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Method of aminopyridine modified resin for adsorbing rhodium octanoate dimer and metal ions

A technology of aminopyridine and modified resin, applied in chemical instruments and methods, ion exchange, selective adsorption, etc., can solve the problems of long production cycle, large discharge of three wastes, damage, etc., and achieve the effect of simple method and good adsorption performance

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

AI Technical Summary

Problems solved by technology

The advantage of this method is that it is easy to implement and easy to operate, but its disadvantages are high energy consumption, long production cycle, large discharge of three wastes, and the components of rhodium octanoate are destroyed, so only rhodium chloride can be recovered and cannot be used again.

Method used

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  • Method of aminopyridine modified resin for adsorbing rhodium octanoate dimer and metal ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 8.00g of chlorine ball resin and place it in a dry four-necked bottle, and add 200mL of 1,4-dioxane to reflux for swelling for 3h; accurately weigh 8.30g of 3-aminopyridine and add it to the above solution, and add 17.8g of triethylamine , using electromagnetic stirring (stirring speed is enough to disperse the resin), control the reaction temperature to 60°C, and the reaction time to 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 functional group content of the obtained modified resin was 3.1 mmol FG / g resin.

[0034] Pretreatment of 3-aminopyridine modified resin: wash with warm water first, then soak in 0.1mol / L NaOH solution for 17h, wash with water until neutral, then soak with (0.1mol / L) HCl solu...

Embodiment 2

[0036] 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 into the above solution , add 21.3 grams of triethylamine, under the condition of magnetic stirring (the stirring speed can be dispersed by 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 functional group content of the obtained modified resin was 3.5 mmol FG / g resin.

[0037] Pretreatment of 2-aminopyridine modified resin: wash with warm water first, then soak in 0.1mol / L NaOH solution for 20h, wash with water until neutral, then soak with (0.1mol / L) HCl solut...

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 and add it to the above solution, add 23.5g of triethylamine, and stir under magnetic force ( Stirring speed is enough to disperse the resin), control the reaction temperature to 55°C, and the reaction time to 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 functional group content of the obtained modified resin was 2.9 mmol FG / g resin.

[0040] Pretreatment of 2-aminopyridine modified resin: wash with warm water first, then soak in 0.1mol / L NaOH solution for 15 hours, wash with water until neutral, then soak with (0.1mol / L) HCl solution f...

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Abstract

The invention relates to a method of aminopyridine modified resin for adsorbing rhodium octanoate dimer and metal ions. The aminopyridine modified resin serves as an adsorbent, and adsorbs rhodium or the metal ions from a solution containing rhodium octanoate dimer or other metal ions on the surface, and metal is effectively recovered. The method comprises the steps of aminopyridine modified resin preparation and pretreatment. In an adsorbing step, the aminopyridine modified resin can be used independently or filled as an adsorbing column. The resin has good adsorbability for the metal ions, particularly rhodium octanoate dimer in industrial waste water, rhodium octanoate dimer can be directly recovered, and a rhodium octanoate dimer preparation process of condensing, burning and pickling rhodium octanoate dimer in the solution to prepare rhodium chloride to react with octanoic acid. The method is simple, and is very easy to implement in a laboratory or middle and small chemical plants.

Description

technical field [0001] The invention belongs to the application technical field of polymer resin materials, in particular to an aminopyridine-modified resin to a rhodium (II) dimer in solution (hereinafter referred to as rhodium octanoate) and a method for recovering metal ions. Background technique [0002] Rhodium(II) octanoate dimer is a carboxylic acid complex of rhodium, which has remarkable catalytic activity for C—H insertion reaction and is an important catalyst. The synthesis of rhodium octanoate was first reported by Giround-Godguin et al. in 1986. At present, the synthesis of rhodium octanoate mainly adopts the ligand exchange method, that is, rhodium acetate is mixed with excess octanoic acid, and rhodium octanoate is obtained through a coordination substitution reaction. Due to the lack of rhodium resources and the complex production process of rhodium octoate, the price of rhodium octoate is expensive. [0003] As a catalyst, rhodium octanoate has outstanding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01D15/08C07C53/126C07C51/47C22B7/00C22B11/00C22B15/00C22B34/32
Inventor 王荣耕庞雪蕾赵海燕
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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