Nut shell of Camellia oleifera Abel which has large scale of plantation in mountainous region of southern China is abundant renewable resource. The nut shell is suitable for preparation of furfural, as the content of which is as much as 16% (based the dried nut shell). In early time, mineral acids were employed as typically catalyst for preparing of furfural from the nut shells. These mineral acids could pollute water and corrode equipment. In this paper we used various mineral acids coating with niobic acid as catalysts to investigate reactions for preparation of furfural. Among these catalysts, the catalyst of sulfuric acid coating with niobic acid was found to be very effective, which had higher hammett acidity and better effect of hydrolysis of the nut shells; The catalysts of sulfuric acid coating with niobic acid was characterized, and the conditions of preparation of the catalyst were investigated. The optimum conditions were: sulfuric acid as coating acid, the concentration of sulfuric 1.1 mol/L, impregnation time 8 h, calcination time 8 h and calcination temperature 450˚C. Then hydrolysis of the nut shells was explored, the optimum conditions were as follows: dose of catalyst 20%, ratio of solid to liquid 1:15, reaction temperature 100˚C, reaction time 4 h; Under this condition, the yield of furfural was 8.7%.