Fumaric Acid → Rosin fumaric acid

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반응 단계

A resin was prepared according to the method of the present invention by placing 1000 grams of tall oil rosin in an autoclave equipped for heating, cooling, pressurizing and stirring the reaction medium. The rosin was heated to 200° C. under a nitrogen atmosphere. Fumaric acid in the amount of 240 grams was added to the heated rosin and the mixture was reacted for 4 hours at 200° C. at atmospheric pressure under a nitrogen gas blanket in order to form a rosin/fumaric acid adduct. At the end of the 4 hour reaction period, 300 grams of pentaerythritol were added to the rosin/fumaric acid adduct. The autoclave was sealed under nitrogen, and the temperature of the reaction mass was increased to 210° C. The pressure in the autoclave was allowed to build autogenously as the reaction progressed due to the formation of water during the esterification of the adduct. After approximately 8 hours, the reaction mixture had an acid number of about 141.5 (ASTM D465-59) and a softening point of 132° C. (ASTM E28-67). At this point, the pressure in the autoclave was about 135 psia (929 kPa). The reaction mass was maintained at 210° C. and 135 psia (929 KPa) for an additional 5 hours after which the acid number was 134.1 and the softening point was 136° C. After being held for a total of 15 hours at this temperature and pressure, the product remained a flowable liquid without an appreciable change in the acid number (124.8) and softening point (140.5° C.) of the resin from that of the product after the initial 8 hour reaction period. Analysis of the resin product by Gel Permeation Chromatography confirmed that only minor changes in the molecular weight distribution of the partially esterified resin occurred during the 15 hour hold time after the initial 8 hour reaction time.

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