Abstract: This article introduce a new method for preparation of a cryloyl chloride with acrylic acid and phosphorous oxychloride as raw materials and adopts a new technology that acrylic acid is added dropwise and acryloyl chl oride is distilled continuously.The results indicated that,owning to the signif icant decrease in the polymerization acrylic acid and acryloyl chloride by addin g reactant and distilling resultant continuousely,the demand of inhabitor could be decreased,so as to increase the yield and purity of the product.When the mole ratio of acrylic acid and phosphorous oxychloride is 1∶1,the yield of acryloy l chloride is 92.2%,the purity is 98.3%.