Browse Prior Art Database

Process for the purification of photo acid generator; Iodonium-[4-(1-methylethyl)phenyl][4-methylphenyl]tetrakis(pentafluorophenyl)]borate.

IP.com Disclosure Number: IPCOM000012224D
Publication Date: 2003-Apr-18
Document File: 1 page(s) / 26K

Publishing Venue

The IP.com Prior Art Database

Abstract

Abstract: This invention relates to a process for the purification of Iodonium-[4-(1-methylethyl)phenyl][4-methylphenyl]tetrakis(pentafluorophenyl)]borate, (CAS No. 178233-72-2), a photoacid generator (PAG) sold commercially as Rhodorsil PI-2074. This process yields the PAG as a purified crystalline solid with improved solubility in epoxy functional monomers and improved epoxy formulation stability.

This text was extracted from a Microsoft Word document.
At least one non-text object (such as an image or picture) has been suppressed.
This is the abbreviated version, containing approximately 100% of the total text.

Title:� � Process for the purification of photo acid generator; Iodonium-[4-(1-methylethyl)phenyl][4-methylphenyl]tetrakis(pentafluorophenyl)]borate.

Abstract:� This invention relates to a process for the purification of Iodonium-[4-(1-methylethyl)phenyl][4-methylphenyl]tetrakis(pentafluorophenyl)]borate, (CAS No. 178233-72-2), a photoacid generator (PAG) sold commercially as Rhodorsil PI-2074.� This process yields the PAG as a purified crystalline solid with improved solubility in epoxy functional monomers and improved epoxy formulation stability.� Also, PAG purified by this process exhibits rapid photo-polymerization kinetics by either direct or dye sensitized initiation.� The purification process involves chromatography of the PAG using dichloromethane as the mobile phase and silica gel as the stationary phase.� After elution, volatiles were removed using a rotary evaporator to yield a tan colored oil which solidified upon standing at room temperature.� The solid was dissolved in methanol.� Water was added to the methanol solution until the stirred solution became cloudy.� Continued stirring leads to the formation of a crystalline solid.� After stirring for an additional 30-60 minutes the crystalline PAG was recovered using by vacuum filtration using a buchner funnel. The collected solids were transferred to an amber bottle and dried under vacuum at room temperature overnight (generally 16 hours).� Melting point by DSC, 132 +/- 0.05 °C; heating rate of 10 deg/min.� �