SULFATION OF PACHYMAN WITH CHLOROSULFONIC ACID USING THE IMPROVED WOLFROM METHOD

来源 :Chinese Journal of Polymer Science | 被引量 : 0次 | 上传用户:qqanjun
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High purity polysaccharide of pachyman was isolated from the powder of Poria cocos sclerotium with an yield of 77.8%. The intrinsic viscosity of polysaccharide was found to be 78.95 mL/g in DMSO solution at 25℃. The isolated polysaccharide was reacted with chlorosulfonic acid to obtain pachyman sulfate using the improved Wolfram method. The results of the orthogonality experiment on the sulfation reaction identified that the effectiveness of the reaction conditions on the degree of sulfation and the value of intrinsic viscosity is in the following order: molar ratio of chlorosulfonic acid to glucoside (3-5) > reaction temperature (60-80℃) > reaction time (1-2 h). The kinetic studies of the pachyman sulfation indicated that the hydrolysis is accompanied with the sulfation process. The decrease in intrinsic viscosity of the sulfated pachyman is proportional to the increase in the degree of sulfation under the mild reaction conditions of < 80℃, chlorosulfonic acid/glucoside mole ratio < 5, and reaction time < 2 h. Beyond the above reaction conditions, excessive loss of -OH group occurs during hydrolysis. The NMR results indicated a complete sulfation on C-6 and a partial sulfation on the C-2 and C-4 of glucoside. High purity polysaccharide of pachyman was isolated from the powder of Poria cocos sclerotium with an yield of 77.8%. The intrinsic viscosity of polysaccharide was found to be 78.95 mL / g in DMSO solution at 25 ° C. The isolated polysaccharide was reacted with chlorosulfonic acid to obtain results for the orthogonality experiment on the sulfation reaction that that the effectiveness of the reaction conditions on the degree of sulfation and the value of intrinsic viscosity is in the following order: molar ratio of chlorosulfonic acid to The kinetic studies of the pachyman sulfation indicated that the hydrolysis is accompanied by the sulfation process. The decrease in intrinsic viscosity of the glucoside (3-5)> reaction temperature (60-80 ° C)> reaction time (1-2 h) sulfated pachyman is proportional to the increase in the degree of sulfation under the mild reaction conditions of <80 ° C, chlorosulfonic acid / glucoside mole rat io <5, and reaction time <2 h. Beyond the above reaction conditions, excessive loss of -OH group occurs during hydrolysis. The NMR results indicated a complete sulfation on C-6 and a partial sulfation on the C-2 and C- 4 of glucoside.
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