Ultra-high crosslinked weak-polarity framework absorption resin and synthesis method thereof

A technology of ultra-high cross-linking and adsorption resin, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of reduced adsorption capacity, inability to obtain ultra-high cross-linked structure of weak polar skeleton, etc., and achieve high adsorption selectivity , high adsorption capacity, simple steps

Inactive Publication Date: 2012-05-30
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the limitation of the synthesis method, this type of resin generally has the following defects: 1) while improving the adsorption selectivity, the adsorption capacity is obviously reduced
Weakly polar adsorption resins with high crosslinking and high functional group content have good adsorption selectivity in the extraction and purification of natural plant active ingredients, but the methods of synthesis and structure regulation need to be improved. Based on the traditional polystyrene large The functional grouping of porous resin and the control method of ultra-high cross-linking of resin skeleton are difficult to be directly used in the structure regulation of weak polarity skeleton adsorption resin, such as Davankov’s Friedel-Craft alkylation and then cross-linking to form ultra-high cross-linking adsorption resin The method of this method is limited to polystyrene skeleton, can't get the hypercross-linked structure of weak polarity skeleton (Davankov V.A., Rogozhin S.V., Tsyu rupa M.P., Polym.Sci.Polym.Symp.[J], 1974,47:95 -102), but this secondary cross-linking method based on the chemical reaction between the functional reagent and the resin skeleton to synthesize the ultra-high cross-linked resin will give us great inspiration in the synthesis of the resin of the present invention

Method used

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  • Ultra-high crosslinked weak-polarity framework absorption resin and synthesis method thereof
  • Ultra-high crosslinked weak-polarity framework absorption resin and synthesis method thereof
  • Ultra-high crosslinked weak-polarity framework absorption resin and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] At room temperature, dissolve 5g PVA and 25g NaCl in 470g deionized water in a 1000ml three-necked flask, and heat to 40°C; Mix the nitrile evenly, add it into the three-necked bottle, start stirring, adjust the size of the oil droplet between 0.3-1.0mm, start to heat up to 70°C, react for 4 hours, then continue to heat up to 85°C, react for 6 hours, stop the reaction, and let it stand After reaching room temperature, the resin is filtered out, and after washing and drying, a polyacrylate resin is obtained, which is a post-crosslinked matrix resin of the resin.

[0023] Add 50g of the above-mentioned polyacrylate matrix resin into a 1000ml three-necked bottle, fully swell with 200ml N,N-dimethylformamide, add 150g of ethylenediamine, stir evenly, raise the temperature to 110°C for 20 hours, stop the reaction, and Put it at room temperature, filter out the resin, wash the resin with a large amount of deionized water until the pH of the washing solution is 7-8, and dry it...

Embodiment 2

[0026] At room temperature, dissolve 5g PVA and 25g NaCl in 470g deionized water in a 1000ml three-necked flask, and heat to 40°C; Mix the nitrile evenly, add it into the three-necked bottle, start stirring, adjust the size of the oil droplet between 0.3-1.0mm, start to heat up to 70°C, react for 4 hours, then continue to heat up to 85°C, react for 6 hours, stop the reaction, and let it stand After reaching room temperature, the resin is filtered out, and after washing and drying, a polyacrylate resin is obtained, which is a post-crosslinked matrix resin of the resin.

[0027] Add 50g of the above-mentioned polyacrylate matrix resin into a 1000ml three-necked bottle, fully swell with 200ml N,N-dimethylformamide, add 300g of hexamethylenediamine, stir evenly, heat up to 140°C for 15 hours, stop the reaction, and Put it at room temperature, filter out the resin, wash the resin with a large amount of deionized water until the pH of the washing solution is 7-8, and dry it in a vac...

Embodiment 3

[0030] At room temperature, dissolve 5g PVA and 25g NaCl in 470g deionized water in a 1000ml three-necked flask, and heat to 40°C; mix 135g methyl acrylate, 15g divinylbenzene, and 1.5g azobisisobutyronitrile evenly, and add In the three-necked bottle, start stirring, adjust the size of the oil droplet between 0.3-1.0mm, start to heat up to 70°C, react for 4 hours, then continue to heat up to 85°C, react for 6 hours, stop the reaction, let it stand at room temperature, put the resin Filtrate, wash and dry to obtain polyacrylate resin, which is the matrix resin of resin post-crosslinking.

[0031] Add 40g of the above-mentioned polyacrylate matrix resin into a 500ml three-necked bottle, fully swell with 200ml N,N-dimethylformamide, add 120g of ethylenediamine, stir evenly, raise the temperature to 110°C for 20 hours, stop the reaction, and Put it at room temperature, filter out the resin, wash the resin with a large amount of deionized water until the pH of the washing solution...

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Abstract

The invention discloses an ultra-high crosslinked weak-polarity framework absorption resin, of which the grain diameter is 0.3 to 1.0mm, the moisture content is 50 to 65 percent, the expansion degree is 70 to 350 percent, and the N element content is 11 to 15 percent. A method for synthesizing the ultra-high crosslinked weak-polarity framework absorption resin comprises the following steps of: 1)dissolving dispersing agents and NaCl to prepare an aqueous phase; 2) introducing initiators into a total monomer phase consisting of methyl acrylate and cross-linking agents, and uniformly mixing toprepare an oil phase; 3) adding the aqueous phase and the oil phase into a reactor, stirring and raising the temperature for reaction, standing to room temperature, and filtering, washing and drying to obtain a matrix resin; and 4) fully swelling the matrix resin, adding diamine, raising the temperature for reaction, standing to the room temperature, and filtering, cleaning and drying the resin. The ultra-high crosslinked weak-polarity framework absorption resin has the advantages that: the resin meets multiple structural requirements on high degree of cross linking, high functional group content, weak polar framework, and the like; and the synthesis method has simple steps, high efficiency in functional group reaction, and has good application in separation of flavonoid active ingredients in natural plants.

Description

【Technical field】 [0001] The invention relates to a synthesis method of a polymer adsorption resin, in particular to a weakly polar skeleton adsorption resin and a synthesis method thereof. 【Background technique】 [0002] The extraction and separation method of natural plant active ingredients, especially in the production process suitable for large-scale industrial preparation, the adsorption resin separation method has become the most competitive modern method due to its advantages of low cost, simple process, renewable use of resin, and environmental friendliness. The method has been successfully applied in the extraction and separation of various plant active ingredients, such as the extraction and purification of flavonoids, alkaloids, saponins, polysaccharides, etc. ([1] G.F.Payne, M.L.Shuler, Selective adsorption of plant Products. Biotechnology & Bioengineering[1] J], 1988, 31(9): 922-928; [2] Shi Zuoqing, Shi Rongfu, Fan Yunge, etc.; Application of resin adsorption ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/14C08F8/32C08J3/24C08K5/17B01J20/26B01J20/30
Inventor 王春红施荣富白金超
Owner NANKAI UNIV
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