The effect of bis‐(2‐ethylhexyl)phosphoric acid (DEHPA) on the region of existence, conductivity and structure of sodium bis‐(2‐ethylhexyl)phosphate (NaDEHP) microemulsion has a dual nature and depends on DEHPA concentration. In the system NaDEHP–DEHPA–kerosene–water, the narrowing of the microemulsion region is observed with DEHPA concentration in the organic phase growth from 0.1 to 0.5 mol/L. The increase of DEHPA concentration in the organic phase from 0.1 to 0.4 mol/L leads to the reduction of electrical conductivity of the microemulsions. Based on the conductivity and viscosity measurements, we suppose the transition from reverse microemulsion with isolated droplets to percolate microemulsion at volume fraction of water 0.18 ( W=CH2O/CNaDEHP = 8). Droplet size of the microemulsions increases linearly with W growth. The rise of DEHPA concentration in the organic phase from 0.1 to 0.3 mol/L causes the growth of the coefficient at W in the equation d = kW + b from 0.038 to 0.249, i.e., it increases the slope of the lines. In contrast, DEHPA introduction at the concentration 0.1 mol/L (in the organic phase) leads to the expansion of the microemulsion region, does not affect the conductivity and decreases the coefficient at W. The rate of copper recovery into the microemulsion increases considerably with the rise of DEHPA concentration from 0.0 to 0.3 mol/L; no dual effect is observed. The following composition of the microemulsion for non‐ferrous metals leaching is recommended: CNaDEHP = 1.6 mol/L, CDEHPA = 0.3 mol/L (in the organic phase); W = 8–32.

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