Benzoic Acid → HCID 21285052, compound

Participants

Reaction Conditions

Reaction Steps

The process for Example 1 was initiated by charging 546.0 grams (g) phenol (5.80 moles), 1.1 g benzoic acid (0.2% of phenol), and 79.1 g melamine (0.63 moles) into a reaction vessel to form a reaction mixture. The reaction mixture was heated to 80° C., and 55.8 g of 50.4% aqueous formaldehyde (60% of total charge) was added over 40 minutes. The reaction mixture was atmospherically distilled while heating to 123° C., and then maintaining the 123° C. temperature for 2 hours, followed by reducing the reaction mixture temperature to 80° C. 37.2 g of 50.4% aqueous formaldehyde (40% of total charge) was added over 30 minutes to the reaction mixture and then atmospherically distilling the reaction mixture to 123° C., maintaining the temperature at 123° C. for 1.5 hours, and increasing the temperature over 45-50 minutes to 165° C. and continuing to distill atmospherically. Next, the reaction mixture was under a gradually increasing vacuum over 3 hours to a full vacuum of at least 27 inches while maintaining a temperature of 163°-165° C., then heating the reaction mixture to 175° C. over 1 hour under full vacuum, followed by maintaining the vacuum and temperature at 175° C. for 15 minutes, and then steaming the reaction mixture (or water sparge) at 175° C. for 60 minutes, and after 60 minutes, cooling the resin to 164°-167° C. in about 15 minutes. Further, the process was concluded by removing the vacuum distillate (426.6 g) and discharging the product (212.9 g) from the reaction vessel.

Provenance & Evidence