Study On Synthesis Of Polymerized Rosin And Hydrogenated Rosin In Supercritical Carbon Dioxide

Firstly, AL-MCM-41, Mo-MCM-41, Zr-MCM-41 series were prepared by hydrothermal synthesis and characterized by XRD, N2/ adsorption-desorption, FT-IR and NH₃-TPD. The results show that the molecular sieve obtained possesses the characteristics of mesopores, better long-range order and crystallinity, and that SO₄^2-, BO₃^3- and ZrO₂ are combined with the molecular sieve so that its acidity is improved. Under the condition of supercritical CO₂, the mesoporous molecular sieve was firstly used in polymerized rosin. In contrast to other sieves, it was shown that BO₃^3- /ZrO₂/Mo-MCM-41 molecular sieve was of higher catalytic activity. After BO₃^3- /ZrO₂/Mo-MCM-41 molecular sieve being chosen as the catalyst of reaction, it was carefully examined that the reaction conditions affected the polymeric reaction of rosin results, such as supercritical CO₂ condition, temperature, pressure, time, solvent, life of catalyst, etc. The optimum process parameters has been ascertained through experimentation. As follow, at 90℃,making BO₃^3-/ZrO₂-Mo-MCM-41 strong acid mesoporous molecular sieves as catalyst, the quality ratio of catalyst to rosin is 1:10, for an hour,and under the pressure 12Mpa-14Mpa of CO₂. At last, the experimentation obtained the polymeric rosin with 106℃ softening point. The result shows that abietic acid and polymerized product are resolvable in supercritical carbon dioxide fliud. It is improved that diffusivity of reactant in supercritical carbon dioxide, so the supercritical CO₂ fluid was good for the polymerized rosin reaction and improved the softening point of product. In addition, because mesoporous molecular sieves have large hole inside, and abietic acid molecules are able to get into the hole of sieves, mesoporous molecular sieve was of higher catalytic activity.