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The synthesis process of organic montmorillonite was designed and some kinds of montmorillonite/ unsaturated polyester composites using different interlayer spacing montmorillonite were prepared. The interlayer spacing of montmorillonite was investigated by XRD and was increased to 3.98 nm. The relationship between the four influential factors and the interlayer spacing were regressively analyzed and the mathematical model was established, and the result shows when the content of organic reagent was less than 70% , the relationship between the interlayer spacing and the content was linear as follows : interlayer spacing = 1. 771 + 2. 828 × concentration,the effect of the other factors was not significant. Additionally, the testing of mechanical properties of the composites showed the impact strength was improved by 217% , and the bending strength was improved by 355% , when using the montmorillonite (MMT) of the largest interlayer spacing (3.98 nm). The result of ESEM shows the interface is bonded well when the composite specimen contains the 3.98 nm MMT.