The invention relates to an adsorbent material with excellent adsorbing performance for uranyl ions under high acidity, which is a nano-particle compound material comprising silicon oxide serving as a shell and ASAIII (arsenazo III) serving as a core. The material is prepared by the following steps: performing ultrasonic treatment and uniform stirring on 15mL of saturated ASAIII aqueous solution, 150mL of cyclohexane, 30-200mu L of Tween 80, and regulating pH to be 8 with ammonia water; weighing 100-600 mu L of TEOS, diluting to 40mL with cyclohexane to prepare a TEOS-cyclohexane solution; putting a container filled with the mixed solution on a magnetic stirrer, dropwise adding to prepare a TEOS-cyclohexane solution at a rotating speed of 400 revolutions/ minute, dropwise adding 200-500mu L every 15-20 minutes, and stopping stirring until dropwise adding is completed, pouring the liquid out, centrifuging, removing supernate, washing with alcohol, and drying at 80 DEG C. The material shows better adsorbing performance for uranyl ions under high acidity (pH is 1), has an adsorption rate of 65 percent which is remarkably higher than those of activated carbon balls and ASAIII-treated activated carbon materials, can be repeatedly used, and is especially suitable for treatment of low-concentration uranium-containing wastewater under the condition of high acidity.