A novel bimetallic CuZn-BTC coordination polymer was successfully prepared through a new "Acidic etching-Self assembly" method with ZIF-8 as sacrificial template. This method was different from one-pot synthesis or post-synthetic methods, had higher Cu/Zn molar ratio and uniform distribution of metal elements. Compared with most of the bimetallic coordination polymers reported, the method reported in this paper had relatively short synthesis time when the content of two metals reached a similar level. Using CuZn-BTC as precursor, the highly dispersed Cu/ZnO catalyst for CO2 hydrogenation to methanol was synthesized, and exhibited excellent catalytic performance, which benefited from adequate and stable Cu/ZnO interfacial interaction. Especially the methanol selectivity would not decrease obviously with the increase of temperature. This new approach based on CuZn-BTC precursor took advantage of the unique structural feature of CuZn-BTC such as uniformly distributed bimetallic ions, prevented the aggregation of Cu and ZnO nanoparticles, and generated more stable CuZnO interfacial sites. Therefore, this "Acidic etching-Self assembly" synthetic method for bimetallic coordination polymer was advantageous.