Oligomeric glucose sulfuric ester and preparation thereof
A technology of oligoglucose and sulfuric acid ester, which is applied in the field of sugar derivative production to achieve the effect of abundant raw material sources and simple process
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Embodiment 1
[0019] Embodiment 1: the preparation method of oligoglucose sulfate
[0020] Measure 800ml of concentrated sulfuric acid (98%) into a beaker, place the beaker in a low-temperature thermostat at -5°C, and add 600ml of n-propanol. Weigh 40 g of dry cotton and add it to the above-mentioned prepared reaction solution, keep the temperature at 0°C, and react for 5 hours. Remove the reaction solution by suction filtration with a sand core funnel, and wash with 5 L of propanol until the washing solution no longer shows acidity. Dissolve the residue after suction filtration in 2L of water, keep the temperature at 60°C, and stir to make it uniform. Suction filtration at room temperature, the filtrate is glucose sulfate aqueous solution, 10 times the volume of ethanol is added to the above aqueous solution, and the resulting solution is centrifuged in a high-speed centrifuge at 3000rpm for 10 minutes to obtain oligoglucose sulfate precipitate. After precipitation, drying and pulverizat...
Embodiment 2
[0021] Embodiment 2: the preparation method of oligoglucose potassium sulfate
[0022] Measure 800ml of concentrated sulfuric acid (98%) into a beaker, place the beaker in a low-temperature thermostat at -5°C, and add 600ml of n-propanol. Weigh 40 g of dry cotton and add it to the above-mentioned prepared reaction solution, keep the temperature at 0°C, and react for 5 hours. Remove the reaction solution by suction filtration with a sand core funnel, and wash with 5 L of propanol until the washing solution no longer shows acidity. Dissolve the residue after suction filtration in 2L of water, keep the temperature at 60°C, stir to make it uniform, and at the same time add KOH solution dropwise to adjust its pH to 9, and stir for 2 hours. Suction filtration at room temperature, the filtrate is glucose sodium sulfate aqueous solution, 10 times the volume of ethanol is added to the above aqueous solution, and the resulting solution is centrifuged in a high-speed centrifuge at 3000 ...
Embodiment 3
[0023] Embodiment 3: the preparation method of oligoglucose potassium sulfate
[0024] Measure 800ml of concentrated sulfuric acid (98%) into a beaker, place the beaker in a low-temperature thermostat at -5°C, and add 400ml of n-propanol. Weigh 40g of dry cotton and add it to the above-mentioned prepared reaction solution, keep the temperature at 0°C, and react for 10h. Remove the reaction solution by suction filtration with a sand core funnel, and wash with 5 L of propanol until the washing solution no longer shows acidity. Dissolve the residue after suction filtration in 2L of water, keep the temperature at 90°C, stir to make it uniform, and at the same time add KOH solution dropwise, adjust its pH to 9, and stir for 4h. Suction filtration at room temperature, the filtrate is glucose sodium sulfate aqueous solution, 50 times the volume of ethanol is added to the above aqueous solution, and the resulting solution is centrifuged in a high-speed centrifuge at 3000 rpm for 15 m...
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