Study On Separation Of Liquefied Resultant Of Salix Psammophila, Caragana Intermedia And Components Structure Analysis

Facing the lack of energy resources all over the world, it is an urgent matter that exploring a new energy resource for dissolving the energy shortage. Liquefaction is one of the promising techniques for effective utilization of woody biomass, by which the lignocellulosics can be converted to liquid reactive materials. These materials could be employed as alternative intermediates to the conventional petrochemical derived phenol in production of resin. Conversion of solid biomass into liquid mass can not only supply a new type of biofuel, but also produce some chemicals. Therefore, to develop liquefaction technology will have a wide application prospective. It is realized that desert shrub is transformed into liquefied product relying on the rich desert shrub resource. The research provides the theoretical basis and experimental evidence.Research results are summed up as follows:1. In this thesis, the liquefaction of Salix and Caragana using Phenol, sulfuric acid as liquefied solvents and as catalyst was carried out, and the effects of reaction temperature, time and catalyst dosage were discussed. The optimum processing parameters for Salix and Caragana liquefaction is: temperature: 150°C, the reaction time: 120min, liquid ratio (phenol/wood ratio): 4 and catalyst content: 7%. Based on orthogonal experiments, the optimum conditions were determined. Under the optimum conditions, the relative residue ratios are 4.08% and 11.21%.2. In order to study on the components of liquefied resultant of Salix psammophila and explore the liquefaction mechanism of wood material deeply, the method of thin-layer chromatogram (TLC) is adopted to determine the best eluent of column chromatography separation, which is the mixture of Petroleum ether and Ethyl acetate (P.E) at 2:3 (V/V). And analyze the effect of different solvents as eluent on separation of liquefied resultant of Salix psammophila and Caragana.3. The next step is conducted with a column filled with silica gel G as an adsorbent (the stationary phase), crossed by the eluent mixture of Petroleum ether and Ethyl acetate (the mobile phase), which elutes the sample according to its polarity. And two pure components are extracted, it is easy to identify respectively by NMR spectra.4. Finally, the structures of the sample of liquefied resultant of S.P and the two extracted components are identified respectively by 1H NMR and 13C NMR spectra. The results show: in the comparability of analysis about the liquefied resultant of S.P and C.I by 1H NMR, the peak area is larger averagely and much more protons contribution in liquefied resultant of S.P. The reason is that contains less cellulose and hemicelluloses contents. The change of chemical shifts is not obvious which is tested by 13C NMR spectra. However, there is some difference in strength of spectra lines comparably.It is considered that the cellulose, hemicelluloses and lignin of S.P and C.I produceβ-D-glucose and condensed guaiacyl units, coniferyl alcohol aromatic nucleophilic protons of lignin in liquefaction in phenol. There is the reaction of degradation, polycondensation when the Salix psammophila and Caragana intermedia are liquefied in the condition of phenol as liquefied solvents, sulfuric acid as catalyst.