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Title: Isolation of levoglucosan from pyrolysis oil derived from cellulose

High purity levoglucosan is obtained from pyrolysis oil derived from cellulose by: mixing pyrolysis oil with water and a basic metal hydroxide, oxide, or salt in amount sufficient to elevate pH values to a range of from about 12 to about 12.5, and adding an amount of the hydroxide, oxide, or salt in excess of the amount needed to obtain the pH range until colored materials of impurities from the oil are removed and a slurry is formed; drying the slurry azeotropically with methyl isobutyl ketone solvent to form a residue, and further drying the residue by evaporation; reducing the residue into a powder; continuously extracting the powder residue with ethyl acetate to provide a levoglucosan-rich extract; and concentrating the extract by removing ethyl acetate to provide crystalline levoglucosan. Preferably, Ca(OH).sub.2 is added to adjust the pH to the elevated values, and then Ca(OH).sub.2 is added in an excess amount needed.
Inventors:
 [1]
  1. (Lakewood, CO)
Issue Date:
OSTI Identifier:
869636
Assignee:
Midwest Research Institute (Kansas City, MO) NREL
Patent Number(s):
US 5371212
Contract Number:
AC02-83CH10093
Research Org:
MIDWEST RESEARCH INSTITUTE
Country of Publication:
United States
Language:
English
Subject:
isolation; levoglucosan; pyrolysis; oil; derived; cellulose; purity; obtained; mixing; water; basic; metal; hydroxide; oxide; salt; amount; sufficient; elevate; ph; values; range; 12; adding; excess; obtain; colored; materials; impurities; removed; slurry; formed; drying; azeotropically; methyl; isobutyl; ketone; solvent; form; residue; evaporation; reducing; powder; continuously; extracting; ethyl; acetate; provide; levoglucosan-rich; extract; concentrating; removing; crystalline; preferably; oh; added; adjust; elevated; ph range; pyrolysis oil; amount sufficient; metal hydroxide; ph value; ethyl acetate; ph values; basic metal; isobutyl ketone; oil derived; methyl isobutyl; purity levoglucosan; excess amount; /999/