This paper investigates the structure and phase composition of Al–TiB2 metal matrix composites prepared from the Al–Ti–B system powder using self-propagating high-temperature synthesis (SHS) in semi-industrial conditions (the amount of the initial powder mixture was 1000 g). The samples produced in semi-industrial conditions do not differ from the laboratory samples, and consist of the aluminum matrix and TiB2 ceramic particles. The temperature rise leads to the growth in the average size of TiB2 particles from 0.4 to 0.6 µm as compared to the laboratory samples. SHS-produced composites are milled to the average particle size of 42.3 µm. The powder particles are fragmented, their structure is inherited from the SHS-produced Al–TiB2 metal matrix composite. The obtained powder can be used as the main raw material and additive in selective laser sintering, vacuum sintering, and hot pressing products. It is worth noting that these products can find their own application in the automotive industry: brake pads, drums, rail discs, etc.