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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) / 82K

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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.

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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.