The Systhesies Of Terpineol By One-step Hydration Of Turpentine With Solid Acid Catalysts

Terpineol was synthesized via hydration reaction in which pinene was raw material, and macroporous sulfonic acid resin or homemade carbon-based solid acids from lignin gel were used as catalysts. The main research contents and results were as follows:1. The reaction conditions for two-phase hydration of pinene with macroporous sulfonic acid resin as catalyst were studied. The effect of solvent type, water amount, reaction temperature and catalyst amount on terpineol yield was studied. The optimum conditions for two-phase hydration reaction of pinene were investigated by single factor experiment: turpentine was 4.0g, water was 4.0m L, dosage of catalysts was 0.4g, reaction temperature was 80 ℃. Under these conditions pinene conversion was 97.0%, and terpineol yield was up to 42.1%.2. The dynamic experiment of pinene hydration with macroporous sulfonic acid resin as catalyst was studied at different reaction temperature. The results indicated that the reaction was first order reaction. The reaction rate constant was 0.507 h-1 at 80 oC, and the reaction activation energy was 126.66 KJ/mol.3. The reaction conditions for three-phase hydration of pinene with macroporous sulfonic acid resin as catalyst were studied. The optimum conditions for three-phase hydration reaction of pinene were investigated by orthogonal experiment: Hexadecyl trimethyl ammonium Bromide was 0.004 g, turpentine was 4.0g, water was 4.0g, solvent was 10 m L, reaction temperature was 70℃, the dosage of catalysts was 0.4g, reaction time was 12 h. Under these conditions pinene conversion was 77.8%, and α- terpineol yield was up to 27.6%.4. The carbon-based solid acid prepared by gel method had a developed pore structure comparing with the suspension polymerization.5. The analysis and characterization of carbon-based solid acid. The results of XRD showed that the carbon-based solid acids were composed of amorphous carbon. The results of FT-IR and photoelectron spectroscopy(EDS) showed that the active center of carbon-based solid acid existed in the form of sulfonic group. Thermogravimetric Analysis(TG) of carbon-based solid acid showed that thecarbon-based solid acid had good thermal stability, and carbon-based solid acid can be used under 200 ℃.6. Iodine number and methylene blue adsorption value of carbon-based solid acid were studied, the micropore and mesoporous of catalyst had an effect on pinene hydration, results showed that the methylene blue adsorption value had a bigger effect on the pinene hydration.7. The reaction conditions for two-phase hydration of pinene with porous carbon-based solid acid as catalyst were studied. Isopropanol was solvent, the optimum conditions for two-phase hydration reaction of pinene were investigated by single factor experiment: turpentine was 4.0g, water was 4.0g, the dosage of catalysts was 0.4g, reaction temperature was 80℃. Under these conditions, pinene conversion was 94.7.0%, terpineol yield was up to 40.2%.8. The dynamic experiment of pinene hydration with porous carbon-based solid acid as catalyst was studied at different reaction temperature. This reaction was first order reaction. The reaction rate constant was 0.225h-1 at 80 oC, the reaction activation energy was 87.9 KJ/mol.