A method for production and purification of pyrocatechol (I) from low-temperature carbonization effluents was described. Phenosolvan, a mixture of isobutyl, butyl, and amyl acetates, was used for extraction of I from the effluent. After removing most of the solvent by distillation, the separation was completed by batch vacuum distillation at 25 to 50 millimeter Hg. The 4th fraction, containing I 49.2, I homologues 31.1, o-cresol 6.8, xylenols 7.3, and higher boiling material and residue 5.6 percent, was treated in a purification pilot plant, which was described. This fraction was dissolved in an equal weight of C/sub 6/H/sub 6/, then cooled. I was crystallized out in a vacuum crystallizer, centrifuged, and washed with C/sub 6/H/sub 6/, dried in a rotating-plate drier and taken to storage. The purified I melted 100/sup 0/ to 102/sup 0/ and contained 4 to 8 percent homologues or other impurities. A further recrystallization raised its purity to 99.2 percent. Plant capacities and production costs are given.