Formaldehyde → Formaldehyde;phenol

Temperature

110 °C

A glass reactor equipped with a stirrer, reflux condenser, addition funnel, and a device for controlling temperature was charged with 550 grams (5.85 moles) of phenol and 2.75 grams (0.03 mole) of oxalic acid. This mixture was heated to 110° C., and 298.8 grams (3.68 moles) of formalin, 37% aqueous formaldehyde, was slowly added during approximately 60 minutes (3600 s). The reaction mixture was allowed to reflux during the formalin addition, and for about 60 minutes (3600 s) thereafter. A vacuum was then applied, and the excess phenol and water were removed by vacuum distillation at a final temperature of 180° C. The solid novolac resin had a Mettler softening point of 87.9° C., analysis by gel permeation chromatography (GPC) showed the product to have a wt. avg. M.W. of 1,044, a no. avg. M.W. of 700, with a polydispersity of 1.49. The product contained 16.3% 2-functional components, and the ratio of 2-functional to 3-functional was 1.2 to 1.0.

1. customA glass reactor equipped with a stirrer
2. temperaturereflux
3. additioncondenser, addition funnel
4. customthe excess phenol and water were removed by vacuum distillation at a final temperature of 180° C
5. customa Mettler softening point of 87.9° C., analysis

ORD record

ord-f36e81d30eb24155b70dfd1fd92ce833

Source dataset

uspto-grants-1988_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04755543