Preparation method of aminopyridine modified resin adsorbing material

An aminopyridine and modified resin technology, applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as inconvenience and long reaction time, and achieve the effects of easy elution, short reaction time and good adsorption performance

Inactive Publication Date: 2014-02-19
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The existing aminopyridine modified resin method has the solvent immersion method reported by Chen Yiyong of Hangzhou University (Chen Yiyong, Lu Buxiang, Synthesis of aminopyridine resin and its adsorption to noble metal ions, Acta Polymerica Sinica, 1989 (4), 437-442) Or soak under the protection of nitrogen atmosphere (Chen Yiyong, Wei Xiang, etc., 3-aminomethylpyridine resin synthesis and comparison of five kinds of aminopyridine resins for gold and platinum adsorption performance, Functional Polymer Science, 1994, 7 (4), 373 -380), the above method requires a long reaction time, reaching more than 15 hours, which is inconvenient in practical application

Method used

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  • Preparation method of aminopyridine modified resin adsorbing material
  • Preparation method of aminopyridine modified resin adsorbing material
  • Preparation method of aminopyridine modified resin adsorbing material

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 8.00g of chlorine spheres (chloromethylated polystyrene spheres) resin into a dry four-neck bottle, add 200mL of 1,4-dioxane to reflux for swelling for 3 hours; accurately weigh 8.30g of 3-aminopyridine ( 3-AP) was added to the above solution, 17.8 g of triethylamine was added, and electromagnetic stirring was used (stirring speed was enough to disperse the resin), and the reaction temperature was controlled at 60°C, and the reaction time was 6 hours. After the reaction, use the Buchner funnel to suction filter, the solvent can be recycled, and then rinse several times with water, absolute ethanol, acetone, ether, etc., the amount of each solvent is about 50 milliliters, the modified 3-aminopyridine resin In a vacuum oven, dry below 60 degrees for later use. The aminopyridine functional group content of the obtained 3-aminopyridine modified resin was 3.1 mmol FG / g resin.

Embodiment 2

[0037]Weigh 7.50g of polyglycidyl methacrylate into a dry four-necked bottle, add 150mL of 1,4-dioxane under stirring at room temperature, reflux and swell for 3 hours; accurately weigh 10.20g of 2-aminopyridine (2-AP ) into the above solution, add 21.3 grams of triethylamine, under the condition of magnetic stirring (stirring speed is enough to disperse the resin), control the reaction temperature to 70°C, and the reaction time to 4h. Using Buchner funnel suction filtration, the solvent can be recycled, and then washed several times with water, absolute ethanol, acetone, ether, etc., the amount of solvent is about 50 ml each time, the modified resin is in a vacuum oven, less than 60 Dry it for later use. The aminopyridine functional group content of the obtained 2-aminopyridine modified resin was 3.5 mmol FG / g resin.

Embodiment 3

[0039] Weigh 9.00g of chlorine ball resin and place it in a dry four-necked bottle, add 200mL of toluene, and swell under reflux for 5h; accurately weigh 11.50g of 2-aminopyridine (2-AP) and add it to the above solution, add 23.5g of triethylamine, Under the condition of magnetic stirring (stirring speed is enough to disperse the resin), the reaction temperature is controlled at 55°C, and the reaction time is 6h. After the reaction, use Buchner funnel to suction filter, the solvent can be recycled, and then rinse several times with water, absolute ethanol, acetone, ether, etc., the amount of solvent is about 50 ml each time, and the modified resin is stored in a vacuum oven. , Dry below 60 degrees for later use. The aminopyridine functional group content of the obtained 2-aminopyridine modified resin was 2.9 mmol FG / g resin.

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Abstract

The invention relates to a preparation method of aminopyridine modified resin, which comprises the steps of allowing high polymer resin to swell in an organic solvent under backflow, adding an aminopyridine compound with a charge ratio of (1-7):1 to the high polymer resin, and an acid-binding agent at a mole ratio of (1-5):1 to the aminopyridine compound, allowing a mixed reaction system to react for 2-24h at 45-70 DEG C under a stirring condition to form the aminopyridine modified resin, separating, washing sequentially with water, alcohol, acetone and ether, and airing to form the aminopyridine modified resin of which a functional group content is 2.9-4.0mmol FG/g. The method is simple to operate, short in reaction time and convenient in preparation, and the modified resin can be independently used or filled as an adsorbing column, has good adsorbability for metal, particularly rhodium octanoate dimer in industrial waste water, and metal ions, particularly noble metal ions, and has important applications in environmental protection, analytical chemistry, metal ion extraction from waste liquid and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of modified polymer resin materials, and in particular relates to a preparation method and application of aminopyridine modified resin adsorption materials. Background technique [0002] Aminopyridine (AP) is a common important intermediate in the synthesis of medicines, dyes, and pesticides, and can also be used as a drug and analytical reagent. Both the amino group and the nitrogen atom of the pyridyl group in aminopyridine compounds have strong coordination functions, and can coordinate with many metal ions to form stable complexes. Therefore, pyridine rings are often used as functional groups of chelating resins. In addition, the nitrogen atom in the pyridine ring in the aminopyridine molecule has certain basicity and nucleophilicity, so aminopyridine can be widely used in the preparation of supernucleophilic catalysts with excellent performance. The amino group in the ami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F12/08C08F20/32C08F8/32B01J20/26
Inventor 庞雪蕾王荣耕赵海燕
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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