The invention relates to an organic solvent tolerant NBR/PVC (nitrile-butadiene rubber/polyvinyl chloride) composition and a preparation method of the composition. The preparation method is characterized by comprising the steps of compounding double coupling agents to prepare talcum powder/silicon oxide functional hybridization filling, and further adopting a thin-passing orientation-pre-curing-stress tension-vulcanization shaping technology to form the organic solvent tolerant NBR/PVC composition with good filling-rubber interaction, an effective organic solvent obstruction layer and a smallcross-linked network molecular clearance.