The invention belongs to the field of inorganic nanomaterials, and involves a preparation method for sulfur compounds of lead nanomaterial by calixarene in a specific thermal control system solvent. Said method comprises placing lead salt and calixarene in a container, using toluene as solvent, stirring at 70-90DEG C for 0.8-1.5 hours to obtain a mixture, transferring the mixture into a reactor and adding sulfur source, adding toluene to 3 / 5-4 / 5 of the reactor volume and sealing, reacting at 150-200DEG C for 18-30 hours and cooling to room temperature, washing, separating, and drying to obtain the final product. The molar ratio of sulfur source to lead salt is 1 : 1, wherein the lead salt is one of lead nitrate and lead acetate and sulfur source is one of thiourea, sulfur powders, and selenium powders. The raw materials of this invention are easy to get and cheap. This invention also has the advantages of simple operation and equipment, high purity, convenient treatment, and being easy for industrialization. This invention provides a new method for preparing nanomaterials by controlled synthesis.