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Zeolitic aluminophosphate, a three‐dimensional microporous material, with an average pore size of 0.38 nm is good candidate for molecular sieve application in CO2 gas separation. The separation of CO2/CH4 gas mixtures for precombustion processes is desirable from the standpoint of both environmental concerns and energy efficiency. This study concerns an environmentally friendly method to synthesize zeolitic aluminophosphate thin films on various configurations and low‐cost kaolin porous substrates with high performance in the separation of CO2/CH4 mixtures. The membranes are prepared by a gelless seed growth method that uses lower amounts of chemicals, forms no liquid gel, chemical waste, or byproducts and generates no washing water. The obtained membranes show very high selectivity for CO2 with a CO2/CH4 separation factor above 1000 in the separation of CO2/CH4 gas mixtures.