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

Active Publication Date: 2011-07-13
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Referring to the above molecular structure characteristics of tea polyphenols and caffeine, people introduce functional groups capable of forming hydrogen bonds into the resin skeleton. Compared with caffeine, tea polyphenols can form stronger hydrogen bonds with the resin. The role of the resin greatly improves the adsorption selectivity of tea polyphenols and caffeine. For example, Ye Jianhui et al. used polyamide materials to remove caffeine in tea polyphenols (Ye J H, Wang L X, Chen H, et al. Preparation of tea catechins using polyamide[J]. Journal of Bioscience and Bioengineering, 2010, In Press, Corrected Proof.), achieved good results, but polyamide materials are mostly amorphous and can only be used as column chromatography packing materials, and the separation is based on The number of theoretical plates of the chromatographic column is increased, so the processing capacity is low and the operation is complicated,

Method used

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  • Methods for preparing high-hydrophilcity macroporous absorption resin and removing caffeine in crude tea extracts
  • Methods for preparing high-hydrophilcity macroporous absorption resin and removing caffeine in crude tea extracts

Examples

Experimental program
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Example Embodiment

[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...

Example Embodiment

[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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Abstract

The invention discloses preparation of high-hydrophilcity macroporous absorption resin and a method for removing caffeine in crude tea extracts. A method for preparing the resin comprises the steps of: dissolving gelatin or polyvinyl alcohol in water to prepare an aqueous phase, mixing TAIC (triallyl isocyanurate) and VAc to form a polymeric monomer, adding long-chain aliphatic paraffins of C7-C12 as a porogenic agent and adding AIBN (azo-bis-isobutyronitrile) as an initiator to form an oil phase for polymerization; mixing the aqueous phase with the oil phase, stirring and heating, filtering out resin, washing the resin with deionized water and drying; and mixing the dried resin with a sodium hydroxide aqueous solution, stirring and heating for reaction, standing for cooling to room temperature after the reaction to prepare the high-hydrophilcity macroporous absorption resin. By using the high-hydrophilcity macroporous absorption resin for separating commercial crude tea extracts, the caffeine in the crude tea extracts can be completely eliminated only through a simple continuous process including adsorption and elution in one step, and the yield of tea polyphenol is more than 90%. The process for removing the caffeine is simple to operate and is free from the application of toxic solvents, the resin is recyclable, the production cost is low, and the method is particularly suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to a synthesis method of a new type of highly hydrophilic alcohol hydroxyl macroporous adsorption resin and a process for removing caffeine in tea crude extract, especially under the premise of ensuring high recovery rate of effective components of tea polyphenols, A new method for preparing caffeine-free high-purity tea polyphenol extracts only through the one-step continuous process of "adsorption-elution" of resin. Background technique [0002] Tea is a rich natural plant resource in my country, and tea drinking and tea culture have a history of thousands of years. The main physiologically active substances in tea are divided into two categories, namely tea polyphenols and caffeine. Among them, tea polyphenols (Tea-polyphenols, abbreviated as TP) is a class of polyphenolic compounds mainly composed of catechins, accounting for about 20% to 33% of the dry weight of tea leaves, mainly including catechins (C). Catechin (...

Claims

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Application Information

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IPC IPC(8): C08F218/08C08F226/06C08J9/00B01J20/26B01J20/30B01J20/28A23F3/38
Inventor 王春红施荣富王芃麻宁
Owner NANKAI UNIV
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