A major problem encountered in investigating the spontaneous combustion phenomenon of ferrous sulfide in processing high-sulfur crude oil is difficult to get active ferrous sulfide.In the paper,higher purity ferrous sulfide were prepared with three different synthesis methods,their self-ignition activity were studied and compared with the commercial ferrous sulfide. The experimental results shown that the ferrous sulfide synthesized in laboratory can self - ignite when exposed to air at room temperature, but the commercial sample did not combust spontaneously.And the research on spontaneous combustion characteristics of ferrous sulfide by means of thermogravimetric and differential thermal analysis showed that the ferrous sulfide prepared by the reaction of sodium sulfide reacted with ammonium ferrous sulfate solution has the highest self-ignition activity.%高含硫原油加工过程硫化亚铁自燃现象遇到的一个主要问题是很难得到活性硫化亚铁，通过3种不同方法制备高纯度硫化亚铁，并对比测定了市售硫化亚铁与3种实验室制备硫化亚铁的自燃活性。实验结果表明：在空气中，常温下实验室制备的硫化亚铁均可自燃，市售的硫化亚铁不具备自燃活性。利用热重/差热分析法对硫化亚铁的自燃特性进行了研究，结果表明，硫化钠溶液与硫酸亚铁铵溶液反应制备的硫化亚铁自燃活性最高。
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