The aim of this work is to study the catalyst prepared by glucose-starch mixture. Assessment experiments showed that solid acid behaved the highest esterification activity when glucose and corn powder were mixed at ratio of 1:1, carbonized at 400 degrees C for 75 min and sulfonated with concentrated H(2)SO(4) (98%) at 150 degrees C for 5 h. The catalyst was characterized by acid activity measurement,. XPS, TEM and FT-IR. The results indicated that solid acid composed of CS(0.073)O(0.541) has both Lewis acid sites and Bronsted acid sites caused by -SO(3)H and -COOH. The conversions of oleic acid esterification and triolein transesterification are 96% and 60%, respectively. Catalyst for biodiesel production from waste cottonseed oil containing high free fatty acid (FFA 55.2 wt.%) afforded the methyl ester yield of about 90% after 12 h. The catalyst deactivated gradually after recycles usage, but it could be regenerated by H(2)SO(4) treatment. (C) 2010 Elsevier Ltd. All rights reserved.