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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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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, often requiring external pressure, and the separation process cannot be completed at normal pressure
For this reason, functional groups such as amides and amine groups have been introduced into the backbone of polystyrene and polyacrylate resins through functional group reactions ([1] Lu J L, Wu M Y, Yang X L, et al. Decaffeination of tea extracts by using poly (acrylamide-co-ethylene glycol dimethylacrylate) as adsorbent[J]. Journal of Food Engineering, 2010, 97(4): 555-562. [2]Huang J H, Huang K L, Liu S Q, et al. Adsorption properties of tea polyphenols onto three polymeric adsorbents with amide group[J]. Journal of Colloid and Interface Science, 2007, 315 (2): 407-414.), which improves the adsorption capacity of tea polyphenols, but due to the strong resin skeleton Hydrophobic, so that the resin can still adsorb part of caffeine by hydrophobic effect, and can not achieve complete separation of tea polyphenols and caffeine

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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Effect test

Embodiment 1

[0022] Example 1: Preparation of Highly Hydrophilic Alcohol Hydroxyl Macroporous Adsorption Resin

[0023] Add 425mL of 0.5% gelatin aqueous solution into a 1000mL three-necked bottle at room temperature, and heat to 40°C. Mix 28g TAIC, 56g VAc, 84g n-heptane, and 0.84g AIBN evenly, pour it into a three-necked flask, start stirring and slowly raise the temperature to 60°C at a heating rate of 0.5°C / min, react for 5 hours, and then raise the temperature to 80°C , reacted for 6 hours, stopped stirring and heating, let it stand to room temperature, filtered out the resin, washed it with a large amount of deionized water, and dried it in vacuum.

[0024] Add 60g of the above-mentioned dry resin into a 500mL three-necked flask, add 250g of sodium hydroxide aqueous solution with a mass percentage concentration of 5%, start stirring, raise the temperature to 50°C, and react for 5 hours, stop stirring and heating, and let it stand at room temperature. Filter out, wash with a large ...

Embodiment 2

[0025] Example 2 : Preparation of Highly Hydrophilic Alcoholic Hydroxyl Macroporous Adsorbent Resin

[0026] Add 900mL of 1% gelatin aqueous solution into a 2000mL three-necked bottle at room temperature, and heat to 45°C. Mix 40g TAIC, 160g VAc, 100g n-octane, and 1.5g AIBN evenly, pour it into a three-necked flask, start stirring and slowly raise the temperature to 70°C at a heating rate of 0.2°C / min, react for 8 hours, and then raise the temperature to 90°C , reacted for 4 hours, stopped stirring and heating, let stand to room temperature, filtered out the resin, washed with a large amount of deionized water, and dried in vacuum.

[0027] Add 150g of the above-mentioned dried resin into a 1000mL three-necked flask, add 750g of sodium hydroxide aqueous solution with a mass percentage concentration of 10%, start stirring, raise the temperature to 60°C, and react for 2 hours, stop stirring and heating, and let it stand at room temperature. Filter out, wash with a large am...

Embodiment 3

[0028] Example 3: Preparation of Highly Hydrophilic Alcohol Hydroxyl Macroporous Adsorption Resin

[0029] Add 1200mL of 0.5% gelatin aqueous solution into a 3000mL three-necked bottle at room temperature, and heat to 50°C. Mix 80g TAIC, 80g VAc, 240g dodecane, and 1.0g AIBN evenly, pour it into a three-necked bottle, start stirring and slowly raise the temperature to 62°C at a heating rate of 0.4°C / min, react for 6 hours, and then raise the temperature to 87°C , reacted for 4 hours, stopped stirring and heating, let stand to room temperature, filtered out the resin, washed with a large amount of deionized water, and dried in vacuum.

[0030] Add 120g of the above-mentioned dried resin into a 1000mL three-necked flask, add 540g of sodium hydroxide aqueous solution with a concentration of 7% by mass, start stirring, raise the temperature to 55°C, and react for 4 hours, stop stirring and heating, and let it stand at room temperature. Filter out, wash with a large amount of de...

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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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