In Korea, plastic use increases by 10% every years, because of its good material characteristics such as high function, hygienic, convenient and economic. Especially, Korea ranks 4th in the world in the plastic production and about 4 million tons of waste plastics are generated annually. But, at present, over 80% of waste plastic is disposed by reclamation and incineration and only 20% of waste plastic is recycled, causing problems such as loss of valuable material and environmental pollution by disposal of waste plastics. Among various methods for recycling of waste plastic, the material recycling is the one of the best methods. Therefore, a good separation technique for material recycling has to be developed prior to other techniques. In this study, we carried out the research on development of material separation technique by triboelectrosatic separation. At optimum test conditions, we were able to remove PVC up to 99% from PET.