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A kind of 6-aminopyridine-3-carboxylic acid chelating resin and preparation method thereof

A technology of aminopyridine and chelating resin, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of unreported synthesis methods, and achieve the effects of superior adsorption selectivity, wide application fields, and outstanding application value

Active Publication Date: 2011-12-28
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Literature search shows that there is no report on the synthesis method of aminopyridine resin prepared by using the carboxyl group on the pyridine ring to introduce pyridine into the resin

Method used

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  • A kind of 6-aminopyridine-3-carboxylic acid chelating resin and preparation method thereof
  • A kind of 6-aminopyridine-3-carboxylic acid chelating resin and preparation method thereof
  • A kind of 6-aminopyridine-3-carboxylic acid chelating resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (a) Suspension polymerization

[0027] Add a certain amount of dilute sodium hydroxide solution to the styrene monomer or directly filter the monomer through a resin column equipped with a strong base anion exchange resin to remove the polymerization inhibitor.

[0028] In a 1000 mL beaker, add 210 g styrene, 26 g divinylbenzene, and 140 g liquid paraffin, stir well and set aside.

[0029] In a 1000 mL three-neck flask, add 600 g of distilled water and raise the temperature to 40 °C, then add 6 g of gelatin, stir until completely dissolved, at the same time raise the temperature to 50 °C, add 2 mL of methylene blue, stir evenly, add the above styrene, di Add 4.0 g of initiator benzoyl peroxide to the mixture of vinylbenzene and liquid wax; adjust the stirring speed to make the oil droplet size appropriate, gradually raise the temperature to 80 °C at a speed of 1 °C / 6 min, and keep it warm for 4 h. Then gradually raise the temperature to 85°C for 3 hours, 90°C for 2 hou...

Embodiment 2

[0045] (a) Suspension polymerization

[0046] Using styrene as a monomer, divinylbenzene as a crosslinking agent, liquid wax as a porogen, magnesium carbonate as a dispersant, benzoyl peroxide as an initiator, and a low crosslinking degree synthesized by suspension polymerization The macroporous polystyrene-divinylbenzene copolymer is steam distilled or extracted with ethanol to remove the porogen remaining in the resin pores, and then dried by airflow to obtain low-crosslinked macroporous polystyrene-divinylbenzene Benzene resin, that is, white balls.

[0047] Wherein the dosage of the crosslinking agent is 4% of the total amount of the monomer and the crosslinking agent, the dosage of the porogen is 40% of the weight of the monomer, and the crosslinking degree of the low crosslinking macroporous polystyrene is 2%.

[0048] (b) Chloromethylation

[0049] Soak the white ball in chloromethyl ether which is 4 times its weight, add 20% of the weight of the white ball with zinc ...

Embodiment 3

[0053] (a) Suspension polymerization

[0054] Using styrene as a monomer, divinylbenzene as a cross-linking agent, using No. 200 solvent oil as a porogen, magnesium carbonate as a dispersant, and benzoyl peroxide as an initiator, a low cross-linking agent was synthesized by suspension polymerization. Linked macroporous polystyrene-divinylbenzene copolymer, using industrial alcohol as solvent extraction to remove the residual porogen in the resin pores, and then air-dried to obtain low cross-linked macroporous polystyrene-divinylbenzene resin , the white ball.

[0055] Wherein the dosage of the crosslinking agent is 8% of the total amount of the monomer and the crosslinking agent, the dosage of the porogen is 40% of the weight of the monomer, and the crosslinking degree of the low crosslinking macroporous polystyrene is 2%.

[0056] (b) Chloromethylation

[0057] Soak the white ball in chloromethyl ether which is 7 times its weight, add zinc chloride 50% of the weight of the ...

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Abstract

The invention discloses a 6-aminopyridine-3-carboxylic acid chelating resin and its preparation method, which belongs to the field of chelating resin. The resin has a following structural unit: a functional group is 6-aminopyridine-3-carboxylic acid, wherein the color is yellowish, the particle size is 0.45-0.6 mm, the content of the functional group is 1.37-2.38 mmol / g. The preparation method comprises the following steps: using styrene as a monomer, employing a suspension polymerization method to prepare a low crosslinking degree macroporous styrene-divinylbenzens copolymer, air-flow dryingto obtain low crosslinking macroporous polystyrene-divinylbenzens resin (white ball for short); immersing the white ball in chloromethyl ether, adding zinc chloride as a catalyst, carrying out a chloromethylation reaction to obtain chloromethylated low crosslinking polystyrene-divinylbenzens resin (chlorine ball for short); taking N,N-dimethyl formamide as a swelling agent, taking DMF as a swelling agent to swell the chlorine ball, dissolving 6-aminopyridine-3-carboxylic acid and sodium carbonate in N, N-dimethyl formamide for reaction, then adding the above swelled chlorine ball, stirring for reacting to prepare 6-aminopyridine-3-carboxylic acid chelating resin. The resin prepared by the invention is suitable for selectively absorbing and separating heavy metal ions of copper and the like.

Description

technical field [0001] The invention relates to a chelating resin and a preparation method thereof, in particular to a 6-aminopyridine-3-carboxylic acid chelating resin and a preparation method thereof. Background technique [0002] Pyridine chelating resin is a nitrogen-heterocyclic nitrogen coordination chelating resin, including chelating resins with pyridylamine derivatives and polyvinylpyridine. The nitrogen atom on the pyridine ring has a strong coordination Function, can form stable complexes with metal ions, suitable for selective separation and recovery of heavy metal ions in solution, and has a wide range of application values ​​in analytical chemistry, environmental protection, hydrometallurgy, etc. Chelating resins with pyridylamine derivatives reported at present are usually prepared by reacting chloromethylated polystyrene with pyridyl compounds. The earlier domestic report was seen in 1988, which used the reactivity of the amino groups on 2-aminopyridine, 3-a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F2/18C08F8/24C08F8/32C08J9/28B01J20/26B01J20/30
Inventor 刘福强李保花李兰娟凌晨高洁白志平李爱民游效曾
Owner NANJING UNIV
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