Poly (3-valerylpyrrole) (PVPy)/multi-wall carbon nanotubes (MWNTs) composites have been pre- pared by in situ chemical polymerization of 3-valerylpyrrole (VPy) on MWNTs. The structure and properties of the samples were studied by FT-IR,XRD,SEM,TEM,TGA and four probe method. FT-IR suggested an exist- ence of interaction between PVPy and MWNTs. TEM indicated that PVPy was only coated on the external sur- face of MWNTs. XRD patterns implied that the intensity of the peaks at around 25.82~ and 42.92~ decreased with the increase of the mass ratio of VPy to MWNTs. In addition,the electrical conductivity of the samples was investigated at room temperature, and the results exhibited that MWNTs enhanced the conductivity of PVPy/ MWNTs composites compared to PVPy. The conductivity of PVPy/MWNTs composites was 2.37 S/cm( VPy: MWNTs = 2.5: 1 ) and 0.25 S/cm ( VPy: MWNTs = 5: 1 ), respectively.%通过原位化学聚合法制备了聚3-戊酰基吡咯（PVPy）／多壁碳纳米管（MWNTs）复合材料，利用傅里叶变换红外光谱（FT－IR）、X射线衍射（XRD）、扫描电镜（SEM）、透射电镜（TEM）、热重分析（TGA）与四探针法对样品的结构和性能进行了研究，FT－IR表明，PVPy与MWNTs分子问存在相互作用力，TEM显示，3－戊酰基吡咯（VPy）单体仅在MWNTs的外表面发生聚合，XRD谱显示，PVPy／MWNTs复合材料中MWNTs的两个特征结晶峰强度随着VPy／MWNTs原料比增加而逐渐降低，主要表现出PVPy的结晶峰，电导率测试结果表明，通过MWNTs与PVPy复合，可以显著的提高PVPy／MWNTs复合材料的导电性，其电导率分别为2．37S／cmrVPv／MWNTs=2．5／1）与0．25S／cm（VPv／MWNTs＝5／11。
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