Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof

A composite function, ultra-high cross-linking technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of single coordination, no microporous structure, low cross-linking degree, etc., and achieve improved thermal stability , good affinity and broad application prospects

Inactive Publication Date: 2008-07-23
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent involves the use of functionalized imidazole-modified adsorption resin to obtain imidazole-modified styrene-type macroporous adsorption resin in the resin synthesis step, but the resin has not undergone post-crosslinking reaction, the degree of crosslinking is low, and the specific surface area is usually less than 100m 2 / g, and basically does not have a microporous structure, the adsorption performance of lipophilic organic matter is very poor, and it only has a single coordination effect on hydrophilic organic matter, and the mechanical properties of the resin particles are not high.
[0003] Literature search shows that there is no literature report on imidazolyl-modified composite functional ultra-high cross-linked adsorption resin and its preparation method

Method used

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  • Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof
  • Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof
  • Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof

Examples

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Effect test

Embodiment 1

[0025] Take 30g of chlorine balls with a cross-linking degree of 8% (produced by Hebei Langfang Electric Power Resin Factory, etc., with a chlorine content of 18%), add 60ml of nitrobenzene and dissolve it in a 250ml three-necked bottle for 12h; heat up at a speed of 1°C / 2min to 80°C, add 2g of zinc chloride at a certain stirring speed, and continue the reaction until the residual chlorine content of the resin is 12%; exhaust the reaction mother liquor, and wash the polystyrene resin with 600ml of methylal and methanol. Add 60ml of nitrobenzene to swell for 12 hours; control the temperature of the solution at 40°C, and continuously add 80ml of methylimidazole dropwise at a stirring speed of 110rpm to continue the reaction for 8 hours, take it out and filter, rinse with 4% hydrochloric acid, extract, and dry. The resulting product is methylimidazole-modified composite functional ultra-high cross-linked adsorption resin, the resin methylimidazole content is 4.9mmol / g, and the mic...

Embodiment 2

[0031] Take 30g of chlorine balls with a cross-linking degree of 8% (produced by Hebei Langfang Electric Power Resin Factory, etc., with a chlorine content of 18%), add 150ml of nitrobenzene and dissolve it in a 500ml three-necked bottle for 18h; heat up at a speed of 1°C / 4min To 120°C, add 15g of tin chloride at a certain stirring speed, and continue the reaction until the residual chlorine content of the resin is 4%; exhaust the reaction mother liquor, and wash the polystyrene resin with 2L of ethanol and acetone. Add 150ml of nitrobenzene to swell for 8 hours; control the temperature of the solution to 70°C, and continuously add 15ml of imidazole acetate dropwise at a stirring speed of 50rpm to continue the reaction for 6 hours, take it out and filter, rinse with 5% sodium bicarbonate, extract, and dry Dry, the resulting product is imidazole acetate modified composite function ultra-high cross-linked adsorption resin, the imidazole acetate content of the resin is 0.15mmol / g,...

Embodiment 3

[0033]Take 30g of chlorine balls with a cross-linking degree of 8% (produced by Hebei Langfang Electric Power Resin Factory, etc., with a chlorine content of 18%), add 120ml of dichloroethane and swell in a 500ml three-necked bottle for 10h; at a speed of 1°C / 6min Raise the temperature to 40°C, add 9g of ferric chloride at a certain stirring speed, and continue the reaction until the residual chlorine content of the resin is 9%; exhaust the reaction mother liquor, and wash the polystyrene resin with 500ml of acetone. Add 120ml of dichloroethane to swell for 10 hours; control the temperature of the solution at 50°C, and continuously drop 60ml of imidazole at a stirring speed of 90rpm to continue the reaction for 6 hours, take it out and filter, rinse with 7% phosphoric acid, extract, and dry. The obtained product is an imidazole group-modified composite function ultra-high cross-linked adsorption resin, the content of the imidazole group in the resin is 3.1mmol / g, and the microp...

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Abstract

The invention discloses an imidazolyl-modified multifunctional high-crosslinked adsorption resin and a preparation method of the multifunctional high-crosslinked adsorption resin, the building unit of which is represented by the right formula. The preparation method is that: firstly, chloromethyl polystyrene resin is swelled in an organic solvent and catalyst is added into the solution, the temperature of the solution is increased to 20 to 120 degrees gradually, when the content of the residual chlorine in the resin is 4 to 15 percent, the reaction reaches the reaction endpoint, and then the polystyrene-divinylbenzene adsorption resin is obtained; secondly, after the reaction, the reaction mother liquor is pumped out totally, the residual solvent and the residual catalyst are washed away by water or an organic solvent; thirdly, the production is swelled, functionalized imidazole reagent are added into the solution and takes a further reaction with the residual chloromethyl on the inner and the external surfaces of the resin. The preparation method for the imidazolyl-modified multifunctional high-crosslinked adsorption resin has the advantages that: the resin has the double functions of adsorption and ion exchange (coordination); the multifunctional high-crosslinked adsorption resin with the imidazolyl by adopting functional imidazole modification has the hydrophilic imidazole function group and the hydrophobic styrene frame, so the resin has favorable affinity to protein and other biological reagents.

Description

technical field [0001] The invention relates to an imidazole-based modified composite functional ultra-high cross-linked adsorption resin and a preparation method thereof. Background technique [0002] In recent years, due to the characteristics of high specific surface area, diverse surface chemistry, and high mechanical strength, composite functional polystyrene resins have been increasingly widely used in water purification, drug extraction, and chromatographic separation technologies. There have been patent reports on the preparation of imidazole-modified styrene type macroporous adsorption resin, but the resin has not undergone post-crosslinking reaction, the specific surface area is usually very low, basically does not have microporous structure, and has relatively poor adsorption performance for lipophilic organic matter. Poor, the mechanical properties of the resin particles are not high; while the general adsorption resin can only absorb and separate organic matter ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08L25/08C08K5/3445B01J20/26
Inventor 张炜铭潘丙才吕路张全兴陈金龙
Owner NANJING UNIV
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