1.5% of the nano montmorillonite (M) and palygorskite (P) were separately added to the phenol prepolymer, and phenolic resins were synthesized in in-situ method (called PF/M and PF/P). The TG analysis of the synthetic resins was carried out. The synthetic resins PF/M and PF/P were used as the new resin matrix to prepare semimetal friction material samples. Tribological performance test was carried on an XD-MSM fixed speed type friction-wear the testing machine. The results show that the heat resistance of PF/M by nano-particles for 1.5% and its tribological performance of friction material are better than no nanoparticle composite PF and PF/P. The carbon residue rate of mass fraction of 1.5% synthetic resin PF/M is more than PF/P and PF, separately increased by 4% and 12% at 600 ℃. The temperature thermal recession of the sample prepared by PF/M is increased by 50 ℃ and 100 ℃ more than the sample prepared by PF/P and no nano-particles composite resin, and has stable friction coefficient. Its wear rate is separately reduced by 16.8% and 27% than FP-1.5 and F-0.0 at the high temperature of 350 ℃.