One of the earliest cases of overexploitation and pollution in Europe has been found in SE Iberia, a key center of Early Bronze in Western Europe (Argaric civilization). The sediments of a lake in Sierra Nevada (Andalusia), known as Laguna de Río Seco (pictured), have provided the evidence for important pollution c. 3900 years ago, just when the Bronze Age began in the region. This is attributed mostly not to industry but to increase in fires and deforestation.
However, as we get into the Late Bronze (post-Argaric culture) and Iron age (Iberian culture), the evidence speaks of a type of pollution which can only be attributed to manufacture: lead. This kind of pollution reached a peak c. 2900 years ago (beginnings of Iron Age) and then again in the Roman era (as well as in the Industrial Age).
It is worth mentioning that lead pollution has decreased in the last decades, caused no doubt by the environmental awareness of these times and derived normative, like banning lead from gasoline.
Ref. A. García Alix et al., Anthropogenic impact and lead pollution throughout the Holocene in Southern Iberia. Science of the Total Environment 2013. Pay per view → LINK [doi:10.1016/j.scitotenv.2013.01.081]