precipitant to cause said polymer to precipitate, and separating said polymer from the remaining liquid phase, the polymer cement having about 15 to 80% solids concentration and being a honey-like solution in a nonpolar hydrocarbon solvent of a polymer formed by ring opening polymerization of at least one monomer containing at least one norbornene group. The precipitation process can be either batch or continuous throughout.

Precipitation of polymeric cycloolefins

Precipitation of polymer from a polymer cement comprising the polymer dissolved in cyclohexane is accomplished by mixing the cement with methanol whereby the polymer precipitates forming a polymer slurry comprising polymer solids dispersed in cyclohexane and methanol, heating the polymer slurry to vaporize methanol and cyclohexane in azeotropic proportion, condensing the vaporized methanol and cyclohexane whereby it separates into an upper phase that is nearly all cyclohexane and a lower phase that is rich in methanol, separating the phases, and separating the polymer from the residual slurry comprising polymer solids dispersed in methanol, the polymer being a reaction product formed by ring opening polymerization of at least one monomer containing at least one norbornene group. The process can be conducted in batchwise segments or continuously throughout.

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Birmingham, AL, United States of America

Linwood P Tenney