Browse Prior Art Database

PROCESS FOR PRODUCING TELECHELIC BRANCHED AND STAR THERMOPLASTIC RESINS

IP.com Disclosure Number: IPCOM000027233D
Original Publication Date: 1995-Oct-31
Included in the Prior Art Database: 2004-Apr-07
Document File: 2 page(s) / 105K

Publishing Venue

Xerox Disclosure Journal

Abstract

Disclosed is a free radical polymerization process for the preparation of telechelic branched and star thermoplastic resins, comprising: heating a mixture of a multifunctional nitroxide compound and at least one polymerizable monomer compound to form the thermoplastic resin; cooling the mixture; optionally isolating the thermoplastic resin; wherein the multifunctional nitroxide compound is formed from a stable free radical agent and a compound having one or more halide functional groups.

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XEROX DISCLOSURE JOURNAL

PROCESS FOR PRODUCING Proposed Classification TELECHELIC BRANCHED AND U.S. C1.430/110 STAR THERMOPLASTIC RESINS
Karen A. Moffat
Peter M. Kazmaier
Gordon K. Hamer
Michael K. Georges

Int. C1. G03g 09/097

Disclosed is a free radical polymerization process for the preparation of telechelic branched and star thermoplastic resins, comprising: heating a mixture of a multifunctional nitroxide compound and at least one polymerizable monomer compound to form the thermoplastic resin; cooling the mixture; optionally isolating the thermoplastic resin; wherein the multifunctional nitroxide compound is formed from a stable free radical agent and a compound having one or more halide functional groups.

The following example demonstrates the formation of the multifunctional nitroxide compound 1,1'-bis-[2,2,6,6-tetramethylpiperidinyl-l-oxyl]-l,1'-
methyl-p-xylene, and the use of that compound in the subsequent in situ stable free radical polymerization of styrene to form a telechelic branched resin.

A 100 mL round bottom flask equipped with a stir bar was placed in an ice bath. Into the flask were added 25 mL distilled styrene, 7.68 g TEMPO and
6.79 g a,a'-[di-2-bromoethyl]-p-benzene. A stream of argon gas was bubbled through the reacting medium to provide an inert atmosphere. Into a dropping funnel were added 10.7 g tri-n-butyl tin hydride (n-BusSnH), and then added into the reaction system dropwise over a 30 to 60 minute period. The addition of the hydride was slow enough so that the temperature of the system does not exceed 10°C. After complete addition of the tin hydride, the solution was stirred for an additional hour at 10°C. The temperature was then increased to 35°C for 2 hours to f...