Methods for preparing high-hydrophilcity macroporous absorption resin and removing caffeine in crude tea extracts
A pore adsorption and caffeine technology, which is applied in the field of high-purity tea polyphenol extracts, can solve the problems of inability to achieve complete separation of tea polyphenols and caffeine, the separation process cannot be completed at normal pressure, and the operation is complicated, so as to ensure recovery. , suitable for large-scale industrial production, the effect of simple synthesis process
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[0022] Example 1: Preparation of highly hydrophilic alcoholic hydroxyl macroporous adsorption resin
[0023] At room temperature, add 425 mL of 0.5% gelatin aqueous solution in a 1000 mL three-necked flask, and heat to 40°C. Mix 28g TAIC, 56g VAc, 84g n-heptane, 0.84g AIBN uniformly, pour it into a three-necked flask, start stirring and slowly raise the temperature to 60℃, the heating rate is 0.5℃ / min, react for 5 hours, and then raise the temperature to 80℃ After reacting for 6 hours, stop stirring and heating, let it stand to room temperature, filter out the resin, wash with a large amount of deionized water, and vacuum dry.
[0024] Add 60g of the above-mentioned dry resin into a 500mL three-necked flask, add 250g of sodium hydroxide aqueous solution with a concentration of 5% by mass, start stirring, heat up to 50°C, react for 5 hours, stop stirring and heating, and let it stand to room temperature. It is filtered, washed with a large amount of deionized water to the pH value...
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[0025] Example 2 : Preparation of Highly Hydrophilic Alcohol-hydroxy Macroporous Adsorption Resin
[0026] Add 900 mL of 1% gelatin aqueous solution into a 2000 mL three-necked flask at room temperature, and heat to 45°C. Mix 40g TAIC, 160g VAc, 100g n-octane, 1.5g AIBN uniformly, pour it into a three-necked flask, start stirring and slowly heat up to 70°C at a rate of 0.2°C / min, react for 8 hours, and then heat up to 90°C , React for 4 hours, stop stirring and heating, let stand to room temperature, filter out the resin, wash with a large amount of deionized water, and vacuum dry.
[0027] Add 150g of the above-mentioned dry resin to a 1000mL three-necked flask, add 750g of sodium hydroxide aqueous solution with a concentration of 10% by mass, start stirring, heat up to 60℃, react for 2 hours, stop stirring and heating, and let it stand to room temperature. It is filtered out, washed with a large amount of deionized water to the pH of the aqueous solution to be 7.2, centrifuged...
Example Embodiment
[0028] Example 3: Preparation of Highly Hydrophilic Alcohol Hydroxy Macroporous Adsorption Resin
[0029] Add 1200 mL of 0.5% gelatin aqueous solution to a 3000 mL three-necked flask at room temperature, and heat to 50°C. Mix 80g TAIC, 80g VAc, 240g dodecane, 1.0g AIBN uniformly, pour it into a three-necked flask, start stirring and slowly heat up to 62°C at a rate of 0.4°C / min, react for 6 hours, then heat up to 87°C , React for 4 hours, stop stirring and heating, let stand to room temperature, filter out the resin, wash with a large amount of deionized water, and vacuum dry.
[0030] Add 120g of the above-mentioned dry resin into a 1000mL three-necked flask, add 540g of sodium hydroxide aqueous solution with a concentration of 7% by mass, start stirring, heat up to 55°C, react for 4 hours, stop stirring and heating, and let it stand to room temperature. It is filtered, washed with a large amount of deionized water until the pH value of the aqueous solution is 7.5, centrifuged, ...
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